Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
2 0 1 6
International Seminar on
PROCEEDINGS
January 5 - 7, 2016
TCS Sahyadri Park Campus,
Hinjewadi, Pune
PLATINUM SPONSORS
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Contents
1.1 Invited The role of convergence technologies for the utilization of bauxite residue to man-
ufacture green cement ’Calcium Sulfo Aluminate (CSA)’
Thenepalli Thriveni , Ahn Ji Whan . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.2 Deformation behaviour of Al-10% red mud particle reinforced nano composites: Wear
studies
G Satyanarayana, G Swami Naidu , N Hari Babu . . . . . . . . . . . . . . . . . . . . . 13
2 Beach Sands 21
2.1 A study on mineralogical characterization of leucoxene and its separation from other
minerals
Simanchal Rath, Franflin Daniel , A J Janarthanan , C K Asnani . . . . . . . . . . . . . 22
2.2 Processing of indigenously mined columbite tantalite ore for production of pure tantalum
and niobium oxide
G Samyuktha, K V Mirji , Sheela , N Saibaba . . . . . . . . . . . . . . . . . . . . . . . 30
2.3 Value addition of ilmenite-Opportunities and challenges
G Krishna Kumar . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
2.4 Evaluation and processing study of rare earth elements in the Gazestan deposit (central
Iran)
R Mollataheri, S Afsari , D Piruzan . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
2.5 Understanding the performance of gravity concentration circuits for placer minerals: A
review
Karamjith Sharma , Y Rama Murthy , R Venugopal . . . . . . . . . . . . . . . . . . . . 56
2.6 Innovation In Exploitation Of Monazite Mineral in order to extract Thorium
Aadri Vishal, Tonmit Talukdar , Vishwas Kumar . . . . . . . . . . . . . . . . . . . . . . 68
3.1 Effects of reagents and kinetic studies on flotation performance of Dugda coal
Abhyarthana Pattanaik, R Venugopal , Diptimayee Nanda . . . . . . . . . . . . . . . . 76
3.2 Analysis of effect of dissolved ion-water chemistry on the performance of coal flotation
Mousumi Gharai, R Venugopal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
i
3.3 Studies on separation of macerals from coal by froth flotation
Saroj Kumar Sahoo, Nikkam Suresh , A K Varma . . . . . . . . . . . . . . . . . . . . . 98
3.4 Characterization of coal fines and its influence on dewatering of tailing slurry
Shravan Kumar, S Bhattacharya , N R Mandre . . . . . . . . . . . . . . . . . . . . . . 110
3.5 Study on process consumables and identification of sources of media losses at west
Bokaro
Kunal Mathanker, Bijay Shankar Tiwari , D P Chakraborty . . . . . . . . . . . . . . . . 116
3.6 Studies on caking behavior of wet bulk solids due to storage and consolidation stress
T V S Subrahmanyam, Somiran Mondal , Rajan Kumar . . . . . . . . . . . . . . . . . . 123
3.7 Beneficiation of oxidized coking coal fines through froth flotation
Nanda Kishore Patra, Shalini Gautam , Sanjay Choudhuri , T Gouri Charan . . . . . . 131
3.8 Development of a combined beneficiation process for ash reduction in finer size coals
Suribabu Pandiri, T Umadevi , Mudhunuru Varma Raju , R Sah , K Marutiram . . . . . 139
3.9 Insights into the abnormal characteristics of tertiary coals in Makum coalfield, Assam for
their efficient end utilization
Sujoy Chattaraj, Bageshwari Sanga , Akanksha , Hindol Ghatak , Debadutta Mohanty . 147
3.10 Performance of water-only cyclone to treat open cast coal mines
Abhishek Anand Hembrom, Nikkam Suresh . . . . . . . . . . . . . . . . . . . . . . . . 159
3.11 Characterisation studies of low volatile high rank coal and cleaning products
Divya Jyoti, Sumantra Bhattacharya , Sanchita Chakraborty , Vinod Kumar Saxena . . . 166
3.12 Comparative study of jigging and DMS for coal on laboratory scale
Abhijeet Manasingh, Abhisek Mohapatra , Lenin Mohapatra , Kotini Rahul Ganesh . . . 173
3.13 Assessment of coking potentials of coal blends of coking coal and non-coking coal
Shaik Saida, Sanchita Chakravarthy , Rina Sahu . . . . . . . . . . . . . . . . . . . . . 180
3.14 Chemical treatment of high sulphur coal and its characterization study
Bhupendra Singh Ken, Alok Kumar , V K Saxena . . . . . . . . . . . . . . . . . . . . . 183
3.15 Necessity of GPS-based proximity warning system in mining industry - A tool to prevent
mine transport accidents
Krishan Kumar Aggarwal, Akash Aggarwal , Utkarsh Tripathi . . . . . . . . . . . . . . 190
4.1 Crash stop analysis of an industrial dry grinding ball mill: Performance evaluation and
modelling
K Bhanu Venkatesh, S Dwarapudi , Abhishek Choudhary , Narasimha Mangadoddy , Veerendra Prakash
, B K Chatterjee . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 198
5.1 Invited Stability assessment and remedial measures adopted for tailing dumps at Hutti
Gold Mines
Prabhakar Sangurmath, T J Sri Sriraghava . . . . . . . . . . . . . . . . . . . . . . . . 208
5.2 Beneficiation studies on a gold ore sample from Togo, Africa
B Suresh Kumar, Dev Prasad Ananth , Indira Ravindran . . . . . . . . . . . . . . . . . 215
5.3 Flotation studies on a copper plant tails sample of Democratic Republic of Congo
V A J Aruna, Prathama Diwakar , P P Pathak , B R Ramteke , Sandhya Lal . . . . . . . 221
5.4 Significance of beneficiation studies on a very lean grade copper ore from central Indian
view of mineral conservation : A case study
M G Raut, V A J Aruna , Sandhya Lal . . . . . . . . . . . . . . . . . . . . . . . . . . . 229
5.5 Comparision studies of grates and modified grates on SAG mill performance in the pro-
cessing of gold ore at the Hutti Gold Mines Company Limited
Gurubasayya, Umesh Bellad . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 233
5.6 The studies of determination of grinding time on rougher flotation on rangin flez copper
concentration plant.
Amir Pazoki, Ali Pourbahaadini . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 243
6.1 Amenability of Au CIP plant tails to pelletization for mine back fill
B P Ravi, P Sharathkumar , C Rudrappa , M V Rudramuniyappa , G Shaila . . . . . . . 252
6.2 Environmental pollution and forming of Kermanshah Ophiolitic complex (West of Iran)
Reza Zarei Sahamieh, Ali Moradpour . . . . . . . . . . . . . . . . . . . . . . . . . . . 258
6.3 Utilisation of manganese dump rejects of central India region for industrial applications
V A Sontakkey, Ipsita Mohanram , R S Aehdi , V A J Aruna , S M Lal . . . . . . . . . . . 274
6.4 Economical and environment friendly recycling of PCBs from DVDs for recovery of met-
als adopting physical beneficiation process
Vinod Kumar, Jae-chun Lee , Jinki Jeong , Manis Kumar Jha , Byung-su Kim , Ratnakar Singh
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 280
6.5 Energy generation from coal mine waste
D S Panwar, V K Saxena , A K Singh . . . . . . . . . . . . . . . . . . . . . . . . . . . 289
7.1 Invited Process compression and flowsheet development for the mining and metallurgical
industry
V I Lakshmanan, R Sridhar , M A Halim . . . . . . . . . . . . . . . . . . . . . . . . . . 296
7.2 Mathematical modelling of alkaline leaching of uranium
K Anand Rao, T Sreenivas , J K Chakravartty . . . . . . . . . . . . . . . . . . . . . . . 305
7.3 Hydrometallurgy of beryllium in Indian perspective
D D Thorat, P K Sinha , J K Chakravartty . . . . . . . . . . . . . . . . . . . . . . . . . 318
7.4 Indian strategic minerals - A review
Patel Himeshkumar Ashokbhai, Suchit Sharma . . . . . . . . . . . . . . . . . . . . . . 326
9.1 Preliminary beneficiation studies on Barsua iron ore by spiral concentrator followed by
WHIMS
Satyananda Patra, R Venugopal . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 410
9.2 Beneficiation of iron ore slimes using a natural polymer by selective flocculation process
Rakesh Kumar, N R Mandre . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 421
9.3 Beneficiation of low-grade iron ore fines by using selective flocculation
Kichakeswari Tudu, N R Mandre . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 429
9.4 Optimization of pelletization process for iron ore with high alumina by use of high silica
fluxes
Dhiraj Kadhe, Abhishek Kumar , T Umadevi , Marutiram Kaza , R Sah , K Sampath . . . 435
9.5 Cold bonded pelletization of low grade goethitic iron ore fines
Jyoti Sharma, T Sharma , N R Mandre . . . . . . . . . . . . . . . . . . . . . . . . . . . 447
9.6 Upgradation and maximization of Fe recovery from process waste through flotation
Varun Kakathkar, Supartick Gupta , Raghavendra Kandare , Rameshwar Sah , K Marutiram
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 452
9.7 Beneficiation of low grade iron ore using enhanced gravity concentrator
Sourav Gupta, Aditya Ranjan . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 460
9.8 Beneficiation of specularite
B P Ravi, S J Gopalkrishna , P Sharthkumar , M R Patil , P C Naganoor . . . . . . . . . 472
9.9 Re-jigging of jig tailings to recover blast furnace grade iron ore concentrate
Dilip Makhija, Prashant Dixit , A K Mukherjee . . . . . . . . . . . . . . . . . . . . . . 479
9.10 Feasibility studies on beneficiation of sub grade iron ore from deposit 5, Bacheli complex,
Bailadila, Chhattisgarh using Mozley mineral separator
G Venkateswara Rao, R Markandeya , Rajan Kumar . . . . . . . . . . . . . . . . . . . 488
9.11 Feasibility of producing sinter fines from a low grade and fine grained hematite-goethitic
ore
R K Rath, M K Mohanta , R Singh . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 500
9.12 Study on pelletisation of iron ore slimes (concentrate) using non-conventional and con-
ventional binders
Ashiwani Bharti . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 507
9.13 Studies on characterization and beneficiation of low grade iron ore fines from Gua ore
mines (SAIL), Jharkhand
Rahul Ganesh Kotini, Ram Pravesh Bhagat . . . . . . . . . . . . . . . . . . . . . . . . 514
11.1 Characterisation and assessment of goethite rich iron ore for beneficiation from deposit
14 & 11c, Kirandul complex, Bailadila, Chhattisgarh, India
Basant Rath, G Venkateswara Rao , Rajan Kumar . . . . . . . . . . . . . . . . . . . . . 530
11.2 Bauxite mineralogy at Mombi deposit SW Iran.
Hassan Zamanian . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 544
11.3 Mineralogical and geochemical evolution of the bauxite ores from Gadhsisa group of
mines, Kachchh, Gujarat, India
P S Choudhury, D U Vyas , G N Jadhav , N N Sharma . . . . . . . . . . . . . . . . . . 550
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THE ROLE OF CONVERGENCE TECHNOLOGIES FOR THE UTILIZATION OF BAUXITE
RESIDUE TO MANUFACTURE GREEN CEMENT “CALCIUM SULFO ALUMINATE (CSA)”
Korea Institute of Geosciences and Mineral Resources (KIGAM), Daejeon, 124 Gwahagno,
*Corresponding author: ahnjw@kigam.re.kr
Abstract
The objective of this paper is to discuss about the role of convergence technologies for the utilization of
bauxite residue (red mud) to manufacture green cement called “Calcium Sulfo Aluminate” and
simultaneous CO2 capture and utilization (CCU). Convergence technologies offered a lot of benefits and
opportunities to overcome the environmental challenges. Bauxite residue or red mud is generated in the
Bayers process of aluminium. The disposal of the red mud or storage is a major threat to the environment
due to its caustic nature. The researchers still searched for the opportunities to reuse bauxite residue. The
bauxite residue can be used for construction back fill, general fill, and use in road base construction or
golf bunker sand. Sustainable recycling technologies are necessary for the bauxite residue utilization for
the recovery of rare earth elements and cement materials. Carbonation or CO2 sequestration of carbon
dioxide, a method pioneered for the bauxite residue is modified to reduce alkalinity. The carbonation of
alkaline material is an inexpensive and safe process that leads to the formation of thermodynamically
stable products. The use of the carbonation can be an advantageous solution for overcoming problems
associated with red mud storage and the emissions of several thousand tons of CO2 from aluminium
manufacturers each year. In this paper, we report the convergence technologies for the utilization of
bauxite residue by ecofriendly carbonation and also the recovery of rare earths from bauxite residue.
1. Introduction
In alumina production or alumina refining, bauxite is converted to alumina (aluminium oxide) using the
Bayer Process.1 Aluminium is integral to our everyday lives. It is used in trains, planes, cars and buses,
laptops, mobile phones, DVDs, building construction, outdoor furniture, screw cap bottle tops, beverage
cans, aluminium foil and so much more. Growth in primary aluminium production continues to be driven
by China and the Arabian Gulf. Fig. 1 shows the global primary aluminium production in 2012 was a
record 46 million tonnes.2 Bauxite residue, sometimes referred to as ‘red mud’ is the by-product of the
Bayer process. In the Bayer process, bauxite ore is dissolved using sodium hydroxide (caustic soda).
Alumina is then extracted from the solution and the residual bauxite residue is sent to a storage area. The
characteristic red color of bauxite residue results from the high concentrations of naturally occurring iron
compounds in the original bauxite ore.
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Figure 1: Global primary aluminium production, 1990 & 2006-2012 (SOURCE: IAI & CRU).
2. Alumina processing
Refining alumina (aluminium oxide) is the second step in the production of aluminium. Alumina is
refined from bauxite using a chemical process known as the Bayer process. This process proceeded by 4
ways3
i) digestion-bauxite is finely ground in mills and then mixed with a hot, caustic soda solution which
dissolves the alumina contained in the bauxite.
ii) clarification- the solution of alumina and caustic soda passes into rows of thickener tanks, where
the solid impurities sink to the bottom as fine red mud, a by-product of the process. It is
washed several times with water, neutralized, and then stored at the residue management area.
The clear solution is sent to precipitation for the alumina to be recovered from it.
iii) precipitation- alumina trihydrate is added to the alumina solution in a line of precipitation tanks to
seed the formation of additional alumina trihydrate crystals.
iv) calcination- the alumina trihydrate crystals are washed, filtered and then heated in gas-fired kilns
at temperatures greater than 11000C to remove water molecules, creating a fine white powder
known as alumina.
3. Bauxite residue (red mud)
Throughout the entire history of alumina production, there has been a desire to utilize the bauxite residue
created in the Bayer process with either by recovering additional products from it or using it. The red mud
applications falls into several categories such as rare earths recovery, manufactured construction materials
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(cement, bricks, tiles, aggregate blocks and wood substitute) and bulk impermeable material for covering
landfill. Considerable effort has been expended in finding applications for bauxite residue but a number
of key factors affect the feasibility and economics of its adoption. The main application areas that have
been evaluated are briefly summarized below:
Table 1: Composition of redmud4.
Contents Typical Composition
Al2O3 15-19%
Fe2O3 33-40%
SiO2 10-15%
TiO2 4-6%
CaO 3-9%
MgO 0.3-1.0%
Na2O 7-11%
V2O5 0.2-0.4%
P2O5 0.5-1.0%
CO2 2-3%
As shown in Table 1, red mud contains a considerable amount of titania. Although this concentration is
less to utilize but this titanium is a metal and alloying ingredient of strategic importance in defense and in
the aerospace industries and also utilizes in producing medical implants and chemical catalysts etc.
4. Utilization
China, above 10% utilizes the red mud for metal recovery or for brick production. In Australia ALCOA
and Japan tried to utilize red mud in the building and construction materials produced from it and as an
additive in cement production.
The main application areas that have been evaluated are cement production, Road construction, brick
production, iron production, acid mine drainage and heavy metals absorption.
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elements from Bayer Process red mud includes the following steps: (a) digesting red mud containing rare
earth elements with a dilute acid solution, e.g. sulphur dioxide dissolved in water, to selectively dissolve
the rare earth elements while leaving iron in the red mud substantially undissolved; (b) separating the
solution obtained from the solid residue and (c) recovering the rare earth elements from the solution8.
Only a few processes are reported for extraction of scandium from red-mud, the residue generated from
the bauxite9-12. Solvent extraction technology has been used for the recovery of scandium from leach
solutions. A number of extractants can be used for scandium extraction13,14.
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Table 2: Rare earth elements in red mud
Analyte Compound Measured Used Concentration
formula (kcps) (kcps) (%)
H2O 8.22
Na Na2O 71 77.321 10.767
Mg MgO 1.377 1.499 0.135
Al Al2O3 204.404 247.345 22.723
Si SiO2 136.413 165.071 18.87
P P2O5 4.194 4.602 0.283
S SO3 5.917 6.505 0.367
K K2O 0.707 0.772 0.034
Ca CaO 40.993 44.779 2.439
Ti TiO2 154.19 168.429 7.779
Cr Cr2O3 1.736 1.852 0.095
Mn MnO 0.587 0.418 0.02
Fe Fe2O3 600.378 640.725 27.662
Ni NiO 0.263 0 0.01
Zn ZnO 0.116 0.132 0.004
Ga Ga2O3 0.259 0.293 0.007
Y Y2O3 1.151 1.187 0.011
Zr ZrO2 32.997 36.129 0.348
Nb Nb2O5 1.329 1.455 0.013
Ba BaO 0.475 0.518 0.076
Pb PbO 0.509 0.578 0.014
Cl Cl 2.905 3.195 0.107
Th ThO2 0.812 0.923 0.014
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The developed innovative residue treatment process that delivers a range of sustainability benefits. The
carbonation of red mud, in which CO2 adds to bauxite residue which is a mixture of minerals that are left
behind when alumina is removed from bauxite. Carbonation of red mud has tremendous environmental
benefits, economic and social benefits by reducing residue drying times and less residue storage.
We investigated the red mud carbonation and carbonation efficiency by XRD (Fig. 2) and TG-DTA
analysis of red mud (Fig. 3).
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1200 1100
Sintering Temp (℃) 1300~1400
[8hrs] [8hrs]
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More ettringite formation or expansion after drying gives less cracking for buildings.
9. Conclusions
This preliminary data in the present study have indicated that the red mud carbonation at ambient
conditions (temperature of 25 1°C and atmospheric pressure) could present an effective option for the
carbon dioxide sequestration. The carbonation efficiency of red mud is 2.18 g CO2/kg. The results are
indexed that a promising parameter for CSA is strength and it would be an interesting extension. The use
of this type of system could thus become a source of additional income for aluminum manufacturers and
reduce environmental problems associated with red mud storage.
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References
1. World Aluminium, Global life cycle inventory data for the primary aluminium industry 2010 data,
published 2013.pp.1-53.
2. International Aluminium Institute, “Results of the 2012 Anode Effect Survey” 2012. pp.1-24.
3. Sustainable development report, Rio Tinto Alcan Yarwun, 2012, pp.1-66.
4. Kozeky Laszlo, Utilization of the red mud, 2012, pp.1-14.
5. P. M. Orhsenkiihnn, T. Lybempudu, and K. M. Ochsenkiihn, Recovery of lmththanides and
yttrium from red mud by selective leaching, Analytica Chimica Acta, 319, 1996, pp. 249 - 254.
6. M. Ochsenk¨uhn-Petropulu, T. Lyberopulu, and G. Parissakis, Selective separation and
determination of scandium from yttrium and lanthanides in red mud by a combined ion
exchange/solvent extraction method,” Analytica Chimica Acta, 315(1-2), 1995, pp. 231–237.
7. D. I. Smirnov, T. V. Molchanova, The investigation of sulphuric acid sorption recovery of
scandium and uranium from the red mud of alumina production, Hydrometallurgy, 45(3), 1997,
pp. 249–259.
8. George D. Fulford, Gordon Lever, Taichi Sato, Recovery of rare earth elements from bayer
process red mud, US Patent No. 5,030,424, July 9, 1991.
9. P.K.N. Raghavan, N.K. Kshatriya, K. Wawrynink, Recovery of metal values from red mud. In:
Lindsay, S.J. (Ed.), Light Metals 2011. John Wiley & Sons, Inc., Hoboken, NJ USA, 2011, pp.12-
15.
10. S. Samal, A.K. Ray, A. Bandopadhyay, Proposal for resources, utilization and processes of red
mud in India -a review. International Journal of Mineral Processing 118, 43, 2013, pp.1-55.
11. H. Zhou, L. Dongyan, Y. Tian, Y. Chen, Extraction of scandium from red mud by modified
activated carbon and kinetics study, Rare Metals, 27 (3), 2008, pp.223–227.
12. Abhilash, Shivendra Sinha, Manish Kumar Sinha, Banshi Dhar Pandey, Extraction of lanthanum
and cerium from Indian redmud, International Journal of Mineral Processing, 127, 2014, pp. 70-
73.
13. W. Wang, C.Y. Cheng, Separation and purification of scandium by solvent extraction and related
technologies: a review, J. Chemical Technology and Biotechnology, 86, 2011, 1237-1246.
14. Weiwei Wang, Yoko Pranolo, Chu Yong Cheng, Recovery of scandium from synthetic red mud
leach solutions by solvent extraction with D2EHPA, Separation and Purification Technology, 108,
2013, pp. 96-102.
15. Danielle Bonenfant, Lynda Kharoune, Sebastien Sauve, Robert Hausler, Patrick Niquette,
Murielle Mimeault, Mourad Kharoune, CO2 Sequestration by Aqueous Red Mud Carbonation at
Ambient Pressure and Temperature, Ind. Eng. Chem. Res. 47, 2008, pp. 7617–7622.
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16. C. Brunori, C.Cremisini, P.Massanisso, V.Pinto, L.Torricelli, Reuse of a treated red mud bauxite
waste: studies on environmental compatibility, Journal of Hazardous Materials B,117(1), 2005,pp.
55–63.
17. Y.Pontikes,G.N. Angelopoulos, Bauxite residue in cement and cementitious applications: Current
status and a possible way forward, Resources, Conservation and Recycling, 73, 2013, pp.53-63.
18. G.Stavrinides, Alternative cements in concrete construction. University College London:
Assessment, Prospects & Commercialisation Strategies [MSc.]; 2010.
19. M.Schneider, M. Romer, M.Tschudin, H.Bolio, Sustainable cement production present and future,
Cement and Concrete Research, 41, 2011, pp. 642–50.
20. C.Shi, A.F.Jiménez, A.Palomo, New cements for the 21st century: the pursuit of an alternative to
Portland cement, Cement and Concrete Research, 41, 2011, pp.750- 63.
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DEFORMATION BEHAVIOUR OF AL-10 WT% RED MUD PARTICLE REINFORCED NANO
COMPOSITES – WEAR STUDIES
Satyanarayana G 1*, Swami Naidu G 2 Hari Babu N 3
1
Department of Mechanical Engg., M R A G R Government Polytechnic, Vizianagaram, Andhra Pradesh,
India.
2
Department of Metallurgical Engg., JNTUK University College of Engg., Vizianagaram, Andhra
Pradesh, India.
3
Department of Mechanical Engg., Aditya Institute of Technology and Management, Srikakulam, Andhra
Pradesh, India.
*Corresponding author: gsn569@gmail.com
Abstract
Nanoscience and nanotechnology has become the buzzword in recent years and it literally means any
technology performed in the nanoscale down to molecular level. It is generally agreed that resistance to
wear and other mechanical properties of MMNCs can be improved remarkably by introducing hard
intermetallic compound into the aluminium matrix. In view of the generation of large quantities of red
mud during the production of alumina from bauxite, an attempt is made to see the possibility of adding
red mud solid waste as reinforcing particles in Aluminium matrix to produce the low cost, light weight
and wear resistant metal matrix nano composites. The micro sized redmud particles have been modified
to nano structured red mud using High energy ball milling and after 30 hours of ball milling, the size was
reduced from 106 microns to 40 nanometers. Composites were fabricated by stir casting and experiments
were conducted under laboratory condition to assess the wear characteristics of Al- 10 wt% red mud
(micro sized) and Al- 10 wt% red mud (nano structured) composites under different working conditions
in pure sliding mode on a pin-on-disc machine. The hardness of the composites with coarse grained red
mud particle reinforcement was significantly increased with increase in deformation under compression.
On the other hand, the hardness measurements of the composites with nano structured red mud particle
reinforcement were decreased with increase in deformation under compression which is due to strain
softening occurred under compression. The wear rate of the composites was decreased with deformation
and for deformations beyond 30%, the wear rate was increased due to strain softening. The increased
frictional thrust at higher load results in increased debonding and caused easy removal of material and
hence the wear rate is increased with increase in normal load. The coefficient of friction in all cases is
decreased with the increase of normal load. This is attributed to the wear of the matrix from the pin
surface leaving the particulates standing proud.
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Keywords: Redmud, Nano composites, Ball milling, Wear, deformation.
1. Introduction:
Nanostructured materials exhibit unusual physical and mechanical properties compared to the coarse
grained ones and hence they are of great research interest. Extensive researches have been conducted to
investigate the plastic deformation and the micro structural evaluation of the nanostructured materials due
to the scientific and technological importance. The nanostructured materials are produced by various
methods and high energy ball milling is one of the most convenient techniques to produce powders of
nano level. A critical appraisal of the current state of understanding and of possible avenues for further
exploration in the broad field of mechanical properties of nanoscrystalline metals and alloys, particularly
in the context of processing-structure property connections, seems appropriate at this time. A good
combination of high strength and ductility of the Aluminium based metal matrix composites have
introduced the material to a wide area of possible advanced applications. Discontinuously reinforced
metal matrix composites have received much attention because of their improved specific strength, good
wear resistance and modified thermal properties (Rittner, 2000). There is a variety of manufacturing
processes available for discontinuous metal matrix composites; stir casting is generally accepted as a
particularly promising route, currently practiced commercially. In general stir casting of MMCs involves
producing a melt of the selected matrix material, followed by introducing reinforcement material into the
melt, obtaining a suitable dispersion through stirring. Its advantages lie in its simplicity, flexibility and
applicability to large quantity production, (Hashim et al., 1999). It is also attractive because, in principle
this method suitable for engineering application in terms of production capacity and cost efficiency (Zhou
et al., 1997).
Wear behaviour of aluminium matrix composite was studied by Rosenberger et al., in which the matrix
alloy AA6061, was reinforced with Al2O3, B4C, Ti3Al and B2Ti in volume fraction ranging from 5% to
15%. The Al-fly ash composite has shown better wear resistance compared to unreinforced alloy upto a
load of 80N and fly ash particle size and its volume fraction significantly affect the wear and friction
properties of composites (Sudarsan et al., 2008). The effects of sliding velocity on the frictional and wear
behaviour of aluminium MMC sliding against ferrous counter body have been studied by a number of
researchers (Manish Narayan et al., 1995, Lee et at., 1992 and Kwok et al., 1999).
An attempt has been made to study the wear behaviour of the Aluminium Metal Matrix nano composite
with 10 wt% nano structured redmud as reinforcement. Emphasis is given in the present investigations to
determine the effect of deformation on wear behaviour of these composites.
14
Bauxite & Laterites
2. Experimental Studies
2.1 Materials and High energy ball milling
Aluminium based metal matrix composites containing 10 wt% nano structured red mud particulates are
synthesized by stir cast (vortex) method. Commercially pure Aluminum with 99.5% purity obtained from
NALCO is used as the matrix material. Red mud, a solid waste during the production of alumina is used
as reinforcement phase in the present investigations. Red mud sample of 1 Kg weight is taken in a
graphite crucible and allowed to preheat in the muffle furnace at 10000 C for 2 hours to find out the loss
on ignition and it is found to be 7.56%. Milling is carried using high energy ball milling for 30 hours and
X-ray diffraction measurements are carried out with the help of a Goniometer model 2036E201 using Cu
Kα radiation (Kα = 1.54056 A0) at an accelerating voltage of 40 kV and a current of 20 mA. A steady
decrease in the crystallite size is observed and it is found that the crystallite size has been reduced from
106 µm to 40 nm in 30 hr of milling
15
Bauxite & Laterites
with woollen cloth to avoid entrapment of wear debris and to achieve uniformity in experimental
procedure.
3. Results and Discussion
3.1 Hardness tests
The composites with coarse grained red mud reinforcement and nano red mud reinforcement are tested
for the hardness using Vickers hardness tester and the results are furnished in table 1. A significant
increase in hardness is observed with increase in deformation for the composites with coarse grained red
mud particle reinforcement. This is due to the strain hardening that occurred in conventional coarse
grained materials and is related to dislocation movements. On the other hand, the hardness measurements
of the composites with nano red mud particle reinforcement are not increased with increase in
deformation under compression which is due to strain softening occurred under compression. It is
consistent with the studies reported by Ko et al (2005) on compression of fine grained aluminium alloys
at room temperature.
Table 1. Vickers hardness measurements
Metal Matrix Composite VHN.
0% def 10% def 20% def 30% def 40% def
Al + 10% micro sized Red mud 50.24 56.44 63.21 69.34 76.06
Al + 10% nano structured red mud 54.36 55.94 56.88 50.42 48.28
16
Bauxite & Laterites
the surface energy and inter atomic bonding will also increase. This might be the reason for the increase
in wear resistance of nano particle reinforced composites.
An increase in wear rate is observed with increase in normal load. This is because, the increased
frictional thrust at higher load results in increased debonding and causes easy removal of material. The
similar effect of normal load on volumetric wear rate has been observed by Cirino et. al. (1987) in the
case of carbon epoxy composite.
0.35 0.35
Wear ratex 10-6 N/m
0.3
(a) (b)
0.35
Wear ratex 10-6 N/m
(c)
Figure 1. The effect of load and particle size on wear rate with sliding distance (a) 200 rpm (b) 400 rpm
(c) 600 rpm
17
Bauxite & Laterites
deformation on wear rate with sliding distance at 30N load and at different sliding velocities are furnished
in Fig 2.
0.3
0.35
Wear rate x 10-6 N/m
0.35
Wear rate x 10-6 N/m
0.3
0.25
0.2
0.15 0%
10%
0.1 20%
0.05 30%
40%
0
0 5 10 15
Sliding Distance x 103 m
(c)
Figure 2. The effect of deformation on wear rate with sliding distance at load 30N and (a) 200RPM, (b)
400RPM and (c) 600 RPM
18
Bauxite & Laterites
aluminium. This might be due to (Savchenko et al., 2002) strain hardening of aluminium during sliding
with the applied load and due to pulling up of hard red mud particles from the aluminium grain
boundaries (Korkut, 2004).
a b c
a b c
w
4. Conclusions:
After 30 hours of milling the red mud is reduced from 106 µm to 40 nm. The hardness of the composites
with coarse grained red mud particle reinforcement was significantly increased with increase in
deformation under compression. On the other hand, the hardness measurements of the composites with
nano red mud particle reinforcement were not increased with increase in deformation under compression
which is due to strain softening occurred under compression. Minimum wear loss is observed for 30%
deformation and beyond this the wear loss is increased due to strain softening. The micro structural
observation of the worn out sample has revealed the formation of cavities in the matrix of the composite
at slow sliding velocity i.e. at 200 RPM. The amount of cavities is reduced with increase in sliding
velocities and minimum cavities are observed with sliding velocity of 600 RPM. At higher loads, deep
cracks and grooves are observed in the optical micrographs. From the micrograph, it is seen that some
cracks are originated at the grain boundaries of aluminium. This might be due to strain hardening of
aluminium during sliding with the applied load and due to pulling up of hard red mud particles from the
aluminium grain boundaries. With increasing applied load this effect is more pronounced because of
embrittlement of hard particles during sliding.
19
Bauxite & Laterites
References
Akhlaghi F., Zare-Bidaki A., 2009, Influence of graphite content on the dry sliding and oil impregnated
sliding wear behaviour of Al 2024–graphite composites produced by in situ powder metallurgy method,
Wear, Vol. 266, pp. 37-45.
C.S.Lee,Y.H.Kim,K.S.Han,T.lim, Wear behaviour of aluminium matrix composite materials, Journal of
Material Science, Vol. 27(3), 1992, pp 793-800.
Callister William D Jr., 2007, “Materials Science and Engineering- an introduction”, 7th edition, John
Wiley & Sons. Inc.– NewYork, USA.
Hashim, J., L. Looney, M.S.J. Hashmi, 1999. Metal matrix composites: production by the stir casting
method, Journal of materials processing technology, Elsevier B.V., Netherlands, Volume92-93, pp. 1-7.
J.K.M. Kwok, S.C.Lim, High speed tribological properties of some Al /SiCp composites.1. Friction and
wear rate characteristics, compos. Sci.Technol. Vol. 59, 1999, pp 169- 188.
M.H.Korkut, “Effect of Particulate Reinforcement on Wear Behaviour of Aluminum Matrix Composites”.
Materials Science and Technology Vol.20, 2004,pp.73-81.
M.Cirino, R.B.Pipes and K.Friedrich. “The Abrasive Wear Behaviour of Continuous Fibre Polymer
Composites”. Journal of Material Science, Vol 22, 1987, p. 2481.
Manish Narayan, M.K.Surappa & B.N. Pramila Bai. “Dry sliding wear of Al alloy 2024-Al2O3 particle
matrix composites”, wear, Vol. 181-183, 1995, pp 563-570.
N.L.Savchenko, P.V.Korolev, A.G.Melnikov, et.al. “Wear and Friction of transformation–toughened
CMC and MMC”.Wear Vol. 249, 2002, pp-892-900.
Natarajan N., Vijayarangan S., Rajendran I., 2006, Wear behaviour of A356/25SiCp aluminium matrix
composites sliding against automobile friction materials, Wear, Vol. 261,p. 812-822.
Rittner M., 2000. Metal matrix composites in the 21st century: markets and opportunities. BCC Inc.
Norwalk, CT.
S. H. Ko, J. M. Jang and W. Lee: Materials Science Forum 475–479 (2005) 3489–3492.
Sudarsan X, Surappa MK, Dry Sliding wear of fly ash particle reinforced A356 Al composites. Wear,
2008; (264) : 555-561
Valdez S., Campillo B., Perez R., Martinez L., Garcia A., 2008, Synthesis and microstructural
characterization of Al-Mg alloy-SiC particle composite, Materials Letters, Vol. 62, pp. 2623-2625.
Zhou, W., and Z. M. Xu, 1997. Casting of SiC reinforced metal matrix composites. Journal of material
processing technology, Elsevier B.V., Netherlands, Volume 63, pp.358-363.
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21
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A STUDY ON MINERAL CHARACTERIZATION OF LEUCOXENE AND ITS SEPARATION
FROM OTHER MINERALS
The Indian subcontinent is well endowed with placer minerals on and off its east and west coasts. Important
heavy minerals identified in order of abundance are ilmenite, garnet, sillimanite, rutile, leucoxene, zircon and
monazite. The heavy mineral suit at Manavalakurchi in Tamil Nadu and Chavara in Kerala contains about
0.7% of leucoxene with estimated reserve of 0.35 million tones. Leucoxene is an opaque, amorphous,
chemically variable titanium oxide usually with small amount of adsorbed water with chemical formula:
Fe2O3 .TiO2.nH2O.
It has semi magnetic susceptibility, high electrical conductivity, specific gravity: 3.5, TiO 2 content: 70 to
90%. It is grey in colour with light brownish tinge in reflected light and is formed by alteration of ilmenite.
Hence it is often called as Brown Ilmenite. It is not a recognized mineral species as it lacks crystal structure.
The parent mineral of leucoxene is ilmenite, the most common titanium mineral in the earth’s crust. The
alteration of ilmenite has resulted in three successive stages.
Leucoxene is sold for use in welding electrodes as a fluxing agent which are extensively used in ship
building and civil engineering. Leucoxene is very attractive to titanium dioxide producers as it represents an
effective substitute for rutile at lower price in chloride pigment production.
The dissolution of iron oxide induces the relative increase in TiO2 and causes a large range of magnetic
susceptibility extending from that of ilmenite to nonmagnetic rutile and so leucoxene reports to magnetic,
middling and nonmagnetic fractions in magnetic separators.
Due to wide range of magnetic susceptibility, recovery of leucoxene is a complex process in the mineral
separation plant. Very often, magnetic susceptibility of leucoxene is similar to that of monazite whose
presence as impurity in leucoxene product is highly hazardous in the process. However sensitively exploiting
its electrical conductivity and magnetic susceptibility, I.R.E. Ltd. Chavara is able to separate it as a product.
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Keywords: Leucoxene, alteration, properties, separation.
1. Introduction
The Indian subcontinent is well endowed with placer minerals on and off its east and west coasts. They are
often referred to as beach sand minerals which contain heavy minerals with a specific gravity greater than
2.9. Important heavy minerals identified in order of abundance are ilmenite, garnet, sillimanite, rutile,
leucoxene, zircon and monazite. These minerals grow as crystals in igneous rocks such as granite, pegmatite,
and basalt and in some metamorphic rocks like khondalite. Over millions of years, these rocks were eroded
by weather and the minerals were washed to rivers and streams and into the sea. These heavy minerals were
then carried back onto the beach by waves, which in turn drag the lighter minerals such as quartz back into
the sea. The tidal process leaves the heavy minerals on the beach. Wind further concentrates the heavy
minerals as the lighter quartz sand is blown away more easily. This process is constantly repeated resulting
heavy concentration of minerals along the beach.
Ilmenite, leucoxene, and rutile are titanium bearing minerals used mainly as feedstock for the production of
titanium dioxide pigments. Zircon is a zirconium bearing mineral used for the manufacture of ceramics,
refractories and also in a range of industrial and chemical applications. Monazite is a rare earth bearing
mineral used for the preparation of rare earth magnets, phosphors, polish, catalysts, glasses, metal alloys,
misch metals. Thorium in its oxide form is used in the manufacture of incandescent mantles. Thorium oxide
in combination with uranium is used as a nuclear fuel in thorium high temperature reactor (THTR).
The heavy mineral suit at Manavalakurchi in Tamil Nadu and Chavara in Kerala contains about 0.7% of
leucoxene with estimated reserve of 0.35 million tones.
Leucoxene is an opaque, amorphous, chemically variable titanium oxide usually with small amount of
adsorbed water with a chemical formula Fe2O3.TiO2.nH2O. It has semi magnetic susceptibility, high
electrical conductivity, specific gravity of 3.5, and TiO2 content of 70 to 90%. It is grey in colour with light
brownish tinge in reflected light and is formed by alteration of ilmenite. Hence, it is often called as Brown
Ilmenite. It is not a recognized mineral species as it lacks crystal structure. The parent mineral of leucoxene
is ilmenite, the most common titanium mineral in the earth’s crust.
After the ilmenite is released from solid rocks, it is subject to weathering. Particularly under humid tropical
conditions, iron increasingly dissolves and titanium becomes relatively enriched. The final member in the
weathering process is the mineral mixture leucoxene, predominantly consisting of Ti oxides and, to a far
23
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lesser degree, Fe oxides. The process of weathering is therefore called leucoxenization. Leucoxenization only
occurs above groundwater level. The influence of humic acids plays an important role. The dissolution of the
iron oxides induces the relative increase in TiO2 and the reduction of magnetic susceptibility.
2. Process of alteration
i. The alteration begins at the rim and proceeds into the grains along fissures, cleavage planes, twin
planes and other crystallographic weakness zones.
ii. Hematite lamellae often found in primary ilmenite and resulting from initial high temperature
exsolution are characteristically leached out of placer ilmenite. This process proceeds from the
periphery of grains inwards.
iii. As the hematite lamellae are removed, iron content is decreased from the ilmenite structure resulting
in the enrichment of Ti in ilmenite.
iv. Trace elements like Mg, Cr and Mn are also removed along with iron in the alteration process. This is
an added advantage, as these elements pose problems for processing and also cause coloration effect
in pigments.
v. The transformation of ilmenite into pseudo-rutile involves the oxidation of all the ferrous iron into
ferric iron which is leached out from ilmenite lattice by electrochemical erosion and generally occurs
in a mildly acidic ground water situation.
vi. Alteration beyond pseudo rutile occurs via a dissolution precipitation process whereby both the iron
and titanium are dissolved but the iron is leached out while the titanium is deposited as nonmagnetic
leucoxene containing high TiO2.
3Fe2+TiO3+2H+ +1/2O22Fe3++Ti3O9+Fe2++H2O
vii. Coarse leucoxene is formed by the growth of fewer large crystals at the expense of several ones.
Ilmenite (FeTiO3) → “leached out” ilmenite →pseudorutile (Fe2Ti3O9) → “leached out” pseudorutile
(FeTi3O6(OH)3) → leucoxene.
24
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68 – 75 auburn
75 – 80 yellowish-brown
80 – 85 yellow orange
85 – 90 yellowish-gray
90 – 95 yellowish-white
95 – 100 white
4. Application
Leucoxene with TiO2 >68% is used for Chloride process and welding rods. Leucoxene is sold for use in
welding electrodes as a fluxing agent which are extensively used in ship building and civil engineering.
Leucoxene is very attractive to titanium dioxide producers as it represents an effective substitute for rutile at
lower price in chloride pigment production.
Titanium metal is valued for three main positive characteristics:
Low apparent density (4.507 g/cm3). Volume for volume, titanium is 43 % lighter than steel (7.85
g/cm3) and only 66 % heavier than aluminum (2.70 g/cm3). This means that 1m2 steel sheet has the same
weight as 1.75 m2 titanium sheet metal of the same thickness.
Titanium and its alloys at room temperatures have close to the same strength characteristics as steel and
therefore generally higher strengths than light alloys. During continuous stress at elevated temperatures
of up to around 500 °C, the relationship between strength and apparent density is particularly
advantageous.
The corrosion resistance of titanium - particularly in oxidizing and chloride-ion containing media -
allows economic combination options in the different areas of application.
Other outstanding characteristics are:
25
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high melting point: 1668o C
good thermal conductivity: 21.9 W/m · K
small coefficient of expansion: 8.36 [10-6 K-1]
high electrical resistivity: 54 μΩ · cm
non-toxicity and non-irritation of human skin.
For the above reasons, titanium metal and its numerous alloys (with Fe, Nb, Sn, V, Al, Zr, Mn,
Ni, Cr) are used in the following areas:
• aircraft engineering: landing gear support beams, engine supports, fuselage, engine blades, rotor blades,
compressor disks, spacers, suspensions, bolts, exterior skin, exterior skin jacking points, spars, spar frames,
wing spar box, undercarriage components
• helicopter engineering: gearbox, boom, rotor hub, tail rotor driveshaft, fasteners, exterior skin and floor pan
components, rotor leading edge
• Spacecraft: helium and nitrogen tanks, hydrogen tanks, jet components, rings, bracers in the propulsion
area, spars, spar frames
• drive systems: connecting rods, valves, butterfly valves, rocker arms, water jet propulsion systems,
maglevs, batteries
• chemical and industrial plant engineering: pumps and valves and fittings, chemical and seawater pipes,
bleach tanks in paper mills, hydrogen tanks, anodes in chlorine, chlorate and hypochloride production,
catalysts, nuclear fuel canisters
• Defense: submarine cladding, weapons systems
• IT, electronics: supercomputers, superconductor systems
• Casting and molding: rotors, suction covers, housing components for plate valves and y valves, ball valves,
valve plates
• Jewelry and watchmaking industry: watches, rings, frames for glasses, body piercing jewelry
• Sports: golf clubs, tennis rackets, baseball bats, racing bike frames, billiard cues
• Housing: roofs, air conditioning systems
• Medicine: prostheses, surgical implants and devices, dental technology, pacemaker covers Titanium metal
powder is used in pyrotechnics and serves as the initiator for the inflation of airbags. It is also an alloying
agent for the manufacture of magnets, and a deoxidizer.
Other areas of application for titanium and titanium dioxide are:
26
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• Nanotechnology: In sunscreens, clear wood varnishes and plastic films, ultra-fine TiO2 (1-50nm) generates
high UV protection due to its property of strongly absorbing and dispersing UV light. Deposited on glass
with a thickness of approx. 15 nm, ultra-fine TiO2 gives the glasses self-cleaning properties. Further areas of
application are emerging in the areas of electro-ceramics and photocatalysis.
• Batteries: Titanium has been used as an insulator in alkaline batteries for a long time. Recently it has been
used in rechargeable Mn-Ti-Li batteries that use Li-Mn complex oxide cathode and Li-Ti oxide anode. The
Li-Ti oxide and the cell structure improves electron flow and leads to an increased capacity in miniature
format, superior charging properties and excellent voltage and overload resistance characteristics.
- Titanium tetrachloride, TiCl4, a liquid which is only colorless after distillation, and that fumes strongly
upon contact with moist air. Intermediate product in the production of titanium metal, TiO2 and organic
titanium changes the structure of aluminum alloys, special glazes for glasses and ceramic products, feedstock
for pharmaceuticals.
- Titanium oxide chloride, TiOCl2, a pearlescent pigment frequently used for coatings, cosmetics and sanitary
products, packaging, plastics and printing inks. It is also used in metal treatment and as a feedstock for the
manufacturing of barium titanate and inorganic titanates.
- Titanium carbide, TiC, a hard (Mohs: 9), dense refractory with high thermal shock and abrasion resistance
as well as low friction resistance. Used in powder metallurgy in cutting tool end fittings, fittings, wear parts
and high strength coatings; additive for plastic or rubber replacement parts instead of metals; in mixed
crystals such as (Ti,W)C, (Ti,Ta,W)C, (Ti,Ta,Nb,W) C for hard metals.
- Titanium nitride, TiN, a yellow brown crystalline solid with a melting point of 2,950 0 C and Vickers
hardness of 2,100 and is used in crucibles for melting lanthanum alloys, coatings on cemented carbides and
golden yellow coloration on jewelry.
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Other 8 %
Total: about 1200 mill. T
5. Effects of alteration
The dissolution of iron oxide induces the relative increase in TiO2 and causes a large range of magnetic
susceptibility extending from that of ilmenite to nonmagnetic rutile and so leucoxene reports to magnetic,
middling and nonmagnetic fractions in magnetic separators.
Based on magnetic susceptibility, three groups of leucoxene exist:
1. Magnetic Leucoxene reporting in magnetic fraction has a similar magnetic susceptibility to ilmenite.
2. Transition Leucoxene reporting in middling fraction has a magnetic susceptibility between that of
ilmenite and rutile.
3. Non-magnetic leucoxene having a similar magnetic susceptibility as rutile.
Flow sheet
HTS
Cond
HTS
Cond
EPS
Cond
IRMS
Midd.
70#
OS
Product
28
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Due to wide range of magnetic susceptibility, recovery of leucoxene is a complex process in the mineral
separation plant. Very often, magnetic susceptibility of leucoxene is similar to that of monazite whose
presence as impurity in leucoxene product is highly hazardous in the process. However, sensitively
exploiting its electrical conductivity and magnetic susceptibility, I.R.E. Ltd Chavara is able to separate it as a
product.
Leucoxene product with 10% Ilmenite, 25% rutile and 65% leucoxene is produced through this process.
References
An introduction to the Rock forming Minerals by W.A. Deer, R.A. Howie, J. Zussman.
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PROCESSING OF INDIGENOUSLY MINED COLUMBITE TANTALITE ORE
FOR PRODUCTION OF PURE TANTALUM & NIOBIUM OXIDE
Abstract
Tantalum & niobium exhibit very interesting properties such as high melting temperature, ductility,
corrosion resistance and significant thermal and electric conductivities. The pentoxides of tantalum and
niobium are by far the most important compounds since they are starting material for the production of
other niobium and tantalum compounds and have applications in electronics, tool manufacturing etc. In
nature, tantalum and niobium exist primarily as refractory oxides (Ta2O5 and Nb2O5) and no free metal
deposits are known. Tantalum is invariably associated with its co-genitor niobium, on account of their
very similar chemical properties and atomic & ionic radii. Hydrometallurgical processing of columbite
tantalite (CT) ore with typical crystallite formula of (Fe,Mn) (Ta,Nb)2O6 involves complete dissolution of
the complex mineral ore with the subsequent stepwise enrichment and separation of some of the
impurities or the elements of interest. CT ore is leached either by acid digestion with HF or alkali fusion.
Among the two routes, hydrofluoric acid digestion is the most practiced route. Development works were
carried out at Special Materials Plant, NFC for processing of Ta-Nb minerals from various sources. The
process developed for processing the hydro flouro niobic and tantalic acids consists of various chemical
and hydrometallurgical operations such as solvent extraction, precipitation, pyro hydrolysis, calcination
etc. Tonnage quantities of pure tantalum oxide and niobium oxide have been produced at SMP to meet
the requirements of nuclear industry. This paper details with the process developments, parameters
standardization and adaptation along with experience in plant operation for processing of columbite-
tantalite ore to produce pure tantalum and niobium oxide & their metals.
Keywords: Columbite tantalite ore, tantalum oxide, niobium oxide, hydrometallurgy, nuclear.
1. Introduction
Niobium ranks 31st in the order of concentration of elements in the earth’s crust (20 ppm in crystal
abundance). It always occurs together with tantalum. In India, niobium and tantalum mineral occurs
chiefly as pegmatite minerals and are generally mixed oxides of the two metals with iron, magnesium,
titanium, silicon, tungsten etc. The columbite-tantalite bearing pegmatites are located in Bastar district,
Chhattisgarh, Mandya district, Karnataka and in parts of Bihar, Jharkhand besides the known mica belts
of Andhra Pradesh, Bihar and a good stockpile of this ore has been accumulated as a by product in mica
mining by Atomic Minerals Division.
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More than 80% of the Nb being produced all over the world is for steel industries and it is the standard
“Ferro niobium grade’’, which is used in High Strength Low Alloy Steel (HSLA), wherein Nb is added to
the extent of about 0.05% level. A small percentage of niobium of high purity is also being produced by
selective countries for special applications such as in the production of NbTi, NbZr, NbCu, C-103 etc.
and chemical compounds like Nb2O5, NbCl5 etc. High purity tantalum metal and tantalum pentoxide have
become increasingly important to the electronics industry in the preparation of advanced electronic
materials used in the manufacture of devices such as surface acoustic wave filters, pyroelectric infrared
sensors and optoelectronic devices. High purity tantalum pentoxide is also required for the preparation of
tantalate X-ray phosphors for X-ray intensifier screens, special optical applications, high-speed cutting
tools manufacture and production of sputtering targets.
Special Materials Plant at NFC has mastered the technology in production and developments relating to
niobium and tantalum. Production of pure niobium and tantalum metals involves complex
hydrometallurgical & pyrometallurgical processing of columbite-tantalite (CT) ore. The effective
separation of Ta from Nb calls for special techniques, among which solvent extraction is well adaptable
for industrial scale of production. Columbite, tantalite, columbite-tantalite, pyrochlore, and euxenite
constitute the major primary sources for niobium and tantalum and are located in Canada, Brazil, Nigeria,
Zaire and Russia. Various processes involved in the breakdown treatment of niobium and tantalum
primary sources, extraction and separation and newer processes of extraction have been discussed in
literature [1-6].
In India, the primary source is columbite-tantalite ore. The processing of Indian ore beginswith opening
of the ore with technical grade hydrofluoric acid (40% conc.) followed by separation of the co-genetic
niobium and tantalum by solvent extraction using tri-n-butyl phosphate (TBP) as an organic solvent. This
paper describes in brief the developments carried out in the last few years on processing of indigenous
columbite tantalite minerals by hydrometallurgical route.
2. Experimental
Process description
The process involves various hydrometallurgical and chemical operations like comminution, break down
treatment of ore, solvent extraction, precipitation, calcination etc. Pilot scale studies have been carried out
to study the effect of various parameters on each operation.
2.1 Mineral recovery & comminution
Columbite tantalite mineral present in pegmatite gravels in India contains around 26-80% Nb2O5 and 6-
70% Ta2O5. AMD operates pilot plants for recovery of columbite tantalite from pegmatitic gravel.
Columbite-tantalite is heavy (sp. gravity 5.3-7.8) and therefore gravity separation is used to separate it
31
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from the other pegmatitic minerals such as quartz and feldspar which are light (sp. gravity 2.8). Beryl,
which occurs in these pegmatites is generally hand sorted and recovered, based on colour, lustre and
hexagonal crystalline form.
Further, the columbite-tantalite mineral is crushed in a jaw crusher and wet ground in ball mill to a size of
-100 mesh. In our case, we are procuring –100 mesh columbite tantalite mineral from Atomic Minerals
division, where the mineral up gradation step is being carried out.
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33
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pure niobium pentoxide & tantalum pentoxide powders. Certain entrapped impurities like fluoride,
ammoniacal ions are removed during calcination. Effect of temperature, material of construction and
steam on removal of fluoride in the final product was studied.
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In acid digestion, it is observed that the extent of dissolution with 40% HF increases with solid-liquid
ratio. Nearly complete dissolution is obtained with a solid-liquid ration of 1:2. As the ratio is further
increased, niobium forms H2NbF7 extractable complex with TBP which makes separation of Ta and Nb
difficult.
At a solid-liquid ration of 1:2, Nb forms H2NbOF5 complex. This complex is not extractable with TBP,
hence leading to effective separation of Ta and Nb.
3.3 Solvent extraction
Selection of solvent:
In view of the higher flash point of TBP (146 0C) as compared to MIBK (14 0C) and also in the light of
substantial consumption of TBP for extraction of other metals in NFC, SMP had opted TBP as the choice
of solvent in Nb/Ta extraction (as Hyderabad, India is a tropical region, ambient temperature shoots up of
up to 43 0C in summer). As TBP is having higher viscosity (3.2 cp), kerosene (0.8-0.9 cp) is used as
diluent.
Theory of extraction of Ta & Nb
Tantalum reacts with HF at lower acidities to form H2TaF6 and at higher aciditiesto form H2TaF7 and
H2TaF8. Niobium reacts with HF at lower acidities to form H2NbOF5 and higher acidities to form
H2NbF7.
At lower acidity
Ta2O5 + 12 HF 2 H2TaF6 (org) + 4H2O - (9)
Ta2O5 + 14 HF 2 H2TaF7 (org) + 5H2O - (10)
Nb2O5 + 10 HF 2 H2NbOF5 (aq) + 3H2O - (11)
At higher acidity
Ta2O5 + 16 HF 2 H2TaF8 (org) + 6H2O - (12)
Nb2O5 + 14 HF 2 H2NbF7 (org) + 5H2O - (13)
In the above equations, (org) indicates that the compound is stable in the organic phase, and (aq) in the
aqueous phase. Those compounds which are stable in organic phase (in TBP) will form a solvation
complex with TBP as shown below:
H2TaF6 + 2 TBP H2TaF6.2TBP - (14)
H2TaF7 + 2 TBP H2TaF7.2TBP - (15)
H2TaF8 + 2 TBP H2TaF8.2TBP - (16)
H2NbF7 + 2 TBP H2NbF7.2TBP - (17)
Effect of concentration of TBP
Studies have revealed that the increase in extractability of Nb/Ta is marginal with increase in
concentration of the TBP from 50% to 100% in the mixture TBP & kerosene. Hence after optimizing the
35
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extractability of Nb/Ta and hydrodynamic properties, 50% TBP – kerosene mixture is selected as solvent
for Nb/Ta extraction system
Effect of acidity
Extractability of tantalum decreases with increasing acidity whereas the extractability of niobium
increases with increase in acidity (Fig. 2). At lower acidity, the extractability of tantalum is considerable
whereas niobium is scarcely extractable at the same condition. Hence, the separation factor (Ta/Nb)
reduces with increasing acidity (Fig. 3).
160
80 120
% Extraction
60 80
Ta
40
Nb 40
20
0 0
0 5 10 15 20 0 5 10 15 20
HF Acidity (N) HF Acidity (N)
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3.4 Precipitation
Pure solution of Nb & Ta obtained after solvent extraction are precipitated with ammonia. The interaction
between ammonia and fluoro tantalic & fluoro niobic acids initiates the hydrolysis of complex fluoride
compounds.
2 H2TaF7 + 14 NH4OH Ta2O5.nH2O(s) + 14 NH4F + (9-n)H2O - (18)
2 H2NbF7 + 14 NH4OHNb2O5.nH2O(s) + 14 NH4F + (9-n)H2O - (19)
Precipitation of niobium & tantalum from the solution starts at a pH of 1 and complete precipitation can
be achieved by adding ammonia solution up to pH of 8-9. But the obtained cake contains entrapped
fluoride (fluoride complex) (20-30%). Most important factor that affects the content of fluorine in
niobium hydroxide cake is amount of ammonia added during precipitation.
From the studies, it is observed that fluoride content is ~ 20% at a pH of 8.
Precipitation with gaseous ammonia results in amorphous phase of products and reduced volume of
effluents when compared to use of ammonium hydroxide.
Figure 4: Ta2O5 oxide content vs pH[3] Figure 5: Nb2O5 oxide content vs pH[3]
1: solution containing no ammonium fluoride of solutions prepared by dissolution of
2 to 5: solutions with increased initial ammonium (NH4)3NbOF6 (1) and (NH4)2NbOF5 (2)
fluoride content. in water or Nb in HF solution (3).
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content. It is observed that fluorine content in niobium oxide reduces to <10 ppm when subject to thermal
treatment at a temperature of 850oC.
The calcined oxides are ground by rod milling & sieved to obtain -100 mesh powder. Purity of the final
niobium & tantalum oxide obtained is 99.5%.
5. Conclusions
A pilot scale process has been developed at SMP, NFC to obtain pure tantalum & niobium oxides from
columbitet Tantalite ore by hydrometallurgical processing. Effect of various parameters on each unit
operation/process involved have been studied and optimized.
SMP, NFC has produced and supplied tonnage quantities of niobium oxide, Nb metal, tool grade tantalum
oxide, K2TaF7, tantalum powder and tantalum anodes for nuclear applications, applications in electronics
industries and applications in cutting tools etc.
References
1. Olushola S. Ayanda, Folahan A.Adekola, Journal of Minerals & Materials Characterization &
Engineering, Vol. 10, No.3, pp.245-256, 2011
2. D. Damodaran, S. G. Deshpande, A. A. Majmudar and M. S. Sastri, Proceeding of Indian National
Science Academy,1969,Vol.36, No. 5, pp. 306-318
3. Agulyansky (2004) The Chemistry of Tantalum and Niobium Fluoride Compounds, Elsevier,
ISBN 9780444516046.
4. O. M. El hussaini, N. M. Rice (2004), Hydrometallurgy, 72, 259-267.
5. Sanjo Nisimura & Isaoushima, Transaction of the Japan Institute of Metals, vol. 4, Oct 1963,
page 260-262
6. Sanjo Nisimura & Isokushima, Transactions of the Japan Institute of Metals, vol. 5, No. 1, 1964,
pg 40 -42
7. T R Bhat, Y. W. Gokhale& B.S. Mathur, Indian Journal of Technology,1963, Vol. I, No 4, page
165- 169
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8. AA Majumdar, Y.W. Ghokale & R.L. Iyer; Indian Journal of Technology vol.21, Dec 1983, pages
532-534
9. C K Gupta, International Metals Reviews, 1984 vol. 29, No. 6, page 405-440
10. P K Jena C L Gupta D K Boje& A K Taneja, Proceedings of Symposium of Non-Ferrous Metals
Technology Vol. III
11. K V Mirji, N C Raghuram, V K G Kutty& S C Jain, International symposium on Solvent
Extraction, Sep 26 – 27, 2002 at RRL, Bhuvaneswar, India
39
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Abstract
India is endowed with large resources of heavy minerals which occur mainly along coastal stretches of the
country and also in inland placers. However, the contribution towards the Global Titanium value chain
industry by India is very miniscule. The expected growth of Titanium value chain around the world is going
to be significant and hence we have got tremendous opportunities. But there are certain impediments also in
capitalizing these opportunities. An attempt is made below to bring out these opportunities and the challenges
in utilizing the same.
Key words: Ilmenite, Rutile, Slag, TiO2, Titanium
1. Introduction
The global airline industry consists of over 2000 airlines operating more than 23,000 aircraft, providing
service to over 3700 airports. The world fleet of passenger aircraft is forecast to double by 2025. Each
aircraft requires 12 to 80 tonnes of metallic Titanium depending upon the model. Additionally defense
aircraft uses Titanium as a major metal in their manufacture. Titanium’s demand in other chemical industries
is also very significant. Its high strength to weight ratio; twice as compared to steel and comparatively better
corrosion resistance than 18 – 8 Stainless steel (SS) are unique and hence an unavoidable raw material in the
aviation industry and other critical application in the chemical industries. However, even though India holds
huge high quality a reserve of Titanium, i.e Ilmenite in the beach sands, our contribution to this demand is
practically zero. While we consider the Titanium dioxide Pigment, which is another product in the Ilmenite
value chain and a major component in the paint industry, also the scenario is not very encouraging.
2. Resources
2.1 India
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India is endowed with large resources of heavy minerals which occur mainly along coastal stretches of the
country and also in inland placers. Heavy mineral sands comprise a group of seven minerals, viz, ilmenite,
leucoxene (brown ilmenite), rutile, zircon, sillimanite, garnet and monazite. Ilmenite (FeO.TiO2) and rutile
(TiO2) are the two chief minerals of titanium. Titaniumdioxide occurs in polymorphic forms as rutile,
anatase (octahedrite) and brookite. Though, brookite is not found on a large-scale in nature, it is an alteration
product of other titanium minerals. Leucoxene is an alteration product of ilmenite and found associated with
ilmenite.
Ilmenite and rutile along with other heavy minerals are important constituents of beach sand deposits found
right from Moti Daman-Umbrat coast (Gujarat) in the west to Odisha coast in the east. These minerals are
Over a stretch of 22 km between Neendakara and Kayamkulam, Kollam district, Kerala (known as
'Chavara' deposit after the main mining centre).
Over a stretch of 6 km from the mouth of Valliyar river to Colachal, Manavalakurichi and little
beyond in Kanyakumari district, Tamil Nadu (known as MK deposit).
On Chatrapur coast stretching for 18 km between Rushikulya river mouth and Gopalpur lighthouse
with an average width of 1.4 km in Ganjam district, Odisha (known as 'OSCOM' deposit after IREL's
Orissa Sands Complex).
Brahmagiri deposit stretches for 30 km from Girala nala to Bhabunia villages with an average width
of 1.91 km in Puri district, Odisha.
Bhavanapadu coast between Nilarevu and Sandipeta with 25 km length and 700 m average width in
Srikakulam district, Andhra Pradesh.
The most significant deposits which are readily available and attract attention of industry for large- scale
operations are found in Andhrapradesh, Kerala, Maharashtra, Gujarat, Odisha and Tamilnadu The average
grade of total heavy minerals in these deposits is 10-25% of which 30-35% is ilmenite. The overall state wise
reserves of ilmenite and rutile which occur together in beach sand deposits are given in Table-1.
41
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Mining and processing of beach sand are carried out by the IREL, a Government of India Undertaking,
KMML, a Kerala State Government Undertaking and two private sector producers; viz, M/s V. V. Mineral,
Thoothukudi (Tamil Nadu) and M/s Beach Minerals Co. Pvt. Ltd, Kuttam (Tamil Nadu). IREL is exploiting
beach sand deposits located at Chavara in Kerala, Gopalpur in Odisha and Manavalakurichi in Tamil Nadu.
The production of ilmenite at 739 thousand tonnes in 2012-13 was decreased by 2% as compared to that in
the preceding year. Tamil Nadu was the leading producer of ilmenite during the year under review,
contributing 66% of the total production followed by Odisha 25% and Kerala 9 per cent.
The production of rutile at 17 thousand tonnes in 2012-13 registered nominal decrease as compared to that in
the previous year. Odisha was the leading producer of rutile accounting for 43% of the total production
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followed by Tamil Nadu 38% and Kerala 19 per cent. The production of Ilmenite and Rutile state wise in
India is given below in Table-2.
2.2 World
World resources of anatase, ilmenite and rutile are more than 2 billion tonnes. World reserves of ilmenite are
estimated at 700 million tonnes in terms of TiO2 content. Major reserves are in China (29%), Australia
(23%), India (13%), South Africa (9%), Brazil and Madagascar (6% each), Norway (5%) and Mozambique
(2%). The world reserves of rutile are 48 million tonnes in terms of TiO2 content. Major rutile reserves are
located in Australia (50%), followed by South Africa (17%), India (15%), Sierra Leone (8%) and Ukraine
(5%).
World production of ilmenite and rutile concentrates was 11.40 million and 0.84 million tonnes, respectively.
Canada contributed 23% of ilmenite production, followed by South Africa and Australia (12% each).
Australia produced 52% of world rutile output, followed by South Africa with 15% and Ukraine 12%. World
reserves and production of titanium minerals, viz, ilmenite and rutile, are furnished in Table-3 and Table-4
respectively.
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3 Canada 31000 --
4 China 200000 --
5 India* 85000 7400
6 Madgaskar 40000
7 Mozambique 14000 510
8 Sierra Leone -- 3800
9 Norway 37000 --
10 South Africa 63000 8300
11 Ukrain 5900 2500
12 USA 2000 --
13 Vietnam 1600 --
14 Other Countries 26000 400
Total (Rounded) 700000 48000
Source: Indian Minerals Year book 2013 (Part III : Mineral Review); 52nd Edition
published in July 2015
* As per NMI, the total resources of titanium minerals in India are estimated at about
549.49 million tonnes.
3. Value chain
3.1 General
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The Titanium value chain is indicated below in the Figure-1. A typical Titanium value chain starts from the
beach sand mining to Titanium metal in one branch and Titanium dioxide (TiO2) in the other branch.
There are other intermediate products such as Synthetic Rutile and Titanium slag which can be sold in the
market as per the market dynamics.
45
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for the production of TiO2. Due to various limitations Ilmenite is not used as the feedstock in the chloride
process. Hence, the Ilmenite is upgraded to various levels of TiO2 (85% to 92 %+). Up-gradation of Ilmenite
is basically removing the Iron content from Ilmenite to get higher concentrating of TiO2. The major
upgraded Ilmenite are Synthetic Rutile (>90% TiO2) and Titanium Slag (>85% TiO2).
The total installed capacity of Synthetic Rutile in India is around 243,000tpa and the average production for
the last three years is around 70,000tpa. There is no titanium slag production in India. The total feedstock
requirement is expected to grow to reach 7.822 million TiO2 units by 2020 and virtually all this growth in
supply will be of chloride quality. It can be seen that current level of production is very small compared to
the resources. The current technology being used by India is also very old and has got certain environmental
issues and need to be addressed in the long term.
The installed capacity of Titanium Dioxide Pigment in India is around 85600tpa and average production for
the last three years is around 85000tpa (Both anatase and rutile grade). Current world production of Titanium
Dioxide pigment is hovering around 5.5million tonnes per annum and projected to grow to 7.8million tonnes
per annum within next couple of years.
The main constraint in the pigment manufacturing area is the non availability of chloride route pigment
manufacturing technology. This is kept as very guarded technology and not available easily. The sulphate
route technology is available fairly easily. But the environmental impact and mitigation is the main issue.
Due to these reasons there is no momentum in the mining sector also.
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production is hovering around 19200tpa. Since, the demand is very much cyclical, the manufacturers are
using this latent capacity to take advantages of sudden spike in the demand.
Recent business forecasts and quarterly reports from major aerospace original equipment manufacturers
suggests “upward and onward” growth during the next 10 years and beyond, which, by extension, translates
into strong business opportunities for the titanium industry. It is estimated that that the titanium supply chain
or “value chain” for the global aerospace industry represents an annual output volume of 130 million pounds
of titanium. Also the requirement for Titanium metals and alloys in other industries are also increasing due to
long life provided by Titanium alloys.
4.2 Challenges
The availability of the latest technology is the basic impediments in realizing the true potential in the value
addition of Ilmenite. These technologies are guarded and not shared very easily. Many attempts made by
leading Indian entrepreneurs to bring the technology to India were not successful. There are certain Indian
Research and development organizations that are working towards development of new technologies for
carbo-chlorination of Ilmenite and Titanium Slag and Electrolysis process for Titanium metal manufacturing
and are in pilot plant stage. Another critical thing to be addressed is that since many deposits are situated at
47
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densely populated areas and ecologically sensitive areas, a very cautious approach is needed from the
prospective investors.
Acknowledgements
I would like to place on records my sincere gratitude for the opportunity and the assistance provided for
preparing and presenting this paper by my management. I give my heartfelt thanks to MPT2016 for accepting
my paper and providing an opportunity for presenting to the august audience.
References
www.ibm.gov.in
http://www.titane.asso.fr/aeronautics.html
www.titanium.org
Mineral Commodity Summaries 2015
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EVALUATION AND PROCESSING STUDY OF RARE EARTH ELEMENTS IN THE
GAZESTAN DEPOSIT (CENTRAL IRAN)
Abstract
Gazestan deposit is located at 78 km from eastern of Bafgh (Central Iran) within carbonate rocks, shale,
tuff, sandstone and volcanic rocks. Mineralization is the mixture of iron minerals and apatite together
with minor quartz and calcite which occurs as various forms mainly in green rocks and rarely in rhyolite.
Apatite is fluorapatite and content of Cl is very low. Monazite is the main mineral of gazestan that has
been concentrated in apatitie and quarts. Based on assessments and simulation by mining software, the
deposit tonnage of ore bodies is about 60 Mt. The grades of Fe, P and TREEs are 26%, 2%, 0.1 %,
respectively.
The beneficiation studies on a representative sample have been carried out in the lab scale.
Rare earth elements include 17 elements of lanthanides group, scandium and yttrium. These elements
concentrate in solid solution, minor mineral (monazite and bastansite) and other minerals such as apatite.
Mineral resources of rare earth elements can be found in granites, pegmatites, alkaline rocks and
carbonatites. (Rezapour, 2014) Bastansite, monazite, xenotime are the important minerals that contain
these elements. Twenty percent of rare earth elements have been found in monazite and the remaining
elements exist in bastansite and other minerals (Samiee Bayragh, et al., 2015).
Physical and chemical processes have been utilized to produce misch metals containing TREEs
(Rezapour, 2014). Regarding to properties of minerals containing REEs which are different from others,
through dissolving and sedimentation phenomena of hydrometallurgical methods, they can be extracted
(R. D. Abreu, et.al., 2010; N.B. Egorov, et al., 2014; W. Kim, et al., 2009; A. Kumari, et al., 2015; S.
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Peelman, et al., 2014). Moreover, it is possible to process other minerals of Gazestan as by-product using
physical upgrading method. (Rezapour, 2014).
According to the survey, rare earth elements mineralization is associated with apatite mineralization in
central Iran. The target of this study is to evaluate the REEs resources and estimate the tonnage amount of
ore bodies. In addition, representative samples were also taken from Gazestan deposit for mineral
processing studies.
2. Geological characteristics
The Gazestan deposit is located at 78 km from eastern of Bafgh (south eastern of Yazd) which belongs to
central-Iran zone of Iran’s structural zones. Main rocks in this area are related to Precambrian to
Cambrian Rizo Series which include sedimentary units (shale, sandstone, carbonate), volcanic and
plutonic rocks (Figure 1).
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known as "green rock". According to alkali diagram versus SiO2 Gazestan rocks are mainly dacite,
rhyolite, andesite and trachyte. Intrusive rocks are monzonite and gabbroin the western part (Figure 2).
Five different mineralized zones were formed in this area: 1) iron ore, 2) magnetite-apatite ore, 3) stock
work ore, 4) disseminated ore and 5) massive apatite veins (Babakhani, 2015).
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Iron ore
Black iron ore with weathered surface which has inharmonious convexities. Iron-bearing massive consist
of magnetite, hematite, apatite, quartz and calcite. Secondary amphibole is observed and also, Sericitic
and Chloritic alterations are dominated. Iron ores are mainly magnetite which converted to hematite
during Martitization process. In addition, secondary goethite and limonite occurred. Moreover, there is a
negative correlation between Fe2O3 and P2O5 contents (Table 1).
Magnetite-apatite ore
The Gazestan iron lens is a set of iron and apatite minerals. The contact of this zone with iron ore is
gradual and both sides are extreme in terms of apatite and magnetite. Both iron ore and apatite-iron have
170 meters length and 20 to 30 meters wide with thickness between 7 to 10 meters. Average P2O5 of the
mineralized zone is more than 8 percent.
Disseminated ore: This mineralization was expanded but it is low grade which contains magnetite and
apatite.
Massive apatite veins: There are pure apatite bearing veins interrupt the other ores.
Mineralization of REE deposit include iron minerals and apatite with minor quartz and calcite which
occurs as various forms mainly in green rocks and rarely in rhyolite. Apatite is fluorapatite and content of
Cl is very low.
Topographic and geologic maps (1000 & 2000 scale), magnetometery, geophysics, trenches (2400 m) and
drilled bore holes (6133 m) are used for REE exploration in the Gazestan deposit. In this study, 34 bore
52
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holes have been drilled and sampled for XRD, XRF, ICP and AAS analyses. Geological data, samples
grades of bore holes, lateral and vertical profile are used for ore modelling and estimating and geo-
statistical modelling. The sub-cell dimensions are 5 m×10 m ×10 m in this block model (A. Hallagi,
2015). According to the type of deposit and volumes of exploratory data, the inverse distance squared
(IDS) method used for resources estimation and the deposit tonnage of ore bodies is resulted about 60 Mt
(Fig. 4). The grades of Fe, P and TREEs are 26%, 2% and 0.1 %, respectively.
Some representative samples were taken from Gazestan deposits for processing study. After sample
preparation via crushing, grinding and sample division, it was sent for mineralogical studies as well as
chemical analyses.
Based on sample characterization identification, upgrading processes were carried out. As illustrated in
Table 3, Fe percent of feed is about 25.6% which is economically effective for magnetic separation. By
operating wet magnetic separation flow-sheet, consisting cobber, rougher, and 3-step cleaner, it is
possible to increase the grade of Fe content in concentrate to 67%.
Magnetic product is also appropriate in terms of TREEs content which is the least amount possible, about
121 ppm. Unlike this, non-magnetic fraction consisting of tailings produced in different steps of magnetic
separation flow-sheet (called blend tail.), contains 1661-ppm TREEs.
Initial hydrometallurgical studies have been done on blend tail so far, and results show that it is possible
to recover TREEs to about 80% by applying precipitation methods.
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Table 3: REEs extraction project of Gazestan.
Feed characteristics
Fe (%) 25.58
TREEs (ppm) 965.21
Magnetic Separation Concentration
Separation Steps Cobber (3500 G), Rougher (2000 G), and 3 steps of Cleaner (1000 G)
Magnetic Product
Magnetic Product Final Concentrate of magnetic flowsheet operation
TFe Recovery (%) 74.27
Fe (%) in Mag. Product 67.12
TREEs (ppm) in Mag. Product 121.3
Non-Magnetic Product
Non-Magnetic Product (Blend Tail.) Blend of Cobber Tail. Rougher Tail. And First Cleaner Tail.
Fe (%) in Blend Tail. 9.8
TREEs in Blend Tail (ppm) 1661.33
TREEs Recovery (%) 96.44
Hydrometallurgical Study
Equipment Construction Furnace equipped stirrer
TREEs Recovery (%) 83
Total of TREEs Recovery (%) 80.04
5. Conclusions
a) Mineralization of deposit include iron minerals and apatite with minor quartz and calcite which
occurs as various forms mainly in green rocks and rarely in rhyolite. Apatite is fluorapatite and
content of Cl is very low.
b) Monazite is the main mineral of Gazestan that has been concentrated in apatitie and quarts.
c) Based on assessments and simulation by mining software, the deposit tonnage of ore bodies is
about 60 Mt. The grades of Fe, P and TREEs are 26%, 2%, 0.1 %, respectively.
d) The beneficiation studies on a representative sample have been carried out in the lab scale. By
operating magnetic separation flow-sheet, it is possible to produce a proper magnetic product
containing about 67% Fe. Then non-magnetic fraction was led to hydrometallurgical study.
e) Rare earth elements of which recovery values are about 80%, are produced by magnetic separation
and hydrometallurgical methods.
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References
R. D. Abreu, C. A. Morais, Purification of Rare Earth Elements from Monazite Sulphuric Acid Leach
Liquor and the Production of High-Purity ceric oxide, Minerals Engineering, 23, pp: 536–540, 2010
N.B. Egorov, A. N. Dayachenko, D.V. Akimov, A.D. Kiselev, K.V. Obmuch, Extraction of REE by using
solutions of H2SO4 and NH4F, 1st International Symposium on Inorganic Fluorides: Chemistry and
Technology, Procedia Chemistry 11, 15 – 19, 2014
A.Kumari, R. Panda, M.Jha, J. Kumar, J. Lee, Process Development to Recover Rare Earth Metals from
Monazite Mineral: A review, Minerals Engineering, 79, 102–115, 2015
S. Peelman, Z. Sun, J. Sietsma,Y.Yang, Leaching of Rare Earth Elements: Past and Present, 1st European
Rare Earth Resources Conference, 2014
A. SamieeBayragh, M. Meshkini, A. Barzin. Rare Earth Elements (Overview, Processing and Marketing)
Amirkabir University Publication, 2015.
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UNDERSTANDING THE PERFORMACNE OF GRAVITY CONCENTRATION CIRCUITS FOR
PALCER MINERALS –A REVIEW
Karamjith Sharma1,*, R. Venugopal1 and Y. Rama Murthy2
1
Department of Mineral Engineering, ISM Dhanbad University, India
2
Dep. of Research and Development, TATA Steel Ltd., Jamshedpur, India
*Corresponding author: sharmakaramjith@gmail.com
Abstract
Conservation of natural mineral resources to cater the future needs while satisfying the continuous demand
from different end users is the need of the hour. From the mineral conservation point, utilization of lean ores
to preserve high grade resources is inevitable. Further, techno economically viable ways of beneficiating lean
and sub-grade ores is also essential. Along with resource conservation, there is a need to focus on innovative
strategy and advancement in development of new devices with modified circuits for processing of low grade
complex ores and reduce loss of valuable minerals in tailings and recover values from previously generated
tailings. Mineral sands, term given to a group of minerals commonly found in beach sand placers. The
principal valuable minerals are ilmenite (Fe.TiO3), rutile (TiO2), zircon (ZrSiO4), garnet (Fe, Mg, Ca, Al
Silicates), sillimanite (Al2SiO5) and monazite (Ce, La, Th, Nd, Y) PO4. Some of the available performance
analysis methods like grade-recovery method, particle characterization (size, shape and density by latest
equipment’s (like QEMSCAN) that determines the particle behavior in a separation media) are reported. The
technical concept like incremental quality concept and linear circuit analysis helps in better understanding of
the circuits. Different methods of simulation developed are used in analyzing the equipment performance and
provide better data to troubleshoot the problems.
Availability of literature and data relevant to gravity separation circuit performance analysis is very scanty.
Hence there is a scope and need to work on such areas. In this work all the above relevant problems were
studied in details and summarized.
Keywords: Gravity concentration, enhanced gravity concentrators, grade and recovery, qemscan, increment
quality concept and linear circuit analysis, simulation, pilot plant experiments.
1. Introduction
Gravity concentration (GC) is one of the oldest techniques, used to separate the mineral particles based on
their relative density. The ease and efficiency of separation is dependent on a number of factors including
relative density, particle size and shape, liberation etc, all of which affect the selection of equipment type.
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1.1 Advantages and Limitations in GC methods, followed by emerge of Enhanced Gravity
Concentrators (EGC) to sustain and overcome the demerits of Gravity Separation techniques:
GC over other techniques has lower overall cost per ton of through put with wide range of selectivity of
equipment based on the plant adaptability with mere usage of chemicals. Ability to treat malleable/friable
ores, with minimum space required and demands simplicity of circuits. Able to handle large tonnage to
reject barren waste for initial pre-concentration, scavenging plant tailing to reduce the burden to
downstream processes.
GC performance/efficiency is optimum when there is a large difference in the specific gravity of the
minerals to be separated, particles shape is almost spherical and nearby size range limited to <50µm but
the above conditions doesn’t prevail in practical basis. Ineffective to treat complex ores, which require
grinding <10µm for liberation of minerals with optimum feed pulp, percentage solids, feed rate and grade
desired.
In the last 15 years, various types of EGC have been developed to recover mineral values at fine and
slime sizes (Burt et.al., 1995). With the advent of EGC techniques by suitably imposing the centrifugal
accelerations over conventional jigs, tables and fluidized bed separators, the concentration limit of gravity
techniques have extended down to 1μm size with maximized grade and recovery. The EGC equipment
includes Knelson concentrator, Kelsey jig, Mozley Multi Gravity separator, Falcon Concentrator are
some of them [1 2 3 4].
Mineral sands, term given to a group of minerals commonly found in beach sand placers. The principal
valuable minerals are ilmenite (Fe.TiO3), rutile (TiO2), zircon (ZrSiO4), garnet (Fe, Mg, Ca, Al Silicates),
sillimanite (Al2SiO5) and monazite (Ce, La, Th, Nd, Y) PO4. Parental rock is subjected to weathering and
erosion and transferred along with sea water and finally sediment in a suitable basin. The components of
mineral sands deposits all have high specific gravity (>2.85 gcm-3) and tend to concentrate during storms
when lighter components are carried offshore by strong littoral drift. Repeated storm erosion and reworking
over centuries may progressively enrich a mineral sand deposit. Most mineral sand deposits being mined
today were formed during the Holocene and Pleistocene periods(that is over the past 1.8 million years) but
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some date back into the Eocene period (58 million years ago)(Baxter, 1977; Shepherd 1990; Wallis and
Oakes, 1990; Hou and Warland, 2005). Globally, three heavy-mineral concentrate prospects began
production in 2014. World resources of anatase, ilmenite, and rutile are more than 2 billion tons. World
leading producers of heavy minerals are Australia, South Africa, USA, China, India and Ukraine and others
in minor quantities. Heavy Mineral placer deposits are distributed throughout the world with varying
mineralogical compositions, chemical and physical characteristics, and content of the heavy minerals w.r.t
gangue minerals in the placers deposits. Because of the above factors, there is a difference in grading of the
minerals in terms of their size, chemical composition and processing which plays a vital role in pricing the
valuable mineral in the international market.
Table 1: The classification of heavy minerals found throughout the world in beach placers.
Sl. Mineral/ [S.G] Composition Mass% Properties
Concentration of minerals from beach sand placers is primarily carried out in two stages based on the above
information tabulated regarding the properties of the minerals i.e.
Gravity separation (exploiting the difference between very heavy minerals (VHM), heavy
minerals (HM) from gangue like quartz, clay etc.) and
Magnetic and electrostatic separation (exploiting the magnetic, electrostatic and to a lesser extent
specific gravity (SG) properties of the minerals).
Gravity concentration circuits play a prominent role in beneficiation of heavy minerals. For instance:
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Beach Sands
Mineral Jig is used to treat placer deposits. Example of this type is Cleveland & Pan American Placer Jig.
Denver Mineral Jig is used to remove heavy mineral (HM) form closed grinding circuit, thus preventing
over grinding.
In-line pressure jig is used to treatment of alluvial deposits of precious metals or gemstones.
Kelsey Centrifugal Jig (Clifford 1999) is a batch centrifugal separation with an activated fluidized bed to
capture heavy minerals is applicable for high grade zircon recovery from mineral sand plant tailings and
also from aluminum silicate minerals, removal of tin impurities from rutile minerals, recovery of titanium
minerals from pigment plant tailings.
Combination of wet tables and air tables is used in beach sand mineral processing for recovery of fine
zircon from the heavy minerals.
Spiral Concentrator is the most prominent flowing film gravity separator used in beneficiation beach sand
placer deposits. Shallow angles to separate coal from shale, steeper angles for HM-silica separations,
steepest for HM from heavy waste minerals eg: Zircon (sp.gr:4.7) from kyanite & staurolite (sp.gr.3.6).
Pinched sluices includes Reichert Cone, application in beach sand beneficiation, pre-concentrate of tin,
gold and silver from the base metal sulphides, concentration of magnetite, chromite beneficiation, works
on the principle of the buddle.
Hence the gravity separation devices are widely accepted in many fields and are proved to efficient in usage
with ease of operation and maintenance, eco-friendly, low installation and operating cost, no reagents used,
high capacity and through output and less floor area occupation, and other related benefits that make these
devices recommended in many fields [5,6].
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methodology that are discussed to understand the gravity circuit in a better way and help in analyzing the
performance of the plant:
The performance of gravity separator circuit is measured by using the grade and recovery of valuable
minerals. This information can be used for both circuit design and evaluation. Drawback is that the
relationship between the enrichment ratio and the recovery is feed rate dependent (Burgess, 1997; Beneventi
et al., 2003) and also that the resulted shape and position of the curve obtained from the graphical data,
depend not only on the operating conditions but also the feed rate and feed grade respectively[7].
The combination of particle density, size, and shape determines where the particle reports to in separation
process. A standard industrial technique that can quickly and easily divide the size particle package into its
different density classes is not available. For heavy minerals the particle size <200µm no accurate
determination of the particle mass is possible. Sink and float method at higher densities (3.5 - 4g/cm3) is a
costly and time intensive exercise and it does not fractionate the more dense minerals (for example ilmenite,
zircon and monazite). Water based separation techniques (shaking tables or elutriators) have separation
inefficiencies that compromise the accuracy. Effective density fraction remains a challenge unless a
technique can be utilized that does not divide the mineral particles into physical fractions.
The Qemscan produces a textural data such as particle size, shape & mineralogical data that help in
predicting the density of the particle [8]. The density of the specified mineral is developed by the sip file that
describes the relation between the mineral data and analyzed data helps in converting the electron raw output
to mineral output i.e., particle surface to particle mass. That can be made available by analytical technique
such as X-ray diffraction analysis, X-ray fluorescence analysis, and inductively coupled plasma analysis and
iron titration to cross check the data obtained.
The Qemscan® software does consider the stereological effect in the assignment of a diameter to the particle
[9]. There are numerous articles discussing the theory behind stereological corrections [10, 11]. Rather than
aiming to demonstrate the available size density outputs, comparing it to other available techniques and
applying the technique to a density separator to evaluate the potential to improve the understanding of its
performance. Error is that the analyzer predicts the agglomerated particle in the resin as single particle and
gives the result based on it. The accuracy of the analysis is directly correlated with the number of particles
being analyzed. Particles smaller than 1µm are problematic since the interference with the background
becomes too significance. The size range (-500µm +1µm) restricts the application of this particle-by-particle
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technique to mostly heavy minerals, since other small types need to be milled finer which destroys the
natural particle entity.
Particle shape is difficult to define as a single number and for ease of sphericity is adopted. There is no
known technique available to use as a direct comparison with the high resolution particle density distribution
from the output from the Qemscan. The PDD line clearly demonstrates the characteristic densities of the
different mineral samples. The zircon product around 4.6gm/cm3 and rutile at 4.1gm/cm3, ilmenite showed a
density variation between 4.2 & 4.5gm/cm3. The non-magnetic fraction contained zircon by (60% by mass),
rutile around (15% by mass), lower density trash minerals (10% by mass between 3 & 4 gm/cm3) and with
quartz below 3.0 gm/cm3 (5% by mass). Applying the particle size distribution characterization and the
particle density distribution characterization to the products of a gravity separation process can lead to a
better understanding of the behavior of the separation of device. The high resolution size-density data can be
effectively used for gravity separator modelling.
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mineral concentrated in the last block in both the stream A&B containing 50% valuable mineral. Hence the
case (b) provides a higher combined yield about 4-5% more than that of case (a) with the same targeted grade
75% respectively. In fact, the grade of the valuable mineral in an individual particle can be mathematically
shown to be directly proportional to the reciprocal of the particle density of the two component system
(Anon, 1996). For instance particles of size range (1 & 0.1mm) both contains 50% of a high density
component will both have same grade. Accordingly from the above scenario incremental quality concept can
often be held constant by maintaining the same specific gravity cut points in all density separation circuits
and holds good for two component feed system prevailing the efficient separation in the circuits and the
densities of the host minerals does not vary that contribute the particle characteristic.
Note:
Stream – A
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Linear circuit analysis is a technique adopted for evaluating the effectiveness of different configurations of
unit operations in a mineral processing circuits initiated by Meloy (1983). It is used for evaluating different
arrangements of unit operations within a processing flowsheet. Drawback is that the details of yield and
grade are not framed. Some of the data that are outcome of linear circuit analysis are.
In Primary circuit separation, the products generated are not too crossed between the scavengers, cleaner or
else re-cleaner circuits rather than the product stream that are recycled back to the previous stages are capable
of obtaining sharpness of separation providing additional opportunity for misplaced particles to get a chance
to align themselves in respective streams. In case of multi-stage circuit the most efficient process is framed as
the rougher’s and placed ahead in the circuits, rather than that of scavenger and cleaner that has no sharpness
of separation in the process stream and this can be achieved by increased number of unit operations down the
scavenger and cleaner branches of circuits. The performance of a rougher- scavenger-cleaner circuit along
with their recycling streams approaches that of an ideal separator as the number of units in each branch
reaches infinity. Both incremental quality concept and circuit analysis, provide useful data regarding the
design, optimization and control of density based separation processes. Which include the optimization of
heavy media circuit performance, design of two stage spiral circuits and the real time control of plant grade.
Simulation is the latest and fastest seeding technological tool resulting in valuable information to understand
the equipment as well as the circuit performance in a better way than ever before. It gives a complete
characterization of individual streams and performance indicators such as power drawn, total flow rate etc.,
are computed and also design data to assess the capital cost involved. Mineral processing plant simulator
analyses are classified into three groups:
(i) Separation units (ii) Size reduction units and (iii) Medium separation units
The material in a flow stream is processed by one of the above three units [13]. The calculated product
stream properties are passed on by the simulator as feed to the next unit in the flowsheet. Hence, the material
is tracked completely through the plant and all the process streams are thus defined. The unit modules in any
simulator are linked together by an executive program. The success of a simulator lies in the accuracy of the
mathematical models of the unit operations an example of this is MODSIM that MODISM incorporates
excellent loop finding and tearing algorithm and provides detailed data i.e., the composition and
characterization of the particulate material in each stream and mass balance for an ore dressing plant [14]. It
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has a user friendly graphic interface for data input and modular structure to add new models of unit
processes.
The operators of mineral processing plants are often required to reduce the variability of a process output,
having three main sources, natural disturbances that affect the feed characteristics, the operation of the plant
and errors on the measurements used to calculate the plant performance. Data reconciliation (Hodouin et al.,
1989) can be used to attenuate the variation in the estimated performance indices due to measurement errors
[15]. The variability due to operation includes the way the equipment’s are operated and the quality of the
consumables (reagent, water…) required for the process. A problem due to the operation may be attenuated
by training practices and control strategies. If the problem is caused by variations in the feed characteristics
blending of the ore or stocking ores in different bins and feed forward control may attenuate the impact on
the variation of the process performances. Simulation was used to identify the sources of the variability
observed in the production results.
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concentrate after spiral concentration [18]. The presence of fine silica in the heavy mineral concentrate
affects the performance of dry electrostatic and magnetic separation processes.
For case of spiral-only separation in wet circuit removing of fine silica the recovery of coarser ilmenite and
other heavy minerals which are pushed to spirals outer rim resulting in decline of efficiency of separation. In
case of wet circuit spiral-only, maximizing the recovery by reducing the amount of material reporting to the
rougher and scavenger tailings, will result in an increase in the re-circulating middling material, hence
resulting in increase of no. of spirals and cause of over complexity of the circuit. The below flowsheet
describes about the systematic arrangement of spiral-floatex circuit for high grade mineral sand ore material.
It is found to be successful if the floatex comes at the end of the spiral circuit, in case of higher-grade mineral
sand ore material the concentrate from the rougher and scavenger is fed to the floatex, where the underflow
of the floatex is accepted as concentrate along with the cleaner concentrate and the overflow is subjected on
the spiral for recover of fine heavy mineral. In case of lower-grade mineral sand ore material, the concentrate
of the rougher and scavenger banks is fed to the cleaner bank and the concentrate produced in the cleaner
banks is fed to the floatex, where the floatex underflow material is screened and accepted as concentrate and
the overflow is fed to spirals for the recovery of fine heavy minerals.
Figure 4: Spiral-Floatex circuit for higher grade mineral sand ore material.
Studies conducted at carpco show that by moving the floatex density separator higher into the spiral circuit,
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Improves the performance of wet-gravity circuit and reducing the complexity of the circuit.
Increase in heavy mineral recovery was achieved without a reduction in concentrate grade for the higher
and lower grade ore material.
Reduces the number of spiral concentrate, and the costs of the associated with installation, operation and
maintenance.
Provides operator a control mechanism than can be quickly adjusted to accommodate variation in plant
feed.
3. Conclusions
Conservation of valuable resources while satisfying the continuously increasing demand from different end
users makes the beneficiation of lean & sub-grade ores essential. From the mineral conservation point of
view it is necessary to maximize utilization of lean ores to preserve high grade resources. It has also become
essential to reduce loss of values in tailings and recover values from previously generated tailings. Methods
for evaluating the gravity concentration circuits for better performance and optimizing of the process for
getting good grade and recovery is the need. Some of the available performance analysis methods like grade-
recovery method, particle characterization (size, shape and density by latest equipment’s (like Qemscan) that
determines the particle behavior in a separation media) are reported. The technical concept like incremental
quality concept and linear circuit analysis helps in better understanding of the circuits. Different methods of
simulation developed are used in analyzing the equipment performance and provide better data to
troubleshoot the problems. With the advancement in other combined fields, where gravity devices relay are
mechanical pumping devices, instrumentation (DCS) developments and others make possible to get the
desired input variables for better performance of the devices. Availability of literature and data relevant to
gravity separation circuit performance analysis is very scanty. Hence there is a scope and need to work on
such areas.
References
Mineral Processing Tecnology, By B.A. Wills; T.J. Naiper-Munn seventh edition Mineral Processing Design
and Opeartions By A. Gupta and D.S. Yan
Mineral Processing Plant Design, Practice, and Control. By Andrew L. Mular; Doug N. Halbe and Derek J.
Barratt. Volume 1
SME Mining Engineering Handbook; By Peter Darling 3rd edition Vol.2
66
Beach Sands
The role of concentration in modern processing plants, R.BURT, presented at Gravity ’99, Amsterdam.
Mineral Sands Geology and Exploration, ILUKA by Peter Benjamin May 2011.
Predicting and correcting grade-recovery curves: Theoretical aspects; By S.J. Neethling, J.J. Cilliers.
Grobler, J.D. and Bosman, J.B. Gravity separator performance evaluation using Qemscan® particle mineral
analysis. The 7th International Heavy Minerals Conference ‘What next’, The Southern African Institute of
Mining and Metallurgy, 2009.
Gay, S.L. and Keith, J.M. Geometric probability based stereological corrections, Anziam, M J. 45 (E), 2004.
pp. C618–C631.
Gay, S.L. and Keith, J.M. Stereological correction of the surface area of particle, Applied mineralogy ’01.
Brisbane, March 26–28.
Advances in G.C, By Ricky Quay Honaker, William Richard Forrest Page No. 01-10
Simulation of industrial gravity separation processes using a general purpose simulator A. Katti, B. K.
Mishra and S. P. Mehrotra IIT, Kanpur - 208 016.
King, R.P., (1993), MODSIM: A modular method for the design, balancing and simulation of ore dressing
plant flowsheets, Det. of Metallurgy University of Utah. Salt Lake City, USA.
The use of simulation for process diagnosis: Application to a gravity separator; By Bazin et al. /VInt. J. of
mineral processing (2012).
Gravity Concentration – A Better Way (or How to Produce Heavy Mineral Conc. and Not Recirculating
Load) By J Elder1, W Kow1, J Domenico2, and D Wyatt3. (IHMC June 2001).
Sivamohan, R & Forssberg, E, 1985. Principals of Spiral Conc. Int J Min Proc 15:157 – 171
Litter, A, 1986. Automatic hinder-settling classifier for hydraulic sizing and mineral beneficiation, Trans Inst
Min Metall (Sect C; Mineral Process Extr Metall), 95 C: 133-138.
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Beach Sands
INNOVATION IN THE EXPLOITATION OF MONAZITE IN ORDER TO EXTRACT THORIUM
Abstract
Monazite, which consists principally of the phosphates of rare earths and thorium, is the world's largest
source of thorium. Recent discoveries of thorium ores around the world have also signaled opportunity for
recovering large tonnages of thorium as a by-product of monazite mining operations in that area. India
having the 2nd highest reserves of thorium should utilize this source of energy to meet its future needs.
According to USGS, the estimated amount of thorium in India is 963,000 tonnes. Andra Pradesh, Kerela,
Bihar and Jharkhand have the highest thorium reserves in India. In this paper attempts have been made to
provide a suggestion in which the monazite should be exploited more from the inner parts of the Andhra
Pradesh and Jharkhand because the sea might show regression over there due to less rainfall annually which
in turn makes the lower deposits of monazite sand to come upwards more towards the coast. After the
extraction process, the thorium content containing 230Th, can be converted into (229Th) by beta decay method.
229
As Th is the only isotope of Thorium which shows fissionable reaction and chain reaction, it can be used
as a fuel. The isotope 229Th has a nuclear isomer (or metastable state) with remarkably low excitation energy.
Hence, it can be used as prosperous fuel in future.
1. Introduction
India is bestowed with its mineral deposits especially with a coastline of 6000 km. Heavy mineral deposits of
Manavalakuruchi in the state of Travancore (now Tamilnadu) was discovered by Schomberg , a German
chemist in 1909 which was proved richer and economical compared to rest of the world .
Interestingly, mineral sands then mined from rich seasonal beach washings for only one mineral i.e.
Monazite, which produce incandescence by infusing the paraffin mantle in a solution of thorium and cerium
compounds, lost its worth due to arrival of filament lamp.
The Atomic Energy Commission was commissioned in 1948 by Govt. of India. Indian Rare Earths Limited
was incorporated as a private company as a joint venture with the then Government of Travancore, Cochin in
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Beach Sands
1950 under the Indian Companies Act, 1913. IREL became a full-fledged Govt. undertaking under DAE in
1963. OSCOM was set up during 1972, construction had been started in 1975 and mining had been started in
1984.
Main objective of IREL is to emerge as a leading international player in the area of mining and separation of
beach sand deposits to produce minerals as well as process value added products.
2. Present scenario
This paper basically tackles on the areas where the mining of monazite on the beach placer deposit has been
conducted in the past few years. The few coastal areas are,
Atomic Minerals Directorate for Exploration and Research (AMD), a constituent unit of DAE, has
established Beach Sand Mineral Deposits containing the mineral Monazite along the coastal tracts in parts of
Odisha, Andhra Pradesh, Tamil Nadu and Kerala. The state-wise resources of in-situ monazite established by
AMD are as follows.
Monazite
State
(Millon Tonne)
Odisha 2.41
Andra Pradesh 3.72
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Beach Sands
Tamil Nadu 2.46
Kerela 1.90
West Bengal 1.22
Jharkhand 0.22
Total 11.93
Indian Rare Earths Limited (IREL), a Public Sector Undertaking under DAE has been producing monazite, a
mineral containing thorium from its mining and mineral separation plants located at Chavara, Kerala;
Manavalakurichi, Tamil Nadu and Orissa Sand Complex, Odisha. Indian monazite has an average content of
about 9-10% of Thorium Oxide.
In India, coastal placers are best developed along the beaches of the south-west coast of India, in Kerela and
south-western Tamilnadu. They are essentially beach or barrier deposits with development of dunes produced
by aeolian action which is prominent during the dry months. The beach sands of the Chavara bar (Kollam,
Kerela) contain 0.5-1% monazite at 9.0% ThO2. On the east coast of India, monazite concentrations consist
of extensive dunes fringing the coast in the Andra Pradesh state and the eastern part of the Tamilnadu and the
Orissa state. At Cuttak and Ganjam in the Orissa state, the thickness of the placer is about 30 cm with a
monazite content of 2.5%. The higher percentage of monazite in this area is attributed to the high density of
intrusion of the pegmatites and the leptynites in the hinterland. Elsewhere in India, monazite sand deposits
occur in other parts of Andra Pradesh. Monazite content of placers rarely exceeds 3 %, and the maximum Th
concentration is about 3,000 ppm in the sediment, with an average concentration of 60 ppm. In Andra
Pradesh, thick ilmenite and monazite placers are found around Vishakhapatnam and Bhimunipatnam.
Here, we are going to suggest some areas in which this mining should be done, in order to extract more
concentration of monazite sand. We have considered some parameters on which we are defining this
suggestion of ours. The parameters are,
Rather than concentrating on the States like Odisha, Kerela, Jharkhand, we should target on some selective
districts of Andra Pradesh and Tamil Nadu like :-
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Beach Sands
1. Andra Pradesh (Guntur, Prakasam, Coastal Part Of Chittor)
2. Tamil Nadu (Tuticorin , Ramanathpuram, Thanjavur, Pudukottal)
Annual rainfall
This map shows the annual scenario of rainfall in India; our main concern will only be Andhra Pradesh and
Tamilnadu. This map highlighted the areas in an increasing order from lowest to highest rainfall.
Andhra Pradesh
Now, if we take into consideration both the maps and we can circle out Guntur, Prakasam and Chittor. These
3 districts have an annual rainfall of about 750 – 1000 mm per annum; they have lesser amount of rainfall as
compared to the coastal areas in the state like Nellore, East Godavari etc., where the annual rainfall is about
(1000 – 1250 mm).
Due to lesser rainfall, these districts mainly Guntur and Prakasam become regressive zone, this means the sea
will show more regression. It is true that transgression and regression are the simultaneous processes, but the
71
Beach Sands
tides in these districts will be less and have lesser impact on these areas. Hence, once the transgression is
being done, then whatever the monazite sand is present will come up, will have lesser possibility that it will
erode back into the sea, because the rate of deposition in transgression is more as compared to that of erosion.
And being a regressive zone, these districts to some extent will have a higher concentration of monazite sand
as compared to other districts of the state.
Tamilnadu
Same, in the case of Tamilnadu, the districts like Tuticorin, Ramanathapuram, Thanjavur and Pudukottal,
these 4 districts will also show the regressive nature as Guntur and Prakasam are showing due to lesser
rainfall in region i.e. (750mm – 1000mm). Monazite mining in Tamilnadu is being conducted in
Manavalakuruchi, where the annual rainfall is about (1250mm-1500mm) so here the probability of more and
more occurrence to tides increases, hence we will not get much amount of monazite sand that we could get in
these 4 districts. Hence, the mining should be done in these districts, so that we can get more and more
amount of sand through which we can extract our desired element i.e. Thorium.
4. Conclusions
Monazite, which consists principally of the phosphates of rare earths and thorium, is the world's largest
source of thorium. Recent discoveries of thorium ores around the world have also signaled opportunity for
recovering large tonnages of thorium as a by-product of monazite mining operations in that area. India
having the 2nd highest reserves of thorium should utilize this source of energy to meet its future needs. In
order to meet these needs, we through this paper of ours try to give some suggestion that should be included
in the mining of monazite. The mining should be conducted in Andhra Pradesh, particulary in Guntur and
Prakasam, where due to lesser rainfall we can get more amount of monazite sand. Same in the case of Tamil
72
Beach Sands
nadu, the 4 shoreline districts i.e (Tuticorin, Thanjavur, Pudukottal, Ramanathapuram) will also show the
regressive nature, which ultimately increase the deposition of the monazite on the coast.
References
Rao Gajapathi, R, Sahoo P & Panda N K, Heavy mineral of sand deposits of Orissa, Exploration and
Research for Atomic Minerals , 13 (2001) 23-52.
Vaidyanathan R & Ghosh R N, Quaternary of the east coast of India, Curr Sci , 64 (1993) 804-816.
Komar P D & Wang Chi , Processes of selective grain transport and the formation of placers on beach, J.
Geol, 92(1984) 637-655.
Borreswar Rao C, Beach erosion and concentration of heavy minerals , J.Sed Petrol, 27 (1957) 143-147.
73
Beach Sands
74
Coal & Lignite
75
Coal & Lignite
EFFECTS OF REAGENTS AND KINETIC STUDIES ON FLOTATION PERFORMANCE OF
DUGDA COAL
Abhyarthana Pattanaik* and R. Venugopal, Diptimayee Nanda
Department of Fuel & Mineral Engineering, Indian School of Mines, Dhanbad
*Corresponding author: abhyap10@gmail.com
Abstract
Indian coals, in general, are of low grade, has high ash content and difficult-to-wash characteristics. For
meeting the quality requirement of industries and for compliance of environmental stipulation, it is
necessary to produce clean coal of high yield and desired ash content by adopting suitable beneficiation.
Froth flotation is commonly used for beneficiation of coal fines in India and abroad, and the efficiency of
flotation depends on the reagents i.e. collector and frother dosages.
Coal sample was collected from Dugda coal washery (BCCL) and the sample was of Carbon content
46.5%, moisture content 1.13%, volatile matter 18.72% and ash content 33.65%. Flotation experiments
were carried out by varying collector and frother dosages, at three levels, each to study their influence on
yield and ash content of clean coal.
Pine oil has been used as frother at different dosages of 0.25, 0.50 and 0.75kg/ton. Diesel oil has been
used as collector at various dosages of 0.50, 0.75 and 1.0kg/ton. From the results, it was found that the
coal responded well to the collector dosage of 0.75kg/ton and frother dosages of 0.75kg/ton.
It was observed that the best overall result has been achieved at collector dosage 0.75kg/ton and frother
dosage 0.75kg/ton with an ash content of 18.8% and 64.44% yield.
The concentrates were collected at different time intervals (15, 30, 45, 60, 75 and 90 secs) and then
kinetic studies were carried out. The process follows first order kinetics and from the experiments, the
rate constant values at different collector and frother dosages were estimated. Rate constant was found to
be highest at collector dosage of 0.75kg/ton and frother dosage of 0.50 kg/ton within a less time period. It
means that Dugda coal responds well to flotation and can be floated easily within a short flotation time.
1. Introduction
With the rapid depletion of oil and natural gas as main energy sources and growing power consumption,
utilization of the coal deposits has become a natural alternative for electrical power generation. In India,
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Coal & Lignite
only 26.9% of the total reserves is commercially viable coking coal which is very limited for vastly
growing demand of steel plants, which makes the coal more precious[1]. An increase in the ash content of
a coal concentrate by 1% over a critical limit results in an increase in coke consumption by about 4–5% as
well as decreasing blast furnace productivity by about 3–6%; therefore coal preparation plants are always
pressurised to supply coal with low ash content [2].But this source of energy is facing problems due to
varied reasons, which include grade, mining technology, marketing and business policies etc. The coal
grade in India is depleting day by day, as mining of deeper seams increase the ash percentage gradually.
This is further aggravated by mechanisation of mining method, where it is unable to mine only coal as in
manual mining, but nowadays along with the coal, stone or dirt band is mined resulting in more fines[3].In
India , coal mining was started in the year 1974 in eastern part of west Bengal. India produced
approximately 600 Mt of coal in 2013-14 becoming the third biggest coal producer in the world.
In order to upgrade the coal quality to 17-19% ash, good washing techniques are needed. Hence froth
flotation, one of the efficient and established techniques to treat fines, is practised widely. At present,
flotation is the only process available that permits the production of concentrates from fine grained base
metal mined at the majority of the ore deposits [4].
Froth flotation can be coined as a highly adaptable method for the physical separation of particles, based
on the difference in surface hydrophobicity, the ability of air bubbles to selectively adhere to the specific
mineral surfaces. Flotation is one of the most effective separation methods for fine coal processing [5]. It is
very effective for coal cleaning, since coal is naturally hydrophobic.
Coal flotation is a compound process involving several phases .These phases interact with each other
involving other species like promoting reagents and dissolved ions in water. The physical and
chemical interaction induces the execution of flotation. In this process, frothers should also be able
to enhance collector adsorption on coal particle surface. This combined adsorption improves
kinetics, final recovery and decreases reagent consumption. [6] It is beneficial that due to hydrophobic
nature of coal, frother adsorb not only on gas/liquid interface but also on the coal. Several researchers
have examined the adsorption of frothers like MIBC and a-terpineol on coal [7,8]. Literature reviews about
[9,10,11]
the adsorption of cresols, and phenol onto coals of various ranks . The reverse flotation, in which
collectors are used to render the gangue particle surfaces hydrophobicity, seems to be a good alternative
for the cleaning of low rank coals because low rank coals are hydrophobic, so by increasing the electrical
charge of the particles and promoting repulsive forces, flotation reagents are not compatible with
viscosity reducers [12].
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Coal & Lignite
According to Laurila et al. (2002)[13], the major variables in this process can be listed as :
• Slurry flow rate (or retention time)
• Slurry composition (Nature of solid content, concentration)
• Chemical reagents (Frothers, collectors, pH controllers)
• Electrochemical potential (Eh) and Conductivity
• Froth properties (Bubble size, density, froth stability)
• Slurry levels and air flow rates
Flotation kinetics models that draw direct analogy with chemical reaction kinetics, particularly the first
[14]
order models, are most widely used in the literature. Mika and Fuerstenau experimentally found that
the first order kinetic phenomenon for ideal mixing is convenient for both batch and continuous flotation
operations. Beloglozov[15] and Schuman[16] found from batch test experiments that the first order rate
[17]
constant increased with collector dosage up to a certain limit. Mori et al. observed that initially the
flotation process obeys zero order kinetics whereas at the end it follows second order. Other factors
affecting the flotation kinetics are discussed below.
Aeration and agitation:- The flotation rate constant is established in response to variation of aeration.
Thorne et.al.[18] examined the linearity between the air addition rate and the recovery of valuable mineral.
The interaction characteristics of each ore depends upon its mineralogy and the quality & quantity of
reagents [19,20,21]. Flotation experiments were carried out on coal fines from Dugda Coal Washery, BCCL,
Dhanbad, Jharkhand to understand the flotation behaviour. The main objective of present study is to
investigate the response of material in a single stage flotation in terms of recovery and to discuss kinetic
analysis of flotation phenomena as a function of reagent dosages.
2. Experiments
2.1 Materials
20 kg of coal sample was collected and then sieving was carried out through the 0.5mm sieve. The -
0.5mm sample was subjected to systematic sampling using riffling, coning and quartering. Proximate
analysis and size analysis were done on the representative sample.
2.2 Methods
The size analysis data were given in table 1:
One poly pack of sample was passed through 212 micron for proximate analysis and the -212 micron was
subjected to proximate analysis and results obtained are given below.
Moisture (%) = 1.13
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Coal & Lignite
Ash (%) = 33.65
Volatile matter (%) = 18.72
The experiments were carried out in a Denver D-12 laboratory flotation machine, using 3.5litre cell. The
arrangement of constant water level was provided, to supply constant water in the cell to maintain a
continuous flow of froth from the collecting end of the cell. The compressed air supply is done through a
rubber pipe to hollow impeller shaft through which air is released at bottom of the cell. The baffle
arrangement is provided to increase the turbulence for proper mixing.
The flotation experiments, comprising three levels each of diesel oil (as collector) and pine oil (as
frother), were carried out.
Collector dosage (kg/ton): 0.5, 0.75 and 1.0
Frother dosage (kg/ton): 0.25, 0.5 and 0.75
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Coal & Lignite
10% pulp density of coal slurry was prepared by taking 360 gm of coal and adding the required volume of
water, and then it was thoroughly mixed and transferred to the cell. The slurry was conditioned for five
minutes and pre-estimated amount of diesel oil was added. After conditioning the slurry for 5 minutes,
required amount of pine oil was added and again conditioned for 5 minutes. Aeration was done by
opening inlet valve and froth was collected at different time intervals (15, 30, 45, 60, 75, 90 secs). The
concentrates collected at the above time intervals were filtered, dried and the dry coal was weighed. Ash
percentage of concentrate collected at different intervals of time and different reagent levels and the
tailings were determined.
60 60
15 sec
50 50 50
15 sec 30 sec
40 15 sec 40 30 sec 40
45 sec
30 sec 30 45 sec 30
30 60 sec
Ash%
45 sec 60 sec
20 20 20 75 sec
60 sec 75 sec
10 75 sec 10 90 sec 10 90 sec
90 sec
0 0 0
0
0 1
Collector dose
2 0 1
Collector dose
2 Collector1 Dose 2
Figure 1(a), (b), (c): Plots between the ash% and various collector dosages at constant frother dosages,
F1(0.25 kg/ton), F2(0.5kg/ton), F3(0.75kg/ton) respectively.
The ash content decrease gradually with increase in collector dosage at F1 in all flotation periods as in Fig
1(a).The trend reverses to a steady but marginal increase in percentage of ash as the collector dosage is
increased at F2 at all the flotation time intervals as in Fig 1(b). Fig1(c) shows a contrasting trend in the
percentage of ash, for a change in collector dosage, at 0.75 kg/ton of frother dosage, at different time
intervals. With the increasing collector dosage, the hydrophobicity increases and thus the ash content may
have decreased and yield may have increased due to high probability of adhesion between colliding
particles and air bubble. With the increase in time, the ash% increases, because initially, more amount of
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Coal & Lignite
collector gets sorbed on fully liberated coal particles and they get more chances to float, whereas, at later
time intervals interlocked particles also float due to partially hydrophobic nature.
60 60
50 50
15 sec 15 sec
40 30 sec 40 30 sec
Ash%
30 45 sec 30 45 sec
20 60 sec 20 60 sec
10 75 sec 10 75 sec
0 90 sec 90 sec
0
0 0.5 1 0 0.5 1
Frother dose
Figure 2(a) Figure 2 (b)
60
50 15 sec
40 30 sec
30 45 sec
20 60 sec
10 75 sec
0 90 sec
0 0.5 1
Figure 2(c)
Figure 2 (a), (b), (c): represent the ash% at C1 (0.50 kg/ton), C2 (0.75kg/ton), C3 (1 kg/ton) at various
frother dosages respectively.
The ash content of clean coal decreases gradually with increase in frother dosage at C1 in all experiment
periods (Fig 2a).The trend reverses to a steady but marginal increase in percentage of ash as the frother
dosage is increased to C2 at all the flotation time intervals (Fig 2b). Fig 2c shows contrasting trend in
percentage of ash for a change in frother dosage at 1.0 kg/ton of collector dosage at different time
intervals. This decreasing recovery may be due to the bubbles coalescing with each other, thus resulting
in the particles detaching from or remain attached to the coalesced bubble. The more frequently a bubble
coalesces with other bubbles whilst rising through the froth, the more likely is the detachment of the
hydrophobic particles at some stage and drain from the froth phase.
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Coal & Lignite
3.3 The recovery and rate constant values (k) at different collector and frother combinations at
different time intervals are given in the tables 3 to 11.
3.4 The recovery and time graphs are plotted below at different collectors and frothers combination
(figs 3 a-c)
90 70
80 R² = 0.9965
R² = 0.9956 60
70
50
60 C1F1
50 40
C2F1 C1F2
Recovery (%)
Recovery (%
40 30 C2F2
C3F1
30 C3F2
20
20 POLY. POLY. (C3F2)
(C3F1) 10
10
0 0
0 20 40 60 80 100 0 20 40 60 80 100
-10
Time (sec) Time (sec) Fig 3(b)
Fig 3(a)
80
70
R² = 0.9963
60
Recovery (%)
50 C1F3
40 C2F3
C3F3
30
POLY. (C2F3)
20
10
0
0 20 40 60 80 100
Time (sec) Fig 3(c)
Figure 3 (a), (b), (c): Plots of recovery over time with various reagents.
The maximum recovery is obtained at C2F1 reagent combination; hence it is the optimum dosage for the
flotation of Dugda coal fines. Fig 3(a) follows polynomial trendline of order 2 while Fig 3(b) and Fig 3(c)
follow polynomial trendline of order 3.
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Coal & Lignite
0.04
0.035
0.03
0.025
Rate constant
C1F1
0.02
0.015 C2F1
0.01 C3F1
0.005
0
0 20 40 60 80 100
Time
Rate constant follows an increasing order at C1F1 and C3F1 whereas at C2F1 dosage, the rate constant
increases initially and after that it depicts a decreasing trend. The hydrophobicity increases gradually with
increased addition of collector dosage which results in enhancement of collection due to high probability
of adhesion between colliding particle and air bubble. Then the value of rate constant remains constant or
follows a decreasing trend, perhaps due to the formation of multi layers.
0.05 0.04
0.035
0.04
Rate constant
0.03
Rate constant
In Fig 4(b), the rate constant first increases then decreases for C2F2 and C3F3 whereas for C1F2, it
increases later decreases marginally and then increases. In Fig 4(c), the rate constant first increases then
decreases and then increases at C1F3, C2F3, C3F3 dosages.
At highest frother dosage, the rate constant value is decreasing because of coalescence of bubbles with
each other, which results in attachment or detachment of particles to the new bubble. More the
coalescence of bubble, more the detachment of hydrophobic particles occur and sink down, which results
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Coal & Lignite
in decreasing trend of rate constant. The rate constant increase at higher dosage may be due to less
drainage of particles from the froth phase.
4
3.5 C1F1
ln (R∞/(R∞-R))
C2F1
3
C3F1
2.5 C1F2
2 C2F2
1.5 C3F2
1 C1F3
C2F3
0.5
C3F3
0
0 50 100
Time(sec)
Figure 5(a): Plot of time vs ln (R∞/(R∞ -R)).
This graph follows a linear trend which clearly supports that rate constant is following 1st order kinetics
i.e. R= R∞ (1-e(-kt)).
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Coal & Lignite
Table 5: Collector – 1.0 kg/ton and frother – 0.25kg/ton (C3F1).
time wt(g) wt(%) ash% cum wt% cum ash% recovery k
0 0 0 0 0 0 0 0
15 125 34.72 22 34.72 22 24.0687249 0.02386
30 98 27.22 29.81 61.94 25.43216338 49.6369619 0.032293
45 45 12.5 35.98 74.44 27.2033611 63.8086589 0.035501
60 20 5.55 39.28 79.99 28.04128266 70.6780011 0.035827
75 10 2.78 43.67 82.77 28.56620515 74.5034171 0.035705
90 6 1.67 46.98 84.44 28.93038134 76.9755976 0.036392
tailing 56 15.56 46.96 100 31.73579 100
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Coal & Lignite
Table 9: Collector - 0.50 kg/ton and frother – 0.75kg/ton (C1F3).
time wt(g) wt(%) ash% cum wt% cum ash% recovery k
0 0 0 0 0 0 0 0
15 185 51.39 17.5 51.39 17.5 29.3695273 0.036265
30 44 12.22 30.7 63.61 20.0358277 41.6210444 0.030095
45 35 9.73 39.11 73.34 22.56639351 54.0484636 0.032865
60 16 4.44 42.26 77.78 23.69058498 60.1760967 0.032728
75 12 3.33 44.7 81.11 24.55313402 65.0371686 0.035287
90 6 1.67 46.11 82.78 24.98802126 67.5519016 0.037258
tailing 62 17.22 57.7 100 30.621024 100
4. Conclusions
The above results indicate that, in general, the intermediate collector dosage (i.e., C2 level) is found to be
the optimum level, below which the recovery is less. Additions of higher dosages have no effect or even
deleterious effect on the recovery and grade of the bulk and individual size fractions. Present study
reveals that the lowest level of frother i.e., F1 is the optimum dosage, the excess addition may result in
deleterious effect. It would be prudent to analyze the behaviour of coal to effectively understand the
flotation and arrive at a flotation strategy to maximise recovery at the desired ash percentage. Rate
constant was found to be maximum at collector dosage of 0.75kg/ton and frother dosage of 0.50 kg/ton
within a less time period. It means that Dugda coal responds well to flotation and can be floated easily
within a short flotation time.
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Coal & Lignite
Acknowledgements
The authors are thankful to Mr. Anil Kumar for his contribution, support and permission to publish the
paper.
References
King R.P., The principles of flotation, 1st Edition(1982).
S.Dey, K.K.Bhattacharya, Split and collectorless flotation to medium coking coal fines for multi-product
zero waste concept. Fuel Process Technology., 88(2007),pp.585-590.
Venugopal. R and Rajendra Prasad. N, Comparative studies on the performance of the frothers on
flotation of coal fines.
Tuli, Praveen, Effects of reagents on flotation process parameters, M.Tech thesis, ISM, Dhanbad 1984.
Renhe Jia, Guy H. Harris, Douglas W, 2000. Fuerstenau. An improved class of universal collectors for
the flotation of oxidized and low-rank coal, International Journal of Mineral Processing, 2000, (58): 99
118.
Tailor,S.R.Miller,K.J.&Deurbrouck,A.W.,surfaces chemical problems in coal
utilization.morgantown,W.V.jan.1980.
Fuerstenau, D.W and Pradip. "Adsorption of frothers at coal/water interfaces", Colloids and Surfaces,
vol. 4, pp. 229-243 (1982).
Miller, J.D., Lin, C.L. and Chang, S.S. “MIBC adsorption at the coal/water interface”,Colloids and
Surfaces, vol. 7, pp. 351-355 (1983).
Gurses, A., Bayrakceken, S. and Sahin, M. “Adsorption of o-cresol from aqueous solution on coal”,
Colloids and Surfaces, vol. 64, pp. 7-13 (1992).
Eveson, G.F.”Removing shale particles from coal or from coal-washing effluent by froth flotation”,
British Patent 863,805 (1961).
Laskowski, J.S. “Fundamental properties of flotation frothers”, Proc. 22nd Int. Mineral Processing
Congress (L. Lorenzen and D.J.Bradshaw, eds.), Cape Town, vol. 2, pp.788-797 (2003).
Pawlik, M. and Laskowski, J.S. “Coal reverse flotation: Part I. Adsorption of dodecyltrimethyl
ammonium bromide and humic acids onto coal and silica”, Coal Preparation, vol. 23, pp. 91-112 (2003).
Laurila H, Karesvuori J, Tiili O. Strategies for instrumentation and control of flotation circuits, Mineral
processing plant design, practice and control. Vol. 1 (2002), 2174-2195.
Mika, T.S., Fuerstenau, D.W.,“A microscopic model of the flotation process”. (Paper no.8-4) VIII,
International mineral processing congress- Leningard, 1969.
Beloglozov KF. “Tsvelyne Metal”. vol.9, 1939, p.891.
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Schumann.R “Flotation kinetics – methods for steady state study of flotation problem” J.Phy.Chem.,
p.1942, p.891.
Mori.S et al., “Kinetic studies of fluoride flotation”, XV International Mineral Processing Congress,
Cannes, France, 1983.
Thorne G.C, Manlapig E.V., Hall J.S. and Lynch A.J., “Modelling of industrial sulphide flotation circuits”,
Flotation–A.M.Gaudin Memorial Volume, (Ed) M.C.Fuerstenau, 1976, p.725.
Bull, W.R., The rate of flotation of mineral particles in sulphides ores, Proc. Of Aus. Inst. Of Min. & Met. ,
vol. 254, 1966, pp.69-78.
Viswanatha D, Sanyal P, Venugopal R., Rao R. & Rao T.C., “Flotation characteristics of chalcopyriye
ore”, J I E (I).
Tomlinson, H.S. and Fleming, M.G., “Flotation rate studies”, Proc. Sixth International 6th process
congress, cannes, (Ed) A.Roberts, Pergamon, 1963, p.5e.
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Coal & Lignite
ANALYSIS OF EFFECT OF DISSOLVED ION-WATER CHEMISTRY ON THE
PERFORMANCE OF COAL FLOTATION
Mousumi Gharai*, R. Venugopal
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad-826004
*Corresponding author: mousumigharai00@gmail.com
Abstract
In coal preparation plants, the run of mines coal undergoes a series of operations, including crushing,
gravity separation, wet screening, froth flotation and dewatering etc. As these unit operations are water-
intensive, a large volume of water is required for processing. Nearly 80-85% of the total volume of plant
water is used in flotation circuits for treating fine coal (-0.5mm). Since the plants operate on closed-
circuit mode, water is reused after single processing of coal. The recycled water contains a variety of
suspended solids, dissolved trace elements, residual reagents (collector, frother and flocculants) and total
dissolved ions, etc. Thus the water chemistry plays an important role in the interaction between minerals
present in coal and the reagents used in flotation process, altering the reagent-solution and mineral-
solution equilibrium. An understanding of these interactions and the effect of the different dissolved ions
on the flotation performance is essential.
In this study, flotation experiments have been carried out on coal sample collected from West Bokaro
Washery, TATA STEEL Ltd, India, to analyze the effect of dissolved ions in recycled water on the yield
and recovery of clean coal using two types of frothers; Frother A and Frother B. Frother A is a relatively
newly developed frother having Ketonic functional group and Frother B is a commercial frother, the
collector in both cases being the High Speed Diesel oil (HSD). The demineralised water has been
collected from de-mineral plant of Tata Steel Ltd. To mimic the plant recycle water, synthetic water has
been prepared by adding different types of ions such as CaCl2, MgCl2, CaSO4, NaCl, Na2SO4, Na2CO3
and NaHCO3 to the recycle water.
The results show that with Frother A, NaCl and MgCl2 are showing negative effect on clean coal yield
whereas Na2SO4 and NaHCO3 are showing positive effects. With Frother B, NaCl, CaCl2, MgCl2,
Na2CO3 and NaHCO3 ions are showing positive effect whereas Na2SO4 is showing marginal
improvement in the yield of clean coal.
1. Introduction
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Coal & Lignite
Separation of naturally hydrophobic particles, such as coal, by flotation is known to be enhanced with the
addition of salt solutions into the system. The flotation of naturally hydrophobic particles in inorganic
electrolyte solutions was first documented during 1930s. Researches show that the addition of electrolytes
to the flotation system enhances the flotation recovery depending on their type and concentration
(Kurniawan et al, 2011). The electrolytes seem to stabilize the bubbles against coalescence (Pugh et al,
1997). Several surface chemical mechanisms have been proposed to explain the flotation process. This
range from the action of the electrolytes in,
a) Disruption of hydration layers surrounding the particles & enhancing bubble-particle capture.
c) Increasing charge on the surface of the bubbles to prevent primary bubble coalescence
A direct correlation is found to exist between the flotation recovery and the bubble size distribution of the
froth phase. With increasing the electrolyte concentration, the bubble size decreases which in turn
increases the flotation recovery (Kurniawan et al, 2011; Rao and Finch, 1989). It is found that the
inorganic electrolyte reduces the surface hydration of the naturally hydrophobic minerals, so that it
provides attractive forces between the air bubbles and the particles (Kurniawan et al, 2011). The
adsorption of salt ions disrupts the hydrated layers surrounding mineral particles. This disruption
primarily occurs at high electrolyte concentrations, where specific adsorption of cations may change the
surface charge of the particles and causes strong attraction between the particles and the bubbles.
It is suggested that the coalescence in pure water is caused by a strong hydrophobic force which opposes
the hydrodynamic repulsion existing between the colliding bubbles. The reduction in attraction between
bubbles occurred with the adsorption of certain ion pairs at the air/water interface which reduces this
hydrophobic force. This is explained by the local influence of ion on water structure which is someway
related to the hydrophobic force.
In this paper, flotation experiments have been carried out to compare the effect of dissolved ions in
recycled water (from washery) on coal flotation using two types of frothers i.e. Frother A, a newly
developed frother having ketonic functional group and frother B, a commercial frother.
2. Experimental
2.1 Material preparation
The representative coal sample was collected from the West Bokaro Washery, TATA Steel Ltd, India.
The flotation reagents, collector: High Speed Diesel oil (HSD) and frother (A&B) were used in the study.
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Coal & Lignite
The demineralised (DM) water has been collected from de-mineral plant from power house of Tata Steel
Ltd, Jamshedpur. The samples were first allowed to settle, decanted and then dried at 600 C. Ash analysis,
carried out according to ASTM D 3174-73 standard, showed that the sample contains 24% ash.
The representative sample of coal flotation feed was screened into different particle size fractions. Total
weight and mineral matter (ash) distribution among each particle size fraction were analyzed.
30 35
25 30
20 25
Ash %
20
Wt%
15
Wt% 15
10 10
Ash%
5 5
0 0
+30 +60 +100 +200 +300 +400 -400
Size (mesh)
Flotation experiments were carried out by using synthetic water. Synthetic water was prepared by adding
the required quantities of electrolytes/salts to the DM water. The effect of each ion on flotation
performance was studied. The flotation experiments were carried out by keeping collector concentration
constant at 1kg/ton and frother concentration at 0.1kg/ton for both frother ‘A’ and ‘B’. The experimental
plan with different ions is shown in Table1.
A 2.5-litre capacity flotation cell of Denver D-12 was used for flotation tests. This unit has a baffle
arrangement at bottom to avoid swirling of the slurry within the cell and an impeller is provided for
proper mixing of slurry, the speed of which can be controlled by a speed regulator. A compressor is also
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Coal & Lignite
provided to supply air to the cell in the range of 0-20 lpm in interval of 1 lpm. The cell has an automatic
pulp level controller through make up water tank and a froth removal system.
For each batch flotation, 250g of coal sample were taken. Additional water was added to maintain
required pulp density i.e. 10% solid content. Slurry was allowed to condition for 3minutes at the impeller
speed of 850rpm to 950rpm. Then Diesel oil (collector) and frother was added and was conditioned for 3
minutes each.
The cell was filled with water up to the marked height; air inlet valve was opened and kept at 3lpm. The
froth samples were collected after 5, 30, 90 and 180seconds of flotation. After the final sample was
collected, the machine was stopped. The froth products and the tailings were dried, weighed and analyzed
for their ash content. The yield and recovery of combustible material calculated at the concentrate 1 is
collected at time 5 seconds.
The parameters which were kept constant during the experiments are given in table 2.
Frother A: There was no change in the pH of the slurry from 100ppm to 500ppm of sodium chloride.
From the figure 2, it is observed that the maximum yield and recovery is obtained at 400ppm of NaCl,
after which the yield and recovery decreased.
Frother B: There was no change in the pH of the slurry from 100ppm to 500ppm of sodium chloride.
From the figure 3, it is observed that the yield and recovery increased up to 200ppm, then decreased at
300ppm and again increased. The maximum yield and recovery was observed at 500ppm of NaCl.
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Coal & Lignite
60 NaCl 60 70 NaCl 70
Recovery%
Recovery%
60 60
40 40 50 50
Yield%
Yield%
40 40
Yield% 30 Yield% 30
20 20 20 20
Recovery% Recovery%
10 10
0 0 0 0
0 100 200 300 400 500 600 0 100 200 300 400 500 600
ppm ppm
Frother A: There was a slightly change in the pH of the slurry from 100ppm to 500ppm of calcium
chloride. From the figure 4, it is observed that the yield and recovery slightly increased and then
decreased at 300ppm and again increased. The maximum yield and recovery is at 500ppm of CaCl2.
Frother B: There was slightly change in the pH of the slurry from 100ppm to 500ppm of calcium
chloride. From the figure 5, it is observed that the yield and recovery slightly increased and then
decreased at 300ppm and again increased. The maximum yield and recovery is at 500ppm of CaCl2.
CaCl2 60 CaCl2 60
Recovery%
Recovery%
50 50 40 40
Yield%
Yield%
Yield% 20 yield% 20
Recovery% Recovery%
0 0 0 0
0 100 200 ppm
300 400 500 600 0 100 200 ppm
300 400 500 600
Frother B: There was change in the pH of the slurry from 100ppm to 500ppm of calcium chloride. From
the figure 7, it is observed that the yield and recovery decreased slightly and then increased at 400ppm
and again decreased. The maximum yield and recovery is at 400ppm of MgCl2.
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Coal & Lignite
MgCl2 70
MgCl2 70
60 60
Recovery%
Recovery%
60 60
Yield %
40 40 50 50
Yield%
40 40
Yield% 30 Yield% 30
20 Recovery% 20 20 Recovery% 20
10 10
0 0 0 0
0 100 200 300 400 500 600 0 100 200 ppm
300 400 500 600
ppm
Frother A: There was change in the pH of the slurry from 150ppm to 600ppm of calcium sulphate. From
the figure 8, it is observed that the yield and recovery decreased continuously. The maximum yield and
recovery is at 150ppm of CaSO4.
60 CaSO4 60
Recovery%
40 40
Yield%
20 Yield% 20
Recovery%
0 0
0 100 200 300 400 500 600 700
ppm
Figure 8: Frother A.
3.1.5 Effect of NaHCO3 on coal flotation:
Frother A: There was change in the pH of the slurry from 100ppm to 500ppm of sodium chloride. From
the figure 9, it is observed that the yield and recovery increased slightly up to 200ppm, decreased at
300ppm and again increased. The maximum yield and recovery is at 400ppm of NaHCO3.
Frother B: There was change in the pH of the slurry from 100ppm to 500ppm of sodium chloride. From
the figure 10, it is observed that the yield and recovery decreased slightly up to 200ppm and then
gradually increased. The maximum yield and recovery is at 100ppm of NaHCO3.
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Coal & Lignite
60
NaHCO3 60 NaHCO3
50 50 100 100
Recovery%
Recovery%
40 40
Yield %
Yield%
30 30
20 Yield% 20 50 50
Recovery% Yield%
10 10
Recovery%
0 0
0 0
0 100 200 300 400 500 600
ppm 0 100 200 ppm
300 400 500 600
Frother A: There was change in the pH of the slurry from 100ppm to 500ppm of sodium chloride. From
the figure 11, it is observed that the yield and recovery decreased slightly up to 200ppm, increased at
300ppm and again decreased. The maximum yield and recovery was observed at 100ppm of Na2CO3.
Na2CO3 Na2CO3
Recovery%
60 60 80 80
Recovery%
70 70
40 40 60 60
Yield%
Yield%
50 50
20 20 40 40
Yield% 30 Yield% 30
20 Recovery% 20
0 0 10 10
0 100 200 300 400 500 600 0 0
ppm 0 100 200 300 400 500 600
ppm
Frother B: There was no change in the pH of the slurry from 200ppm to 800ppm of magnesium chloride
and calcium chloride. From the figure 14, it is observed that the yield and recovery increased slightly up
to 350ppm, then gradually decreased up to 500ppm, increased at 600ppm and then decreased at 800ppm.
The maximum yield and recovery was observed at 200ppm of magnesium chloride and calcium chloride.
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Coal & Lignite
MgCl2+CaCl2 MgCl2+CaCl2
70 70 70 70
Recovery%
60 60 60 60
Recovery%
yield% 50 50 50 50
Yield%
40 40 40 40
30 Yield% 30 30 Yield% 30
20 Recovery% 20 20 Recovery% 20
10 10 10 10
0 0 0 0
0 200 400 600 800 0 200 400 600 800
ppm ppm
Frother A: There was change in the pH of the slurry from 200ppm to 800ppm of sodium chloride. From
the figure 15, it is observed that the yield and recovery decreased slightly up to 400ppm, increased at
600ppm and again decreased. The maximum yield and recovery was observed at 600ppm of Na2SO4.
Frother B: There was change in the pH of the slurry from 200ppm to 800ppm of sodium chloride. From
the figure 16, it is observed that the yield and recovery decreased slightly up to 400ppm, increased at
600ppm and again decreased. The maximum yield and recovery was observed at 600ppm of Na2SO4.
60 Na2SO4 60 70 Na2SO4 70
Recovery%
50 50 60 60
Recovery%
40 40 50 50
Yield%
40 40
Yield
30 30
Yield% 30 Yield% 30
20 20 20 20
Recovery% Recovery%
10 10 10 10
0 0 0 0
0 200 400 600 800 0 200 400 600 800
ppm ppm
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Table 3: Comparison table for frother A and B.
Frother A Frother B
ppm Yield Recovery S.E ppm Yield Recovery S.E
% % % %
DM water --------- 46.81 54.10 28.48 -------- 53.58 60.90 28.81
NaCl 400 39.59 47.16 26.27 500 54.31 62.08 30.25
CaCl2 500 44.52 53.00 30.0 200 51.92 58.11 28.37
MgCl2 400 48.37 56.16 27.01 200 50.78 58.13 30.74
NaHCO3 400 47.1 56.16 32.80 400 57.25 65.03 32.15
Na2CO3 300 44.67 52.19 30.58 300 65.25 72.88 30.60
CaCl2+MgCl2 350 47.88 53.28 22.44 200 51.13 58.92 29.79
Na2SO4 800 46.99 53.68 27.44 600 50.02 57.56 29.90
Acknowledgements
The authors would like to express their deepest thanks and appreciation to Mr. Ajay Kumar Gupta (ISM
Dhanbad). The authors gratefully acknowledge the faculty and staff of the department of Fuel and
Mineral Engineering of ISM for their encouragement and support.
References
A.U. Kurniawan, O. Ozdemir, A.V. Nguyen, P. Ofori, B. Firth, Flotation of coal particles in MgCl2,
NaCl, and NaClO3 solutions in the absence and presence of Dowfroth 250, International Journal of
Mineral Processing, Volume 98, Issues 3–4, 9 March 2011, pages 137–144.
R.J. Pugh, P. Weissenborn, O. Paulson, Flotation in inorganic electrolytes; the relationship between
recover of hydrophobic particles, surface tension, bubble coalescence and gas solubility, International
Journal of Mineral Processing Volume 51, Issues 1–4, October 1997, pages 125–138.
Application of Surface Science to Advancing Flotation Technology.
S.R Rao, J.A Finch, A review of water re-use in flotation, Minerals Engineering, Volume 2, Issue 1,
1989, pages 65-85.
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Coal & Lignite
STUDIES ON SEPARATION OF MACERALS FROM COAL BY FROTH FLOTATION
Saroj Kumar Sahoo*1, Nikkam Suresh1 and A. K. Varma2
Department of Fuel and Mineral Engineering, ISM-Dhanbad
Department of Applied Geology, ISM-Dhanbad
Corresponding author: sarojsahoo.19@gmail.com
Abstract
In the past, coal maceral separation from shale have been carried out based on density difference e.g.,
sink-float analysis, density gradient centrifugation (DGC) techniques etc. These approaches are of limited
success. Froth flotation is a physicochemical process consisting two distinct zones viz., pulp and froth
zones. Rate of floatability of individual size range particles varies with their ash percent and the maceral
content present. Therefore, the flotation rate constant eventually becomes a function of maceral
percentage of a coal particle. In the present paper, an attempt has been made by perform size-wise
flotation tests using Sub-bituminous coal and flotation kinetics have been established based on maceral
percentage reporting at different time intervals of flotation. Petrography and FTIR analysis of each size
ranges, floating at different time intervals have been conducted to determine the compositional value and
functional group of each macerals. These results have been related to the kinetic behaviour of the process.
1. Introduction
Coal macerals can be defined as the microscopically recognizable organic constituents having no definite
crystal structure and chemical composition. These macerals are generally classified into three major
maceral groups and each group represents the macerals having similar properties in a coal of specific rank
[1]
. Several beneficiation techniques were adopted for the concentration of macerals such as froth flotation
[2-3]
, magnetic separation [4] and electrostatic separation [5] etc., except froth flotation technique, none of
the other techniques gained any acceptance due to techno-economic factors. Some success was also
achieved by taking account the gravimetric difference of macerals by using centrifugation technique [6].
Froth flotation is the physicochemical process which consists of three phases such as solid, water and air
phases. It consists of two different zones such as pulp zone and froth zone. In pulp zone, mineral particles
are attached to the bubbles and transform to the froth zone. Froth recovery plays an important role in froth
phase because it determines the recovery of valuable minerals. Froth recovery is mainly affected by
bubble coalescence and water drainage. Froth zone is a very complex zone and affected by multiple
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Coal & Lignite
factors such as solid concentration, particle shape, size and hydrophobicity. Froth flotation is the process
[7]
for fine coal beneficiation, since it depends upon the surface properties of coal . Arnold and Aplan
measured contact angles of several coal samples to quantify the hydrophobicity of individual coal
macerals. It was found that the order of hydrophobicity of the coal macerals was
0
liptinite>vitrinite>inertinite and that these macerals have typical ranges of contact angles of 90-130 , 60-
700and 25-400 respectively [8]. Zhao et al. examined the floatability of coal macerals of Shenfu coals and
tried to change it by microwave irradiation. They found an increase in the difference in surface wettability
of Shenfu fusain and Shenfu vitrain and subsequently increase in the enrichment of inertinite and vitrinite
[9]
. R. Q. Honaker, separated the macerals by using column flotation technique. In this study, they take the
coal sample having size -50mm collected from Illinois no-6 seam having ash, sulphur, mineral matter,
vitrinite, liptinite, inertinite, of 8.3%, 1.1%, 9.50%, 79.10%, 3.90%, and 7.50% respectively. The
laboratory column flotation was used for beneficiation. Sink-float technique and centrifugation technique
was carried out of the flotation feed, concentrates and tailing samples and the flotation rate kinetics (k) for
[10]
the three measured groups were calculated . HGI is most directly related to the coal maceral
composition but it also depends on the rank of the coal. Several researchers have been studied relationship
between ground ability and coal Petrology. They found that, as liptinite concentrates of coal increase, the
HGI value decreased and it shows the direct relationship with the vitrinite percent. Hower and Wild
developed a strong correlation between an increase in liptinite content and decrease in HGI for coals of
narrow vitrinite reflectance ranges [11].
In this paper, an attempt has been made by performing size-wise flotation test using sub-bituminous coal
and flotation kinetics have been established based on maceral percentage reporting at different time
intervals of flotation. Therefore, the flotation rate constant eventually is a function of maceral percentage
of coal particles. The coal samples are taken from Jharkhand colliery nearest to Ranchi with the objective
of determining possibilities of the separation of maceral groups in different size fractions of -35+100#, -
100+200#, -200+400#, -400+550# and -550# and flotation rate constant is studied with size-fraction.
2. Experimental
2.1.Sample preparation, sieving and size-wise maceral analysis
The coal sample was taken from Jharkhand colliery and -35# size fraction was separated and
used for further studies. The -35# fraction of coal samples are wet screened at -35+100#, -100+200#, -
200+400#, -400+550# and -550#. It can be seen that most of the coal fractions are distributed among the
coarser size fraction (-35+100#, -100+200#) [table 1]. The sample retained on each fraction was subjected
to ash analysis according to ASTM D3174-73 standard method [12]. Subsequently 15 sub samples were
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Coal & Lignite
prepared and used for the preparation of the polished section as per ICCP standard method. The maceral
group analysis i.e. the assay of vitrinite, inertinite and liptinite was performed using microscopic studies,
[13]
according to the ISO 7404-3 standard method . Macerals are counted on the organic basis only i.e.
liptinite + vitrinite + inertinite=100% by considering mineral matter free basis.
2.2.Flotation studies
2.4.Petrographic studies
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Coal & Lignite
The microscope used for this study having resolution of 625x, Leitz wetzlar Germany of model number
12.12.78/Tei. Point counter of model no- E1-112DG is used for counting the macerals. The immersion oil
used on the surface of the block having refractive index, density, viscosity in poise are 1.515,1.305-
1.315,1500 respectively. Regulated DC power supply to microscope of model number SVL012010 was of
set voltage 9.0V and set current 7.0A.
Size-wise distribution of coal fines and the corresponding ash content is shown in fig.2. It is clear from
the figure that the distribution of coal is more in first two size fraction. Vitrinite group maceral is
dominant in feed coal sample followed by liptinite group maceral. Within the vitrinite group, collotelenite
is the predominantly noticeable maceral. Vitrinite is noticed more in first size fraction. As size decreases,
the mineral matter percent and the pyrite percent increases. The presence of trimacerite (vitrinite +
liptinite + inertinite) particles was very common in medium size fraction. As the size of the sample
decreases, the vitrinite percent increases and the liptinite content decreases, this is shown below in table 3.
and fig.3.
Table 1: Size and size-wise ash distribution of feed coal sample.
cum wt.% cum wt.%
size(#) Top size Wt. (g) Wt.% ash % retained passing
-35+100# 150 1026 55.76 42.14 55.76 44.24
-100+200# 75 285 15.49 41.14 71.25 28.75
-200+400# 40 165 8.97 38.85 80.22 19.78
-400+550# 25 84 4.57 41.02 84.78 15.22
-550# 0 280 15.22 44.81 100.00 0.00
100.00 50.00
Cumulative wt% passing
80.00 45.00
Cumulative ash%
40.00
60.00
35.00
40.00
30.00
20.00 25.00
0.00 20.00
0 20 40 60 80 100 120 140 160
size (micron)
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Coal & Lignite
Table 2: Proximate and Petrographic analysis of feed coal fines.
90
80
70
60
volume%
50
40
30
20
10
0
0 20 40 60 80 100 120 140 160
size(micron)
Maceral distribution at different time-wise froth concentrate was computed with conventional point
counter procedure and the same has been represented in terms of volume percentage in fig.4 and fig.5. It
can be observed from the figures that about 80% of vitrinite group maceral is floated in first 10 seconds.
Collotelenite is the dominating maceral in vitrinite group. On proceeding to higher time fraction,
percentage of vitrinite group maceral decreases while inertinite group maceral increases and only
deviation is seen at 60 seconds. Image microphotographs observed at different time duration of froth are
shown in fig.9. Table 4 and table 5 show that as time of froth collection increases the mineral matter
percent and pyrite percent increases. Complete liberation of inertinite group maceral i.e. semi-fusinite and
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Coal & Lignite
fusinite is shown in below figure. Liptinite group maceral i.e. sporinite along with small and wide band of
cutinite has been found at different time duration of froth fraction as shown in figure below. Micrinite and
macrinite maceral of inertinite group found widely at different froth fraction.
Table 4: The variation of petrographic components with respect to time for size -35+100#.
TIME V L I MM PY CUM ASH % ASH%
0 0 0 0 0 0 0.00 0.00
5 78.53 12.57 8.9 2.05 0 32.77 32.77
15 77.17 7.31 15.07 4.78 0.43 33.59 34.80
30 68.75 13.89 15.97 7.09 1.29 33.72 34.12
60 78.79 8.08 12.12 8.34 1.92 35.70 42.61
90 62.16 20.27 17.57 18.08 3.19 36.44 50.11
tailings 47.81 5.31 8.49 25.53 12.76 42.01 64.52
Table 5: The variation of petrographic components with respect to time for size -200+400#.
CUM
TIME V L I MM PY ASH% ASH%
0 0 0 0 0 0 0 0.00
5 77.25 2.15 18.9 7.9 1.5 34.02 34.02
15 68.06 0.43 32.19 9.62 2.96 32.88 33.52
30 60.01 4 32.01 0 4 43.19 34.81
60 78.17 7.27 10.89 3.63 0 49.67 35.70
90 60 15 20 20 4 41.61 35.81
tailings 52.31 8.45 8.43 4.22 0 57.95 41.72
50
vitrinite
40
liptinite
30
20 inertinite
10
0
0 20 40 60 80 100
time (second)
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Coal & Lignite
50
vitrinite
40
liptinite
30
20 inertinite
10
0
0 20 40 60 80 100
time (second)
Fig.6 is a plot of the cumulative component recovery versus flotation time for the -35+100# size fraction.
The figure shows that for this size fraction, the liberated vitrinite component has the highest flotation rate
and ultimate recovery. This is followed by inertinite rich component, which has lesser rates of flotation
and ultimate recovery than vitrinite. The component having lowest rate of flotation and ultimate recovery
is the liptinite [15].
80
60
40
20
0
0 20 40 60 80 100
Flotation time (second)
Figure 6: Flotation kinetics of different macerals floated at different time of -35+100# coal size fraction.
Fig.7 shows the cumulative component recovery as a function of flotation time for the intermediate size
fraction of -200+400#. In this size fraction, the rate of recovery and ultimate recovery of inertinite are
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Coal & Lignite
higher than those of the vitrinite component. Unlike the coarse size fraction, they are only slightly higher
than those of inertinite and vitrinite component.
The rate of recovery and ultimate recovery of the liptinite component are significantly lower than vitrinite
and inertinite rich component. For this intermediate size fraction, significantly higher amount of vitrinite
is recovered than the coarse -35+100# size.
100
Cumulative count %
80
60
40
20
0
0 20 40 60 80 100
time(second)
Figure 7: Flotation kinetics of different macerals floated at different time of -200+400# coal size fraction
The flotation rate constant and the ultimate recoveries for the different macerals of the two size fraction
were extracted from the kinetic data by fitting the experimental data to the first order flotation model, and
are presented Table 6.
Table 6: flotation rate constant and the ultimate recoveries for the different macerals
Size fraction Maceral Flotation rate Ultimate
constant(k) recovery(R)
-35+100# Vitrinite 0.046 95.6
Inertinite 0.043 95.0
Liptinite 0.042 92.3
Total 0.046 85.0
-200+400# Vitrinite 0.068 90.0
Inertinite 0.083 98.0
Liptinite 0.026 75.0
Total 0.090 81.0
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Coal & Lignite
vitrinite inertinite liptinite
0.09
Figure 8: Flotation rate constant versus particle size for coal maceral.
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Coal & Lignite
(A) (B)
(C) (D)
(E) (F)
(G) (H)
(I) (J)
A- Collotelenite
B- Tellinite
C- Macrinite
D- Mineral matter
E- Pyrite
F- Strip of micrinite in tellinite
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Coal & Lignite
G- Micrinite +Tellinite
H- Fusinite
I- Strip of Resinite
J- Semifusinite+Tellinite
Figure 9: Image micrographs of macerals observed at various time of collection of froth fraction.
4. Conclusions
The results of the petrographic analysis of the two different size fractions show that the vitrinite
component increased and the liptinite component decreased as the particle size decreased. Out of the two
size-fractions, in coarser size fraction vitrinite is recovered at highest rate and the ultimate recovery value
is more than the other macerals. For intermediate size fraction the floatability rate of inertinite and
ultimate recovery is more than other maceral. This study can relate the rate of floatability of macerals
with the particle size. Froth flotation is the suitable technique to enhance the vitrinite percent of the coal
particle.
References
Yerriswamy, P., Modi, O. P., Rao, K. K., & Rao, T. C. (2000). Characterization of Macerals in Coal
Fines using Image Analysis Technique.
Sarkar, G. G., Ghose, S., Chaudhuri, S. G., Sakha, S., & Daschowdhury, K. P. (1984). Selectivity of coal
macerals during flotation and oil agglomeration: a case study. Coal Perparation, 1(1), 39-52.
Jorjani, E., Esmaeili, S., & Khorami, M. T. (2013). The effect of particle size on coal maceral group’s
separation using flotation. Fuel, 114, 10-15.
Adjaye, J. D., & Bakhshi, N. N. (1995). Production of hydrocarbons by catalytic upgrading of a fast
pyrolysis bio-oil. Part I: Conversion over various catalysts. Fuel Processing Technology, 45(3), 161-183.
Tempelmeyer, K. E., Crelling, J., Hippo, E., Paul, B., & Yen, M. (1991). Coal refining by maceral
liberation and separation. In ANNUAL INTERNATIONAL PITTSBURGH COAL CONFERENCE (pp.
329-336). UNIVERSITY OF PITTSBURGH SCHOOL OF ENGINEERING CENTRE FOR ENERGY.
Crelling, J. C. (1989). Separation and characterization of coal macerals: accomplishments and future
possibilities. Prepr. Pap., Am. Chem. Soc., Div. Fuel Chem.;(United States), 34(CONF-8904170-).
Liang, L., Li, Z., Peng, Y., Tan, J., & Xie, G. (2015). Influence of coal particles on froth stability and
flotation performance. Minerals Engineering, 81, 96-102.
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Coal & Lignite
Arnold, B. J., & Aplan, F. F. (1989). The hydrophobicity of coal macerals. Fuel,68(5), 651-658.
Shu, X., Wang, Z., & Xu, J. (2002). Separation and preparation of macerals in Shenfu coals by
flotation. Fuel, 81(4), 495-501.
Honaker, R. Q., Mohanty, M. K., & Crelling, J. C. (1996). Coal maceral separation using column
flotation. Minerals Engineering, 9(4), 449-464.
Trimble, A. S., & Hower, J. C. (2003). Studies of the relationship between coal petrology and grinding
properties. International Journal of Coal Geology, 54(3), 253-260.
Aylmer, D. M., & Rowe, M. W. (1984). A new method for the simultaneous determination of pyrite
content and proximate analysis in coal. Thermochimica acta, 78(1), 81-92.
Ting, F. T. (1978). Petrographic techniques in coal analysis. In Analytical methods for coal and coal
products (Vol. 1, pp. 3-26). Academic Press New York, NY.
Taylor, G. H. (1998). Organic petrology: A new handbook incorporating some revised parts of Stach's
textbook of coal petrology. Gebruder Borntraeger Verlagsbuchhandlung.
Ofori, P., O’Brien, G., Hapugoda, P., & Firth, B. (2014). Distributed flotation kinetics models–A new
implementation approach for coal flotation. Minerals Engineering, 66, 77-83.
109
Coal & Lignite
CHARACTERIZATION OF COAL FINES AND ITS INFLUENCE ON DEWATERING OF
TAILING SLURRY
Shravan Kumar*, S. Bhattacharya, N. R. Mandre
Department of Fuel and Mineral Engineering, Indian School of Mines Dhanbad, India,
*Corresponding author: shravankumar.ism@gmail.com
Abstract
Processing of coal fines, subsequent dewatering and disposal of dilute tailing slurry, poses major
technological and environmental challenges to coal processing industries world-wide. A typical coal
preparation plant produces approximately 20% of the mined coal of size less than about 500 µm. This fine
size fraction is often discarded in the form of dilute slurry due to high processing and dewatering cost.
The parameters that affect the flocculation and dewatering of coal fines are such as physico-chemical
properties, mineral matter content, particle size distribution, particles shapes, specific gravity and their
interaction with the medium. These components also influence the plant circuit water balance which
increases the required water make up to the plant. In the present study, coal fines tailing samples were
collected from different coal washeries and investigations were made to find out the effect of their
characterization on the flocculation and dewatering. For this purpose a high molecular weight anionic
polymer (polyacrylamide) as a flocculant was used in the experiments. From the studies, it was observed
that the parameters such as ash content, particle size distribution, presence of mineral matter, zeta
potential significantly affects the dewatering performance. A maximum settling rate of about 180
mm/min was obtained for coal tailings containing 62% ash. The studies also showed that the sample
containing more amount of fines (-63 µm) respond poor to flocculation and hence resulting lower settling
rate. The zeta potential (ZP) studies carried out also indicated that at higher negative ZP values, the
settling rates were found to be lower. During the studies, effects of various interaction of parameters were
also investigated.
1. Introduction
Proved coal reserves of India are estimated to be around 126 Bt. On the domestic production front, Coal
India Ltd. is the largest contributor accounting for 81% of country's coal production. Of the balance, 9 %
is contributed by the Singareni Collieries Company Ltd. (jointly owned by the central government and the
state government of Andhra Pradesh), and the rest by the privately operated collieries and the captive coal
mines. Small mines in the north-eastern state of Meghalaya also add about 6 Mt to the total production
(India Energy Book, 2012).
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Coal & Lignite
The advancement in the mining methods from low capacity conventional to high capacity mechanized
mining has resulted in the generation of large quantities of fines. The amount of fines in coal increases
through the entire flow chain, mining, size reduction, handling, storage, etc. The processing of fine size
fractions and subsequent dewatering and disposal of dilute effluent slurry, pose a major technological and
environmental challenge to mining, mineral and coal processing industries world-wide (Sabah and Erkan,
2006). A typical coal preparation plant (CPP) produces about 20 percent of the mined coal as less than
500 µm size (Parekh, 2009, Kumar et al, 2014), this fine fraction is often discarded in the form of dilute
slurry.
From fundamental point of view, dewatering process is known to depend largely on physico-chemical
properties of the particle surface, mineral matter and size distribution of the solid material (Rong and
Hitchins, 1995). This is also attributed to the presence of coal particles of different shapes and specific
gravities known as relative density (RD) and their unique behaviour in the aqueous environment. Further,
industrial waste slurries containing colloidal particulate matter, with particular reference to coal and
mineral processing plant tailings with a high proportion of clayey materials pose significant challenge in
dewatering (Philip et al, 2011). Also, when a solid particle is in suspension, various forces act on them
and particles also interact among themselves. Gravitational forces are less effective when the particle
sizes are very fine in size. The van der Walls force of attraction and interactional forces due to the
presence of charge on the particles become dominating forces, at very fine sizes, responsible for settling
of particles.
Flocculation and flocculants are generally discussed in the context of the specific requirement of
dewatering systems such as sedimentation. Chemical conditions, reagent selection and process operating
conditions are evaluated based on the fundamental mechanisms involved in particle destabilization and
floc development. The effectiveness of flocculation process depends not only on the use of appropriate
chemical reagents (coagulants, flocculants, dispersants, etc.) and their method of addition, but also on the
composition of the fines. Accurate determination of physical, chemical and electro-kinetic properties of
solid matters in pulp, using flocculants, plays a key role for the success of settling of fine-particles in
suspensions.
The aim of the study was to characterize the coal samples collected from different coal preparation plant
and to analyse the effect of characterization on the flocculation of coal fines.
In the present investigation, coal sample from three coal preparation plant tailings were used. These
samples were collected from the three coal preparation plants located at Jharia coalfield of India. The
111
Coal & Lignite
characterization studies carried out mainly include size analysis, determination of ash, moisture, volatile
matter, fixed carbon, XRD, zeta potential etc.
A high molecular weight polyacrylamide-based anionic polymer was used in the flocculation studies.
Prior to the flocculation tests, a homogeneous stock solution (0.25% w/w) of polymer was prepared using
distilled water. The stock solution was further diluted to 0.02% (w/w) concentration for the flocculation
tests. This freshly prepared flocculants solutions were used in the flocculation studies.
The sieve analysis of a representative samples was carried out using 600 to 53 μm sieve sizes. The
comparative results of the same are given in Table 1.
It may be observed that the Jamadoba tailings contain smallest 80% passing size as 380 µm, whereas the
Bhelatand tailings contain largest size of 460 µm as 80% passing size. However, highest amount of
ultrafines (-63 µm) were observed in Jamadoba tailings followed by Bhelatand and Chasnala tailings.
From the zeta potential studies, it was observed that the absolute value of charge increases with increasing
pH and found to decrease beyond certain pH. The highest value of zeta potential were observed as -42.72
mV for Jamadoba tailings at pH of 9, followed by –29.45 mV at pH 8 for Bhelatand tailings and -29.06
mV at pH of 7 for Chasnala tailing.
The XRD analysis of the three samples showed the presence of kaolinite and quartz. Jamadoba sample
also contained dolomite and muscovite. However, muscovite was found to be absent in Bhelatand and
Chasnala tailing.
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Coal & Lignite
3.2 Flocculation studies
Experimental work was carried out to compare the settling rate, turbidity of supernatant liquid and density
of settled slurry obtained for three tailing samples at 8% feed pulp density. The flocculants dosage was
varied from 6.5 gpt (gm flocculant per ton of solid) to 26 gpt.
150
100
Jamadoba
Bhelatand
50 Chasnala
0
6.5 9.75 13 16.25 19.5 22.75 26
Flocculant dosage, gpt
From the studies, the settling rates of Chasnala tailings were found to be higher than Bhelatand and
Jamadoba tailings (Fig. 1). Such findings may be attributed to the presence of lower percentage of
particles less than 63 µm in size in Chasnala tailings as indicated in Table 1.
40
35 Comparative turbidity
30 (Pulp density: 8% solid, w/w, pH: 8)
Turbidity, NTU
Jamadoba
25 Bhelatand
20 Chasnala
15
10
5
0
6.5 9.75 13 16.25 19.5 22.75 26
Flocculant dosage, gpt
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Coal & Lignite
50
Comparative density of settled slurry
45
35
solid
30 Jamadoba
Bhelatand
25
Chasnala
20
6.5 9.75 13 16.25 19.5 22.75 26
Flocculant dosage, gpt
The turbidity of the supernatant liquid were also measured using a turbidity meter. From the studies,
similar range of turbidity values (Fig. 2) were obtained for Jamadoba and Chasnala tailings, though for
Bhelatand tailings, a higher value of turbidity was recorded within the same range of parameters. The
density of the settled slurry has been shown in Fig. 3. It may be seen that there exists a little difference in
the densities of settled slurry for Bhelatand and Chasnala tailings. However, beyond 19.5 gpt of flocculant
dosage, the densities of the three samples were found to be nearly identical.
From the comparative studies of three samples, the settling rates of Chasnala tailings were found to be
higher than Bhelatand and Jamadoba tailings. This may be attributed to the presence of lower percentage
of particles less than 63 µm in size which is in accordance with the published literature (Rong et al, 1995,
Sabah et al 2004, Das et al 2006), indicating that the presence of particles less than 63 µm in size
significantly affects the settling rate as these possess lower settling characteristics.
From the studies, it may be observed that the Jamadoba tailings show lowest settling rate as compared to
Bhelatand and Chasnala tailings. This may be correlated with the X-ray diffraction studies carried out as
the Jamadoba tailings contain muscovite along with kaolinite, dolomite and carbonate minerals. The flaky
nature of muscovite minerals, in Jamadoba tailings, results in the lower settling rate as compared with the
Bhelatand and Chasnala tailings which do not contain muscovite.
4. Conclusions
Using anionic flocculants, the average settling rates of the tailing samples under investigation can
be increased to about 180 mm/min as compared to about 6 mm/min obtained without flocculants.
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Coal & Lignite
The average density of settled slurry could be improved to about 42% solid, w/w from initial feed
pulp densities of 8% solid (w/w).
The average turbidity of supernatant liquid could be reduced to about 6-8 NTU.
References
Das, B., Prakash, S., Biswal, S. K., Reddy, P. S. R., 2006. Settling characteristics of coal washery
tailings using synthetic polyelectrolytes with fine magnetite. The Journal of the Southern African
Institute of Mining and Metallurgy. 106 707-712.
Parekh, B. K., 2009. Dewatering of fine coal and refuse slurries problems and possibilities. Procedia
Earth and Planetary Science 1. 621-626.
Philip, O., Nguyen, N. V., Bruce, F., McNally, C., Orhan, O., 2011. Shear-induced floc structure
changes for enhanced dewatering of coal preparation plant tailings. Chemical Engineering
Journal. 172 914– 923.
Rong, R. X., Hitchins, J., 1995. Preliminary Study of Correlations between Fine Coal Characteristics
and Properties and their Dewatering behavior. Minerals Engineering. Vol-8, No.-3 293-309.
Sabah, E., Cengiz, I., 2004. An evaluation procedure for flocculation of coal preparation plant
tailings. Water Research. 38 1542–1549.
Sabah, E., Erkan, Z. E., 2006. Interaction mechanism of flocculants with coal waste slurry. Fuel. 85
350–359.
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STUDY ON PROCESS CONSUMABLES AND IDENTIFICATION OF SOURCES OF MEDIA
LOSSES AT WEST BOKARO
Kunal Mathanker*, Bijay Shankar Tiwari and D. P. Chakraborty
Process Technology Group, WGO, TATA Steel ltd., Jamshedpur-831005
*Corresponding author: kunal.mathanker@tatasteel.com
Abstract
Coal washeries consist of two main circuits for beneficiation of raw coal depending on coal size
distribution, namely Dense Media circuit and Fines (flotation) circuit. Magnetite in dense medium
operation and collectors and frothers in froth flotation process are the main process consumables. Process
consumables are the significant components of operational cost in any coal washery. They play very
crucial role in the process & directly affects the plant performance and economics. In this paper, study has
been conducted related to identification of different sources of Magnetite losses in a coal washery and
measures have been identified for their reduction. Magnetite is the major component of operational cost
(~ 13-15 %) in a coal washery. Loss of magnetite mainly occurs from two routes i.e. adhesion to products
and through effluents generated by medium regeneration processes. This work is carried out at Washery #
3 of West Bokaro, TATA Steel. Paper mainly focuses on quantification of losses through coarse coal
products (coarse clean coal, middling’s & rejects).It was observed that coarse coal products account
around 50% of the total magnetite losses due to adhesion. Among these products, losses through rejects
are highest while losses through coarse clean coal are lowest. Raw Magnetite quality (magnetic content &
size distribution) is also considered as it affects the dense medium separation process and regulates loss of
media. It is observed that weight % of +325 mesh size in raw Magnetite affects the dense media cyclone
performance. Apart from adhesion losses, observations related to other sources of losses like spillage,
leakages are also included in this study. This study showed that if specific magnetite consumption is
reduced by 0.1 kg/ton (raw coal basis) than total cost of magnetite will be reduced by ~15%.
Keywords: Process consumables, dense media (DM) cyclone, magnetite loss, media, coal washery
1. Introduction
In any coal beneficiation plant, beneficiation scheme is designed on the basis of feed size distribution of
input material. In India, generally two circuits are employed i.e. Coarse Circuit (above 0.5mm) & Fine
Circuit (below 0.5mm). Both coarse as well as fine circuit consume some type of process consumables for
improvement in separation. Magnetite is the major consumable in Dense Media operation while
Collectors and frothers are consumables in flotation process. Magnetite has some superior characteristics
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which made it very much suitable and acceptable worldwide as dense medium material. Magnetite being
costly, plays a very crucial role in determining plant economics. Some literatures suggest that around 10-
20% cost of operation is incurred due to magnetite loss. Hence, there are benefits in reducing these losses.
Studies related to identification of sources of loss is important to address this issue. There are mainly two
routes of losses:
1. Adhesion of media to different products (concentrate, middling, reject)
2. Loss in effluents from media recovery processes (magnetic separators, settling cones, thickening
cyclone)
This paper aims at to identify various sources of magnetite losses at Washery#3 of West Bokaro. Media
quality (magnetic content & size distribution) also affects the losses.
Loss of magnetite affects dense media circuit performance as well as cost of production. Being a very
costly material its maximum recovery with minimal loss is important. Losses are tracked as specific
magnetite consumption (kg/ton). Specific magnetite consumption is expressed as quantity of magnetite in
kilogram consumed for washing one ton of coal (raw coal feed to DM cyclone/feed to washery).
Probable causes of loss
Forces of attraction between ore and medium particles
Magnetic separation and classification inefficiencies
Corrosion and abrasion of the medium
Excessive circuit loadings during addition of fresh medium
Medium properties (size, shape, magnetic susceptibility)
Screen drainage efficiency (Drainage characteristics, depends upon loading)
Magnetite recovery circuit
Magnetite is easily recoverable due to its magnetic properties. Recovery circuit comprises mainly
magnetic separators (the type of separators can vary). Commonly wet drum separators with permanent
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magnets are employed. In all dense medium plants medium adhering to products is rinsed away with the
water. The diluted medium thus formed is directed to recovery system either by gravity flow or pumping.
This study had been conducted in Washery#3 of West Bokaro Division, TATA Steel. Washery#3
operates in two bays (Bay1 & Bay2). Each bay consists two streams (Stream 1&2 for Bay1, Stream 3&4
for Bay2). Each stream beneficiates coarse coal (-13+0.5 mm) in two successive stages of DM cyclone. In
first stage rejects are separated out at higher cut density whereas in 2nd stage clean coal and middling’s are
separated at lower cut density. Seven months plant data is analysed for this project. Sample collection and
lab analysis was done by NRD (National Resource Division) department of west Bokaro, TATA Steel.
Some part of data was captured from plant information system.
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It is observed from Fig.4 that losses through products (clean coal, middling & rejects) contribute
approximately half of the total loss in which losses through rejects are 18.66%. Media loss through rejects
due to adhesion is highest, as in Washery#3, rejects are separated at higher cut density and report to
underflow of DM cyclone. Media underflow density is higher than overflow because media itself get
separated in DM cyclone based on density difference.
Quality check is done for raw magnetite and magnetite which get processed in DM cyclone.
+325 mesh size in raw magnetite varies in between 6-18% by wt. Magnetic content is 100% for each
point.
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Quality analysis is being carried for both primary and secondary circuit media. Mixing of non-magnetic
materials in media during processing is analysed.
Mixing of non-magnetics in primary circuit media is upto ~14% (Fig.6) while mixing in secondary circuit
is upto ~18% (Fig.7). Mixing of non-magnetic material in secondary circuit media is higher due to mixing
of ultrafine coal particles during DMC process.
A graph is plotted between wt% of +325 mesh size in raw magnetite and DM cyclone yield (unitwise).
Figure 8: Effect of wt% of +325 mesh size in raw magnetite on dense media cyclone (DMC) yield.
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Fresh magnetite in the media circuit is added manually. Spillage occurs during media addition and during
handling of media bags. Some quantity of magnetite got left in bags if not properly inspected. Pipe joints
and old pipes are prone to leakages that also contribute in media spillage.
Cost analysis study for Washery#3 showed that if specific magnetite consumption is reduced by 0.1
kg/ton ( raw coal basis) from the current level, so it could save ~15% cost of magnetite.
4. Conclusions
Adhesion losses through coarse products (coarse clean coal, rejects & middling’s) contribute 51.05 %.
Losses through rejects are highest (18.66%) while losses through coarse clean coal are lowest (14.52%).
Since rejects are separated out at higher cut density hence, more concentrated media adhere to reject
materials. Adhesion loss can be minimized by studying media recovery screen washing configuration
(angle, spraying arrangement) and drainage efficiency. Mixing of non-magnetic material is higher in case
of secondary circuit media as compared to primary circuit media. It shows that ultrafine coal particles get
mixed in secondary circuit media which are not effectively separated out during media recovery through
magnetic separators. Inverse liner relationship is found between wt % of +325 mesh size in raw magnetite
& DM cyclone yield (unit-wise). It suggests that +325 mesh size particles in magnetite suspension
disturbs the homogeneity of solution and produces unclear cut density. This variation in cut density
hampers the DM cyclone performance. Hence, weight % of +325 mesh size should be minimum in raw
magnetite.
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Other losses are also significant though their quantification is difficult. Media spillage, leakages from
joints also contribute in loss of magnetite. Hence, fresh media should be handled carefully. Frequent
checks should be performed to look for leakages and accordingly corrective actions should be taken.
Acknowledgements
We are thankful to Mr. Ashok Kumar (CTO, Process) for his support and encouragement, Mr. P.K. Dhall
(Chief, Coal Beneficiation), Mr. Kajal Hota (Head, Washery-III), Mr. Bharat Garg (Senior Manager,
Washery-III ), Mr. K. Goswami (Manager, Chemical ) & other staff of NRD (West Bokaro) and all those
who are directly or indirectly involved in the trial for their support in carrying out the trial, sample
collection and preparation.
References
G. J. de Korte & J. Engelbrecht, Dense Medium Cyclones, International Journal of Coal Preparation and
Utilization, 34:1, 49-58, 2014.
J. Franko & M. S. Klima, Wet-Drum Magnetic Separation of Dense-Medium Slurries Containing Fine
Coal Refuse, Coal Preparation, 25:3, 155-171, 2005.
T.J. Napier-Munn, T. Kojovic, I.A. Scott, F. Shi, J.H. Masinja and P.J. Baguley, Some Causes of Medium
Loss in Dense Medium Plants, Minerals Engineering, Vol. 8, No. 6, pp. 659-678, 1995.
D. G. Osborne, Coal Preparation Technology Volume: 1, Graham & Trotman Limited, London, 1988.
R. Sripriya, A. Dutta, P.K. Dhall, M. Narasimha, Vikas Kumar, B.S. Tiwari, An analysis of medium
losses in coal washing plants, Int. J. Miner. Process. 80, 177–188, 2006.
R. Sripriya, P.V.T. Rao, J.P. Bapat, N.P. Singh, Partho Das, Development of an alternative to magnetite
for use as heavy media in coal washeries, Int. J. Miner. Process. 71, 55– 71, 2003.
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STUDIES ON CAKING BEHAVIOR OF WET BULK SOLIDS DUE TO STORAGE AND
CONSOLIDATION STRESS
TVS Subrahmanyam*, Somiran Mondal and Rajan Kumar
R&D Centre, NMDC Limited, Hyderabad, INDIA
*
Corresponding author: tvssubrahmanyam@nmdc.co.in
Abstract
Storage and handling is an integral part of any bulk material handling plant. Sometimes it is inevitable to
store the bulk solid in silos or bunkers for longer duration under a state of consolidation owing to break
down in downstream equipments or inherent demand of process cycle. The tendency of some bulk solids
attaining higher unconfined yield strength due to storage (caking) is often experienced and leads to
cohesive arch formation at the outlet of silo resulting in no-flow of material. This will eventually lead to
loss of productivity. It is important to consider the effect of this storage while designing silos, bins and
hoppers which is often ignored. The mechanisms that induce caking are generally, liquid bridge
formation, cohesion, crystallization, sintering, adsorption and/or deformation. The caking is usually
influenced by storage time, moisture, temperature and consolidation stress that acts on bulk solid during
storage. The present study is aimed at understanding influence of caking on silo design parameters
especially the critical outlet dimension to prevent Arching (a no-flow condition). The experimental
investigations were done on three coal samples of varying ash contents at different moisture contents.
Samples were stored for 24 hours and 72 hours for the experimentation. The shear test data generated for
each coal sample for different moistures had been processed to establish the minimum outlet sizes
required to avoid arching in Mass Flow silos. An attempt was made to correlate the minimum outlet
dimension to avoid arching in silos with the storage time.
Key words: Caking, bulk solids, storage time, moisture, ring shear tester, coal, silo
1. Introduction
Storage and handling is an integral part of any bulk material handling plant. Bulk solids are stored in
silos, bunkers, hoppers and stock piles for longer duration under a state of consolidation due to some
break down in downstream equipments or inherent demand of process cycle. The tendency of some bulk
solids to attain higher cohesive strength due to storage is often experienced while handling bulk solids. If
the bulk solids consolidate, then external machinery, manpower and time are needed to dislodge the solids
in addition to costly downtime. If the bulk solid is stored and handled in a silo, caking tendency leads to
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cohesive arch formation at the outlet of silo resulting in no-flow of material. This will eventually lead to
production loss. It is important to consider the effect of this storage while designing silos, bins and
hoppers which is often ignored.
Three coal samples viz. one Indonesian and two Indian coal samples were selected for the study. Samples
of -4mm was generated for each selected coal variety and used for shear testing to determine its flow
properties. Initially the moisture content and saturation moisture of each sample was determined. The
shear tests were performed at saturation moisture of 55%, 65%, 75% and 85% for the Indian coal samples
by physically altering the moistures while the Indonesian coal was tested at 70%, 75%, 80% and 85%
saturation moistures. The storage time tests were conducted at worst case moisture levels for each coal
sample for storage up to 24 hours and 72 hours to establish the effect of undisturbed coal storage.
3. Experimental procedure
3.1. Moisture content
The moisture content of the samples has been established by keeping a known weight of the sample of -
4mm in electric oven, maintained at 107 +/- 30C until dry. The loss in weight of each sample divided by
its original weight before drying is denoted as moisture content in the sample. The saturation moisture of
each sample is established by taking a known quantity of coal sample on 38 micron aperture screen cloth.
The sample is completely soaked in water for 30 minutes and then allowed to drain until constant
moisture is attained. This process is carried out in a closed container maintained at controlled temperature
and humidity. The moisture content of the resultant sample is considered as saturation moisture [100%].
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The size analysis of the coal samples is determined by using standard tests sieves and presented in Table
2.
Table 2: Size analysis of coal sample.
Nominal Cumulative weight percent passing
screen
Mesh #
aperture (Low ash (Medium ash (High ash
size (mm) Indonesian coal) Indian Coal) Indian Coal )
5# 4 100.0 100.0 100.0
8# 2.36 68.3 67.7 74.4
10 # 1.70 56.5 55.7 62.1
18 # 1.00 35.7 31.9 35.1
20 # 0.850 30.1 27.0 28.9
28 # 0.600 23.3 20.2 22.1
35 # 0.425 17.6 14.9 16.1
48 # 0.300 13.3 11.0 11.6
65 # 0.212 9.9 7.9 8.8
100 # 0.150 5.4 4.4 4.7
150 # 0.106 5.0 4.1 4.4
200 # 0.075 3.8 3.4 3.6
250 # 0.063 2.7 2.7 2.7
325 # 0.045 0.9 1.9 2.0
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4.4 Shear Test Data
The data generated through shear testing is analyzed by plotting yield loci and constructing Mohr stress
circles. It was observed from the shear tests data that the three coal samples (Low ash Indonesian coal,
Medium ash Indian coal & High ash Indian coal) are exhibiting highest yield strength at 41.2%, 24.7%
and 23.3% respectively which are designated as worst case moistures. The storage time tests were
performed on coal samples of these moistures. The flow functions, time flow functions and variation of
unconfined yield strength with storage time for worst case moistures are presented in Fig.3 to 8. The flow
functions are generated for 0 hours (instantaneous), 24 hours and 72 hours of storage. Based on the flow
parameters like effective angle of friction and flow functions, the minimum outlet dimension to prevent
cohesive arching(Dc) near the outlet of a silo (circular in plan) is calculated using Jenike theory. A flow
factor of 1.25 is assumed for the purpose of arriving at the arching dimensions (Dc). The variation of Dc
with moisture and storage time are plotted and presented in Fig.9 to Fig.12.
It is observed that at the worst case moisture, the Dc value is increasing from 0.55m to 1.11m due to
storage from 0 hours to 72 hours in case of low ash Indonesian coal. While it is increasing from 0.63m to
1.01m in case of medium ash Indian coal and 0.42m to 0.70m for the high ash Indian coal.
Flow function & Time flow function @ @ 10Kpa Consolidation stress, 41.2%mc
6000 41.2%mc
Unconfined yeild stress, Pa
5500
Unconfined yeild stress (Pa)
5000
5000
4000
4500
3000
Instanteneous 4000
2000 24 Hours Storage
72 Hours storage 3500 41.2%mc
1000 Flow Factor, conical=1.25 Poly. (41.2%mc)
0 3000
0 5000 10000 15000 0 20 40 60 80
Major consolidation stress, Pa Storage time at rest (hours)
Figure 3: Flow Function and Time Flow Function- Figure 4: Unconfined yield stress vs. storage time-
Low ash Indonesian coal @ 41.2% mc. Low ash Indonesian coal @41.2% mc.
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Flow function & Time flow function @ @ 10Kpa Consolidation stress , 24.7%mc
24.7%mc
12000 5000
10000 4500
8000 4000
6000 3500
4000 3000
Instanteneous
24 Hours Storage 24.7%mc
2000 72 Hours Storage 2500
Poly. (24.7%mc)
"Flow Factor, conical=1.25"
0 2000
0 10000 20000 30000 40000 0 20 40 60 80
Major consolidation stress, Pa Storage time at Rest, (Hours)
Figure 5: Flow Function and Time Flow Function Figure 6: Unconfined yield stress vs. storage time
-Medium ash Indian coal @ 24.7% mc. – Medium ash Indian coal @ 24.7% mc.
Flow function & Time flow @ 23.3%mc @ 10Kpa consolidation stress, 23.3%mc
6000
5500
Unconfined yeild stress, Pa
5000
4000
4500
4000
Figure 7: Flow Function and Time Flow Function Figure 8: Unconfined yield stress vs. storage time
-High ash Indian coal @ 23.3% mc. – High ash Indian coal @ 23.3% mc.
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Variation of Dc with Moisture - Low ash Variation of Dc with Moisture - Medium
Indonesian coal ash Indian coal
Minimum outlet dimension Dc
1.2
1.2 Instanteneous
0.8
0.4
Instanteneous 0.6
24hrs
72hrs
0 0.4
36 38 40 42 24 26 28 30 32 34
Moisture content (%) Moisture content (%)
1
0.6
0.8
y = -0.0001x2 + 0.0164x + 0.5367
0.4
0.2 Instanteneous Low ash Indonesian coal
24hrs 0.2 Medium ash Indian coal
72hrs
High ash Indian coal
0 0
20 22 24 26 28 0 20 40 60 80
Moisture content (%) Storage time at rest(Hours)
Figure 11: Variation of Dc with Moisture Figure 12: Variation of Dc with Storage time for
-High ash Indian coal. all tested coals at worst case moisture.
5. Conclusions
The following conclusions are drawn after evaluation of test data. The time storage has a definite effect
on the yield strength (caking tendency) of tested bulk solids especially at elevated moisture contents.
Moisture content is a key parameter influencing the flow properties of tested materials. The yield strength
increases (in general) with storage time at rest. This is found to be significant in the low ash coal which
has significantly higher moisture content. Minimum outlet dimension to prevent arching (Dc) is highest at
the worst case moisture for tested coal samples. The gain in strength is significant in the first 24 hours of
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storage for the tested coal samples. An attempt was made to correlate the minimum outlet dimension with
the storage time. A best fit equation with a regression coefficient (R2) of 0.62 was obtained. As the yield
strength depends on various other parameters as well, an agreeable general correlation between Dc and
storage time encompassing all kinds of coals appears questionable. This shows that the specific material
properties have to be considered for design of material handling systems. The study outlines the
significance of time storage effect on silo design parameters and emphasizes the need for due care during
plant detailed engineering to avoid operational problems.
Acknowledgements
The authors are grateful to the management of NMDC for their support in the completion of this project
work. The authors wish to acknowledge the guidance and encouragement received from Shri N. K.
Nanda, Director [Technical], NMDC Limited.
References
A. W. Jenike, Storage and flow of solids, Bulletin 123, Engineering experiment station, University of
Utah, Salt lake city, UT, 1964 .
ASTM D 6773-08: Standard Test Method for Bulk Solids using Schulze Ring Shear Tester.
Dietmar Schulze, Powders and Bulk Solids, Behavior, Characterization, Storage and Flow.
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BENEFICIATION OF OXIDIZED COKING COAL FINES THROUGH FROTH FLOTATION
Nanda Kishore Patra*1, Shalini Gautam2, Sanjay Choudhuri3 and T. Gouricharan3
1
Indian School of Mines, Dhanbad ,
2
Indian School of Mines, Dhanbad
3
CSIR-Central Institute of Mining and Fuel Research, Dhanbad
* Corresponding author: nandakishore.patra@yahoo.com
Abstract
Coal is a major resource of energy for domestic as well as for industrial purpose. It is necessary to beneficiate
the Indian coal before it is dispatched to various end users. Though conventional gravity separation processes
is preferable for coarse coal beneficiation but for beneficiation of coal fines, froth flotation still remains the
most effective method of separating gangue from the carbonaceous materials. Flotation is a physico-chemical
process of separation of hydrophobic particles from hydrophilics but practically it is influenced by many
mineralogical, chemical and operational variables. If the surface of the coal is oxidized it reduces its
hydrophobicity. Investigations were carried out to improve the flotation performances of coal washery slurry
sample, which is weathered. An attempt has been made using different operation parameters such as;
different reagents, reagent dosages, impeller speed to understand the flotation characteristics. The feed
material has been subjected to characterization with respect to size analysis, proximate analysis, ultimate
analysis, GCV, sink-float, FTIR analysis etc. The ash content of the coal sample is 27%. Extensive
laboratory flotation tests were carried out and the paper discusses the various results obtained and suggests
improving the flotation recovery of oxidized coal fines.
1. Introduction
Froth flotation is a conventional technique used in the beneficiation of fine coal. The flotation behaviour of
coal depends on many factors, such as macerals, rank, origin, quality of impurities and degree of oxidation.
The low rank or oxidized coals show unpleasant flotation behavior (Shobhana Dey et al 2013). The coal
undergoes oxidation due to weathering (Tan et al 2015; Xia et al 2014).Weathering also increases the
brittleness of oxidized coal, lowers the pulp pH and increases the free cations in the coal pulp and thus
decreases the surface hydrophobicity. Coal oxidation processes usually change both the surface properties
and structures of coal (Xia et al.2104). The oxidation processes result in the formation of oxygen functional
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groups, such as carboxyl, phenol and carbonyl functionalities on the coal surface, which reduces the
hydrophobicity of coal surface by increasing the number of sites which can form hydrogen bond with the
water molecules (Xia, Tan, Mishra et al). The oxidation of coals starts with the physical adsorption of oxygen
on the surface to form an oxycomplex, followed by chemical adsorption of oxygen to form polar phenolic-
OH, carbonyls and phenols and peroxide type oxygenated moieties (Xia, Mishra et al.). These newly formed
hydrophilic functional groups lead to poor flotation performance. Coal oxidation is particularly important in
coal flotation since it can drastically affect the wettability and decrease the floatability of the coal. (Mishra,
Somasundaran).
Several lab tests are available for determine the rate of oxidation of a coal. Contact angle, Oxidation number,
Zeta potential, FTIR, XPS and EPR have been widely used to indicate the changes in surface properties of
coals before and after oxidation processes (Xia et al. 2014). It has been suggested that evaluating the
hydrogen to oxygen ratio based on ultimate chemical analysis is a reasonable measure of coal floatability for
partially oxidised coals. If the ratio of hydrogen to oxygen is <20 than it is difficult/hard to float, it requires
more collector promoter and stronger frother behaviour. If the ratio is >20 than coal is easy to float (Mishra-
Book). A change in the surface properties of the coal particles largely affects their attachment and
detachment characteristics with other dispersed phases in flotation pulp. The addition of surfactant or
oxygenated functional groups to the collector molecule markedly enhances the flotation of lower rank or
oxidized coals due to the hydrogen bonding with the polar part of the coal surface and the reagent. The
promoters also act as surface modifiers and alter the hydrophobicity of the oxidised coal. The mode of
addition of non-ionic surfactant with oily collector has significant role in the flotation response
(Somasundaran). The low rank coal/oxidized coals can be effectively floated using blending of hydrocarbon
and non-hydrocarbon collectors, such as copolymers, long chain amine, fatty acid, etc. Pre-treatments of low
rank/oxidized coals were also studied to enhance the flotation performance by improving the hydrophobicity
(Sobhana dey et al. 2013).
In this investigation, we attempted to find out the effect of the flotation behaviour of Patherdih coal washery
dried slurry which is readily oxidized coal. A comparison study of flotation behaviour using different
collector, frother was made in order to give a useful concept of oxidized coal flotation. The objective of this
investigation is to explore the flotation performance of the weathered coal in a mechanical flotation cell at a
targeted ash level of 12% as the demand of the low ash clean coal is increasing. The recovered clean coal can
be used for various metallurgical purposes
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2. Materials and methods
2.1 Materials
Sample has collected from Patherdih coal washery slurry as a dried fine coal. It was screened in 0.5 mm.
screen. A representative sample was drawn for various characterization studies. The proximate analysis of
the coal was carried out and is presented in Table 1. Results show that this coal is medium volatile coal
having 18.45%. It has 3.6% of moisture and fixed carbon is 51.84%. However, this coal exhibits about 26-27
% of ash as a thickener underflow product. Heat values are related to ash content. It has higher heat value. It
may be due to its lower ash percentage. The gross calorific value is carried out by Bomb Calori meter and it
has found 5500 kcal/kg.
The calculated d80 of this sample was found to be near to 250 µm. It is evident that only 0.2% of coal particle
is reported to +0.5mm which ash content is 14.81%. This implies this sample can use for flotation. The
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lowest ash % value is 11.84 having size range -0.5 to +0.250 mm. Highest weight% is found 46.38% at
below 63 micron and it contains highest ash% i.e. 36.10%. Higher percentage of ash content is contributed to
ultrafine i.e. below 63µm having ash content 36.10%.
In this investigation Denver D12 sub-aeration flotation machine with 3 liter capacity cell was used for
flotation studies. Oxidized coal 250 gm was pre-wetted at a flotation cell for 3 min. After the prewetting
process, the collector was added into the flotation pulp and the pulp was conditioned for 3 min. At last,
frother was added and the pulp was conditioned for another 1min. Another 2250ml of makeup water was
added before froth collection. Then flotation was carried out by releasing the air at 2.07 m3/second for 1 min.
Froth has collected for 1 minute only. Both the froth and tailings were collected separately, dried and
analyzed for ash percentage. The impeller RPM was kept constant 1500 and the pH of the slurry was natural.
There are two types of collectors are used and single frother is used for this present study.
Flotation result was analyzed by three indexes: combustible matter recovery, Floatation Efficiency Index, ash
rejection. Equations 1, 2 and 3 were used to calculate the combustible matter recovery, ash rejection and
flotation efficiency index of the flotation experiments.
Mc(100−Ac)
(CR) Combustible matter recovery (%)=[ Mf(100−Af) ] × 100 (1)
Mc(Af−Ac)
(AR) Ash rejection (%) = 100-[Mf Af(100−Af)] × 100 (2)
Where Mc is the weight of the concentrate (%), Mf the weight of the feed (%), Ac the ash content of the
concentrate (%), and Af the ash content of the feed (%).
There are two sets of experiment was done using two different collector and single frother which is tabulated
in Table no.3. and 9 no. of test was done for each set of experiment.
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Frother ml./ton 240 320 400
Table 4: Effect of variation on collector 1 and frother, ash of feed sample is 26.5%
Clean Reject Clean Reject
Sl. Collector Frother coal yield coal coal
No. 1 kg/ton ml/ton yield % % ash% ash% CR % AR% EI%
1 2 240 38 62 10.98 45.33 46.02 84.26 30.28
2 2 320 42.9 57.1 11.01 51.51 51.94 82.18 34.12
3 2 400 44.24 55.76 11.24 52.62 53.43 81.24 34.66
4 3 240 39.7 60.3 11.33 47.17 47.89 83.03 30.92
5 3 320 43.21 56.79 11.56 51.21 51.99 81.15 33.14
6 3 400 45.21 54.79 11.98 53.32 54.14 79.56 33.70
7 4 240 49.66 50.34 12.2 58.42 59.32 77.14 36.46
8 4 320 54.55 45.45 12.36 64.06 65.04 74.56 39.60
9 4 400 58 42 12.56 67.96 69.00 72.51 41.51
Table 5: Effect of variation on Collector-2 0.72, 1.08, 1.44 kg/ton and frother 240,320,400 ml/ton, Ash of
feed sample is 26.5%
Clean Clean Reject
Mentanol Frother coal Reject coal coal
Sl. No. kg/ton ml/ton yield yield ash% ash% CR AR EI
1 0.72 40 37.25 62.75 13.17 31.49 44.00 81.49 25.49
2 0.72 80 41.13 58.87 13.42 32.25 48.45 79.17 27.62
3 0.72 120 50.20 49.80 14.01 35.71 58.73 73.46 32.19
4 1.08 40 48.39 51.61 13.31 34.27 57.07 75.70 32.77
5 1.08 80 54.00 46.00 13.44 35.94 63.60 72.61 36.21
6 1.08 120 58.00 42.00 14.23 39.21 67.68 68.86 36.54
7 1.44 40 56.85 43.15 13.93 39.28 66.58 70.11 36.69
8 1.44 80 63.45 36.55 14.12 44.99 74.14 66.19 40.33
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9 1.44 120 65.48 34.52 14.34 45.94 76.31 64.57 40.88
Table 4 shows that lowest clean coal yield has found 38% with 10% ash and highest reject yield has found
62% with 45.33% ash. Highest clean coal yield has found 58% with 12.56% ash and lowest reject yield has
found 42% with 68% ash. If the influence of frother increases from 240 ml/t to 400 ml/t with 2 kg/t of
collector 1 than combustible recovery % increases from 46 to 53.43%. Again same dosages of frother with 3
kg/t of collector 1 than combustible recovery % increases from 48 to 54%. Same dosages of frother with 4
kg/t of collector 1 than combustible recovery % increases from 59 to 69%.
Table 5 shows that lowest clean coal yield has found 37% with 13.77% ash and highest reject yield has found
63% with 31.5% ash. Highest clean coal yield has found 65% with 14.34% ash and lowest reject yield has
found 34.52% with 76% ash. If the influence of frother increases from 240 ml/t to 400 ml/t with 0.72 kg/t of
collector 2 than combustible recovery % increases from 44 to 59%. Again same dosages of frother with 1.08
kg/t of collector 2 than combustible recovery % increases from 57 to 67.68%. Same dosages of frother with
1.44 kg/t of collector 2 than combustible recovery % has increased from 66.58 to 76.31%.
4. Conclusion
The oxidation of the coal surface alters both physical and chemical properties and reduces the floatability.
The following inferences can be drawn from the above investigation. The lab scale batch flotation
separations showed different mass yields, ash% of floats for the Patherdih washery coals and hence
optimization of the operation condition is required for each coal.
It was found that with the increase of reagent dosages combustible recovery % and flotation efficiency index
% is increasing but ash rejection % is decreasing. The addition of reagent during conditioning period
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significantly adsorbs on the fresh surface, modifies the surface and hence increases the hydrophobicity. At
natural pH, flotation of oxidized coal can be also more effective. Flotation studies carried out in a mechanical
flotation cell shows that cleaning of the rougher concentrate is necessary to reduce the ash content in the
concentrate again for achieving 12% ash content. Table 6 shows the results comparison studies of two
different collector and single frother.
Acknowledgements
The authors would like to thank the CIMFR-Digwahdih, ISM dhanbad for giving permission to present this
paper.
References
M.S. Jena a,1, S.K. Biswal,2, M.V. Rudramuniyappa b,3, Study on flotation characteristics of oxidised
Indian high ash sub-bituminous coal, Int. J. Miner. Process. 87 (2008) 42–50
Book: Chemistry of fine coal flotation; Fine coal processing, Surendra kumar Mishra, Richard R. Klimpel,
page no.70,80,90
Pradyumna K. Naik, P.S.R. Reddy, Vibhuti N. Misra; Optimization of coal flotation using statistical
technique; Fuel Processing Technology 85 (2004) 1473– 1485
K.B. Quast, D.J. Readett, The surface chemistry of low rank coals, Advances in Colloids and Interface
Science 27 (1987) 169–187.
A.A.S.Seifelnassr, Wetting Properties of an Egyptian coal and their relation to its flotation behaviour
changing scopes in Mineral Processing: Proceeding of the 6th international conference; page 209-213.
Shobhana Dey, Gyana Manjari Paul, Santosh Pani, Flotation behaviour of weathered coal in mechanical and
column flotation cell, Powder Technology 246 (2013) 689–694
P. Somasundaran, C.E.Roberts and R. Ramesh; Effects of oxidizing methods on the flotation of coal; Henry
Krumb School of Mines, Columbia University, New York, NY 10027, USA, page 43-48
Jiakun Tan, Long Liang, Yaoli Peng, Guangyuan Xie, Grinding flotation of bituminous coal of different
oxidation degrees, International Journal of Mineral Processing 142 (2015) 30–34
Jinzhou Qu, Xiuxiang Tao, Longfei Tang, Ning Xu, Huan He; Flotation characteristics and particle size
distribution of micro-fine low rank coal; Procedia Engineering 102 ( 2015 ) 159 – 166
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Coal & Lignite
Wencheng Xia, Jianguo Yang, Chuan Liang, Review A short review of improvement in flotation of low
rank/oxidized coals, Powder Technology 237 (2013) 1–8
Wencheng Xia , Guangyuan Xie , Chuan Liang, Jianguo Yang; Flotation behavior of different size fractions
of fresh and oxidized coals; Powder Technology 267 (2014) 80–85
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Coal & Lignite
Abstract
Coal ash is constituted of mineral matter. Separation of the mineral matter from carbon is mainly
depended on the distribution of the same in the coal matrix. During crushing and size segregation of coal,
the ash content increases in the finer sizes. The ash content of coal plays an important role in steel
processes. At JSW different finer size coals are used in various process units and development of an
appropriate technique for reducing the ash in the coal impacts the cost economics of the plant operations.
This paper describes a new beneficiation circuit adopted for reducing the ash in finer size coals (-6mm).
The beneficiation process incorporates combination of dry and wet methods for optimization of the
operational, environmental and cost efficiencies. The process designed herein under, meets the objectives
of minimum moisture and direct usage of the product in the steel processes and low cost of operations.
The developed process was tested on coals used at JSW iron making furnaces. The raw coal with a
proximate analysis of 54.79% FC, 15.58% ash, 26.35% VM, 0.0121% S, and 6309 kcal/kg GCV has
been beneficiated through the combined process. The beneficiated coal has shown improvements in FC,
GCV and reduction in ash by upto 40 %. The final product with a proximate analysis of 60.15% FC,
9.49% ash with gross calorific value 6659 kcal/kg was achieved. The process has yielded 87.17%
concentrate with 94% of recovery. The new combined process has shown promising results in reducing
the ash in fine size coals with minimum losses. The process is now under extensive trials with wide
variety of high ash coals.
Keywords: Fine coals, beneficiation, air JG, spiral concentrator, dry and wet combined process.
1. Introduction
In INDIA coal is a primary fuel for all industrial needs. Indian coals are generally contains higher
amounts of integrated dirt and normally having high amount of ash and low amount of fixed carbon (FC)
[1]. Consequently the importing of high grade coal from other country is increasing by steel plants and
many more industries to run processes efficiently. The crushing and screening of these coals became
necessary for better usage for in different processes. The need to crush coal to smaller sizes for different
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operation is creates the problem of generation of more coal fines [2]. The above said fine coals have the
high ash compared with course coal. This coal is unable to utilize properly in all processes due to
operational limits and its high ash content [3]. In the present investigation an attempt has been made to
give a solution to the aforesaid problem by treating the coal fines in combination of dry and wet
beneficiation methods like Air Jig, Spiral and Flotation processes. Laboratory Size test and its ash
distribution analysis were revealed different suitable unit operations respective to their sizes.
Beneficiation was also carried out on -0.5 mm coal fines using flotation by splitting at size -0.5 mm. Size
fraction of -6 mm+1 mm, -1 mm+0.5 mm and -0.5 mm size fractions were treated in Air Jig, Spiral
concentrator and Flotation processes respectively. Combined process of Air Jig, Spiral and Flotation has
given a low ash% at high yield.
The treatment of the -6 mm +1 mm size fraction by Air Jig, -1+0.5 mm by Spiral and -0.5 mm fractions
by conventional flotation may provide a complete solution of beneficiation of coal fines and as well
environment.
2. Experimental Procedure
The sample was collected from Corex plant screening area (rejected by Corex) at JSW Steels, Bellary,
India. The average particle size of the sample was 1.5 mm. The sample was thoroughly mixed and
prepared the representative sample for different investigations. Various physico-chemical, mineralogical
and beneficiation studies were carried out to upgrade rejected coal. Size wise analysis was done on
sample to know the particle distribution and elemental distribution at different sizes using wet sieve
shaker.
The laboratory batch scale combined beneficiation studies (wet and dry) were carried out to know the
feasibility of sample using screens, Stub cyclone, Air Jig, Spiral concentrator and flotation
Bench scale screen test was done on received sample using 6 mm, 1 mm and 0.5 mm. Air Jig studies
were investigated on intermediate size fraction of -6 mm+1mm with varying flutter valve rpm from 140 –
160. Laboratory spiral concentrate experiments were carried out by varying flow rate. The classification
studies were carried out using Stub cyclone on under size fraction of 0.5 mm screen using 4 inch cyclone.
Total 4 numbers of experiments were done by varying % of solids 5, 10, 15 and 20% the other operating
parameters like vortex finder diameter 18 mm, cyclone operating pressure 2 bar and spigot dia 15mm
were kept constant for all experiments.
A Denver D-12 sub-aeration flotation cell of 1 litre capacity was used for laboratory batch scale flotation
studies. The sample was conditioned at 12% solids with the desired amounts of reagents for a
predetermined time. The Diesel and methyl isobutyl carbinol (MIBC) was used as the collector and
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frother, respectively. Diluted sodium hydroxide of analytical grade was used as pH regulator. Total 10
numbers of experiments were carried out by varying the slurry pH from 6 to 8, collector dosage from 0.5
to 1.5 kg/t with the interval of 0.25 kg/t. During flotation studies impeller rpm 1200 and frother dosage
0.2 kg/t, conditioning time 4 min and froth collection time 4 min were kept constant for all experiments.
The as-received sample consists of 15.58% ash, 54.79% FC, and 6309 GCV. The size distribution and
chemical analysis of the individual fractions are shown in Table 1. Figure 1 shows the optical micrograph
of the coal sample. The clay which is shown as bright contrast in fig. 1 is a major gangue mineral
abounded with carbon form of fine granules. Hence, theoretically ash can be reduced by the gravity
concentration process for course fraction and froth flotation process for finer size fractions at high
recovery [3]. From the chemical analysis of the various size fractions, it is observed that ash content at
various fractions increased with decrease in size.
Size, FC
wt% Ash% VM(%) GCV
microns (%)
+6000 10.36 12.14 55.12 32.74 6372
-6000+3000 25.63 13.54 56.15 30.31 6363
-3000+2000 18.75 15.1 55.53 29.37 6331
-2000+1000 15.06 15.04 55.86 29.1 6265
-1000+750 1.57 15.6 55.06 29.34 6231
-750+500 8.86 15.7 54.56 29.74 6312 Figure 1: Microscopic image of coal sample.
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Ash reduction and FC enrichment is the main challenging aspect of beneficiation of coal. Liberated clay
gangue minerals can be separated by gravity separation methods, where as flotation process is required to
remove the gangue content present in the form of fines. The characterisation studies revealed that
significant amount of gangue minerals are liberated. In the first step, the FC by 6 mm dry screening and -
6 mm fraction further classified by screens 1 and 0.5 mm.
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recovery of 28.17%. The Jig tailing has been crushed to -0.5mm by roll crusher and mixed with spiral
concentrator feed to subject into spiral concentrator to increase the overall mass recovery.
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collector dosage the product weight recovery decreased and FC grade increased. From the experiments,
optimum collector dosage of 0.75 kg/t is obtained.
Unit
. Operation Operating Parameters
Screens 6mm, 1mm and 0.5mm
Flutter valve 155rpm, ventilator
Air Jig
speed 71.8%
Spiral % of solids 30, Flow rate (rpm -
concentrator 43)
VF – 18 mm, Spigot – 15 mm,
Stub cyclone Pressure – 2 bar and Pulp density
– 1.06
%of solids 12, pH-7,
collector(diesel) dosage-
Flotation
0.75kg/ton, MIBC dosage-02kg/t,
conditioning time-4min
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Table 4: Test results of each unit processes
Fixed Total FC
Wt% Ash% GCV Recovery
Carbon Recovery
Feed 100 15.58 54.79 6309 29.63
6mm screen O/S 10.36 12.44 55.12 6372 32.44
Air Jig conc 46.51 8.32 61.24 6745 30.44 93.95
oal
4. Conclusion and flow sheet
Optimum parameters of each unit operation given in Table 3. The results generated from the several
experiments performed are shown in Table 4. Up gradation of this coal fines is required to follow the
generated flow sheet shown in Fig 6. Gravity separation methods like Air jig can upgrade the coal from
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14.41% ash to 8.32% with high recovery and without using water for process. It is very advantage to
minimise the water usage and minimise the operational cost for dewatering. Remove the high density
gangue minerals and spiral concentrator is required and very efficient to improve the coal FC % 45.32 to
56.87 with good recovery and low operational cost. Froth flotation process can recover 34% of feed
material from 40.95% to 58.41 % of Fc recovery. The overall recovery of concentrate is 93.95 with
9.49% ash, 60.15% FC and 6659 GCV at 87.17% of yield. The final tailing loss would be around 49.05%
ash, 22.91% FC and 4003 GCV at 12.83% weight.
Acknowledgements
I would like to thank all contributors for their guidance and cooperation to successfully complete this
project.
References
Shubhkant Kalsi, Dept. of Chemical Engineering NIT Rourkela, Studies of Washing Characteristics of
Low Grade Coal and Design of a Coal Washing Plant.
M.R.Riazi, Rajender Gupta, Coal production and processing technology, 2015, page: 248,CRC Press.
S.Jayanthi, KMaheswarani, V.Saravanan, Assesment of the effect of high ash content in pulverized coal
combustion, APPL MATH Model, volume 31, pages: 934-953, 2017.
D.V.Subbarao, COAL-Its beneficiation(Book), Em Kay Publications.
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INSIGHTS INTO THE ABNORMAL CHARACTERISTICS OF TERTIARY COALS IN MAKUM
COALFIELD, ASSAM FOR THEIR EFFICIENT END UTILIZATION
Abstract
The North Eastern coalfields of Assam, Arunachal Pradesh and Nagaland are disposed along a linear belt of
overthrust, known as the ‘belt of schuppen’, where Tertiary strata are folded and distributed into a number of
thrust slices. Tertiary coal deposits in Assam belong to Eocene and Oligocene age. Eocene coal deposits are
distributed along Mikir Hills, whereas Makum and Dilli-Jeypore coalfields are of Oligocene age. Among
these coalfields Makum in Assam is by far the most prominent and economical reserve with a reserve of 453
million tonnes. Although along the stratigraphic column coal streaks are diversely present but the workable
coals are constrained to the Tikak Parbat and Baragolai formations of Oligocene Barail Group.
Present work aims at detailed characterization of Makum coals through chemical and petrographic
investigation to suggest suitable end utilization for these coals. Channel samples were collected from five
major seams of Makum coalfield. The petrographic studies, proximate analysis and ultimate analysis were
carried out following standard methods. Proximate analysis shows moisture content of 1.5 - 2.4%, and
generally low ash content of < 5% and high VM content of 43.9 - 45.5% (dmf). Elemental analysis reflects a
high carbon and sulfur content of 75.71 – 79.95% and 1.96 – 5.36% (dmf) respectively. These coals have
unique characteristics by virtue of its low ash, high carbon and high sulfur content compared to Permian
coals of India. These bituminous coals are of abnormally high calorific heat value ranging between 6255-
8650 kcal/kg with high VM. Petrographic studies reveal that vitrinite is the dominant maceral (75.0 – 96.0%,
mineral matter free basis) in Makum coals with %Rr varying between 0.53-0.57%. The inertinite content is
very less in all the samples. The liptinite content is usually found to be less than 21.2%. In the light of the
present investigation, Makum coal can be used for power generation with suitable blending with low VM,
low sulfur coals through combustion/gasification route. However, the possibility of utilizing these coals for
coal-to-liquid conversion and exploiting through underground coal gasification cannot be denied.
Keywords: Tertiary coal, belt of schuppen, carbon, sulfur, reflectance, power generation.
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1. Introduction
Energy scenario in our country is coal dominated due to its huge reserve and high dependency on other
countries for crude oil. Around 50 % of the total energy consumption in India is provided by coal. Higher
energy demand and rapidly depleting recoverable reserves of coal posing serious energy issue for India. Coal
deposits of India broadly confined to two geologic periods, i.e., Permian and Tertiary. The former is
deposited in rift valleys while the latter associated with the closure of Tethys Sea and resulting in thrust
tectonics within the Himalayan orogeny. India’s present coal reserves up to the depth of 1200 meters have
been estimated are 301.56 billion tonnes (Ministry of Coal, 2015). Among which 1.59 billion tonnes of low
ash coal is distributed in five North Eastern states of Assam, Meghalaya, Nagaland, Arunachal Pradesh and
Sikkim. These coals have unique characteristics and hold importance by virtue of its quality for industrial
usage. Although limited attention has been paid for characterization of these coals, it can play a significant
role in future energy scenario of North Eastern region (Chandra, 1979; Chandra et al., 1983; Chandra et al.
1984; Ahmed, 1996; Barooah, 1996; Mishra and Ghosh, 1996; Saikia, 2007; 2009).
The Tertiary coal deposits of northeastern India have been distributed in two different tectonic setting of two
different ages. Firstly, the Eocene coal deposits which are found as isolated patches in the southern part of
the Shillong Plateau (Meghalaya), and the Mikir hills and North Cachar hills (Assam). The Eocene coal
deposits of the Garo, Khasi and Jaintia hills of Meghalaya were formed over the peripheral platform areas of
the Shillong Plateau under stable shelf conditions which is an extension of the Precambrian Indian Peninsular
shield. Secondly, the Oligocene coal deposits which are found in the 'Belt of Schuppen' on the northern flank
of the Naga-Patkai range. These coal bearing horizons extend over the states of Nagaland, Assam and
Arunachal Pradesh. In this region, Makum coalfield is the largest depository of the coal and needs special
emphasis. The present study is focused on qualitative assessment of Makum coals for its industrial
utilization.
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thrust faults that are arranged imbricately along the Naga hills and moved northwest relative to the foreland
ridges. The genetic history of ‘belt of schuppen’ commenced during Late Eocene times with the
emplacement of ophiolites in the eastern part of Naga-Patkai range along the margin of the Indian plate.
On collision of the Indian and the Eurasian plate the Indo-Burmese range was formed. This tectonic resetting
caused the development of Oligo-Miocene molasses basins which extended from Nagaland through Assam to
Arunachal Pradesh in further North. These basins have thick measures of coal believed to be developed
during the same time. The platform areas underwent block adjustment mainly due to vertical movements.
Large scale, open upright folds are present which defines the prominent linearity of this structural belt. These
prominent structures in regional scale developed due to Late Miocene folding of the continental margin
sequence and of the molasse sediments.
Major thrust faults developed in the western part due to crustal shortening which was as a result of Syn-
tectonic adjustment of the crustal blocks. The outer limit of the ‘belt of schuppen’ is defined by Naga thrust
fault while inner limits are defined by Halflong-Disang thrust faults. The structure of the ‘belt of schuppen’ is
further complicated by folds, faults, and thrust surfaces; dips are fairly steep to near vertical. The sediments
were deposited in a deltaic condition. The regional palaeo-slope during the deposition of the upper part of the
Barail Group was possibly from northeast to southwest with more coal accumulation in the Upper Assam
(Makum coalfield). Towards north within the belt, the thickness of the coal seams increases and Makum is
one such example.
It has got five to seven coal seams in this field and the maximum thickness of one particular seam is 18 m,
split into two to three sections. The Makum coalfield (27°16’N:95o43’E to 27°18’N:95o55’E) is situated in
the Dibrugarh district and extends over an area of 30 km long and 5 km wide which includes four major
mines, viz., Tikak, Ledo, Tirap and Tipong. The generalized stratigraphic sequence of the coalfield is shown
in Table 1.
Table 1: Generalized Stratigraphic Sequence of Makum Coalfields (after Raja Rao, 1981; Sarmah, 2013).
3
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Miocene TIPAM
Girujan Clay (+470m to 990m)
Variegated clay, silty clay, bluish green and grey sandstone
Tipam Sandstone (+1000m)
Sandstone, clay, shale, coal streaks and silicified woods
SURMA (~400m)
Grits, conglomerates, sandstone, sandy clays and shale.
------------------------------UNCONFORMITY-----------------------------
Oligocene BARAIL
Tikak Parbat
Upper Arenaceous Unit: Sandstone interbedded with sandy shale, grey
shale, siltstone, claystone, mudstone, carbonaceous shale and several coal
seams.
Lower Argillaceous Unit (600 m): Alternations of siltstone, mudstone,
shale, carbonaceous shale, claystone coal seams.
Baragolai (3300m)
Shaly sandstones alternating with clays, shale, sandy shale, siltstone,
mudstone, carbonaceous shale and thin coal seams
Naogaon (2200m)
Sandstone and inter beds of grey splintery shales
Eocene DISANG (+3000m)
Shale with interbeds of dark grey and fine grained sandstone
Channel samples were collected from 3ft, 5ft, 8ft, 20ft and 60ft seams of Tikak, Tirap, Ledo and Tipong
collieries of Makum coalfield, Assam (Figure 1). Samples were crushed to -16 BSS mesh size for
petrographic analysis and -72 BSS mesh size for proximate and ultimate analysis as per BIS. The properties
of the individual coals were evaluated through the proximate analysis (IS 1350 [Part I]), ultimate analysis (IS
1350 [Part III, IV/1, IV/2]) and petrographic study (Vitrinite reflectance and maceral composition) (IS 9127
and ISO 7404 [Part I-III, V]). Moisture, ash, volatile matters and fixed carbon Percentage were determined
through proximate analysis. Ultimate analysis was done using Elementar Vario macrocube elemental
analyzer to determine the elementary C, H, N, S and O (by difference). Leica make DM 4500 microscope
with MSP attachment was used for vitrinite reflectance and maceral analyses under 50x oil immersion
objective. Liptinite maceral was identified with fluorescence light.
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Petrographic characteristics
The petrographic study of different regional seams of Makum coalfield shows that the coals are composed of
varying proportions of different maceral types along with mineral matters (Table 2). The vitrinite content in
the coal samples varies from 75.0% to 96.0% (mineral matter free basis). Telovitrinites mostly occur as thin
to thick bands (Figure 3A, 3C). Detrovitrinite is also observed in relatively less amount (Figure 3B). Some of
the vitrinites impregnated with bitumen, show weak reddish brown fluorescence. The random reflectance
(%Rr) of vitrinites are distributed over V4 to V6 steps (Figure 2). 20ft seam contain more vitrinite as compare
to others seams (3ft, 5ft, 8ft and 60ft seams) but %Rr is maximum for 60ft seam, i.e., 0.57. The %Rr of
Makum coals lies between 0.53% and 0.57%. These coals may be categorized as high volatile non-caking to
weakly caking bituminous coals with respect to their reflectance values.
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Counts
40
50
20
0 0
V₄ V₅ V₆ V₄ V₅ V₆
Vth steps Vth steps
Counts
100 200
50 100
0 0
V₄ V₅ V₆ V₄ V₅ V₆
Vth steps Vth steps
60ft seam
150 %Rr 0.57
100
counts
50
0
V₄ V₅ V₆
Vth steps
Liptinite content in these coals varies from 2.6% to 21.2% (mineral matter free basis). These are dark, thin to
thick walled and mostly embedded in vitrinites (Figure 3D, 3E). Liptinites show orange or bright yellow
color (Figure 3D, 3E) fluorescence under blue light. Sporinite and cutinite are found in all the samples (3ft,
5ft, 8ft, 20ft and 60ft). Suberinite, another sub maceral of liptinite, is very widely distributed throughout the
coal samples. It originates from part of the outer woody tissues of plants and extensively spread throughout
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the Tertiary period. In Makum coals, inertinite varies between 1.1% and 5.2% (mineral matter free basis).
Fusinite and Funginite are most commonly found marceral types in these coals (Figure 3A, 3B). Funginite is
a unique feature restricted to the Tertiary coals and has a wide occurrence in these coals. In some cases,
macrinite has also been observed.
Amongst all mineral matters, pyrite is the most common and has wide occurrence in most samples studied.
Pyrites occur as framboids, granules or crystals, generally along with vitrinite (Figure 3A, 3F). Framboidal
pyrites indicate the marine influence during formation of these coals (McKay and Longstaffe, 2003; Mohanty
et al., 2011). The mineral matter varies up to 28.3%. In 20 ft seam mineral matters are rare (Table 2) and are
apparent from the low ash content for these coals (1.3%, Table 3).
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Figure 3: A, Groundmass of telovitrinite with multi-chambered funginites and pyrites, under normal incident light; B,
Suberinite, mineral matter and uni-chambered funginite; C, Telinite with dark border of secondary liptinite under normal incident
light; D, Sporenite in detrovitrinite under fluorescence light; E, Bitumen impregnated on vitrinite, under blue light; F, Framboidal
pyrite in vitrinite grain. 50x oil immersion objective. Vt- vitrinite, Fn- funginite, Sb- suberinite, Tl- telinite, Sp- sporenite, Lp-
liptinite, M- mineral matter, Py- pyrite.
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Chemical properties:
The proximate analysis data presented in the Table 3 indicates some abnormality in the Makum coals as
compared to the other Indian coal of same rank. Results indicate that the coals are generally low in ash
content, ranging from 1.3% to 5.0% except for 8ft seam i.e., 28.2%. Deposition of these low ash coals can be
explained by following processes, viz.
1. Either the process of doming of the peat deposits that caused leaching of mineral matter from
previously deposited peat or the deposition of peat on surfaces where inorganic sedimentation
processes are not active (Amijaya and Littke, 2004).
2. Or, where rainfall is higher than evaporation, viz., ombrotrophic mires (raised bog, blanket bog, bog
forest) having less ash content than rheotrophic mires (fen, carr, swamp, swamp forest) or than
wetlands (marsh, salt marsh) (Cohen et al., 1987; Moore, 1987).
Makum coals are low in moisture, lying between 1.5% to 2.5% and high in volatile matter, ranging from
43.9% to 45.5% (dmf basis). Mishra and Ghosh (1996) indicated the calorific value of these coals varies
from 6255kcal/kg to 8650kcal/kg and some of them also show caking property. The fixed carbon of the coals
varies within a narrow range of 54.5% to 56.0%.
On dmf basis, carbon ranges from 75.71% to 79.95%, oxygen ranges from 10.29% to 13.35% and hydrogen
ranges from 5.21% to 5.80%, for the studied coals. Present study reveals high sulphur content of these
Oligocene coals ranges from 1.96% to 5.36%. It clearly indicates dominant marine influence during
deposition of these coals. Previous studies have also indicated that these coals are abnormal coals (Iyenger et
al., 1960). However, there is no definite pattern in vertical distribution of sulphur content. Baruah (1994)
have reported that the presence of high sulphur is due to the atomic exchange reaction in which oxygen is
substituted by elemental sulphur.
Based on the available chemical analysis data, Makum coals can be categorized as high volatile non caking
to caking bituminous coals. Prasad and Verma (1982) indicated that particular coals from Makum coalfields
with caking index 16 to 32 can be utilized by blending with other coals in steel-industry. Optimum blend
proportion of different coals for coke making can be decided based on detailed petrographic and chemical
study of coals and cokes (Choudhury et al., 2008). Additionally, these coals have high potential for tar
generation among all other Indian coals, which can be used in chemical industry.
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Table 3: Results of Proximate and Ultimate analyses of coals
3ft 2.2 5.0 45.1 54.6 79.08 5.80 1.73 1.96 11.54
5ft 2.1 4.5 44.6 55.1 75.71 5.21 1.51 4.22 13.35
8ft 2.4 28.2 45.5 54.5 75.71 5.30 1.64 5.36 11.98
20ft 1.5 1.3 43.9 56.0 79.39 5.50 1.40 3.42 10.29
60ft 1.7 2.6 45.4 54.6 79.95 5.67 1.22 2.48 10.68
5. Conclusions
Petrographic study reveals that, vitrinite is the dominant maceral in the Oligocene coals of Makum coalfield,
Assam and varies from the 75.0% to 96.0% (mmf basis). These coals have the percentage mean Rr value
between 0.53 to 0.57 indicating their potential for generation of early thermogenic methane (Scott, 1993).
Even maximum amount of wet methane gas is generated in this range of reflectance value. So, Petrographic
analyses conclude that the coals may be a source rock for hydrocarbons.
The coals have high volatile matter content (43.9%-45.5%, dmf), high sulphur content (1.96%-5.36%, dmf)
and high hydrogen content (5.21%-5.80%, dmf). As per ASTM standard (ASTM D388-12) classification
these coals comes under the Sub-bituminous A to high volatile bituminous B in rank which is basically a
hydrocarbon potential source rock. Makum coals having high carbon content (75%-80%), general low ash
content (< 5.0%) and higher calorific value (6,255-8,650 kcal/kg) is best suited for the thermal power
generation. But the high sulphur content produces a huge amount of SOx gases during power generation,
which creates serious environmental issues. So, it can be washed and utilized by properly blending with low
sulphur coals for power generation. These coals can be blended with prime coking coals for coke making
with a sulphur content within tolerance limit, provided their ash and Sulphur contents are limited to 17% and
3%, respectively. The Indian Gondwana coking coals tend to have relatively high ash content and the low ash
of these coals would help reduce the ash in the overall blend. Their relatively high sulphur content can be
10
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diluted to tolerance limit upon blending with the low sulphur coking coals. However, a detailed study on
Makum coals is essential for strategic management of this valuable resource.
Acknowledgements
Authors are thankful to Director, CSIR-CIMFR for his kind permission to publish the paper. Department of
Science and Technology, New Delhi and Council of Scientific and Industrial Research, New Delhi are duly
acknowledge, respectively, for funding to carry out the field work in NE India and for developing analytical
facilities at CSIR-CIMFR.
References
A. D. Cohen, W. Spackman and R. Raymond Jr. Interpreting the characteristics of coal seams from chemical, physical
and petrographic studies of peat deposits. In: A. C. Scott (Ed.), Coal and Coal-bearing Strata: Recent Advances,
Geological Society Special Publication, 32:107-125, 1987.
B. K. Saikia, R. K. Boruah and P. K. Gogoi. XRD and FT–IR investigations of sub-bituminous Assam coals. Bull.
Mater. Sci., Indian Aca. of Sci., 30:421–426, 2004.
B. K. Saikia. Scanning electron microscopy of Assam coals, India. J. Geol. Soc. India, 74:749-752, 2009.
B. R. Prasad and A. K. Verma. Geology, reserve and general quality parameters of coals from Northeastern India. Coal
India Ltd, N. E. C. F., Assam (Internal Report), 1-5, 1982.
C.S. Raja Rao. (Ed.) Coalfields of India. Bull. Series A. No. 45, V.I Coalfields of North Eastern India, G. S. I., 5-14,
1981.
D. Chandra, K. Mazumdar and S. Basumallick. Distribution of sulphur in the Tertiary coals of Meghalaya, India. Int.
Jour. Coal Geol., 3:63-75, 1983.
D. Chandra, S. Ghose and S. G. Chaudhuri. Abnormalities in the chemical properties of tertiary coals of upper Assam
and Arunachal Pradesh. Fuel, 63:1318-1323, 1984.
D. Mohanty, S. Kumar, P. Boral and N. Choudhury. Petrographic signatures of marine inundation from the Barakar
coal measures of Mahanadi-Ib Valley, Orissa, India., Curr. Sci., 101-9: 1149-1151, 2011.
H. Amijaya and R. Littke. Microfacies and depositional environment of Tertiary Tanjung Enim low rank coal, South
Sumatra Basin, Indonesia. Int. Jour. Coal Geol. 61:197– 221, 2005.
H. K. Mishra and R. K. Ghosh. Geology, petrology and utilization potential of some Tertiary coals of the northeastern
region of India. Int. Jour. Coal Geol. 30:65-100, 1996.
IS 1350-1. Methods of Test for Coal and Coke, Part-I: Proximate Analysis [PCD 7: Solid Mineral Fuels], 1984.
IS 1350-4-1. Methods of Test for Coal and Coke, Part IV: Ultimate Analysis - Section I: Determination of Carbon and
Hydrogen [PCD 7: Solid Mineral Fuels], 1974.
11
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IS 1350-4-2. Methods of test for coal and coke, Part IV: Ultimate analysis, Section 2: Determination of nitrogen [PCD
7: Solid Mineral Fuels], 1999.
IS 9127-1. Methods of Petrographic Analysis of Coal, Part 1: Definition of Terms Relating to Petrographic Analysis of
Coal [PCD 7: Solid Mineral Fuels], 1992.
IS 9127-3. Methods for the Petrographic Analysis of Bituminous Coal and Anthracite, Part 3: Method of Determining
Maceral Group Composition [PCD 7: Solid Mineral Fuels], 2002.
IS 9127-5. Methods for the Petrographic Analysis of Bituminous Coal and Anthracite, Part 5: Method of Determining
Microscopically the Reflectance of Vitrinite [PCD 7: Solid Mineral Fuels], 2004.
J. L. McKay and F. J. Longstaffe. Sulphur isotope geochemistry of pyrite from the Upper Cretaceous Marshybank
Formation, Western Interior Basin. Sedimentary Geol., 157: 175-195, 2003.
M. Ahmed. Petrology of Oligocene coal, Makum coalfield, Assam, northeast India. Int. Jour. Coal Geol., 30:319-325,
1996.
M. K. Baruah. Is elementary sulphur responsible for high sulphur coal? Fuel Proc. Tech., 40:97-100, 1994.
Ministry of Coal. Annual Report 2014-15, Ministry of Coal, Government of India (http://coal.nic.in/content/coal-
reserves), 2015.
N. Choudhury, D. Mohanty, P. Boral, S. Kumar and S. K. Hazra. Microscopic evaluation of coal and coke for
metallurgical usage. Curr. Sci., 94(1):74-81, 2008.
P. D. Moore. Ecological and hydrological aspects of peat formation. In: A. C. Scott (Ed.), Coal and Coal-bearing
Strata: Recent Advances, Geol. Soc. Spl. Pub., 32:7-15, 1987.
P. K. Barooaha and M. K. Baruah. Sulphur in Assam coal. Fuel Proc. Tech. 46:83-97, 1996.
R. K. Sarmah. Study of maturation trend and utilization characteristics of the Oligocence coals in Makum Coalfield,
North eastern India. Int. J. Inno. Res. Dev. 2(5):1447-1456, 2013.
12
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PERFORMANCE OF WATER-ONLY CYCLONE TO TREAT OPEN CAST COAL MINES
A.A.Hembrom* and N. Suresh
Dept. of Fuel and Mineral Engg, ISM, Dhanbad
*Corresponding author: abhishekism0165@gmail.com
Abstract
Froth floatation is widely use technique in coal fines. Use of this technique has been proved to be
expensive and not an environmental friendly. Water-only cyclones (WOC) have several advantages over
froth floatation because it used centrifugal force for separation and to oxidized coal can be treated
effectively. However the use of WOC in India has not been found to be common because the lack of
information on its separation behavior.
In the present paper the attempted has been made to use 100 mm WOC treating -3mm size coal from an
open cast mine known as Gajlitand under BCCL (CIL). Effect of variable such as the outlet diameters
(vortex finder and spigot) have been analyzed on the separation efficiency of the cyclone, the ash
reduction achieved. It was found that using WOC the coal of feed ash (38%) can be reduced to 28% with
an appreciable yield.
Keywords: Water-Only Cyclone, Vortex finder, Spigot diameter, Separation efficiency, Ash.
1. Introduction
Around the world, there are opening the large number of open cast mines has been producing, where the
large number of coal fines is generating. Processing of these run-of mines (ROM) coal can be separated
through the size separation and specific gravity separation. The most common technique used, which is
froth floatation on the basis of size distribution. Use of this technique has been proved to be expensive
and not an environmental friendly. On the basis of specific gravity separation, Water-only cyclones
(WOC) have several advantages over froth floatation because it used centrifugal force for separation and
to oxidized coal can be treated effectively.
From the literature review of the WOC, there are many important variables that can be changed like
vortex finder diameter (VFD), vortex finder length (VFL), spigot diameter (SPD), cone angle (CA), pulp
density (PD) and feed inlet pressure (FIP). In the present paper, attempts of small study the effects of
main variable like as vortex finder diameter (VFD), and spigot diameter (SPD). However, as mentioned
earlier, the use of a wide cone angle and a long vortex finder, make a WOC geometrically different from a
DMC. It is very important to correctly evaluate the performance of any cyclone-type device to study the
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effects of variation of VFD and SPD. Therefore, for the present study only VFD and SPD were chosen
as variable parameters, whereas the VFL, PD, FIP and CA were kept at constant levels of 170mm, 10%
by weight, 0.8 kgf/cm2 and 1200, respectively.
The efficiency of separation of ROM coal from WOC is measured by performing sink and float analysis.
From this analysis, a partition curve is generated to determine the separation density and efficiency of
WOC. The separation cutpoint (ρ50), is the specific relative density of a particle having an equal chance of
reporting to a float or sink called as partition factor. From the above table the separation cut point of
different size is different. The efficiency is based on the recovery in the fines of the separator. The
separation efficiency of water-only cyclone is calculated as follows:
𝜌25 −𝜌75
𝐸𝑝 = , (1)
2
where ρ25 is the relative density at 25% and ρ75 is the relative density at 75%.
2. Experimental procedure
In the present work, studies and experiment have been carried out on non-coking coal sample from
Gajlitand colliery under BCCI (CIL). The experiment has been carried out on laboratory based 100 mm
cylindrical diameter WOC made of stainless steel. A closed circuit test rig, consisting of a slurry pump
and a bypass line was used for carrying out the experiments. Slurry feed rate to the separator and the
pressure at the inlet could be adjusted using the by-pass valve. A heavy duty stirrer was fitted horizontally
at the bottom level of the slurry tank to keep the slurry in uniform suspension. Before carrying out an
experiment, pre-determined quantities of feed coal and water were mixed in the slurry tank to maintain
the desired feed slurry concentration of 10% by weight. Initially, the slurry was pumped through the
separator by keeping the by-pass valve fully open, and subsequently, the opening of the valve was
adjusted to obtain a feed inlet pressure of 0.8 kgf/cm2. The system was then allowed to run for a few
minutes to attain a steady state condition. The steady state condition was believed to be achieved as soon
as the slurry flow rates through the overflow and underflow were found to be constant. The overflow and
underflow streams were then collected for a known period of time, and the respective slurry weights were
achieved. The slurry samples were weighed and dried to determine the solid weight. Representative
samples of the products were then analyzed for ash content.
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Table 1: Size analysis of feed coal sample.
70
60
50
40
30
20
10
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
Size( mm)
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Coal sample
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10 90
20 80
Cum. Float (Wt. %)
40 60
50 50
Float curve
60 40
Sink curve
70 30
Characteristic curve
80 20
Yield curve
90 10
Ngm curve
100 0
0 10 20 30 40 50 60 70 80 90 100
Ash Content ( %)
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3. Conclusions
From the above results and discussion the following conclusions may be mainly drawn, As spigot
diameter increases, yield of clean coal decreases significantly. As spigot diameter increases, slight
decrease in ash of clean coal is observed.
References
N. Suresh, M. Vanangamudi, and T. C. Rao. A performance model for water-only gravity separators
treating coal. Fuel Vol.75, No. 7, PP. 851-854, 1996.
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E. J. Meyer, I. K. Craig. Development of a steady-state partition curve from a dense medium cyclone
dynamic model in coal beneficiation. Preprints of 18th IFAC world congress.
H. Hacifazlioglu. Application of the modified water-only cyclone for cleaning fine coals in a Turkish
washry, and comparison of its performance results with those of spiral and floatation. Fuel Processing
Technology 102 (2012) 11-17.
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CHARACTERISATION STUDIES OF LOW VOLATILE HIGH RANK COAL AND CLEANING
PRODUCTS
Keywords: Low volatile high rank coal (LVHR), Characteristics, Holistic Utilization
1. Introduction
Consumption of coking coal in India between the years 2013 and 2017 is set to increase by 30% to 59
Mt of which almost 70% will be imports. All coking coal produced is not being cleaned as a major
portion of this is the low volatile high rank (LVHR) (coking) coal which is believed to be difficult to
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clean. At present India has total 16 coking coal cleaning plants owned and operated by both public and
private sector with a combined installed capacity of 27.7Mtpy[MOC 2012, MOC 2015]. Out of 34.07Bt
coking coal reserves at least 6.4Bt, probably much more are in the category of LVHR coal. They have
difficult cleaning characteristics and are thought to be techno-economically not feasible for processing
in the existing cleaning plants. LVHR coals are of high rank (RO% >1.2%), high inertinite content, low
reactive content (30-45%), low volatile matter content (18 to 22%), high ash (>30%) and therefore,
having lower caking propensities [Singh et al. 2011]. They mostly occur in lower seams. Currently this
coal in large share is being dispatched to non-steel sector, mostly power plants, as ROM coal or after
nominal cleaning. Going by the current techno-economics cleaning plants for LVHR coals can be
sustained if the clean coking coal yield is at the level of 55-60%. Given the difficult cleaning
characteristics of the LVHR coals it is a difficult proposition. That difficulty could possibly be
addressed if multiple cleaning products with specific end use could be generated.
Objective of the present investigation was therefore to characterize the ROM coal and its cleaning
products to generate necessary property indices which could indicate towards gainful utilization of all
the products of cleaning.
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Table 1 Cut point densities in bench scale cleaning
Size→ -13+2mm -2+0.5mm -0.5mm
Clean coal/ Middling Clean Middlin Clean coal/ Middling
Middling /Reject coal/ g/Reject
Middling
Kathara 1.58 1.68 1.66 1.75 1.96
Process Dense Media Cyclone DMC/ Spirals Water Only Cyclone
(DMC) (WOC)
Proximate analysis (IS 1350-1: 1984), determination of plastic properties, Free Swelling Index (FSI)
and Caking Index (CI) (IS 1353: 1993) and HGI (IS 4433: 1979) were carried out as per relevant Indian
standards. Gross Calorific Value (GCV) was determined by Bomb Calorimeter Model no LECO AC-
350 (IS 1350: 1984). Elemental analyzer (Model Vario EL III CHNOS Elementar) was used to do the
ultimate analysis.
For petrography studies coal microscope, Leica DM 4500 was used. FESEM (Field Emission Scanning
Electron Microscopy) set up, Model no MONOCL 4, was used to obtain SEM images and Energy
Dispersive X-Ray Analysis (EDAX) was used to obtain the elemental composition. Combustion
reactions were investigated by using TGA, Model no NETZSCH, Jupitor STA449 F3.
Nitrogen known to be present in organic part of coal is high in ROM coal. Sulphur content is in the
range typical for Indian coal. FESEM image of ROM coal indicates limited presence of cracks and low
level of adherence of fine particles on relatively coarser particles (Fig. 1) contributing to a HGI value on
the lower side. The Kathara coal with high inertinite content (Table 4) therefore could be classified as a
hard coal with considerable resistance to crushing and grinding. The hardness got reflected in nominal
generation of fines, less than 7 %, when crushed to -13mm. In ROM coal TG plot, mass gain was
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0 0
noticed after 120 C and up to 400 C (Fig 2) probably because of chemisorption of oxygen prior to
ignition [Rostam-Abadi et al. 2015].
Figure 1. FESEM image of ROM coal Figure 2. TGA-DTA curve of ROM coal
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Sulphur content is in the range typical for Indian coal and remains unchanged for cleaning products
except for reject indicating larger presence of sulphur in combustibles. Nitrogen known to be present in
organic part of coal is high in raw and clean coal followed by middling and reject in descending order.
The trend is typical for Indian coal.
Kathara clean coal (Table 3) can be characterized by high VM and moisture contents. Caking
propensities obtained for clean coal shows large improvement. Noteworthy is the increase in GCV of
clean coal compared to ROM coal. Vitrinite and liptinite content, the reactive, and reflectance
considerably increased for the clean coal with corresponding decrease in inertinite and mineral matter
content (Table 4). Changes in maceral composition from ROM to clean coal with fully liberated
vitrinite are confirmed by microscopic images (Fig. 3a &b). FESEM images of cleaning products (Fig.
4) show distinct difference in surface structure of clean coal compared to middling and reject. Sharp
edges, clear structure and dull coloured particles of clean coal indicate basic characteristics of coal in
FESEM images. Clear structure is also visible in microscopic images (Fig. 3b). Overall, Kathara clean
coal shows considerable improvement over ROM coal in all respect of coking coal.
Microscopic images (Fig. 3a &c) of raw coal and middling show quite similar interlocking of maceral
and mineral matters, inter-banding of vitrinite and inertinite macerals etc in spite of crushing down to -
13mm including in the size fraction -2+0.5mm (Table 1). FESEM images (Fig. 4) of middling and reject
showing flaky, irregular shaped particles of light color in middling and reject indicate presence of high
amount of clay and mineral matters. Large presence of Si and Al (Table 4) in combination with high
level of oxygen in both reject and middling possibly indicates larger share of clay, silica, possibly some
other silicates in mineral matter present in coal.
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I
I
V
V
(a) (b) (c)
Figure 3 Microscopic images of Kathara coal: (a) raw coal; (b) clean coal; (c) middling
Figure 4. FESEM images of Kathara coal: (a) clean coal; (b) middling; (c) reject
The middling product can be characterized as low volatile, high ash and very weakly caking coal (Table
3), caking propensity being well within the tolerance limit for coal fired power plants. In fact Kathara
coal at size level -2+0.5mm appears to have no caking properties. Proximate analysis, ultimate analysis
and GCV are quite similar to the ROM coal currently being supplied to power plants. There is hardly
any difference in FC/ VM ratio in proximate analysis and H/ C ratio in ultimate analysis, both important
combustion parameters, between the ROM coal and middling. Therefore the middling product is as
good as the ROM coal as a feed to pulverized coal fired power plants.
EDAX analysis (Table 4) of reject as expected shows larger presence of heavy elements like Fe, Mg
and Ti. Table 3 indicates the rejects to be, as also expected, very high ash, low VM, relatively high
moisture possibly because of larger presence of clay, yet with acceptable heat values and with no caking
properties. In ultimate analysis low values were obtained for all characteristic combustion parameters.
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Yet, Kathara reject compares well with the characteristics of the fuel used for the 10MW Fluidized Bed
Combustion (FBC) based power plant (Table 3) commissioned and operated by Tata Steel using the
reject generated by their own cleaning plant (Bole, 2014).
Interestingly, hydrogen carbon (H/C) ratio remained in the same broad range for ROM coal and all the
cleaning products. According to Mathews et al. [2014] aromaticity of coal is directly related to H/C
ratio and that was not greatly affected by cleaning.
4. Conclusion
Results obtained on all major property indices demonstrate that ROM Kathara coal could be cleaned
with no discard. Clean coal can be used for blast furnace coke making, the middling can be used as a
feedstock for pulverized coal fired power plants and the so called reject can be used as fuel for FBC
plants. The results bring out the scope and opportunity of gainful utilization of all the three cleaning
products of a LVHR coal reducing the import dependency of I&S industry of energy starved India.
References
Mathews. J. P., Krishnamoorthy, V., Louw, E., Tchapda, A. H. N., Fidel Castro-Marcano, Karri, V.,
Alexis, D. A., Mitchell, G. D., A Review of the Correlations of Coal Properties with Elemental
Composition, Fuel Processing Technology (121), pp 104-113, 2014
Rostam-Abadi, M., Debarr, J.A. and Moran, D.L., Burning Characteristics of Partially Devolatilized
Coals, Illinois State Geological Survey, 615 E. Peabody Drive, pp 869-874,
rd
https://web.anl.gov/.../Files/33_4_LOS%20ANGELES_09-88_0869.pdf, Accessed on 23 July, 2015
Singh, A.K., Sahay, A.N., Mishra, H.K., Effective utilization of beneficiated LVHR coking coals and
low rank Indian coals for BF coke making, MineTech, Vol.32 No1, Jan-Mar, pp 3-12, 2011
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COMPARATIVE STUDY OF JIGGING AND DMS FOR COAL ON LABORATORY SCALE
Abhijeet Manasingh*, Abhisek Mohapatra, Lenin Mohapatra and Kotini Rahul Ganesh
Department of Mineral Engineering, Indian School of Mines, Dhanbad
*Corresponding author: abhijeetrkm@gmail.com
Abstract
Coal preparation is the removal of undesirable material from the run-of-mine (ROM) coal by employing
separation process which is able to differentiate between the physical and surface properties of the coal and
the impurities. Through it, a uniform product is achieved. Jigging and Dense Media Separation (DMS) have
formed important tools for the cleaning of coal. Jigging is based upon the terminal settling velocity in a
specific gravity media, while DMS rules on floating of particles and sinking on the basis of their specific
gravity. The Jig utilize the alternate expansion and compaction of a bed of particles by pulsating fluid flow
and DMS is the gravimetric separation based on heavy media formed with either organic liquids, dissolved
salts in water, aerated solids, and suspensions of fine solids in water. Both the technologies have been used
for quite a time. Our study compares the jigging and DMS effectiveness for coal. Both the jigging and DMS
operations were carried out in the laboratory. The DMS operation was carried out using Zinc chloride salt
solution as separating media while batch type KTH Jig was used for the jigging analysis.
1. Introduction
Coal is an organic rock with inorganic mineral matter embedded in it. It is the third most important fossil fuel
after oil and natural gas. It is the backbone of the industrial and domestic major electricity supply (thermal
power plants utilize coal to generate steam which runs generators to produce electricity). The coal is formed
from the submerged plant and animal matters, during the carbonaceous period. Under the great pressure and
high temperature, the organic matter carbonized to coal, under the Earth’s surface. The soil and the mineral
uptake by the plants and animals formed the inorganic mineral matter. This inorganic matter constitutes the
“ash”. The feed coal is thermal coal from Coal Mine at Sarshatali in Asansol, West Bengal. The aim of the
experiment is to evaluate the efficiency of the dense medium process against jigging process. The proximate
analysis of the feed is as follows:
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Proximate Analysis
Moisture 2.33
Volatile matter (Actual) 18.62
Ash 44.51
Fixed carbon (FC) 34.54
On the basis of VM content, the coal may be Low Volatile Bituminous Coal.
Dense medium process was patented in 1858 by Sir Henry Bessemer, using Fe, Ca, Ba, Mn chloride
solutions in cone-shaped separator. Chance Cone process came in 1917, followed by commercial plant for
anthracite cleaning in 1921 and 1925 for bituminous coal. Chance cone used a sand and water mixture as
separating media.
Commercial application of the laboratory float-sink test is the dense medium separation. Laboratory float-
sink test is a standard gravimetric separation with 100% efficiency. It basically uses true liquids as separating
media, with no upward current or agitation needed for maintenance of suspension with sufficient retention
time. There are basically four types of separating media, which are commercially used. Media should be
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cheap, physically stable, chemically inert to target ore, low viscous, easily recoverable and stable at desired
specific gravity. In this process the effect of specific gravity is utilized more than the shape and size of the
material.
The coal separation specific gravities range within 1.30-1.90. On commercial scale, solid suspensions in
water have proved to be the most successful separating media and hence, widely utilized too. The success
owes to its high specific gravity of the solids, which allows lesser quantity, thereby smaller volumetric
concentration and easy recovery. Zinc chloride (ZnCl2) solution was used as separating media within specific
gravity range of 1.25-1.55. The media was prepared in warm water, by dissolving the salt, using hand
stirring. The specific gravity of ZnCl2 is 2.91.
For coal washing, the vessels are categorized as cones, drums, troughs, solid cylindrical drums, solid and
perforated cylindrical drums rotating in drums, conical tanks and parallelepipeds. In this experiment, buckets
have been used for the vessels, containing ZnCl2 media. In plants, the product is either skimmed off, weir
overflowed, internal or external airlift or a lock- hopper arrangement (cone-type washers), lifters mounted
inside the revolving drums (drum-type washers), or chain conveyors (trough-type washers). In this
experiment, product is removed using tea strainers of plastic body.
3. Jigging
Jigging is an ancient cleaning method. It is similar to up and down movement of basket in water, as used in
our homes during pre-preparation of idli. The lighter pulses move out with the pulsed water while the heavy
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sand remains in the basket. Initially, jigging has been used for gold separation being gold very heavier than
its gangue material. The air impulse jig was developed by Mr. Fritz Baum in 1928.
The process of stratification of particles due to alternate expansion and compaction of the particle bed due to
pulsating fluid flow is known as Jigging. This layer wise particle arrangement takes place from bottom to top
with increasing density, i.e. higher specific gravity particles or heavies at the bottom and vice versa. This
stratification is carried out in rectangular, open-top container, jig, in which the particle bed rests on
perforated base through which vertical media current flows alternately. After particle stratification, the bed is
physically “cut” at desired horizontal density plane of particles to separate clean coal from the high dense
refuse. The harmonic motion of the medium (fluid or air) is the main separating media. Mostly, water is used
for jigging process, but now air is also gaining popularity owing to stricter water regulations.
In this experiment, water has been used in the KHD Jig. This is a lab scale instrument and batch process type.
In commercial plants, raw coal is fed continuously fed across the perforated base through which controlled
frequency of pulsion and suction takes place. The lighter clean coal overflows, while the heavy reject is
collected at the base of the jig by lowering the perforated base at set bed depth. This densimetric stratification
is less accurate in the upper portions of the jig bed. Even higher near-gravity material (>10%) adversely
affects jig performance.
Process Meaning
Differential initial Initial acceleration of particles due to pulsion and dependent on the
acceleration specific gravity of fluid medium and solid
Hindered settling Sinking of particles in crowding condition and dependent upon solid
size and the specific gravity of fluid medium and solid
Consolidated trickling Trickling down of the smaller heavies through the bed interstices under
the gravity
The jigging separation in possible due to effective differences in specific gravity of the minerals as:
(ρh − ρf)
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑐𝑟𝑖𝑡𝑟𝑒𝑟𝑖𝑜𝑛 =
(ρl − ρf)
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ρh , ρl, and ρf are specific gravity of the heavy mineral, light mineral and fluid medium respectively.
The experiment was based upon the yield analysis of the two processes: Dense medium separation and
Jigging. Two size factions were taken as (-12+6mm) and (-6+3mm) for both the processes. The feed coal was
roll crushed at 2mm set and screened at 12, 6 and 3 mm screens. 1Kg of sample from each size fraction was
taken and Jones Riffled to get 2 sets of samples, each of 500g, so total 4 samples. These sample fractions
were processed using KHD jig for 10 min and float-sink test for dense media separation.
Jigging of coal in KHD Jig for 10 min with yield of concentrate at 21% ash.
-12+6mm -6+3mm
wt% ash% wt% ash%
Conc. 39.15 20.91 35.29 20.89
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Tail 60.85 51.15 64.71 49.52
Dense medium separation of coal using ZnCl2 solution using standard float-sink test with cut density at 1.55
specific gravity.
-12+6mm -6+3mm
sp gr. cumm cumm cumm cumm
wt% ash% wt% ash%
1.25 1.22 11.31 4.27 8.65
1.35 11.63 13.45 12.02 12.87
1.45 27.96 17.13 34.42 19.89
1.55 43.27 21.33 43.79 21.75
>1.55 100.00 36.45 100.00 38.74
6. Conclusion
The feed coal upon dense medium separation and jigging, dense medium separation gives the highest yield.
Hence, it is more efficient than jigging process. High NGM in the feed coal could have cause this lower
performance in jig.
References
E.R. Palowitch and A.W. Deurbrouck. Coal Preparation. Wet Concentration of Coarse Coal – Dense Medium
Separation. 9(1):9-1,
H.L. Lovell. Coal Preparation. Wet Concentration of Coarse Coal – Hydraulic Separation. 9(2):9-38,
B.A. Wills and T.J. Napier Munn. Dense Medium Separation. Wills’ Mineral Processing Technology.
Elsevier, 11:246-265,(2008)
B.A. Wills and T.J. Napier Munn. Gravity Concentration. Wills’ Mineral Processing Technology. Elsevier,
11:246-265, (2008)
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ASSESSMENT OF COKING POTENTIALS OF COAL BLENDS OF COKING COAL AND
NON-COKING COAL
Sk.Saida , Sanchita Chakravarty2 and Rina Sahu3
1*
1
Dept. of Metallurgical and Materials science, NIT-Jamshedpur, India
2
ANC Division, NML-Jamshedpur, India
3
Dept. of Metallurgical and Materials science, NIT-Jamshedpur, India
*Corresponding author: shahid.saida@gmail.com
Abstract
Most of the Indian coals formed by the drift origin this lead to the high contamination of dirt and other
debris, due to this higher percentage of inorganic impurities present in Indian coals as compared to the
coals of western world and Australia. Due to this reason most of iron and steel industries in India are
importing coal from other countries causing high transportation cost burden on industries. These
inorganic impurities had strong interlocking with coal matrix which makes them very difficult for
separation by comminution techniques. Aim of this project is to reduce the ash content of Indian origin
non-coking to below 20% by using coal beneficiation technique and to study the properties of blends of
non-coking coal and high prime coking coal at different proportions by that observing the Free swelling
index, caking index, Gieseler plasticity, calorific value and vitrinite reflectance number of these coal
blends. Hard non coking coal from Talchar coal fields contain more than 45% of ash is beneficiated by
using spiral concentrators ash content is reduced to 35.25% with a yield of 42.66%. However, for
effective coke making ash % should be less than 20%. Sink &float (sp.density 1.7) gives ash of 18% and
yield is 40% and this coal is blended with New Zealand (1.3 float) coking coal. Results showed that ash
content is decreased in the blends and good swelling properties are attained up to 20% of non coking coal
blending.
Keywords: Non-coking coal, coking coal, coal beneficiation, spiral concentrators, Sink & float, Coal
blends, Free swelling index, caking ability, Gieseler plasticity, calorific value.
1. Introduction
As the demand for steel is increasing in daily life promotes the increase in consumption of coking coal.
And the resources of coking-coal are very limited throughout the world, so there are lots of alternatives
and developments are taking place in coke making industries in order to preserve the coking coal
resources and to replace it with non-coking coal. India is among those countries which has very little
amount of coking resources and with huge demand for coking coal. India had about 88 % of the reserves
is estimated to comprise of non-coking coal with the balance being of medium, prime and blendable
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coking grade coal. In appropriate reserves of coking coal in India and increased transportation cost due to
imports lead to look for alternatives to coking coal. Experiments showed that non-coking coal was found
to yield a good product coke with pitch blending2, TATA Steel plant has conducted lot of research on coal
blending of different grades of indigenous non-coking coals with coking coals and reported that 20% of
non-coking coal blending can be possible in quality coke production5.
Non-coking coal (NCC) from Talchar coal fields contains more than 45 percentage of ash, this coal is
beneficiated using different wet beneficiation techniques to reduce the ash content. Jigging of size -3mm
to +1mm size coal results in 30% ash and the 6.32% yield is very less, so grinding done to reduce the size
of coal to -1mm to +0.5mm due to this the interlocking between coal and particles will broke and ash will
be concentrated. Recycled spiralling for three times of -1mm to +0.5mm coal results in 24% of ash and
gives a yield of 20%. Sink & Float (Sp.gravity 1.7) tests for -1mm to +0.5mm coal gives 18% of ash and
yield is 40% which is highest among all process.
Ash % 30 24 18
Yield % 6.32 20 40
The resultant output from float (1.7) is blended with New Zealand (float 1.3) coking coal in different
proportions up to 50% and swelling properties has been studied through free swelling index test(FSI).
FSI 6 - 5 4 3 3.5 3
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Ash percentage is decreased in non-coking coal while blended with New Zealand coking coal and the
swelling properties were enhanced by adding coking coals to NCC, upto 20% of NCC and 80% of New
Zealand can give swelling properties.
Acknowledgements
This is to convey my gratitude’s to Dr.Sanchita Chakravarthy (ANC division, NML India) and Dr.Rina
Sahu for their encouragement and support in the work and special thanks to Dr.Ranjit (MNP division,
NML India) for his help.
References
M.R. Anand and D.N Prasad1 ., “Recent trends in production and import of coal in India”
Shekher Das, Sapna Sharma, Ratna Choudhury *. “Non-coking coal to coke: use of biomass based
blending material” 2000.
Jadwiga Wieckowska. “Effect of petroleum residue addition on the carbonization of non-coking coals”
,1992.
S.B. Choudhury, S. Sarkar, P.K. Chatterjee, S.S. Chatterjee, R.R. Prasad, S.N. Mukherjee, S.K. Ghosh,
S.R.K. Rao, A.N. Bose,B.B. Brahmachari, R. Haque *. “Solvent refined coal from high-ash non/weakly
coking coals for use in metallurgical coke making.Part II: utilization as a coking additive” 1996
H.P.Tiwarya, R.Sharmaa, S.K.Haldarb, S.Vermab, S.Paulb, and P.S.Dasa.”An Approach to Maximize the
Use Of Non-Coking Coal in Non-Recovery Coke Making” . Received on December 27,2014.
David A Tillman, Dao N.B. Duong, N.Stanley Harding.”Solid Fuel Blending practice and
problems”.2012
S. Chehreh Chelgani , James C. Hower b , B. Hart a.”Estimation of free-swelling index based on coal
analysis using multivariable regression and artificial neural network”
M. B. Nasirudeen, A. Jauro.” Quality of Some Nigerian Coals as Blending Stock in Metallurgical Coke
Production”. 2011.
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CHEMICAL TREATMENT OF HIGH SULPHUR COAL AND ITS CHARACTERIZATION
STUDY
Bhupendra Singh Ken* and Barun Kumar Nandi
Department of Fuel & Mineral Engineering, ISM, Dhanbad, India
*Corresponding author: kenbhupendra3@gmail.com
Abstract
Coal is the most important non renewal source of energy. It is also the most common fuel in thermal power
plants. However during coal incineration in power plants, high sulfur content in coal possesses serious
environmental problems owing to sulfur dioxide emission. To reduce this fatal problem, the sulfur content of
the coal must be reduced. One of the most effective ways to reduce sulfur content is the desulfurization using
chemical. For this purpose, the coal sample was collected from the Tripta mines of North East which had
higher sulfur content. The proximate and ultimate analysis of the sample was done. The ultimate analysis
showed the higher sulfur content which was in accordance with the data available at the mines. The
proximate analysis showed the low ash content. The sample was treated with potassium hydroxide (KOH) at
two different ambiences at different concentrations. The experiments were carried out at room temperature
and at lower temperature 4-10 °C. Highest sulfur reduction achieved is 47.78% at 24 hrs and at 20% KOH
concentration whereas minimum achieved at 5% concentration is 14.86% at. Further, ultimate analysis of the
treated coal samples showed the reduction of sulfur content of the coal. It was observed that reduction was
more favorable at room temperature than at colder temperature (4-10° C).
Keywords: High Sulfur Coal, Desulfurization, Proximate analysis, Ultimate analysis, Potassium Hydroxide
(KOH), Incineration and Temperature & Time.
1. Introduction
Coal is a fossil fuel. It is a combustible, sedimentary, organic rock, which is composed mainly of carbon,
hydrogen and oxygen. It is formed from vegetation, which has been consolidated between other rock strata
and altered by the combined effects of pressure and heat over millions of years to form coal seams. The
build-up of silt and other sediments, together with movements in the earth’s crust (known as tectonic
movements) buried these swamps and peat bogs, often to great depths. With burial, the plant material was
subjected to high temperatures and pressures. This caused physical and chemical changes in the vegetation,
transforming it into peat and then into coal. Coal formation began during the Carboniferous Period – known
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as the first coal age – which spanned 360 million to 290 million years ago. The quality of each coal deposit is
determined by temperature and pressure and by the length of time in formation, which is referred to as its
‘organic maturity’. Initially the peat is converted into lignite or ‘brown coal’ – these are coal types with low
organic maturity. In comparison to other coals, lignite is quite soft and its colour can range from dark black
to various shades of brown. Over many more millions of years, the continuing effects of temperature and
pressure produces further change in the lignite, progressively increasing its organic maturity and
transforming it into the range known as ‘sub-bituminous’ coals. Further chemical and physical changes occur
until these coals became harder and blacker, forming the ‘bituminous’ or ‘hard coals’. Under the right
conditions, the progressive increase in the organic maturity can continue, finally forming anthracite. Coal is
the world’s main fossil fuel, but a major environmental problem associated with its combustion is emission
of sulfur dioxide into the atmosphere. To minimize this effect, methods such as chemical and microbial
desulfurization have been used in attempts to dissolve water insoluble forms of sulfur. Globally, coals are
reported to contain l-3 wt% sulfur. Most of the Indian coals are also low in sulfur content (0.7 wt% or less)
but many coals in North Eastern India contain high sulfur (around 4-6 wt %). Fairly substantial reserves of
medium to semi-coking coals are found in the coal fields of Assam, these coals being somewhat different
from those found in other coal fields of India in respect of high organic sulfur content. The sulfur in coal can
occur as organic, inorganic and even as elemental sulfur. The inorganic sulfur may be again present as
sulfatic and pyritic forms the organic sulfur occur as a part of the chemical structure of coal substance and it
assume to consist of organic compounds of thiophenic nature and alkyl sulfides the elemental sulfur is rarely
found in coals, though in some north east coals, the presence of free sulfur has been reported. In spite of the
problems faced during desulfurization, an in depth study is essential to overcome these problems. Keeping in
view its advantages and necessity for producing desulfurization has also implication in the use of coal as fuel,
as a reducing agent in metallurgy, keeping in mind the environmental problems and metal quality when coal
is used as a smelting process. Another spin off of the coal desulfurization can be the recovery of scarce
sulfur.
2. Experimental
Coal sample was collected from the Tripta mines of North East, Assam, belonging to north eastern coalfields,
India. The sample was stored under atmospheric conditions for few months and ground to below 212 µm
fineness (72 B.S.) and preserved in airtight container. The proximate analysis of coal sample was done by
following Indian Standard methods (IS: 1350 (part I)-1984). The percentage of carbon, hydrogen and
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nitrogen were estimated by using a Perkin-Elmer (model 2400) elemental analyzer and total sulphur by
following ultimate analysis method. The percentage of oxygen was calculated by difference.
Table 3: Analysis of coal samples treated with different strengths of KOH at 25°c (room temp.)
Strength of KOH Carbon (%) Hydrogen (%) Nitrogen (%) Sulphur (%) Oxygen (%)
Table 4: Analysis of coal samples treated with different strengths of KOH at (4 to 10oC).
Strength of KOH Carbon (%) Hydrogen (%) Nitrogen (%) Sulphur (%) Oxygen (%)
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For KOH treatment, 5g of sample was digested with 100 ml of 5%, 10%, 15% and 20% (by value of KOH
laboratory reagent BDH under two different conditions- (i) At room temperature (25oC) and (ii) with the
reacting vessel kept in ice-water mixture for 24 hours (temperature of the reaction mixture noted 4-10oC with
occasional shaking). The result of the analysis for total sulfur in treated coal in both conditions are given in
the tables 3 and 4 the corresponding graphs showing sulfur reduction as a function of KOH concentration are
given in figures 1 and 2.
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60
50
40
30
20
10
0
0 5 10 15 20 25
% KOH
Figure 3: Plot between total sulfur reduction and % KOH at room temperature
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As it is clear from Fig.3, that sulfur reduction is varying greatly with change in concentration of KOH and
time. % Sulphur reduction is higher at higher dosage of concentration of KOH. It is found that KOH have a
notable effect on sulphur removal, and this can be due to the depolymerization of coal which resulted in
small portion of organic matter to be extracted, thus reduction in sulfur quantity.
4. Conclusion
After performing the experiments, it was concluded that , using KOH help to reduce the total sulfur content
in the north east coal from Tripta mines by 47.78% at room temperature(25oC) and by 19.33% at controlled
temperature( 4 to 10oC ).
During the study on the effect of time and rate of desulfurization through Potassium hydroxide (KOH)
treatment, the reduction in the initial stage was maximize for 5% concentration of KOH and it later increased
and then decreased from 25% KOH concentration While the other hand, of controlled temperature, the
reduction in sulfur content was relatively lower than that at the room temperature. It reduced the maximum at
10% KOH concentration and it later increased for other concentration of KOH.
References
Ivatt S, Shah CL, Astle DR, Clamp R. Sulfur reduction techniques. ECSC Project Final Report No 7220-
EA/003, 1994.
Shah CL, Hall ST. The development of fine coal desulfurization system. ECSC Project Final Report No
7220-EA/010, 1996.
Abbott J, Shah CL, Hall ST. Development of a small-diameter hydro cyclone for fine coal
separation. Innovat Phys Separat Technol Ð Richard Mozley Symp Vol Publ 1997:225±36.
Pal, J and Goswami, MC and Singh, Manjit and Singh, KK (2003), Iron-making and Steel making, 30(6) pp.
441-446
Biotechnology and Bio-engineering, F. Kargi, J. M. Robinson Article published: 18 feb 2004
A Thermal investigation on coal from Assam(INDIA), Binoy K, Saikia, Rajini K. Boruah, Pradip K. Gogoi,
Bimala P. Barauh. Accepted 14 september 2008
Davis, V. L., Jr., Bethell, P. J., Stanley, F. L., and Lutrell, G. H. (1995), “Plant Practices in Fine Coal
Column Flotation”, Chapter 21, High Efficiency Coal Preparation (Kawatra, ed.) Society for Mining,
Metallurgy, and Exploration, Littleton, CO, pp 237-246.
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Fuerstenau, M. C., Miller, J. D., and Kuhn, M. C. (1985), Chemistry of Flotation, Society of Mining
Engineers, AIME, New York, 170 pages.
Glembotskii, V. A., Klassen, V. I., and Plaksin, I. N. (1972), Flotation, Primary Sources, New York, 633
pages.
Degner, V.R, and Sabey, J.B.(1988), “Wemco/Leeds Flotation Column Develompent”, Column Flotation 88-
Proceeding of an International Symposium, Chapter29, pp.267-280
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NECESSITY OF GPS-BASED 'PROXIMITY WARNING SYSTEM' IN MINING INDUSTRY –
A TOOL TO PREVENT MINE TRANSPORT ACCIDENTS
Abstract
Mining technology aimed at increasing productivity and safety has seen a rapid increase in adoption over
the last few years. Every year many workers are killed in mining operations when a component of
haulage transport system collides with other transport machineries operating in mine or with workers
working in mine. Also, fatal accidents occur every year, when haulage equipment backs over the edge of
a dump point or stockpile or blasted face point. Devices which are used to monitor the blind areas of
mining equipment are needed to provide a warning to operators when a vehicle, person, object or change
in terrain is near the equipment. The goal of this paper is to introduce a method known as Proximity
Warning System based on the global positioning system (GPS) and peer- to-peer communication has been
developed to prevent collisions between heavy mining equipment, small vehicles, and stationary objects.
As we know that many mining operations already use GPS technology on their mobile equipment for
tracking and dispatch. This paper will provide necessity to add proximity warning to these existing
systems as a safety feature. Long term test on a large scale are needed to prove the technology adequately.
The impact of this approach on industry is that a PWS (Proximity warning system) that incorporates a
combination of technologies could significantly reduce accidents that involve collisions or driving over an
edge at surface mining operations.
Keywords: Proximity warning system, collision, global positioning system, haulage equipment, surface
mining, blind areas.
1. Introduction
In India, Coal is an important mineral. It is not only the main source of fuel in power plants but also it is
used in household cooking throughout the country. The coal industry employs over 6,50,000 miners and
other workers. Safety in the Indian coal mines as well as foreign mines is therefore a very important issue.
Each year, dozens of accidents and several fatalities occur in large equipment operations when smaller
equipment is run over by larger equipment. These accidents occur when a smaller vehicle is in the blind
spot or path of a larger vehicle and is crushed beneath its tires (Fig.1, left side).
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Figure 1: Run over incident at surface coal operation (left) and (right) grey areas indicate where
driver cannot see a 1.8 m tall person from cab of a 50 ton capacity dump truck.
These accidents are caused by the lack of communication between equipment operators and operator’s
limited visibility from the cab of the equipment. In mining operations, these accidents most often involve
large, off-highway dump trucks. The areas that an equipment operator cannot see while seated in the cab
of these trucks can be extensive, depending on the size and type of equipment. Right side of Fig. 1 shows
the blind areas around a 50 ton capacity dump truck common in construction and sand and gravel
operations. The grey shaded area outside of the truck outline shows those areas where the truck operator
cannot see a 1.8 m tall person. Larger trucks up to 360 ton capacity are common in mining, and the blind
areas for these trucks can extend 12 m in front of the truck. Blind areas to the rear and right side can be
even larger. Researchers are investigating methods to reduce accidents attributed to the lack of visibility
around mining equipment. Many technologies exist that can provide an operator with information on
unseen objects or workers near the equipment, including video cameras, sensors, and mirrors. Many of
these technologies have been popular in other industries, such as ultrasonic sensors in the automotive
industry and video cameras on recreational vehicles, but very few have been successfully applied to
mining equipment. Global positioning system (GPS) technology also shows promise for this application.
Many surface mines already use GPS on equipment for tracking, dispatch, and control. A logical next step
for this technology is to use it to track equipment, workers, and stationary structures and provide a
warning when the possibility of a collision exists. A vehicle proximity warning collision avoidance
system is being developed using GPS and wireless local area networks to improve safety of off-highway
trucks in open pit mines.
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2. GPS based proximity warning system concept
The concept for GPS based proximity warning for mining equipment entails the use of differential GPS
receivers and radios on all equipment having reduced visibility, all smaller vehicles on the mine site, and
all workers on foot. The location of all moving objects must be determined and updated in real time
situation, and this information must be transmitted to all nearby equipment so that the equipment
operators are aware of other vehicles or workers nearby. In addition, the location of stationary structures,
such as buildings, utility poles, and dump points, are stored in a database of potential obstacles. An alarm
interface in the cab is required to provide a visual and audible warning when another vehicle, worker or
stationary obstacle is within a preset danger zone around the equipment. The advantages of using GPS
technology for proximity warnings at mining facilities include (a) the ability to use the existing GPS
infrastructure at many mines, (b) the system’s accurate location and tracking abilities, (c) low-to-zero
occurrence of false alarms, (d) the capability of the system to identify obstacles and (e) the ability to
customize the user interface and warning zones. The proximity zone can be dynamically adjusted
depending of predetermined safety factors and vehicle characteristics (truck weight, speed, visibility,
terrain, and weather). If visibility were low due to fog or bad weather, the zone can be increased to
compensate for poor visibility. The proximity zone is a predetermined area or 'bubble' surrounding the
equipment.
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Figure 2: PWS equipment installed on a caterpillar haul truck (left) and dozer and (right) PWS computer
display.
5. Conclusions
The majority of run over accidents occurs from the in-rest state and is mainly caused by lack of
communication between operators. As the operators are unaware of the intentions and actions of other
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operators, the operator of the larger equipment will move the equipment before the smaller equipment is
clear. An in- rest GPS based proximity warning system with transmission lock will prevent the larger
equipment from moving before the area is clear. It will also provide operators of the large equipment with
the location of smaller equipment that may not be visible to them. According to lots of research and tests
at a surface mine showed that a GPS-based PWS has the potential to significantly reduce accidents that
involve collisions or driving over an edge at surface mining operations. Further research and test is
recommended on GPS-based proximity warning system which focused in developing a more reliable
system for potential applications in expert dispatching systems for shovel operation, real-time mining
control and the development of a friendlier working interface for dumper and truck operators.
Acknowledgements
We thank all contributors for their cooperation.
References
• M. Ruff Todd and P. Holden Thomas: Preventing Collisions involving Surface Mining Equipment-A
GPS Based Approach, Spokane Research Laboratory, National Institute for Occupational Safety and
Health, CA, USA, September (2002).
• K. Dagdelen and A. Nieto: Accuracy Testing of a Vehicle Proximity Warning System based on GPS
and Wireless Networks, International Journal of Surface Mining, Reclamation & Environment 17 (2000),
pp. 156-70.
• K. Dagdelen and A. Nieto: Improving Safety of Off Highway Trucks Through GPS, Presented at 29th
APCOM International Conference Proceedings, Beijing, China (2001).
• K. Dagdelen and A. Nieto: Development and Testing of A Vehicle Collision Avoidance System based
on GPS and Wireless Networks for Open-Pit Mines, 31st International Symposium on Application of
Computers
and Operations Research in the Mineral Industries, APCOM 2003, Symposium Series S31, Cape Town,
South Africa, (2003).
• G. Fesak, R. Breland and J. Spadaro: Analysis of surface powered haulage accidents, January 1990 to
July 1996. Holmes Safety Association Bulletin, pp. 1–9.
• T. Holden and T. Ruff: GPS-based proximity warning system for mining and construction equipment,
Proceedings of the 14th International Technical Meeting of the Satellite Division of the Institute of
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Navigation (ION GPS), Salt Lake City, UT (2001), pp. 517– 525. • T.M. Ruff: Test Results for Collision
Warning Systems for Surface Mining Dump Trucks, Publication No. 2000-129, RI 9652, NIOSH (2000).
• A. Nieto and K. Dagdelen: Development of Dump Edge and Vehicle Proximity Warning System Using
GPS and Wireless Network Communications to Improve Safety in Open Pit Mines, in SME (2002).
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196
Comminution & Classification
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Comminution & Classification
CRASH STOP ANALYSIS OF AN INDUSTRIAL DRY GRINDING BALL MILL:
PERFORMANCE EVALUATION AND MODELLING
Abstract
Comminution is a major unit operation in mineral processing industry and also plays a vital role in feed
preparation step of many metallurgical industries. Iron ore pelletization, requires a specific sized feed (~
65% passing 45 microns) and adopts comminution as its first feed preparation step. Ball mills are
predominantly used grinding machines for this purpose. As many researchers pointed out, ball mills are
very energy intensive and notoriously inefficient machines. Hence, performance and energy optimisation
is a necessity rather than a choice in this competitive world.
Tata Steel Jamshedpur is operating a 6 Mtpa Pellet plant equipped with two parallel closed dry grinding
ball mill circuits to provide feed for pellet making. The mills are of 433 TPH capacities each, with 11.83
m internal length and 5.95 m internal diameter. A crash stop audit has been conducted by Tata Steel to
comprehensively evaluate the health and performance of these ball mills. It provides information about
the health of liners, mill shell inlet, internal diaphragm, and outlet diaphragm, presence of coating on
balls, filling level of material, material and media segregation inside the mill, particle size evolution along
the length of the mill. Knowing the mill contents will also provide an opportunity to model the ball mill
as a number of mills in series through Whiten’s perfect mixing model. This paper also provides the
methodology followed to perform a crash stop and to model a dry grinding circuit through the results
obtained from the crash stop. Further, initiatives taken and are being taken based on the outcomes to
optimize the circuit are also discussed in detail.
Keywords: Dry grinding, ball mills, closed circuit, crash stop audit, performance evaluation, modelling
1. Introduction
Grinding, an important feed preparation step for many industrial processes, is the first step in feed
preparation for Pelletization of iron ore. Ball mills are predominantly used grinding machines for feed
preparation in palletisation. As many researchers pointed out, ball mills are energy intensive and
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notoriously inefficient machines. Hence, performance and energy optimisation is a necessity rather than a
choice in this competitive world.
Tata Steel JSR is operating a 6 Mtpa Pellet plant equipped with two parallel ball mill grinding circuits to
provide feed for downstream processes. The dry grinding circuits, having in-line rotary dryer and air
classification systems, are one of its kind for dry iron ore comminution. Any operating problem
eventually produces a drop in the output causing an increase in specific energy consumption of finished
product. The drop may not necessarily be outstanding and more often it drifts with time. Hence for an
established grinding circuit it is imperative to evaluate and benchmark its performance on regular basis. A
comprehensive evaluation of ball mill can be done through crash stop. Crash stop involves stopping the
mill instantaneously to understand the internal conditions such as filling rate, conditions of liners, Mill
shell inlet, Internal Diaphragm (if any), outlet diaphragm ,coating on the balls, material and media
segregation inside the mill, and particle size evolution inside the mill. The information about the contents
of the mill also provides an opportunity to model the mill as a series of ball mills (Benzer, 2005). The
following paper provides the methodology followed to perform a crash stop and interpret the results to
evaluate the health and performance of a dry grinding ball mill. A number of initiatives taken and are
being taken based on the outcomes are also discussed.
2. Experimental Procedure
The mill in the present study has internal dimensions of 11.83 m (L) and 5.95 m (D).The mill has no
partition along its length and hence it is considered as a single chamber mill. However, it should also be
noted that the liners (lifter liners) along the first one third length are different from the liners (classifying
liners) in the next part. The purpose of such liner design is to segregate the grinding media, and thus
facilitating comminution of larger particles (>2 mm) in the first part and of smaller particles (< 2mm) in
the second part. The ball charge size distribution ranges from 75 mm to 25 mm. The mill is typically
operated at 70 % critical speed with 26 % ball load by volume. The discharge from the mill is fed into an
air classifier through a bucket elevator. An air classifier (Roksh) is used to classify the mill discharge thus
making it a closed circuit. A simplified flow sheet of the circuit is given in Fig. 1
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variations in the feed. Finally all the sets of samples collected were mixed and a representative sample is
taken from the mixture for further testing. Post sample collection outside the mill, the mill was crash
stopped (stopping the mill as if it was a breakdown) to collect the samples from inside the mill. The dust
was allowed to settle down and the bed structure was observed from the inlet. Upon inspection a hard
material damp was observed at about 6 to 7 meters from the feed end. The position of the damp material
as seen from the feed end is marked in fig. 2. Sample points along the central axis were marked for every
meter and surface was dug to 30 cm dept. Samples of media and material were collected at the marked
points, to understand the particle size evolution and media segregation along the length of the mill. A
minimum of 3- 5 kg sample and around 30-50 balls were taken from each point (Benzer, 2005). Fig.3:
Photograph showing the collection of material samples inside the mill along the length of the mill.
Internal samples
Screen setup
Dense Phase
Bucket
Elevator
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Figure 2. Uninterrupted mill material Figure 3. Marked sample points along the
after crash stop length of the Ball Mill
3. Laboratory Studies
All the collected samples were dry sieved in the laboratory from 15 mm to 1 mm. A Malvern particle
analyser, which functions on the principle of laser diffraction method, was used to measure the
distribution of minus 1 mm particles. Further a complete size distribution is obtained by distributing the
minus 1 mm measurements within the undersize of dry sieving measurements. Blaine (gm/cm 2), measure
of specific surface area of given material, is also measured apart from the particle size analysis, as it is
assumed that ballability of feed (for palletisation) is better represented by blaine. An automatic blaine
measuring instrument which measures Blaine on the permeability of a packed bed is used to measure the
blaine of the collected samples. BWI (Bond Work Index) experiment was done in laboratory with
standard Bond Ball Mill. The standard procedure with test sieve as described by the Bond was followed
during the BWI determination (Bond, 1961).
4. Modelling methodology
A number of approaches have been developed by researchers to model the industrial dry grinding circuits.
Benzer has developed a modelling approach, based on the perfect mixing model, to model a dry grinding
mill with the data from inside the mill (Benzer, 2001, 2005). Direct application of this model can be best
realized by the industry with the help of commercial software. However a simple spreadsheet application
can also be developed which can be used for optimization after fine tuning it. The efficiency of an air
classifier can be described by a partition curve. Consequently, modelling and simulation of a classifier
can be achieved by correlating plant and material parameters to the efficiency or partition curve. Whiten’s
expression which includes fish hook phenomenon can be used to describe the partition curve. The
variables in the expression can be related to the plant parameters by deducing simple correlation using the
plant data. The constants in the equation can be found out by simple spreadsheet calculations. A non-
linear fitting module in matlab can also be used in finding the constants. A simple spreadsheet has been
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Comminution & Classification
developed based on the above mentioned approaches. Preliminary results have shown encouraging results
and further development of the model is underway.
The identified unground particles at the mill discharge when tested in the laboratory for BWI (Bond Work
Index) resulted in a value of 19 Kwh/t. These unground particles are resultant of the presence of the plus
10 mm particle in the feed. From present samples and the historical data it was observed that an
appreciably amount of plus 10 mm particles were present in the feed (average-16 %). The standard
deviation of plus 10 mm material was high, which makes the controlling a much difficult task. The reason
for standard deviation may be attributed to the fluctuations in the feed being received by the plant. The
recent ore crisis has much worsened the quality of the input received in terms of its size and also
hardness. Controlling input is an onerous task and moreover out of scope when the ore availability is
limited. However such high percentage of plus 10 mm with high BWI (above 16) will be reported
unground at the discharge end or get recycled and can lead to breakdown or under performance. These
larger particles can also cause excess wear and tear of equipment by the virtue of their size. The high
tonnage value coupled with high fluctuations rules out the possibility of pre-screening the material before
processing in the circuit.
Hence, the Pellet plant operations team has devised an innovative screening technology to remove the
unground particles from the circuit. An in house screen set up was placed immediately after the discharge,
which screens out such material from the circuit. The performance of the plant and the breakdown
frequency has reduced after the installation. The position of the screen set up is showed in the Fig 1.
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Comminution & Classification
The size of the media collected at each place was measured and the mean size was calculated. The mean
size of the media along the length of the mill is as shown in the fig. 5. From the figure it is evident that
the initial parts of the mill (0-4.5 m) were filled with smaller balls and larger balls are accumulated at the
centre of the mill between 5 to 7m. The classification performance of the classifying liners is clearly not
up to the mark as expected. The material damp reported in the previous section is also in the same region
i.e. at about 6 meters from feed end. Also the liners in between 5 and 7m are observed to wear at a faster
rate than the rest of the liner in the mill. Inefficient classification of the media is strongly assumed to be a
reason for both the observations. A scope of improvement for the performance of the ball mill and liner
life can be expected here
50
40
30
20
10
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13
Sample collection position from feed end
Figure 5. Mean Size of the ball along the length of the mill
The collected material samples were sieved in the lab to understand the evolution of particle size along
the length of the mill. The percentage retained on each sieve from 20 mm to 1 mm is given in fig.6. As a
thumb rule it is very important that the material above 2 mm should be completely ground by the end of
4.5 meters (lifter liners portion) (William J. Gormley, Personal Communication) because the grinding
mechanism in the second part (classifying liners portion) doesn’t facilitate its commintuion. From the fig.
6 presence of + 3.15 mm and + 6.3 mm particles to an appreciable extent can be seen. These particles
tend to get stuck in the spaces formed by the balls in the second section (William J. Gormley, Personal
Communication). This is one of the prime reasons for damp formation. It is also evident that unground
particles are being accumulated at the 12 meters of the mill (discharge end). From the fIg.5 it can be seen
that between 6 and 7 mm the reduction for + 1 mm particles was almost nil. The particle size evolution
(percentage passing each size) for – 1 mm particles are given in fig. 6. It was observed that the fineness of
the material was increasing along the length of the mill. However, a non performing zone was observed in
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Comminution & Classification
between 5 to 7m, where size reduction of -250 microns particles was inefficient. This particular portion is
highlighted in table 2. Each column in the table 2 represents the percent passing of material at the sizes
mentioned in each row. Presence of larger particles in the second half, and resultant accumulation of
larger balls at this particular region is assumed to be the prime reason for underperformance of the mill in
comminuting both +1mm and -1mm particles. The operation team is undertaking an initiative to manually
classify the steel media and charge them in the next shutdown.
Figure 6: Particle size evolution for – 1 mm particles along the length of the mill
Table 2: Particle size evolution for -1 mm particle along the length of the mill
75 19.62 31.17 37.08 40.13 46.21 54.49 54.96 54.91 56.86 39.83
45 35 13.50 23.23 27.54 30.47 38.60 43.16 43.23 42.62 45.14 %50.85
retained52.91
16 mm 43.37 30.70
30 %46.93
retained48.75
12.5 mm 40.01
38 12.12 21.16 25.00 27.77 33.06 39.87 39.77 39.06 41.65 28.14
25
20 8.97 15.32 18.04 20.04 23.74 28.95 28.59 28.30 30.02 %34.12
retained35.46
10 mm 29.41 20.55
20
15 % retained 6.3 mm
10 7.08 11.06 13.00 14.49 17.09 20.24 20.21 20.01 20.79 23.99 25.11 20.66 14.49
2 10 2.23 2.75 3.75 4.16 4.93 5.59 5.61 5.41 5.73 % 6.18
retained 3.15
6.45mm 5.69 3.80
5 % retained 1 mm
0
0 1 2 3 4 5 6 7 8 9 10 11 12
Sample points along the length of the mill
Figure 7. Particle Size evolution for + 1 mm particles along the length of the mill
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Comminution & Classification
6. Conclusions
Excess percentage of + 10 mm in feed can lead to accumulation of unground particles at the end of the
mill. Hence it is necessary to control the feed input. The segregation of the media is also clearly not as
expected. Absence of diaphragm and ill design of liners were assumed to be the reasons. From all the
observations made it can be concluded that the presence of high wear zone, non-performing or dead zone
and formation of a damp inside the ball mill are all results of feed fluctuations and ill segregation of ball
mil media. Hence segregation of media is being taken up by the plant to rectify the above problems. It can
be concluded that crash stop can provide vital information in performance analysis of a dry grinding ball
mill and it is recommended to perform the test at frequent intervals.
Acknowledgements
Authors are thankful to Mr. William J. Gormley for guiding us during the experimenting process. We
would also like to gratefully acknowledge the support and guidance rendered by Mr. Ujjal Chakraborti
(Chief Agglomerates, Tata Steel), Mr. Kapil Modi (Chief, pellet plant, Tata Steel), Mr. Jagjit Singh
Bhatti (Head, Pellet Plant) and Mr. Srinivas Dwarapudi (Head, Agglomeration, Tata Steel R&D) during
the entire activity. Thanks are also due to pellet plant staff, CRMT staff and R&D personnel for their
consistent effort in collecting and analysing the samples at the time of need.
References
F. C. Bond, Crushing and Grinding Calculations, Part 1, Allis Chalmers publications, 1961
H. Benzer et al. Modelling cement grinding circuits. Minerals Engineering, Vol 14, No 11, pp 1469-
1482, 2001
Hakan Benzer: Modelling and simulation of a fully air swept ball mill in a raw material grinding circuit.
Powder Technology, 150: 145–154, 2005
Okay Atlun, Hakan Benzer. Selection and mathematical modelling of high efficiency air classifiers.
Powder Technology, 284:1-8, 2014
Napier Munn. T. J, Mineral Comminution Circuits, Their Operation and Optimisation, Julius Kruttschnitt
Mineral Research Centre, 1996
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Comminution & Classification
206
Copper, Lead & Zinc Ores and Precious metals
207
Copper, Lead & Zinc Ores and Precious metals
STABILITY ASSESSMENT AND REMEDIAL MEASURES ADOPTED FOR TAILING
DUMPS AT HUTTI GOLD MINES
Abstract
The tailing disposal is creating lot of apprehension in lot of people’s mind due to misconception of the
disposal and impact on environment. For nation’s economic progress, there is no option than increased
exploitation of mineral resources. While mining ore and minerals, generation of waste is inevitable. This
paper deals with successful, eco-friendly and sustainable tailings disposal, without compromising mineral
conservation, by effective scientific design, development and rehabilitation of waste dump. The tailing
dump disposal has set an example for designing, development and managing taling dumps.
Key words: Tailing, gold ore tailing, tailing disposal, tailing dump stability, tailing dump management,
GOT.
1. Introduction
The Hutti Gold Mine Company Limited (HGML), a Govt. of Karnataka Enterprise, the primary gold
producer in India and 40th member of the World Gold Council, was started in the year 1947 and till now
17.04 million tonnes of ore has been treated with the present day installed capacity of 2000 TPD. The
company has adopted new technologies with the advancement and pertinent to the time. The tailing
generated after treatment of gold ore by the different established processes like mercury amalgam-mation,
there after cyanidation- CIP process are stacked in tailing dump. There are mainly two tailing dumps in
HGML premise. About 8.0 million tonnes old tailing has been stacked in the abandoned old tailing dump.
The new tailing dump of about 4 million tonnes tailings has been stacked.
2. Tailing production
Beginning with processing of 13 tonnes/day (TPD) of ore in the year 1948, it increased to 420 TPD in the
year 1970. It further increased to 910 TPD in November 1996, from January 1998 the production capacity
was increased to 1450 TPD.The combined capacity now is 2000 TPD. The tailings are being pumped
with about 50% water content.
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Copper, Lead & Zinc Ores and Precious metals
(Abandoned 2001)
The Old Tailing dump was built up by pumping the tailing slurry and keeping the edges of the dam raised
by about 0.5 m to 1.0 m. There was no formation of earthern starter dyke. Water was allowed to be
ponded to one side from where, it was recovered and pumped out for reuse in the ore grinding process.
The tailings were being generally discharged around the periphery of the dump so that to perimeterial
coarse graind cover/bund forms, the surface of which in the course of time became hard due to oxidation.
The composition of the tailings is directly dependent on the source of ore fed to the beneficiation plant.
Tailings may contain trace quantities of metals found in the host ore, and they may contain substantial
amount of added compounds used in the extraction process. Elements are rarely in elemental form, more
often as complex compounds.
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Copper, Lead & Zinc Ores and Precious metals
Radical Assay %
SiO2 56.19
Fe2O3 9.14
Al2O3 9.06
CaO 8.45
MgO 3.50
Na2O 2.32
K2O 1.75
S(T) 1.21
As 0.81
Cu 1.01
Pb Trace
Zn 0.014
WO3 0.03
L.O.I 5.13
Typically the foundation soil profile of the dump consists of 0.5 m to 1 m thick black cotton soil,
followed by about 0.5 to 1 m thick murram (gravel sand). This is underlain by highly fractured and
weatheres rock of 1.5 to 1 m thickness laying over fresh metabasalt rock.
As such it may be surmised that the base of the tailing pond having Black Cotton Soil is relatively
impermeable. Also most of the water from the tailing slurry is being collected and recirculated.
The average grain size distribution of the tailings from the old tailing pond is as stated in Table 1.
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Copper, Lead & Zinc Ores and Precious metals
Table 1: Sieve analysis of old tailing dump samples.
The sieve Analysis of the Monthly Final Residue (MFR) is being regularly carried out. The analysis for
the months of May, June and July 2015 is included in Table 2.
It is evident that most of the particles fall into slit size range (-75 microns). The slurry with the coarser
particles is being sent back to the mines for stope refilling.
3. Rainfall data
The annual rainfall from the year 1990 to 2001 was around 800 mm, the average for the last 40 years was
around 600 mm. In the year 1990-1993, the average rainfall was around 820 mm, followed by 475 mm in
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Copper, Lead & Zinc Ores and Precious metals
the year 1994, then again 825 mm and 985 mm in the year 1996 and 1996, reaching 1330 mm in 1998,
followed by the relatively dry spell in 1999, but again increasing to around 850 mm in the year 2000 and
2001, 2009 & 2014.
Thus, in the heavy rainfall months and years, the erosion had been severe, causing, considerable flow of
the tailings, which in turn increased the severity of erosion and resulting in heavy rain cuts and breaching
A collaborative research project “Utilization of Gold ore Tailings (GOT) in agriculture as a source of
Micronutrients for crop production” was carried out between M/s HGML and University of
Agricultural Science (UAS), Dharwad (2003-2007) and was reseated in its use that GOT at 1 ton/Ha
for the cultivation of Wheat, Groundnut, Sunflower, Maize, Bengal Gram, Poatatoes, Chillies, Onion
and Cotton cropping systems have increased the economic yield of the crops.
Possible minerals and metals recoverable from mine – waste and mine tailings:
Beneficiation studies of a gold ore tailings dump sample of Hutti Gold Mines Co. Ltd. is conducted by
Indian Bureau of Mines-regional ore dressing laboratory, Bangalore and have reported that
Utilization of GOT for manufacturing of Bricks, tiles civil works has been entrusted to National
Institute of Technology Karnataka, Surathkal.
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5. Stabilization of old tailing dump
a) Stoppage of further disposal of tailings and allowing the pond to dry.
b) Capping of the top of the tailings mound with local soil impervious material and vegetation.
c) Provided surface water drainage system on the cap.
d) Rock toe protection around the peripheral toe of the mound for intercepting the eroding material
preventing it from reaching the wall/nallah.
e) Erosion protection of steep slopes.
6. Tailing dump stabilization by Coir Mats on the slopes
Coir-mats were implemented in association with Karnataka State Coir Corporation, these mats were laid
on the slopes of tailing dump to minimize the direct impact of the rain on the dump terrain.
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Copper, Lead & Zinc Ores and Precious metals
The mats were plugged properly on the dump slopes and were used to last may mansoons.The coir mats
served the dual purpose firstly controlling the erosion and subsequently, helpful in forming the organic
mulch and direct impact of rain water and its flow thereby controlling the speed of water flow and
erosion.
Plots of forestry and horticulture plants were grown, which has survived well and has given confidence
that the above efforts on dumps can stabilize dumps and forest can be created. Various species planted are
Chikoo, Awala, Tamarind, Custard -apple, etc, are grown, once these fruit –bearing trees are grown on
the slopes of the dump fauna like birds, insects, butterflies, prey birds, and animals are attracted on these
plots. Other in-house initiatives tried are growing of bio-fuel yielding trees like Pongemia, Simaruba,
Neem, Hippe. They are grown in plots to find that the soil can sustain the growth of such plants so that
such waste dumps can be utilized for the commercial plantation.
7. Conclusions
Successful management of Tailing dump is a big challenge, unless all the necessary factors are taken care
properly. Stability assessment and remedial measure need to be adopted. Scientific waste dumping and
Rehabilitation of waste dump by growing vegetation and laying coir mats on the slopes of tailing dumps
has leads to dump stability by reducing the direct impact of rain water thereby controlling the speedy of
water flow and erosion. These dumps are stable for decades and with stood heavy rains and other forces
of the nature, and thick vegetation on the top of the tailing dump and on the slopes.
Acknowledgments
We would like to express our special gratitude and thanks to A.K Monnappa, IAS Managing Director &
Sri A.R Walmiki, Executive Director, The Hutti Gold Mines Co Ltd,Hutti who have given us the golden
opportunity in partipating in this event and for presenting the paper.
*****
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Copper, Lead & Zinc Ores and Precious metals
BENEFICIATION STUDIES ON A GOLD ORE SAMPLE FROM TOGO, AFRICA
Suresh Kumar*, Dev Prasad Ananth, Indira Ravindran
Regional Mineral processing Laboratory, Indian Bureau of Mines, Bangalore.
*Corresponding author: suresh120@rediffmail.com
Abstract
A gold ore sample from Togo, Africa assayed 18.88ppm Au, 10.69 ppm Ag, 83.31% SiO2, 4.63% Al2O3,
3.90% Fe2O3, 1.25% LOI, 0.14% MgO, 1.69% CaO and 0.27% Na2O. Native gold grains, less than 10
microns, were observed commonly in goethite and occasionally in quartz grains. The sample
predominantly consists of quartz + feldspar. Chlorite / amphibole, carbonates (calcite), chloritoid +
epidote, goethite / limonite, muscovite mica+ biotite mica, ilmenite, chalcopyrite, chalcocite, pyrite,
magnetite / martitized magnetite and hematite are present in minor to trace amounts. The as received
sample was ground to minus 0.300mm and subjected to tabling. The table concentrate assayed 142.21ppm
Au with 42.2% Au recovery (Wt% yield is 5.3).
The table concentrate further subjected to dry magnetic separator to improve grade in the table
concentrate. The magnetic concentrate assayed 185.51 ppm gold with 28.3 % recovery (Wt.% yield is
2.7). The table rejects (table tails & slimes) was ground to minus 0.075 mm size and subjected to
cyanidation. Carbon – In – Pulp and Carbon – In – Leach processes were tried and both were found
working successfully on the sample. Pre- concentration of ore employing tabling followed by cyanide
leaching tests on the ground table rejects to minus 200mesh resulted in over allrecovery of 95.2% Au with
residue assaying 0.83g/t gold.
1. Introduction
Togo officially the Togolese Republic is a country in West Africa bordered by Ghana to the west, Benin
to the east and Burkina Faso to the north. It extends south to the Gulf of Guinea. Togo covers 57,000
square kilometers, making it one of the smallest countries in Africa, with a population of approximately
6.7 million. In 2011, mining accounted for about 2.8% of Togo’s gross domestic product, and Togo was
ranked 19th among the world’s leading producers of phosphate rock, by volume. Other mineral
commodities produced in the country included cement, clinker, diamond, gold, and limestone.
Undeveloped mineral resources included bauxite, gypsum, iron ore, manganese, marble, rutile, and zinc.
Togo also produces significant amounts of gold and diamonds by artisanal working. It was sixth largest
producer of gold in Africa [1].
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Copper, Lead & Zinc Ores and Precious metals
2. Methodology
The gold sample was obtained from Togo, Africa. The as received sample was mixed thoroughly and
representative portion was drawn for the study. The chemical analysis was carried out by standard wet
chemical analytical procedure (Anon, 1975) and gold analysis was carried out by fire assay method [2].
The mineralogical examination of the thin and polished sections of the sample was carried out using
Letizpetrograpic microscope. Different opaque and transparent minerals were identified.
3. Beneficiation Study
The as received sample was stage crushed to 1.7 mm size in a roll crusher (KHD Humboldt Wedag,
Germany). The crushed product was stage ground to 0.300 mm in a rod mill (Denver, USA) at 66%
solids using 12.5 kg rod charge. The ground product was subjected to tabling (Deister quarter deck, USA)
to produce table concentrate, table tails and table slimes. The table concentrate was subjected to dry
magnetic separation (Box Mag Rapid, Australia) at 12,000 gauss to get magnetic and non magnetic
product. The table tails and table slimes i.e. table reject was stage ground to 0.075mm in a rod mill. The
ground product was subjected to bottle roll cyanidation test [3].
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Copper, Lead & Zinc Ores and Precious metals
Chemical analysis
Table 1: Chemical analysis.
Radicals %
SiO2 83.31
Al2O3 4.63
Na2O 0.27
K2O 0.13
Fe2O3 3.90
L.O.I. 1.25
CaO 1.69
MgO 0.14
S(T) 0.09
Cu Traces
Pb Traces
Zn Traces
Au 18.88ppm
Ag 10.69 ppm
Mineralogy
Native gold grains, less than 10 microns, were observed commonly in goethite and occasionally in quartz
grains. The sample predominantly consists of quartz + feldspar. Chlorite / amphibole, carbonates
(calcite), chloritoid + epidote, goethite / limonite, muscovite mica+ biotite mica, ilmenite, chalcopyrite,
chalcocite, pyrite and magnetite / martitized magnetite are present in minor to trace amounts. Pyrite is
altering to goethite around the grain boundaries.Chalcopyrite is altering to chalcocite. Approximate
percentage of different mineral constituents in the original sample is as follows
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Copper, Lead & Zinc Ores and Precious metals
As observed mineralogically, presence of native gold of 10 micron size in the inter-granular spaces of
Quartz (Qz) grains (figure 1) and as inclusions within goethite (figure 2). The results of the grinding to
0.300 mm followed by tabling yielded a concentrate assaying 142.21ppm Au with 42.2% Au recovery
and Wt% yield is 5.3. To improve the gold values, the table concentrate was subjected to magnetic
separation, a magnetic concentrate assaying 185.51 ppm gold with 28.3 % recovery with overall Wt%
yield is 2.7. To improve the recovery of gold, the table reject was ground to 0.075 mm and subjected to
cyanidation and carbon –in pulp leach process resulted in overall recovery of 95.2% Au with residue
assaying 0.83g/t gold. Direct cyanide leaching, adopting bottle roll procedure, of ore at 0.075 mm size,
resulted in recovery of 94.3% Au in the solution. Leach residue assayed 1 g/t Au. The metallurgical
results are given in Table 3 and process flowsheet is given in Figure 3.
Figure 1: Native Gold (Au) in the inter-granular spaces of Quartz (Qz) grains.
Free Goethite (Go) and Quartz grains are also present in Table Concentrate.
(Reflected light, Air, 20 X)
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Copper, Lead & Zinc Ores and Precious metals
Figure 2: Native Gold (Au) present as inclusions within the Goethite (Go).
free Quartz (Qz), Martitized magnetite (M.Ma) and Pyrite grains are also
present in Table Concentrate. (Reflected light, Air, 20 X)
AS RECEIVED SAMPLE
Crushing
GROUND TO 48 MESH
TABLING
CONCENTRATE REJECTS
CYANIDATION - CIP
Direct cyanidation
Acknowledgements
The authors acknowledge with thanks Dr. M. Hanuma Prasad for arranging the sample from Global
Industries Sarl, Togo. The authors are thankful to Shri R K Sinha. Controller General (I/c) and
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Copper, Lead & Zinc Ores and Precious metals
SmtS.M.Lal, SO(OD) & In charge, mineral processing division, Indian Bureau of Mines, Nagpur for their
keen interest and guidance throughout this study.Authors also express their thanks to all those who were
directly or indirectly involved with the above study.
References
Anon, USGS 2011 Mineral Year Book- Advance release Central African Republic and Togo, March 2013
Anon, Manual of procedure for chemical and instrumental analysis of ores, minerals and ore dressing
products, Indian Bureau of Mines, Nagpur, India .1975.
Unpublished internal reports, Regional Mineral Processing Laboratory, Indian Bureau of Mines,
Bangalore
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Copper, Lead & Zinc Ores and Precious metals
FLOTATION STUDIES ON A COPPER PLANT TAILS SAMPLE OF DEMOCRATIC
REPUBLIC OF CONGO
V.A.J.Aruna, Prathama Diwakar, P.P.Pathak, B.R.Ramteke*, and S.M.Lal
Modern Mineral Processing laboratory & Pilot Plant, Indian Bureau of Mines, Nagpur
Corresponding author: indian75@bsnl.in
Abstract
Bench scale beneficiation studies on a copper flotation concentrator tailings sample from the Democratic
Republic of Congo were conducted to obtain a copper pre-concentrate of ~8% Cu for the subsequent
recovery of copper through hydrometallurgy. The copper tailings sample assayed Cu: 0.82%, NiO:
0.006%, SiO2: 58.70%, Fe2O3: 4.08%, Al2O3: 13.01%, S(T): 0.58%, and LOI: 3.45%.Mineralogical
analysis of the copper tailings sample revealed that malachite and azurite (1-2%) are the main copper
bearing minerals present in very minor amounts. Chalcopyrite is present in trace amounts. Quartz (45-
50%) is the predominant gangue mineral in the sample with major amount of clay(18-20%), feldspar
(microcline, plagioclase) (18-20%), subordinate amount of mica (muscovite, biotite) (8-10%), very minor
amount of pyroxene (diopside) (1-2%), pyrite (1-2%), and traces of goethite, limonite, hematite and
tourmaline. The beneficiation process involved wet screening of the copper tailings sample at 30 mesh to
remove wood material followed by flotation of -30 mesh size of the tailings sample at 36% solids.
Flotation of - 30 mesh sample using sodium oleate as collector, light diesel oil and kerosene as supporting
collectors, pine oil as frother, sodium silicate as depressant for silicate gangue minerals yielded a copper
concentrate assaying Cu: 8.0%, NiO: 0.011%, Al2O3: 12.78%; SiO2: 34.39%; Fe2O3: 6.958%; S(T):
1.398; and LOI: 12.06% with a copper recovery of 40.4%. (Wt.% yield: 4.3). The copper pre-concentrate
of desired copper grade with reasonable recovery was achieved.The present study suggests that
reprocessing of plant tailings using cheap collectors like sodium oleate along with supplementary
collectors like light diesel oil and kerosene are found to be effective in the recovery of oxide copper
minerals from plant tailings sample. Reprocessing of plant tailings aids is significant from the mineral
conservation and environmental protection point of view.
Keywords: Reprocessing, plant tailings, copper oxide, flotation, mineral conservation, environmental
protection.
1. Introduction
About 1150 million tons of heavy metals (copper, lead, cobalt, zinc, cadmium and chromium ) have been
mined since the stone age with estimates of contemporary mine tailings production ranging from 5 and 7
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Copper, Lead & Zinc Ores and Precious metals
billion tonnesper year worldwide.(Mudd and Boger 2013). The processed tailing of copper generally
consists of 95-99% of the crushed and ground ores of size ranging (1-600 µm), along with process water
which includes dissolved metals and ore processing reagents. With the depletion of high grade ores and
mining complex ores, more intense grinding and changes to processing technology, a larger volume of
tailings has been produced as a function of each unit of ore extracted, prompts increased scrutiny from
environmental regulators. The physical and chemical characteristics of the tailings vary with the ore type.
There are three types of approaches for tailing management viz., (i)paste and thickened tailings; (ii)
tailings reuse, recycling and reprocessing; and (iii) proactive management.(Edraki et al 2014)
The as received copper tailings sample assayed Cu : 0.82%, NiO: 0.006%, Y2O3: 0.003%, MnO: 0.024%,
BaO: 0.068%, ZrO2: 0.03%, Cr2O3: 0.03%, SiO2: 58.70%, Fe2O3 : 4.08%, Al2O3: 13.01%, P2O5: 0.27%,
Acid Insoluble: 82.32%, CaO: 0.46%, MgO: 0.93%, and S(T): 0.58%, TiO2: 0.75%, Na2O: 0.62%, K2O:
8.77%, Rb2O: 0.016%, and LOI: 3.45%.
Mineralogical analysis of the copper tailings sample revealed that malachite and azurite (1-2%) are the
main copper bearing minerals present in very minor amounts. Chalcopyrite is present in trace amounts.
Quartz (45-50%) is the predominant gangue mineral in the sample with major amount of clay (18-20%),
feldspar (microcline, plagioclase) (18-20%), subordinate amount of mica (muscovite, biotite) (8-10%),
very minor amount of pyroxene (diopside) (1-2%), pyrite (1-2%), and traces of goethite, limonite,
hematite and tourmaline.
A representative portion of as received tails sample was subjected to wet sieve analysis from 10 mesh to
325 mesh size. The results indicate that copper values are predominantly distributed in -325 mesh size
fraction. The -325 mesh size fraction assayed 1.16% Cu with Cu recovery of 73.6 (Wt.% yield: 52.7). As
the major portion of the sample is present at fine size, froth flotation is the suitable method for pre-
concentration of copper values from the tailing sample. As per the mineralogical observation most of the
copper bearing minerals are in the liberated form, there is no need for further grinding of the tailing
sample for pre-concentration by froth flotation process.
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2.4 Choice of collector
In order to identify a suitable collector, flotation tests were carried out under identical conditions using
different collectors.It is inferred from the results that Na-Oleate as collector with kerosene as supporting
collector (A) and Na-Oleate as collector with Light Diesel Oil to Kerosene (4:1) (Vol/Vol) as supporting
collector (B) are found to be strong collectors. The rougher float obtained with Na-Oleate as collector and
kerosene as supporting collector (A) assayed 1.37% Cu with 82.7% Cu recovery (Wt.% yield: 54.3),
whereas the rougher float obtained with Na-Oleate as collector with Light Diesel Oil to Kerosene (4:1)
(Vol/Vol) as supporting collector (B) assayed 1.08% Cu with 86.1% Cu recovery (Wt.% yield: 66.0).
The III cleaner float obtained with Na-Oleate as collector and kerosene as supporting collector (A)
assayed 2.40% Cu with 52.6% Cu recovery (Wt.% yield: 19.7), whereas the III cleaner float obtained
with Na-Oleate as collector with Light Diesel Oil to Kerosene (4:1) (Vol/Vol) as supporting collector (B)
assayed 1.92% Cu with 55.0% Cu recovery (Wt.% yield: 23.8). Thus the Wt.% yield and Cu recovery of
the III cleaner float concentrate obtained using Na-Oleate as collector with Light Diesel Oil to Kerosene
(4:1) (Vol/Vol) as supporting collector (B) is relatively better than that obtained with Na-oleate as
collector with kerosene as supporting collector (A). Thus, (B) is chosen as the suitable collector.
Moreover, Na-Oleate is a cheaper collector in comparison with other collectors. The other collectors (C)
and (D) although they are selective in flotation of copper as evidenced by the assay of rougher float
1.80% Cu for (C) and 1.42% Cu for (D) and III cleaner float 4.25% Cu for (C) and 3.65% Cu for (D),
their Cu recoveryand weight % yield were lower than that of (A) and (B).Collector A: Sodium Oleate +
Kerosene. Collector B: Sodium Oleate + Light Diesel Oil (LDO) + Kerosene.Collector C:
Dithiophosphate + Light Diesel Oil (LDO) + Kerosene,Collector D: Aryl Hydroxamate + Light Diesel
Oil (LDO)+ Kerosene.
2.5 Optimisation of collector dosage
In order to optimise the dosage of collector, flotation tests were carried out under identical conditions
while varying the dosage of sodium oleate + (Light Diesel Oil to Kerosene) (4:1). From the results it is
clear that as the dosage of collector and supporting collector increases, the copper recovery increases.
The rougher float (calc.) copper recoveries for Na-Oleate dosage of 0.5, 0.78 and 0.85 Kg/t are found to
be 67.7%, 81.0% and 85.8%, respectively. This suggests that with the increased dosage of collector and
supporting collectors during cleaner flotation the copper recovery increases. Furthermore, it is observed
that in order to enhance copper grade the cleaner flotation stages are to be increased. Hence, in further
tests the cleaner stages were increased.From the results it is clear that as the dosage of collector and
supporting collector increases, the copper recovery increases. This suggests that with the increased
dosage of collector and supporting collectors during cleaner flotation the copper recovery increases.
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Copper, Lead & Zinc Ores and Precious metals
Furthermore, it is observed that in order to enhance copper grade the cleaner flotation stages are to be
increased. Hence in further tests the cleaner stages are increased.
In order to identify the suitable depressant for gangue minerals flotation tests were carried out using
different depressants. From the results it is inferred that sodium silicate can be used as depressant for the
silicate gangue minerals as there is no improvement in grade when lactic acid is used as depressant.
Therefore, sodium silicate alone is identified as a suitable silicate depressant in the present sample for
achieving the desired copper grade.
In order to optimise the dosage of depressant, flotation tests were carried out under identical conditions
while varying the dosage of sodium silicate. It is observed that with the increase in dosage of depressant,
the copper grade increases. When no depressant Na2SiO3 is added the copper IV cleaner float concentrate
obtained assayed 1.18% Cu with 67.7% Cu recovery, with 1.75 Kg/t Na2SiO3 the copper IV cleaner float
concentrate obtained assayed 3.62 % Cu with 52.8% Cu recovery and with 2.5 Kg/t Na2SiO3 the copper
IV cleaner float concentrate obtained assayed 4.05% Cu with 23.8 % Cu recovery. This suggests that
with the increased dosage of depressant during cleaner flotation the copper grade increases, however, it is
seen that beyond 1.75 Kg/t Na2SiO3 the copper recovery decreases. Furthermore, it is observed that while
increasing the dosage of depressant the collector dosage also needs to be increased to keep the copper
minerals floating otherwise, presence of excess depressant lead to loss of copper in cleaner tails.
Therefore, 1.75 Kg/t Na2SiO3 is found to be the optimum depressant dosage to obtain reasonably good
copper grade and copper recovery.
In order to optimise the flotation pulp density, flotation tests were carried out under identical conditions
while varying the pulp density. It is seen that as the pulp density increases, copper recovery in rougher
float increases. The rougher float (calc.) copper grade and recoveries of the rougher flotation carried out
at ~20, 35, and 45% solids are found to be 1.2% Cu with 67.5% Cu recovery, (wt.% yield: 42.0), 1.40%
Cu with 81.0% Cu recovery, (wt.% yield: 49.4),and 0.91% Cu with 79.4% Cu recovery, (wt.% yield:
66.8), respectively. This suggests that with the increased pulp density the copper recovery increases
during rougher flotation.
The III cleaner float (calc.) copper grade and recoveries of the III cleaner flotation carried out at ~4, 13,
and 24% solids are found to be 3.12% Cu with 7.5% Cu recovery, (wt.% yield: 1.8); 2.37% Cu with
65.0% Cu recovery, (wt.% yield: 23.4); and 1.69% Cu with 52.5% Cu recovery, (wt.% yield: 23.8),
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Copper, Lead & Zinc Ores and Precious metals
respectively. This suggests that pulp density of 13% solids is found to be optimum during III cleaner
flotation stage.
The IV cleaner float copper grade and recoveries obtained at ~ 2,10 and 15% solids are found to be
3.27% Cu with 3.9% Cu recovery, (wt.% yield: 0.9); 3.62% Cu with 52.8% Cu recovery, (wt.% yield:
12.4); and 3.53% Cu with 23.5% Cu recovery, (wt.% yield: 5.1), respectively. This suggests that pulp
density of 10% solids is found to be optimum during IV cleaner flotation stage.
Hence, the medium pulp density of 35% solids during rougher flotation, and about 20, 16, 13 and 10%
solids during I to IV cleaner flotation stages is found to be optimum pulp density for maximum recovery
of copper.
The V Cleaner float (Calc.) assayed 2.86% Cu with 43.8% Cu recovery; the VI Cleaner float (Calc.)
assayed 4.22% Cu with 37.2% Cu recovery; and the VII Cleaner float obtained assayed 7.13% Cu with
31.8% Cu recovery, (Wt.% yield: 3.7). Thus, with increased cleaner flotation stages copper concentrate
with enhanced grade with reasonable recovery could be achieved.
The Copper grade and recovery during different cleaner flotation stages is illustrated in Fig.1.
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Copper, Lead & Zinc Ores and Precious metals
Final test
Copper tails
Cu Concentrate
Figure.2: Schematic flow sheet proposed for Copper recovery from copper tails sample. (Dashed arrow
applicable while closing the circuit in plant)
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Copper, Lead & Zinc Ores and Precious metals
The test was conducted under the optimized dosage of collector, supporting collector, silicate depressant
with extended cleaner flotation stages. It is inferred that by minimizing the copper loss during cleaner
flotation stages, and using optimum dosage of sodium oleate: 0.95 Kg/t, Light Diesel Oil: 3.25 kg/t;
Kerosene: 0.636 kg/t and sodium silicate: 2 Kg/t, Pine Oil: 0.02 kg/t a copper V stage cleaner float
concentrate assaying 8.00% Cu with 40.4% Cu recovery could be obtained. The weight % yield was 4.3.
The schematic flow sheet for the recovery of copper from copper tails sample is depicted in Figure.2
Cu
4. Conclusions
The objective of the investigation was to develop a flotation process flow sheet to obtain a copper pre-
concentrate of ~8% Cu for the subsequent recovery through hydrometallurgy in the Democratic Republic
of Congo.The beneficiation process evolved comprises of wet screening of the copper tailings sample
over 30 mesh to remove wood material followed by flotation of -30 mesh size of the tailings sample at
36% solids. Flotation beneficiation under optimized test conditions yielded a copper concentrate assaying
Cu: 8.0%, Al2O3: 12.78%; SiO2: 34.39%; P2O5: 3.809%; K2O: 5.43%; CaO : 4.19%; MgO : 3.31%;
TiO2: 2.0%; Fe2O3: 6.958%; S(T)1.398; and LOI: 12.06% with copper recovery of 40.4%. (Wt.% yield:
4.3).The grade of copper pre-concentrate with reasonable copper recovery as desired by the party was
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Copper, Lead & Zinc Ores and Precious metals
achieved.Mineralogical analysis of the copper concentrate reveals that the copper concentrate is diluted
by the presence of hydrophobic gangue minerals like mica, feldspar and quartz. Attempts were made to
depress the silicate gangue minerals with carboxy methyl cellulose, or excess sodium silicate, but these
reagents depressed the flotation of copper oxide minerals. However, these gangue minerals will not
interfere in the downstream hydrometallurgical processing.
Acknowledgements
The authors express their sincere thanks to Shri R.K.Sinha, Controller General (In-Charge), Indian
Bureau of Mines, Nagpur, for giving permission to present the paper.
References
G.Mudd and D.V.Boger. The ever growing case for paste and thickened tailings - towards more
sustainable mine waste management. Aust. Inst.Min. Metall.Bull., 2, 56-59, 2013.
MansousEdraki, T.Barmgantil, E.Manlapig, Dee Bradshaw, D. M. Franks, C. J .Moran, Designing mine
tailings for better environmental, social and economic outcomes: a review of alternative approaches. J. of
Cleaner Production 84, 411-420, 2014.
Indian Bureau of Mines, Mineral Processing Division’s Unpublished Report of Investigation
(IBM / NGP / R.I. No. 2048).
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Copper, Lead & Zinc Ores and Precious metals
BENCH SCALE UPGRADATION STUDIES ON A VERY LEAN COPPER ORE DEPOSIT FROM
MALANJKHAND, MADHYA PRADESH
M.G. Raut*, V.A.J. Aruna and S. M. Lal
Modern Mineral Processing laboratory & Pilot Plant, Indian Bureau of Mines, Nagpur
Corresponding author: ibmhngn@bsnl.in
Abstract
Copper is an important non-ferrous metal having wide range of applications in industries like electrical,
electronics, consumer durables , copper based alloys etc. India isdeficient in its copper resources and has
to depend upon indigenous production as well as imports. Hindustan Copper Limited a public sector
undertaking is the sole producer of copper ore in our country. The average grade of copper ore in our
country is about 0.90 to1% Cu and the main copper bearing mineral is chalcopyrite. Because of the
yawning gap between requirement and indigenous production it has become imperative to exploit very
lean copper ore deposits to meet the ever increasing demand.
This study pertains to a very lean copper ore deposit from Malanjkhand, Madhya Pradesh. The ore
assayed 0.38% Cu and contained chalcopyrite as the main copper bearing mineral. Quartz was the
predominant gangue mineral along with minor to trace amounts of other associated gangue minerals. The
process route evolved consisted of crushing and grinding followed by froth flotation of the ground
product. The reagents used were sodium isopropyl xanthate as a collector for chalcopyrite, pine oil as a
frother, lime as a pH regulator or sodium silicate as a depressant. The ore was ground to 79.5% minus 200
mesh size. The ground pulp was subjected to froth flotation at 33% pulp density using the aforesaid
reagents. The best results obtained consisted of a cleaner concentrate assaying 19.06% Cu with a recovery
of 93.6% with a weight yield of 1.87%. Alternatively by slightly modifying the reagent combination
another concentrate assaying 18.29% Cu with a recovery of 93.1% with a weight yield of 2.01% could be
obtained. The process route developed will surely pave the way for the use of very lean copper ores in our
country.
1. Introduction
Copper is an important non-ferrous base metal having wide industrial applications. Electrical/electronics
industry is by far the largest consumer of copper. Other industries which use copper are construction
industry, transport industry, consumer durables, copper based alloys such as brass and bronze. India is not
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Copper, Lead & Zinc Ores and Precious metals
self-sufficient in the resources of copper ore. In addition to domestic production of ore and concentrates,
India imports copper concentrates and ore from countries like Chile, Australia, Indonesia and Brazil. Thus
the demand of copper is met through domestic production, recycling of scrap and by imports.
Hindustan copper limited HCL, a public sector undertaking is the only producer of refined copper in our
country which utilizes both indigenous and imported concentrates as well as scrap. HCL operates the
Indian Copper Complex (ICC) in Jharkhand, the Khetri Copper Complex (KCC) in Rajasthan,
Malanjkhand Copper Project (MCP) in Madhya Pradesh and Taloja Copper Project (TCP) in
Maharashtra. Copper ore is being treated by froth flotation process. The concentrate obtained is smelted
by flash-smelting technique at Khetri and Ghatsila. Taloja Copper Project produces continuous cast wire
rods. In private sectors, the Sterlite Industries (India) Ltd., Hindalco Industries Ltd. (Birla Copper) and
Jhangdia Copper Ltd. use imported copper concentrates for their smelters.
The main ore in indigenous production is chalcopyrite and Indian deposits have an average grade of
0.90% to 1.00% Cu in them. The copper concentrates produced have an average grade of 27.00% Cu in
Madhya Pradesh, 25.00% in Jharkhand and 17.00% in Rajasthan.
4. Experimental work
Extensive test work was carried out to assess various flotation parameters including mesh of grind,
selection of collector and selection of depressant and optimization of collector quantity. The collector
sodium isopropyl xanthate and the frother pine oil were made available by HCL while the depressant
sodium silicate and pH regulator lime were made available from the local market. After carrying out
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Copper, Lead & Zinc Ores and Precious metals
extensive test work two routes were evolved which produced more or less the same results and a third
route was also tested to examine the possibility of saving in the grinding energy.
Route 1 - Test parameters:
Grinding - Feed to ball mill - 2.0 kg minus 10 mesh ore
Ball mill - 300 mm × 125 mm Denver laboratory ball mill
Ball charge - 18.2 kgs
Pulp density - 67% solids
Grind - 79.5 % minus 200 mesh
Rougher flotation - Flotation cell - 4.5 liters Denver
Pulp density - 33% solid
pH - natural, 8.0 to 8.5
Sodium silicate - 0.5 kg/ton
Conditioning time - 5 minutes
Sodium isopropyl - 20 gms/ton xanthate
Conditioning time - 1 minute
Pine oil - 15 gms/ton
Conditioning time - 1 minute
Flotation time - 2 minutes
Cleaner flotation - Feed - Rougher float
Flotation cell - 1.25 liters Denver
Pine oil - 15 gms/ton
Conditioning time - 1 minute
Flotation time - 1 minute
Cu AI Cu
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Copper, Lead & Zinc Ores and Precious metals
Route 2
The test parameters were the same as route 1 except that the use of sodium silicate was discontinued and,
lime 1.0 kg/ton was added in the ball mill during grinding. This route produced the resultsgiven in the
following table.
Cu AI Cu
Cu AI Cu
5. Conclusion
The copper concentrate (cleaner float) produced by any of the routes meets the requirement of HCL. Thus
the production of a copper flotation concentrate with satisfactory grade and recovery will surely pave the
way for utilization of very low grade copper deposits in our country.
Acknowledgements
The authors express their sincere thanks to Shri R.K.Sinha, Controller General (In-Charge), Indian
Bureau of Mines, Nagpur, for giving permission to present the paper.
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Copper, Lead & Zinc Ores and Precious metals
COMPARISION STUDIES OF GRATES AND MODIFIED GRATES ON SAG MILL
PEROFRMANCE IN THE PROCESSING OF GOLD ORE AT THE HUTTI GOLD MINES
COMPANY LIMITED
Metallurgical Department, Hutti Gold Mines Company Limited, Hutti, Karnataka, India
*Corresponding author: guruhgml@gmail.com
Abstract
This paper presents the comparison studies of grates and modified grates on sag mill performance in the
processing of gold ore. The objective of present study is to improve the performance of semi-autogenous
grinding mill by increasing the life of grates and reducing the mill breakdown time and liner cost. Sag
mill grates design & developments aim to provide good impact & wear life of grates, high production &
less breakdown. The use of large SAG (Semi-autogenous) mills in the mineral industry has been on rise
due to a significant reduction in capital and operating costs and increase in the plants throughputs. A
notable advantage of SAG mills is their flexibility in accommodating feed hardness variations. The
availability of these mills plays an important role in the economics of the operation. One of the main
reasons for mills down time is the time required to change worn or broken liners. Monitoring the
progressive wear of grates and relating this to the performance of the mill are presented in this study. The
value of wear monitoring in ongoing liner optimization and cost saving, through balancing the lives of the
grates and providing reliable comparative data for testing different liner materials and designs, is
explained. Liner design needs to respond to the process aspects of mill liner action that are critical to good
SAG mill performance, i.e., the impact of shell liners on the grinding action and the grates and pulp lifters
on pulp discharge. In recent years, the trends in large SAG mills has been to use lifter grates, primarily to
reduce liner damages, and to use large, hence fewer, mill liner parts to reduce downtime at liner change-
outs. Based on the results obtained from the comparison studies of grates and modified grates on sag mill
performance, it can be observed that by installation of modified grates, SAG mill production increased,
re-circulation load reduced, grates life doubled, breakdown time decreased by 50% and cost savings in
liner procurement and re-lining occured.
Keywords: Sag mill, grates & modified grates, wear rate, tonnage & circulating load.
1. Introduction
Semi-autogenous grinding mills (SAG mills) are tumbling mills that most commonly have a shell
diameter-to-length ratio of around two. With this high aspect ratio, SAG mills generate both thrown and
cascading ball-milling actions with shell linings shaped to lift and to throw alloy steel grinding balls of up
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Copper, Lead & Zinc Ores and Precious metals
to 150 mm (6 in.) in diameter. These actions apply crushing, attrition and abrasion comminution
processes to reduce primary-crushed ores down to ball-mill sized feed. SAG mills are currently the
technology of choice in hard rock milling operations for reducing primary-crushed ore to ball mill feed.
Mill liners provide the replaceable wear-resistant surface within grinding mills; they also impart the
grinding action to the mill charge, and at the discharge end, remove the ground contents of the mill. In
recent years, as SAG mills have grown in size, the process aspects of liner design and their impact on mill
performance have become particularly important. Grates play an important role in sag mill
performance/throughput as it allows the controlled passage of slurry and pebbles from the charge inside
the mill into the pulp-lifter chamber. . For the efficient and effective performance of sag mill, grates
proper design is very important. Poor grates design has a detrimental effect on milling performance and
on grates life, (Powell 1991a).
This results in a loss of revenue and increased operational costs. Reduced milling efficiency can result in
excess power usage and decreased recovery of the valuable minerals. Excess grates wear results in
exorbitant grates materials costs, and excessive downtime which reduces mill availability and impacts on
plant throughput. For a plant with a number of mills this also entails the employment of extra mill relining
staff and the risks and costs associated with frequent relining. Optimised liner design can be used to strike
the best economic balance between liner life and mill grinding performance, thus enhancing the
profitability of a mining operation. Liners were treated merely as a cost overhead, and a cause of
downtime, and the maintenance approach has been to reduce the cost, while remaining within acceptable
downtime constraints. Costs saving lead to the development of profile grates with lifters, as these
dramatically increase the life of the grates. The downtime constraints and high stresses in large SAG mills
helped to drive the development of greatly improved grates materials. SAG mills running in single stream
circuits, it became apparent to the operating staff that the liner having a significant influence on mill
performance. However, the gains to be had through good liner design and selection are just as great as on
the large SAG mill. The Hutti Gold Mines grinding circuit comprises a SABC circuit with a single SAG
and Ball mill in closed circuit with cyclones. Pebble crusher treats the SAG mill discharge screen (+)
12mm oversize material. The crushed product is combined with the SAG mill feed. The slurry (-) 12 mm
from the underflow of the screen is pumped into a cyclone cluster for classification, 2/3 of cyclone
underflow feeds into wet overflow type ball mill for further grinding, the remaining 1/3 of the underflow
from hydrocyclone will be fed into the gravity concentrator to recover free roastable gold concentrate.
The concentrate is passed through a shaking table to separate the free gold. The concentrate obtained from
the shaking table is subjected for roasting & smelting to obtain saleable bullion. The grinding circuit at
HGML is shown in Figure 1.
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Copper, Lead & Zinc Ores and Precious metals
2. Materials and methods
After mill commissioning a number of problems appeared including a serious discharge grate failure,
pegging problem resulting in throughput reductions and mill overloads. While alternative grate designs
with different chemical composition were sourced and fabricated. Three different grates were tested. The
selection of the material of construction is a function of the application, abrasivity of ore, size of mill,
corrosion environment, size of balls, mill speed, etc. liner design and material of construction are integral
and cannot be chosen in isolation. The chemical composition and hardness of grates are given in table 1.
The discharge grate design chosen incorporated design features is developed by the vendors. These
features included the use of plain grates with 20 No’s 20 mm slotted grates, and other 20 No’s of 50 mm
pebble port type were installed during commissioning. Later each 20 No’s 20 mm slotted and 50 mm
pebble port lifter type( “top hat” design) grates to protect the grates from balls and material impact were
installed.
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Copper, Lead & Zinc Ores and Precious metals
shear work for the front and top faces but predicts much lower wear on the liner and the rear face. The
impact damage on the grates is also estimated using two different measures. The first is the energy
dissipated in the normal direction during collisions between the particles and the liner. The second is a
measure of excess kinetic energy of impact. Low speed collisions which are large in number but of
limited importance for damage make no contribution to the damage estimate, but high speed collisions do
much more damage because of the quadratic dependence on speed. The distributions are quite different to
those of the normal stress distributions. In particular, the wear is substantially higher across the entire top
of the grates with peaks near the corners. There is little impact damage on either front or back faces. The
impact damage measure is shown on the surface of the grates in Figure 2 (b).The Influence of Grates
Wear Rate on Sag Mill Performance is given in table 2 and figure 3.From the results obtained it has been
observed that wear rate of manganese steel grates are much faster than chrome moly. Chrome Moly grates
performed better in terms of life, tonnage and power consumed. The actual erosion rates, however, is
dependent on the material properties of the liner and its resistance to impact and abrasion damage. High
quality steel might be expected to be very resistant to impact and erode predominantly by abrasion.
Ultimately, it will be a combination of an impact and an abrasion measure weighted by the resistance of
the liner material to each damage mechanism.
3.2 Influence of plain grates and modified grates on SAG mill performance
It is well known that the height of the grates lifter directly influences the life of the grates as whole - the
higher the lifter height the lower the wear rate of the liner. The trade-off is in mill production, which
drops as the lifter height is increased above an optimal height. In assessing the wear of grates it is useful
to monitor the wear of the lifter height. This can be used to assess the useful operating height of the grates
lifter. In work conducted on monitoring the wear of grates this measure provided a direct correlation
between lifter height and grates wear, (Powell 1991a). This is illustrated in Figure 3 which shows grates
wear rate increases fast when the lifters height were worn/decreased from 100 mm to 20 mm. This is
because the direct impact/abrasion of particles and grinding media on grates. This dramatic change clearly
showed that the grates lifters plays important role in grates life and sag mill performance. The onset of
accelerated grates wear can also be used to give a reliable indication of when slip of the charge on the
grates begins to occur, with the resultant reduction in milling efficiency. Whether the grates lifter is
removable or integral to the liner, this is an essential piece of data in optimising the life and cost of liners.
Ideally the grates lifter and grates plate should wear to minimum productivity height and safe thickness
simultaneously. This prevents the scrapping of excess unworn liner and losses in mill throughput. Grates
Lifters not only consumables for protection against wear, but also critical machine elements. The
attainment of expected useful life of a set of lifter depend not only on their initial shape, material and
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Copper, Lead & Zinc Ores and Precious metals
quality of fabrication but a matching between expected and real operating conditions inside the mill. The
main issue is the direct impact of balls on the lifters in the absence of the damping effect of bed mineral
ore and ball charge. Comparative study of plain and modified grates on sag mill performance indicates
that grates with lifters has great impact on liner wear and sag mill performance as they effects the
grinding kinetics of the mill. The results of effect of modified grates on sag mill performance are
presented in table 3 and fig 4. From the results obtained it has been observed that life of sag mill
discharge grates increased drastically, it is doubled, reduced the downtime of sag mill and simultaneously
increased the production of mill.
4. Cost analysis
a) Estimated Cost for fixing of Discharge End Grates in SAG Mill is given below:
Description Quantity/ Total Cost/Price
Days in INR
1.Cost of Plain Grates along with hardware replaced in a year (Cost of 4 Sets 1,05,64,000.00
one set along with hardware: Rs 26,41,000.00)
2.Incentive of Relining for Discharge end Grates (4 Times) 12 Days 4,36,000.00
(Cost per Re-lining : Rs 1,09,000/-) (3 Days per Set)
3.Cost of Down Time for replacing the Discharge End Plain Grates 12 Days 11,04,00,000.00
(4 Times) (Milling/day*recovery grade=Production)
4.Total Cost 12,14,00,000.00
b) Estimated Cost for fixing of Discharge End Modified Grates in SAG Mill is given below:
Description Quantity/ Total Cost/Price
Days in INR
1.Cost of Modified Grates along with hardware replaced in a year 2 Sets 60,43,400.00
(Cost of one complete set along with hardware : Rs 30,21,700.00)
2.Incentive of Relining for Modified Grates ( 2 Times) in a year 06 Days 2,18,000.00
(Cost per Re-lining : Rs 1,09,000/-)(3 Days per set)
3.Cost of Down Time for replacing the Modified Grates 06 Days 05,52,00000.00
(2 Times) (Milling/day*recovery grade=Production)
4.Total Cost 06,14,61,400.00
5. Conclusions
Based on the results obtained from the comparison studies of grates and modified grates on Sag mill
performance the following conclusions are made.
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Copper, Lead & Zinc Ores and Precious metals
• Virtually eliminated downtime of SAG Mill
Since the installation of modified grates sag mill downtime time for re-lining of grates decreased
by 50% .i.e. from 240hrs to 120hrs
• Increased grinding of critical size particle in the SAG Mill.
Immediately after installation of modified grates it has been noticed that less pebbles being
recycled to the pebble crusher. This suggested more grinding of critical sized particle in the Sag
mill. Which resulted in energy save for crushing critical sized particles.
• Increased Grates life.
Measurements and calculations done on both plain and modified grates reveal that modified grates
life increased to double that of plain grates. Life of plain grates was 1500 hrs whereas of modified
grates is 3500hrs. Steel Loss due to liner wear per day decreased from 65 kgs/day for plain grates
to 45kgs/day for modified grates.
Increased Sag Mill Production
Due to installation of modified grates Sag mill production increased to 12,000 MT per annuam.
The increased production of 12,000 tons translates to 24,000 grams of incremental gold
production. This amounts to 5, 52, 00,000 incremental revenue increase at a gold price of 23,000
per 10 gram per annum.
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Copper, Lead & Zinc Ores and Precious metals
4000
3500
3000
LIFE OF 2500
Polymetal
2000
LINERS Cr-Mo
1500
Mn-Steel
1000
500
0
2010 2011 2012 2013 2014
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Copper, Lead & Zinc Ores and Precious metals
Table 2: Influence of Grates Wear Rates on Sag Mill Performance.
Chrome-Moly Manganese Steel
Life,Hrs Tonnage,MT Tonnage Rate,tph Power,Kw/Mt Life,Hrs Tonnage,MT Tonnage Rate,tph Power,Kw/Mt
1451 120794 83.25 35 1305 89808 68.82 40
1511 132161 87.47 34 1439 119704 83.19 35
2048 172122 84.05 35 1344 118562 83.25 36
2725 238456 87.51 37 592 52287 88.32 37
3835 326524 85.14 39 1626 119140 73.44 41
3611 311078 86.15 40 1868 145189 77.72 40
Table 3: Influence of Plain and Modified Grates on Sag Mill Performance.
PLAIN
Chrome-Moly
GRATES MODIFIED
Chrome-Moly
GRATES
Life,Hrs Tonnage,MT Tonnage Rate,tph Power,Kw/Mt Life,Hrs Tonnage,MT Tonnage Rate,tph Power,Kw/Mt
1451 120794 83.25 35 2725 238456 87.51 37
1511 132161 87.47 34 3835 326524 85.14 39
2048 172122 84.05 35 3611 311078 86.15 40
Acknowledgements
We are highly indebted to Sri Monappa, IAS, Managing Director, for providing us the golden opportunity
to present the technical papers and to attend the International seminar MPT-2016, Pune. With great
pleasure, we take this opportunity to express our deep gratitude and reverence to Sri A.R.Walmiki
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Copper, Lead & Zinc Ores and Precious metals
Executive Director, Dr. P. Sangurmath G.M (Co-Ord) and Sri.C.R.Ravi Dy.General Manger (Met), for
permitting to attend the seminar.
References
R Morrell, S., Morrison, R., 1996, AG and SAG Mill Circuit, Selection and Design by Simulation, SAG
1996, Vancouver, Canada.
Morrell, S., Stephenson, I., 1996, Slurry Discharge Capacity of Autogenous and Semi-autogenous Mills
and the Effect of Grate Design,
Royston, D., 2000, “Grate and pulp-lifter interaction in SAG/AG mills,” Seventh Mill Operators’
Conference, AusIMM, 12-14 October, Kalgoorlie, WA, Australia, pp. 63-67.
Napier-Munn T.J., Morrell, S., Morrison, R.D., and Kojovic, T., 1996, “Mineral comminution circuits
their operation and optimization,” JKMRC Monograph Series in Mining and Mineral Processing, Julius
Kruttschnitt Mineral Research Centre, Indooroopilly, Qld., Vol. 2, Chap. 7.
Powell, M.S. 1991a. The effect of liner design on the motion of the outer grinding media in a rotary mill.
International Journal Mineral Processing 31: 163-193.
Cleary, P.W. 1998a. Predicting charge motion, power draft, segration, wear and particle breakage in
tumbling mills using discrete element methods, Minerals Engineering, 11: 1061-1080.
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242
Copper, Lead & Zinc Ores and Precious metals
THE STUDIES OF DETERMINATION OF GRINDING TIME ON ROUGHER FLOTATION ON
RANGIN FLEZ COPPER CONCENTRATION PLANT
A. Pazoki* and A. Pourbahaadini
Department of Mining Engineering, Lorestan University, Lorestan, Iran
*Corresponding author: a_pazoki@yahoo.com
Abstract
Flotation is the most important way of sulphidic copper beneficiation and crushing is an important and
inseparable part of the process. The purpose of this research is to study the effect of grinding time on
rougher flotation of copper in Rangin Flez copper plant. Optimization of this parameter is necessary to
decrease the costs of operation. Crushing and grinding are done to achieve desired grade and recovery,
after study of different factors, like pH and consumption of reagents, in the existing plant conditions. And
others parameters like pulp density, impeller speed, and flotation time in all of the tests have been kept
constant. Results show that the best results are produced with grinding time of 18 minutes but better
recovery is at 16 minutes. Based on the condition of operations and economics of industries, 16 minutes
have been chosen as the best time for grinding. Also to increase the grade and recovery, it is suggested to
use better depressants and optimize the reagents and operation parameters.
1. Introduction
The general practice copper processing is recovery of sulphide minerals by flotation method. Flotation is
an effective process for increasing the assay, and recovery of minerals and it is industrial practice
(Talvardi, 2006). Flotation is selective process as it can be observed from results with good grade and less
gangue minerals mineral based on it, this research have been taken up to consider the effect of grinding
time on flotation the rougher cells of Rangin Flez copper processing plant which is 40 km away from NE
of Shahrbabak in the SE of Iran that is nearby Meiduk copper mine. The feed could be provided from
Meiduk mine, it has different mineral processing plant of copper concentration compared to Meiduk
concentration factory. Lines of ore crushing, the models of crushing equipment, chemical reagents that
are used and the type of concentration cells in this factory are the most important difference.
Moazemi et al. (2014) in their study of Meiduk concentration plant optimized concentration assay to 2.94
and 90.8% recovery. Ghodrati et al. (2011), just with optimized the density of chemical materials in
flotation of Shahrbabak copper have arrived to 1.31% recovery.
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Copper, Lead & Zinc Ores and Precious metals
Lime Bai and coworkers (2012) in their studies on flotation of chalcopyrite, have arrived to 92%
recovery. Arana and coworkers (2010) have considered flotation of chalcopyrite with silicon hydrophobic
waste and have arrived to 92.4% recovery.
2. Sample preparation
To prepare the representative sample, sampling is done in time interval with every ten minutes and more
than 200kg of sample have been collected. Then the sample was subjected to further crushing by jaw
crusher and cone crusher and the crushed sample was sieved on 1.4mm sieve. The product has been
mixed thoroughly to homogenize, then the samples have been subjected for refilling to get each batch of
one kg with use of riffle sampler. For mineralogical studies, 40 manual samples of 10 mesh size are
collected and ground to 75-1000 micron range, thin sections have been prepared for mineralogical studies
with use of polarizing dual-purpose microscope (MEIJI). Summary of mineralogy study results is
available in table 1.
No. Result
Basically the gangue minerals are cericite, quartz and pyrite. A long with a minor amount of
1
epidote, potassium, Feldespate and traces of magnetite with copper ore.
More than 95% of pyrite grains are in the form of opaque mineral phase, It is observed that
2
ore minerals in the polished section are in coarse form
3 Less than 5% of cooper ore has been identify in opaque phases
In the copper phase less of chalcopyrite in the range of 50 to 150 micron and more in the
4 range of 500 micron. The presence of pyrite is negligible even under the microscope hardly
we can observe these mineral.
The primary and free copper mineral in the polished section is in the range of 250 micron,
5 could be observed that the percentage of liberation in this size fraction of copper is about
60%.
Approximately all the minerals in copper phase, in the size fraction of 75 micron are
6
liberated. The percentage of liberation in this size fraction is about 99%.
7 Mineralogical studies shows that the texture, of host rock and alterated rock are different.
To identify the minerals in the sample and also to determine amounts of metal elements and different
oxide compounds available in sample, XRD and XRF analysis have been done and the results are shown
in table 2.
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Table 2: Result of XRD and XRF.
The type of reagents used and their amounts is same as the condition of factory. To achieve maximum
recovery, skimming has been done till that froth is loaded. Concentrate and tailings of respective
floatation test are collected and dried, and weighed to determine weight percentage. Some of the test
conditions are illustrated in table 3.
Parameter Quantity
Pulp density 25 %
Impeller speed 1200 rpm
Collector (SIPX) 30 g/t
Frother (MIBC) 60 g/t
Time pH F c t R S.E
12 10 0.77 3.52 0.13 86.304 69.231
14 10 0.77 3.58 0.13 86.249 69.488
16 10 0.77 3.71 0.12 87.237 71.115
18 10 0.77 4.3 0.12 86.839 73.114
20 10 0.77 3.8 0.13 86.061 70.356
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Copper, Lead & Zinc Ores and Precious metals
Figure 1 shows provided assays in terms of different times of crushing.
(1)
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Copper, Lead & Zinc Ores and Precious metals
Where c, f, t respectively are stand for concentrate assay, feed assay and tailings assay. Results obtained
from calculation of separation proficiency in different grinding time intervals are shown in figure 2.
(2)
In figure 4 and 5 respectively the relation of grinding time with separation efficiency and assay, and
relation with grinding time on recovery and separation efficiency have been shown.
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Copper, Lead & Zinc Ores and Precious metals
5. Conclusions
From the results we can find that to increase grade it is necessary to increase grinding time which
increases the degree of liberation to more than 18 minutes that leads to generation of fines, which may
create slimes in floatation process, ultimately which creates problem in separation of ore and gangue
minerals particles in concentrate phase. The separation proficiency has a high convergence with assay and
the most convergence is in crushing times 16 and 18 minutes. As it is seen, liberation proficiency
increases when grinding time arrive to 18 but after this time it decreases. Although the effect of time on
recovery is low with the present condition but the more recovery in grinding time of 16 minutes is seen
and even this slight increase of recovery is so important for the owners of industry. The low effect of
grinding time on recovery could be due to this reality that more grinding causes increase in the specific
surface area of material and increase the need of more reagents. According to the results, selection of the
16 and 18 minutes grinding time for optimized grinding seem to be suitable and the importance of
grinding costs in making the operation more economical, and selection of 16 minute for grinding is more
suitable. To increase the liberation efficiency in this grinding time, use of optimized reagents quantity and
suitable depressant are the suggestions.
References
V.A.J. Aruna, S.N. Goswami, P.R. Bawane, Mohan Ram and C.S. Gundewar. ENHANCING
CHALCOPYRITE FLOTATION BY TACKLING HYDROPHOBIC SILICATE GANGUE. Proceedings
of the XI International Seminar on Mineral Processing Technology (MPT-2010) NML Jamshedpur, pp.
216–222, 2010.
L. Bai, Y. Han, Z. Yuan and G. Li. Study on Different Depressants to Influence on Chalcopyrite
Flotation. Advanced Materials Research Vol. 454 (2012) pp 337-341, 2012.
248
Copper, Lead & Zinc Ores and Precious metals
S. Ghodrati, M. Abdollahi, M. J. Koleini and M. Hekmati. Optimization of the chemical reagent in
proposed of increasing recovery in meiduk copper plant. 30th national conference, geological survey Iran,
Tehran, Iran, 2010.
M. A. Talvardi. The application of column flotation on concentration plant of lead-zinc anguran circuit.
national conference of mining, Iran,. feb, 2006.
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Copper, Lead & Zinc Ores and Precious metals
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Abstract
Due to lack of full availability of river sand for mine back fill, environmental effect of surface tailing
impoundment, an attempt was made to study the amenability of CIP plant tails to pelletization producing
granules – micro pellets of 3 mm mean size [<5mm ], 2 kg/cm2 compression strength and drop number
>10 for reuse as mine back fill. Tests were done in a disc pelletizer varying rpm, angle of inclination,
cement [OPC] binder %. The amenability tests indicated that micro pellets meeting the specification
could be produced at low feed quantity, high angle of inclination of 60o, low rpm of 25, 10% 1:1 mix of
cement and anhydrous gypsum as binder and 10-11% moisture, at low feed quantity. The granulation
amenability tests indicate the possibility of finding a tangible solution for mine back fill and vexed
problem associated with CIP tail dumps.
Keywords: CIP tails, granulation, cold bonded pelletization, micro pellets, mine back fill.
1. Introduction
Hutti Gold Mine Company Limited [HGML] is the state government undertaking and is the sole primary
gold producer in our country. HGML mines the gold ore at Hutti, Hira-Budini and Uti and treats its
captive plant with 0.5 million tons capacity. The process comprises of conventional crushing/semi
autogenous milling of ROM, grinding the SAG-crusher fines in ball mill cyclone circuit, coarse gold
recovery of mill discharge through centrifugal gravity concentrators, thickening, cyanidation in Dorr
agitators, carbon loading of dissolved gold in CIP tanks, screening to collect gold loaded carbon,
treatment of CIP tails for removal of free cyanide, discharge of cyno killed tails to tailing pond. The gold
from loaded carbon is electrolytically won and the gravity gold and gold from electrolysis is melted into
bars which are released to local market. It is estimated that more than 50 million tons of tails are stacked
around Hutti. Further, the mines stopes has to be backfilled as mine safety steps. The quantum of sand
from tails is meager due to tail’s fine granulometry and large quantum of river sand had to be used. Due
to stringent environmental regulations for mining of sand from river beds, the availability of sand for sand
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stowing is limited. Also the environmental impacts of acid mine rock drainage is well documented by
Ritcy (1989) and HGML is no exception as contamination of subsurface waters with toxic arsenic, base
metal salts, sulfates is slowly on the rise despite following stringent control measures.
In industrialized countries, issues pertaining to environmental regulatory compliance have become the
impetus for comprehensive engineering design and effective management of mining, other wastes and
industrial by-products. This has resulted in a renewed interest within the mining industry to explore and
evaluate innovative strategies for managing potentially acid generating mining waste besides to backfill
mined empty stopes by tails. Contrary to the conventional thickened tailings for surface disposal
applications, binder agents impart chemical stabilization and physical solidification of cemented paste
tails [CPT]. This approach is particularly beneficial for environmentally protected disposal of sulphide
mine waste because it can minimize (depending on the binder) the subsequent mobilization of potentially
toxic heavy metals and arsenic (As). A. Tariq and E.K. Yanful (2013) reviewed the role of binders for
CPT as mine backfill and recommended use of cement kiln dust, fly ash in addition to cement for
cemented paste backfill [CPB] and it is gaining importance Annon (2012). Alternatively, a mix or
standalone of granulated tails with binders like cement, granulated blast furnace slag sand, granulated fly
ash is being investigated to solve the vexed problem of mine back fill, acid mine drainage and
contamination of sub surface waters by heavy metals. In view of the above, about 25 kgs of tails were
received from HGML to study the granulation of tails for subsequent use in mine back fill. The objective
of the present study was to study the granulation of HGML CIP dry tails. The agglomerate shall have size
range from 0.2 to 5 mm with mean size of 3 mm. The agglomerates should have a minimum drop number
of 10 and a compressive strength of 2 kg/cm2. Such agglomerates mixed with granulated slag sand, fly
ash, may be used as back fill should be pumpable during hydraulic back filling.
2. Experimental
2.1 Materials
The materials consist of CIP tails, ordinary port land cement [OPC] and anhydrous gypsum [CaSO4] of -
100 mesh [-0.15mm].
2.2 Equipment
600 mm dia disc pelletize of M/s MPE Co Ltd. Mumbai was used for granulating.
2.3 Method
The as received sample was dried and subjected to standard sampling methods and stored in 16 plastic
bags. The standard granulation / pelletizaton method as enumerated by the manufacturer and hand books
was followed. The micro pellet / granulated product was subjected standard tests for determining %
moisture after drying, strengths, drop tests and size analysis after curing the pellets for 72 hours. During
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the pelletization experiments, the choice of binder, binder dosage, effect of machine parameters like rpm
and inclination were studied. The optimum condition products were sent to HGML for their review.
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3.4 Effect of combination of binders
With regard to the aforementioned statistics, PC appears to be the most expensive component of
operations and hence becomes the primary setback in its use as a sole binder. A. Tariq and E.K. Yanful
(2013) reviewed the role of binders for CPT as mine backfill and recommended use of cement kiln dust,
fly ash in addition to cement for cemented paste backfill [CPB]. Peyronnard and Benzaazoua (2011) have
tested waste gypsum as hydration activator for cemented mine backfill applications and found that 4.5
wt% binder (42% PC 40% waste glass 18% anhydrite) mixed with mining waste can produce a monolith
with UCS of 0.6 MPa after 14 days of curing. In view of the above ratio of OPC with anhydrous gypsum
was varied from 0.50 and 80% keeping total binder consumption at maximum level of 10%. The results
are given in Table 4. The results indicate that the dilution of cement binder with anhydrous gypsum
reduced the drop number and quality was affected significantly when the OPC - anhydrous gypsum ratio
was less than 1. The overall OPC consumption was 5%.
4. Conclusions
Dried CIP tails sample from HGML was subjected to limited granulation studies using OPC, anhydrous
gypsum as binder in a laboratory disc pelletizer with the aim of producing the agglomerate with size
range from 0.2 to 5 mm [mean size of 3 mm] and having minimum drop number of 10 and a compressive
strength of 2 kg/cm2. The preliminary amenability granulation tests indicated that [1] the sample is
amenable as granules – micro pellets meeting the requirements and was obtained at low feed quantity,
high angle of inclination of 60o, low rpm of 25, 10%OPC as binder and 10-11% moisture [2]. Micro
pellets – granules meeting the specification was obtained under above conditions even by using 10 kg/t of
1:1 mix of OPC and anhydrous gypsum. Detailed test works using diverse binders and mix of granulated
slag powder are recommended for use as mine back fill. Paste mine back fill tests are also recommended
as a progressive alternative.
References
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1. Amjad Tariq, Ernest K. Yanful (2013), “A review of binders used in cemented paste tailings for
underground and surface disposal practices”, J. Env. Management, 131, PP 138-149.
2. Pratiksha Pandey, Naveen F Lobo, Prasanna Kumar (2012), “Optimization of Disc Parameters
Producing More Suitable Size Range of Green Pellets”, I. J. Met.Engg., 1(4):PP 48-59.
3. Peyronnard, O., Benzaazoua, M. (2011), “ Estimation of the cementitious properties of various
industrial by-products for applications requiring low mechanical strength”, Resour. Conserv.
Recycl. 56, PP 22-33.
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ENVIRONMENTAL POLLUTION AND FORMING OF KERMANSHAH OPHIOLITIC
COMPLEX (WEST OF IRAN)
Abstract
Ophiolites of the Zagros orogenic belt of Iran are part of the Tethys ophiolites, linking the Middle East
ophiolites and other Asian ophiolites (e.g., Pakistani and Tibetan) to the Mediterranean ophiolites (e.g.,
Troodos, Greek, and East European) due to their geographical position. The nature of Harsin–Sahneh
ophiolite (Kermanshah), studied in this paper, is traditionally considered as one of the Mesozoic southern
branch of the Neo-Tethys Ocean, and remnants of the Peri-Arabic ophiolite system abducted onto Arabian
shield (Gondwana).
To determine and estimate the environmental impacts of certain elements, 10 soil samples from various areas
in these massifs have been investigated. The obtained results show that most of heavy and major elements
were exceeding the permissible levels in soil samples in the study area. On the subject of soil quality,
concentrations of elements Cr, Mn, Fe, Ca, Mg, Ca, Ni, and Zn are above permissible levels. Comparing the
concentrations of elements with results of grain size analysis illustrates that the concentrations of Cr, Ni, Fe,
Mg, and Co are positively correlated with sand fraction and the concentrations of Al, P, Mn, and Pb are
directly proportional with clay fraction in soil samples.
Petrographic evidence indicates that this ophiolitic sequence consists of both mantle and crustal suites. In this
complex, generally lithologies include harzburgitic and lherzolitic peridotites, isotropic and mylonitic
gabbros, dyke complex, basaltic pillow lavas, and small out crop of plagiogranite. The mineral chemistry of
Harsin mafic rocks is island arc setting for this part of complex and geochemistry of mafic and ultramafic
rocks of Sahneh region displaying P-type mid-ocean ridge basalt (MORB) nature.
The presence of basalts with different compositions in this region can be interpreted as the interaction
between MORB-type and OIA-type asthenosphere. Field relationships and geochemical evidence indicate
that involved ophiolites were part of a rifted basin at the ocean–continent transition zone formed in the south
of the Neo-Tethyan Ocean.
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Based on evidence, in Late Cretaceous, the subduction of Southern Neo-Tethyan Ocean beneath itself leads
to not only the cessation of Southern Neo-Tethyan subduction to the branch of Sanandaj–Sirjan block but
also the formation of arc and back arc basin and related rocks in Kermanshah ophiolite. MORB magmatism
occurred in the response to slowing down of the convergence rate of Neo-Tethyan and slab retreat in the
Eurasian continental margin. This would also explain both the contemporaneous occurrence of MORB-type
and OIB-type magmatism, as well as the lack of a magmatic evolution from depleted to enriched rocks.
Keywords: Environmental impact, heavy elements, tethyan ophiolites, arc magmatism, p-type MORB,
zagros
1. Introduction
During the last years, various studies on Tethyan ophiolites have improved our comprehension of the various
geodynamic environments in which these ophiolites were born. Peri-Arabic ophiolites, 3000 km long, formed
Cretaceous ophiolites, which cover an area from Oman to northwestern Syria, Cyprus, and Antalya abducted
over the Arabic–Tauric platform. Southern ophiolites of Iran which cropping out along Main Zagros Thrust
Zone, are part of the the “Peri-Arabic ophiolitic crescent” which recorded evolved geodynamic of Southern
Neo-Tethys Ocean located between Arabian shield (Gondwana) and Sanandaj–Sirjan continental block
(Allahyari et al. 2010; Agard et al. 2011).
Generally three major tectonic elements, Zagros fold-thrust belt, the Sanandaj–Sirjan Zone, and the
Urumieh–Dokhtar magmatic arc in western and south western parts of Iran, are recognized as being related to
the subduction of Southern Neo-Tethyan oceanic crust and the collision of the Arabian plate with the central
Iran micro plate. The Urumieh–Dokhtar Magmatic Arc (UDMA) consists of intrusive and extrusive rocks of
Eocene–Quaternary age that forms a zone 50 km wide and up to 4 km thick.
Sanandaj–Sirjan Zone (SSZ) contains the metamorphic core of the Zagros continental collision zone in
western Iran. SSZ has the length of 1500 km and the width up to 200 km from northwest to southeast of Iran
(Mohajjel et al. 2003). The subduction inception of the different parts of Southern Neo-Tethyan oceanic crust
beneath the SSZ dates back to the Late Triassic to Late Cretaceous. Harsin–Sahneh ophiolites (Fig. 1a), with
a NW–SE trend, is located between SSZ in the northeast and Bisitoun limestones and Kermanshah radiolarite
in the southwest. These ophiolites were thrust over an Arabic platform during Maastrichtian to Paleocene.
Heavy and trace metal contamination of soils is one of the important concerns in environmental issues.
Natural weathering processes in soils, alike to the formation of secondary minerals or organic
2
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degradation/mineralization, have a profound effect on the mobility and bioavailability of trace metals
(Ventura et al. 2012). Ultramafic parent materials (e.g. serpentinite) are associated with high levels of toxic
trace elements, particularly nickel, chromium, cobalt, zinc, mercury, and lead. Such regions are therefore
generally not suitable for agriculture (Sarikhani et al. 2014). Soils developed over serpentine showed the
highest metal concentrations (Miati et al. 2013). The serpentine soils are more enriched in Mg and Fe due to
weathering of some specific minerals existing in such geologic environments (e.g., forsterite, fayalite, and
serpentines). It has been proved that high concentrations of some elements such as Cr and Ni are due to
presence of ultramafic rocks, development of soils over them and also leachate, and loss of mobile elements
from soil profiles.
2. Geological setting
The southern Iranian ophiolites that located along the Main Zagros Thrust Zone recorded the geodynamic
evolution of southern Neo-Tethys oceanic branch between the Arabian shield (Gondwana) and the Sanandaj–
Sirjan continental block of Iran. Harsin–Sahneh ophiolites with 34º 00´ N to 34º 30´ N and 47º 10´ E to 47º
50´ E coordinates are located along the Main Zagros Thrust (between the Zagros belt and the SSZ; Fig. 1b).
Harsin–Sahneh ophiolites consists of both mantle and crustal suites, include peridotite (harzburgite and
lherzolite), serpentinited peridotite, gabbro (isotropic and mylonitic gabbros), dyke complex, and basaltic
pillow lavas; dyke and pillow lava complexes are limited to Tamark and Gashor areas (between Harsin and
Nurabad; Fig. 1a).The Kermanshah ophiolite was first considered to be a mid-ocean ridge remnant analogous
to those of Oman and Neyriz (Ricou 1971). Delaloye and Desmons (1980) suggested the age of the diorites
as 86.3 ± 7.8 Ma (i.e., Campanian), while Whitechurch et al. (2013) estimated it as 58 ± 9 Ma. These diorites
cut the volcanic rocks and flyshic sediment (located along the Gamasiab River). Field evidence indicates that
peridotites and intrusive ultramafic and gabbroic rocks mainly crop out between Harsin and Sahneh, along
the Gamasiab River.
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Figure 1: (a) Geological map of the Harsin-Sahneh ophiolite complex (modified after Saccani et al. 2013).
(b) Structural sketch map of the Iran and position of Harsin-Sahneh (K) ophiolite complex (modified after
Allahyari et al. 2014).
They characterized Harsin–Sahneh domain as a mélange with ophiolitic fragments. No sedimentary cover
stratigraphically overlying the various ophiolitic rocks is observed in the Kermanshah area. Although some
radiolarite layers are interbedded between the pillow basalts of the Gashor unit and around Harsin, the
limestones directly overlying serpentinites were dated as Upper Triassic, while the limestones resting on
radiolarites overlying the same serpentinites were dated as Malm. The serpentinised peridotites are
4
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considered to be mantle material exhumed during the Early Mesozoic break-up of the Neo-Tethyan Ocean
(Wrobel-Daveau et al. 2010).
3. Petrographic description
3.1 Pridotite
The lowest lithological unit begins with mantle pridotites. Pridotites occurred between Harsin–Sahneh
regions (Fig. 2a). Dunites are not volumetrically most abundant rock in the ultramafic sequence. Lherzolites
show a porphyry texture. Both pyroxenes show exsolution lamellae along cleavage (Fig. 2b) and kink
banding. Cr-spinel crystals in peridotite samples are sub-anhedral (Fig. 2c). In some areas, the peridotite
samples have been pervasively altered (serpentinized) to a mixture of lizardite, chrysotile, and brucite; the
extensive alteration of peridotite has led to the development of mesh texture (Fig. 2d). In some samples,
orthopyroxene (enstatite) is forming asymmetrical kinking and double-hinge disharmonic micro-folds (Fig.
2e).
3.2 Gabbro
The coarse-grained gabbros show ad-to mesocumulate texture with large crystals of plagioclase (50–60%)
clinopyroxene (20–30%) and olivine (10–20%) (Fig. 2f). Mylonitic gabbros are generally coarse grained with
mylonitic texture (occurred between Shoveh valley and Garoos valley). These gabbros occasionally and
locally affected by alteration; the secondary minerals are mainly actinolite, tremolite, and epidote. In some
samples, scarce clinopyroxene relics are locally preserved, while in other samples porphyroblasts are
composed of plagioclase, clinopyroxene, and locally olivine (Fig. 2g).
The dykes occur between Harsin and Sahneh, crosscutting harzburgites and gabbros. No true sheeted dyke
complex exists in the Harsin–Sahneh ophiolites. The texture of the dykes is fine grained and intersertal; the
mineral assemblage (e.g., epidote, albite, zeolite, or calcite) depends on the degree of hydrothermal
alteration. Pillow basalts display aphyric, fine-grained intergranular and/or sub-ophitic textures. Like dyke
samples, the development of the typical mineral assemblage indicate the low degree of hydrothermal
alteration conditions (Fig. 2i).
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4. Results
4.1 Soil contamination
Table 1 illustrates the analyzed concentration of elements in 10 soil samples. The relationships of the studied
elements with each other and also soil particle fractions were determined by calculating the correlation
coefficients of element pairs and clay, silt, and sand fractions (Table 2). Nonzero correlation coefficient with
accompanying p ≤ 0.05 is considered statistically significant at the 95% confidence limit.
The presence of outliers in the dataset was determined using the Tukey (1977) box plot method. It can be
seen from Table 2 that elements Co, Ni, and Mg considering the main elements of ultramafic environments
are well inter correlated. The elements Al, P, Pb, and Zn are well correlated with each other showing poor
abundance of these elements in ophiolitic regions. Cr, which is geochemically categorized in the first group,
also shows good correlation, but its relation is not as strong as those elements. There is an intense negative
correlation among Al, Mg, Ni, and Co. These relationships seem to be rational, as Al predominately occurs in
acidic rocks. The similar correlations are also observed among Pb, P, and Zn with the mentioned elements.
The relations of the studied elements with percentage of clay and sand content of soil samples are categorized
into three groups: 1- elements have a better relationship with sand fraction, e.g., Cr, Ni, Fe, Mg, and Co. 2-
elements have a better relationship with clay fraction, e.g., Al, P, Mn, and Pb. 3- elements do not show any
considerable relationship with soil texture, e.g., Zn and Ca.
6
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Table 1: Concentration of metals (milligrams per kilogram) and grain distribution (percent) of soil samples.
Sample Cr Mn Fe Al Ca P Mg Co Ni Pb Zn Sand% Silt% Clay%
S1 844 821 48900 19200 24500 136 197000 85.7 1470 5.3 64.3 75.8 16.6 7.6
S2 435 1100 50500 70900 46200 868 67100 35.6 346 12.5 93.8 63.4 11.6 25
S3 1080 827 45100 41200 54600 195 135000 53 845 7.9 72.6 74 14 12
S4 717 806 42700 34100 69700 159 136000 60.2 919 8.3 72.1 68 12 20
S5 2600 947 59900 40000 53600 268 122000 53.9 751 6.8 96.2 76.6 12.4 11
S6 1200 882 47200 37800 49000 397 159000 60.2 1010 7.2 72.3 77 13 10
S7 819 969 52900 53000 60500 826 95700 42.3 550 11.1 111 78 1 21
S8 663 997 43400 39100 34200 431 142000 59.1 895 6.9 65.5 56.8 9 34.2
S9 690 739 41100 29900 40100 130 172000 77 1240 6.7 74.6 78 2 20
S10 1210 949 48600 35600 42000 212 160000 60.8 997 7.3 76.9 87.2 3.8 9
Mean 1025.8 903.7 48030 39780 47440 362.2 138580 58.78 902.3 8.0 79.9 - - -
St. dev. 606.4 108.2 5567.2 14098 13099 275.4 37505 14.6 319.2 2.2 15.2 - - -
Coeff. Of
59.1 11.9 11.6 35.4 27.6 76.03 27.1 24.9 35.4 27.2 19.0 - - -
variation
Coarse-grained materials probably showing the presence of parent materials; thus, elements in the first group
are dominantly distributed via coarse grains weathered from ultramafic rocks than adsorbed on clay minerals.
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Elements in group 2 are placed in silicate layers easily, and with increase of clay content, their concentration
increases. Given this, the sorption and desorption processes play a more important role in transportation of
these elements in soils of the study area. A soil is considered “clean” when the substance under
environmental concern occurs in concentrations equal or lower than the value found in nature, which is used
as reference and usually named background concentration. Table 3 shows the background concentrations for
different elements in some international standards. Comparing the metal and major elements of the soil
samples with those of standards shows that concentrations of the elements Cr, Mn, Mg, Co, Ni, and Zn for
most of the soil samples were above permissible levels. To identify the natural enrichment of most common
elements in the study area, enrichment factor was calculated according to:
(C/R) sample
EF = /(C/R) crust
Table 2: Correlation matrix of heavy and major elements of soil samples.
Table 3: Limits for heavy metals and major elements in soils (mg/kg).
Standard Co Cr Mg Mn Ni P Pb Zn
Lindsaya 8 10 5000 600 40 600 10 50
USEPAb 8 10 5000 600 40 600 10 50
UKc - 50 - - 50 - 100 300
Australiac - 100 - - 100 - 100 300
a
Lindsay (1979) b USEPA (1983) c
Kabata-Pendias (1995)
Here, EF is the enrichment factor, C is the concentration in soil or earth crust, and R is the reference element
concentration (normalizing element). Sc was used as the reference element. Crust concentrations were
adopted from Rudnick and Gao (2003). Enrichment factor greater than 1 indicates that the metal is more
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abundant in the soil relative to earth crust in the regional background. The calculated enrichment factors for
elements Cr, Mn, Co, Ni, Pb, Zn, and P in 10 soil samples of the study area are shown in Fig. 3.
Figure 3: Calculated enrichment factor for the studied elements in Harsin-Sahneh region.
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Another index that has been used to assess the degree of contamination of soil samples is geoaccumulation
index (Muller 1979). The index is calculated as follows:
Cn
Igeo = Log2 ( )
1.5 Bn
where Igeo is the geoaccumulation index, Log2 is log base 2, Cn is the concentration in soil or sediment and
Bn is the background or reference concentration. Similar to the enrichment factor, the reference values
adopted were the average concentration of elements in the earth’s crust estimated by Rudnick and Gao
(2003). Muller (1979) classified soils in terms of quality (Table 4). Based on this index, Table 5 shows
calculated geoaccumulation. As can be seen from this table, few heavy metals like Cr, Ni, and Co have
values above zero, and hence, degree of contamination in these heavy metals is a matter of consideration.
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11
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is somewhat related to the forstrite contents. Moreover, high NiO content in Sahneh samples indicate that the
olivine (with high NiO content) is crystallized from relatively primitive magmas.
Studing Sahneh gabbro in Al2O3, FeO and MgO diagram to determine paleotectonic setting (Fig. 4h) and V
versus Ti diagram (not shown) proved that samples fall in the mid-ocean ridge basalt (MORB) field. In order
to clarify the nature of the environment of basalts (MORB), analyze results plotted in Zr-Nb-Y diagram. This
plot indicates that the samples were located in the MORB field in Fig. 11 and is likely from the E-MORB
environment (Fig. 4i).
The incompatible element pattern of the Harsin gabbro (Fig. 4j) indicates both negative anomalies in Zr, Nb,
and Ce and positive in Sr and La anomalies for samples. These incompatible element patterns are
characterized by an overall negative slope (generally sloping downward to the right). Positive anomalies in
Sr are characteristic of rocks that have high modal concentrations of calcic plagioclase. As a matter of fact,
both negative anomalies in Nb, Ti, Hf, and Zr and positive anomalies in U are considered to be a signature of
a mantle source over a subduction zone. Most likely, they were derived from a depleted mantle which was
slightly metasomatised over a subduction zone. The rare earth element (REE) patterns for the mantle rocks of
Sahneh region show depletion in the light REE (LREE) but enrichment in heavy REE (HREE) (Fig. 4k).
These patterns are similar to the E-MORB-type tholeiites; based on the evidence of the normalized
incompatible trace element diagram and the discrimination plots, it is concluded that Sahneh basalts were
derived from melts generated in the E-MORB environment.
5. Discussion
Based on analyses results of soils samples were collected from the study area, the obtained results show that
most of heavy and major elements were exceeding the permissible levels in soil samples in the study area.
The main reason for such enrichment would be the presence of ultramafic rocks and weathering and leaching
of elements from them. Therefore, natural contamination and also morphology play important roles in
producing such a high concentration of heavy metals in a region.
Most of the soil samples are below the standard limits for P and Pb. The low concentration of these two
elements is due to a low concentration of these elements in ultramafic rocks. Based on EF factor most
elements in most samples are enriched compared to those in earth crust. Cr and Ni are by far more enriched
than other elements in this area (Fig. 3). After these two heavy metals, Co is slightly more enriched
comparing with others. Pb and P had an EF lower than 1, showing that the contents of these elements in
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Environmental control & Waste utilization
topsoils are lower than those in earth crust. The higher enrichment of heavy and toxic metals Cr, Ni, and Co
is due to development of soil in ultramafic environments.
The Igeo values in some elements (e.g. Mn, Pb, Zn, and P) are below zero, but in chromium content, 80% of
the soil samples are moderately to highly polluted, ten percent are highly polluted, and 10% are moderately
polluted. Ni has a similar condition. Sixty percent of the soil samples are moderately to highly polluted. Co is
another abundant element in ultramafic environments, which their contamination degree is classified as
moderately polluted; other samples are uncontaminated. These studies suggested that during intra-oceanic
subduction, an immature island arc developed before ocean closure. Subduction slab collapsed during this
phase mostly led to the large-scale extension of overriding oceanic plate and thereby to the generation of
supra-subduction ophiolites. Tectonic events lead to the formation of Kermanshah arc to occur as follows:
Sanandaj–Sirjan continental arc magmatism had ended in the Late Cretaceous. It may be that the Southern
Neo Tethyan oceanic crust broke into the Late Cretaceous, subdued beneath itself, and developed arc
magmatism in Kermanshah region. As a result, Neo-Tethyan oceanic crust subduction beneath the SSZ
stopped at this time. Therefore, in the Late Cretaceous, arc magmatic-related rocks developed in Kermanshah
ophiolites. All of mafic and ultramafic rocks in Harsin Sahneh ophiolites are resting on the top of Neo-
Tethyan slab under Eurasia. Sedimentary age constraints in Kamyaran region (NW Kermanshah) and North
of Harsin–Sahneh, along the Gamasiab River, indicate that the subduction-related magmatism has been
active mainly between the Paleocene and the Eocene (Whitechurch et al. 2013). Paleocene to Eocene
magmatism quiescent period spanning in SSZ roughly coincides with arc-related magmatism in Kermanshah
region. By the end of short-live magmatism in Kermanshah, continental arc magmatism resumed in Middle
Eocene onwards along Urumieh– Dokhtar arc, which caused an inland shift around 200 km (shift from the
Sanandaj–Sirjan arc to the Urumieh–
Dokhtar arc). Based on evidence, Harsin–Sahneh ophiolites were a magmatic arc built on the Neo- Tethyan
oceanic lithosphere at the distal part of Eurasian margin, but MORB-related magmatism occurred in response
to the reduction of convergence rate of Neo-Tethyan. During the Paleocene–Eocene, the rate of convergence
of Eurasian continental margin slowed down; this reduction may have subdued slab retreat, triggering the
development of back-arc extension at Eurasian margin. This would also explain the simultaneous occurrence
of MORB-type and arc-type magmatism.
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a b c
d e
f g h FeOt
4 5
3 2
Mg O A l2 O3
i j k
4000
1000
100
Sample/PrimitiveMantle
10
0.1
0.02
Cs Rb U K Nb Sr Zr Tb Cr Ni Ta
Ba Th Pb Li Ce Ti Y Zn
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Environmental control & Waste utilization
6. Conclusions
Such a finding suggests that mainly ultramafic-originated elements are transported in coarse grain particles
specifically via physical factors. Heavy and major elements of soil samples are above permissible levels of
the Environmental Protection Agency, UK, Australia, and Lindsay for Cr, Mn, Mg, Co and Zn. Calculated
EF for soil samples are significant for Cr and Ni. Geoaccumulation factor index also showed which of the
elements Cr, Ni, and Co are among the most contaminating metals of soil samples in the study area. Studies
in recent years indicate that oceanic components abducted over the Arabic–Tauric platform during the Late
Eocene to Early Oligocene which is considered as the final closure of Southern Neo- Tethyan and Iran–
Eurasia collision. In the Late Cretaceous, the subduction of Southern Neo-Tethyan Ocean beneath itself leads
to the cessation of subduction beneath the SSZ; therefore, at this time, Sanandaj–Sirjan continental arc
magmatism had ended and arc magmatism activity developed in the Kermanshah region. Radiometric age
indicates that the quiescent period of magmatism in SSZ roughly coincides with arc-related magmatism in
the Kermanshah region. The resumption of subduction in region leads to forming arc-, back-arc-, and E-
MORB-related rocks in Sahneh–Harsin regions and Sonqor–Baneh and Hamedan–Tabriz volcanic belts. The
reduction in the rate of convergence and slab retreat subduction had back-arc extended in the Eurasian
margin; this could be considered as a factor in mixed MORB and arc geochemical signatures of Kermanshah
magmatism. The secondary stage of magmatism occurred after Kermanshah ophiolite abduction; in this
stage, magmatism activity shifted from Sanandaj–Sirjan arc to the Urumieh–Dokhtar arc.
References
Agard P, Omrani J, Jolivet L, Whitechurch H, Vrielynck B, Spakman W, Monie P, Meyer B, Wortel R
(2011) Zagros orogeny: a subduction-dominated process. Geological Magazine 148, 692–725.
Delaloye M, Desmons J (1980) Ophiolites andmelange terranes in Iran: a geochronological study and its
paleotectonic implications. Tectonophysics 68, 83–111.
Gharib F (2009) Biostratigraphy des radiolarites de Kermanshah (Iran). Unpublished doctoral dissertation,
Museum Nationald’Histoire Naturelle (Paris), 343 p.
Miati S, Gupta G, Erram V, Tiwari R (2013) Delineation of shallow resistivity structure around Malvan,
Konkan region, Maharashtra by neural network inversion using vertical elecrtical sounding measurments.
Environ Earth Sci 68(3):779–794.
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Mohajjel M, Fergusson CL, Sahandi MR (2003) Cretaceous–Tertiary convergence and continental collision,
Sanandaj–Sirjan Zone, western Iran. Journal of Asian Earth Sciences. 21, 397–412.
Muller G (1979) Schwermetalle in den sedimenten des Rheins-Veranderungen seit 1971. Umschau, 79, 778–
783.
Nisbet EG, Pearce JA (1977) Clinopyroxene composition in mafic lavas from different tectonic
settings.Contribution to Mineralogy and Petrology 63, 149-160.
Parlak O, Ho¨ck V, Delaloye M (2002) The supra-subduction zone Pozanti–Karsanti ophiolite, southern
Turkey: evidence for high-pressure crystal fractionation of ultramafic cumulates. Lithos 65, 205-224.
Rudnick R L, Gao S (2003) The composition of the Continental Crust (pp. 1–64). In R. L. Rudnick (Ed.),
The Crust (Vol. 3), H. D. Holland & K. K. Turekian (Eds.), Treatise on geochemistry. Oxford: Elsevier-
Pergamon.
Saccani E, Allahyari K, Beccaluva L, Bianchini G (2013) Geochemistry and petrology of the Kermanshah
ophiolites (Iran): implication for the interaction between passive rifting, oceanic accretion, and OIB-type
components in the Southern Neo-Tethys Ocean. Gondwana Research 24 (1), 392–411.
Shahabpour J (2005) Tectonic evolution of the orogenic belt in the region located between Kerman and
Neyriz. Journal of Asian Earth Sciences. 24, 405–417.
Ventura F, Salvatorelli F , Piana S, Pieri L, Pisa P (2012) The effects of biochar on the physical properties of
bare soil. Earth and Environmental Science Transactions of the Royal Society of Edinburgh , Volume 103,
pp 5-11.
Whitechurch H, Omrani J, Agard P, Humbert F, Montigny R, Jolivet L(2013) Evidence for Paleocene–
Eocene evolution of the foot of the Eurasian margin(Kermanshah ophiolite, SWIran) from back-arc to
arc:Implications for regional geodynamics and obduction.Lithos182–183.
Wrobel-Daveau JC, Ringenbach JC, Tavakoli S, Ruiz G,Masse P, Frizonde Lamotte D(2010) Evidence for
mantle exhumation along the Arabian margin in the Zagros (Kermanshah area, Iran). Arabian Journal of
Geosciences.Springer Berlin/Heidelberg 499–513.
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UTILISATION OF MANGANESE DUMP REJECTS OF CENTRAL INDIA REGION FOR
INDUSTRIAL APPLICATIONS
Abstract
Bench scale beneficiation studies on manganese dump rejects from a mine of central India was
undertaken with the objective to develop a process flow sheet to produce manganese concentrate suitable
for end user industry. The as received sample assayed 8.02% Mn, 2.61% Fe(T), 75.41% SiO2, 2.63%
Al2O3, 0.13% P, 0.02% TiO2, 0.2% S(T) and 1.26% LOI. Mineralogical studies on the sample revealed
that the sample consists predominantly of quartz with subordinate amount of manganese oxide minerals
and minor amount of mica. Rhodonite, pyroxene, amphibole, carbonate, garnet, feldspar, apatite, barite
and goethite/limonite are the other minerals noticed in very minor to traces. Among the manganese
minerals braunite is present in major amount with minor amounts of pyrolusite, very minor amount of
bixbyite, hollandite and rhodonite. Traces of jacobsite, psilomelane and cryptomelane are also present in
the sample. Heavy liquid separation test carried out at -65 mesh using tetra bromo ethane indicated that
heavy manganese concentrate assaying around 34% Mn, 21% SiO2 could be obtained with a maximum
Mn recovery of around 80% (Wt% yield: 15) could be obtained. Gravity concentration by employing
tabling at -65 mesh size followed by wet high intensity magnetic separation at 12000 Gauss of table tails
yielded a composite manganese concentrate with a reasonably good grade and recovery. The composite
concentrate obtained by combining the table concentrate and magnetic fraction of table tails assayed
30.08% Mn, 7.76% Fe(T), 29.42% SiO2, 2.62% Al2O3, 0.21% P, and 3.10% LOI with a Mn recovery of
72.2%. (Wt.% yield: 18.4). The Mn to Fe ratio is 3.87. The high silica content of the manganese
concentrate is further corroborated by the mineralogical analysis of the manganese concentrate which
revealed that braunite and manganese oxide minerals carry fine disseminated inclusion of silicate gangue
minerals. Braunite grains are also intermixed with silicates. The fine concentrate may find utilisation in
steel industry after agglomeration of fines.
Keywords: Dump rejects, gravity separation, magnetic separation, value addition, mineral conservation
1. Introduction
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Environmental control & Waste utilization
Manganese ore is an indispensable raw material in the manufacture of steel where it is used in the form of
Ferro-manganese and also as a direct feed to the blast furnace. The important non-metallurgical uses of
manganese ore are in the manufacture of dry battery and chemicals. In agriculture, it is used as a micro
nutrient for the plants. Manganese is also used in the manufacture of drier for paints and varnishes. It has
important application in ceramic and glass industry as colouring agent. Manganese is also known for its
decolorizing properties. No satisfactory substitution of Manganese in Steel has been identified which
combines its relatively low price with outstanding technical benefit.
India is the 2nd largest importer of Manganese ore. High and medium grade ore is used in the production
of Ferro Manganese. Medium to low grade ore is used in the production of Silico Manganese. Grade
Specification of Manganese are as follows; High grade Mn. ore with > 44% Mn. Content, Medium grade
Mn. ore with > 30% and ≤ 44% Mn. content Low grade Mn. ore with ≤ 30% Mn. Content. With the
targeted capacity of 300 million tonnes of crude steel in next 10-15 years, the requirement of manganese
ore will be around 10 million tonnes excluding manganese ore requirement for export of ferro alloys.
With the anticipated increase in steel production as well higher export of Alloys the gap between the
Supply and Demand of Manganese ore will increase, necessitating higher imports. The Average grade of
Mn. Ore produced in India is low (Mn 32-33%). This necessitates imports of High grade Mn ore to blend
with domestic quality of Mn ore for producing Ferro/Silico Manganese required for steel Industry.
Besides above, India is also a major exporter in world for Silico Manganese. There is a need for acquiring
high/medium grade manganese ore property to supplement the manganese ore requirement. Therefore, to
meet the growing requirement in the future it is necessary to utilise manganese ore deposits of our country
in a judicious manner. Therefore it is essential to explore the possibility of exploiting low grade
manganese ores.
Chemical characteristics: The as received sample assayed 8.02% Mn, 2.61% Fe(T), 75.41% SiO2,
2.63% Al2O3, 0.13% P, 0.02% TiO2, 0.2% S(T) and 1.26% LOI.
Physical and Mineralogical characteristics: The lumps sample received was in the size range of 1-4
inches, are hard and compact in nature and possesses low to moderate specific gravity. The colour varies
from light grey to dark grey. Mineralogical analysis of the sample revealed that the sample consists
predominantly of quartz with subordinate amount of manganese oxide minerals and minor amount of
mica. Rhodonite, pyroxene, amphibole, carbonate, garnet, feldspar, apatite, barite and goethite/limonite
are the other minerals noticed in very minor to traces. Among the manganese minerals braunite is present
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Environmental control & Waste utilization
in major amount with minor amounts of pyrolusite, very minor amount of bixbyite, hollandite and
rhodonite. Traces of jacobsite, psilomelane and cryptomelane are also present in the sample.
Wet size analysis of as received sample: A representative portion of as received tails sample was
subjected to wet sieve analysis from 10 mesh to 200 mesh size. The results indicate that manganese
values are slightly enriched in -200 mesh size fraction, otherwise it is uniformly distributed among the
various coarse size fractions. The -200 mesh size fraction assayed 11.57% Mn, 3.88% Fe(T), 67.79%
SiO2, 3.99% Al2O3 and 2.52% LOI with Mn recovery of 18.9 (Wt.% yield: 13.1).
Gravity separation at different size: The as received sample crushed to -10 mesh size were sampled
and taken into different batches. Each batch of the sample was wet ground to different sizes, viz., -30, -
50, 72 and -100 mesh size in multiple stages, to avoid fine generation. The ground slurries of each size
were individually subjected to gravity separation by tabling under identical conditions. The test
conditions and the results are presented in Table.1.
Size Assay% Mn
Products Wt.%
Mn Fe (T) SiO2 Al2O3 P LOI Dist.%
-30 mesh size Table Conc. 13.7 27.30 6.80 35.98 2.33 0.27 2.56 46.5
Table Middling 76.0 4.47 1.72 83.34 2.46 0.09 0.84 42.3
Table Tails 5.7 7.97 3.23 71.13 4.07 0.20 2.05 5.7
Table Conc. 9.2 38.12 8.55 16.53 1.97 0.23 2.97 43.6
-65 mesh size Table Middling 49.7 3.99 1.54 84.52 2.27 0.10 0.80 24.8
Table Tails 41.1 6.16 2.52 77.46 3.16 0.14 1.48 31.6
Table Conc. 7.0 40.02 9.30 12.6 1.83 0.22 2.91 34.8
-100 mesh size Table Tails 52.0 3.56 1.36 85.71 2.45 0.09 0.65 23.1
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Environmental control & Waste utilization
It is inferred from the results that as the fineness of the grind increases from 30 mesh through -100 mesh
size, the Mn grade increases at the same time the recovery decreases. A manganese concentrate assaying
38.12% Mn, 8.55% Fe(T), 16.53% SiO2, 1.97% Al2O3, 0.23% P, and 2.97% LOI with Mn recovery of
43.6% (wt%.yield: 9.2) could be obtained at a grind of -65 mesh size, by gravity concentration using
tabling. Although the Mn grade of the concentrate is found to increase at -100 mesh size, the Mn
recovery falls down considerably. Hence, -65 mesh size is found to be the optimum size for achieving
good grade of Mn with a reasonably good recovery.
Gravity separation followed by magnetic separation: In order to enhance the Mn recovery attempts
were made to carryout magnetic separation of table middling products at different sizes viz., -30, -72 and
-100 mesh, respectively. The test conditions and the results are presented in Table-2.
Table 2. Gravity followed by magnetic separation of manganese ore sample at different size
Test O.A.
Assay %
condition Products Wt% Dist.%
Mn Fe(T) SiO2 Al2O3 P LOI Mn
Tabling Con.-I* 13.7 27.30 6.80 35.98 2.33 0.27 2.56 46.5
& WMS Con.-II* 2.3 25.47 8.21 34.24 4.0 0.16 3.4 7.3
on -30 Composite
mesh Conc. 16.0 27.04 7.0 35.73 2.57 0.25 2.68 53.8
(Tabling Con.-I 9.2 38.12 8.55 16.53 1.97 0.23 2.97 43.7
& WMS Con.-II 16.3 20.70 5.95 48.57 3.25 0.13 2.91 42.1
on – 65) Composite
Conc. 25.5 26.99 6.89 37.01 2.79 0.16 2.93 85.8
(Tabling Con.-I 7.0 40.02 9.30 12.60 1.83 0.22 2.91 34.8
& WMS Con.-II 18.7 20.02 5.89 50.06 2.88 0.14 2.40 26.7
on – 100) Composite
Conc. 25.7 25.47 6.82 39.85 2.60 0.16 2.54 81.4
*Con.Iare gravity concentrates and Con.II are gravity cum magnetic concentrates
It is inferred from the results that the concentrate-II obtained by subjecting the table middling fraction of -
65 mesh size to wet magnetic separation yielded a concentrate of 20.70% Mn, 5.95% Fe(T), 48.57%
SiO2, 3.25% Al2O3, 0.13% P, and 2.91% LOI with Mn recovery of 42.1% (wt% yield: 16.3). Although,
the table middling fraction is upgraded, upto 20% Mn, it is not upgraded to obtain a composite
concentrate above 35% Mn. The similar product obtained at -100 mesh under identical condition also
yielded a Mn concentrate assaying around 20% Mn with a relatively lower yield. Hence, -65 mesh size is
found to be the optimum size for obtaining both Conc. I as well as Con. II.
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The price of the manganese concentrates for different grade is given in Table 3. So by combining the
individual price of Conc. I and Conc. II a total revenue of Rs.1, 27, 652/- could be obtained. If the price is
calculated for the composite concentrate assaying 26.99% Mn (Wt% yield : 25.5) the revenue generated
will be as follows;
The price of manganese concentrates were calculated for Conc.I and Conc.II, individually.
Conc. I 9.2 x 10424 = 95,900/-
Con. II16.3 x 1948 = 31,752/-
1, 27, 652/-
Composite Conc. 25.5 x 4667 = 1, 19, 009/-. Therefore, it is better to sell the high grade concentrate
separately rather than selling it as a composite concentrate.
3. Conclusions
Waste dumps all along the mining belt are to be investigated before declaring it as reject. Although the
chemical analysis of the dump reject assayed 8.02% Mn which is less than the threshold value for
manganese minerals for implementation declared for Mn ores (10% Mn), beneficiation study on the reject
sample revealed that a saleable concentrate of +35% Mn could be achieved by gravity concentration.
Therefore, any mine dump considered as waste should be investigated before declaring it as a reject
sample. High grade concentrate fraction will always fetch more price than composite concentrates as
evidenced the cost benefit analysis.
Acknowledgement:
The authors express their sincere thanks to Shri R.K.Sinha, Controller General (In-Charge), Indian
Bureau of Mines, Nagpur, for giving permission to present the paper.
References:
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Indian Bureau of Mines, Mineral Processing Division’s Unpublished Report of Investigation (IBM / NGP
/ R.I. No.).
Monthly statistics of mineral production June 2014.
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ECONOMICAL AND ENVIRONMENT FRIENDLY RECYCLING OF PCBS FROM DVDS FOR
RECOVERY OF METALS ADOPTING PHYSICAL BENEFICIATION PROCESS
Vinod Kumar1*, Jae-chun Lee2, Jinki Jeong2, Manis Kumar Jha1, Byung-su Kim2, Ratnakar Singh1
1
CSIR- National Metallurgical Laboratory, Jamshedpur, India
2
Korea Institute of Geoscience & Mineral Resources, Republic of Korea
*Corresponding author: vk@nmlindia.org
Abstract
A novel physical processing technique has been developed comprising manual disintegration and sorting
of components/ PCBs, followed by shredding and crushing in scutter crusher. The output product is then
subjected for grinding in high speed hammer mill for metal liberation, ultimately leading to separation of
valuable metals and plastic components. The process, as developed, for efficacious separation of metallic
from non-metallic fraction, assists liberation of different constituents based on size fractions. Size
classification of the ground materials demonstrated enrichment of metals in coarser particles (-1000 +150
µm) while non-metals in the finer particles’ size of around -150 µm. A grade of 95-97% metals with a
separation efficiency of around 95% was accomplished adopting froth flotation and pneumatic separation
methodology/technique. Presence of rare metals in different fractions in varying amounts from 1.88 to
4.18% has been observed, however, bulk of the quantity has been observed to be present in finer fractions
< 500 µm in contrast to major valuable metals with enrichment of up to 9% after beneficiation. The
novelty or the USP of the process lies in its cost effectiveness and environmental friendliness (without
any chemical reagents/additives) for recovery and recycling of valuable metallic components which can
be used in small scale processing by engaging high-skill workers under supervision of technical experts.
1. Introduction
The rapid proliferation of information technologies has resulted in deep market penetration and
accelerated propagation of advanced technology electronic products in the market. This leads to
unprecedented and frequent dumping of regular use information technology products, home appliances,
etc. and generation of large quantities of end-of-life electrical and electronic equipment (EOL-EEEs).
This alarming phenomenon is causing immense environmental concern and health hazard in many parts
of the world, especially in developing countries. In India, the problem has attained an alarming dimension
today because of inappropriate collection system, rudimentary disposal and recycling methodologies of
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Environmental control & Waste utilization
EOL-EEEs, especially, due to in-accessibility to efficacious and cost-effective processing technology.
The typical constituents of PCBs are non-metals (plastics, epoxy resins, glass) 60% and metals
containing copper ~16%, solder ~4%, iron ferrite ~3%, nickel ~2%, silver 0.05%, gold 0.03%, palladium
0.01%, others (bismuth, antimony, tantalum, platinum, etc.) 0.01% (Goosey and Kellner, 2003),
although their actual composition varies depending on the specific electrical and electronic equipments
(EEEs), unscientific processing of which triggers immense toxic pollutions, ecological imbalances and
threat to life.
The process of recovery and recycling of metals from PCBs is very complex due to the heterogeneous
mix of organic materials, metals, glass fiber and epoxy resins and their multilayered construction.
Random discard of such substances in the open or land fill leads to the leachate infiltrating into the
groundwater and soil (Kumar et al., 2015; Kumar et al., 2013; Kumar et al., 2010; Chao et al., 2011; Yoo
et al., 2009; Lee et al., 2007). These materials could be processed either by hydrometallurgical or
pyrometallurgical process after physical treatment, albeit pyrometallurgical processing generates
carcinogenic dioxins gases. Suggestion was also made to use plastics of EoL-EEEs as combustible
material in a furnace.
In this paper, scientific investigation has been discussed for the liberation of metallic values from the
plastics / resins based on the particle size distribution, exploitation of differential density and other
physical properties including froth floatation, achieving enriched concentrate comprising metallic values
up to 90% with 75% recovery, with process optimization. The classicality of this environmentally safe
recycling methodology, apart from being a very simplistic and economical process, will factually
incentivize its penetration in the mini/ small scale processing industries across the board who cannot
afford access to scientific/technical personnel. The economy of process hinges on the fact that no
consumables whatsoever (viz., additives, chemical, etc.) is essential in the entire processing method.
2. Experimental
2.1 Materials
Discarded DVD video player systems from Korean EOL-EEE recycling industries were collected,
disassembled and their components such as plastics, external metallic case, interior metallic components,
cables, wires and PCB etc. were hand sorted and weighed to know their percentage composition to
recover valuable metals from PCBs. The undesirable attachments such as cords, frames, hard metal
composites and wires were removed from the PCBs of DVD video players manually. The circuit boards
were then cut into small (about 10 cm x 8 cm) pieces using manual and mechanical cutting tools. These
small pieces were then subjected to scutter crusher to reduce the size of the PCBs below 10 mm and
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further down size reduction carried out in a high speed hammer mill to a top size of 1.5 mm. The ground
PCBs powder was used as the feed material for further characterization and processing studies. The total
metal content in the PCBs of DVD video player (DVD-PCBs) is ~43% with metal content as copper
(17.80%), aluminum (10.10%), iron (5.51%), lead (3.33%). tin (2.57%), zinc (1.99), nickel (0.36%) and
several other rare and precious metals at minor concentration as given in Table 1.
Table 1: Composition of different components of EOL- DVD video player after dismembering and
chemical analysis of EOL- PCBs (weight %).
Al Cu Fe Sn Pb Zn Ni Sb Ti Ba Cr Mg V Sr
10.10 17.80 5.51 2.57 3.33 1.99 0.36 0.30 0.28 0.15 0.17 0.14 0.01 0.11
Mn Bi Co Zr Ra Mo Ca K Br Si Cl P S LOI
0.24 0.05 0.04 0.04 0.02 0.01 0.88 0.04 7.30 3.79 0.69 0.59 0.02 43.16
2.2 Methods
The physical mechanical recycling process investigated for enriching the metallic components from waste
PCBs and sequence of operation for generating enriched metallic concentrate with higher yield and
recovery are presented in this paper.
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using a multiplex laboratory zig-zag classifier (Model: B 1–40 MZM, Hosokawa Alpine AG., introducing
air stream from the bottom for pushing out low density light materials in the overflow, while the higher
density metal content reports to the underflow (Murugan et al.,2008) by maintaining requisite volume of
supply air through adjustments, for the effective separation. The average metal compositions of the light
and heavy fractions were analyzed to assess the enrichment of the metallic components with the particle
size of the milled PCBs. The zig-zag configuration of the pneumatic channels factually aid generating
clean metallic concentrate with minimal loss of fines metals. The relevant contact surface portions may be
provided with suitable wear resistant liners, against the negligible wear, from durability perception.
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reduction in the particle size had no impact on the non-metallic fraction which remained at about 70% of
the non-metallic components, even up to 45 µm.
Table 2: Mass distribution (weight %) and liberation analysis in different particle size fractions of the
ground PCBs at varying hammer speed.
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observed. The experiments demonstrate the crucial contribution of controlled grinding in a hammer mill
for the effective liberation of metals and their segregation.
Table 3: Pneumatic separation studies with ground materials of EOL DVD- PCBs (-1500 µm).
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formation of strong froth particularly with non-metallic constituents (Ogunniyi and Vermaak, 2009).
Hydrophilic and hydrophobic particles have been observed to stabilize froth in finer size. Close packing
of particles in the froth lamella as well as flocculation of particles (as suggested by thick bubble
interstices seen in the froth) are two major mechanisms that can be inferred for attributing to stabilization
of the froth. Secondly, it may be recalled that in PCB production, the fibres were impregnated with the
resin until it sets in place on the fibre. Strong adhesion between the reinforcement and the matrix is a pre-
required qualitative requirement in composites. Flotation due to air bubble attachment to the resin
impregnated pseudo hydrophobic surface can therefore be another strong reason for the glass fibres’
transfer to the froth.
The studies carried out in froth flotation cell under the different stirring speed in presence of water
without use of a collector or frother showed the formation of stable froth with non-metallic components
when air was sparged. The froth was then removed from the top of the cell which mainly contains the
non-metallic constituents along with minor amount of metals. The studies showed the formation of
natural hydrophobic response with formation of stable froth in natural condition. The results for the
separation of metals, their yield and recovery are presented in Table 4 under agitation of 1500, 2000 and
2300 rpm respectively. The total recovery of metal was found to decrease from ~87 % to ~75% with
increase in agitation speed from 1500 to 2300 due to the suspension of even heavy metallic particles with
the froth containing non-metallic components. The yield of the metallic constituent and metal grade was
found to vary in the range of ~46% to ~36% and ~81% to ~90% respectively under the above agitation
speed. At higher speed, grade of the total metal concentrate improved to approx 90% at ~10% loss of
recovery of metals in the final concentrate in DVD-PCBs. Concentration of rare metal including Cr, Sr,
Ti, Sb, Ni etc are comparatively less encouraging with increasing impeller speed and indicated
enrichment of rare metals up to 5.8%. On comparing the results of pneumatic separation and froth
flotation, the enrichment of rare metals was observed to be encouraging in pneumatic separation wherein
the grade of rare metals in the metallic concentrate improved to 9.4% compared to 5.8% by flotation.
However, the loss in recovery of total metals in the pneumatic separation is more than the froth flotation
thus, froth flotation is more promising from the perspective of enhanced grade and recovery of metals in
the metallic concentrate. Froth flotation has provided excellent results without using any additive,
chemicals or floatation reagents.
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Table 4: Froth flotation studies with ground materials of EOL DVD- PCBs (-1500 µm).
4. Conclusions
Milling, size classification and beneficiation adapting pneumatic separation, froth flotation techniques
etc., have been observed to be best suited for physical beneficiation, for enrichment of concentrates
containing up to ~90% metals in recovering primarily valuable metals and also rare metals, from the
waste PCBs, under optimal processing condition. The economy of process hinges on the fact that no
consumable whatsoever (viz. additives, chemical, etc.) is essential in the entire processing method.
Acknowledgements
This research work was supported by the Korea Institute of Energy Technology Evaluation and Planning
(KETEP) under the project entitled “Development of Technology for the Recycling of Valuable Metals from
EOL Small Electrical & Electronic Equipment”. The first author is thankful to the students Ji-Hye-Kim,
Woo-Chul Sin and Moo-Ki Bae and other colleagues of KIGAM for their support in this research work.
References
M. Goosey,and R. Kellner, 2003. Circuit World, 29 (3), 33-37.
V. Kumar, J.-c., Lee, J. Jeong, B.S. Kim. Korea Earth System Science & Engineering 47(5) (2010) 593–
608.
R.V. Murugan, S. Bharat, A.P. Deshpande, S. Vaughese P. Haridoss. Powder Technology 183 (2008)
169–176.
J.M. Yoo, J. Jeong, K. Yoo, J.-c. Lee, W. Kim. Waste Management 29 (2009) 1132–1137.
J.-c. Lee, H.T. Song, J.M. Yoo. Resource Conservation and Recycling 50 (2007) 380–397.
I.O. Ogunniyi, M.K.G. Vermaak. Mineral Engineering 22 (2009) 378–385.
V. Kumar, Jae-chun Lee, Jinki Jeong, Manis Kumar Jha, Byung-Su Kim, Ratnakar Singh,2015; Journal
of Industrial and Engineering Chemistry, Vol.21, pp.805-813, 2015.
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V. Kumar, Jae-chun Lee, Jinki Jeong, Manis Kumar Jha, Byung-Su Kim, Ratnakar Singh, 2014;
Separation and Purification Technology, Vol. 111, pp. 145-154, 2013.
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ENERGY GENERATION FROM COALEnvironmental
MINE WASTE control & Waste utilization
D.S.Panwar*1, V.K.Saxena1 and A.K.Singh2
1
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad-826004
2
Department of Methane emission and degasification, CIMFER, Dhanbad-826001
*Corresponding author: deepaksingh.4268@gmail.com
Abstract
The Indian energy expenditure is still heavily dependents on fossil fuel to meet basic human needs. To fulfill
fastest growing energy demand of the country we have to focus on alternate energy resources like coal bed
methane. Coal bed methane is formed during the coalification process and store in coal seam as gas reservoir.
During mining operation a lot of methane is released which comes in atmosphere by the ventilation system.
The direct emission of methane into the environment creates a host of serious environmental problems. Coal
bed methane, which has huge calorific value for power generation can help us to minimize emissions of
greenhouse gases and pollutants by proper utilization of this unconventional energy resource. The present
paper discusses about the coal and gas resource estimation in Kulti and Sitarampur block of Raniganj coal
field. In the present study some coal samples were collected from two bore holes located in Sitarampur block
of Raniganj coal field, India. The effect of chemical properties, on gas content has been studied in order to
find a correlation between them. Mathematical regression was also analysed in this study.
Keywords: CBM, field geology, proximate analysis, gas content, regression analysis.
1. Introduction
Coal bed methane is a gas formed as by product of the geological process of coal formation. The gas content
in coal depends upon the maturity of coal, low rank coals tend to have lower gas content than high rank coals
such as anthracite. The anthracite coal is a rich source of methane but desorption study shows that anthracite
is an insignificant source of coal bed methane. The commercial coal bed methane production takes place in
coals of low to high volatile bituminous coals. Coal bed methane is extremely pure compared to conventional
natural gas, containing only very less amount of other gases. The enrichment value of methane is high in coal
bed gas which make it suitable for introduce into a commercial pipeline with little treatment.
Coal bed methane has been considered a major mine hazard since the early to mid-19th century. Methane
emitted in mines during coal exploration which create problem in underground coal mines. Coal bed methane
comes in focus from mine safety purpose for measuring the gas content of coal beds. The ventilation system
was provided to reduce the methane level in mines. Ventilation methane comes into the atmosphere and
creates several problems related with greenhouse gas emission. Methane is a most significant greenhouse gas
which is mainly responsible for global warming; absorbs atmospheric heat approximately 23 times more than
carbon dioxide is used as unconventional source of energy. The commercial gas production from this
unconventional gas resource has resulted in an increased interest in this new technology. Coal bed gas
content data are used for the calculation of gas resources and as input data for reservoir models and
production simulators to forecast gas production.
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Environmental
The present paper discusses about the coal and gas resource estimation in Kulti andcontrol & Waste
Sitarampur utilization
block of
Raniganj coal field. In the present study some coal samples were collected from two bore holes located in
Sitarampur block of Raniganj coal field, India. The effect of chemical properties, on gas content has been
studied in order to find a correlation between them. Mathematical regression was also analysed in this study.
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Table 1: Coal quality of blocks
The Vitrinite reflectance value shows that the coal samples which were collected from the field belongs to
this bituminous stage. The Vitrinite reflectance value of collecting coal samples from both of blocks varies
from 1.255 to 1.552% (Kulti) and 1.37 to 1.58% (Sitarampur).
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Y = a+ b*ln(X1) + c*ln(X1)2 + d*ln(X1)3 + e*ln(X1)4 + f*ln(X1)5 + g/X2+h/X22+i/X23+j/X24+k/X25 (3)
Where Y is the gas content of a coal sample on d.a.f basis, a, b, c, d, e, f, g, h, i, j and k represent regression
coefficients, X1 stands for volatile matter and X2 for fixed carbon of coal samples on the dry ash free basis.
To test the significance of each of the coefficients, Fishers test (F test) was carried out at 99% confidence
level. To find out the accuracy of equations the actual value plotted with predicted value are shown in below.
4. Conclusion
The Vitrinite reflectance value of the studied coal samples reflect that the rank is to be in a range of medium-
volatile bituminous to low volatile bituminous. From the current study it was observed that all the samples
from different well and the depth shows high gas content. The gas content values of the studied coal samples
shows the linear relationship with depth which is increasing with depth. The Kulti and Sitarampur blocks are
having a good potential for mining of high quality coal as the available data indicates consistency. There is
considerable amount of gas resource as well.The gas resources of 1.77 BCM and 1.63 BCM are likely to be
contained in the Kulti and Sitarampur Blocks respectively. Same coal seams are generally present in both the
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blocks. Total gas resource in both of blocks is estimated as 3.40 BCM. control
Therefore a CMM &ofWaste
project utilization
medium
scale may scale may be started in these blocks. The overall study concluded that the valuable gas resource
can be recovered by CMM technology for energy generation from coal mines waste.
References
Meissner, F.F. 1984. cretaceous and Lower Tertiary coals as sources for gas accumulations in the Rocky
Mountain area. In Hydrocarbon source rocks of the greater rocky
Bertard, C., Bruyet, B. and Gunther, J., (1970). Determination of desorbable gas concentration of coal (Direct
method), Int. J. of Rock Mechanics and Min. Sci. Vol.7, pp. 43-65.
Kissel, F.N., McCulloch, C.M. and Elder, C.H., (1973). The direct method of determining methane content of
coal beds for ventilation design, US Bureau of Investigation, RI 8043.
McCulloch, C.M., Levine, J.R., Kissel, F.N., and Deul, M., (1977). Measuring the methane content of
bituminous coalbeds, US Bureau of Mines Report of Investigation, RI 8043.
Diamond, W.P. and Levine, J.R., (1981). Direct method for determination of the gas content of coal:
procedure and results, US Bureau of Mines Report of Investigation, RI 8515.
Feng, K.K., Cheng, K.C. and Augsten, R., (1984). Preliminary evaluation of the methane production
potential of coal seams at Green-hills mine, Elkford, British Columbia, CIM Bull., 77, pp. 56-60.
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Hydrometallurgy & Bio-hydrometallurgy
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Hydrometallurgy & Bio-hydrometallurgy
PROCESS COMPRESSION AND FLOWSHEET DEVELOPMENT FOR THE MINING AND
METALLURGICAL INDUSTRY
V. I. Lakshmanan, R. Sridhar and M. A. Halim*
Process Research ORTECH Inc., 2350 Sheridan Park Drive, Mississauga, ON, L5K 2T4
*
Corresponding author: halim@processortech.com
Abstract
Process compression is the elimination of a process step to make the process more economical. It helps in
cutting the cost of production without affecting the quality of the product. Some examples of process
compression are Carbon-in-Pulp process, Resin-in-Pulp process, heap leaching, in-situ leaching and
development of Krebs-Mixer-Settler equipment for metal recovery. In contrast, development of a
flowsheet starts with identification of raw material(s) and potential product(s) and by-product(s). First
step in the development of flowsheet is to consider various process options and prepare a conceptual
flowsheet. The conceptual flowsheet is then tested at bench scale for feasibility of the concept followed
by pilot scale testing to optimize the operating parameters and to conduct detailed mass balance, energy
balance and water balance to obtain design criteria for preliminary capital (CAPEX) and operating cost
(OPEX) estimation. Before the construction and commissioning of full-scale production plant, the
flowsheet can also be tested in a demonstration plant to further minimize technical, operational and
financial risks.
1. Process compression
Falling commodity prices along with rising production costs is putting a squeeze on the bottom line of the
mining and metallurgical industry. In order to stay competitive, production costs need to be minimized
without affecting the quality of the product. One of the innovative ways to achieve this goal is by process
compression. Process compression is the elimination of a process step to make the process more
economical. Many times technology available in other process industries can be applied to mining and
metallurgical industry to eliminate certain process steps, if sustainable. Some examples of process
compression are provided below:
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cyanide complex is adsorbed on the activated carbon, which is then separated from leach slurry by
screening. Figure 1 shows the typical process flowsheet for CIP process (Hill, 1986). Gold is desorbed
from activated carbon by stripping and recovered by electrowinning. Carbon is reactivated and recycled
to the process. CIP process minimizes costly solid/liquid separation steps.
Figure 1: Typical process flowsheet for carbon in pulp (CIP) process (Hill, 1986).
1.2 Resin-in-pulp (RIP) process
Resin-in-Pulp (RIP) process is similar to the CIP process except that activated carbon is replaced by solid
spherical polystyrene resin beads and has been practiced in the uranium industry. Generally, uranium ore
is leached with sulphuric acid followed by solid/liquid separation to produce uranium-rich pregnant leach
liquor. The leach liquor is then passed through ion exchange resin columns to extract uranium from leach
liquor. The loaded uranium is removed by passing an eluting liquid through the ion exchange resin
columns. Due to low grade of uranium ore, process requires separation of pregnant leach liquor from
large amount of residue by filtration, which adds significantly to the process cost. In addition, resin-
packed columns also involve high capital cost. In contrast, moderately coarse resin beads are mixed with
pulp and separated by screening when the ion-exchange resin is loaded with uranium. This RIP process
eliminates the costly filtration step and reduces capital cost by eliminating the need for ion-exchange resin
columns. The RIP process has been practiced in USA, Russia, France, South Africa, China and Canada
for the processing of uranium ore (Mirjalili and Roshani, 2007).
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leach liquor is pumped out for further processing. Heap leaching eliminates the need for grinding, which
makes it an economical process option for the treatment of low grade ores. Heap leaching has been used
for the treatment of copper, uranium, nickel, silver and gold ores. Poor recovery due to non-uniform
percolation has been faced by many heap leach operations, particularly the ones with significant clay
content in the ore. To overcome this problem, modern heap leach operations include
agglomeration/stacking as one of the process steps before leaching. Agglomeration of ore particles results
in agglomerates of similar size particles avoiding the problem of segregation. This results in uniform
percolation of the lixiviant through the ore heaps. Figure 2 shows the flowsheet of a heap leach operation
(Zanbak, 2015).
Figure 3: Flowsheet of an in-situ leach operation for uranium ore (US Nuclear Regulatory Commission,
2014).
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Krebs mixer-settlers have been installed in many uranium solvent extraction plants and some copper
solvent extraction plants. Advantages of the Krebs mixer-settler include smaller footprint area, simplified
plant layout, shorter inter-stage and recycle piping, and lower CAPEX, while disadvantages include
limited access for crud removal, higher power consumption, higher reported organic entrainment and
proprietary design subject to license fee (Taylor, 2014).
2. Flowsheet development
Flowsheet should be economically viable and environmentally sustainable. A new flowsheet may be
required if the type of ore changes. As non-refractory gold ores are exhausted, the need to extract gold
from refractory and double refractory ores has arisen. Gold producing companies are responding to the
challenge by developing new flowsheets for processing refractory and double refractory ores. A new
flowsheet may also be necessitated to comply with stricter environmental regulations. A new flowsheet
for production of zinc using pressure hydrometallurgy was developed to avoid the emission of sulphur
dioxide resulting from the roasting of zinc. A new flowsheet may become feasible with advances in
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materials of construction. The development of polymeric materials has led to development of flowsheets
with aggressive lixiviants such as chlorides.
Development of a flowsheet starts with identification of raw material(s) and potential product(s) and by-
product(s). First step in the development of flowsheet is to consider various process options and prepare a
conceptual flowsheet. The conceptual flowsheet is then tested at bench scale for feasibility of the concept,
to obtain a good understanding of the process chemistry and to investigate the operating parameters. The
pilot scale test work is then performed to optimize the operating parameters and to conduct detailed mass
balance, energy balance and water balance to obtain design criteria for preliminary capital costs (CAPEX)
and operating costs (OPEX) estimation. Pilot scale test work also generates samples for market evaluation
and testing for compliance to environmental regulations. A demonstration plant may be commissioned to
test the process before the construction and commissioning of full-scale production plant. Running a
demonstration plant provides an opportunity to further minimize technical, operational and financial risks.
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The evaluation of different process options will typically include a database search for existing operations
of a similar nature, but for different products. Once a number of potential process options are identified,
then testing of the processes is required to establish which of them offers the potential to be viable.
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and to optimize the process. The bench scale tests are typically carried out on a batch basis. The problem
with batch testing is that it does not investigate the impact of recycle streams. One way that is used to
overcome this problem for hydrometallurgical operations is to set up a mini scale continuous circuit with
the necessary streams recycled as required. It is particularly useful to start developing a computer model
of the process at this stage and to progressively incorporate the results of the test work into the model.
The model can also be used to investigate some different possible flowsheet options and to provide
direction to the test work program. At the end of detailed bench scale test work, a detailed process
flowsheet is constructed, which is tested under continuous operation at a much larger scale than bench
scale test work during pilot scale test work.
Pilot plant testing is usually carried out at the facilities of established metallurgical testing organizations
as they have a large inventory of small process equipment items that can be installed to form a
representative circuit. Also, the organizations have the required analytical facilities and the operating
staffing that are required for a continuous pilot plant operation working 24 hours/day. Solid-liquid
separation is typically a very important part of both mineral processing and hydrometallurgical processes
and so it is essential that settling and filtration test work be carried out on samples from the pilot plant.
The samples should be fresh to obtain the most realistic results, so it is usual that the solid-liquid
separation tests are performed at the facility where the pilot plant campaign is being carried out. The
solid-liquid separation test work is typically performed by vendors of this type of equipment or by
organizations that specialize in this type of test work.
Running a pilot plant is a very important step towards reducing the risk of any unforeseen complication in
operating the actual plant. It provides an opportunity to minimize technical, operational and financial
risks. Pilot plant can be run with a variety of feed stocks and under different operating conditions to check
the robustness of the flowsheet. Pilot plant can also be used for training the employees for full scale
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production plant. After the pilot scale test work is completed, next step could be either the construction of
a full scale production plant or a demonstration plant.
concerns regarding the scaling-up of the process from the pilot plant to the commercial plant
capacity;
size required to satisfy the requirements of financing organizations;
ability to produce sufficient product to supply samples to potential users;
concerns with the process consistently producing a product of satisfactory quality;
Development of an innovative process will often require the construction of a demonstration plant. As the
process is not well established, it may require specialized equipment and design and it may be a good idea
to test the process at demonstration scale before the construction and commissioning of full-scale
production plant. Running a demonstration plant provides an opportunity to further minimize technical,
operational and financial risks.
3. Conclusions
Process compression helps in reducing the cost of production by eliminating process step without
affecting the quality of the product. For example sustainable resin-in-pulp and similar carbon-in-pulp
processes have been developed to recover uranium and gold from low-grade ore bodies, where resin and
pulp are contacted counter-currently in a series of agitated contactors. The loaded resin is separated from
the pulp over screens, washed, and transferred to elution. The eluted resin is then returned to the
adsorption circuit. This process provides an attractive and economical option by avoiding solid/liquid
separation step, which is usually problematic. This also reduces the wash water volume and minimizes the
loss of value metals.
Flowsheet should be economically viable and environmentally sustainable. Flowsheet needs to be robust
and forgiving. It should be viable for a wide range of parameters. First step in the development of
flowsheet is to prepare a conceptual flowsheet by considering various process options. The conceptual
flowsheet is then tested at bench scale for feasibility of the concept, to obtain a good understanding of the
process chemistry and to investigate the operating parameters. The pilot scale test work is then performed
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Hydrometallurgy & Bio-hydrometallurgy
to optimize the operating parameters and to obtain design criteria for preliminary capital costs (CAPEX)
and operating costs (OPEX) estimation. Pilot scale test work also generates samples for market evaluation
and testing for compliance to environmental regulations. A demonstration plant may be commissioned to
test the process before the construction and commissioning of full-scale production plant. Running a
demonstration plant provides an opportunity to further minimize technical, operational and financial risks.
References
S. D. Hill. The carbon-in-pulp process. U.S. Bureau of Mines Information Circular 9059:40-43, 1986.
V.I. Lakshmanan, R. Roy, and R. Ramachandran. Innovative process development in metallurgical
industry: concept to commissioning. Springer, pp. 437, 2015.
K. Mirjalili, and M. Roshani. Resin-in-pulp method for uranium recovery from leached pulp of low grade
uranium ore. Hydrometallurgy 85:103-109, (2007)
U.S. Nuclear Regulatory Commission. Information Digest. 2013–2014 (NUREG-1350, Volume 25).
Section 4. Nuclear Materials, retrieved on September 6, 2014
(http://en.wikipedia.org/wiki/In_situ_leach#mediaviewer/File:NRC_Uranium_In_Situ_Leach.png).
A. Taylor. Review of mixer-settler types and other possible contactors for copper SX. ALTA
Metallurgical Services. Retrieved on August 30, 2014 (http://www.altamet.com.au/wp-
content/uploads/2012/12/Review-of-Mixer-Settler-Types-and-Other-Possible-Contactors-for-Copper-
SX.pdf).
C. Zanbak. Heap leaching technique in mining, retrieved on May 29, 2015
(http://www.euromines.org/files/mining-europe/mining-techniques/batforheapleaching-feb2013-c.zanbak-
euromines.pdf).
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MATHEMATICAL MODELLING OF ALKALINE LEACHING OF URANIUM
Abstract
The modelling approaches for leaching of ores for extraction of valuable metals range from deterministic
to stochastic, mechanistic to phenomenological / statistical, micro to macro models including population
balance methodologies. The leaching behaviour related to the fundamental mechanisms governing the
system behaviour is incorporated by deterministic models, while the uncertainty in input parameters are
accounted by stochastic models. Each of the models have their scope and suitable instances of
applicability. Identification of the best modelling strategy is critical for accurate prediction of leaching
efficiency / behaviour of an ore with residence time. Various deterministic and mechanistic models based
on homogeneous and heterogeneous chemical reaction rate equations are available for leaching of pure
uranium minerals as well as uranium ores. However, not a single model is applicable in all the cases of
leaching and more particularly, rate information obtained for a set of conditions of leaching of particular
ore may not be applicable in another set of conditions. This paper discusses the applicability of a
deterministic model, namely topochemical rate equation, for leaching of uranium dioxide from synthetic
mixture using solution of Na2CO3 and NaHCO3 as leachant.
1. Introduction
The leaching of uranium from an ore is a complex process which depends on several critical factors like:
[1] degree of liberation, [2] grain size, [3] porosity of the host rock, [4] type of leachant and oxidant, and
[5] operating conditions of leaching such as temperature, pressure, stirring speed and type of stirrer in the
case of agitation leaching or the advective flow conditions in the case of heap leaching. Mathematical
models based on various fundamental mechanisms of leaching can be termed as deterministic models.
Even though leaching is a heterogeneous process, it is sometimes modeled by homogeneous reaction rate
equations (Levenspiel, 2001; Hossain et al., 2006). These rate equations obviously do not take into
account the specific properties of solid phase such as particle size, specific surface area, and porosity.
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They are applied to leaching based on an assumption that the particle size of solids is so small that the
percentage of molecules physically free to react is high enough and the behavior of a solid becomes more
nearly like the behavior of a dissolved reactant (Schortmann and DeSesa, 1958). The first order
homogeneous rate equation can be explained by law of mass action. Nevertheless, many times the
experimental data does not adequately fit the first order rate equation, but fit the rate equations of higher
order. There is no strong phenomenological evidence for higher orders in the rate equations other than an
analogy with that of first order rate equation (Harris and Chakravarti, 1970). Thus, the ‘order’ with
respect to each reactant merely serve as empirical constant. Avrami model is another homogeneous model
used extensively for rate of crystallization, but also rarely for leaching (Demirkiran and Asim, 2007). This
rate function is sigmoidal, with an initial lag-period, where reaction occurs very slowly, followed by a
rapid increase and eventually reaching a plateau towards end of the reaction. The Michaelis–Menten
kinetics is one of the best known homogeneous models for enzyme kinetics. However, this form of rate
equation is also frequently used for leaching reactions of uranium, pyrites etc. which are driven by
electrochemical mechanism (Burkin, 2001; Song et al., 2013). At lower concentrations of reactants, the
Michaelis–Menten rate equation reduces to general homogeneous model equation. And at higher reactant
concentrations the leaching progresses as zero order reaction.
The heterogeneous rate equations are based on phenomena taking into consideration the solid phase
participating in leaching reaction. Fundamentals of kinetics of heterogeneous reaction systems in
hydrometallurgy have been dealt with extensively by Sohn and Wadsworth (1979). Under this class of
leaching models, the progressive conversion model is not generally considered as it does not represent
reality of the physical systems (Levenspiel, 2001). The shrinking core model is most widely applied for
leaching reactions taking into account the solid phase. It is also known as topochemical model according
to which the rate of leaching is given by product of thermal function, chemical function encompassing
concentration of reagents and the topological function representing changing solid grain topology (Sylvie
et al, 2006). The penetration of dissolved reactants and products through pores of the ore particles is aptly
represented by another heterogeneous leaching model described by pore diffusion control.
The particles of the ground ore that are subjected to leaching are not identical but have the distributed
properties like size, density, mineralogy, morphological properties, uranium content etc. Hence, it is
appropriate to assume that the solid phase with distributed attributes would have distributed first order
rate constant, k. Several references are available in the literature on flotation kinetics following
distributed first order rate constant (Harris and Chakravarti, 1970), from which analogy can be drawn for
developing model equation for batch leaching of uranium ore with distributed first order rate constant. A
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few population balance models addressing the heterogeneous nature of the leaching feed material are also
available in literature (Peters, 1991; Dixon, 1995).
Phenomenological modeling of extraction of a metal through leaching involves searching for a reaction
mechanism that fits best to experimental data (Fogler and Scott, 2004; Levenspiel, 2001). Often, it is
difficult to know which parameters influence the leaching efficiency, owing to the complex mechanisms
involved in both desirable and undesirable chemical reactions. The classical, one factor at a time,
methodology cannot be applied to the leaching processes in which effect of one independent variable on
the response depends on the value of another independent variable. Statistical models effectively
addresses this issue of interaction of two input variables on response (Douglas, 2013).
The commercial importance of alkaline leaching of uraniferous ores in India has increased due to the
discovery of two uranium ore deposits: Tummalapalle (Andhra Pradesh) and Gogi (Karnataka). The host
rock of former deposit is phosphatic silicious calcitic dolostone (PSCD) and that of the latter is brecciated
Limestone. The uranium resource at Tummalapalle is a low grade one (≈ 0.04% U3O8 along with 1.5%
pyrite), with proven estimates of 81,000 tons of uranium till date. Another medium-grade low-tonnage
deposit at Gogi in the Karnataka state of India also has high calcium carbonate content. Utilization of the
above two important resources of uranium in India is essential for reducing the gap between demand and
supply of uranium required for indigenous nuclear power reactors.
Understanding the dissolution of pure uranium dioxide and iron pyrite minerals is important for the
understanding of their leaching from complex natural ores. Hence, experiments were carried out on the
leaching of synthetic mixture whose composition was chosen close and intermediate to the compositions
of the above mentioned two alkaline rock hosted Indian uranium ores. This paper presents the
development of topochemical leaching model for extraction of uranium from synthetic mixture using
alkaline reagents.
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2Na4 UO2 (CO3 )3 + 6NaOH → Na2 U2 O7 + 6Na2 CO3 + 3H2 O [3]
Chemical reaction (3) precipitates uranium as Na2U2O7 if NaOH formed in reaction (2a) is not neutralized
by reaction (2b). If any pyrite (FeS2) is present in the ore, the following reaction also takes place during
alkaline leaching with Na2CO3-NaHCO3 leachants.
4FeS2 + 15O2 + 16Na2 CO3 + 14H2 O → 16NaHCO3 + 4Fe(OH)3 + 8Na2 SO4 [4]
Experimental set up for one-liter capacity laboratory autoclave consisted of two separate interchangeable
cylindrical vessels of same size (0.1 m inside diameter, 0.16 m height), one made of glass (for
temperatures and pressures below 150°C and 6 atm) and the other made of stainless steel (for
temperatures and pressures below 200°C and 50 atm pressure). Both vessels have a common top lid made
of stainless steel coupled to motor drive with a magnetic seal. It is equipped with two stage gas induction
pitched blade turbine type impeller of 0.04 m diameter (height from bottom = 0.005 m), thermo well for
thermocouple, oxygen inlet pipe, sample addition devise to add samples under high temperature and
pressure, cooling water coil, pressure sensor, rupture disk and solenoid valve to release pressure in the
reactor if it exceeds the set point. The oxygen inlet pipe is connected to an oxygen cylinder through a
mass flow controller that opens whenever there is a drop in the pressure inside the reactor. Electrical
heater was wrapped outside the stainless steel vessel and covered with insulation. The heater is provided
at the bottom for the glass vessel. Heaters of both the vessels are connected to a common temperature
indicator and controller to maintain constant temperature in the vessels. When the temperature rises
(which could be due to exothermic reactions) above the set point, water is pumped from a cooling tank
into the cooling coil provided inside the vessel.
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The pulp density in each experiment was maintained low (5% solids by weight) in order to minimize the
effect of change in pulp density when liquor samples are withdrawn periodically during experiment. In
each leaching experiment conducted with synthetic materials, predetermined amounts of the reacting
materials (UO2 and FeS2) were filled in the sample addition device of autoclave and the cap of sample
addition device was plugged. Required amounts of sodium carbonate and sodium bicarbonate, dissolved
in 700 ml of distilled water, silica and calcite powders were loaded into the autoclave. Autoclave lid was
then closed and the agitator was started at a low speed. The autoclave was heated up to 70°C during
which period the vent valve was kept open to expel the atmospheric gases like N2 out of the autoclave and
fill the autoclave with water vapor. The vent valve was then closed and heating continued. When the
autoclave attained the desired temperature, the tube connected to the sample addition device was
pressurized with O2 gas from a pressurized cylinder so that the cap of sample addition device opens and
the feed solids contained are dropped into the autoclave. The pressure of the reactor was increased to the
desired total pressure using the same gas. The agitator motor was set to the desired stirring speed. The
time course of the experiment began at this point. Leaching continued for 6 h. Small samples of leach
liquor were drawn at time intervals of 0.166, 0.333, 0.5, 0.666, 1, 1.5, 2, 2.5, 3, 4, 5 and 6 h through dip
tube and analyzed for their U3O8 and sulfate content by Spectrophotometry and Gravimetry (precipitation
with BaCl2) respectively. The U3O8 and S contents of leach residue sample obtained at the end (6 h) of
each experiment were also determined by Pellet Fluorimetry and Gravimetric techniques respectively.
The back calculated feed values of both pyrite and UO2 from the assays of leach liquor and residue were
confirmed with the original quantities of UO2 and pyrite used in each experiment.
Table 1 Scheme of experiments followed for alkaline leaching of synthetic mixture of pure materials
Parameter Levels of parameters Base level*
Concentration of Na2CO3, M 0, 0.1, 0.3, 0.5, 0.7, 1 0.5
Concentration of NaHCO3, M 0, 0.1, 0.3, 0.5, 0.7, 1 0.5
Particle size, µm 6, 44, 58, 87, 123, 253 87
Temperature, K 373, 383, 393, 413, 428 413
Oxygen partial pressure, atm 8, 9, 10 10
* Constant value while other parameters are varied
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The fractional conversion UO2, XUO2, with time in each leaching experiment is calculated from the
analysis of U3O8 in the leach liquor at time t using the Eq. 5.
Shrinking core model (Levenspiel, 2001) is considered to fit the experimental data for leaching reactions
of uranium oxide. Since experiments in the present study were conducted in an autoclave with continuous
agitation, film diffusion does not control the leaching reaction as the film layer on the particles is
continuously replaced due to agitation which leads to fast diffusion of solutes in the film. The reaction
products (reactions (1) and (2)) are soluble in lixiviant without leaving any ash product. Hence, ash
diffusion controlled mechanism is ignored, and thereby only the chemical reaction controlled model is
attempted. Du Preez et al. (1981) had also found pure UO2 leaching by carbonate medium to follow
chemical reaction controlled shrinking core model.
The plots to fit experimental data generated on alkaline leaching of uranium from synthetic mixture, to
the chemical reaction controlled topochemical model, are given in Figures 1 through 11 in the following
Sections.
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The order with respect to the Na2CO3 concentration is found to be 0.4, indicating that the conversion of
uranium increases, with increasing concentration of Na2CO3, as observed by other workers (Schortmann
and DeSesa, 1958; Torma et al., 1985).
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Figure 5: Chemical reaction controlled model plot of dissolution of uranium at different temperatures
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The Arrhenius activation energy of dissolution of UO2 at 10 atm oxygen pressure is determined to be 13.4
kJ/mol from the slope of the straight line fitted in Figure 6 whereas the Arrhenius energy found by several
other authors for dissolution of uraninite ranged from 29.2 to 54.34 kJ/mol (Sharma et al., 1996; Du Preez
et al., 1981; Schortmann and DeSesa, 1958). The difference in Arrhenius activation energies found by
different authors could be due to the difference in the origin and nature of pure uranium oxide (UO 2) used
by different workers. The synthetic UO2 used in the present study is obtained by crushing and grinding of
a sintered material.
Na2CO3=0.5 M, NaHCO3=0.5 M,
PO2= 10 atm, Temperature=413 K,
stirring speed = 1000 rpm
Figure 7: Effect of particle size on uranium leaching, plotted according to topochemical model
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Figure 8: Plot of ln (k) Vs ln (d) for uranium leaching from synthetic mixture
Na2CO3=0.5 M, NaHCO3=0.5 M,
Temperature=413 K, size=87µm,
stirring speed = 1000 rpm
Figure 10: Plot of ln (k) Vs ln [PO2] for uranium leaching from synthetic mixture
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The order of the leaching of uranium with respect to partial pressure of oxygen is observed to be 1.9, from
the slope of the straight line obtained in Figure 10, for agitation leaching conducted in the present study.
De Pablo et al. [34] observed this value to be 1 using a thin layer flow-through reactor.
Determination of apparent rate constant (ko): A linear fit is established between the 1-(1-XUO2)1/3, and
1637.3
the product term 𝑝𝑂2 1.9149 [𝑁𝑎2 𝐶𝑂3 ]0.3647 [𝑁𝑎𝐻𝐶𝑂3 ]0.4255 𝑑 −0.1735 𝑒 − 𝑇 t corresponding to all the
experiments for the time duration from 0 to 6 h to determine the apparent rate constant, k0, for uranium
dissolution from synthetic mixture, using carbonate medium. The corresponding plot is shown in Figure
11. The slope of the line, k0, is found to be 0.1147. Thus, the overall rate equation for leaching of uranium
is given by Eq. 2.
1 1637
1 − (1 − 𝑋𝑈𝑂2 )3 = 0.1147 𝑝𝑂2 1.9149 [𝑁𝑎2 𝐶𝑂3 ]0.3647 [𝑁𝑎𝐻𝐶𝑂3 ]0.4255 𝑑 −0.1735 𝑒 − 𝑇 t [2]
Figure 11: Overall rate constant for the leaching of uranium from synthetic mixture
5. Conclusion
The leaching of pure UO2 (in a time period of 0 to 6 h) from a synthetic mixture (with composition
similar to that of actual Indian uranium ores) in sodium carbonate and bicarbonate solution (using 5%
solids (w/v)), at temperatures between 373 K and 428 K (base level = 413 K), oxygen partial pressure
from 7 to 10 atm (base level = 10 atm), Na2CO3 and NaHCO3 concentrations between 0.1 M and 1 M
(base level=0.5 M), average particle sizes 6 to 253 µm (base level = 87 µm) can be described by the rate
equation
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1 1637
1 − (1 − 𝑋𝑈𝑂2 )3 = 0.1147 𝑝𝑂2 1.9149 [𝑁𝑎2 𝐶𝑂3 ]0.3647 [𝑁𝑎𝐻𝐶𝑂3 ]0.4255 𝑑 −0.1735 𝑒 − 𝑇 t
The Arrhenius activation energy of dissolution of UO2 in alkaline media is found to be 8.75 kcal/mol.
Acknowledgements
The authors thank Shri R.N. Jayaraj, Ex Chief Executive of Nuclear Fuel Complex, Hyderabad, for
providing pure UO2 samples. They also convey sincere thanks to their colleagues in chemical laboratory
of Mineral Processing Division for the timely chemical analyses of uranium and sulfur.
References
A.R. Burkin. Chemical Hydrometallurgy. Imperial College Press, London. 271, 2001.
Demirkiran Nizamettin and Kunkul Asim. Dissolution kinetics of ulexite in perchloric acid solutions.
International Journal of Mineral Processing, 83: 76-80, 2007.
G. Dixon David. Improved methods for the design of multistage leaching systems. Hydrometallurgy, 39:
337-351, 1995.
Douglas C. Montgomery. Design and Analysis of Experiments, 8th Edition, Wiley India, 2013.
P. Prosser Alan. Review of uncertainty in the collection and interpretation of leaching data.
Hydrometallurgy, 41: 133, 1996.
J.G.H. Du Preez, D.C. Morris, C.P.J. Van Vuuren. The chemistry of uranium, part XXVII. Kinetics of the
dissolution of uranium dioxide powder in a solution containing sodium carbonate, sodium bicarbonate
and potassium cyanide. Hydrometallurgy, 6: 197–201, 1981.
Fogler, H. Scott. Elements of Chemical Reaction Engineering. Prentice-Hall, U.S.A., 3rd Edition, 811,
2004.
C.C. Harris and A. Chakravarti. Semi-Batch Froth Flotation Kinetics: Species Distribution Analysis.
Trans. Am. Inst. Min. Engrs. 247: 162, 1970.
Hossain Mohammad Mohsin, Ella Ekeroth, Mats Jonsson. Effects of HCO3 - on the kinetics of UO2
oxidation by H2O2. Journal of Nuclear Materials, 358:202-208, 2006.
O. Levenspiel. Chemical Reaction Engineering. John Wiley & Sons, New York. 2001.
E. Peters. The Mathematical modelling of Leaching systems. Journal of Metals, 20-26, 1991.
W.E. Schortmann and M.A. DeSesa. Kinetics of the dissolution of uranium dioxide in carbonate–
bicarbonate solution. Proc. 2nd United Nations Int. Conf. on the Peaceful Uses Atomic Energy, 3. United
Nations, Geneva, 333–341, 1958.
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J.N. Sharma, K. Bhattacharya, R.G. Swami, S.K. Tangri, T.K. Mukherjee. Studies on the kinetics of UO 2
dissolution in carbonate-bicarbonate medium using sodium hypochlorite as oxidant. Journal of
Radioanalytical and Nuclear Chemistry, Letters, 214 (3):223-233, 1996.
H.Y. Sohn and E. Wadsworth Milton. Rate Processes of Extractive Metallurgy. Plenum Press, New York,
1979.
Song Jian, Gao Ling, Lin Jianqun, Wu Hongbin, Lin Jianquiang. Kinetics and modeling of chemical
leaching of sphalerite concentrate using ferric iron in a redox-controlled reactor. Chinese Journal of
Chemical Engineering, 21(8):933-936, 2013.
Sylvie C. Bouffard, Berny F. Rivera-Vasquez, David G. Dixon. Leaching kinetics and stiochiometry of
pyrite oxidation from a pyrite-marcasite concentrate in acid ferric sulfate media. Hydrometallurgy,
84:225-238, 2006.
A.E. Torma, N.R. Pendleton, and W.M. Fleming. Sodium carbonate-bicarbonate leaching of a new
mexico uranium ore and removal of long half-life radio nuclides from the leach residue. Uranium 2:17-
36, 1985.
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HYDROMETALLURGY OF BERYLLIUM IN INDIAN PERSPECTIVE
Abstract
Beryllium possesses remarkable physical and mechanical properties which make it a useful engineering
material in nuclear, aerospace, medical science, and electronic industries. However, beryllium being one
of the most toxic elements in the periodic table and strategic in nature, its processing and usage are
restricted to only government sectors. An indigenous beryllium technology for extraction of beryllium
from beryl ore was developed by Bhabha Atomic Research Centre, Mumbai. This paper discusses
technical advancements in hydrometallurgical processes starting from beneficiation of beryl ore to the
production of high purity beryllium hydroxide to meet the strategic requirements of beryllium
components for the Indian nuclear and space programme. The experience gained over more than three
decades in this area is discussed. This paper also covers all important aspects of beryllium extraction
technology, namely, the resources of the metal; processing of ores; production of high purity beryllium
intermediates to produce nuclear grade beryllia ceramics and its shaping into the required shapes. Beryl
lumps handpicked during mica mining are ground to -200 mesh size. The ground beryl ore is mixed with
fluorinating agent and sintered at 750°C to selectively extract beryllium value. The beryllium rich
compound is converted into high purity beryllium hydroxide using hydrometallurgical operations. The
product is calcined, milled, compacted and finally sintered into the required shapes by using CIP/VHP
techniques. The safety measures devised and installed for safeguarding personnel health, neighbourhood
environment and the waste management practices followed during production of beryllium are also
discussed.
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Hydrometallurgy & Bio-hydrometallurgy
Thermonuclear Experimental Reactor (ITER). Beryllium is also considered as a plasma facing material
(PFM) (Scaffidi-Argentina, Longhurstet al, 2000) in ITER. Beryllium metal due to its unique properties
like light weight, good dimensional stability over a wide range of temperature, high elastic modulus and
high strength to weight ratio are also considered as an attractive material in space industries. Among the
beryllium compounds beryllium oxide (BeO) has found its application because of its unique properties,
such as, highest thermal conductivity among the known ceramics, high melting point (2570°C) and high
electrical resistivity. BeO is a suitable crucible material for melting reactive metals because of its
chemical stability and refractoriness. (Saha 1994). More recently, beryllia has been selected as a support
material for satellite multiplexer application of Indian space programme. Currently,
forsterite(Magnesium silicate) is used for this purpose.Use of the BeO in place of forsterite is found to
be beneficial for superior thermal management (200W/mK vs. 4W/mK for forsterite). Because of this
unique property of beryllia the efficiency, stability and overall performance of multiplexer have found
to increase by many folds. The ever increasing number of applications of beryllium metal and beryllia
ceramic in various domains of science and technology stimulated us to develop an efficient method of
beryllium extraction from its ore and its processing to make various products. It may be mentioned here
that beryllium oxide in the form of blocks has been considered as a neutron reflector material for
upgradation of one of the research reactors in BARC.
Beryllium is a steel-gray colored metallic element. that occurs as a natural minerals. There are about 30
minerals containing beryllium, and the most significant of these are beryl (3BeO.Al 2O3.6SiO2),
phenacite (2BeO.SiO2), chrysoberyl (BeO.Al2O3) and bertrandite (4BeO.2SiO2.H2O) ( Kenneth Walsh,
2009). For commercial extraction of beryllium, mainly beryl and bertrandite ores are used. A large
number of methods have been proposed for extraction of beryllium from its ore. However, only two are
currently used for beryllium extraction from its ores. These are the sulphate and the fluoride process
( Kenneth Walsh, 2009]. The fluoride process which is more economical, less hazardous and selectively
extract beryllium from beryl has been adopted at BARC. This paper describes beneficiation and the
opening of beryl ore, production of nuclear grade beryllia and its fabrication into shapes. The safety
aspects involved in beryllium handling are also covered.
In India, fairly large deposits of beryl ore are available in Andhra Pradesh, Bihar, Rajasthan, and Tamil
Nadu. Indian beryl ore containing 11-12% BeO, 19% Al2O3, 64% SiO2 and 3% Fe2O3 is used as input
source for beryllium extraction.
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During sintering the following reaction takes place rendering beryllium as sodium beryllium fluoride
(Na2BeF4) which is a water soluble compound.
3BeO Al2O3 6SiO2 + 2Na2SiF6 + Na2CO3 3Na2BeF4 + Al2O3 + 8SiO2 + CO2 (1)
One of the primary advantages of using sodium silico-fluoride process is that it selectively attacks
beryllium values in the ore; thereby reducing reagent consumption and also making it easier to separate it
from aluminium and silica. It may be mentioned here that in some batches sodium silico fluoride is partly
replaced by iron cryolite, a by-product produced during effluent treatment.
The sintered mass is wet ground in a ball mill after size reduction in jaw crusher and sodium beryllium
fluoride is leached out using water. The sintered mass leached three times to extract as much sodium
beryllium fluoride as possible. The leach liquor contains sodium beryllium fluoride equivalent to 5 g of
beryllium oxide per liter. Traces of silica, iron, and aluminium are also present in the leach liquor. The
leach liquor is filtered in order to separate it from solid mud residue. The red mud which contains about
0.8% beryllium is disposed off after proper treatment.The filtered leach liquor is then allowed to stand
overnight in order to let the sub micron silica particles agglomerate and settle down. The resultant aged
leach liquor, is again filtered to remove fine solids and is transferred to the precipitation tank. The sodium
beryllium fluoride is precipitated as beryllium hydroxide by the addition of sodium hydroxide at a
temperature of 90°C and a pH of 11.5. The beryllium hydroxide cake is separated from the filtrate using a
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Hydrometallurgy & Bio-hydrometallurgy
vacuum pan filter. Beryllium hydroxide so obtained is 98% pure and it is called technical grade beryllium
hydroxide. This beryllium hydroxide is calcined to produce BeO powder that is used for making melting
crucible. For nuclear application the beryllium hydroxide precipitate obtained is further purified and
calcined to give nuclear grade beryllium oxide. The purification process is described below.
For purification of beryllium hydroxide solvent extraction (Zaki, Ismail et al. 2005), ammonium
carbonate and beryllate methods have been reported in literature (Saha S, 1994). In the first step, the
technical grade beryllium hydroxide is dissolved in 9N sulphuric acid to give beryllium sulphate solution.
One of the major impurities in the solution is reactive silica, which is removed by dehydration with
sulphuric acid. The solution is immediately filtered to remove the precipitated silica. Water soluble
sodium beryllate (Na2BeO2) is produced by excess addition of 40% sodium hydroxide solution in the
filtrate. This solution is filtered to remove hydroxides of iron, magnesium, copper, nickel. Alumininum
remains in the solution as sodium aluminates along with sodium beryllate. This solution is boiled to
precipitate beryllium hydroxide. In this process, aluminium (present as aluminate) does not get
hydrolyzed and remains in the solution. The beryllium hydroxide precipitate is filtered out and washed
thoroughly to remove sodium salts from the precipitate. Since large amounts of caustic soda are used in
the process, it becomes necessary to wash the precipitate with hot water to increase the efficiency of
washing. The beryllium hydroxide precipitate is dried to remove water and calcined at 1100 oC to give
nuclear grade beryllium oxide (Beryllia) powder ( 99.6 % pure). The process flow sheet for production
of nuclear grade beryllium oxide is presented in Figure 1. The calcined powder was analysed for
impurities by using DC arc spectrophotometer (DC arc carrier distillation method). The chemical assay of
a typical batch is shown in Table 1. The elemental analysis of nuclear grade beryllia indicated purity
level 99.6% with crucial elemental levels, including boron, cadmium and lithium well belowthe
required nuclear grade powder.
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PRICIPITATION &
RE-DISSOLUTION NaOH
Na2BeO2
FILTRATION
HYDROLYSIS WATER
Be(OH)2(99.6% Pure)
Be(OH)2
LIQUID WASTE CENTRIFUSING
DRYING 950C
CALCINATION 10000C
BeO POWDER
Figure 1: Process flow sheet for production of nuclear grade beryllium oxide
Beryllia powder is consolidated to blocks, as required for end applications, by hot pressing or cold
pressing and sintering. The next requirement was to develop a suitable process for densification because
beryllia block of specified shape and density is requiredfor research nuclear reactors.
Elemental Al B Ca Cd Cr Cu Fe Li Mg Mn Na Ni Si Zn
impuritie in
ppm
Crude BeO 2000 <5 1000 <5 <10 20 510 66 2000 270 2350 90 >2000 <40
The calcined powder having an average particle size of 13 µm was ball milled for 24h and the average
size was reduced to 1.4 µm. The milled powder was dried and compacted at a pressure of 150 MPa. The
green compacts are sintered in air at 1700 oC. For achieving near to theoretical density BeO powders are
vacuum hot pressed at 1600 oC under 30 MPa pressure using graphire die toolings. A process flow sheet
developd for fabrication of beryllia blocks is presented in Figure 2.
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Use of recycled fluoride byproduct: Iron cryolite is one of the by-products in the hydrometallurgy
process practiced in BARC. In order to reduce burden on the environment attempt was made to use iron
cryolite as a fluorinating agent for opening of ore thus reducing the consumption of sodium silicofluoride.
It was observed that recovery increases when iron cyolite is used for opeing of ore.
Leaching parameters: Recover recreases with multiple leaching. During the leaching process, it was
observed that more than 90% of beryllium could be extracted in first three leaching stages. There is scope
of further improving the recovery but this gives additional load on the effluent treatment area. Hence, in
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the flowsheet three leaching have been adopted. Cold leaching was preferred over hot leaching to avoid
leaching of excess silica into the product.
Nature of beryllium hydroxide precipitate: To minimise the silica content in beryllium hydroxide it is
desirable to form granular precipitate having good filterability. It was observed that precipitation at 95°C
gives a filterable and granular precipitate.
Quality of calcined BeO powder: In order to achieve density close to theoretical density it is desirable
that the powder is free from hard aggregates. The calcined powder is required to be ball milled to break
the agglomerates. Using the ball milled powder density close to 95% of the theoretical density is
achieved in conventional cold pressing and sintering approach. Hot pressing has been adopted whenever
density above 97% of theoretical density is required.
Beryllium is considered as one of the most toxic elements in the periodic table. Excess inhalation of
beryllium in the form of fumes or dust causes lung disease which is treatable but no curable. Skin and
eye contamination with soluble beryllium compounds causes skin dermatitis and eye conjuctivity
respectively. Beryllium is confirmed human carcinogen. Beryllium has the lowest threshold limit value
(TLV) i.e. 2.0µg/m3. However, its ill effects can be controlled to a satisfactory level by implementing
suitable control measures. In the present facility, for protecting the health of personnel engaged in
beryllium processing, engineering, personal, medical and administrative control measures have been
implemented. Local exhaust ventilation and fifteen air changes per hour have been provided in the
facility. To protect the neighbourhood environment, process exhaust emissions are filtered through two
layers of high efficiency particulate filters (HEPA) before discharging to the environment through 30
meters high stack. All personnel have been provided respiratory protection during handling of beryllium.
Industrial hygiene surveillance has been provided to monitor air, surface and effluent levels of beryllium.
Liquid effluent generated in the facility is treated in-house to bring down beryllium levels below the
discharge standard. Solid waste generated during the hydrometallurgical process, is being vitrified to
reduce leachibility, and packed in plastic drums prior to its near surface disposal.
6. Conclusions
The hydrometallurgical process developed at BARC is being used suceessfully to produce beryllium
hydroxide with more than 90% recovery. Beryllate process has been integrated in the process flow sheet
in order to produce nuclear grade BeO for use in nuclear reactor. The developed process is useful to
remove efficiently undesirable impurities in the end product, beryllia. Iron cryolite by-product has been
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judiciously recycled in the process flow sheet to reduce envirimental burden of fluoride. The vacuum hot
pressing as well as cold isostatic techniques were found suitable for fabrication of beryllia ceramic as per
the specifications provided by the end users. The control measures adopted during beryllium processing
found to be adequate in maintaing personnel exposures well below the permissible values.
References
Scaffidi-Argentina F, Longhurst GR, Shestakov V, Kawamura H (2000) Beryllium R&D for fusion
applications. Fusion Engineering and Design 51: 23–41.
Kenneth A. Walsh. Beryllium Chemistry and Processing.ASM International, 2009.
Saha S (1994) Preparation of high purity beryllia and synthesis of alexandrite. Mineral Processing and
Extractive Metallurgy Review 13: 69-75.
Zaki EE, Ismail ZH, Daoud JA, Aly HF (2005) Extraction equilibrium of berylliumand aluminium and
recovery of beryllium from Egyptian beryl solution usingCYANEX 921. Hydrometallurgy 80: 221–231.
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INDIAN STRATEGIC MINERAL – A REVIEW
Patel Himeshkumar Ashokbhai* and Suchit Sharma
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad, India
*Corresponding author: himeshpatel.ism@gmail.com
Abstract
As an aspiring super power, India’s demand for energy resources including petroleum and nuclear energy
is likely to increase manifold. It is no surprise that a third of 51 countries’ foreign exchange is fed into
procuring crude oil and stocks of industrial and strategic minerals. These are vital to India’s all over
development and its power projection strategy in south East Asia.
The present paper aims to review India’s strategic mineral scenario. It reviews strategic mineral
production, utilization and imports in the country. Due consideration has been given to study the
exploration, prospects in strategic mineral, petroleum, and future and healthy demands’ trends. The paper
underlines that apart from uninterrupted imports, storage and availability of strategic minerals during the
time of crisis will be equally important. Hence, above factors will determine India wartime readiness
whether or not and dream of becoming a super power is realized.
Keywords: Industrial minerals, strategic minerals, sustainability of India.
1. Introduction
Development of mankind can be partially attributed to abundant natural resources that they can control to
fuel its ambitions. However, due to emergence of Nation states and other similar institutions, competition
has intensified over the control of these resources. In this respect, some vital minerals which are very
important for maintaining sovereignty of a country come under the category of strategic minerals. The
importance of strategic minerals can be gauged from their importance in international geo-politics.
Probably, the first attempt to define strategic materials was made by the US Army and Navy Munitions
Board following World War I. Two classifications were identified: strategic materials and critical
materials. Strategic materials were distinguished by their essentiality to the national defence, their high
degree of important reliance in wartime and the need for strict conservation and distribution control.
Critical materials were considered less essential and more available domestically, requiring some degree
of conservation. Post-1994, the US agencies have stopped using the terminology critical materials, and
identified them as either those materials being essential in war or those that would require prior
provisioning or stockpiling. In general, the terminology “critical materials” have been rarely used in the
literature. Broadly, strategic materials could be defined as the materials needed for the military, industrial
and essential civilian needs of a state during a national emergency and material not found or produced in
sufficient quantities to meet such needs of the state such as Aluminium, Antimony, Chromium,
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Columbium, Copper, Iron Lead, Manganese, Mercury, Molybdenum, Mica, Nickel, Petroleum, Platinum,
Potash, Sulphur, Tantalum, Tin, Tungsten, Uranium, Vanadium, Zinc. In general, strategic materials are
viewed as key resources that transcend individual industries in their application.
In respect of strategic minerals, India is well supplied in some of them and even has considerable
exportable surpluses but she lacks in other notably critical minerals. Critical minerals are minerals of
essential uses, the supply and procurement of which in adequate amount in the event of any national
emergency is uncertain, then there are serious issues to be addressed. Critical minerals which are in
deficit supply in India notably are petroleum and petroleum products, sulphur, base metals e.g. lead, zinc,
copper, nickel, tin, mercury and platinum, and minerals, e.g., industrial diamonds, graphite, alkalis,
potash, cryolite, selenium, etc. India's resources in strategic minerals of world importance are: abundant
and rich iron ores, ores of manganese, titanium, thorium and of the light alloy metals, aluminium and
magnesium. There is a sufficiency of ores of Ferro-alloy metals, chromium, vanadium, tungsten and flux
minerals, refractory, abrasives, bauxite, the industrial clays, while its resources of mica, manganese
ilmenite, monazite and beryl, essential for a wide variety of strategic uses, India occupies a commanding
position.
2. List of Minerals Discussed in the paper
2.1 Aluminium
The aluminium industry in India is strategically well-placed and ranks seventh largest in the world with
discernible growth plans and prospects for the future. India's rich bauxite mineral base renders a
competitive edge to the industry as compared to its counterparts globally. The aluminium industry in
India scaled lofty notches since the establishment of the first manufacturing company, namely, Indian
Aluminium Company (INDAL) in 1938. All business activities of INDAL have been merged
subsequently with HINDALCO Industries Limited. National Aluminium Co. Ltd., Hindalco Industries
Ltd., Bharat Aluminium Co. Ltd., and Vedanta Aluminium Ltd (VAL) are at the forefront of aluminium
production. The total annual installed capacity of aluminium in the country has risen to 19.07 lakh tpy
during 2012-13. The actual production of aluminium comes from a plant capacity of 17.67 lakh tpy as
capacity of 1.40 lakh tpy is presently non-operational. The installed capacity of alumina plants in the
country was 48.85 lakh tpy, out of which, the plant capacity of 46.00 lakh tpy reported alumina
production during the year. Alumina capacity of 2.85 lakh tpy remained non-operational.
2.2 Antimony
Antimony is a strategic metal. The predominant ore of antimony is stibnite composed of antimony
trisulphide, Sb2S3, (Sb 71.4%). The occurrence of antimony in the earth’s crust ranges from 0.2 to 0.5
parts per million. Antimony is geochemically categorised as a chalcophile, occurring with sulphur and
associated with heavy metals, lead, copper and silver. The metal is obtained commonly as a by-product in
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lead-zinc, silver smelting. Presently, there is no production of antimony in India. The entire requirement
of antimony in the country is met through imports of its ore and concentrates. Total resources are
estimated at 10,588 tonnes ore with metal content of 174 tonnes, all in inferred category in Lahaul & Spiti
district, Himachal Pradesh. Antimony and its alloys find numerous applications in a wide range of high
technology industries like electronic, space and defence, photographic materials, electroplating, besides
cosmetic, paint, plastics and textile industries. Traditionally, it is used in type metal and other alloys.
Imports of antimony ores and concentrates increased considerably to 4,917 tonnes in 2012-13 from 3,712
tonnes in the previous year. Imports were mainly from South Africa (92%), China and Singapore (2%)
each. Import of antimony alloys and scrap increased drastically in 2012-13 from 380 tonnes in the
previous year to 769 tonnes in the current year.
2.3 Coal
India has the world’s 4th largest coal reserves and is 3rd largest producer with 565.64 million-tons of coal
mined in 2013-14. In India, coal is the bulk of the primary energy contributor with 54.5% share out of the
total 595 Mtoe (Million Tonnes of Oil Equivalent) produced in 2013-14.The Indian coal deposits are
primarily concentrated in the Gondwana sediments occurring mainly in the eastern and central parts of
Peninsular India, although Gondwana coal deposits also occur in Assam and Sikkim in north eastern part
of the country. The Tertiary coal-bearing sediments are found in Assam, Arunachal Pradesh, Nagaland
and Meghalaya. As a result of exploration carried out by GSI, CMPDI and other agencies, 293.50 billion
tonnes (including that estimated in Sikkim) coal reserves up to 1,200 m depth have been established in the
country as on 1.4.2012. Out of these reserves, 118.15 billion tonnes were proved reserves, 142.17 billion
tonnes were indicated reserves and the remaining 33.18 billion tonnes were in inferred category. Of the
total reserves, prime-coking coal reserves were 5.31 billion tonnes, medium-coking & semi-coking
reserves were 28.38 billion tonnes and non-coking coal including high sulphur reserves were 259.81
billion tonnes. Indian lignite deposits occur in the tertiary sediments in the southern and western parts of
peninsular shield particularly in Tamil Nadu, Pondicherry, Kerala, Gujarat, Rajasthan and Jammu &
Kashmir. The total known geological reserves of lignite as on 1.4.2012 were about 41.96 billion tonnes.
Of which, 81% reserves are located in Tamil Nadu with about 33.88 billion tonnes. Other states where
lignite deposits have been located are Gujarat, Jammu & Kashmir, Kerala, Rajasthan, West Bengal and
the Union Territory of Puducherry. Coal is chiefly used for power generation, cement making, iron &
steel and syn-gas production. Coal India Limited (CIL) an Indian state-owned coal mining company
headquartered in Kolkata, West Bengal is the largest coal producer with 81% of coal production in India.
Since Indian coals are of average quality, India imported high quality coal of about 102.85 million tons in
and exported 2.03 million tons in 2011-12. Coal imports far exceeded exports with net import of 100.82
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million tons in 2011-12.The demand for coal is only to shoot up and further complicate India’s energy
security.
2.4 Copper
Copper is an important non-ferrous base metal having wide industrial applications, ranging from defence,
space programme, railways, power cables, mint, telecommunication cables, etc. India is not self-
sufficient in the resources of copper ore. In addition to domestic production of ore and concentrates,
India imports copper concentrates for its smelters. The domestic demand of copper and its alloys is met
through domestic production, recycling of scrap and by imports. The total resources of copper ore (as on
1.4.2010 as per UNFC system) are estimated at 1.55 billion tonnes. Of these, 394.37 million tonnes
(25.31%) fall under 'reserves' proved (STD111) and probable (STD121 & 122) categories) while the
balance 1.16 billion tonnes (74.69%) are 'remaining resources' (under feasibility (STD211), pre-feasibility
(STD221 & STD222), measured (STD331), indicated (STD332) and inferred (STD333) categories). Of
the total ore resources, 2.64 million tonnes (0.16%) comprise ore containing 1.85% Cu or more and 676
million tonnes (43.38%) of 1% to below 1.85% Cu grade. Now with regard to reserves of copper, there
were no reserves above 1.85% Cu grade. However, 381.69 million tonnes fall under 1% to below 1.85%
Cu grade. The total copper metal content in the resources is 12.28 million tonnes of which 4.76 million
tonnes constitute reserves.
2.5 Iron
Steel is decidedly the vital component of a country’s economy and is considered amongst the driving
force of modernisation. The level of per capita consumption of steel is treated as one of the important
indicators of socioeconomic development and living standards in any country. Steel continues to be the
foremost engineering material, environment-friendly and recyclable. The finished steel production in
India has grown from a mere 1.1 million tonnes in 1951 to 81.68 million tonnes in 2012-13. India ranked
fourth as a largest producer of crude steel in the world and is expected to be the 2nd largest producer by
2015-16, provided all requirements for fresh capacity creation are met.
2.6 Ferro-Alloys
Ferro-alloys are one of the important inputs in the manufacture of alloys and special steel. Ferro-alloys
impart special properties to steel. The alloys provide increased resistance to corrosion, improve hardness
and tensile strength at high temperature, give wear and abrasion resistance and increase creep strength etc.
The growth of Ferro-alloys Industry is, thus, linked with the development of the Iron and Steel Industry,
Foundry Industry and to some extent Electrode Industry. The principal ferro-alloys are chromium,
manganese and silicon. Ferro-alloys are classified into two main categories, viz, bulk ferro-alloys and
noble ferro-alloys. Due to high cost of power, Ferroalloys Industry has not been operating to its full
capacity in India. Ferro-alloys Industry spends 40 to 70% production cost on power consumption. The
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power consumption per tonne of ferroalloys production in the country varies from 3,000 to 12,000 kWh.
As per Indian Ferro-Alloys Producers' Association (IFAPA), the total installed capacity of bulk Ferro-
alloys Industry in India is estimated at 5.15 million tonnes per annum and for noble Ferro-alloys it is
50,000 tonnes per annum. The Industry is reported to be working at about 60-65% capacity utilisation. In
2012-13, exports of ferro-alloys increased to 16, 83,184 tonnes valued at `10,196 crore from 15, 32,694
tonnes valued at `8,399 crore in the previous year. In terms of quantity, exports of ferro-silico-manganese
accounted for 58%, followed by ferro-chrome (31%), ferromanganese (9%) and ferro-silicon (1%) in
201213. The other ferro-alloys together accounted for remaining 1% of exports. Exports were mainly to
China (15%), Korea Rep. and Japan (13% each), Italy (9%), Netherlands (8%), Chinese Taipei/Taiwan
(7%), Turkey (5%), Thailand (3%) Malaysia (2%). Imports of ferro-alloys increased from 2, 78,759
tonnes valued at `2,975 crore in 2011-12 to 2, 79,513 tonnes valued at `3,580 crore in 2012-13.
2.7 Lead & Zinc
The total resources of lead and zinc ores in India as of 2010 were estimated at 685.59 million tonnes. In
terms of reserves, 2.24 million tonnes of lead metal and 12.45 million tonnes of zinc metal were
estimated. Rajasthan is endowed with the largest resources of lead-zinc ore amounting to 607.53 million
tonnes (88.61%), followed by Andhra Pradesh 22.69 million tonnes (3.31%), Madhya Pradesh 14.84
million tonnes (2.16%), Bihar 11.43 million tonnes (1.67%) and Maharashtra 9.27 million tonnes
(1.35%). Resources are also established in Gujarat, Meghalaya, Odisha, Sikkim, Tamil Nadu,
Uttarakhand and West Bengal. Among major industries utilizing lead, battery industry consumes about
majority of lead followed by pigments and compounds, rolled and extruded products, alloys, cable
sheathing and the balance is consumed by other industries. Owing to its corrosion resistance in varying
types of environment, zinc is used for protecting steel by way of galvanizing and therefore used in
galvanizing industry.
2.8 Molybdenum
Molybdenum (Mo) is a refractory metal used principally as an alloying agent in steel, cast iron &
superalloys to enhance strength, wear resistance and corrosion resistance. It does not occur in nature in
free-state. Usually, it is found in chemically combined form with other elements. Molybdenite (MoS 2) is
the principal ore of molybdenum. About two-thirds of global molybdenum production is as by-product of
copper mining and only about one-third is obtained from primary molybdenum mines. In India, by-
product concentrates of molybdenum are produced intermittently from uranium ore of Jaduguda mine
belonging to Uranium Corporation of India Ltd (UCIL) in Jharkhand. The internal demand for
molybdenum and its products is met mostly through imports. India continues to lack in several critical
minerals and one of them is molybdenum. In India, molybdenum is associated generally with copper, lead
and zinc ores. Rakha copper deposit in Jharkhand contains 45 to 48 ppm molybdenum. Malanjkhand
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copper deposit in Madhya Pradesh contains 0.04% recoverable molybdenum. Molybdenum is a versatile
alloying agent for alloy steel, cast iron, nickel, cobalt and titanium alloys. Imports of molybdenum ores &
concentrate increased to 6,861 tonnes in 2012-13 from 5,223 tonnes in the previous year. Imports were
mainly from Chile, USA, Thailand & Mexico.
2.9 Natural Gas
Natural gas is an important clean energy source and fuels fertilizer industry, power generation,
petrochemicals, CNG and LPG, steel etc. Natural gas reserves in India stood at 1.241 trillion cu.m. (1
January 2013 EST.). Gross Production of Natural gas stood at 35,390.91 million cu.m. in 2013-14. LNG
import was at 14,257 million cu.m. or 29% of total consumption of 48,811.64 million cu.m. Major LNG
producing sites is western offshore regions, particularly the Mumbai High Complex. The onshore fields in
Assam, Andhra Pradesh, and Gujarat states are also major producers of natural gas. At present, the
country has a gas pipeline network length of 14,987 Km having capacity of 401 MMSCMD spread over
15 States & UTs. Relative to crude oil, India imports only small fraction of consumption. State companies
of ONGC and OIL remain major players in the production of Natural Gas.
2.10 Nickel
When added in small quantity to iron, increases its properties manifold and makes the product hard. The
reason behind the demand of primary nickel all over the world is for the production of stainless steel.
When it is used in plating, it makes the surface tarnish-resistant and provides polished appearance.
Important occurrence is nickeliferous limonite in the overburden of chromite in Sukinda Valley, Jajpur
district, Odisha, where it occurs as oxide. As per UNFC, as on 1.4.2010, the total resources of nickel ore
have been estimated at 189 million tonnes. About 92% resources i.e. 175 million tonnes are in Odisha.
During 2012-13, imports of nickel ores & concentrates decreased manifold to only 865 tonnes in
comparison to 41,729 tonnes in the previous year. Imports were mainly from Australia & China. Imports
of nickel & alloys including scrap were 54,424 tonnes in 2012-13 compared to 34,787 tonnes in the
previous year. Over 60% of world nickel demand is for the production of stainless steel. Nickel accounts
for 10 to 20% input cost in stainless steel production depending on the nickel content. The future outlook
for nickel depends mainly on the production of stainless steel which is one of the main drivers for nickel
produced. The production of stainless steel is estimated to be 5 million tonnes by 2016-17 as per the 12th
Five Year Plan Report.
2.11 Petroleum
India is historically deficit in petroleum with current estimated reserves at 1190.3 million tonne. The
combination of rising oil consumption and fairly unwavering production levels leaves India highly
dependent on imports to meet the consumption needs. Most of India's crude oil reserves are located in the
western coast (Mumbai High) and in the northeastern parts of the country, although considerable
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undeveloped reserves are also located in the offshore Bay of Bengal and in the state of Rajasthan. India
consumed 158.2 MMT (Million Metric Tonnes) (source:http://petroleum.nic.in) in 2013-14 and produced
220.2 MMT of petroleum products. However, crude production in India remained at 37.8 MMT, falling
way short of 143.8 MMT imports of crude oil and 12.0 MMT of POL(Petroleum Products). Hence, Gross
Petroleum Imports stood at 155.8 MMT with whopping Import Dependency (Based on Consumption) of
77.6 %. These imports were 34.5% of India’s Gross Imports of $ 450.9 billion equalling $155.56 billion.
Major oil producing companies are state owned with ONGC (Oil & Natural Gas Corporation) producing
55% of total crude, Oil India Limited producing 10% and rest being produced by JVs/Pvt companies. As
part of the effort to improve domestic production, the Ministry of Petroleum and Natural Gas crafted the
New Exploration License Policy (NELP) in 2000, which permits foreign companies to hold 100% equity
possession in oil and natural gas projects. However, to date, only a handful of oil fields are controlled by
foreign firms. India’s downstream sector is also dominated by state-owned entities, though private
companies have enlarged their market share in past recent years
2.12 Platinum & Palladium
They belong to platinum group of metals (PGM). Major applications of platinum and palladium are in
automotive sector for emission control and in chemical and petroleum refining. The major part of 15.7
tonnes UNFC resources of PGMs estimated so far, i.e. 14.2 tonnes are located in Nilgiri, Boula-Nuasahi
and Sukinda areas in Odisha and remaining 1.5 tonnes in Hanumalpura area in Shimoga schist belt of
Karnataka. About 49% resources are in pre-feasibility category and the remaining in inferred and
reconnaissance category. Platinum and palladium are primarily used as catalyst in controlling the toxicity
of emissions from automobile, chemical and petroleum refining plants. Nearly half of the total platinum
used worldwide is as catalysts in catalytic converters in automobiles. Catalysts for automobile sector use
platinum and palladium. Automobiles that run on diesel predominantly use platinum for catalytic
conversion. The chemical inertness and refractory properties of these metals are conducive for their
applications in electrical, electronics, dental, medical fields and glass industry. India is not a platinum
group of elements (PGEs) producing country and is meeting its demand entirely by imports. The demand
for PGEs is expected to touch 80 tonnes by 2017 and may touch 120 tonnes by 2025, as per the Report of
the Sub Group for 12th Plan period.
2.13 Tin
Tin is one of the earliest metals known and used mainly in bronze implements. It is a scarce element
having an incidence of about 2 ppm in the earth's crust. Its unique combination of properties like non-
toxic nature, high malleability, chemical inertness and ease with which it can form an amalgam and alloy
with other metals has given it a special status among non-ferrous metals. Pure tin is a silvery-white metal
which is soft and malleable. It does not occur naturally as metal. By far, the most important tin mineral is
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cassiterite (SnO2), which, in its purest form contains 78.6% tin. The less common tin ore is stannite
(Cu2SnFeS4). Tin is now used mostly for tin plating, soldering special alloys and in making bronze.
Chhattisgarh was the only state producing tin concentrates. The production of tin concentrates in 2012-13
was 47,776 kg as against 48,765 kg in the preceding year. Six mines, one in public sector and five in
private sector reported production in 2012-13. All these mines are located in Dantewada district of
Chhattisgarh. The mine-head stocks of tin concentrates were 23,733 kg at the beginning of the year as
against 46,503 kg at the end of the year. Tin Metal plant owned by Precious Minerals and Smelting
Limited reported production of 13,938 kg of tin metal in 2012-13 against 23,451 kg in the preceding year.
An import of tin ores and concentrates was 21 tonnes in 2012-13 from negligible quantity in the previous
year. Imports were only from Nigeria. Imports of tin and alloys including scrap were 7,803 tonnes in
2012-13 and 8,055 tonnes in the previous year. Out of the total imports in 2012-13, tin and alloys
comprised 7,638 tonnes, tin and alloys (worked, NES) 165 tonnes, tin & alloys (NES) 77 tonnes, tin &
alloys (worked) 145 tonnes, anode/cathode, etc. of tin unwrought 7,169 tonnes, tin blocks 247 tonnes and
tin (scrap) negligible quantity. Worldwide demand for primary tin was expected to increase at moderate
annual rate. The rate of increase, however, could balloon or go up in a few years if new applications
continue to find acceptance in the market place, especially in the electronics (solder) field. ITRI estimated
that global tin demand in 2015 would be about 400,000 tonnes per year.
2.14 Tungsten
The total in situ recoverable reserves in India of tungsten ore are estimated at 43.15 million tonnes or
1,32,478 tonnes in terms of tungsten (WO3) content. The yearly production is 45 to 50 thousand kg of ore.
This is not sufficient to meet our requirements and parts of the domestic requirements are met by imports.
Deposits of wolframite, the chief ore of tungsten, are found in Degana (near Rawat Hills) in Rajasthan
and Chendpathar in Bankura district of West Bengal. Seven mineralized zones in Sakoli basin in
Bhandara and Nagpur districts of Maharashtra have also been identified. The tailings of the Kolar gold
field in Karnataka have been reckoned as potential source of scheelite. Some deposits are also found in
Kangundi area of Chittoor district at Rampachadodavaram in East Godavari district of Andhra Pradesh,
Ahmedabad in Gujarat and Singhbhum in Jharkhand. Haryana and West Bengal also have some deposits
of tungsten. The main use of tungsten is in the form of ferro-tungsten in the making of special and alloy
steels.
2.15 Uranium & Thorium
Uranium reserves in India stood at 80,200 tonnes or 1.5% of global reserves in 2009. At the same time
India is considered to have 25% of thorium reserves in monazite sands of coastal regions of South India.
Of the total uranium sources identified so far, Jharkhand accounts for about 45%, Andhra Pradesh 26%,
Meghalaya 16%, Rajasthan and Karnataka 4% each. Uranium and Thorium are the pillars of India’s
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three-stage nuclear policy that aims to secure country’s long term energy dependence through nuclear
power. Stage 1 is PHWR (Pressurised Heavy Water Reactors), Stage 2 being Fast Breeder Reactors and
Stage 3 being Thorium Based Reactors. Currently, twenty-one nuclear power reactors have a total install
capacity of 5,780.00 MW (3.5% of total installed base).Uranium Corporation of India (UCIL) is centrally
owned Public Sector Undertaking (PSU) under the Department of Atomic Energy entrusted with uranium
mining and processing in India. It should be noted that India now envisages increasing the contribution of
nuclear power from 3.5% to 9% within 25 years. By 2020, India is to have total nuclear power generation
capacity of about 20,000MW. However due to decommissioning of Jaduguda mine in Jharkhand in 2014,
domestic production of the yellow cake has declined by 10-15%.Department of Atomic Energy sources
said that it has taken steps to increase the production from other mines to maintain the supply and
demand, but the low quality of ore from other mines has led to increase in the production cost. Apart from
importing uranium from Kazakhstan and Russia, India is in the process of getting the ore from Australia,
with which it inked a pact for the same, few years back. Also, with passing of US-India Civil Nuclear
Agreement in 2005, India will now trade civilian grade nuclear material and technologies with other
countries. On military side, India is one of the 5 nuclear-weapon states (NWS). Though India has not
made any official statements about the size of its nuclear arsenal, recent estimates suggest that India has
between 90 and 110 nuclear weapons consistent with earlier estimates that it had produced enough
weapons-grade plutonium for up to 75–110 nuclear weapons. In 1999 India was estimated to have
4,200 kg of separated reactor-grade plutonium, enough for approximately 1,000 nuclear weapons. India
has close ties with Russia for supplying nuclear material.
2.16 Vanadium
The total estimated resources of vanadium ore in India as of 2010 are placed at 24.72 million tonnes with
an estimated V2O5 content of 64,887 tonnes. Out of the total resources, the reserves of 0.41 million
tonnes are having 1,603 tonnes of V2O5 content while the remaining resources are 24.31 million tonnes
having 63,284 tonnes of V2O5. Chief producer states are Karnataka, Maharashtra and Orissa. It is used
primarily as an alloying element in iron & steel industry and to some extent as a stabiliser in titanium and
aluminium alloys which are used in aerospace applications. Ferro-vanadium producing units in India
consume either imported V2O5 concentrates or indigenous vanadium sludge. The domestic availability of
vanadium sludge from aluminium industry is limited for ferro-vanadium production and gap is met by
imports. In future also, India will not be able to generate adequate quantity of vanadium sludge to meet
the internal demand. On the other hand, with growth of automobile and casting sectors, demand for ferro-
vanadium is expected to increase and this has to be met by imports.
3. Conclusions
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After a thorough study of strategic mineral situation in India, one can understand that India is blessed in
some important strategic minerals like bituminous coal, industry grade iron ore etc. but is seriously
lacking in others notably Sulphur, Lead, Petroleum, Zinc, Mercury, Platinum, Nickel, Graphite, Tin,
Ferro-tungsten. This state of disequilibrium in the country's mineral economy may not be apparent in time
of international peace, but is a source of great danger to national security in a war or emergency; when
imports of essential commodities for example petroleum may be stopped and the off-take of credit
earning exports may face economic slump. Hence it is vital to come up with strategies to mitigate their
effects. It can do this by building up a strong peace-time industry that profitably mines, stockpiles and
processes into final products. In case of unavailable minerals the government can arrange for off-set
surpluses against deficiencies by exchange or barter. Other measures may include State controlled
stockpile of essential minerals and raw materials as previously discussed. Here it should be noted that
keeping stockpile of 13 essential strategic, India can assure its sovereignty. Parallel on R&D side,
attention should be given to developing substitutes and synthetics. However it should be brought to notice
that India till now has done commendable job in achieving peace and harmony in South Asia despite
strained strategic reserves and disturbing course of international events.
References
Indian Mineral Yearbook 2007/08/09/10/11/12/13
Indian Bureau of Mines (http://ibm.gov.in)
Geological Survey of India (GSI), Ministry of Mines (http://www.portal.gsi.gov.in )
Ministry of Natural Resources and Environment (http://www.mnre.gov.ws )
Ministry of Coal (http://www.coal.nic.in )
Ministry of Petroleum & Natural Gas (http://petroleum.nic.in )
Department of Atomic Energy, (http://www.dae.gov.in)
Strategic Minerals of India’ by Dr. D. N. Wadia
Defence Research & Development Organization (http://drdo.gov.in)
Indexmundi.com
wikipedia (http://en.wikipedia.com )
Ministry of Defence (http://mod.nic.in )
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Hydrometallurgy & Bio-hydrometallurgy
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A PILOT PLANT STUDY ON BENEFICIATION OF MANGAMPET BARYTE FOR DRILLING
MUD APPLICATION
Silpa Sweta Jena1*, G.Siva Kumar2 and R.Venugopal1
1
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad, India
2
Indian Bureau of Mines, Bengaluru, India
*Corresponding author: jenasilpasweta@gmail.com
Abstract
Baryte is one of the most important industrial minerals having broad industrial utilization. The chief /
primary end user of Baryte is oil & gas, chemical, paint and electronics industries. China is the leading
producer and the second place is occupied by India. Mangampet Baryte deposit of Cuddapah district,
Andhra Pradesh is the single largest deposit of its kind in the world, and is the main producer of the total
output in India. About 50% or more of the total deposit lie below stipulated grade of BaSO4 and specific
gravity by the customer industry (oil well industry) i.e. 90% BaSO4 & 4.15 specific gravity.
There is an extensive low grade Baryte generation due to hand sorting and selective mining practice. Even
after the blending of low and high grade ore to suit the specification, it is not possible to completely
utilize the entire low grade deposit. The generation of low grade ore is a continuous process and therefore
it is necessary to control the consumption of high grade deposits with upgradation and utilization of the
lean ores.
The sample was collected from Mangampet Baryte deposit. The sample was subjected to mineralogy,
sampling, sizing and chemical analysis. It was found that liberation takes place at finer sizes and thus
froth flotation process was chosen. After preliminary studies on direct and reverse flotation, the pilot scale
studies were undertaken. The sample contained 77.42% BaSO4 with a specific gravity of 3.8, which after
cleaning of rougher pyritic tails produced a concentrate assaying 89.95% BaSO4, 4.18 specific gravity,
70% yield by weight with 83.9% recovery, and on first stage cleaning of rougher baryte, float produce a
baryte concentrate assaying 93.49% BaSO4, 4.27 specific gravity, 64.3 weight percent yield with 80.1%
recovery. By combining both the concentrates, a product with 91.85% BaSO4 was obtained which is
suitable for drilling mud grade.
Keywords: Baryte, fine lean grade, froth flotation, rougher and cleaning stage.
1. Introduction
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Baryte is one of the most important industrial minerals with wide utilization. It is used in oil well industry
(drilling mud), chemical, paint, glass and electronics industries.
India is one of the major producers of barite. Mangampet baryte deposit of Cuddapah district, Andhra
Pradesh, is the only largest deposit of its kind in the world and accounts for major proportion of baryte
production in India. More than 50% of the total deposit lie below the stipulated grade of BaSO4 and
specific gravity of the customer industry(oil well industry) i.e. 90% BaSO4 and 4.15 specific gravity.
There is an extensive low grade Baryte generation due to hand sorting and selective mining practice. Even
after the blending of low and high grade ore to suit the specification, it is not possible to completely
utilize the entire low grade deposit.
The generation of low grade ore is a continuous process and therefore it is necessary to control the
consumption of high grade deposits with upgradation and utilization of the lean ores. Besides the oil and
gas industry, the demand for high quality baryte product exists in many other industries such as glass
making, barium based chemicals, electromagnectic alloys, pigment and colour, rubber etc., which
enhance the scope for beneficiation of low grade barite deposits. The present study was initiated to evolve
a basic process flow scheme at bench scale and pilot plant scale.
Sample of 0.5m was collected from Vijayalaxmi Mines and then crushed to 0.3m. Then by bulk sampling
50 ton of sample was taken for present study. The sample contains black light shale impurity in both free
form and associated form with baryte, which was removed manually and estimated to be about 7%. This
has the advantages of minimizing handling cost, power saving during comminution, less wear and tear on
process machinery and removal of pyritic gangue since it is mostly associated with shale. After hand
sorting, the material was mixed thoroughly and a representative sample for pilot plant experiments was
prepared in a pilot plant crushing section. The representative ore was fed to a double deck vibrating
screen with 50mm and 10mm aperture screen in top and bottom deck, respectively. The +50 mm size
material was crushed to -50mm in a jaw crusher. Then the -50mm, +10mm and jaw crusher product was
conveyed to a cone crusher to reduce them to -10mm. The cone crusher product was send back to the
double deck vibrating screen.
A representative sample of 250 kg was obtained after through mixing -10mm material by riffling and
coning & quartering. About 125 kg was kept reserved for future test by riffling. The rest 125 kg was
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mixed and ground to -10mesh (1.7mm) size in roll crusher and riffled into several parts, each weighing
1kg and stored.
Specific gravity: The specific gravity values of the samples were found to be 3.86. The specific gravities
are determined by Lechatelier flask since the baryte industry mainly the oil well drilling industry sets the
specific gravity with the help of Lechatelier Flask.
Characterization: A representative quantity of sample, of -200 mesh was subjected to chemical analysis
which analysed BaSO4 77.42%, SiO2 14.12%, S(T) 8.12%, S(Py) 0.39%, FeO 0.06%, Fe(T) 1.26%, Al2O3
2.84%, CaO 1.02% ,MgO 0.24%, LOI 1.14%. The liberation analysis revealed that baryte was found to
be highly liberated at 200mesh. Mineralogical studies indicated presence of Baryte along with quartz,
while clay is found in minor quantity and Pyrite, Hematite, Carbonates, Goethite and Feldspar in trace
amount.
3. Flotation experiments
The preliminary pilot scale flotation tests were conducted on -10mesh sample ground to an m-o-g of 96%
passing 200mesh as the characterization and mineralogical studies indicated that baryte is fairly liberated
at finer size. Anionic flotation of baryte needs the removal of pyrite prior to baryte flotation to avoid the
interference of pyritic gangue during baryte flotation. The anionic flotation was carried out in two stages,
Direct flotation involves pyritic flotation followed by the baryte flotation of tails obtained from pyritic
flotation. The concentrate produced from rougher baryte flotation was further subjected to cleaning stages
for increasing baryte grade which can be directly used in drilling mud application.
The m-o-g studies were carried out on material obtained after 12 minutes (d80=68 micron), 15 minutes
(d80=46micron) & (d80=40 micron) grind. From the metallurgical result, the recovery and grade as m-o-g
(d80 = 46 micron) was found to be better than those obtained at other m-o-g and therefore 90.8% passing
of -200 mesh (d80= 46micron) was selected for pilot scale flotation tests.
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3.1.1 Selection of anionic collector for direct flotation of baryte
Several tests were conducted by using different collectors for flotation of baryte from pyritic tails. The
mesh of grind, pH, pyritic flotation conditions and the dosages of anionic collector were kept consant.
1 kg of -10 mesh ore obtained from 15 minutes grinding was floated at pH 6-7 using 0.8kg/t potassium
amyl xanthate and pine oil respectively to remove pyrite. The rejects from the test was subjected to direct
baryte flotation at pH 8 using 0.32kg/t various anionic collectors and 0.38kg/t sodium silicate.
BaSO4
Collector Product Wt%
Assay% Dist.%
Rougher baryte float 66.7 93.48 82.6
Rougher baryte tails 7.3 21.96 2.0
Sodium oleate
Pyritic float rejects 18.7 53.92 13.4
Pyritic float conc. 5.0 29.41 2.0
Rougher baryte float 65.0 93.96 81.4
Sodium
Rougher baryte tails 10.3 18.12 2.5
petroleum
Pyritic float rejects 19.7 53.92 14.1
sulphonate
Pyritic float conc. 5.0 29.41 2.0
Rougher baryte float 53.7 92.73 66.5
Aero floate- Rougher baryte tails 23.2 62.96 19.5
565 Pyritic float rejects 18.1 49.98 12.0
Pyritic float conc. 5.0 29.41 2.0
From the table 1, both sodium oleate and sodium petroleum sulphonate give rougher baryte float assaying
more than 93% BaSO4 with a recovery more than 80%. As sodium oleate is cheap, easily available and
produces high recovery concentrate, it was choosen as the collector for present study.
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Pyrite flotation
pH 6-7, KAX( 0.04/ 0.06/ 0.08 kg/t), Pyrite float (reject)
Pine oil( 0.08kg/t)
The above tests indicated that high grade baryte concentrate assaying about 95% BaSO4 can be produced
with 75% recovery at 0.06kg/t of KAX and hence chosen for pyrite flotation.
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Pyrite flotation
Pyrite float (reject)
pH= 6-7, KAX=0.06kg/t, Pine oil=0.06kg/t
Baryte flotation
The above test concluded that high grade baryte concentrate can be produced with 77% recovery at
0.38kg/t of sodium oleate and hence this dosage chosen for baryte flotation.
Tests were carried out by varying the dosages of sodium silicate (gangue depressant & slime dispersant)
keeping the other conditions constant. It is ovserved that the dosage 0.83kg/t gives best result and finally
this dosage was chosen.
Pyrite flotation
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After cleaning of rougher baryte, pyritic tails produced a concentrate assaying 89.95% BaSO4, 4.18
specific gravity, 70% yield by weight with 83.9% recovery and on first stage cleaning of rougher baryte
float produce a baryte concentrate assaying 93.49% BaSO4, 4.27 specific gravity, 64.3 weight percent
yield with 80.1% recovery. By combining both the concentrates a product with 91.85% BaSO4 was
obtained which is suitable for drilling mud grade.
Flow sheet:
PYRITE
FLOTATION
70 4.18
89.95 83.9 Sodium silicate 1ST CLEANER Ba TAILS
1ST CLEANER
Ba- FLOTATION
Rejects
64.3 4.27
93.49 80.1
67.15 4.23
WT% SPEC.
91.85 82.3 GRAVITY
BaSO4 % BaSO4
GRADE DIST%
LEGAND
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5. Conclusion
The chemical analysis indicates that sample contains BaSO4 75%, SiO2 14.12%, S(T) 8.12%, S(Py)
0.39%, FeO 0.06%, Fe(T) 1.26%, Al2O3 2.84%, CaO 1.02% ,MgO 0.24%, LOI 1.14% which improved to
BaSO4 77.42% after manual ore sorting. Liberation of baryte could be obtained at the size range of 200
mesh. Mineralogical study indicates the presence of baryte (major), quartz, clay (minor), Pyrite ,
Hematite, Carbonates, Goethite & Feldspar in traces.The pilot scale flotation involves pyritic flotation
followed by the baryte flotation of tails obtained from pyritic flotation. The concentrate produced from
rougher baryte flotation was further subjected to cleaning stages for increasing baryte grade which can be
directly used in drilling mud application. Potassium amyl xanthate (KAX) was used for pyrite flotation.
Different collectors were examined for baryte flotation and finally sodium oleate was found to be
appropriate and the flotation experiments were done.The Baryte of Mangampet, Cuddapah district could
be upgraded to the 91.85% BaSO4 with 82.3% recovery which is suitable for drilling mud application.
Acknowledgements
We thank all contributors for their cooperation
References
Indian Bureau of Mines monograph on barites, mineral facts and problem no. 15, 199, pp 75-102.
Karine Pearson, Natural born fillers, vast potential on India’s door step, Industrial Minerals, August
2000, p 38.
Indian Bureau of Mines monograph on barites, mineral facts and problem no. 15, 199, pp 103-107.
Neelakantan S. et.al. Project Barytes, Mangampet, Cuddapah dist, A.P., Geological Survey of India,
1980, pp122-123.
Gaudin A.M. Principles of Mineral Dressing, TATA McGraw- Hill publishing con. Ltd., NEW
DELHI, 1980, p 522.
Weiss N. L., Mineral Processing Hand Book Vol.I, Society of Mining Engineers, New York
(AIMMPE), 1985, p 9-3.
Weiss N. L., Mineral Processing Hand Book Vol.II, Society of Mining Engineers, New
York(AIMMPE), 1985, P 30-97
Deepak Malhotra and William F. Riggs, chapter 6, Reagent Teasting Improving the odds for correct
decision, Society of Mining Engineers Inc., Colorado’1986, p 63, pp 73-74.
Neelakantan S. et.al., Project Barytes, Mangampet, Cuddapah Dist., A.P, Geological Survey of india,
pp122-123.
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CHARACTERISATION AND BENEFICIATION OF LOW GRADE MAGNESITE OF PARSHAD
AREA (UDAIPUR, RAJASTHAN)
Ajita Kumari*, Bhim Chandra Bhattacharya and R. Venugopal
Department of Fuel & Mineral Engineering, Indian School of Mines, Dhanbad
Corresponding author: akajitakumari@gmail.com
Abstract
Magnesite deposit mainly occurs in three districts of Rajasthan namely Ajmer, Pali and Rajsamand. The
deposits of these districts are of amorphous (cryptocrystalline) and are found associated with ultrabasic rocks.
Magnesite deposit of coarse crystalline variety has been first found in Parshad village of Rajasthan followed
by another three areas.
In the present work, main emphasis has been given to the characterisation and beneficiation of low grade
magnesite. Characterisation study includes mineralogy, petrography, physicochemical characteristics,
differential thermo-gravimetric analysis and X-Ray analysis. On the basis of characterisation studies, it is
found that Magnesite ore is mainly composed of Magnesite with minor amount of quartz and Iron in the form
of hematite. The methods adopted for beneficiation (Bench Scale Beneficiation studies) are flotation and
magnetic separation to remove main impurities like silica and iron. Beneficiation study has been carried out
on low grade Magnesite sample containing SiO2-6.36%, Fe2O3-5.36%, Al2O3-0.20%, TiO2-0.20%, CaO-
1.12%, MgO-37.0%, Na2O & K2O-0.20% and LOI-48.2%.
Flotation tests were carried out to determine the liberation size, mesh of grind, selection of collector,
optimisation of collector dosage, selection and optimisation of depressant, effect of pH and the optimum
conditions of flotation.
Based on the results obtained, it was observed that SiO2 is reduced from 6.36% to 1.36% and MgO is
increased from 37.0% to 42.6%. A clean concentrate of magnesite obtained is analysed to have SiO2-1.36%,
MgO-42.6%, R2O3-5.26% with a weight recovery of 65% and MgO recovery of 74.63%. Presence of 5.26%
iron oxide is allowable for refractory and allied products as it is within the maximum allowable limit of 7%.
So, it can be concluded that Parshad magnesite is amenable to beneficiation and the product is suitable for
refractory and allied products.
Keywords: Parshad magnesite rocks, characterisation studies, magnesite flotation, magnetic separation,
refractories and allied products.
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1. Introduction
The mineral Magnesite is magnesium carbonate (MgCO3), having carbon dioxide 52.4% and magnesia
47.6%. The term “magnesia” has been applied to various materials including a rock shining like silver-
perhaps with talc. As a member of the isomorphous group of minerals that include calcite and dolomite,
magnesite crystallizes in the hexagonal system and has a rhombohedral cleavage. Individual crystals of
magnesite are rare and the mineral is commonly massive. Like calcite and dolomite, magnesite looses CO 2
on heating. Its structure is assumed to differ from that of calcite only in the cell parameters and it has been
determined from “powder diffraction patterns”.
Magnesia (MgO) has many direct and indirect uses; the primary use of raw magnesite is in calcination
industry, where it is calcined to form caustic magnesia (low calcined magnesite), dead-burnt magnesite or
fused magnesia. The other industries where raw magnesite is used are mosaic tiles, electrode, chemical and
manufacture of magnesium metal.
The dead-burnt magnesite and fused magnesia, either in the form of loose grains or as shaped bricks are used
in refractory products. Refractories are the fundamental pre-requisites for any high temperature operation.
These are not only indispensable for protection against cracking, melting, warping of furnace walls, but also
for effective confinement, storage and transfer of heat.
Magnesite is used for extraction of magnesium metal. Because magnesium is the lightest metal known
(Specific Gravity 1.74) and is fairly strong, it is in demand for the light alloys that are used extensively in
aeroplanes and automobiles and many other materials requiring lightness. Its alloys are non corrosive in air
but not in sea water. The chief alloying element is aluminium, generally with some zinc and manganese.
Such alloys have low weight for unit bulk, high rigidity and greater strength than most aluminium alloys.
They are used for microscope mountings, field glasses, cameras, surveying instruments, artificial limbs,
shuttles, bobbins, musical instruments and so forth. The magnesite (MgO) is also used as a fluxing material
in iron ore agglomeration.
The present study outlines the characterization and flotation studies carried out on the magnesite of Parshad
area, Rajasthan.
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Samples of the host rocks and magnesite were collected from the Parshad area of district Udaipur, Rajasthan.
The coarse crystalline magnesite of Parshad area is grey-white to creamish white in color. Crystal aggregates
of magnesite, as clusters, form the ore. Individual crystals lengths usually vary between 5 mm and 30 mm.
Crystals are elongated and bladed in nature. The hardness is 4.5 in Mohs’ scale and specific gravity is 3.2.
2.2 Methods
In order to identify the minerals and the association of valuable ore mineral with the gangue, characterization
studies of low grade magnesite were carried out. Physico-chemical characteristics, DTA, TGA, DTGA,
vitrification study and X-ray analysis were carried out to characterize the mineral. The characterization
studies reveal that the magnesite ore is mainly composed of magnesite with minor amounts of quartz and
iron. Other minerals, mainly, calcite, sericite and clinzoisite are present in traces.
Study of thin sections of magnesite shows that the mineral is polygonal granular usually having smooth grain
boundary (Fig. 1), but rarely the grains have serrated outline (Fig. 2).
The grains are mostly inclusion-free and are devoid of iron oxide staining, which can be expected of
Precambrian ore exposed for a prolonged weathering. Lack of iron carbonate component in the ore possibly
explains this observation. Ore from the contact with the wall rock contains fine grained inclusion of Quartz,
Sericite (Figs. 3 & 4).
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Differential thermal analysis (Fig. 5) has been carried out on the sample at the heating rate of 10oC per
minute up to a temperature of 1000oC. The calcined alumina has been used as the reference material. The
results are given in table 1
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Table 1: Results of Differential Thermal Analysis.
Meter
Temperature Nature of
o Reading
( C) peak
(Unit)
100 - -
300 -2 Endothermic
350 -1 Endothermic
395 -1 Endothermic
650 -33 Endothermic
775 -1 Endothermic
800 -1 Endothermic
955 -1 Endothermic
2.3.3 Thermo Gravimetric Analysis (TGA)
Similar to differential thermal analysis, thermo gravimetric analysis (Fig. 6) has been carried out taking 1
gram of powdered sample of 75 micron size, weighed in a platinum crucible inserted in a furnace from a
thermobalance. The furnace was heated at 10oC per minute. The weight loss behavior of magnesite has been
recorded and the results obtained are given in table 2.
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Direct weighing of sample throughout a heating cycle does not prove entirely satisfactory because of wide
range of changes, so that a small weight loss, following a large one will not be distinguished. Differentiation
of weight loss with respect to temperature to get a plot of dw/dt against ‘t’ gives more useful information
with sharp peaks and troughs whereas in TGA ‘w’ against ‘t’ is an indeterminate curve (Fig. 7). The results
of the thermogram are given in table 3.
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Calcination of magnesite at high temperatures removes the possibility of shrinkage. During calcination, MgO
crystallizes, the grains become bigger and compact and free from possible hydration. Specific gravity of
magnesite increases up to the maximum on fusion. To examine this characteristic property, tests were carried
out up to a temperature of1400oC. It was observed that specific gravity of the sample increases from 3.2 to
4.0 with increase in temperature from 1000 to 1400oC.
The sample was crushed and ground to -75 micron and subjected to X-ray diffraction study using X-ray
diffractometer (type PW 1730) with monochromatic Cu Kα radiation and nickel as filter.
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A scanning speed of 0.5o per minute was used. The sample was screened between 7 o and 90o (2θ) at 40 KV
and 10 mA setting (Fig. H).
3. Flotation studies
Mineralogical composition of magnesite indicated that the magnesite of Parshad area is having silica and iron
oxide as main impurities. To study the beneficiation characteristics of this low grade magnesite, froth
flotation technique has been adopted.
The flotation process involves the production of mineralized froth into which the desired mineral constituent
is firmly bound enough to ensure transport to and removal from the froth of the original pulp.
Low grade magnesite sample, weighing about 80 kg from Parshad area is subjected to bench scale flotation
studies. The objective of the investigation is to ascertain the possibility of producing a magnesite concentrate
suitable for use in refractory and other allied industries.
The sample in lump form was subjected to crushing in stages to -12 mm size and -1.6 mm size in jaw and roll
crushers respectively. The -1.6 mm size material was used as the feed stock for the test work. By coning &
quartering, a representative sample was obtained and subjected to chemical analysis. The percentages of
MgO, CaO, SiO2, R2O3 etc. were estimated and the results are given in table 5.
Constituents MgO SiO2 Fe2O3 Al2O3 TiO2 CaO Alkalies (Na2O + K2O) LOI
Assay (%) 37.0 6.36 5.36 0.20 0.20 1.12 0.20 48.24
A representative portion of the -1.6 mm size material was subjected to sieve analysis to determine size
distribution of the feed. The resultant sieve fractions were chemically analysed for their MgO, SiO2, Fe2O3
and Al2O3 content. Since Al2O3 content in the crude sample is 0.2% only, the R2O3 i.e. (Al2O3 + Fe2O3) was
considered in all the experiments. CaO content in the magnesite sample is also very small and well within the
limit of the standard requirement for its industrial use. Hence, only two major impurities i.e. SiO2 and R2O3
have to be minimized from the magnesite. Result of size and size-wise chemical analysis of -1.6mm sample
is given in table 6.
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Table 6: Size analysis of -1.6 mm sample.
The result shows that the MgO, SiO2 and R2O3 are distributed in all the size fractions with no clear
segregation in the coarser (or) finer size range. Hence it was decided to reduce the sample to 60 & 100 mesh
sizes and carry out froth flotation studies.
Flotation Experiments have been carried out under different conditions to optimize the flotation parameters
for achieving maximum recovery. All experiments have been performed in a Dorr-Oliver Flotation Cell. The
optimum MOG at which further flotation tests to be carried out was determined by MOG tests. It was found
that flotation results were best at -60 mesh. Hence, -60 mesh was chosen for detailed flotation experiments.
The objective of the flotation tests was to reduce the SiO2 and Al2O3 to acceptable levels of the refractory
grade with MgO upgraded. Hence, the focus was on selection of an effective collector (collector
combination) and the identification of the optimum dosage of collector and depressant dosages and pH of
slurry.
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Flotation experiments have been carried out to ascertain the most effective and selective collector for
flotation of magnesite. The collectors used are Sodium Oleate, combination of Boramac ‘C’ with Sodium
Oleate, combination of Boramac ‘C’, Sodium Oleate and Pine Oil, combination of Oleic Acid and Pine Oil.
The flotation parameters were kept constant during the experiments. The results of flotation experiments in
selection of collector are given in table 8.
It can be observed that the flotation experiments carried out with Sodium Oleate and Boramac ‘C’ in equal
weight ratio (1:1), with pine oil to stabilize the froth, yielded comparatively better result in respect of grade
and recovery of MgO. Hence, this combination of collectors has been used for further flotation experiments.
Sodium Silicate for depressing silica (SiO2), Sodium Carbonate to maintain the pH 8.5 were used while
optimizing the collector dosages with Sodium Oleate and Boramac ‘C’ (in different proportions), and Pine
Oil as frother (Table 9). The results are presented in table 10.
Combination A B C D E F G
Sodium Oleate (Kg/ton) 1.0 0.5 0.8 0.6 0.5 0.5 0.4
Boramac ‘C’ (Kg/ton) 0.5 1.0 0.5 0.5 0.5 0.4 0.4
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Table 10: Optimization of collector dosage.
Reagents
Product Wt% MgO% SiO2% R2O3%
Combination
Concentrate 80 37.90 5.80 5.32
A
Tailing 20 35.80 6.80 5.46
Concentrate 50.5 40.20 3.64 5.24
B
Tailing 49.5 34.26 9.12 5.13
Concentrate 70 41.12 2.14 5.20
C
Tailing 30 27.56 13.74 5.80
Concentrate 66.2 41.98 2.14 5.22
D
Tailing 33.8 27.78 14.20 6.30
Concentrate 65 42.60 1.32 5.28
E
Tailing 35 26.94 15.88 5.86
Concentrate 65.5 40.82 3.16 5.36
F
Tailing 34.5 29.83 12.10 5.38
Concentrate 58 39.98 4.86 5.42
G
Tailing 42 33.28 8.30 5.90
It can be seen from table 10, that the required grade of the concentrate could be achieved by using
‘combination E’ i.e. Sodium Oleate and Boramac ‘C’, each 0.5 Kg/ton wherein there is a good yield of
Concentrate (65%). However, the other combinations e.g. ‘C’, ‘D’, ‘F’ could yield a little better yield but
with lower MgO. Hence, further experiments were carried out using combination ‘E’ (1:1 Boromac ‘C’ and
Sodium Oleate).
While studying the performance of collectors for selection, Sodium Silicate was used as a depressant;
because for any carbonate mineral containing silica (SiO2) as impurity, Sodium Silicate has proven to be an
effective depressing agent.
For optimization of depressant dosage, the combination ‘E’ as collector and Sodium Silicate at three levels
i.e. 0, 0.5 and 1.0 kg/ton have been taken. The results obtained are given in table 11.
It can be seen that the grade and recovery of magnesite concentrate is better when 0.5 kg/ton Sodium Silicate
has been used as depressant. With the use of more quantity i.e. 1.0 kg/ton Sodium Silicate, the yield of
magnesite decreases.
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Table 11: Results of optimization of depressant.
Sod. Silicate
Product Wt% MgO% SiO2% R2O3%
(Kg/ton)
Concentrate 67 38.2 5.98 5.42
Nil
Tailing 33 34.78 7.00 6.15
Concentrate 64.8 42.62 1.36 5.20
0.5
Tailing 35.2 28.58 15.33 5.82
Concentrate 57 42.60 1.78 5.56
1.0
Tailing 43 31.30 12.06 5.52
5. Conclusions
Studies indicate that the magnesite ore of this area is mainly composed of magnesite with minor amount of
quartz and iron in the form of hematite. Other minerals identified are Calcite, Sericite and Clinozoisite, which
are present in traces.The main impurities in the magnesite are silica and iron; Calcium Oxide (CaO) content
is very small and well within the standard limit required for its industrial use. Bench scale beneficiation
studies have been carried out on a low grade magnesite sample containing SiO2 – 6.36%, Fe2O3 – 5.36%,
Al2O3 – 0.20%, TiO2 – 0.20%, CaO – 1.12%, MgO – 37.0%, Na2O & K2O – 0.20% and LOI – 48.24%. It
was observed that Silica (SiO2) is liberated at 60 mesh to a considerable extent and by flotation test, a
concentrate is obtained having optimum grade with better recovery of magnesite at this mesh of grind.
Various combinations and optimization of collector dosages have been made using Sodium Oleate, Oleic
acid and Boramac ‘C’. Sodium Silicate has been used as depressant. Sodium Carbonate was used to regulate
pH and Pine Oil to stabilize the froth. Best result was achieved by the combination of Sodium Oleate and
Boramac ‘C’ (each 0.5 kg/ton) as collector and Sodium Silicate as depressant. It may be concluded that
Parshad magnesite is amenable to beneficiation by flotation. It has been observed that Silica (SiO 2) is
reduced from 6.36 to 1.36% and Magnesium Oxide (MgO) is increased from 37.0 to 42.6% with a weight
recovery of 65% and MgO recovery of 74.63%. It can be concluded that the beneficiated magnesite is
suitable for refractory and allied industries.
References
Banerjee, J.C., Banerjee, S.P. & Sircar , N.R., 1964: “Studies on Indian magnesites as refractory materials (i)
Aggar Sirechchina deposits of Almora district, Uttar Pradesh”, Cent. Glass Ceram. Res. Instt. Bull. II (4) 86-
93.
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Banerjee, J.C., Sircar, N.R., 1964: “A comprehensive study of Indian magnesites as refractory materials”,
Trans. Indian Ceram. Soc. (2) 49-59.
Chattopadhyay, N. & Gangopadhyay, S., 1984: “Petrological Study of the ultramafic rocks of Rajasthan”,
Spec. Pub. Geol. Surv. Ind., Vol. 12, 17-24.
Heron, A.M., 1953: “The Geology of Central Rajputana”, Mem. Geol. Surv. Ind., V. 79.
Jhunihunwala, R., 1993: “Indian Magnesite-Problems and Prospects”, Industrial Minerals, 52.
Khichi, N.S. & Rai, S.C., 1991: “Magnesite investigation in Prashad, Bhauva and Kotra area, district
Udaipur, Rajasthan”, Project report of DMS (inpub.).
Mackenzie, R.C, 1972: “Differential Thermal Analysis”, Vol. 2, Academic Press London, 312-316.
Morti, G., 1986: “A user view of challenges for the magnesite industry”, Industrial Minerals., 29-39.
Ray, S.B., 1968: “Suitability of talc-magnesite as a medium for insulating fire brick and others”, Indian
Ceram., 13(2) 54-57.
Bhattacharya, B.C., Dashora, R.S., Venugopal. R., Nov. 1995: “Characterization of Magnesite of Parshad
Area, Rajasthan”, Trans. Indian Ceram. Soc., Vol. 54 (6) 242-245.
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FEASIBILITY STUDIES ON TALC BENEFICIATION BY FLOTATION
N. Vasumathi*, M. Ananda Rao, T.V. Vijaya Kumar, S. Subba Rao, S. Prabhakar and
G. Bhaskar Raju
CSIR - NML Madras Centre, CMC, Taramani, Chennai - 600 113.
*Corresponding author: vasumatisamy@gmail.com
Abstract
Talc’s unique properties make it an important ingredient for making ceramics, paint, paper, roofing
material, plastics, rubber, insecticides, cosmetics and many other products. A talc sample from Karnataka
state, India consisting of quartz and calcite as gangue and analyzing 43.99% SiO2, 23.36% MgO and
15.50% CaO was attempted for its quality improvement by flotation. Effect of process parameters such as
mesh-of-grind, different types of depressants, collectors, combination of collectors, frothers and pH on
the separation of talc from calcite was studied. The MgO content in talc could be improved to 28.09%
and CaO was decreased to 10.42% using sodium hexa meta phosphate (2.0 kg/t) as dispersant and MIBC
(0.159 kg/t) as frother with 75.51% recovery of MgO. Introduction of oleic acid, tertiary amine, a
combination of oleic acid and diesel and octyl hydroxamate as collectors for talc, starch as depressant for
calcite did not result in further reduction of CaO in the talc concentrate during flotation. Dissolution of
calcite in talc by dilute HCl (inorganic acid) and acetic acid (organic acid) proved to be very effective in
improving the talc quality. Talc concentrate assaying 30.38% MgO and 60.27% SiO 2 could be achieved
by using dil. HCl. The brightness of talc was slightly affected due to the dissolution of iron present in talc.
However, by using acetic acid, the brightness of talc was improved along with the chemical assay which
could be attributed to the selective dissolution of calcite and buffering effect of acetate.
1. Introduction
Talc is a naturally occurring crystalline hydrated magnesium silicate mineral. The talcum powder is
produced from this mineral which has the ability to absorb moisture and oils. Talc's unique properties like
its hydrophobicity, chemical inertness, organophilicity and platy cleavage, low electrical and high thermal
conductivity make it an important ingredient for making ceramics, paint, paper, roofing materials,
plastics, rubber, insecticides and many other products (Taylor, 2003).
Talc’s chemical composition is Mg3Si4O10(OH)2. When expressed in the standard oxide form, the ideal
chemical composition is: 31.9% MgO, 63.4% SiO2 and 4.8% H2O. Talc is a monoclinic mineral with a
sheet structure similar to the mica. The most common minerals found in talc products include chlorite,
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magnesite, dolomite, tremolite, anthrophyllite, serpentine and quartz. Talc has perfect cleavage that
follows planes between weakly bonded sheets. These sheets are held together only by Van der Waals
bonds which allows them to slip past one another easily. This characteristic is responsible for talc’s
extreme softness and greasy/soapy feel. It can be used as a high temperature lubricant.
The natural floatability of talc can be explained due to its breakage. The double-sheet units are easily
separated by slight forces that result in a perfect cleavage direction in the basal plane which is highly
hydrophobic (Rohl et al., 1976; Pooley & Rowlands, 1975). It was revealed that even though talc appears
to be macroscopically hydrophobic in its natural form it is microscopically very hydrophilic. The flotation
of pure talc mineral was studied by measuring its contact angle, flotation recovery and zeta potential.
Polypropylene glycol was used as a frother to increase the rate of talc flotation. Clean talc concentrate at
a recovery of 70% with a grade of 93.5 % from an ore containing 48.69 % talc was obtained (Yehia and
Al-Wakeel, 2000). The flotation rate and recovery of talc and entrainment of fine calcite particles were
investigated using individual minerals and a mixture of talc and calcite. The effects of various frothers
were tested. The results indicated that the type of frother had significant effect on the recovery, flotation
rate and fine gangue entrainment. The addition of kerosene as a collector enhanced selectivity between
talc and calcite without any reduction in talc recovery. This was attributed to increasing the rate constant
of talc upon kerosene addition without any increase in the calcite fines recovery (Ünal Akdemir et al.,
2005). In yet another study, the talc sample containing asbestos, the effect of phytic acid and sodium
dodecyl benzene sulfonate was attempted. New flow-sheet consisting of roughing, three stage cleaning
and scavenging was proposed (Hao Wu et al., 2012). The interaction of guar gum and dextrin with talc
has been investigated through adsorption, flotation, and electrokinetic measurements (Rath et al., 1997).
The effects of depressants namely, guar gum (IMP4) and carboxymethyl cellulose (CMC) on talc were
enhanced by ultrasonication. The microtopographic studies by atomic force microscopy indicated that
surface defects generated by ultrasound could serve as active sites for water adsorption rendering the
naturally hydrophobic talc to hydrophilic (Dingwu Feng and Chris Aldrich, 2004). The flotation
behaviour of talc products having different particle shapes produced by different grinding mills (ball and
rod mill) was determined by using column flotation process (Hulya Kursun and Ugur Ulusoy, 2006). The
results showed that particles possessing higher elongation and flatness properties were recovered better
during column flotation, whilst roundness and relative width had a negative effect on the flotation
behaviour of the talc mineral studied. Consequently, as the shape of the particles produced by the mill
deviated from the ideal sphere, their floatability was increased (Yekeler et al., 2004). Thus depending on
the nature of gangue minerals, different strategies were adopted to enrich talc powder. In the present
investigation, combination of reagents were tried to upgrade the talc by flotation.
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2. Materials and methods
The talc sample used in the present study was sourced from Karnataka state, India. It analyzed 43.99%
SiO2, 23.36% MgO and 15.50% CaO. The sample was characterized for mineralogical phase
identification using x-ray powder diffraction method. It is identified that calcite, talc and quartz mineral
phases are predominant in the sample. The presence of pyroxenes, olivine, biotite, amphiboles and
tectosilicates in talc could not be established. The diffractogram of the sample is shown as figure 1.
350 C
T T-Talc
300 C-Calcite
Q-Quartz
250
Intensity, cps
200
T T
150 Q
T C
100
C
T Q C
C C C
50 T Q
Q C
0
10 20 30 40 50 60
2Theta, degree
Talc sample was passed through the jaw crusher and roll crusher for size reduction. The output of the roll
crusher with a maximum particle size of 1mm was ground in a pulverizer (pulverisette 5, Fritsch,
Germany) equipped with agate jars and balls to obtain the desired particle size range of flotation. Bench
scale flotation tests were conducted in a D12 Denver Flotation machine. Conditioning was carried out at
50% solids (by weight) followed by flotation at 33% solids. Different frothers viz., poly ethylene glycol
(PEG), pine oil and methyl isobutyl carbinol (MIBC) were used. Soluble starch procured from MERCK
was tried as depressant for calcite. Float and non-float products are filtered, dried, weighed and analyzed.
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The results clearly suggest that the recovery was improved from 36% to 74% with the fineness of the talc
powder (d80). However, the quality of the concentrate was found to be affected when the sample was
ground to a fine size. Though the calcite assay in tailings is more, the overall improvement in the quality
of talc concentrate is negligible. This may be attributed due to adsorption of oleic acid on calcite.
15
14 CaO in Concentrate
%
13
12
11
26
MgO in Concentrate
25
%
24
23
70
Recovery of MgO
60
%
in Concentrate
50
40
90 80 70 60 50 40 30
Particle size (d80), microns
Figure 2: Effect of particle size on grade and recovery of Talc using oleic acid.
Alternatively, tertiary amine (0.116 Kg/t) was tried as collector which can adsorb only on silica and
silicate minerals and expected to enhance the flotation of talc. From the results presented in figure 3, it is
apparent that the recovery of talc is increased from 36% to 72% as the particle size is decreased.
However, the improvement in the quality of the talc concentrate is marginal. The calcite content was
found to increase as the particle size is decreased. This behaviour may be due to the fact that calcite was
ground more easily than the siliceous gangue. The degree of liberation of the valuable minerals was
evidently increasing with the particle fineness.
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20
18
CaO in Concentrate
16
%
14
12
30
28
26 MgO in Concentrate
%
24
22
20
70
60 Recovery of MgO
%
in Concentrate
50
40
90 80 70 60 50 40 30
Particle size (d80), microns
Figure 3: Effect of particle size on grade and recovery of Talc using tertiary amine.
Since talc is naturally hydrophobic, flotation was carried out using frother alone. Different frothers viz.
poly ethylene glycol (PEG), pine oil and methyl isobutyl carbinol (MIBC). The dosage of these frothers
was also varied and the results obtained are tabulated in table 1. The results indicate that MIBC is more
selective compared to pine oil and PEG. The MgO content in talc was improved to 25. 50% and CaO was
decreased to 12.00% from its original value of 15.50%.
Table 1: Effect of frother and its concentration on grade and recovery of talc
Conditions: Grind size: 38 µm, Sodium hexametaphosphate: 2 Kg/t.
Frother Dosage, Weight, % Concentrate Tailings Recovery
Kg/t assay, % assay, % of MgO, %
Concentrate Tailings MgO CaO MgO CaO
PEG 0.092 80.85 19.15 26.19 14.65 22.69 19.09 78.53
PEG 0.137 38.46 61.54 24.34 12.32 22.75 17.49 38.73
PEG 0.183 42.07 57.93 25.09 13.38 20.46 17.04 49.24
Pine oil 0.0764 50.50 49.50 24.44 12.82 22.26 18.24 52.84
Pine oil 0.1146 52.00 48.00 24.80 13.63 21.80 17.53 55.21
Pine oil 0.1528 66.27 33.73 25.17 15.33 22.44 15.83 63.65
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The effect of slurry pH on grade and recovery of talc was studied and the results are shown in table 2.
Pine oil (0.1528) 10 55.89 44.11 26.03 11.45 19.98 20.63 62.28
Pine oil (0.1528) 9 54.77 45.33 24.90 11.36 21.50 20.51 58.37
The quality of talc was better at pH 10. The iso electric point of talc, quartz and calcite are 1.7, 2.9 and
8.5 respectively. By adjusting the pH to above 9.0, the charge of these minerals will become negative and
thus all the three minerals dispersed properly. Better quality of talc concentrate at pH 10 is attributed to
effective dispersion of minerals in water.
Starch, as depressant for calcite, was varied from 0.2-1.0 Kg/t. MIBC (0.198 Kg/t) was used as frother
while maintaining the slurry pH at 10.0 and grind size at 38 µm. The results are shown in figure 4. It is
evident that CaO content in the concentrate was reduced from 15.50% to 12.80% by increasing the starch
dosage while the recovery of talc was improved with increase in starch dosage.
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20
18
CaO in Concentrate
16
%
14
12
30
28
26 MgO in Concentrate
%
24
22
20
70
60
%
50 Recovery of MgO
40 in Concentrate
Combination of oleic acid, diesel oil and MIBC reagents was attempted to improve grade and recovery. It
was observed that the recovery of talc is very much influenced by oleic acid whereas grade by MIBC
dosage. Experiments on natural floatability of talc (without reagents), split addition of reagents and also
various combinations of reagents was also tried to eliminate calcium carbonate. But the desired results
could not be achieved. Octyl hydroxamate, supposed to be selective was also tried as collector. The
results indicated that there was no improvement in quality of talc concentrate.
Since separation of calcite from talc by flotation was found to be ineffective, efforts were made to
dissolve the same by using inorganic and organic acids. Dilute hydrochloric acid and acetic acid were
tried to eliminate calcite and thereby improve talc grade. The calcite was removed to the extent where
MgO content was improved from 23% to 30% and SiO2 from 47% to 60%. Acetic acid also was tried to
dissolve calcium carbonate. While treating with HCl, talc brightness can be affected if iron is present. To
avoid the contamination of FeCl3 and also to minimize the chloride content in talc, acetic acid was used
for iron dissolution. Since acetic acid is weak acid, only calcite is dissolved and removed. Thus the
brightness of talc is enhanced.
4. Conclusions
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Beneficiation of talc containing calcite as major gangue by flotation was carried out using sodium
hexametaphosphate as dispersing agent, oleic acid as collector and poly ethylene glycol as frother and the
selectivity of separation was found to be poor. Starch was tried as depressant for calcite and the
depressing effect of starch is not enough to achieve desired selectivity. Flotation of talc using tertiary
amine, octyl hydroxamate as collectors was also found to be futile. Flotation of talc using pine oil/
MIBC/poly ethylene glycol at slurry pH of 9.0 and 10.0 was tested and found slight improvement in
grade but the recovery was decreased. Since major impurity is calcite, it can be easily dissolved using
acids and separated by filtration. Dilute HCl acid and acetic acid was proved to be very effective in
improving the talc quality. Talc concentrate assaying 30.38% MgO and 60.40% SiO2 was achieved by
using dilute hydrochloric acid. The brightness of talc was slightly affected due to the dissolution of iron
present in talc. By using acetic acid, the brightness also was improved along with chemical assay. This
was attributed to the selective dissolution of calcite and buffering effect of acetate.
Acknowledgements
The authors are grateful to the Director, CSIR - National Metallurgical Laboratory, Jamshedpur for his
valuable guidance, encouragement and permission to publish the work. The authors would like to thank
M/s Radiant Minerals, Bengaluru for sponsoring the project and providing chemical analysis of the
samples.
References
Dingwu Feng and Chris Aldrich. Effect of ultrasonication on the flotation of talc. Ind. Eng. Chem. Res.,
43(15):4422-4427, 2004.
Hao Wu, Wan Zhong Yin, Ming Bao Liu and Peng Jie Tian, Effect of phytic acid on flotation of talc
impurity. Advanced Materials Research, 454:174-178, 2012.
Hulya Kursun and Ugur Ulusoy. Influence of shape characteristics of talc mineral on the column flotation
behaviour. International Journal of Mineral Processing, 78(4):262-268, 2006.
F. D. Pooley and N. Rowlands. Chemical and physical properties of British talc properties. Inhaled Part,
4:639-646, 1975.
R. K. Rath, S. Subramanian and J. S. Laskowski. Adsortion of dextrin and guar gum onto talc. A
comparative study. Langmuir, 13(23):6260-6266, 1997.
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L. Taylor. Smooth operator: talc gets specialized for growth. Industrial Minerals, 428:24-33, 2003.
Ünal Akdemir, Taki Güler and Güvengez Yildiztekin. Flotation and entrainment behavior of minerals in
talc-calcite separation. Scandinavian Journal of Metallurgy, 34 (4):241-244, 2005.
A. Yehia and M. I. Al-Wakeel. Talc separation from talc-carbonate ore to be suitable for different
industrial applications. Minerals Engineering, 13(1):111-116, 2000.
M. Yekeler, U. Ulusoy and C. Hicyilmaz. Effect of particle shape and roughness of talc mineral ground
by different mills on the wettability and floatability. Powder Technology, 140:68-78, 2004.
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IMPROVING WATER SORPTION CAPACITY OF GUJARAT CLAY
Deepa Dixit, Seethalakshmi P, Chinmay Ghoroi*
DryProTech Lab, Chemical Engineering, Indian Institute of Technology Gandhinagar,
VGEC Campus, Chandkheda, Ahmedabad, Gujarat-382424, India
*Corresponding author: chinmayg@iitgn.ac.in
Abstract
In this work moisture adsorption capacity of Gujarat clay is improved for its use as an alternative low cost
desiccant. The original clay collected from specific area of Gujarat was modified using mechanical and
chemical activation. The original and composite clay along with the standard silica gel were exposed at
different relative humidity and characterized for their performance as an adsorbent material. The
adsorption capacity of composite clay was found to be substantially improved from the original clay and
comparable to that of commercially available silica gel. The preliminary result shows that after suitable
modification, the Gujarat clay could be an alternative low cost desiccant material.
Keywords: Desiccant, Gujarat clay, Mechanical and chemical activation, moisture adsorption, adsorbent.
1. Introduction
Commercial desiccants such as regenerative silica gel, zeolite and molecular sieves have been applied to
various dehumidification and air drying system. However, they are all expensive desiccant material (Zhu,
Wu, and Wang 2006). Bentonite is considered as an attractive environmental friendly low cost alternative
desiccant which can be regenerated easily (Bulut et al. 2009; Guerra et al. 2013; Zaghouane-Boudiaf et al.
2014).It has great ability to adsorb moisture (Barbanti, D’Orazio, and Versari 1997; Thoruwa et al. 2000).
In geological and petro-graphical term, bentonite is a rock formed from altered volcanic ashes and largely
composed of montmorillonite, a member of the smectite group, consists of two tetrahedral sheets (silicon
/ oxygen) separated by an octahedral sheet (aluminum / oxygen / hydroxyl) (Barbanti, D’Orazio, and
Versari 1997). However, adsorption capacity of naturally available bentonite is lower than traditionally
used desiccant. The adsorption capacity of naturally occurring clay can be improved by appropriate
modification such as formation of a clay composite (Aristov et al. 2002; Gordeeva et al. 2002).
In India, Bhavnagar and Kutch districts of Gujarat have major occurrence of bentonite. The deposit in
Kutch is regarded as one of the world's best deposits (Bhatt J.V. 1990). However, very little information
is available on the moisture adsorption capacity of the available bentonite clay deposits of Gujarat. The
present work aims to improve the water adsorption capacity of the Gujarat clay up to the level of
commercially available silica gel using mechanical and chemical activation.
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2. Experimental procedure
The naturally available bentonite clay of Gujarat was first activated through mechanical activation using a
ball mill and then chemically activated by adding 5%, 7%, 10% and 15% (wt %) of CaCl 2 along with the
10 wt % of montmorillonite to avoid wetting due to high dosage of CaCl2. The moisture adsorption
capacity of composite clay was studied by exposing the composite materials along with the commercially
available silica gel at different relative humidity (RH 30%, 45%, 60%, 75% and 90% at 25˚C) for 24
hours. The equilibrium moisture content of all the samples was then measured and compared. The
microstructure and physical appearance of the composite clay and original clay were observed using SEM
(JEOL JSM 7600F, USA) and ordinary camera.
3. Results and Discussion
Fig 1 shows SEM pictures of original and composite clay after mechanical and chemical activation using
10% of each CaCl2 and montmorillonite. The SEM image shows that both original and composite clay
has irregular microstructure. However, the original clay has smaller clusters of layered structures. In
contrast, the composite clay contains less but bigger clusters.
(a) (b)
Figure 1: SEM images of (a) original clay and (b) composite clay samples at a working distance (WD) of
7.8 mm and a voltage of 5 kV using FESEM.
Fig 2a shows the picture of mechanically activated clay. Fig 2b shows the composite clay without
montmorillonite (not added externally) which shows wetness over increasing CaCl2 content. The wetness
for clay with 15% CaCl2 is much higher than that of clay with 10% CaCl2. Fig 2c shows the reduction in
wetness after adding 10% of montmorillonite with different percentage of CaCl2.
Figure 3 shows the adsorption isotherms for all samples. It indicates that all the samples shows the
progressive increase in moisture content with an increase in RH (typical hygroscopic nature). However,
the adsorption capacity of original clay found to be much lower than silica gel at all RH (Fig 3). After
mechanical activation of the clay, the amount of equilibrium moisture content (EMC) increases at low
RH. But it becomes constant beyond 60% RH. The addition of different wt% of CaCl 2 in the
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mechanically activated clay increases the EMC. At 10% and 15% dose of CaCl 2, EMC is increased to the
level of silica gel.
Figure 2: Deliquescence behavior of (a) Mechanically activated clay (b) Mechanically activated clay
with different wt % of CaCl2 and (c) composite clay after exposing to 75%RH for 24 hours at 25˚C.
45
Original Clay
Equilibrium Moisture Content (%)
40
Silica gel
Mechanically activated Clay
35 Composite Clay(5%)
Composite Clay(7%)
30 Composite clay(10%)
Composite Clay(15%)
25
20
15
10
0
30 40 50 60 70 80 90
Relative Humidity(%)
Figure 3. Percentage equilibrium moisture content of original clay, composite clay and silica gel samples
at different relative humidity conditions.
4. Conclusion
Overall, the results of this study demonstrated that moisture adsorption capacity of Gujarat clay can be
improved by mechanical and chemical activation. The moisture adsorption capacity of clay composite
with 10% of each montmorillonite and CaCl2 found to be comparable with the commercially available
silica gel. The preliminary result shows that composite clay can be used as an alternative desiccant
material.
Acknowledgement
Authors want to acknowledge IITGN for providing financial support for this work.
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References
Aristov, Yi Yu.I, G Restuccia, G Cacciola, and Vn V.N Parmon. 2002. “A Family of New Working
Materials for Solid Sorption Air Conditioning Systems.” Applied Thermal Engineering 22(2): 191–204.
Barbanti, D., M. D’Orazio, and a. Versari. 1997. “The Use of Bentonite as a Moisture Regulating System
1. Study on Some Sorption Properties of Bentonites for Their Potential Use in Food Technology.” Journal
of Food Engineering 33(1-2): 193–206.
Bhatt J.V. 1990. Prospect for Bentonite Based Industries in Gujarat. Industrial Extension Bureau (A Govt
of Gujarat Organization) Ahmedabad.
Bulut, G., M. Chimeddorj, F. Esenli, and M. S. Çelik. 2009. “Production of Desiccants from Turkish
Bentonites.” Applied Clay Science 46(2): 141–47.
Gordeeva, L. G., G. Restuccia, a. Freni, and Yu I. Aristov. 2002. “Water Sorption on Composites ‘LiBr in
a Porous Carbon.’” Fuel Processing Technology 79(3): 225–31.
Guerra, D. J L, I. Mello, R. Resende, and R. Silva. 2013. “Application as Absorbents of Natural and
Functionalized Brazilian Bentonite in Pb2+ Adsorption: Equilibrium, Kinetic, pH, and Thermodynamic
Effects.” Water Resources and Industry 4: 32–50. http://dx.doi.org/10.1016/j.wri.2013.11.001.
Thoruwa, T.F.N, C.M Johnstone, a.D Grant, and J.E Smith. 2000. “Novel, Low Cost CaCl2 Based
Desiccants for Solar Crop Drying Applications.” Renewable Energy 19(4): 513–20.
http://www.sciencedirect.com/science/article/pii/S0960148199000725.
Zhu, Dongsheng, Huijun Wu, and Shengwei Wang. 2006. “Experimental Study on Composite Silica Gel
Supported CaCl2 Sorbent for Low Grade Heat Storage.” International Journal of Thermal Sciences 45(8):
804–13.
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Abstract
A low-grade complex siliceous &magnesia rich rockphosphate ore sample from Madhya Pradesh was
taken up for bench scale beneficiation studies with the objective to develop a process flow-sheet to
produce phosphate concentrate suitable for manufacture of phosphoric acid. Mineralogical studies
revealed the presence of apatite, quartz, dolomite and calcite as main minerals and chemically assayed
17.26% P2O5, 33.15% Acid Insol., 32.65% SiO2(T), 3.52% MgO and 30.61% CaO.
Beneficiation studies evolved a processflow-sheet comprising of ball mill wet grinding to d80 size 61
microns, to liberate phosphate from gangue minerals, with addition of sodium silicate in the mill as silica
depressant.Single stage rougher phosphate-carbonates bulk flotation, at pH 10-11, using anionic collector
sodium oleate could yield bulk rougher phosphate-carbonate float and discard silica (quartz) and silica
bearing minerals, in the rougher tails forming reject.Three cleanings ofrougher phosphate-carbonate bulk
float, at pH 10, followed by reverse flotation of the III cleaner bulk float for separation of phosphate from
carbonate at pH 5-6 using sulfuric acid as pH modifier,orthophosphoric acidas phosphate depressant and
pine oil as frother could yield a phosphate concentrateassayed 32.66% P 2O5, 9.77% Acid insoluble,
9.42% SiO2(T), 0.65% MgO, 1.11% Fe2O3, 0.62% Al2O3,1.73% R2O3(Fe2O3+Al2O3), 47.34% CaO,
3.29% F and 4.32% LOI with phosphate recovery of 63.1% and weight % yield of 33.1. The paper
reflects the importance of beneficiation studies in producing a phosphate concentrate suitable for
phosphoric acid manufacture in view of utilization of low grade and complex ores.
1. Introduction
A low-grade siliceous & dolomitic rock-phosphate ore sample from district Jhabua, Madhya Pradesh,
Indiawas studied at IBM with an objective to develop a beneficiation process flow-sheet to produce a
phosphate concentrate for manufacture of phosphoric acid.
Feed sample preparation for characterization and bench scale flotation studies
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Industrial Minerals
The ore sample with top size 75 mm was crushed down to -10 mesh (-1.7 mm) size using laboratory jaw
crusher, roll crusher in stages in close circuit with a 10 mesh opening vibrating screen; thoroughly mixed
and divided by riffle sampler into small portions. From this, original feed sample was taken for
characterization studies (mineralogical and chemical analysis) and for various batch tests.
The ore sample was hard, compact, heterogeneous lumps, some of which were porous, soft and friable
and loosely coated with fine dusty material, which on washing were of different colours viz., dark grey,
brown, yellowish-white, white, light pink and pinkish-brown. Some crystalline quartz and some lumps
with streaks, bands and patches of silicates, carbonates and phosphate bearing mineral phases were
distinctly observed. Some amount of yellowish-orange fines (< 2 mm) was also present.
Detailedchemical analysis of the ore sample is P2O5 17.26%, Acid Insoluble 33.15%, SiO2(T) 32.65%,
MgO 3.52%, CaO 30.61%, Fe2O32.82%, Al2O31.31%, R2O3 (Fe2O3+Al2O3) 4.13%, F 1.84%, LOI 9.81%,
Cl 0.017%, Na2O 0.01%, K2O 0.28%, TiO20.07%, Organic Carbon 1.93%.
3. Experimental work
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3.1 Size analysis of sieve fractions of original feed sample (-10 mesh size, d80 size 940 microns)
The study showed that all size fractions assayed more or less same in P2O5, SiO2 and MgO contents
indicating no preferential segregation of any particular mineral in any fraction. Mineralogically, the -10
mesh size sample contained apatite, carbonates (dolomite, calcite), quartz & other gangue minerals
invariably in all size fractions.
The ore on grinding in a ball mill under identical conditions ranging from 10 to 30 min. with a difference
of 5 min., followed by size analysis of the ground pulp showed that with increasing grind time the % -200
mesh fractions also increased, with corresponding d80 size of 125, 93, 71, 61 & 56 microns, respectively.
Sodium oleate was optimized as the ideal collector for this sample as the collecting response was
excellent. Moreover, no extra frother is required while using sodium oleate. Chemical activity of sodium
oleate as collector for phosphate was found temperature dependent.
On using sodium silicate (a good silica depressant) and sodium oleate, the pH remained between 9 &10
and the anionic collector oleate functioned well at this ideal pH range.
This was determined by flotation of bulk phosphate-carbonate minerals and compared with respect to
P2O5 grade, recovery and wt. % yield vis-à-vis the grind. The grinds mentioned in item 3 above were
subjected to flotation under identical conditions.
These were done with sole aim to reduce SiO2 and MgO content to the desired level in the Phosphate
Concentrate:
This was studied at 0.4, 0.5 & 0.6 kg/t of dry feed. With increasing collector dosage the weight yield of
the concentrate increased correspondingly and with P2O5% remaining nearly same, consequently there
was increased recovery of phosphate in Rougher Bulk Float. Higher oleate dosage resulted in picking up
more gangue material in the Rougher Bulk Float. Hence, 0.5 kg/t was considered to be the optimum
collector dose, which was applied in all subsequent tests.
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3.8 Effect and optimization of number of cleaning stages
Three cleanings were given to the Rougher Bulk Float with the purpose to reduce silica. It was observed
that fourth stagedid not reduce SiO2% appreciably. Hence, three cleanings to Rougher bulk float were
sufficient to reduce SiO2% to the desired level.
Inclined belt
Belt ore feeder conveyor
o/s
Single deck
vibrating screen
u/s
o/s
Inclined belt
Single deck conveyor
vibrating screen u/s Hy. o/f
Sodium
Fine ore bin Silicate
(1.5 kg/t) Hydrocyclone
Water
Hy. u/f
Constant Sulphuric acid (2.5 kg/t) +
weigh feeder Orthophosphoric acid (5.0 kg/t)
Sodium oleate Ball Mill
(0.45 kg/t) Discharge
Ball Mill
Phosphate
Phos. - Carb. depressant
collector Sump Pump conditioner
conditioner Hy. o/f: ~88% -200 mesh (-0.075 mm)
III Cleaner Bulk Flotation III Cl. Bulk Tails Phosphate Conc. Carbonate Float
(Recirculated) (Non-Float) (Reject)
2.0 18.78 2.2
III Cl. Bulk Conc. 9.7 5.58 3.2
28.20 3.81 3.92
42.8 26.52 66.3 1.69 14.42 3.68
7.67 3.77 2.17
O/f
Thickener
Composite Process Rejects
(Carbonate Float + Ro. Tails) U/f
47.9 7.31 20.4
46.36 5.44 5.22
Disc filter
LEGEND
P2O5
Wt. % P 2O 5 % Recovery % 33.1 32.66 63.1
Phosphate Concentrate stockpile
SiO2 % MgO % R2O3 % 9.42 0.65 1.73
Collector addition in single dose vis-à-vis divided starvation dosage was studied.A single dose addition
with 2 min. conditioning time, the flotation time the metallurgical results were on the lower side.
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Addition of collector in divided dose resulted inincreased phosphate recovery due to increased weight %
yield, due to additional conditioning & flotation time. Two divide dosage was found better than three
divided dosages, as the third dose floated more silica than phosphate. But the same resultsof two divide
dosages was also obtained on single doseaddition, but with higher conditioning time of 5 min.Hence,
single dose with higher cond. time was found optimum.
To maximise depression of quartz & silicates the sodium silicate dosage was varied from 0.5 through to
1.5 kg/t. Addition of 1.5 kg/t sodium silicate was found optimum.Addition of extra dosages of sodium
silicate in I& II Cleaner Bulk Flotation did not help in reduction SiO2% content in the Phosphate
Concentrate.
3.11 Effect of change of point of addition of silica depressant from flotation cell to the grinding
mill
The proposed flow-sheet got simpler by addition of sodium silicate depressant in the ball mill itself
instead of flotation cell. The quality of Phosphate Concentrate remained almost same i.e. SiO2 around 9%,
MgO around 1%, P2O5 plus 32% with phosphate recovery of 60% and weight% yield about 33.This study
confirmed that adding in mill was equally effective. This not only removed the need for a separate
depressant conditioner but also saved additional conditioning time.
With a view toreduce SiO2%below 9 in the phosphate concentrate, other methods were also tried. Taking
the advantage of hardness difference between apatite and quartz,differential grinding was applied, which
resulted in formation of coarser silica and finer phosphate grains.Though in laboratory silica could be
reduced by fine sieving to about 6%, the same is not practicable industrially treating high tonnage. Hence,
screening as a process option was ruled out.
3.13 Other methods tested to further reduce MgO content in Phosphate Concentrate
The Phosphate Concentrate produced contained dolomite 6.5% and calcite 3.5% and MgO analysed
around 1–1.3%. To reduce the MgO content below 0.7% in the final phosphate concentrate other methods
were tried viz. addition of dolomite activator (Ethylene Diamine Tetra-acetic Acid), collector extender
(Poly Vinyl Alcohol) during phosphate-carbonate separation stage to enhance dolomite flotation werenot
effective. Frother pine oil successfully reduced the froth instability, thereby making carbonate float
collection easier. This resulted in reduction of MgO% from 1% to 0.66%, making addition of pine oil
essential.
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Table 1: Target Specification of Phosphate Concentrate for Phosphoric Acid manufacture
Vis-à-vis Original Feed Sample &Phosphate Concentrate.
With a view to have plus 60% phosphate recovery in the Phosphate Concentrate, keeping P2O5 plus 32%,
SiO2 within 9-10% and MgO below 0.7%, final tests were carried out with 0.4, 0.45 &0.5 kg/t collector as
single dose with 5 min. conditioning time. Also 5 min. conditioning time was given for phosphate
depression and the results were quite encouraging.
The final test was conducted on the sample to reconfirm the optimized conditions and a suitable process
flow-sheet was developed to produce Phosphate Concentrate of desired quality (Fig. 1). The chemical
assay of the above Phosphate Concentrate met almost all Target Specifications (Table 1). Worldwide, 9-
10% SiO2(quartz form) is acceptable to several phosphoric acid manufacturing plants as it is required for
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Industrial Minerals
arresting the corrosive hydrofluoric acid produced during acidulation stage of phosphoric acid
manufacture.
The low-grade siliceous and dolomitic rock-phosphate ore sample contained mainly apatite (40-45%),
quartz (30-35%), dolomite (~15%) calcite (~7%) with 17.26% P2O5,32.65% SiO2(T) and 3.52% MgO.
Removal of gangue resulted in upgradation of phosphate. All sieve fractions of -10 mesh size original
feed sample assayed more or less same in P2O5, SiO2 and MgO contents indicating no preferential
segregation of phosphate mineral in any fraction. The entire sample required fine grinding for adequate
liberation of apatite from associated quartz and carbonate gangue minerals. Sodium oleate was chosen as
collector for phosphate+carbonates in this sample as the collecting response was excellent. No extra
frother is required while using sodium oleate. Sodium silicate (a good silica depressant) and sodium
oleate resulted in pH 9 to 10 and the anionic collector oleate functioned well in this ideal pH range.
Results indicated that 87.6% -200 mesh grind having d80 size of 61 microns was MOG, with relatively
higher weight yield, higher P2O5grade and recovery with less MgO & SiO2 content. The collector sodium
oleate dose of 0.5 kg/t was found the optimum collector dose. Three cleanings were found to be the
optimum cleaning stages. Divided collector dosages was found better than single dose and two divide
dosages better than three divided dosages, as the third dose floated more silica than phosphate. But single
dose with higher conditioning time of 5 min. was found equivalent to divided dosages. The sodium
silicate dosage was varied from 0.5 through to 1.5 kg/t. With dose of 1.5 kg/t Sodium silicate (to depress
silica) the P2O5% in the Rougher Bulk Float increased from 27.36% to 32.15%, but the phosphate
recovery reduced from 73.6% to 63.6%, due to fall in weight % yield because of depression of more
gangue material, butachieving the P2O5 grade above 32% was important, than recovery, hence 1.5 kg/t
sodium silicate was sufficient & effective in improving the quality of Phosphate Concentrate. Addition of
sodium silicate depressant in the ball mill itself instead of flotation cell made the proposed flow-sheet
simpler, with the quality of Phosphate Concentrate remained similar i.e. SiO2 around 9%, MgO around
1%, P2O5 plus 32% with phosphate recovery of 60% and weight% yield about 33. Thus there was no need
for a separate depressant conditioner and also saved conditioning time. The reasons for SiO2%not reduce
below 9 in the phosphate concentrate, was probed mineralogically. It revealed that nearly 25% of the
silica (quartz) was present as interlocking/ inclusions with phosphate and carbonates, the rest free and of
very fine size. The fine size silica were generated during grinding of coarse quartz particles and from
dislodging of fine grained quartz aggregates present in the sample. This fine silica grains got physically
trapped in the dense froth of Rougher Bulk Float and therefore difficult to separate even after three
cleanings. After differential grinding the phosphate concentrate was wet screened at 200, 270 & 325 mesh
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Industrial Minerals
sieves to separate fine phosphate from coarser silica. The silica content in the Phosphate Concentrate (-
325 mesh) analysed 6.17% reducing from 9.0%. Simultaneously, the P2O5% increased from 32.71% to
34.11%.Conversely due to significant drop in weight % yield from 34.3 to 25.6, the phosphate recovery
reduced from 63.6% to 49.5%. To have plus 60% phosphate recovery in the Phosphate Concentrate, with
P2O5 plus 32%, SiO2 within 9-10% and MgO below 0.7%, final tests for fine tuning the flotation
parameters was carried out with 0.4, 0.45 & 0.5 kg/t collector as single dose with 5 min. conditioning
time and5 min. conditioning time for phosphate depression. At 0.4 kg/t collector dose though P2O5% was
high with low SiO2% and MgO%, the phosphate recovery fell to 41% due to low weight % yield. At 0.5
kg/t, the phosphate recovery improved to 51.6% but SiO2% increased to 10.88%, possibly due to higher
collector concentration, but P2O5% was high and MgO% lowest. To maintain a balance between higher
phosphate recovery with low silica, a lower dose 0.45 kg/t finally produced the best Phosphate
Concentrate assaying 32.59% P2O5, 0.68% MgO and SiO2 9.55% well within the desired level, with
phosphate recovery of 62.5% and weight % yield to 32.9. The Phosphate Concentrate produced was of
desired quality that assayed 32.66% P2O5, 9.42% SiO2(T), 0.65% MgO, 1.11% Fe2O3, 0.62% Al2O3
47.34%, 1.73% R2O3, 47.34% CaO, 3.29% F, and 4.32% LOI with weight % yield of 33.1. The chemical
assay of the above Phosphate Concentrate meets almost all Target Specifications. SiO2 9-10% is
acceptable to several phosphoric acid manufacturing plants for arresting the corrosive hydrofluoric acid
produced during acidulation stage of phosphoric acid manufacture.
5. Conclusions
A low-grade, siliceous &dolomitic rock-phosphate ore sample from district Jhabua, Madhya Pradesh was
studied for on bench scale to develop a beneficiation process flow-sheet to produce phosphate concentrate
for manufacture of phosphoric acid. The sample was lumpy, hard and compact exhibiting heterogeneity.
Main minerals are apatite, quartz, dolomite and calcite. It mainly assayed 17.26% P 2O5, 33.15% Acid
Insol., 32.65% SiO2(T), 3.52% MgO and 30.61% CaO. Finally from beneficiation studies, the process
flow-sheet evolved comprised of (a) ball mill wet grinding to d80 size 61 microns, to liberate phosphate
from gangue minerals, with addition of sodium silicate in the mill as silica depressant. (b) Single stage
Rougher Phosphate-Carbonates Bulk Flotation, at pH 10-11, using anionic collector sodium oleate to
float Rougher Bulk Phosphate-Carbonate to discard silica (quartz) and silica bearing minerals, with
Rougher Tails forming reject. (c) Three cleanings to Rougher Phosphate-Carbonate Bulk Float, at pH 9-
10, mainly to discard more silica. (d) From the III Cleaner Bulk Conc. Phosphate separated from
carbonates by reverse flotation, in three stages, at pH 5-6, using sulphuric acid as pH modifier,
orthophosphoric acid as phosphate depressant and pine oil as frother. Phosphate Concentrate produced
assayed 32.66% P2O5, 9.77% Acid insoluble, 9.42% SiO2(T), 0.65% MgO, 1.11% Fe2O3, 0.62% Al2O3,
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1.73% R2O3(Fe2O3+Al2O3), 47.34% CaO, 3.29% F and 4.32% LOI with phosphate recovery of 63.1%
and weight % yield of 33.1. This assay met almost all the requirements of Target Specification.
Acknowledgements
The authors wish to express thanks to Shri R. K. Sinha, Controller General (In-Charge), Indian Bureau of
Mines, for his keen interest in the investigation and for giving permission to present this paper in MPT-
2015 conference.
References
Indian Bureau of Mines, Mineral Processing Division’s Unpublished Report of Investigation (IBM / NGP
/ R.I. No. 2068).
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EFFECT OF HIGH VOLTAGE ELECTRIC PULSES ON SPECIFIC RATE OF BREAKAGE OF
PHOSPHATE ORE
Seyed Mohammad Razavian 1*, Bahram Rezai 2 and Mehdi Irannajad 2
1
Department of Mining Engineering, University of Kashan, Kashan, Iran
2
Department of Mining and Metallurgical Engineering, Amirkabir University of Technology,
Tehran, Iran
*Corresponding author: razavian@kashanu.ac.ir
Abstract
Comminution, or particle size reduction, involving crushing and grinding, is responsible for at least 40%
of total energy usage in mining and mineral processing. This is largely due to the prevailing use of
tumbling mills for grinding, where the nature of the particle breakage process is unconstrained and
random. In this study, the effect of high voltage electrical pulses on the specific rate of breakage of
phosphate ore was assessed using mono-sized materials of -3.35+2.36 mm, -2+1.4 mm, -1.4+1mm, and -
1+0.71 mm as feed. A novel High Voltage Electric Pulses Crusher (HVEPC) was designed and developed
for electrical treatment. The grinding tests were conducted using a laboratory ball mill under identical
conditions to allow a comparative analysis of the results and the specific rates of breakage (Si) were
determined for those size fractions of mechanical-treated and electrical-treated feeds. It was determined
that breakage of phosphate ore followed a first-order behaviour for fine feed sizes and deviated from first
order for coarse feed size. The specific rate of breakage parameter of mechanical-treated was compared
with electrical-treated phosphate ore under the same experimental conditions and it was found that
electrical-treated materials break faster than mechanical-treated in terms of the Si and A values.
Keywords: High voltage electric pulses treatment, specific rate of breakage, phosphate ore.
1. Introduction
The term high voltage usually means electrical energy at voltages high enough to inflict harm or death
upon living things. Equipment and conductors that carry high voltage warrant particular safety
requirements and procedures. In certain industries, high voltage means voltage above a particular
threshold. One of the high voltage terms is pulse (or impulse) voltage. High-voltage pulses are used to
test electrical equipment and to simulate system-generated over-voltages and lightening surges in power
distribution systems and lightening-protection equipment. In experimental physics, high-voltage pulses
are used to generate strong pulsed electric fields, to study processes of electric breakdown, to produce
short bursts of X radiation (10−7 to 10−6 sec), to generate pulsed electron and ion beams, and to provide
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power supply for spark chambers, image converters, Kerr cells, and charged-particle accelerators (Kuffel
et al., 2000). In recent years, application of high voltage electrical pulse in mineral processing field has
been developed. The history of research in this field is mainly related to the works by Andres (Andres
1989; 1995; 1996; 2010; Andres et al., 1999; 2001). Application of high voltage electrical pulses for the
liberation of minerals was started in 1970 by rejecting the reliance on the water shock waves (Andres
2010). Resulted liberating effect did not much differ from that of the mechanical compression in
crushers, and the impact of balls in tumbling mills. Nevertheless, the results showed that disintegration by
the shock waves was less affected by attrition, comparing to that of mechanical comminution, and also
generated fewer amounts of untreatable fine particles. The first systematic comparative liberation tests
were performed in 1971 on a sample of apatite–nepheline ore from Kola Peninsula. The experimental
results indicated higher percentage of the liberated minerals and lower fine particles in electrical
comminution compared to mechanical comminution (Andres 2010). There are some other reports
demonstrating the effectiveness of mineral liberation by high voltage pulses (Anon 1986; Lastra et al.,
2003; Ito, et al., 2009; Dal Martello, et al., 2012; Dodbiba, et al., 2012). Cabri (2008) at the Institute of
CNT Mineral Consulting in Canada have also investigated electrical and electrohydraulic disaggregation
especially, development of instruments and practical field of mineral processing.
The most comprehensive activity carried out on electrical comminution in the past five years with the aim
of energy consumption optimization was at JKMRC (Julius Kruttschnitt Mineral Research Center) (Wang
et al., 2011; 2012a; 2012b; 2012c; Shi 2013). The activities of JKMRC have been conducted in two major
areas using high voltage pulses: particle pre-weakening and mineral liberation which both focused on
improving energy efficiency. These studies showed that the ores treated by high voltage electrical pulses
with low specific energy input (a few kWh/t) developed cracks and microcracks in the rock, and became
weaker than untreated particles. Comparison of Bond work indices showed that the electrical treatment
can reduce the energy consumption in downstream grinding processes by up to 24%. Moreover, research
conducted at JKMRC showed that higher mineral liberation can be achieved in the electrical
comminution which can lower the consumption of energy (Wang et al., 2011). Wang et al. (2012a)
studied the factors affecting the electrical grinding for six different ores. In this study, parameters such as
feed particle size, undersize aperture, failure potential and energy input were investigated. In addition,
numerical simulation was employed to show the distribution and intensity of the electric field around and
within the particles. The outcomes proved that the electrical comminution performance strongly depends
on the electrical characteristics of the ore. Shi et al. (2013) reported that the pre-weakening effect was
found more pronounced for larger fragments, suggesting that the use of high voltage pulses to pre-weaken
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Industrial Minerals
AG/SAG mill feed may result in more significant benefits in terms of energy savings or increased
throughput than pre-weakening ball mill feed.
The purpose of this research is to study the effect of high voltage electrical pulses treatment on specific
rate of breakage of phosphate ore.
Table 1: Chemical analysis of the important elements and oxides of phosphate ore.
Crushing chamber consisted of a rod-shaped electrode made of copper. The voltage between the generator
and ground electrode made of an iron plate was measured by a probe connected to the oscilloscope. The
ground electrode consists of circular apertures to pass the crushed particles and prevent over-crushing
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(control sieve). The sample was immersed in the water in the chamber between two electrodes and then a
high-voltage pulse was directly discharged to disintegrate the sample.
Figure 1: 3D schematic diagram of high voltage electric pulses crusher (HVEPC); C: Capacitor.
Two representative samples were crushed to -3.35 mm by jaw crusher and HVEPC, separately and then
screened by standard ASTM sieves. 300 g of seven particle size classes (-3.35+2.36mm, -2+1.4 mm, -
1.4+1 mm, -1+0.7 mm) were prepared to determine the breakage function. The tests were conducted in a
steel cylindrical ball mill of 200 mm internal diameter and 250 mm length with smooth end walls in
which one end could be removed and locked in its position with a quick release locking clamp. Detailed
information of laboratory breakage function test is shown in table 2.
Diameter (cm) 20
Length (cm) 25
Mill
Volume (𝑉𝑚 ) (cm3) 7850
Fraction of critical speed 0.75
Diameter of balls (mm) 35 25 15
Percent of balls (%) 40 45 15
Balls Total mass of balls (𝑀𝑏 ) (g) 7600
Balls density (𝜌𝑏 ) (g/cm3) 7.76
Percent of formal ball filling, J a 20
Sample weight (𝑀𝑠 ) (g) 300
Sample Solid density (𝜌𝑠 ) (g/cm3) 3.2
Percent of formal sample filling, F b 2
𝑀𝑏 /𝜌𝑏 100b Ms /ρs 100
a
𝐽=( )× 𝐹=( )×
𝑉𝑚 0.6 Vm 0.6
2.4. Methods
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When an efficient breakage occurs in a mill, it is useful to assume that the breakage of each size fraction
is of first order in nature (Austin, 1972).
𝑆1 𝑡 (2)
log[𝑊1 (𝑡)] = log[𝑊1 (0)] −
2.3
Where W1(0) and W1(t) are the weight fractions of the top size fraction at time zero and t, respectively. Si
is a proportionality constant called the specific rate of breakage, with unit of time-1. A straight line whose
slope is –S/2.3 is obtained from plot of W1(t) on log scale versus t, on linear scale. However, the rate of
particle breakage may deviate from linearity due to changes in the nature of comminution events or due to
changes in the heterogeneity of particles being ground. Austin, Klimpel, and Lucki (1984) proposed the
relationship for the variation of the specific rate of breakage Si with particle size,
𝑋𝑖 𝛼 (3)
𝑆𝑖 = 𝐴 ( ) 𝑄𝑖
𝑋𝑂
Where, X0 is the standard size (taken here as 1 mm), Xi is the upper limit of the size interval i, A and α
are model parameters that depend on the properties of the material and grinding conditions. Qi is a
correction factor, which is 1 for small particles (normal breakage) and less than 1 (abnormal breakage) for
too large particles to be nipped and fractured properly by the ball size in the mill. In the abnormal
breakage region, each size behaves as if it has some fraction of weak materials and the remaining fraction
of stronger material. Using a mean value for Si in this region, values of Qi are empirically described by
1 (4)
𝑄𝑖 =
𝑋
1 + ( 𝜇𝑖 )𝜆
Where, µ is the particles size when the correction factor is 0.5 and λ is a positive number (𝜆 ≥ 1).
Experience has shown that λ can be satisfactorily taken as 3 for most materials, especially when the top
size of the feed to the mill to be simulated is not much larger than µ (Austin, Julianelli, and Schneider
2007).
The first-order plots for various feed size of phosphate ore are illustrated in figures 2–4. The results
indicated that grinding of fine size fractions could be described by the first-order law. However, the
coarse size fraction (-3.35+2.36 mm) showed deviations from it. This is a typical result for a feed that has
some too large particles to be nipped by the ball size in the mill, thus the rate of breakage is less than
expected and decreases as grinding proceeds, probably due to the accumulation of the harder (stronger)
material in the remaining feed material (Austin, Julianelli, and Schneider 2007). The S i values are
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Industrial Minerals
estimated from the average of the plots as shown in Table 3. The results show that in the electrical
treatment, the increase in the breakage rate occurs as particle size is increased. For example, at -3.35+2.36
mm feed, in comparison of electrical treatment and mechanical treatment about 17% increase in breakage
rate was achieved.
Figure 5 shows the variation of Si values against feed particle sizes for mechanical-treated and electrical-
treated feeds. It can be seen that for both conditions, the values sharply increased until about 1.4 mm and
then decreased. This means that there is an optimal feed size (in this condition, approximately 1.4 mm)
where the greatest breakage occurs. After 1.4 mm, the values decreased. This can be explained by the fact
that large particle sizes are difficult to be reduced and ground by the medium, so the grinding efficiency
has to be decreased. The variation of Si values with particle size were fitted to Equation (3) and specific
rate of breakage parameters A, α, µ, and λ that depend on the properties of the materials and the grinding
conditions are given in Table 4.
Figure 2: First-order plot for batch dry grinding of feed -3.35+2.36 mm (1).
Figure 3: First-order plot for batch dry grinding of feed -2+1.4 mm.
1
ET: Electrical Treatment, MT: Mechanical Treatment
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Industrial Minerals
Figure 4: First-order plot for batch dry grinding of feed -1+0.71 mm.
Parameter A α µ λ
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4. Conclusions
Dry grinding of single-sized fractions of phosphate ore showed that fine fractions of this material follow
the first-order breakage law, but breakage rate of coarse fraction deviates from first-order. The specific
rates of breakage (Si) values of phosphate ore increase with increasing feed size fractions until reaching a
maximum value, and then decrease at coarse fractions. Electrical treatment increases the breakage rate of
phosphate ore especially at smaller size fractions. Electrical treatment creates new cracks and develops
network cracks at the borders between minerals. The specific rate of breakage parameters of mechanical-
treated phosphate ore were determined and compared with parameters of electrical-treated phosphate ore
ground under the same experimental conditions; it can be expressed that the electrical-treated phosphate
ore is broken faster than the mechanical in terms of the Si and A values. Based on the above findings, it
can be concluded that electrical-treated phosphate ore will be ground faster and will give lower proportion
of fines compared with untreated ore under the same grinding conditions. In other words, electrical
treatment of phosphate ore increases the breakage rate and throughput of grinding with a minimum
proportion of fines.
Acknowledgments
The authors would like to acknowledge Iran Mineral Processing Research Center (IMPRC) for their
cooperation and substantial input into the research essential for this paper and Esfordi phosphate complex
for supplying grinding circuit data.
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Dodbiba, G., Nagai, H. Wang, L. P., Okaya, K., Fujita, T., 2012, "Leaching of indium from obsolete
liquid crystal displays: comparing grinding with electrical disintegration in contex of LCA," Waste
Management, Vol. 32, No. 10, pp. 1937-1944.
Ito, M., Owada, S., Nishimura, T., Ota, T., 2009, "Experimental study of coal liberation: electrical
disintegration versus roll- crusher comminution," International Journal of Mineral Processing, Vol. 92,
pp. 7-14.
Kuffel E., Zaengl W.S., Kuffel J., 2000, High Voltage Engineering Fundamentals, Second edition
published by Butterworth-Heinemann, 539 pp.
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Lastra, R., Cabri, L., Weiblen, P., 2003, "Comparative Liberation study by image analysis of Merensky
Reef samples comminuted by electric- pulse disaggregation and by conventional crusher," Proceeding of
XXII International Mineral Processing Congress, Cape Town, South Africa, Vol. 1, pp. 251-260.
Makokha, A. and Moys, M. H., 2006, ‘‘Towards optimizing ball-milling capacity: Effect oflifter design.’’
Minerals Engineering, 19, pp. 1439–1445.
Shi, F., Zuo, W., Manlapig, E., 2013, “Characterisation of pre-weakening effect on ores by high voltage
electrical pulses based on single-particle tests”, Minerals Engineering, Vol. 50-51, pp. 69-76.
Wang, E., Shi, F., Manlapig, E., 2011, "Pre-weakening of mineral ores by high voltage pulses," Minerals
Engineering, Vol. 24, pp. 455-462.
Wang, E., Shi, F., Manlapig, E., 2012a, "Factors affecting electrical comminution performance,"
Minerals Engineering, Vol. 34, pp. 48-54.
Wang, E., Shi, F., Manlapig, E., 2012b, "Experimental and numerical studies of selective fragmentation
of mineral ores in electrical comminution," International Journal of Minerals Processing, Vol. 112-113,
pp. 30-36.
Wang, E., Shi, F., Manlapig, E., 2012c, "Mineral liberation by high voltage pulses and conventional
comminution with same specific energy levels," Minerals Engineering, Vol. 27-28, pp. 28-36.
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CHARACTERIZATION & EXTRACTION OF POTASH FROM INDIAN GLAUCONITIC
SANDSTONE
Abstract
Potassic fertilizers have a vital role in Indian agriculture. At present, the country entire demand of potash is
met through imports. India doesn’t have marine evaporative deposits, but have huge deposits of low grade
potash resources in the form of k-feldspar and glauconitic sandstone. About 3000 million tonnes of
glauconitic sandstone containing 4 to 6% K2O is available which can be a potential source for potash.
Glauconitic sandstone is a complex rock having dicotahedral T-O-T structure and promising source for the
recovery of potassium values. An attempt is therefore made to study the mineralogy and chemical
composition of glauconitic sandstone collected from Guneri area of Kuchchh district, Gujarat (India). The
detail characterization of collected glauconitic sandstone has been performed using XRD, SEM-EDX, XRF,
AAS, and conventional analytical tools. Analysis of various size fractions of sample with compositions:
3.93% K2O, 10.75% Fe2O3, 4.41 Al2O3 and 70.35% SiO2 was carried out and it was observed that rejection
of + 425µm size fraction (~30%) could enrich the potash content from 3.9% to 5.5%. The enriched fraction
with 5.5% K2O was further treated to recover potash by chemical treatment. Various parameters for pre-
treatment as well as dissolution conditions for potash were optimized and achieved >90% K2O dissolution.
1. Introduction
Potassium is one of the three primary nutrients for plant growth, together with nitrogen and phosphorous.
About 90% of potassium use is in the production of fertilizers. Initially it was produced from burning wood
in pots. Later the demands for potash go on increasing and rose to 34.6 million tonnes in 2013 throughout the
world (United State Geological Survey, 2013). Today most of the potash demands are meet through bedded
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marine evaporite deposits such as sylvite, carnalite, kainite, etc. These deposits are mainly concentrated in
countries like Canada, Russia, Belarus, Brazil, and China. Since India does not have any commercial
resources of potash, a large quantity is imported every year from the global market to meet the agricultural
demand. So, attempts are being made to find and exploit alternative sources of potassium which can, at least
partly, substitute for the imported potassium fertilizer. In India the potential of the different non-conventional
sources of potassium for use in agriculture was reviewed earlier by Soni et al. (1990).Out of different non-
conventional source glauconitic sandstones deposits which are available in plenty is one of the important
indigenous resources for potash in India. India has vast reserves of more than 3,000 million tonnes of
glauconitic sandstone containing 4 to 6 % K2O have been estimated to occurs in Madhya Pradesh, Uttar
Pradesh, Rajasthan and Gujarat (Geological Survey of India, 2005). Glauconite is a group of dioctahedral,
potassium, iron-rich, compositionally heterogeneous, phyllosilicate (clay) minerals. Indian glauconitic
sandstone is mainly associated with quarts, muscovite, chlorite, feldspars, microcline, orthoclase, calcite,
brucite and ferromagnesian minerals. The detail mineralogical composition of Indian glauconitic sandstone in
different size fraction was studied by Rawlley et al. (1994). He attempted different processes in the
laboratory for extraction of potash (Rawlley, 1991; Rawlley and Amritphale. (1991a-c) and Rawlley et al.
(1991). A few initial attempts are being made by Choudhuri et al. (1973), Sharma et al. (1979), Yadav and
Sharma et al. (1992), Mazumder et al. (1993) and Sharma et al. (1993) in India to extract potassium from
glauconitic sandstones through thermal and chemical treatments. Rao et al. (1993) have conducted tests in
presence of fluoride salts such as NaF, HF and LiF for dissolution of potassium. Majumdar et al. (1995) have
used some empirical correlations to describe the kinetics of high temperature reactions. Yadav et al. (2000)
have conducted leaching tests and studied the dissolution kinetics of potassium with sulphuric acid.
The reported processes use high concentration of acid, fluoride salt and high dissolution temperature etc. for
recovery of potash. However in the present work, an attempt has been made to recover potash under a mild
condition by breaking the matrix through a suitable pre-treatment. Findings reported here is part of a
preliminary study undertaken to explore the possibility to use glauconitic sandstone deposit of Guneri area of
Kuchchh district, Gujrat (India) for recovery of potash values.
Glauconitic sandstone samples were collected from the Guneri area of Kuchchh district, Gujarat (India). The
reserve of this belt contains an average of 5% K2O with 0.02 million tones of glauconitic sandstone up to a
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depth of 2.0m. The location index of this area is latitude (23°46'55.3") and longitude (68°52'17.4"). The
Sample collected is belongs to Bhuj formation and these rocks are thinly laminated and thinly bedded
between ferruginous sandstone is shown in Figure 1. The figure shows the pit (made by GSI-2015) (a) and
the collected sample (b).
The collected sample were first crushed and ground to -2360 µm and then a representative sample of total
bulk was selected by conning and quartering after proper mixing. The representative sample was ground in a
steel mortar and passed through a Standard Sieves of -75 µm for characterization study. The Sample was
examined by the following instrumental methods. Chemical analysis was performed by using Bruker X-ray
fluorescence (XRF), SRS 3400 operated at 40 kV and 60 mA, Atomic absorption spectrometer (AAS) of
Thermo S-series, Gravimetric and Volumetric method. XRD pattern is obtained with a Bruker diffractometer
model D8 discover using Ni filtered Cu Kα radiation and operated at 40 kV and 40 mA. The XRD pattern
was recorded from 6⁰ to 90° 2θ with a scanning speed of 0.02° 2θ per second to identify different phases
present in the sample. The back scattered electron image and morphology of the sample are analyzed by
scanning electron microscopy attached with EDX by using Hitachi S-3400N. Based on these studies sample
was further beneficiated through screening. The leaching experiments were carried out in a 500 mL glass
vessel placed on a magnetic stirrer at different temperature. The beneficiated glauconitic sandstone was
further pre-treated in presence of a suitable reagent for further dissolution study to achieve higher potash
recovery.
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3.1 Physical and Chemical properties
To initiate a method for extracting potassium it is necessary to confirm the different mineral phases and their
associations, which is performed by systematic characterization study. The elements aluminum, titanium,
sulphur, phosphorous, chlorine, vanadium, chromium, zinc & nickel etc was quantitatively determined by
XRF analysis. Element such as potassium, calcium, sodium and magnesium where determine by using AAS
after suitable tri acid dilution of the sample. Silica and total iron was determining by conventional method.
Prior to analysis the sample was heated at 378 K for 24 hours to remove moisture. The sample was treated at
1223 K for 3 hours to determine volatile content. The complete chemical analyses of sample for size fraction
(-2360 µm) in weight percent of their oxide are reported in Table 1. The sample contains only 3.93% K2O as
the valuable component. The other major constituents present are: SiO2 - 70.35%, Fe2O3 - 10.75% and Al2O3
- 4.41%.
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Some of the lines for quartz (4.25, 3.34, 2.45, 2.28, 2.12, 1.81, 1.67, 1.37 and 1.25 Angstrom) are overlapped
by the lines for the other mineral phases present, while the intensities of the lines that are not overlapped at
(1.81, 1.38, 2.12, 1.21 and 1.19 Angstrom). The presence of glauconite mineral is indicated by d-values
10.06, 4.54, 3.34, 2.58, 2.23, 2.12, 1.81, 1.67, 1.51 and 1.37 Angstrom. Whereas orthoclase (4.25, 3.34, 3.24,
2.58, 2.12 and 1.98 Angstrom), microcline (4.25, 3.34, 3.24, 2.58 and 2.45 Angstrom) and brucite (4.36,
2.23, 1.67, 1.53, 1.51 and 1.25 Angstrom) are other phases associated with the glauconitic sandstone. Sample
was also scanned in secondary electrons (SE) for study the morphology of major mineral present. From this
electron micrograph, it is evident that the silica is present in facet shape whereas mineral glauconite is
present in irregular shape. The SE image along with EDX analysis is shown in Figure 3.
Elemental mapping of the area shows the presence of Si, Al, Mg, K, and Fe that is all the possible
constituents of glauconite mineral. It clearly shows the major elements present in the sample where silica as
the corresponding peak have highest intensity as amply supported by chemical analysis and XRD.
For beneficiation study the entire sample was crushed and ground to below -2360 µm for experimental work.
A representative sample of the total bulk was collected for particle size analysis along with K2O, SiO2 and
total Fe values as given in Table 2. From this table it is clear that coarser fraction bears more SiO2 and its
value decreases with the reduction in the particle size of the sample. The K2O and Fe value increase with
particle size reduction. Particles size above 425µm contains more than 90% SiO2 and very less amount of
K2O value. More than 30% of the sample lies above 425 µm with average content of only 0.17% K2O can
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easily be rejected. Thus the total rejection of potash was only 1.3% of the original content. So, for further
leaching study particle size below 425 µm was considered. For particles below this size fraction the head
sample analysis give K2O value up to 5.52%.
Table 2: Size and size-wise K2O, SiO2 and total Fe analysis of glauconitic sandstone.
All the leaching experiments were carried out in a 500 mL three naked glass vessel using 10% pulp density at
303 K and 353 K for 20 minutes with stirring speed of 200 rpm. Initially, the glauconitic sandstone sample
was subjected to water leaching at 303 K as well as 353 K. It was observed that the soluble potash was less
than 2%. A measured amount hydrochloric acid of concentration in the range of 1.1 - 3.3 N (10-30% v/v)
was added into the glass vessel and heated slowly to the desired temperature of 353 K. Though potassium
recovery was increasing with increasing the hydrochloric acid concentration, the maximum recovery
achieved was only about 12% (figure 4a) at 353 K using 3.3N (30% v/v) acid. The iron dissolution was also
found in similar range (figure 4b).
This indicates that the potassium is locked between dioctahedral T-O-T structures. An attempt has been made
to break the structure before chemical treatment.
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20 20
% Fe extracted
% K extracted
12 12
10 10
8 8
6 6
4 4
2
2
0
0
10 15 20 25 30
10 15 20 25 30
HCL Concentration (v/v) HCL Concentration (v/v)
(a) (b)
Figure 4: Dissolution of potassium (a) & iron (b) against HCL concentration.
100 100
90
Raw Sample
Reduced Sample
90 Raw Sample
80 80 Reduced Sample
70 70
% K extracted
% Fe extracted
60 60
50 50
40 40
30 30
20 20
10 10
0 0
10 15 20 25 30 10 15 20 25 30
HCL Concentration (v/v) HCL Concentration (v/v)
(a) (b)
4. Conclusion
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The glauconite sandstone collected from Guneri area of Kuchchh district, Gujarat (India) containing -3.9%
K2O could be enriched to 5.5% by mild grinding and screening to below 425µm. The potassium present in
glauconitic sandstone is intricately associated with different mineral phases present in the host rock.
Chemical leaching with 30% (v/v) hydrochloric acid at 353 K could extract only 12% potassium. More than
91% potassium recovery was achieved through pre-treatment of the sample followed by acid leaching under
similar condition.
Acknowledgment
The authors are thankful to the Director, CSIR- National Metallurgical Laboratory for his permission to
present this paper. Thanks to Dr. P.R. Golani, Director, GSI (Jaipur) and Mr. Hajaj Basheer, Geologist (Sr.)
for helping us in collecting the samples.
References
A.K. Mazumder, T. Sharma, and T.C.Rao. Extraction of potassium from glauconitic sandstone by the roast-
leach method. Int. J. Miner. Process., 38: 111-123, 1993.
A.K. Majumder, B. Govindarajan, T. Sharma, H.S. Ray, and T.C. Rao. 1995. An empirical model for
chloridising-roasting of potassium in glauconitic sandstone. Int. J. Miner. Process.43, 81–89, 1995.
B.R. Rao, L.S. Rao, A.K. Mazumder, G.M. Rao, and T.C. Rao. Fluoride aided potassium extraction from
glauconitic sandstone for liquid fertilizer. Miner. Eng., 6 : 405-413, 1993.
M.K. Soni. On the possibility of using glauconitic sandstone as a source of raw material for potash fertilizer.
Indian Min. Eng. J.,11: 3-10, 1990.
R. Choudhuri, A.T. Balagopal, and K.C. Banerjee. Availability of potash from non-traditional sources.
Technology., 10: 128-131, 1973.
R.K. Rawlley. A process for the extraction of potassium from glauconitic sandstone useful for fertilizer
application. Indian Patent, Application No. 243/DEL/91.
R.K. Rawlley, and S.S. Amritphale. A process for recovering potash and a PK composition for fertilizer use
from glauconitic sandstone. Indian Patent, Application No. 244/DEL/91 (a).
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R.K. Rawlley, and S.S. Amritphale. A process for the preparation of a bi nutrient composition useful in
agriculture by utilizing glauconitic sandstone and rock phosphate. Indian Patent, Application No.
245/DEL/91(b).
R.K. Rawlley, and S.S. Amritphale. A novel process for making potassic fertilizer from glauconitic
sandstone using a double salt. Indian Patent, Application No. 566/DEL/91(c).
R.K. Rawlley, S.S. Amritphale, and B. Kujur. A process for recovering potash values from glauconitic
sandstone using common salt. Indian Patent, Application No. 247/DEL/91.
R.K. Rawlley. Mineralogical investigations on an Indian glauconitic sandstone of Madhya Pradesh state.
Applied Clay Science., 8: 449-465, 1994.
S.K. Sharma, A.K. Roy, A.T. Balagopal, and H. Roy. High temperature interaction of glauconite with
calcium salts. Fert. Technol., 16: 41-46, 1979.
T. Sharma, T.C. Rao. Acid leaching of glauconitic sandstone. Trans. JMM Sec. C 101, 165–170, 1992.
United State Geological Survey, 2013 “Potash”, Mineral Year book. www.usgc.gov.
V.P. Yadav, and T. Sharma. Leaching of glauconitic sandstone in acid lixiviants, Miner. Eng., 5: 715-720,
1992.
V.P. Yadav, T. Sharma, V.K. Saxena. Dissolution kinetics of potassium from glauconitic sandstone in acid
lixiviant. Int. J. Miner. Process. 60, 15–36, 2000.
V. Kumar, and P.C. Bakliwal. Potash in india. Geological Survey of India. 2005.
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CURRENT PRACTICES AND INNOVATION IN THE MINERAL SECTOR: A FOCUS ON
SUSTAINABLE DEVELOPMENT
Nikhil Agrawal1,*, Neeloy Choudhury2, Pranjal Dwivedi3
1
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad.
2
Department of Mining Engineering, Indian School of Mines, Dhanbad
3
Department of Environmental Engineering, Indian School of Mines, Dhanbad
*Corresponding author: nkhlgrwl900@gmail.com
Abstract
In the wake of a major boost to infrastructure development and industrialization initiatives in India it is
inevitable that relevant activities in the mineral sector like exploration, mining and processing will also
increase proportionally. This has highlighted many aspects with serious implications for the future. The main
infrastructural mineral resources like iron ore deposits are already declining in quality and quantity. A vast
portion of the industrial coal demands in India are met by imports. Exploration of new reserves and their
extraction will be necessary to meet heavy demands from the domestic industrial market segment. Apart
from putting excessive strain on the existing natural resources in India and raising the pressure on imports,
this is a great cause for environmental concern. Environmental sustainability and energy efficiency is a must
for any developmental activity. Putting this scenario in perspective it has become absolutely necessary to
promote sustainable development in all sectors and keep environmental viability at top priority during
planning, assessment and execution. This paper deals with four aspects of the mineral sector: exploration,
mining, processing and end-usage, keeping a focus on sustainable practices and environment-friendly
solutions to industrial problems. The concept of Life Cycle Assessment and its applications has also been
discussed.
1. Introduction
Development is a continuous process and will keep on affecting changes in the interactions between man and
nature. Whenever a technological problem is faced by the society, scientific and engineering solutions are
sought to solve it. The resultant solution is termed as development. Unfortunately, more often than not, a
solution or development leads to other eventualities. These can be both environmental as well as
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humanitarian. Hence each decision regarding solving a problem must be taken with regard to all facets and
not just a few.
The concept of sustainability is based on the need of a holistic approach in planning and execution of
developmental activities. It has now been finally agreed upon that any major anthropogenic activity is not an
isolated event, and has much greater implications rather than just a localized change. Just as all ecosystems
on earth are mutually interdependent, similarly, any major change resulting from human activities in one
corner of the globe has the potential to impact other zones as well.
From the point of view of the mineral sector, sustainability deals with those practices which ensures
conservation of the resource under consideration, conservation of environment, positive impact on local
communities and their involvement, reduction in wastage and increase in the efficiency of utilization.
The mining and mineral industry has been beset with troubles since quite a long period of time. But the crux
of the issues lies within the hurdles of global market slowdown and environmental concerns. This situation
was partly inevitable since India is a developing economy and it is unable to make a drastic cut in its
emission levels without jeopardizing its growth rate. These factors, combined with illegal mining activities
have often prompted the government as well the judiciary to impose bans. In September, 2012 iron ore
mining was banned in Goa. This was sanctioned by the Ministry of Environment and Forests. In the year
2011-12 Goa had exported 42 million tons of iron ore. However, this ban was lifted in January, 2015,
following the formulation of new mining policies for the state.
On July and August, 2011 following a mining scandal and concerns over environmental degradation, iron
mining was banned in Karnataka by the Supreme Court. The State Government of Odisha had imposed
similar bans on iron ore exporting. These bans on exports and mining activities have lead to a loss of about
50,000 crores INR to the Indian economy over the past three years.
Though several of such bans have been removed by now, the iron ore industry will take time to revive and
reflect on the economy. The above situations highlight the fact that mining must be undertaken in a well
planned manner with due regard to the environment. Ever increasing demands of materials like iron ore, coal,
aluminium, etc. along with the fear of environmental degradation makes it imperative that sustainability is
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incorporated into each stage in the life cycle of a mineral. Prior to that advanced exploration techniques are
also needed to ensure that new reserves are located before current run out.
2.1 Mining
The mining industry is inarguably one of the most important sectors of the economy. The rising demand for
steel and power makes it imperative that this industry is expanded in India and abroad. On the other hand,
mining activities also contribute to land, water, air and noise pollution as well. Therefore the need of the hour
is to adopt green practices which are environmentally as well as economically sustainable.
One such method is In-situ leaching (ISL). It is a process to recover minerals such as copper, uranium, gold
and salt deposits through boreholes drilled into the deposit. It is applicable to deposits which are too deep or
too thin for underground mines and the ore body needs to be permeable to the liquids used, and located so
that they do not contaminate groundwater away from the ore body. Surface disturbances and soil
contamination are prevented. Other advantages of in-situ leaching include reduction in hazards for the
employees from dust, radiation and accidents. Further, no tailings or waste rocks are generated, which in turn
eliminates the cost involved in tailing-mill operations.
In-situ leaching is practiced in more than 47 % of uranium mining in whole world. USA, Kazakhstan,
Uzbekistan, Australia, China and Russia are the countries who have implemented ISL for their mining
activities. With further advancements in the technology this process might gradually be used in other areas as
well.
It is infeasible to convert all current mines to more environmentally friendly mining methods due to
economic constraints and ore deposit geography. However, when opening new mines in areas with low risks
of water contamination, in-situ leaching should be the choice method when physically possible.
Another technology relevant to the energy sector is Underground Coal Gasification (UGC). Underground
Coal Gasification (UCG) is a clean coal technology. UCG permits coal to be gasified in situ within the coal
seam, via a matrix of wells. The coal is ignited and air is injected underground to sustain a fire, which is
essentially used to “mine” the coal and produce a combustible synthetic gas. This can be used as a fuel for
power generation and heating process. UCG is able to extract coal reserves that would not normally be mined
which would increase the resources available.
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The need for finding alternatives to coal-fired power plants has necessitated more research into this
technology. Also, the high prices and availability constraints of natural gas widen the scope of coal gas
usage. In the past few decades, crude oil prices have risen continuously, with the exception of a few months
of lean period owing to a glut in supply and low demands. Hence, a low cost alternative like UCG would be
economically viable.
The biggest advantage of this process is that those coal deposits which were previously considered non-
amenable to conventional mining can be utilized. The hassles of ash handling and transportation are also
eliminated. Typically, the chemical efficiency of this process is about 75 %, but the recovery is as high 95 %.
Recently, the Bamunara Industrial Belt near Durgapur, West Bengal, has switched over to natural gas for its
cast iron foundries and steel rolling mills. This has resulted into lower costs and reduced emissions to a great
extent. Currently, with the increasing shortage and severe odds of using coal, opting for natural gas is a major
step towards sustainable development. In cases where procuring natural gas is difficult, UCG can be
implemented on long term basis, leading to further cost cuts. The only drawback is that the calorific value of
Coal Gas is lower than natural gas. Hence, more volume of coal gas is required for fuelling the same
operations which are run by natural gas.
2.2 Processing
In the field of mineral processing, iron ore and coal are two most investigated materials. Beneficiation of
both is a necessity as well as challenge to the industry. In India, the prevalent practice is to wash coking coal
and met-grade coal, but thermal coal is usually charged directly into boiler furnaces after size reduction.
Most of the coal found in the Indian Subcontinent is of drift origin and hence high in ash content. This
generates huge amounts of ash every year and also leads to a lot of pollution.
In 2011, an ash dyke built in Korba Super Thermal Power Station in Chattisgarh gave away after heavy rains
in the area. Following heavy seepage and land subsidence, an entire section of the ground beneath the ash
dyke failed. Huge amount of water and ash mixture flowed into the nearby village and township. Further, the
vast ash dyke fields of NTPC in Farakka, West Bengal has created several health related casualties and
environmental degradation. There had been numerous complaints regarding diseases like skin cancer and
eczema in the nearby villages. This has been caused drying up of the surface ash in the dykes, which are
subsequently blown away by winds and carried into the air space of surrounding land area.
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Another crisis engendered by excessive ash generation is the shortage of land that could be used for creating
ash dykes. India, being a vastly populated country, is already reeling under the demand of land for
industrialization, housing as well as agriculture. Available land resources are already strained and further
acquisition of land would result into deforestation, which in turn would create severe environmental
concerns.
Such ash handling problems raise serious issues about the production of ash annually. Dumping and storage
is no more a viable solution owing to various problems that come up. A sustainable solution in this regard
would be to wash thermal coal to reduce the ash percentage prior to burning in furnaces.
Changes can also be made by using other tailings storage techniques. Paste-tailings can be dried out and laid
flat in a facility, which makes them less volatile and more compact. This reduces the supply of fresh water
needed, since the water from tailings can be recycled and the chemical reagents in tailings that can be
recycled along with the water. Sometimes amounts of the metals being mined end up in the wastes.
Reprocessing these wastes can result in more usable material.
It has been found that traditionally, the tribesmen living in the Indian forestlands used to practice
conservation principles which were inherited down the generations. They derived their subsistence from the
forests but also took care of the replenishment of resources. Hence, the forest ecosystems were intact in spite
of human habitation. But unfortunately, since the onset of industrialization, large scale deforestation has
occurred. Apart from the loss of biodiversity and ecosystems, the original inhabitants of those lands are also
displaced. They not only lose their livelihoods but they are also cut-off from their hereditary knowledge and
principles regarding the environment. Consequently, when these people are relocated to other places, they
contribute to degradation of the environment instead. In a survey conducted on 25 households in the project
affected region of NTPC Rihandnagar in the state of Uttar Pradesh reveals that.
Government and the corporate houses have developed rules and laws with an aim to compensate for the
losses of these people in various ways. Some of these measures include providing them with jobs in the
upcoming projects, relocating them elsewhere and offering monetary compensation, etc. among these
measures, monetary compensation is arguably not the best form of compensation until and unless other
infrastructure and amenities are provided. Proper counseling and rehabilitation programs are must in order to
assimilate them into the mainstream society.
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Class-C fly ash, produced by burning lignite and sub-bituminous coal, has self-cementing properties. Hence,
this can be used by the cement manufacturing industry. Also, fly ash can be used for manufacturing bricks
and glazed tiles, fertilizers and extraction of other chemicals. A host of other applications are also being
considered. In this way, a bulk of the ash generated each year by the coal-powered electricity generating
plants would be utilized. In developed nations like Germany, more than 80 % of the fly ash generated is
utilized, whereas, in India such practices are very limited. Green practices involving fly ash must be
encouraged in order to address pollution and land availability issues.
Indian thermal plant boilers are designed according to 45% ash Indian coal. Whereas, imported coal from
Indonesia, Australia and South Africa contain less than 10 % ash. Due to these reasons, it is a common
practice to charge coal into furnaces after blending Indian coal with imported coal. This improves furnace
efficiency and also reduces the overall ash percentage in the coal feed. Another option is to manufacture
boilers with specifications allowing for higher GCV coal. Then, higher GCV imported coal could be charged
in a higher proportion.
Environmental trading, in the form of carbon dating and Clean Development Mechanism(CDM) are also
relevant to SA mining industry in terms of CP. The mining industry is a major source of greenhouse gases
both directly through mining and mineral beneficiation activities and indirectly through production of coal.
CDM projects can earn saleable certified emission reduction (CER) credits, each equivalent to one ton of
CO2, which can be counted towards meeting Kyoto targets. Most potential CDM projects in the mining
industry will fall into one of the following categories:
1. Reduction of emission of methane gas, either directly from coal seams or indirectly from industrial
processes.
2. Reduction of consumption of fossil fuels.
3. Reduction in the use of electricity.
4. Improvement of the efficiency of mineral extraction or processing.
5. Improvement the management of oil usage.
6. Introduce incentive schemes for all employees with practical, effective cleaner production
suggestions.
3. Life Cycle Assessment
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LCA is called a "cradle-to-grave" assessment which involves an assessment of the environmental impacts of
products, processes or services from raw materials to waste. This practice is critically relevant to the mining
and mineral processing sector. The entire process can be summed up in 4 basic steps.
An effective use of this assessment tool has been seen in a Baryte based mineral processing unit in the
Kadapa district in Andhra Pradesh, India.
The supply data for processes were collected and collated directly by visiting the factory for around 15 times.
Open interview method was undertaken with factory management officials to know the input data for the
processes to be included inside the system boundaries. Majority of the industries of this kind are using more
or less the same infrastructure and processes and thus comparison among different processes was not
undertaken. The Baryte minerals which were mined and transported to the factory, sorted then grinded to fine
grained size and exported to other regions for its varied utilization in various industries like oil drilling
mud, medicines, plastic fillers, paint, foam, crackers, glass and urea manufacture, floor coverings and textiles
were studied. The electrical energy utilized by motors of capacity 5hp to 25hp mainly for running roller
machines was considered. Water utilized for cleaning the rock material was considered. Handling of raw
and waste material and precautions taken by the work was considered Secondary data were used to
describe the environmental impact of energy use and transport. Mining hazards at mine places were not
included. The study was confined to impacts on natural environment. It does not include the risks of
accidents or parameters for which the environmental impact has not yet been thoroughly examined like
radiation etc.
These are the kind of sample parameters and data which need to be collected before a comprehensive Life
Cycle Assessment in a mineral processing industry of any kind. The full analysis of this which includes the
Impact Assessment report and the Inventory Assessment can help the industry to minimize costs and
optimize their process while checking for sources of noise, land and air pollution helps cut down the
environmental impact of the industry. A SWOT (Strengths, Weaknesses, Opportunities, and Threats) analysis
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Industrial Minerals
also helps judge the overall sustainability and feasibility of the whole project taking into account factors
across all spectrum.
4. Conclusion
It is an accepted fact that the cost of prevention is lesser than the cost of mitigation. Experts have predicted
that industrialization of India would be completed by 2050. To power such growth at a constant rate, cheap
power is needed. This implies building up many more thermal power stations, which will further create
pollution and ash handling problems. In the future, it is likely that environmental conservation norms and
requirements will be made even more stringent in order to mitigate climate change and related environmental
issues. If the malpractices aren’t given up immediately and green technology isn’t adopted soon, then the
mitigation costs will be enormous in the future. Hence, if preventive measures are implemented now, then the
cumulative costs will be much less than for all the stakeholders.
Another motivation for adopting sustainability in industrial practices is that the rights of the future
generations will be reserved in terms of mineral usage and other resources. Resource utilization must be done
in a prescient manner in order to leave enough for tomorrow. The higher costs involved and the risks
imposed by unpredictable market dynamics will be justified on the long run, if the environmental and ethical
costs are taken into account.
References
http://timesofindia.indiatimes.com/city/goa/Goa-revokes-ban-on-mining/articleshow/45903724.cms
http://articles.economictimes.indiatimes.com/2014-10-28/news/55521355_1_mining-operations-machinery-
owners-mining-companies
Mihir Shah, “Cash transfers, the lazy shortcut”, The Hindu, 14th Jan, 2015
Manas Ranjan Senapati, “Fly ash from thermal power plants – waste management and overview”,
CURRENT SCIENCE, VOL. 100, NO. 12, 25 JUNE 2011
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408
Iron Ore Processing
409
Iron Ore Processing
Abstract:
Eastern Indian iron ore is generally known as high alumina iron ore. The sample was taken from Barsua,
Eastern India, for beneficiation studies. Representative samples were subjected to detailed investigation
by size analysis, chemical analysis, microscopic analysis, XRD and heating cycle, for determination of
liberation size of the sample, identification of major as well as minor ore and associated gangue minerals.
Chemical analysis showed that percentage (%) of Fe, Al2O3, SiO2 and LOI present in +16#/+1000 µm to -
300#/-52 µm fractions are 52.73 to 61.19%, 9.54 to 4.64, 6.42 to 2.80 and 8.70 to 4.78, respectively.
Investigations reveal that Barsua iron ore is composed of hematite, goethite and lesser association of
martite in association with major gangue minerals such as clay minerals (kaolinite), bauxitic minerals
(gibbsite) and crystalline quartz. Adequate liberation was obtained at a finer size (-150 µm). Based on the
liberation size and nature of the ore, beneficiation study using spiral concentrator followed by WHIMS
was carried out. In spiral concentrator experiment pulp density was varied from 10% to 40%. The Fe%
increased from 59% to 64%. Lower pulp density results in the better grade & recovery. WHIMS results
indicate Upgradation of approximately 66% of Fe from 59%. It may thus be concluded that the spiral-
concentrator and WHIMS can be employed (individually or in combination) for beneficiation of Barsua
iron ore.
Keywords: Iron ore, size analysis, chemical analysis, microscopic studies, XRD, heating cycle, spiral
concentrator, WHIMS.
1. Introduction
Important iron ore deposits occur in the eastern, central and southern parts of India in the states of
Jharkhand, Odisha, Karnataka, Chhattisgarh, Goa, etc. Indian iron ore is relatively rich in Fe and contains
higher amounts of alumina compared to the other major deposits of the world. Very low grade iron ore
cannot be used in metallurgical plants and needs to be upgraded to increase the iron content and reduce
gangue contents. Iron ore is beneficiated all around the world to meet the quality requirement of large
steel industries. Several technologies are available such as washing, jigging, magnetic separation,
enhanced gravity separation and floatation to enhance the quantity of the iron ore.
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Iron Ore Processing
Enrichment of low grade iron ores always involves comminution for mineral liberation and significant
amount of ultra-fines are generated during this process and these ultra-fines are difficult to concentrate.
Main difficulty in processing and utilization of low grade iron ores primarily stems from their
compositional characteristics as well as the separation of finer size ranges [3].
The fast depletion of rich iron ore and increasing demand of iron and steel have forced the attention of the
scientists and engineers towards the up gradation of low grade ores and fines.
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Iron Ore Processing
2.2 Size wise chemical analysis
Chemical analysis of the size fractions helps in studying the distribution pattern of different elements [5].
Percentage (%) of Fe, SiO2, Al2O3 and LOI obtained for size fraction +1000 µm to -52 µm was varied
from 52.73 to 61.19, 6.42 to 2.80, 9.54 to 4.64 and 8.70 to 4.78 respectively. The result of chemical
analysis is presented in Table 1.
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Iron Ore Processing
2.4 Microscopic analysis
Microscopic analysis deals with the geological aspects of the ore. It includes origin of the ore, the types of
ore formations present in the sample, etc. Data are obtained by studying a thin section of the sample or by
observing a hand specimen. Polished section study revealed that the received iron ore sample contains
hematite and goethite as the major minerals while quartz, gibbsite and kaolinite occurs as gangue
minerals. Quartz appears as minute grain of different sizes. Results are given in Fig. 3.
a c
b d
Figure 3: (a) & (b) Photomicrograph showing complex interlocking texture hematite and goethite along
with clay mineral assemblages, (c) photomicrograph showing Goethite encloses patches of Hematite with
typical colloform texture and concentric zoning, (d) photomicrograph showing fine grained disseminated
hematite grains within clay-rich ground mass.
The sample is heated at 110 0C; it gives the percentage of surface moisture.
The sample is heated at 400 0C; it gives the percentage of goethite and gibbsite.
The sample is heated at 950 0C; it gives the percentage of carbonate minerals.
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Iron Ore Processing
Table 2: Overall composition of Barsua iron ore by heating cycle.
Serial no: Name of the Ore Percentage available
1 Hematite 36.86
2 Goethite 39.56
3 Magnetite 1.60
4 Kaolinite 15.58
5 Gibbsite 5.17
6 Silica 0.83
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Iron Ore Processing
Table 3: Experimental results (spiral concentrator).
Sl Pulp Fe (%) Al2O3 SiO2 LOI Yield Recovery
no: Density (%) (%) (%) (%) (%)
(%)
s1 10 C 64.211 1.840 1.538 4.582 45.12 65.71
T 52.413 9.971 6.401 8.357
2 15 C 63.971 1.983 1.662 4.633 51.53 62.57
T 53.510 9.170 5.913 8.344
3 20 C 63.960 2.041 1.719 4.759 59.32 58.15
T 54.463 8.602 5.036 8.234
4 25 C 63.712 2.107 1.805 5.053 64.11 57.99
T 54. 743 7.911 4.394 8.027
5 30 C 63.289 2.411 1.911 5.244 68.25 54.83
T 55.675 7.739 4.317 7.946
6 35 C 62.831 2.724 2.023 5.444 69.68 54.14
T 56.208 7.586 4.119 7.902
7 40 C 62.552 3.001 2.132 5.489 72.22 52.66
T 56.646 7.488 3.989 7.662
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Iron Ore Processing
2.6.2 Beneficiation by WHIMS with steel wool matrix
Beneficiation using steel wool matrix. The result obtained are given in Table 4 and Fig. 5.
Increase in magnetic field intensity increased the yield while the grade decreased. Maximum yield was
obtained at higher intensity. Maximum grade of 64.28% Fe and maximum yield of 68.2% were obtained
at 0.4 T and 2.0 T magnetic intensity, respectively.
Wet high intensity magnetic separator experiments were carried out, varying the magnetic field
intensity over 5 levels (0.4, 0.8, 1.2, 1.6 and 2.0 Tesla), using steel wool matrix and ball matrix.
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Iron Ore Processing
Table 5: Experimental results (ball matrix).
Sl Magnetic Intensity Products Wt. % Yield, (%) Fe %
No. in (Tesla)
1 0.4 Magnetic 22.5 45.0 66.6
Non-magnetic 27.5 55.0 53.8
2 0.8 Magnetic 25.7 51.4 65.9
Non-magnetic 24.3 48.6 52.9
3 1.2 Magnetic 28.6 57.2 63.7
Non-magnetic 21.4 42.8 54.1
4 1.6 Magnetic 30.4 60.8 62.3
Non-magnetic 19.6 39.2 55.4
5 2.0 Magnetic 31.5 63.0 61.8
Non-magnetic 18.5 37.0 55.8
Size analysis of Barsua iron ore indicated that the d80= 1.9 mm and d50= 150 µm. Most of the
sample is distributed in -150+50 µm.
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Iron Ore Processing
As the size range decreases, percentage of Fe increases with decrease in Al2O3, SiO2 & LOI
percentage.
Characterization studies concluded that Barsua iron ore is goethite-rich. Distribution of ore
minerals and gangue minerals are very complex. As presence of goethite and alumina is high, it
will create problem in beneficiation. Liberation study determines liberation can be possible at a
finer fraction.
DTA/TGA and heating cycle determined the LOI and phase changes at different temperatures.
FTIR analysis concluded the presence of mineral phases based on different IR bands.
Davis tube magnetic separator determined around 3-5% of magnetic material present in the Barsua
iron ore.
Spiral concentrator and WHIMS were chosen based on the physical and mineralogical studies.
Spiral concentrator produced a concentrate with 64.21% Fe, recovery of 65.71% at 10% pulp
density.
WHIMS with steel wool matrix gave better results than with ball matrix.
Acknowledgements
The support extended during the test work by Shri Ganesh Gope and Shri S. N. Gope is gratefully
acknowledged. The author (satyananda patra) thanks Prof N. R. Mandre HOD, Dept. of Fuel & Mineral
Engineering for his encouragement and permission to present the work as a paper.
References:
[1] S. Roy, A. Das, and M. K. Mohanty, “Feasibility to producing pellet grade concentrate by
beneficiation of iron ore slimes in India”, Separation Science and Technology, vol. 42, pp. 3271- 3287,
2007.
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Iron Ore Processing
[2] S. Roy, and A. Das, “Characterization and processing of low grade iron ore slime from Jilling area of
India”, Mineral Processing and Extractive Metallurgy Review, vol. 29, pp. 213-231, 2008.
[3] S. Roy, A. Das, and A. S. Venkatesh, “A comparative mineralogical and geochemical characterisation
of iron ores from two Indian Precambrian deposits and Krivoy rog deposit, Ukraine: implications for the
upgrading of lean grade ore”, Applied Earth Science: IMM Transactions Section B, vol. 117 (23), pp.
125-147, 2008.
[4] Nirlipta. P. Nayak, “Mineralogical Constraints in Beneficiation of Low Grade Iron Ores of Barsua,
Eastern India”, International Journal of Engineering and Innovative Technology, Volume 3, Issue 5,
November 2013.
[6] B. Das, S. Prakash, S. K. Das and P. S. R. Reddy, “Effective Beneficiation of Low Grade Iron Ore
through Jigging Operation”, Journal of Minerals and Materials Characterisation and Engineering, Vol. 7,
No. 1, 2008, pp. 27- 37.
[7] Vinod Kumar, G.N. Jadhav1, N.K. Khosla2, U.S. Chattoraj, R. Singh R.P. Bhagat, B. Nayak, M.K.
Mohanta, K.K. Bhattacharyya and S.P. Mehrotra, “Characterization and its implication on Beneficiation
of low grade iron ore by Gravity separation”, ISBN: 81-87053-54-7, 2007, pp. 10-23.
[9] S. Roy and A. Das, “A Comparative Study on Characterisation and Processing of Iron Ore Slimes”,
“Proceedings of the International Seminar on Mineral Processing Technology – 2006”, Chennai, India.
pp. 476 - 484.
[10] Tekkalakote Umadevi, Amit Pratap Singh, Kumar Abhishek, Basavareddy Suresh, Rameshwar Sah,
“Recovery of Iron Bearing Minerals from Beneficiation Plant 2 Thickner Underflow of JSW Steel
Limited”, “Journal of Minerals and Materials Characterization and Engineering”, 2013, 1, 55-60.
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Iron Ore Processing
BENEFICIATION OF IRON ORE SLIMES USING A NATURAL POLYMER BY SELECTIVE
FLOCCULATION PROCESS
Rakesh Kumar* and N.R.Mandre
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad, India
*Corresponding author: rakeshraj2009@gmail.com
Abstract
Steel production is increasing gradually year after year leading to the increase in the requirement of iron
ore. As per the projection of National Steel policy, India has set a target of achieving a production
capacity of 110 million tons of steel by 2020 for which requires 190 million tons of iron ore. However,
high grade iron ore deposits are fast depleting and there is a need to address issues related to
beneficiation. Therefore, it is imperative to use low grade iron ores, fines and slimes in order to meet the
demand. In India, huge amount of slimes are generated during mining and processing of iron ores due to
soft and friable nature of the ore. The generated slimes are disposed into tailing pond as a waste.
However, the generated slimes contain substantial amount of iron value i.e. 48-62% Fe. It is essential to
recover the iron value from these slimes which will not only increase the recovery of the plant but also
would reduce the environmental related problems. Therefore, in the present study an attempt has been
made to study the possibility of upgrading the iron ore slimes by employing selective flocculation.
Selective flocculation is a physicochemical process which could process the slimes effectively. For this
purpose iron ore slimes were collected from tailing pond of Kiriburu processing plant. The chemical
analyses indicated that the sample contains 58.24% Fe, 4.72% SiO2, 3.47% Al2O3 and 5.18% LOI. The
beneficiation studies were carried out by employing selective flocculation process using guar gum, a
natural polymer as a flocculant. During the studies, various parameters such as pH, pulp density, and
flocculant dosage etc., have been investigated. From the studies, it was possible to obtain a maximum
63.2% Fe with a recovery of 68.04%. Further, the results obtained from the studies were also subjected
for statistical analysis by using factorial design.
Keywords: Iron ore slimes, beneficiation, guar gum, selective flocculation.
1. Introduction
In India, huge amount of iron ore slimes are generated during mining and processing operations. The
generation of slimes is projected to be 10-25% by weight of the total ore mined. The generated slimes are
having a diameter of less than 150 µm not regarded to be useful. Hence, these materials are discarded as
waste and disposed into tailing pond without any prior treatment. However, these generated slimes
contain a substantial amount of iron value. Kiriburu mine of M/s SAIL alone has 30 million tonnes of
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Iron Ore Processing
slimes accumulated at tailing ponds with almost 30 years of operation (Srivastava et al., 2001). Therefore,
utilization of iron ore slimes has become necessary for conservation of ore minerals. Due to stringent
environmental regulation act imposed by the statutory body in disposing the tailings, many iron ore
industries are seriously exploring the possibility to recover the valuable mineral from these slimes. These
activities are not only to recover minerals, but also to address various environmental issues associated
with slimes treatment. In this regard, by applying a suitable beneficiation technique to recover iron values
from these slimes, it can be used as an end user product. Thus, iron ore slime which is considered as a
hazardous waste, can be a potential resource for future.
From the literature, it may be observed that many conventional methods such as gravity separation,
flotation and magnetic separation, etc. have been employed for the treatment of iron ore slimes. In a
typical study carried out by Srivastava et al. (2001) on Kiriburu slimes using hydrocyclone followed by
spiral concentration showed that it was possible to achieve 64.17% Fe at a yield of 37.3% with
simultaneous decrease in alumina content to 1.17%. The flotation of Joda iron ore slimes carried out by
Rao et al. (2011) indicated that it was possible to achieve 58.89% Fe, 4.62% SiO2, and 5.28% Al2O3 from
a feed grade of 54.4% Fe, 6.21% SiO2 and 6.80% Al2O3. A similar study carried out by Kumar et al.
(2013) on iron ore slimes using column flotation showed that it was possible to upgrade 58.54% Fe,
5.29% SiO2 and 4.77% Al2O3 with a recovery of 86.90% from feed grade of 58% Fe, 6.72% SiO2 and
5.7% Al2O3. Prasad et al. (1988) studied the beneficiation of Kiriburu iron ore slimes using wet high
magnetic separation followed by hydrocyclone. They showed that a concentrate grade of 63% Fe and
3.3% alumina could be produced with an overall recovery of 56%. However, these methods are found to
be ineffective in improving the grade of the slimes.
From the earlier studies, it may be seen that selective flocculation is one of the promising technique for
treating slimes. Selective flocculation is a physicochemical process in which polymeric flocculants are
used to form flocs of desired minerals and separation of such aggregates from other minerals in dispersed
phase. Many researchers have been using different types of polymeric flocculants such polyacrylamide
(PAM), starches, polyacrylic acid (PAA) for selective flocculation studies (Weissenborn et al., 1994;
Pradip et al., 1993; Mandre, 2012; Kumar and Mandre, 2015). Mathur et al. (2000) has carried out a
comprehensive review on selective flocculation for better understanding of the selectivity of the mixed
mineral system and suggested that the selective flocculation technique is useful in treating fines/slimes in
industrial applications.
Therefore, it is in this context an attempt has been made to study the beneficiation of iron ore slimes by
selective flocculation using guar gum as a flocculant and also to understand the effect of different process
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Iron Ore Processing
parameters on the performance of the process. The performance of the process was analysed by
employing statistical method.
2.2 Reagents
Guar gum was obtained from Saiguru food and gum industries, Mumbai. It was used as a flocculant in
this study. Sodiumhexameta phosphate was used as dispersant, procured from Merck, India. Sodium
hydroxide and hydrochloric acid used as pH modifiers in this study were of analytical grade.
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Iron Ore Processing
and every factor at a time by classical approach. Thus, Factorial design of experiment is employed to
minimise the total number of experiments and achieve best overall optimization of the process. The
important parameters and their corresponding levels selected for this study are shown in table 1.
Table 1: Experimental ranges and levels of the factors used in the factorial design.
Variables Coded symbol Level and Range
-1 1
pH A 8 10
Pulp Density B 1 5
Flocculant dose (mg/g) C 0.03 0.27
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Iron Ore Processing
Further, a series of experimental runs have been performed as per full factorial design to study the
flocculation behaviour of iron slimes with guar gum. A factorial design was used to determine the grade
of concentrate with three variables i.e. pH, pulp density and flocculant dosage. Design matrix was
calculated in actual levels of the variables as given in table 3. The results obtained of the factorial design
of experiments were analysed through Standard Analysis of Variance (ANOVA) methods with respect to
grade as a response. ANOVA for grade of concentrate is shown in table 4. Grade of concentrate is
significantly affected by the variables and interactions. From the table 4, it may be seen that grade of
concentrate is more sensitive to flocculant dose as compared to pH of the pulp and pulp density. This
study also indicated that the order of significant terms that affect the grade of concentrate was found to be
flocculant dose>pH>pulp density×flocculant dose>pulp density. Thus, resultant mathematical model for
grade of the concentrate can be represented as,
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Iron Ore Processing
%Grade = 59.6588+0.5387A-0.2487B+0.7187C+0.2687BC (1)
The goodness of fit of the resultant model for grade was also analysed by ANOVA. The R2 value of the
model obtained is 99.85% for grade. From the table 3, it is observed that the experimental values of the
grade are well in agreement with the predicted values.
4. Conclusions
XRD study revealed that the presence of hematite and goethite as major iron bearing minerals and
quartz and kaolinite as gangue minerals in the sample. It was possible to increase the grade of iron from
58.24% to 63.2% Fe with a recovery of 68.04% after washing of flocs with pulp density 1%, pH 10 and
flocculant dosage of 0.21 mg/g. The statistical deign reveals that pH, pulp density, flocculant dosage and
second order interaction pulp density×flocculant dose are found to be significant.
References
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Iron Ore Processing
Rakesh Kumar and N.R.Mandre. Development of statistical model for selective flocculationof iron ore
slimes. Journal of dispersion science and Technology. 37(2), 2016. doi:10.1080/01932691.2015.1039024.
Rakesh kumar and N.R.Mandre. Characterization and Beneficiation of iron ore tailings by selective
flocculation. Trans. Indian Inst. Met. 2015 (Accepted).
T.V.V. Kumar, D.S. Rao, S.S. Rao, S. Prabhakar, G.B. Raju, Column flotation studies on low grade iron
ore slimes of an operating plant in India, J. Min. Metall. Sect. A 49 (1) : 57–66, 2013.
N.R. Mandre, and D. Panigrahi. Studies on selective flocculation of complex sulphides using cellulose
xanthate. Int. J. Miner. Process. 50: 117-186, 1997.
N.R. Mandre. Selective flocculation of low grade iron ore fines. In New Delhi, 24-28 September, XXVI
International Mineral Processing Congress, 3220-3226, 2012.
S. Mathur, P. Singh, & B.M. Moudgil. Advances in selective flocculation technology for solid solid
separations, Int. J. Miner. Process. 58: 201-222, 2000.
P.K. Naik, L.B. Sukla, S.C. Das. Application of statistical design in the leaching study of low grade
manganese ore using aqueous sulfur dioxide. Separation Science and Technology. 37 (6) : 1375, 2002b.
P.K. Naik, L.B. Sukla, S.C. Das. Extraction of manganese from low grade nishikhal ore using pyritiferous
lignite in acidic medium, Minerals and Metallurgical Processing, 19 (2) :110, 2002c.
B.K. Pandey, T. Sharma. Reducing agents and double layered iron ore pellets. Int. J. Miner. Process. 59 :
295-304, 2000.
Pradip. Beneficiation of Alumina-Rich Indian Iron Ore Slimes. Metals, Materials & Processes. 6(3): 170-
194, 1994.
N. Prasad, M.A. Ponomarev, S.K. Mukherjee, P.K. Sengupta, P.K. Roy, S.K. Gupta. Introduction of new
technologies for beneficiation of Indian hematite ores, reduction of losses and increase in their quality. In:
Forssberg, E. Ed., XVI International Mineral Processing Congress, pp. 1369–1380, 1988.
D.S. Rao, T.V.V. Kumar, S.S. Rao, S. Prabhakar, G.B. Raju. Effectiveness of sodium silicate as gangue
depressants in iron ore slimes flotation. Int. J. Miner. Metall. Mater. 18 (5) : 515–522, 2011.
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Iron Ore Processing
S.A. Ravishankar, Pradip, N.K. Khosla. Selective flocculation of iron oxides from its synthetic mixtures
with clays: A comparison of polyacrylic acid and starch polymers. Int. J. Miner. Process., 43 (3-4) : 235,
1995.
M.P. Srivastava, S.K. Pan, N. Prasad, B.K. Mishra. Characterization and processing of iron ore fines of
Kiriburu deposit of India. Int. J. Miner. Process., 61: 93–107, 2001.
P.K. Weissenborn, L.J. Warren, & J.G. Dunn. Optimisation of selective flocculation of ultrafine iron ore.
Int. J. Miner. Process., 42: 191-213,1994.
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BENEFICIATION OF LOW –GRADE IRON ORE FINES BY USING SELECTIVE
FLOCCULATION
Kichakeswari Tudu* and N.R.Mandre
1
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad-826004, India
*Corresponding author: tudukichakeswari10@gmail.com
Abstract
In the present paper, an attempt has been made to study selective flocculation of low-grade iron ore using
starch. The starch molecules shows good selectivity for hematite particles at a pH range of 10. For the study,
low- grade iron ore containing 56.23% Fe2O3, 5.45% Al2O3 & 4.22% % SiO2 was used. From the selective
flocculation process, it was possible to obtain 56.23% Fe to 64.92 with 96% recovery employing starch
flocculants.
1. Introduction
Increase in mining and mineral processing activities has led to explore the possibilities of beneficiation of
low-grade and complex ores. Presently more emphasis has been given to recover mineral values from low
grade ores and tailing with special reference to iron ore. From the investigations reported in the literature, it
may be seen that different methods such as gravity concentration, magnetic separation, froth flotation etc.,
have been tried for beneficiation of low-grade ores and tailings (Dworzanowski 2012). However, there
processes suffer from inherent disadvantages such as enhanced slime content, decreased response to
magnetic separation and reduced floatability due to slime coating (Mandre 2012).
Therefore, it has become imperative to explore the possibility of developing an alternate beneficiation
technique for the treatment of low- grade iron ores. Among the various techniques reported, selective
flocculation process has found to be more promising in recent years (Panda et al., 2013).
From a critical literature survey, it may be seen that wide range of flocculants such as starch, CMC, PAM,
PAA, guar gum etc. have been employed for the selective flocculation process (Ahemed and Mahran, 2012).
Hence, in present study, an attempt has been made to investigate selective flocculation of low-grade iron ore
by employing starch as a flocculant.
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Iron Ore Processing
2. Materials and methods
The low- grade iron ore used in this study was collected from the Gua mines, Paschimi Singhbhum district of
Jharkhand, India. The representative samples obtained were subjected for chemical analysis, which indicated
56.23% total Fe, 5.45% silica and 4.22% alumina. Further, the representative samples were subjected to for
crushing and grinding to produce 80% passing of -75 μm size fractions, which were used for selective
flocculation process.
2.1. Flocculant
During the selective flocculation studies, starch (analytical grade make Switzerland) has been used as the
flocculant.
The flocculation tests were carried out in a 1000 ml, graduated cylinder and during the studies, desired
amount of mineral was mixed with 950 ml of water. The required solid concentration was maintained for all
experiments. The slurry was thoroughly mixed by perforated plunger for 2-3 minutes and pH of the slurry
adjusted by using dilute HCl and NaOH. Then the slurry thoroughly agitated by inverting the cylinder 10-12
times. After mixing of particles, the cylinder allowed to stand undisturbed and the particles are allowed to
settle for definite times. Further, 75% of the slimes was siphoned out after noting the mud line height. Both
the flocculated and non-flocculated fractions were collected separately and subjected to chemical analysis.
3. Characterization studies
Microscopic studies were carried out using oil reflected light microscope of Leica make interfaced with
QWIN image analysis software. From the microscopic analysis, it was observed that the sample contain
different mineral such as micro-platy hematite, martite goethite, magnetite, quartz and clay (Fig. 1).
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Iron Ore Processing
Figure 1: Microscopic study of iron ore sample by using oil reflectance microscope which indicate M-
martite, G-goethite, Cl-clay mineral.
Prior to the selective flocculation tests, initially some tests were carried out at 6-10% solids by weight to
know the settling characteristics and the effect of pH on the settling rate.
For this purpose, an experimental method described by Thamlage and Fitch (1955) were used and the results
of the tests are shown in Fig. 2. From the results, it may be seen that increase in pH increases the settling rate
and a maximum settling rate of 0.2 cm/sec has been obtained at pH 10. Therefore, in all flocculation tests, a
constant pH 10 was maintained in all further tests.
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Iron Ore Processing
4.2 Grade and recovery
After completion of above tests, the sample was subjected for selective flocculation process. The results of
tests are given in Fig. 3. From Fig. 3, it may be seen that the grade of iron increases with increase in
concentration of the flocculant. However, increased concentration beyond 0.020 mg/g, the grade was found
to remain constant.
From the studies, it was possible to obtain 64.74% Fe grade with recovery 95% recovery using starch as
flocculant.
Figure 3: Recovery and grade of iron as a function of concentration 0.02 mg/g for 1% starch flocculant.
Further, investigations were extended to study the effect of washing, in presence of a dispersing agent
(Na2SiO3). For this purpose, the experiments were carried out using variable concentration of the dispersant
and four stages of cleaning. The results of the studies are given in Fig. 4. From Fig. 4, it may be seen that a
maximum grade of Fe (64.92%) can be obtain using starch after three stages of washing. This phenomena
may be attributed to breaking of flocs with enhanced number of washings.
The above investigations were further supported by carrying out XRD analysis, which is given below.
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Iron Ore Processing
From the analysis of XRD result shows that the iron bearing minerals are mainly hematite, martite, goethite
and magnetite while the main gangue minerals in the sample are quartz and kaolinite (Fig. 5). Two prominent
mineral peaks of aluminium oxide and hematite are observed in three samples. It is also observed that the
different pattern of starch and feed sample (without flocculant) are identical. The intensity of diffraction
peaks of hematite in starch is found to be increased as compared to feed sample.
Figure 5: XRD analysis for starch flocculant and Feed that indicate G-goethite, K-kainite, H-hematite, M-
magnetite Q-quartz and A-allay of iron ore sample.
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Iron Ore Processing
5. Conclusions
(A) Microscopic studies carried out indicate the presence of principal minerals such as martite, hematite and
goethite along with magnetite in traces and gangue minerals quartz and clay. (B) Studies carried out on
settling rate of the particles show an increase in settling rate with increase in pH irrespective of the variation
of solid content. (C) Experiments performed to know the effect of flocculant dosages indicated that best
results could be obtained for 0.02 mg/g of starch flocculant for a pulp with 6% solid content. (D) The effect
of cleaning of flocs as well as the addition of a dispersant improves the selective flocculation. A maximum
improvement of grade 56.23 to 64.92 by using starch flocculant with the addition of 0.02 mg/g of dosages
with recovery 95% and 95% were achieved after three stages of cleaning.
Acknowledgements
Thanks are due to SAIL, for providing necessary low grade iron ore samples. Thanks are also due to CRF,
ISM, NML and Tata steel for extending the support to carry out analytical work.
References
Ahmed, Hussin A. M., and Mahran, Gamal M.A., 2013, “Processing of iron ore fines from Alswaween
kingdom of Saudiarabia”, Physicochem. Probl. Miner. Process, 49(2), 419-430.
Dworzanowski, M., 2012 “Maximizing the recovery of fine iron ore using magnetic separation”, The Journal
of Southern African Institute of Mining and Metallurgy, 112(3), 197-202.
Mandre, N.R., 2012, “Selective flocculation of low-grade iron ore fines”, XXVI International Mineral
Processing congress, New Delhi, No.0681, 3220-3226.
Panda , Lopamudra., Banerjee, pradip K., Biswal, Surendra Kumar., Venugopal, R., and Mandre, N.R.,
2013, “ Performance evaluation for Selectivity of the flocculant on hematite in selective flocculation”, In. J.
Minerals, Metallurgy and Materials.,20,No.12, 1123-1128.
Thalmage, W.P., Fitch, E.B., 1955 “Determining thickener unit areas”, Ind.Eng.Chem, 47, 38-41.
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Iron Ore Processing
OPTIMIZATION OF PELLETIZATION PROCESS FOR IRON ORE WITH
HIGH ALUMINA BY USE OF HIGH SILICA FLUXES
D. kadhe*, A. Kumar, T. Umadevi, M. Kaza, R. Sah, K. Sampath
JSW Steel Limited, Toranagallu, Karnataka, India
*Corresponding author: dhraj.kadhe@jsw.in
Abstract:
Depletion of high grade iron ores with low alumina and silica content has forced the steel industry to
utilize low grade iron ores with high gangue content. The low grade ores available in Sandur-Hospet
region has either high alumina with low silica or high silica with low alumina. At JSW the low grade iron
ore is beneficiated for use in pellet making.
This paper presents the methods adopted to optimize the process parameters to facilitate the use of high
alumina low silica concentrates in pellet making. A high alumina/silica ratio greater than 1.2-1.9 in pellet
feed adversely affects the firing temperatures, slag melt distribution and hence the physical strength of the
fired pellets. As alumina is a refractory material requires higher temperature for melting and formation of
slag melt, the firing temperatures rise to 1350 deg C which is detrimental to the induration furnace and is
also energy intensive. At normal operating temperature of 1300 deg C, the metallurgical and physical
properties of the pellets deteriorate due to the insufficient fusion and bonding of the silicate melt to the
recrystallized hematite grains. Lower volume of silicate melts results in low wetting, low diffusion and
grain growth.
Extensive laboratory studies have been conducted to optimize the process parameters including the pellet
mix composition. Management of Al2O3/SiO2 ratio below 1 is achieved by using high silica fluxes (lime
stone and Quartz) while maintaining the basicity at desired values for over all slag volume control.
Characterization of fired pellet revealed that the silicate slag was fused and bonded with hematite grains
and homogeneous distribution of slag results in improved strength at given predicted firing temperature.
A blend composition and firing temperature matrix has been developed and established at the pellet plants
of JSW.
Keywords: Pelletization, high alumina iron ore, slag melt, characterization, limestone, quartz.
1. Introduction
The quality of the pellet is affected by the type of the raw chemical composition, raw material mix
proportion, gangue content, and flux proportion and their subsequent treatment to produce pellets. These
factors results in variation in the physicochemical properties of coexisting phases, structure, distribution
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Iron Ore Processing
of phases, and porosity in the pellets. It is generally accepted that the properties of pellets are closely
related to mineral constituents, distribution of liquid slag and porosity during firing of pellets [3].
The properties of the pellets are also largely governed by the type and degree of bonding achieved
between ore particles and also by the stability of these bonding phases’. The stability and wet ability of
liquid slag formed during firing of pellets is largely governed by alumina and silica content in raw
material and in turns its ratio [1].
001
600.0
500.0
400.0
Counts
300.0 Al
Si
200.0
Fe Fe
Fe Fe
100.0 FeKesc
0.0
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
keV
Figure 1: Electron probe micro analysis of iron ore concentrate from Hospet -Sandur region.
During induration of pellets at 1250 0C to 13200C, two types of bonds are formed. They are (i) Crystal
bonding (oxide bonding) (ii) Slag/glassy bonding
However, pellets with higher alumina and lower silica exhibits crystal bonding during firing which results
in poorer metallurgical properties of pellets [7].
Melt formation in pellets starts with solid state reactions of lime and silica at contact points to form an
ortho-silicate phase, and of lime with the hematite to form simple calcium ferrites (CaO.Fe2O3 and
2CaO.Fe2O3). With increase in temperature above 12500C, silica, hematite and lime are dissolved from
the surrounding particles. In alumina rich areas, and at temperatures 13000C, SFCA is formed which
precipitates as solid phases. The remainder of the melt solidifies as a ferrous calcium silicate glass (slag)
with the excess iron oxide migrating to nearby hematite particle. So basicity, amount of slag and and slag
composition plays vital role in deciding the pellet strength [6].
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Iron Ore Processing
to remove during beneficiation and hence at last the iron ore concentrate end up with higher alumina and
lower silica content (Al2O3/SiO2 is in range of 1.3-1.6).
Figure 2(a) shows that the compressive strength of the pellets is largely reduced with increase in alumina
silica ratio in pellets. The reasons may be obvious that the slag melts which formed during firing is highly
viscous and the volume of melts phase is drastically reduced due to insufficient firing temperature leads
to increase reduced tumbler and abrasion index of the pellet. Figure 2(b) showed that pellets with high
Al2O3/SiO2 ratio exhibited high degradation during reduction. Alumina was reported to increase the
viscosity of the primary melt formed during sintering of iron ore. The alumina is very effective in
increasing the viscosity of calcium ferrite slag particularly at temperatures below 1200°C, increase in
alumina in iron ore sinter increases the pore area and the pore shape becomes more irregular.
Figure 2a: Influence of alumina silica ratio Figure 2b: Influence of alumina silica ratio
on physical property of pellets. on degradation and porosity.
Alumina, being dissolved in the melt phase, reduces its strength by increasing its brittleness. M. Valdez et
al. stated that alumina diffuses in to the hematite crystal during sintering process to form solid solution.
During low temperature reduction, hematite, diffused with alumina, generates magnetite phase with
distorted structure causing crack generation and propagation leading to increased disintegration [4].
Figure 3: Optical micrograph of pellets with Al2O3/SiO2 of 1.3 and 1.15 at basicity of 0.31.
The optical micrograph reveals that with higher alumina and silica ratio in pellets fired at temperature of
1280-12900C exhibits lower CCS as shown in Figure 3. The large hematite particles were bonded with
small hematite particles. Here small hematite crystals forms the main bonding phase. Pellets associated
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Iron Ore Processing
with large number of pores and these pores were internally connected with each other and form the open
texture. The presence of minor quantity of free silica was observed in the pellets [6].
However, firing at 1310-13200C with Al2O3/SiO2 of 1.15 showing marginally improvement in strength of
pellet. The reason is due to the fact that the more crystal bonding and lower slag bonding at lower
basicity. The distribution of slag phase and pores volume are shown in Table 1.
2.1 Influence of basicity on properties of pellets with higher alumina silica ratio
In order to attain better pellet property, it is necessary to keep the basicity of pellet at optimum level.
From Figure 4, it is investigated that at optimum basicity, the volume of silicate glassy slag phase is
around 10-15% and with pellet porosity of 32-35%. At basicity of range of 0.4-0.5 it is found that the
silicate phase distribution throughout the pellet is homogeneous and the silicate phases cover the
recrystallized grains of hematite which in results provides good strength to the pellet with optimum
porosity shown in Figure 5.
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Iron Ore Processing
At high temperature around 1300°C, the small fraction of hematite grains fuse together to form bridge
type binder between hematite particles.
With increase in alumina silica ratio, the melting point of slag will move to alumina sides and hence the
slag will not fuse to the hematite grain. However, the fusion/melting point of slag will further bring down
by addition of limestone and lowering the alumina silica ratio.
Figure 6 shows that if alumina/silica ratio is more than 1, then the ternary point will shifted to higher
temperature range and pellets need to fire at 1330o C-1340o C. However, lowering the ratio less than 1
indicates the firing temperature of 1300-1310oC will be sufficient to fuse the slag and getting good
strength.
3. Experimental plan
Pelletization studies have been carried out using high silica lime stone and quartz fines to achieve the
desired alumina silica ratio. The proportions were made as below.
1. Mix proportion made with varying basicity from 0.4 to 0.8.
2. Mix proportion made keeping basicity constant and quartz added to vary alumina silica ratio of
fired pellet.
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Iron Ore Processing
3. The firing temperature is estimate using slag ternary system with respect to alumina silica ratio in
all the mix proportion.
The raw materials used for the preparation of the green pellets are iron ore, limestone, bentonite coke
breeze and quartz. The chemical analysis of the raw material is shown in Table 1. Iron ore fines, limestone
and quartz of -10 mm size were ground separately in laboratory ball mill.
Fluxes like limestone and quartz are put in grinding mill together to get the desired particle size of the
fluxes for pelletization. Limestone and quartz having close bond work index which makes them to get
grind at same power and revolution of ball mill. The bond work indexes of limestone and quartz are 11.9
Kwh/st and 12.5 Kwh/st respectively. The details of blend proportion used for pelletization using high
silica limestone are shown in Table 2.
The raw material analysis and particle size are shown in Table 3 and Table 4, respectively.
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Iron Ore Processing
Green pellet mix was prepared by mixing the iron ore fines, limestone, bentonite and quartz green pellets
were prepared using laboratory scale balling disc.
Each set of experiment comprises firing of 20 kg green pellets. The green pellets were subjected to firing
in Raising Hearth Furnace (RHF) to study the physical and metallurgical properties. The heating rate was
maintained @10oC/min and the firing temperature was kept as per experimental plan. The total induration
cycle for the pellets was 50 min.
The chemical analysis and green ball properties of the fired pellets are shown in Table 6. The firing
conditions during the laboratory experiments have been maintained the same. Pellets were subjected to
various tests under different conditions to study the physical and metallurgical properties. To understand
the effect of firing temperature, basicity and alumina silica ratio on phase formation, micro-structural
investigation has been carried out.
4.1 Influence of firing temperature and basicity on CCS of pellets at different Al2O3/SiO2
Addition of high silica limestone from 2% to 5.1% to the mix achieves basicity of 0.4 to 0.8. The alumina
silica ratio in pellets gets reduced to 1-1.3 from 1.6. Based on the ratio, the pellets are fired at different
temperature to achieve the required quantity of silicate slag. The effect of firing temperature on pellet
strength with different basicity and at constant basicity are shown in Figure 8a and Figure 8b,
respectively.
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Iron Ore Processing
.
Figure 8a: Effect of firing temperature on pellet Figure 8b: Effect of firing temperature on
properties at basicity 0.4-0.8. strength at basicity 0.4.
Figure 8a reveals that the pellets with ratio of 1 at basicity 0.8 required lesser firing temperature then
pellets with basicity 0.4 and 0.6. However, the strength of pellet is lower at basicity of 0.8. The reason is
that more amount of slag phase is formed. Strength attained more due to slag phase and crystal bonding is
less dominant. However, addition of high silica limestone alone is not sufficient to bring down the
alumina silica ratio less than 1 and so it required higher firing temperature of 13400C to get the desired
strength. Figure 8b indicates that the pellets are fired with constant basicity of 0.4. Quartz is purposefully
added to bring down the ratio close to or less than 1. Addition of quartz along with high silica limestone
results in lowering the ratio and hence required lesser firing temperature. The strength of pellet is superior
then pellets made with basicity of 0.8.
4.2 Influence of Al2O3/SiO2 ratio on reduction degradation index (RDI) and porosity
As showed in Figure 2a higher silica to alumina ratio results in higher porosity and increase reduction
degradation index.
The reduction degration degradation index of pellets with higher silica- alumina ratio (RDI-10.23/AI-3.6)
at bascity of 0.8 which further improved as basicity lower down to 0.4 (RDI-9.7/AI-3.1). Pellets at
basicity of 0.4 and at lower ratio of alumina and silica shows lower RDI compared to pellets with basicity
0.8. Pellets with basicity 0.4 consist of high silicate glassy binder and pellets with basicity 0.8 consist of
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Iron Ore Processing
high calcium glassy phase [4]. During reduction process at lower temperature 800 to 1000°C the silicate
slag in the form of plastic state reduce the stress and at above 1000°C the metallic frame provides the
strength to the pellet. These pellets do not disintegrate on heat treatment during reduction and retains the
shape until the metal separated from the slag.
Figure 10: Microstructure of pellets with varying basicity and at different alumina silica ratio.
However, with addition of quartz along with high silica limestone lowers the alumina silica ratio. At
constant basicity of 0.4 reveals that quartz easily combines with the silicate slag and become liquid at
given firing temperature. This results in uniform and homogeneous distribution of silicate slag throughout
the pellets. The pores are uniformly distributed leading to attain the better strength as shown in Figure 10.
4.4 Electron probe micro analysis (EPMA) of pellets with different alumina silica ratio
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Iron Ore Processing
Pellets with higher alumina by silica ration contain slag saturated with alumina which in turns increases
the melting and fusing temperature of the slag and lowering the total slag volume. Similarly higher
viscosity of slag tends to increase the viscosity of the slag and hence reduces the strength. The
temperature predicted for the pellets is also higher around 1340oC as shown in Figure 11a.
5. Conclusions
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Iron Ore Processing
The compressive strength and other high temperature properties of pellets largely depend on the type of
bonding and increase in the order of hematite, ferrite and silicate. The firing temperature during pellet
induration is as high as 1300°C-1320°C, so that a significant amount of liquid slag forms in the pellets.
After cooling, the slag/melt phase solidifies and acts as important bonding phase in the finished pellets. In
this study, pellets of different alumina to silica ratio and at different basicity values were tested for their
mechanical and metallurgical properties. Amount and distribution of different phases were determined
using quantitative image analysis and SEM-EDS. An attempt was made to correlate the pellet properties
with alumina to silica ratio with the addition of high silica limestone and quartz. The following
conclusions can be drawn from the present work:
Pellets’ physical and high temperature properties deteriorated at higher alumina to silica ratio
(Al2O3/SiO2>1). At higher ratio, the silicate slag is saturated with alumina which in turn required
higher temperature to melt and fuse.
As per ternary slag system, with increase in Al2O3/SiO2 ratio firing temperature will increase.
Addition of high silica limestone to maintain the basicity from 0.4 to 0.8 help in reducing the
firing temperature of pellets.
Addition of local limestone with 13% silica will not be sufficient to maintain Al2O3/SiO2<1. So,
purposefully quartz is added from 0.5-1.3% to bring down the ratio.
The superior quality of pellet with CCS from 276-278 kg/pellets is obtained at basicity of 0.4 with
Al2O3/SiO2 of 1-0.8 fired at temperature of 1290-13150C.
RDI, AI and porosity of pellets are improved with reduction in alumina to silica ratio in pellets
and it is find optimum at basicity of 0.4.
It is confirmed from optical micrographs that externally added quartz is fully taking part in slag
and readily make slag fluid helping in improving pellet strength.
References
1. A. R. Firth and J. R. Manuel: ISIJ Int., 2005, 45, (11), 1561–1566.
2. M. Valdez, K. Prapakorn, A.W. Cramb, and S. Sridhar “Dissolution of alumina particles in CaO–
Al2O3–SiO2–MgO slags” Ironmaking Steelmaking, 29 (2002), No. 1, 87
3. P. P. Kumar, S. C. Barman, B. M. Reddy and V. R. Sekhar: Ironmaking Steelmaking, 36 (2009),
No. 2, 87
4. Srinivas Dwarapudi and Madhu Ranjan “Influence of Oxide and Silicate Melt Phases on the RDI
of Iron Ore Pellets Suitable for Shaft Furnace of Direct Reduction Process” ISIJ International,
Vol. 50 (2010), No. 11, pp. 1581–1589
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Iron Ore Processing
5. T. Umadevi, and S s gupta“Effect of Microstructure on Iron Ore Pellet Strength” Proceedings of
“Int. Conf. on Emerging Trends in Mineral Processing and Extractive Metallurgy”, Bhubaneswar,
India,June 2005, pp 35 – 41
6. T. Umadevi, Prasanna kumar, Naveen F. lobo, M. Prabhu, P.C. Mahapatra and Madhu
Ranjan“Influence of Pellet Basicity on Pellet Properties and microstructure” ISIJ
International, Vol. 51 (2011), No. 1, pp. 14–20
7. J. F. Wilhemy and M. E. Boucher: ISIJ Tech. Conf. Proc., 2003, 81–89
446
Iron Ore Processing
Abstract
Binders are widely used in agglomeration operations such as briquetting and pelletization to assure that the
agglomerate possesses desired properties with regard to subsequent handling, transportation and processing.
These properties depend on the requirements of a particular operation and installation. Cold bonded
pelletization processes, in general, involve use of portland cement as binder or mixtures such as lime–silica,
slag–silica, lime–carbon dioxide etc. Cold bonded pelletization processes developed for utilization of iron ore
fines require about 8% or more cement as a binders. In the prasent paper an attempt has been made to study
the behavior of cold bonded pellets from goethitic iron ore fines. For this purpose, low-grade iron ore
containing 60.71% Fe, 4.79% SiO2 6.51 % Al2O3 was used. The samples were subjected for comminution to
produces -0.44mm size fraction with 5-10 % cement as a binder. From the studies it was observed that the
pellets posses crushing strength of around 80–100 Kg/pellet which were prepared by using around 8%
Portland cement followed by curing under normal humid condition for about 20 days. Drop strength and
shatter index values of composite pellets were also measured. From the studies, it was observed a maximum
of 63 % reduction at temperature ranging from 800 to 950 0C.
1. Introduction
Genrally, magnetite ore is preferred over other iron mineral for pelletization, however now a days due to
generation of huge amount of fines, it has become essential to use Hematitic and Goethitic iron ore fines for
pelletization. Goethitic iron ore is not directly used for the extraction of iron, as it is present in hydroxide
form and possesses high LOI.
Cold bonded ore-coal composite pellets have been successfully used in some of the emerging processes
which produce sponge iron using rotary hearth furnace (Inmetco, Pelletech, Fastment, Drylron, etc.). In these
processes, pellets are placed on the hearth of the furnace with minimum of tumbling, as though these are
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Iron Ore Processing
'flowers.' Pellets are consequently placed either in single layer or in two to three layers. Therefore, several
researchers have studied on the cold bonded pellets using different reducing agent under variable operating
conditions. Ladin et. al. have carried out the reduction of cold-bonded pellets produced from the solid
wastes of Eregli Integrated Iron and Steel Works (ERDEMIR), using different reducing agents. They have
found that the activation energy of the reduction was found to be 48.5 kJ/mol. Dipak et. al. have studied on
cold bonded pelletization processes for utilization of iron ore fines and slimes require about 10% or more
cementitious binders. The physico-metallurgical properties of the cured pellets indicate potentiality for use as
burden material in low/ moderate shaft furnaces. Agrawal et. al. have, work on pelletize iron ore fines after
mixing with up to 10% non-coking coal, and utilize these composite pellets in coal based rotary kiln DR
plants. Zhu De-Qing et. al. have studies the direct reduction cold-bound pellets from iron ore concentrate
with coal-based rotary kiln, possesses. They investigated that the strength of cold bound pellets can fully
meet the requirements for a commercial rotary kiln. Therefore, it is in this direction an attempt has been
made to study the cold bonded pelletization of low grade goethitic iron ore fines obtained from West
Singhbhum belt, Jharkhand, India.
2. Experimental work
Goethitic iron ore fines were collected from Gua mines, Jharkhand. After sampling and sizing, iron ore was
ground to proper size for pelletization. Iron ore fines (-0.44mm size) and Portland cement were used for
preparing the cold bonded pellets. Chemical analysis of iron ore is show in Table.1. Coal was used as a
reducing agent in the reduction process. The proximate and ultimate analysis of coal results are shown in
Table 2. From the results, it is seen that the coal is low volatile coking coal it can be used as a reduction
process of cold bonded pellets. Mineralogical studies of iron ore fines by optical microscope were also
carried out. The observations are as follows:
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Iron Ore Processing
Table 2. Proximate and Ultimate analysis of coal
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Iron Ore Processing
strength of 60 kg/pellet which enhances to 80–110 kg/pellet on prolonging the normal curing to 20 days or
subjecting to heat/steam treatment for a few hours.
The reduction kinetics of pellets was carried out using non coking coal as the reducing agent. The results
obtained are discussed in following sections. The reduction behavior of cold bonded pellets (8–12 mm size)
with non coking coal was studied at four different temperatures (800, 850, 900, and 950 0C) at different time
interval (10, 20, 30, 40, 50 and 60 minutes) under the non- isothermal conditions. For this purpose,
pellets/non coking coal were taken in crucibles and kept in the furnaces at room temperature. The samples
were taken out at regular time intervals, and cooled, weighed to know the loss in weight. Further, the degree
of redaction was calculated by the equation (1),
Carbon pickup by pellets during reduction was estimated by Strohlein apparatus, which helped in calculating
the exact amount of oxygen, removed from the pellets. The results obtained are shown in Figure 3. From the
figure, it may be observed that the rate of reduction decreased with increasing temperature. It may also be
observed that, maximum degree of reduction rate of 62.7 % was achieved at 850 0C after 30 minutes. From
the studies, it may be observed that the crack developed on pellets surfaces with increased the time and
temperature. From the study, it may be also observed increase the cement content at 8 % also adversely affect
on blast furnaces obtained because it increased the amount of slag formation and moisture to be removed and
it decreased that rate of reduction. From the above reduction results, it can be observed that the high
temperature on reduction, from the hematite to magnetite, the week pellets fines particles develop cracks and
disintegrate to smaller and detached particles. At this stage, the wustite particles are still close to each other
and the rough outline of the original particles may still be there.
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Iron Ore Processing
60
Degree of Reduction % 40
0
0 10 20 30 40 50 60
Time (min)
4. Conclusions
Utilization of waste dump fines for pelletization process.
Higher crushing strength is observed for pellets cured under accelerated condition than the normal
one.
References
Guanzing quin and Tho Jiang., Characterization of preparing of cold bonded pellets for direct reduction using
an organic binder” ISIJ international journal, 2003, 43(10): 1: 20-25.
Sharma. T. ( 1993), "Reduction of iron ore fines with coal fines ", Iron making and Steel Making. V. 20, No.
5,. 362.
Ladin C. AMCI, S¨uheyla AYDIN, C¨uneyt ARSLAN “Reduction of Iron Oxides in Solid Wastes Generated
by Steel works” Turkish., J. Eng. Env. Sci. 26 (2002) ., 37 - 44.
Dipak K. Dutta, Dipok Bordoloi, Prakash C. Borthakur “Investigation on reduction of cement binder in cold
bonded pelletization of iron ore fines” Int. J. Miner. Process. 49 1997., 97–105.
B. B. Agrawal. K.K. Prasad And H.S. Ray., “Utilization of iron oxide waste through cold bonded
pelletizaion” ISBN : 81-87053-53-4 Processing of Fines.
ZHU De-qing, QIU Guan-zhou, JIANG Tao,XU Jin-chang “An Innovative Process for Direct Reduction of
Cold-bound Pellets from Iron Concentrate with a Coal-based Rotary Kiln” VOL.7 No.2 June 2000., J. Cent.
South Univ. Technology
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Iron Ore Processing
UPGRADATION AND MAXIMIZATION OF Fe RECOVERY FROM PROCESS WASTE
THROUGH FLOTATION
Abstract
Tailing generated from iron ore beneficiation at JSW Steel contains 48-52% Fe, 6-10% alumina and
10-14% silica. Sludges from BF and Corex units, normally referred to as the cyclone dust, contain
0.05-0.1% ZnO, 10-12% of silica and 4-6% alumina and balance iron bearing oxides. In order to recover
the iron ore concentrates from the tailings dumped, flotation studies have been made both at laboratory
scale. Subsequent to the encouraging results obtained in lab trials, full scale plant trials were conducted to
maximize the Fe recovery in the concentrate, which is a suitable feed for pellet making. The Slime
Recovery Plant (SRP) at JSW Steel has been running successfully since last two years and has been
producing good quality iron ore concentrate. In recent past, the feed Fe has gone down to around 46 to
48% with an increase in silica (12-14%) and alumina (9-11%). The flotation process is found more
amicable for removal of silica and alumina is removed partially from tailing.
For efficient removal of alumina, an innovative idea of mixing the Corex sludge with iron ore tailing was
applied and the blended mix was beneficiated. A set of experiments were conducted in combination of
process wastes (iron ore tailing and sludges) and the results are found encouraging. Processing of Corex
sludge, containing 0.06% ZnO, showed that the ZnO is getting reduced from 0.06 to 0.04% in the cyclone
underflow and further in concentrate it is reduced to 0.01%. Different proportions of Corex sludge (10, 15
and 20%) was used in processing of iron ore slime. It was observed that alumina got reduced by 2-3% in
the feed. The alumina to silica ration in the concentrate is found below 0.7, which is suitable for pellet
making. Also, a considerable reduction in ZnO and loss on ignition (LOI) in the concentrate is observed.
The feed (Fe 44-46%) is upgraded to concentrate (Fe 58-60%) with alumina to silica ratio of less than 0.7
which is suitable feed for pellet making. This practice has enabled to utilize the Corex sludge successfully
(which otherwise was partly dumped) and also high alumina tailing, thereby ensuring creation of wealth
from waste.
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Iron Ore Processing
1. Introduction
Iron ores are valuable natural resources being finite and non-renewable. They constitute the vital raw
material for iron and steel industries and are a major resource for national development. India is not
endowed with high grade iron ore resources. It is therefore, imperative to achieve the best use of available
low grade hematite iron ore as well as recovery of micro-fines of iron phase minerals from slimes/tailings
from iron ore washing/beneficiation plants should be taken seriously to maximize the utilization of these
resources for long-term sustainability. Similarly, the economic and eco-friendly process is essential to
maximize the recovery of iron value from the tailings. The nature of iron phase minerals, associated
gangue minerals and the particle size decide the process flow sheet of beneficiation to be adopted [1].
Depletion of high-grade iron ore reserves, has led to process medium and low grade iron ore to meet the
rapidly growing demand. Though there was a ban on mining, Indian iron ore industry has produced about
127.7 million tons of Iron ore in the year 2014-15 [2]. India is currently producing iron ore in the form of
lumps, fines, ore concentrates, and iron oxide powder. Indian hematite ores are typically rich in iron but
contain high alumina (as high as 7%) [3]. One of the most challenging tasks is to process high alumina
rich iron ore fines and slimes. The iron ore washing results in generation of substantial amount of slimes
(containing 6-10% alumina) which are currently discarded as waste. The generation of iron ore slimes in
India is estimated about 15-28% by weight of the total iron ore mined and thus, 20-30 million tonnes of
the iron ore values are lost every year [4]. Considering the fact of increase in the iron ore demand, finding
suitable means of safe disposal/utilization of slimes is very much essential.
The beneficiation techniques for iron ore fines and slimes are receiving worldwide attention due to fast
utilization of blast furnace grade iron ore. Most conventional beneficiation processes are not effective for
slimes. One of the important technological challenges facing the iron ore industry in India is to find
commercially viable technologies to process alumina rich iron ore fines and slimes [5]. Other important
issue is that the high cost of land for dumping the slimes and environmental impact factors made JSW to
make worthwhile attempt to minimize the tailings pond volume.
Iron ore tailing and a part of Corex sludge were discarded as waste in past. Chemical composition and
particle size analysis of iron ore tailing are given in Table 1 and 2, respectively. Similarly, chemical
composition and particle size analysis of Corex sludge are given tin Table 3 and 4, respectively. The
Corex sludge is discarded due to high ZnO (0.05 - 0.10%) and carbon content (15-20%). JSW has set up
Slime Recovery Plant (SRP) for the recovery of Fe concentrate from the discarded iron ore tailing of
beneficiation plant. Previously, the chemistry of tailing feed was around 48-52% Fe. But in recent past,
the feed Fe has gone down to around 45 - 48% with an increase in silica (12-14%) and alumina (9-11%).
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Iron Ore Processing
For efficient removal of silica and alumina from slime, Corex sludge was mixed with iron ore tailing and
the blended mix was beneficiated. Flotation was found to be the most suitable technique for the recovery
of finer iron values from slimes. Direct flotation of iron ore is relatively expensive in terms of high
reagent consumption and entrapment of gangue minerals in the froth [6], hence, reverse flotation process
was adopted for floating silica and alumina. It was observed that, alumina percentage reduced by ~ 2-3%
in the feed itself. ZnO, LOI and Carbon also reduced considerably making the concentrate suitable for
pellet making which ensures the creation of wealth from waste.
Fe(tot) SiO2 Al2O3 MgO MnO Na2O K2O CaO TiO2 P LOI
50.03 11.3 9.36 0.24 0.11 0.055 0.10 0.17 0.32 0.085 6.52
Fe(tot) SiO2 Al2O3 MgO MnO K2O TiO2 CaO ZnO SO3 C S LOI
37.95 9.3 5.9 2.16 0.38 0.146 0.21 6.37 0.10 0.72 16.0 0.40 19.1
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Iron Ore Processing
by the addition of reagents in the separate conditioning tanks. Conditioning of slurry helps in the
separation of gang particles and pure iron ore concentrate by creating difference in density.
Now, this conditioned slurry is fed into the Dual Extraction Reverse Flotation Column, for separation of
iron values from gangue particles. Air along with high pressure water is injected in to the system through
infusers to create the air bubbles & proper mixing of the slurry. During the process, the gangue particles
will adhere to the air bubbles and is collected in the froth collection launder at the top. After separation in
the top chamber the remaining slurry will pass to the bottom chamber for further separation. Concentrate
which is discharging from the bottom of the chamber is collected in concentrate tank. The froth from both
the chamber is collected in the froth/tails tank. The concentrate slurry, collected in concentrate tank, is
pumped to the de-watering cyclone banks to reduce the percentage of liquids. The cyclone overflow
contains mostly of water is taken back into the process. The concentrate which is discharging from de-
watering cyclone bank is suitable for pellet making.
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Iron Ore Processing
Results of processing of Corex sludge is given in Table 5. Corex sludge containing 0.06% ZnO showed
that the ZnO is getting reduced from 0.06 to 0.044% in the cyclone underflow and further to 0.015% in
concentrate obtained after Dual Extraction Column (flotation). Chemical analysis of cyclone overflow
and underflow is given in Table 6.
Iron ore tailing contains more alumina (8-12%) whereas Corex sludge contains less alumina (4-6%).
Blending of Corex sludge in different proportion (10, 15 and 20%) with iron ore tailings resulted in
dilution of overall alumina in feed. Effect of Corex sludge on assay of cyclone and flotation are presented
in Table 7.
It was observed that, in all the samples containing different percentages of Corex sludge, alumina got
reduced by 2-3% in the feed. Sample with 80% tailing and 20% Corex sludge has resulted in maximum
alumina removal. The alumina to silica ratio in the concentrate was found below 0.70, which is suitable
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Iron Ore Processing
for pellet making. Also, a considerable reduction in loss on ignition (LOI) in the concentrate was
observed.
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Iron Ore Processing
4. Mineralogy of feed and concentrate
5. Conclusions:
The feed (Fe 44 - 46%) is upgraded to concentrate (Fe 58-60%) with alumina to silica ratio of less than
0.70 which is suitable feed for pellet making. This practice has enabled to utilize the Corex sludge
successfully (which otherwise was partly dumped) and high alumina tailing, thereby ensuring creation of
wealth from waste.
References:
1. S.K. Biswal, Technological challenges on low-grade iron ore beneficiation and pelletization, Iron &
Steel Review, Vol. 59, No. 6, Nov 2015, pp. 2-8.
2. Indian Minerals Year Book 2014-15, Indian Bureau of Mines Publication (2015), pp. 9-10.
3. Mark Ma, Froth Flotation of Iron Ores, Int. Journal of Mining Engineering and Mineral Processing,
2012, 1(2), pp. 56-61.
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Iron Ore Processing
4. Ch. V.G.K. Murty, A. De, A Chatterjee and V.S. Rao, Reduction of alumina in iron ore classifier fines
and its influence on sinter properties, Tata Search, 1994, pp. 7-13.
5. Pradip, Processing of alumina-rich Indian iron ore slimes, Int. Journal of Minerals, Metals and
Materials Engineering, 59(5), 2006, pp. 551-568.
6. D.S. Rao, S Prabhakar, T Vijaya Kumar, Beneficiation of Iron ore fines by conventional methods,
CSIR-NML Jamshedpur, India, 2005, pp. 88-93.
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Iron Ore Processing
BENEFICIATION OF LOW GRADE IRON ORE USING ENHANCED GRAVITY
CONCENTRATOR
Abstract
Conventional gravity methods have limitations in processing very fine material and in removal of
aluminous impurities. Differential settling velocity of particles is the basis of gravity concentration which
is governed jointly by weight, buoyancy and drag force. Gravitational force is not sufficient for fine
particles because of their poor settling rates and thus it is not sufficient to create differential mobility on
fines and ultra-fines.
Enhanced gravity separators, can generate high ‘G’ force up to 300 which can effectively separate very
fine iron particles from the aluminous clayey particles. Over the last decade, EGS have found wide
acceptance to mineral industries for concentration of fines and ultrafine minerals in particular to precious
metals such as Au, Ag, Pt.
A Falcon Model SB40 Lab Scale Centrifugal Concentrator, supplied by Falcon Concentrators Inc.,
Canada was used for the present investigation. The feed stream particles are subjected to large
Centrifugal force and are segregated according to effective specific gravity along the smooth spinning
rotor wall. The ROM iron ore sample of JSPL was used for the present study.ROM iron ore was crushed
to different size ranges i.e 150,75 & 45µ for carrying out the experiments.100 g sample was mixed with
1 litre water and the feed was allowed to enter in downward direction where the rotating bowl is spinning
with very high speed. The operating conditions are as follows-Pulp density 10%,bowl rotation speed(20-
80) rpm ,Fluidization water pressure (1-13)psi. The product i.e. falcon underflow and falcon overflow of
the sample were collected, dried, weighed and their iron analysis was carried out.
Based on the above studies,at bowl rotation speed of 80 rpm & back water flow rate of 5 psi it is
possible to obtain a concentrate with a higher recovery of 78.7 & containing 58.24 % Fe. At bowl
rotation speed of 20 rpm & back water flow rate of 5 psi higher grade of underflow is obtained i.e. 62.6
% Fe with a recovery of 29.1.At 20 rpm 74 % overflow material was produced.It was retreated again in
the Falcon concentrator.The yield of the concentrate product obtained was 13.45% with a grade of 58.3
% Fe.After Roughing & Scavenging process the grade of the total U/F obtained was 61.14 % with a
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Iron Ore Processing
recovery of 43.08.The results obtained indicate that we can beneficiate low grade iron ore reserves and
obtain optimum grade and recovery using Falcon Concentrator.
Keywords: Low Grade iron ore, Falcon Concentrator,rotation speed,back water flow rate,grade,recovery.
1. Introduction
The most important minerals in these iron ore deposits are magnetite (Fe3O4), hematite (Fe2O3), goethite
(FeO (OH)), limonite (FeO (OH).n(H2O)), ilmenite (FeTiO3), siderite (FeCO3) and pyrite (FeS2).
India has huge reserves of quality iron ore which can fulfil the growing demand for domestic iron and
steel industry as well as sustain large external trade. India is the fourth largest steel producer in the world
according to the data provided by the World Steel Association. The iron ore resource in India is found to
be 13,843.94 million tones(Geological Survey of India,2010). The most important iron ore types found in
India are hematite and magnetite. Nearly 61% of hematite ore deposits are found in the eastern part of
India and 82% of magnetite ore deposits occur in southern part of India, especially in the state of
Karnataka. India possesses around hematite resources of 11,464 million tons of which 6,013 million
tonnes are reserves and 5,442 million tonnes are residual resources. According to Indian Bureau of Mines
the ratio of lumps to fine ratio produced in the country is 2:3. About 2,842 million tons (25.8%) are
medium grade lumpy ore resources while 945 million tons (8.4%) are high-grade lumpy ore. Out of the
fines resources about 2,543 million tons (22%) are medium grade ore,39.9 million tonnes (1%) are high-
grade and 17.7 million tons (1%) resources are of blue dust range. The residual are low grade,
unclassified resources of lumps and fines or high, medium, low or unclassified grades of lumps and fines
mixed.
It is also reported that nearly 60% of the iron ore come in the form of fines (-5mm) (Geological survey
2010) and a large fraction of these fines belong to low grade or medium grade iron ore. Thus, it is
required to beneficiate these fines and improve their grade in order to use these fines in the form of pellets
or sinters.
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Iron Ore Processing
1.3 Beneficiation of iron ore fines
Conventional gravity methods have limitations in processing very fine material and in removal of
aluminous impurities. Differential settling velocity of particles is the basis of gravity concentration which
is governed jointly by weight, and drag force. Gravitational force is not sufficient for fine particles
because of their poor settling rates and thus, it is not sufficient to create differential mobility on fines and
ultra-fines. The motion of particle in case of gravity separation is governed by following equation:
𝒅𝒗
𝐦 𝒅𝒕 = Fg-Fb-Fd
Where,
Fg is gravitational force,
Fb is buoyant force,
Fd is drag force.
Enhanced gravity separators, can generate high ‘G’ force up to 300 which can effectively separate very
fine iron particles from the aluminous clayey particles. Over the last decade, EGS have found wide
acceptance to mineral industries for concentration of fines and ultrafine minerals in particular to precious
metals such as Au, Ag, Pt. Different enhanced gravity concentrators are:
• Knelson Concentrator,
• Falcon concentrator,
• Kelsey jig,
• Multi-gravity separator,
In enhanced gravity concentrators gravity is increased by using centrifugal force expressed as :
𝒅𝑽𝒓
𝐦 𝒅𝒕
=Fc-Fb-Fd
During the study, low grade iron ore fines are beneficiated using falcon concentrator and optimization of
parameters (frequency of rotation and back water flow pressure) are done.
2. Experimental
2.1 Material:
Ore sample: A low grade Run Off Mine iron ore sample was used for the present study.
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Iron Ore Processing
Feed preparation: ROM was crushed to different size ranges i.e 150,75 & 50 µm for carrying out the
experiments. Different representative samples of 100 grams corresponding to each size range was
prepared using coning and quartering methods and used in studying iron ore beneficiation using falcon
concentrator at different parameters.
2.2 Methods:
About 0.1 gm of ore sample (-75µm) was taken in a conical flask and 40ml of conc. HCL was added in it.
Digestion was carried out on hot plate. The conical flask containing the ore and acid was boiled for 5
minutes and SnCl2 was added drop wise in hot condition till yellow colour disappears completely. The
solution was cooled then about 10 ml HgCl2 solution was added. A silky white precipitate was observed.
About 20 ml of acid mixture (H2SO4+ H3PO4) and a few drops Barium diphenyl amine sulphonate (BDS)
indicator were added sequentially. The solution was titrated against 0.02 N K2Cr2O7 Solution. Total Fe%
= Burette reading*0.02*0.05585*100/sample wt in gm.
Reactions involved:-
Fe2O3 +6HCl →2Fe2cl3 +3H2O
Enhanced gravity separators are often used in mineral processing operations. Their fast rotating bowl
generates an artificially enhanced gravity field several hundred times greater than earth gravity. This
produces a drastically augmented sedimentation velocity, such that enhanced gravity separators can
process large flowrates of fine and ultrafine particles with high separation efficiency. Enhanced gravity
separators are widely used in minerals beneficiation, as their superior gravity field enables them to
separate particle within narrow classes of density and size.
Falcon concentrator
2.2.2.1 Introduction
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Iron Ore Processing
SB FALCON CONCENTRATOR Falcon SB Concentrators are known as “Semi-Batch” because they
continually accept feed during the run cycle, but only produce concentrate during the periodic rinse
cycles. Run times span from five minutes to several hours, depending on the application. Rinse times are
generally less than a minute as Falcon Concentrators utilize a dynamic braking system to quickly slow the
bowl down, rinse out the concentrate, and then return to full operational speed. Equipped with a variable
frequency drive, this gravity concentrator can operate anywhere from 50 to 200 G’s. The typical
application for a Falcon SB Concentrator is recovering liberated precious metals (Au, Ag, Pt, etc.) within
a grinding circuit. Outside of grinding circuits, Falcon SB Concentrators are also used for precious metal
separation from aggregate or placer deposits. The target mineral will usually be in extremely low
concentration (grams per tonne) and a very high upgrade is desired (up to 10,000x).
2.2.2.2 Principle
Falcon concentrator is an enhanced gravity concentrator ,which is usually used for separation of fine
valuable minerals from tailing or rejects. The rotating bowl is spinning with at a very high speed and the
materials experience a very high centrifugal force. The feed stream particles are subjected to gravitational
force up to 200 G’s and are segregated according to effective specific gravity along the smooth spinning
rotor wall. The heaviest layers pass over the concentrate bed retained in the riffles at the top of the rotor
bowl.
A Falcon Model SB40 Lab Scale Centrifugal Concentrator, supplied by Falcon Concentrators Inc.,
Canada was used for the present investigation. The feed stream particles are subjected to large Centrifugal
force and are segregated according to effective specific gravity along the smooth spinning rotor wall. The
Run Off Mine iron ore sample of JSPL was used for the present study.ROM was crushed to different size
ranges i.e 150, 75 and 50µm for carrying out the experiments.100 g sample was mixed with 1 litre water
and the feed was allowed to enter in downward direction where the rotating bowl is spinning with very
high speed. The operating conditions are as follows-Pulp density 10%, bowl rotation frequency(20-80)
Hz ,Fluidization water pressure (1-13)psi. The product i.e. falcon underflow and falcon overflow of the
sample were collected, dried, weighed and their iron analysis was carried out
The results of various tests carried out are explained and discussed in this section.
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Iron Ore Processing
The average Fe grade obtained after analysing four samples using gravimetric method came as 56.01%.
Falcon Study: Falcon concentrator is one of the enhanced gravity separators which impart high
gravitational (200G) force to the particles inside the separating chamber. The technique was used for
JSPL sample to know the amenability of beneficiation. In this study, parameter such as back water flow
rate, feed size and bowl rotation speed are varied and the results obtained are depicted in Figures 1,2 and
3.
The effect frequency of the rotor bowl of the falcon concentrator was studied and the results are given in
the Figure 1.Here the back water flow rate and the feed size were kept constant at 5 psi and -150µm. With
increase in bowl rotation frequency from 20-80 Hz the yield as well as recovery of the underflow
increases. At 80 Hz the yield & recovery obtained of underflow is highest i.e. 75.56% and 78.77
respectively.
75
65
Percentage
55
Wt%
Grade
45
Recovery
35
25
20 40 60 80
Bowl Rotation Frequency(Hz)
Figure 1: Effect of bowl rotation speed in the concentration of iron ore in Falcon U/F.
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Iron Ore Processing
90
85
80
Percentage
75
Wt%
70
Grade
65 Recovery
60
55
1 5 9 13
Back Water Flow Rate(psi)
Figure 2: Effect of back water flow rate in the concentration of iron ore in Falcon U/F.
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Iron Ore Processing
85.0
80.0
75.0
70.0
yield(%)
65.0 grade(%)
Recovery
60.0
55.0
50.0
150 75 50
Figure 3: Effect of feed size in the concentration of iron ore in Falcon U/F.
3.4 Scavenging
100 g of -150 µm feed sample was treated at bowl rotation frequency of 20 Hz & back water flow rate of
5 psi and was fed to the Falcon Concentrator. Owing to large amount of O/F obtained it was re-treated
back to the Falcon and the results obtained are portrayed in the flowsheet below.
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Iron Ore Processing
4. Conclusion
From the present investigation few important conclusion can be drawn which are as follows:
The given iron ore sample after chemical analysis contained 56.01% Fe.
Based on the above studies, for iron ore sample of 75µm, bowl rotation frequency of 80 Hz &
back water flow rate of 5 psi; it is possible to obtain a concentrate with a higher recovery of 80%
& containing 58.9 % Fe.
At bowl rotation frequency of 20 Hz & back water flow rate of 5 psi, higher grade of underflow is
obtained i.e. 62.6 % Fe with a recovery of 29.1 for 150 µm iron ore sample.
At 20 rpm 74 % overflow material was produced. It was retreated in the Falcon concentrator. The
yield of the concentrate product obtained was 13.45% with a grade of 58.3 % Fe.
After Roughing & Scavenging process the grade of the total U/F obtained was 61.14 % with a
recovery of 43.08.
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Iron Ore Processing
References
Geological survey of India Production of iron ore lumps fine concentrates in India (Source MNI 01 04
2010).
International Steel Seminar Rawmaterials,technology,markets.
LIST OF TABLES:
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Iron Ore Processing
470
Iron Ore Processing
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Iron Ore Processing
BENEFICIATION OF SPECULARITE
Abstract
A specularite sample from Krishnapuram village, Veldurthi Mandal, Kurnool district, Andhra Pradesh was
received for process evolution studies to obtain coating – welding rod - concentrate, assaying Fe>65%,
SiO2 <2%, Al2O3<2%, LOI<1% and 100 % < 0.1mm or pellet grade concentrate assaying Fe>63%, SiO2
<4%, Al2O3<3% LOI<2% and 100 % <0.1mm. The sample was analyzed to get 52.44% Fe (T), 23.63%
SiO2, 0.55% Al2O3 and 0.64% LOI. It contained mainly very fine grained specularite associated with
subordinate amounts of fine grained quartz and minor to trace amounts of hematite, magnetite and
gibbsite. The process amenability test indicated that the sample is amenable to gravity and magnetic
separation. The process comprising of WHIMS at -200 mesh, D80 68 microns, 33% 20 micron, 10000
gauss intensity, 20% S pulp, followed by cleaner WHIMS at 8800 gauss yielded a cleaner concentrate
assaying 67.80% Fe, 1.90 % SiO2, 0.32% Al2O3, 0.22% LOI and 4.9 specific gravity with 63.6% Fe
distribution at wt% yield of 50.0 meeting the specification of coating and welding rod industry. The
evolved process is simple and meets the objectives laid, producing both coating – welding rod grade and
pellet grade concentrates.
1. Introduction
Specularite is a chemically inert, non- toxic ferric oxide mineral with blocky or platy crustal with a strong
micaceous parting. It is mainly used as coatings in pigment industry and as a replacement for iron powder
in welding electrodes. The sample was collected from Krishnapuram village, Veldurthi Mandal Kurnool
AP (15o N and 78oE). The ENE trending Ramalkota-Kalva-Gani, fault alignment in Kurnool basin
extending into archeans genisses –Proterozoic sediments of Kadpa in the west, houses MIO associated
with quartz, due to igneous intrusions near Veldurthi area. The specular hematite quartzite ore assaying
30-60% Fe, 3-18% SiO2 and traces to 0.04%P with 50% mean Fe, is estimated to have indicated reserves
of 3.7 million tons in Veldurthi area. The aim of the work was to evolve a process to produce obtain
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Iron Ore Processing
coating – welding rod-concentrate, assaying Fe>65%, SiO2 <2%, Al2O3<2% LOI<1% and 100 %
<0.1mm or pellet grade concentrate assaying Fe>63%, SiO2 <4%, Al2O3<3% LOI<2% and 100 % <0.1
mm by a simple eco-friendly process.
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Iron Ore Processing
ground products were subjected to wet sieve analysis. MOG results are shown in Fig. 1. The grindability
data indicated that the sample was medium hard in nature.
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Iron Ore Processing
Table 1: Effect of mesh of grind on WHIMS.
MOG, D80 PRODUCT Wt% Fe% grade %Fe Dist
Mag Concentrate 69.1 59.62 79.2
-30#,
N Mag 30.9 34.81 20.8
290 microns
Head (Cal) 100.0 51.98 100.0
Mag Concentrate 61.6 61.97 72.9
-60#
N Mag 38.4 36.84 27.1
180microns
Head (Cal) 100.0 52.30 100.0
Mag Concentrate 63.0 60.30 72.2
-100#
N Mag 37.0 39.56 27.8
96 microns
Head (Cal) 100.0 52.62 100.0
Mag Concentrate 56.0 61.79 66.5
-150#
N Mag 44.0 39.46 33.5
88microns
Head (Cal) 100.0 51.96 100.0
-200# Mag Concentrate 62.7 63.85 76.7
68 microns N Mag 37.3 32.69 23.3
Head (Cal) 100.0 52.24 100.0
Mag Concentrate 47.4 59.30 54.1
-240#
N Mag 52.6 45.23 45.9
56microns
Head (Cal) 100.0 51.94 100.0
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Iron Ore Processing
Table 2: Effect of field intensity on WHIMS.
Intensity gauss Product Fe% GradeWt% Fe% grade %Fe Dist
Mag Concentrate 13.4 67.33 17.3
3000 N Mag 86.6 49.89 82.7
Head (Cal) 100.0 52.22 100.0
Mag Concentrate 27.2 63.54 33.3
5240 N Mag 22.8 47.56 66.7
Head(Cal) 100.0 51.90 100.0
Mag Concentrate 63.0 60.30 72.2
10000 N Mag 37.0 39.56 27.8
Head (Cal) 100.0 52.62 100.0
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Iron Ore Processing
4. Conclusions
A specularite sample from Krishnapuram village, Veldurthi Mandal, Kurnool district, Andhra Pradesh
assaying 52.44% Fe (T), 23.63% SiO2, 0.55% Al2O3 and 0.64% LOI when subjected to WHIMS at -200
mesh, D80 68 microns, 33% 20 micron, 10000 gauss intensity, 20% S pulp, followed by cleaner WHIMS
at 8800 gauss yielded a cleaner concentrate assaying 67.80% Fe, 1.90 % SiO2, 0.32% Al2O3, 0.22% LOI
and 4.9 specific gravity with 63.6% Fe distribution at wt% yield of 50.0 meeting the specification of
coating and welding rod industry. The sample is amenable to processing. The evolved process is simple
and meets the objectives laid, producing both coating – welding rod grade and pellet grade concentrates.
References
1 Dyenforth, (1957), “Processing of specular hematite of Webush USA” AIMME.
2 IBM,(2004), “ Mineral facts and problems : No.17 - Monograph On Iron Ore "
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Iron Ore Processing
3 IBM, (2011) “ Iron and Steel Vision 2020”.
4 Nikolay Hristoy and Sofia, (2003), “Processing of specular hematite by wet attrition and vibration”
Google Scholar web
5 Ramana.Murthy NV, Rao BSS and Suresh Chandra,(2007), “Process Amenability Studies of High
Silica Blue Dust Iron Ore”, Proc.MPT 2007 IIT, Mumbai, pp310-317
6 Ravi BP, Kumar GS, Anath BD, Hussain MI and Kristappa MG, (2013), “Process characterization of
some iron ores of India”,The Ind.Mineralogist,47(1-2), pp125-134
7 Wang Wei –Zhi and Zhan Jin-Rui, (2011), “Beneficiation of Specularite by Gravity, WHIMS and
Reverse flotation.”- Google Scholar Web
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Iron Ore Processing
RE-JIGGING OF JIG TAILINGS TO RECOVER BLAST FURNACE GRADE IRON ORE
CONCENTRATE
Abstract
The effectiveness of rejigging of jig tailings to recover blast furnace grade iron ore concentrate was
investigated in this study. The -10 mm jig tailings sample obtained from Noamundi iron mines of Tata
Steel Ltd. was subjected to rejigging after crushing to a size of less than 6 mm and 3 mm. The operating
variables i.e. water flow rate and jig amplitude were optimized for the individual samples and the
effectiveness of jigging operation was assessed by determining the separation efficiency. The iron values
recovery and the separation efficiency were taken as the index for comparing the performance of
rejigging of -6 mm and -3 mm samples. These indices were assessed by determining the assay values of
concentrate and tailings by wet chemical analysis and XRF techniques. Optimum iron recovery of 35%
with a Fe grade of 64% was achieved for -3 mm, while for -6 mm sample, an iron recovery of 25% with a
Fe grade of 63.5% was achieved.
Keywords: Jig rejects, crushing, rejigging, blast furnace, concentrate.
1. Introduction
Tata Steel Ltd India has iron ore mines in Orissa and Jharkhand which produce lump and fine iron ore to
meet the internal demand for iron making. The iron ore processing circuit involves crushing, scrubbing,
wet screening, classification and jigging of classifier fines (-10 mm). Jigging is a gravity-separation
technique, where bulk materials are separated into light and heavy-density fraction. It is one of the oldest
methods of gravity concentration technique. Even today it is the widespread technology in coal
preparation because of its high separation precision, cost-effectiveness and high throughput rate [1,2]. It is
a technique where particles of mixed bed, size, shape and specific gravity are separated from each other
by the force of gravity with stratification. The jigging technology uses water as the separation medium
and can be applied to minerals and ores where there is a difference between the densities of wanted and
unwanted material. The performance of the jig is controlled by the operating variables like water flow
rate, jig amplitude, jig frequency and also it depends on material property like particle size [3,4]. At Tata
Steel Ltd., Bamnipal, India the recovery of metal values from ferrochrome slag has been successfully
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Iron Ore Processing
carried out by jigging [5]. A commercial jig plant has been installed in South Africa to recover metal
concentrate of 97% grade with 76% metal recovery [6]. Few authors have described jigging as a repetitive
process of fluidization and defluidization which takes place under rapid rate of change of water velocity
[7,8].
The Noamundi Iron Mine of Tata Steel Ltd. has installed BATAC JIG (under bed air pulsated jig) to
upgrade iron ore fines of size less than 10 mm. Over the years a huge quantity of jig tailings assaying
about 58% Fe and 5.34 % Al2O3 have accumulated in the plant at Noamundi. These tailings are lying
unutilized because of their poor assay value. Characterization studies have revealed that jig tailings
contain fine and liberated iron values (of size less than 1 mm). Mineralogically the jig tailings contain
hematite and goethite as the iron bearing mineral while kaolinite and gibbsite contribute as alumina
bearing minerals. In this study, the effectiveness of rejigging of jig tailings was studied after crushing
down to a size of less than 6 mm and 3 mm. The jig parameters were optimized for individual samples of
size -6+0.5 mm and -3+0.5 mm.
2. Experimental
2.1 Material
The representative jig tailings sample was obtained from Noamundi iron mine. The as received sample
was thoroughly mixed and a sample was drawn through coning and quartering method to collect a
representative sample for characterization studies. The size wise analysis of the feed sample was carried
out by wet sieving method. The head sample and the size fractions obtained from wet sieving were
subjected for chemical analysis adopting wet chemical method.
2.2 Method
A representative as-received sample was collected after coning and quartering for conducting rejigging
experiments. The sample was divided into two equal lots of 50 kg each. The two lots were then
individually crushed to -6 mm and -3 mm, respectively. The -6 mm and -3 mm crushed samples were
then screened at 0.5mm to screen out the -0.5 mm particles. The size fraction -6+0.5 mm and -3+0.5 mm
fractions were then individually subjected for rejigging test.
Rejigging tests were conducted in a Mineral Density Separator (MDS) supplied by Mintek. The MDS is a
PLC-controlled, air unit with a cylindrical chamber consisting of a number of rings clamped together and
connected to a water chamber or hutch. The pulsations are provided by air valves, with the PLC
controlling the frequency and the upstroke, holding and release times. Figure 1 shows picture of the MDS
and Figure 2 describes the cycle time.
480
Iron Ore Processing
T1 T2 DT T3
Particles loosen up
Cycle timing (T4) – bed expand
T3 T1 & T2
The MDS is capable of stratifying an ore sample according to particle density differences. After each run,
the contents of the chamber are removed in separate layers and sampled for density determination and
chemical analysis.
The MDS uses a release analysis approach to separate the sample into closely spaced density fractions.
Alternatively, the test determines the potential separation at a given feed size distribution, residence time
and operating conditions, for a jigging type separation process. The test work yields information on the
relationship between recovery and grade of the concentrate.
481
Iron Ore Processing
wise analysis. The size wise analysis of the samples indicates that about 52% of the sample is below 3
mm in size. The size wise chemical analysis shown in Table 1 indicates that the distribution of Al 2O3 is
higher in coarser fractions from 8 mm to 3 mm. The fractions finer than 3 mm contain a comparatively
lower proportion of both Al2O3 and SiO2, while iron values are seen higher compared to that in coarser
fractions.
70
57.99
60
50
40
wt%
30
20
5.34 8.37
10 2.29 0.15
0
Fe% Al2O3% SiO2% P LOI
120
100
cum wt % passing
80
60 Sample 1
Sample 2
40
Sample 3
20 Sample 4
0
0 2000 4000 6000 8000 10000 12000
Size in Microns
482
Iron Ore Processing
Table 1: Size wise chemical analysis of as-received sample.
Cum
Size % % % Al2O3
Wt% Wt% % Fe %P % LOI
(mm) Al2O3 SiO2 distribution
passing
+8 8.4 91.6 55.2 8.29 2.23 0.17 9.34 13.9
-8+6 10.7 80.9 59.16 5.68 2.15 0.16 6.34 12.1
-6+3 29.0 51.9 58.06 4.63 2.1 0.17 6.58 26.9
-3+1 40.0 11.9 60.02 4.63 1.83 0.17 6.58 37.1
-1+0.5 5.2 6.7 59.31 4.08 1.61 0.15 8.43 4.3
-0.5 6.7 100 60.78 4.35 1.24 0.14 6.41 5.7
Total 100 Cal 58.97 5.00 1.92 0.17 6.87 100
Actual 57.99 5.34 2.19 0.15 8.37
It is seen from the above results that there is a gradual increase in grade from a coarser to finer size. The
higher content of iron values in fine size can be attributed to a wider size distribution (10 to 0.5 mm) of
jig feed material that ultimately results in loss of fine iron values due to misplacement in top layer. A
coarser and wider feed size requires higher amplitude to effectively stratify the light and heavy fractions.
At such wider size distribution, the fine heavy particles stratify as top layer because of the higher jig
amplitude which does not allow these particles to trickle down. Thus there is a gradual loss of fine heavy
particles along with the coarse light fraction.
To reveal the different phases present in the ore, XRD study was also conducted. The result of XRD study
is shown in Figure 5. The major iron bearing phases are hematite and goethite while gangue phases are
kaolinite, gibbsite and quartz.
483
Iron Ore Processing
The product was collected by scrapping 5 successive layers. These layers were then subjected for density
determination and for determination of Fe, SiO2 and Al2O3. The bottom most fraction which is also the
heaviest fraction recovered from the jigging test assayed 63.5% Fe, 1.52% SiO2 and 2.45% Al2O3 while
the top most fraction assayed only 50.61% Fe and an Al2O3 of 10.81%. This sharp difference in grade
was also confirmed by a sharp difference in specific gravity of two products. The bottom fraction
(heaviest fraction) was found to have a specific gravity of 4.5 while the top layer (lightest fraction) has a
484
Iron Ore Processing
specific gravity of 3.2. The recovery of iron values is about 25.9%. A recovery-grade curve (R-G curve)
was plotted to reveal the pattern of recovery of iron values against the grade of concentrate. The R-G
curve is shown below in Figure 6.
64 7
% Fe
63 % Al2O3 6
62 5
61 4
% Al2O3
% Fe
60 3
59 2
58 1
57 0
0 20 40 60 80 100 120
% Rec
485
Iron Ore Processing
The yield of bottom most layer (heaviest fraction) was 32.5% with an Al2O3 of 2.34%. The recovery of
iron units is about 35%. The product obtained as different layers was also subjected for density
determination and it was observed that the specific gravity of the top layer was about 3.2 while the bottom
layer had a specific gravity of 4.6. The layer next to bottom layer analysed was 5.54% Al2O3, therefore
recovery of this layer along with the heavy layer would result in a concentrate having 3.4% Al 2O3 and
62.7% Fe. The recovery of iron units by combining these two fractions is 45.7%. Since an iron ore
concentrate assaying Al2O3 ≥ 2.5% is not normally acceptable for sintering process, therefore the
optimum recovery and grade of concentrate will be about 35% and 2.34% Al2O3.
The separation efficiency of the rejigging for the two tests was compared by calculating the separation
efficiencies as follows [9].
The separation efficiency is calculated based on the iron content in feed, jig concentrate and jig tailings.
The separation efficiency is calculated as
Separation efficiency, SE= R x E where E is the enrichment and R is the recovery.
(𝐶−𝐹)
Enrichment is donated by 𝐸 = (69.9−𝐹)
𝐶(𝐹−𝑇)
Recovery 𝑅 = 𝐹(𝐶−𝑇)
Where C, F, T are the concentration of iron in jig concentrates, feed and tailings.
1. For -6 mm
(63.5 − 57.59) 63.5(57.59 − 55.77)
𝑆. 𝐸 = ×
(69.9 − 57.59) 57.59(63.5 − 55.77)
𝑆. 𝐸 = 0.12
2. For -3 mm
(64 − 58.18) 64(58.18 − 55.38)
𝑆. 𝐸 = ×
(69.9 − 58.18) 58.18(64 − 55.38)
𝑆. 𝐸 = 0.18
The separation efficiency of jigging with -3 mm sample is 50% greater than the separation efficiency
obtained with -6 mm sample. This is because of the increased liberation of iron values at -3 mm feed size.
4. Conclusions
The results of this investigation clearly established that rejigging of jig rejects can yield an iron ore
concentrate with acceptable grade. The efficiency of separation is greatly influenced by the particle size
of the feed material. The separation efficiency is better in case of -3 mm compared to -6 mm feed size
486
Iron Ore Processing
because of better liberation of the iron particles from the associated gangues and also because of a narrow
size distribution of the feed. The results of the study have shown that it is possible to obtain a concentrate
with a Fe content of 64% and iron recovery of 35%. This product can be directly utilized in the steel plant
as a sinter feed material.
Acknowledgement
The authors are thankful to Dr Sanjay Chandra, Chief (R&DSS), Tata Steel Limited, Jamshedpur for his
kind permission to publish this paper.
References:
[1] Rong, X Rui and Lyman, Geoffrey J, The effect of Jigging time and air cycle on bed stratification in a
pilot scale Baum jig, Fuel, vol. 71, 1, pp. 115,1992
[2] Xia, Y.K. and Peng, F.F, Numerical simulation of behavior of fine coal in oscillating flows, Mineral
Engineering, vol 20,2, pp.113,2007.
[3] Olubambi, P.A. and Potgietez, J.H, Effectiveness of gravity concentration for the beneficiation of
Itakpe (Nigeria) iron ore achieved through jigging operation, Journal of Mineral and Material
characterization and Engineering, vol.4, No.1, pp21,2005.
[4] Mukherjee, A.K. and Mishra, B.K, Role of water velocity for efficient jigging of iron ore,Mineral
Engineering, vol 19, 9, pp.952,2006.
[5] Sripriya, R. and. Murty, Ch. V.G.K, Recovery of metal from slag/mixed metal generated in ferro-alloy
plants- a case study, Int. Journal of Mineral Processing, vol. 75, 1- 2, pp123, 2005.
[6] Yang, David C., Reenan, Ricus van. and Bhimsan, Vima, Separation of Metals from a Slag Using a
Multi-cell Jig,Journal of Minerals and Material Characterization & Engineering. vol. 2, No.2, pp137,2003
[7] Mukherjee, A.K. and Mishra, B.K, An integral assessment of the role of critical process parameters on
jigging, Int. Journal of Mineral Processing vol.81, 3, pp.187,2006.
[8] Mishra, B.K. and Adhikari, B, Analysis of fluid motion during jigging Mineral Engineering. vol. 12,
12, pp.1469,1999.
[9] B. Das*, S. Prakash, S.K. Das and P.S.R. Reddy, Effective Beneficiation of Low Grade Iron Ore
Through Jigging Operation, Journal of Minerals & Materials Characterization & Engineering, Vol. 7,
No.1, pp 27-37, 2007
487
Iron Ore Processing
FEASIBILITY STUDIES ON BENEFICIATION OF SUB GRADE IRON ORE FROM DEPOSIT 5,
BACHELI COMPLEX, BAILADILA, CHHATTISGARH USING MOZLEY MINERAL
SEPARATOR
G. V. Rao *, R. Markandeya2 and Rajan Kumar1
1
1
R&D Centre, NMDC Limited, Hyderabad, India
2
JNTU College of Engineering, Manthani, Telangana, India
*Corresponding author: vrgottumukkala@gmail.com
Abstract
A laboratory mineral separator is capable of processing particles of less than 2mm in size. It is basically a
laboratory testing device operated in batch scale. In order to establish applicability of flowing film gravity
concentration process and to optimise operating parameters, use of this separator is extremely important.
Laboratory mineral separator not only determines the feasibility of the process but also simulates an
industrial unit at laboratory stage. For rapid testing of the amenability of ore minerals for their beneficiation
using flowing film gravity concentration devices such as tables, spirals and richert cones etc. use of this unit
is found to be most convenient.
The possibility of using a Mozley mineral separator for beneficiation of sub grade iron ore and recovery of
iron values has been examined. Laboratory scale experiments were performed on sub grade iron ore (SGIO)
after stage crushing and griding to -100 mesh (-150 microns). The ‘as received’ Run off Ore Mine (ROM)
sample analysed 40.80% Fe, 40.90%SiO2, 0.24% Al2O3 and 0.22% Loss on Ignition. All other impurities
were within their critical limits. A series of 18 experiments were conducted varying three variables viz. water
flow rate (Litre Per Minute – LPM), angle of inclination (Degrees) and shaking time (Minutes). The RPM
and amplitude were initially optimised and kept constant throughout all the experiments at 80RPM and 3.0
inch. The results of optimisation of process variables and co-relation developed between the operating
variables of the equipment on the concentrate yield, grade and percent recovery of iron values has been
presented. The highest grade obtained is 67.70%Fe with a yield of 37.23% and 61.78% iron values recovery.
The results obtained were discussed in detailed in the paper.
Keywords: Feasibility, sub grade iron ore, Mozley mineral separator, beneficiation, gravity concentration,
Bailadila
1. Introduction
488
Iron Ore Processing
The quality of iron ore deposits has deteriorated worldwide as a result of long-term mining, and the existing
mines are having increasing difficulty in producing ore with a high grade of iron by simple screening. Blast
furnaces are suffering from greatly reduced productivity and a high energy consumption rate, if low-grade
ore were charged as-is. The same applies to direct reduction furnaces. Thus, there is a strong desire to
improve the iron ore grade at the stage of raw material preparation. One of the most common approaches is a
method of upgrading ore by a beneficiation process using a physical separation technique, and a number of
existing mines have introduced such beneficiation processes to upgrade their ore. Furthermore, low grade
mines, which were formerly not profitable, are being intensively developed by incorporating beneficiation
plants right from the beginning.
The accumulation of lower grade lumps and fines are increasing day by day due to increase in the regular
production of iron ore for steel industries. Simple washing of these low grade ores by scrubbing could not
upgrade the iron content as evidenced from some laboratory studies. However, the utility of these ores in
sinter or pellet making have urged many laboratories in India to undertake systematic studies for recovering
iron values from these low-grade ores.
Lot of developments in iron ore processing have been taken place in recent years in many iron ore producing
countries of the world. The emphasis was on development of a cost effective flow sheet to beneficiate the
low-grade iron ores to produce concentrates suitable for blast furnace, sinter or pellet making. The sub grade
ores range between 40-55% Fe content and are lateritic, goethitic, and siliceous. The main difficulty in
processing and utilization of low-grade iron ores primarily stems from their mineralogical characteristics as
well as the soft nature of some ores and their high silica content. Thus, beneficiating the low-grade iron ores
to remove the gangue minerals and enhancing their grade is an attractive proposition today.
The role of gravity concentration is discussed by several authors [4,5]. Beneficiation of low grade iron ore
was studied by other scholars [6,7,8]. Rao et al. studied and experimented on beneficiation of BHQ [9].
Gravity concentration of iron ores was studied by Rath and Singh (2007) [11]. Mozley mineral separator was
used to treat coal washery rejects. In this study, Mozley mineral separator is used to study the amenability of
beneficiation of sub grade iron ore.
489
Iron Ore Processing
The ‘as received’ sample of sub grade iron ore (SGIO) collected from Deposit 5, Bacheli complex, Bailadila,
Chhattisgarh is an admixture of lump and fines and friable ore; where the fines contributes in higher
proportion(up to 36%). The size of the ‘as received’ sample varies from 150mm to less than 1mm. The lump
samples show alternate bands of iron and silica.
The ‘as received’ sample is subjected to characterization studies in order to investigate its amenability for
upgradation and develop beneficiation strategies. The ‘as-received’ sample was mixed thoroughly and
representative samples were drawn for characterisation, screen assay analysis, evolution of physical
properties and beneficiation studies. The chemical analysis was carried out by standard wet chemical
analytical procedure (Anon, 1975) and induction coupled plasma (ICP) model JY2000-2 and make
JOBINYVON.
Table 1: Chemistry of ‘as received’ sub grade iron ore sample from Deposit 5, Bacheli Complex.
Constituent Fe FeO SiO2 Al2O3 LOI P S TiO2 CaO MgO MnO
Assay % 40.80 2.70 40.90 0.24 0.22 0.05 <0.01 0.091 0.119 0.110 0.045
A representative sub sample was drawn after homogeneous mixing from the ‘as received’ sample. The
representative sub sample was subjected to size analysis at 30mm, 6mm 1mm. The individual fractions
obtained after size analysis were weighed separately and subjected for stage crushing and grinding for
evaluation of their chemistry. The size analysis of the ‘as received’ sample indicates that +30mm fraction in
490
Iron Ore Processing
the ‘as received’ sample is 35.14%, which assayed 40.50% Fe and 41.80% SiO2; -6mm+1mm fraction has
48.17% Fe which is highest among all the individual fractions. The ‘as received’ sample was also subjected
to size analysis from 150mm down to 37 microns and the size distribution is shown in the figure 1. The ‘as
received’ sample was stage crushed and ground to 100mesh (150 micron) to liberate the particles as per
mineralogical studies. Size distribution of -100mesh ground product was shown in figure 1.
491
Iron Ore Processing
irrigation pipes around the circumference. The water is able to discharge over the lower edge of the tray via a
launder into bucket. Tray slope (angle of inclination), water flow rate (Liters per Minute – LPM) and
oscillation speed (RPM), amplitude (inch) and residence time may be varied to suit the sample being treated.
Separation of mineral particles is carried out after placing a sample, in aqueous slurry form, on the tray near
the upstream end. The flowing film device, which uses orbital shear, is used in many mineral processing
laboratories, and is designed to retreat small samples (100grams) of ore, allowing a relatively unskilled
operator to obtain information for a recovery grade curve with in a very short time. It very closely simulates
commercial shaking table performance and in this respect has proven invaluable for ore evaluation.
The separator fitted with the ‘V’ profile tray and knock mechanism is recommended for making separations
of samples with particle size range between 2mm to 150 microns where as a flat tray is recommended for
finer than 150 microns. Depending upon the particle size, the tray will be selected for each test.
Before starting the experiments leveling and slope adjustment has to be done. The speed of the tray and
amplitude were optimised first and kept at 80RPM and 3 inch respectively. The angle of inclination, wash
water and residence time were selected in three intervals. When wash water and irrigation water valves are
turned on, it is important that the spray surface is thoroughly wetted before attempting a separation. If any
breaks appear in the water film, greasy or shiny spots are indicated. These should be removed by further
treatment. Place 100 to 200 grams of sample in beaker and mix thoroughly with approximately with 300 ml
of water and a little dispersant such as sodium silicate. Pour the pulp slowly and carefully into the separator
tray using wash pipe or wash bottle to remove the last traces from the beaker. On starting the separator, the
sample spreads out into a thin layer on the tray surface. The mineral particles are kept in motion by the action
of the separator. High density particles, usually valuable minerals sink to the tray surface and are retained.
Low density particles usually gangue or waste minerals are carried down the tray by the flow of irrigation
water to discharge via launder. After specified residence time of sample, concentrate and tails were
separately collected, dried and weighed individually. The concentrate and tails were ground to -200 mesh (75
microns) and subjected for chemical characterisation. By analysing the products collected via the launder
over specific time intervals and the product remaining on the tray surface, at the end of the test run a
complete grade/ recovery picture may be built up for the sample. The results obtained with the flat tray are
comparable with results obtained by commercial slime table and the results obtained with the ‘V’ profile are
comparable with results obtained by commercial sand table installations when running with maximum
efficiency.
492
Iron Ore Processing
100.00
80.00
60.00
40.00
20.00
0.00
1 10 100 1000 10000 100000
Particle size in microns
4. Discussion
493
Iron Ore Processing
During the experiments, the operation variables like slope of the tray (angle of inclination), wash water and
residence time were varied. Other parameters like speed (80RPM) and amplitude (3.0 inch) were maintained
constant throughout the experimentation. The effect of slope of the tray, wash water and residence time on
concentrate yield, grade and percent recovery of iron values were discussed in the following sections.
Table 4: Test results of Mozley mineral separator test results with sub grade iron ore.
494
Iron Ore Processing
As the slope of the tray increased from 0.8 to 1.8 degrees, the concentrate yield decreased and concentrate
grade increased. The effect of tray slope on concentrate yield and grade was shown in figures 2 to 5.
80 60
Concentrate Yield (%)
Figure 2: Effect of tray slope on concentrate Figure 3: Effect of tray slope on grade of the
yield at 1 minute residence time. concentrate at 1 minute residence time.
65 70
68
60
Concentrate Grade (%Fe)
66
Concentrate Yield (%)
55 64
50 62
60
45 58
40 56
54
35
52
30 50
0.5 1 1.5 2 0.5 1 1.5 2
Tray Slope (Degrees) Slope of the tray (Degrees)
Figure 4: Effect of tray slope on concentrate Figure 5: Effect of tray slope on grade of concentrate
yield at 3 minutes residence time. at 3 minute residence time.
495
Iron Ore Processing
As the quantity of wash water increased from 0.5 to 1.5 LPM the concentrate yield decreased and concentrate
grade increased. The effect of wash water on concentrate yield and grade was shown in figures 6 to 9.
80 65
Concentrate Yield (%Weight)
60 50
55
45
50
45 40
0.4 0.9 1.4 0.4 0.9 1.4
Wash Water (LPM) Wash Water (LPM)
1 Minute 2Minute 3 Minute
1 Minute 2Minnute 3Minute
Figure 6: Effect of wash water on concentrate Figure 7: Effect of wash water on concentrate
yield at 0.8 degrees tray slope. grade at 0.8 degrees tray slope.
70 70
68
Concentrate Yield (Weight %)
65
Concentrate Grade (%Fe)
66
60
64
55 62
50 60
45 58
56
40
54
35 52
30 50
0.4 0.9 1.4 0.4 0.9 1.4
Wash Water (LPM) Wash Water (LPM)
1 Minute 2Minnute 3Minute
1 Minute 2Minute 3 Minute
Figure 8: Effect of wash water on concentrate Figure 9: Effect of wash water on concentrate
yield at 1.8 degrees tray slope. grade at 1.8 degrees tray slope.
496
Iron Ore Processing
85
65
80
Concentrate yield (%Fe)
70 55
65
50
60
45
55
50 40
0 1 2 3 4 0 1 2 3 4
Residence Time (Minutes)
Residence time (Minutes)
Wash Water 0.5 LPM Wash Water 1.0 LPM
Wash Water 0.5 LPM Wash Water 1.0 LPM
Wash Water 1.5 LPM
Wash Water 1.5 LPM
Figure 10: Effect of residence time on concentrate Figure 11: Effect of residence time on
yield at 0.8 degrees tray slope. concentrate grade at 0.8 degrees tray slope.
70 70
65 68
Concentrate Grade (%Fe)
Concentrate Yiels (%Fe)
66
60
64
55 62
50 60
58
45
56
40 54
35 52
50
30
0 1 2 3 4
0 1 2 3 4
Residence Time (Minutes) Residence Time (Minutes)
Wash Water 0.5 LPM Wash Water 1.0 LPM
Wash Water 0.5 LPM Wash Water 1.0 LPM
Wash Water 1.5 LPM
Wash Water 1.5 LPM
Figure 12: Effect of residence time on concentrate Figure 13: Effect of residence time on
yield at 1.8 degrees tray slope. concentrate grade at 1.8 degrees tray slope
497
Iron Ore Processing
As the residence time increased from 1 minute to 3 minutes the concentrate yield decreased and concentrate
grade increased. The effect of residence time on concentrate yield and grade was shown in figures 10 to 13.
5. Conclusions
The ‘as received’ sample consists approximately 44% of ore and 56% gangue minerals by area of their
distribution. Hematite (H), Limonite (LIM), Goethite (G) and Martite (M) are in category of ore minerals
whereas gangue minerals are Quartz (Q) and Iron Oxide Coated Gangue. The ‘as received’ Sub grade Iron
Ore sample was amenable for beneficiation by gravity concentration technique. The lowest grade of
concentrate (41.6% Fe) was obtained at 0.8 degrees tray slope, 0.5 LPM wash water and residence time of 1
minute. The highest grade of concentrate (67.7% Fe) was obtained at 1.8 degrees tray slope, 1.5 LPM wash
water and 1 minute residence time, with 61.78% Iron values recovery. The highest iron values recovery
(85.53%) was obtained at 0.8 degrees tray slope, 1.0 LPM wash water and residence time of 1 minute. The
lowest iron values recovery (50.90%) was obtained at 1.8 degrees tray slope, 1.0 LPM wash water and
residence time of 3 minute. The highest yield of concentrate (78.59% weight) was obtained at 0.8 degrees
tray slope, 1.0 LPM wash water and 1 minute residence time, with a grade of 44.40% Fe. The lowest yield of
concentrate (31.09% weight) was obtained at 1.8 degrees tray slope, 1.0 LPM wash water and 3 minute
residence time, with a grade of 66.80% Fe.
Acknowledgements
The authors wish to thank Shri Narendra Kothari, Chairman cum Managing Director, NMDC Limited and
Shri Narendra Kumar Nanda, Director (Technical), NMDC Limited for approval to conduct studies and
permitting to publish this paper.
References
Anon, 1975, Manual of procedure for chemical and instrumental analysis of Ores, Minerals and ore dressing
products (Indian Bureau of Mines, Nagpur).
Anon, 2011. Iron & Steel Vision -2020 (Indian Bureau of Mines : Nagpur).
Basant Rath, G Venkateswara Rao, and S K Sharma, Mineralogy and liberation studies of sub grade iron ore
from Bacheli, Bailadila sector, India. Proceedings of XXVI IMPC 2012, pp 4463- 4471.
BUR.T.R, The role of gravity concentration in modern processing plants, Minerals Engineering, 12 (1999),
pp. 1291–1300
498
Iron Ore Processing
Burt R, 1999, The role of the gravity concentration in Modern Processing Plants, Mineral Engineering 12, pp.
1291- 1300
Kumar, V, Jadhav, G N, Khosla, N K, Chattoraj, V S, Singh, R, Bhagat, R P, Nayak, B, Mohanta,
M K, Bhattacharya, K K and Mehrotra, S P, 2007, Characterisation and its implication on beneficiation of
low grade iron ore by gravity separation, in Advanced Gravity Separation,
R Singh, A Das and N G Goswami (Eds.), NML Publication, Jamshedpur,India:11
Mishra B K, Reddy P S R, Das B, Biswal S K, Prakash S, Das S K, Issues related to characterization and
beneficiation of low grade iron ore fines, Steel world, Vol. 13, No. 11, 2007, pp 34-36.
Rachappa S, Prakash Y and Amit, Iron Ore Recovery from Low grade using Advance Methods,
Proceedings of Global Challenges, Policy Frame work & Sustainable Development for Mining of Mineral
and Fossil Energy Resources (GCPF 2015), Procedia Earth and Planetary Science 11 (2015) pp. 195 – 197
Rao G V, et al 2011, Optimization of process parameters for beneficiation of BHQ, Proceedings of XII
International Conference MPT -2011.
Rao, L S., Bandopadhyay P, Application of a Mozley mineral separator for treatment of coal washery rejects,
International Journal of Mineral Processing, Volume 36, Issues 1–2, September 1992, pp. 137–150.
Rath R K and Singh R, 2007, Garvity concentration of iron ores, in Advanced Gravity Separation.
R Singh, A Das, and N G Goswami (Eds.), NML Publication, Jamshedpur,India:74-88.
499
Iron Ore Processing
FEASIBILITY OF PRODUCING SINTER FINES FROM A LOW GRADE AND FINE GRAINED
HEMATITE-GOETHITIC ORE
Abstract
Iron ore quality in India is deteriorating due to continual increase in consumption of good grade ores. It is
imperative to use low grade iron ores to meet the current demand. In the Jharkhand-Odisha belt hematite
ore containing significant amount of goethite material have difficulty in processing. In the present paper,
response of a low grade hematite-goethitic iron ore to beneficiation for the production of sinter and pellet
feed material has been investigated. The ore sample contained hematite as the major iron bearing mineral
with considerable amount of goethitic material. The major impurities present were quartz and clay. The
sample contained reasonable amount of hematitic with relatively coarse liberation, however, overall the
sample was poorly liberated. This posed difficulty in producing concentrate with desired metallurgical
performance. The modified strategy involved selectively recovering sinter fines with possible recovery of
pellet grade material. Hence, the top size of the ore was kept at 5 mm and ore was subjected to scrubbing
and washing, followed by classification. Beneficiation studies such as jigging, tabling and WHIMS were
carried out on different washed products and results are discussed. A total of 32% with Fe 63.8% sinter
material and a varied amount of pellet material could be achieved from low grade iron ore.
Keywords: Low grade iron ore, beneficiation, gravity, magnetic, sinter, pellet.
1. Introduction
India is one of the leading producers and exporters of iron ore in the world with over 28 billion tonnes of
iron ore reserves[1]. Processing of low grade iron ore is inevitable as a result of increase in production and
consumption of high grade ores . Though Indian iron ore is rich in iron but it contains high alumina,
which is not favorable for efficient operation of blast furnace [2]. Indian iron ore mine have been operated
by selective mining to maintain the high grade iron ore (Fe>60%), however, it is extremely difficult to
practice the same because of two reasons. The first is the huge quantity of material that is needed to cater
the demand of Iron & Steel industry (India’s steel capacity would be nearly 300 million tonnes by 2025)
which is not possible by selective mining alone and secondly, in the process of selective mining, large
amount of overburdens (low grades) and fines are generated and dumped near the mine site which
subsequently creates environmental hazard to the nearby residents.
1
500
Iron Ore Processing
Generally, the beneficiation of high/medium grade hematite iron ores in India includes dry circuit
covering crushing, screening or wet circuit consisting of crushing, scrubbing, washing and classification[3-
4]
. This kind of simple approach of washing and scrubbing is not sufficient enough to produce iron
concentrate with desirable quality from low grade iron ores. In recent times, several development in the
mineral processing in the area of gravity, magnetic separation and flotation namely column has taken
place globally. However, there is need to design newer flowsheet involving advanced techniques for low
grade Indian iron ores. In the present investigation, an attempt made to produce sinter grade fines and also
the pellet-feed material from a low grade iron ore sourced from eastern region of India by using various
beneficiation techniques.
2. Experimental
Methods
Mineralogical characterization of the iron ore sample was carried out by megascopic and microscopic
techniques. For optical microscopic studies polished sections were prepared and studied under a Leitz
(Leica)-orthoplan universal research microscope. Liberation characteristics of the samples were determined
using a Leitz/Leica-Zoom stereomicroscope.
Bench scale beneficiation study was undertaken on the iron ore sample crushed to -5mm. The crushed
material (-5mm) was subjected to scrubbing in a concrete mixer for 4 minutes and wet screened at two
different screens i.e.1 and 0.1mm. The three fractions i.e. -5+1, -1+0.1 and -0.1mm were treated separately
in different units such as air pulsated jig, Humboltz Wedag make, Wilfley table and Mozleys 2”
hydrocyclone respectively. The underflow material from hydrocyclone was treated in a wet high intensity
magnetic separator (WHIMS), Allmineral to enrich the cyclone underflow.
2
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Iron Ore Processing
a) Martite (Mr), microplaty hematite (mpl-H), quartz b) photomicrograph of grains under polarising
(Q) and pore space (P) in a hematitic fragment in the microscope indicating mineralogical variation and
iron ore interlocking attributes. OG- ochreous goethite, VG-
vitreous goethite, HA-G - high-Al goethite, FC-
Ferrugenous clay, C- Clay (Kaolinite/gibbsite), Mr-
martite, H- hematite.
Figure 1: Various structures and complex textures of low grade iron ore.
3
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Iron Ore Processing
Laboratory beneficiation studies
The laboratory beneficiation study results are presented in this section. The results of scrubbing, washing,
and wet screening is shown in Table-2. Scrubbing of the crushed sample produced 86.7% of -5+0.1mm
materials with 57.77% Fe and ~13% of -0.1mm slime with 44.89% Fe. The slime fraction contains
substantial amount of alumina and silica indicating that clayey component are concentrated in this
fraction and can be rejected.
70 66.34
61.12 Bottom Layer
57.19
60 53.05 Layer-2
Weight/Assay,%
50 49.55
Layer-3
40 Layer-4
23.6 19.4
30 Layer-5
23.2
18.4
20 15.4
5.8 7.71 10.23
2.14.4 3.85
10 1.2 5.01
1.6 2.32
0
Weight Fe SiO2 Al2O3
Figure 2: Results of jigging of (-5+1mm) fraction of low grade iron ore sample.
4
503
Iron Ore Processing
Tabling of -1+0.1mm fraction
The (-1+0.1mm) fraction so obtained from scrubbing and wet screening operation was treated in a sand
deck Wilfley Table. The results are given in Fig.3. The concentrate obtained from tabling shows Fe
enrichment to 59.68% with a yield of 32% ( 6 % WRO) with respect to the table feed with 55.84% Fe.
59.68
60 55.61
51.75
Table Heavy
50
Table Middlings
Weight/Assay,%
35.4
40 32.0 32.6 Table Lights
30
20
3.81 7.21 6.21 8.61
10 2.96 5.11
0
Weight Fe SiO2 Al2O3
Figure 3: Results of Tabling of (-1+0.1mm) fraction of low grade iron ore sample.
As tabling didn't yield good grade indicating locking of iron bearing minerals with gangue at 1mm size.
The (-1+0.1mm) fraction and the jig rejects (layers 3-5) were ground to -150 µm with a view to enhance
liberation of valuable mineral.
5
504
Iron Ore Processing
Wet High Intensity Magnetic Separation of cyclone underflow
The cyclone under-flow obtained from hydrocycloning condition was further treated in wet high intensity
magnetic separator at current of 0.6Amp. The results obtained are presented in Fig.4. Magnetic fraction
from WHIMS could produce 4.4 % yield WRO assaying 63.13% Fe.
70 63.13 61.04
60 53.59 Magnetics
Middlings
Weight/Assay,%
50
20
It was observed that sinter fines are possible by fine jigging (-5+1mm) with a grade of ~63.74% Fe.
Similarly, 4.4 % by weight of pellet feed concentrate with Fe content of 63.13% is possible from the
ground product (-150 µm) of fraction (-1+0.1mm) and jig rejects using desliming in hydrocyclone
followed by concentration by WHIMS.
The low yield in beneficiation may be due to poor liberation. As hematite fines interlocked in goethite
report to tailings, and high-Al goethite is equivalent to a ferrugenous gangue they report to a high grade
tailing which could not be processed.
4. Conclusions
The low grade iron ore sample contains hematite and goethitic/limonitic content as major iron
minerals and quartz and clay as the major gangues mineral. High goethitic/limonitic content and
the fine size liberation pose problem in achieving desired metallurgical performance.
6
505
Iron Ore Processing
It was observed that sinter fines 46.8% yield (~32% WRO) are possible in jigging (-5+1mm) with
a grade of ~63.74% Fe.
4.4 % by weight of pellet feed is possible to produce from ground product of (-1+0.1mm) and jig
reject upon desliming using hydrocyclone followed by WHIMS.
Acknowledgements
The authors thank to Dr. S. Srikanth, Director, National Metallurgical Laboratory, Jamshedpur, for kindly
permitting to publish this paper.
References
2. R. Singh, et al., Reduction of alumina in Indian iron ores, Metals Materials And Processes,
Vol.16, No.2 & 3, 2004, p.157-170 (2004).
3. R. Singh, and S.P. Mehrotra, Beneficiation of Iron Ores for Iron and Steelmaking, “Steel Tech”.
vol. 1 No. 5, April 2007, p.17.
7
506
Iron Ore Processing
STUDY ON PELLETISATION OF IRON ORE SLIMES (CONCENTRATE) USING NON-
CONVENTIONAL AND CONVENTIONAL BINDERS
1Ashiwani Bharti* and R. P. Bhagat
Dept. of Fuel & Mineral Engineering, Indian School of Mines, Dhanbad
*Corresponding author: ash.reet17@gmail.com
Abstract
Large amount of fines and super-fines slimes are generated in processing operations of Indian iron ore
mines. With reference to the Gua Iron Ore Mines (GIOM), SAIL, the situation is complicated as a large
amount of fines had been dumped at the mine site in the past. Its enrichment process requires intense
beneficiation. As the concentrate has the size in sub-sieve range, the process of pelletisation is the
preferred route as compared to the sintering to make agglomerate which can be used as feed material in
blast furnace/DRI process.
The paper outlines current status on the usage of non-conventional binders, particularly organic one, the
conventional one, namely bentonite and their effect on the metallurgical properties of pellets so produced.
The use of conventional bentonite binder is favourable in terms of mechanical and metallurgical pellet
properties. Organic binders are the most studied binders since they are free in silica. The use of hydrate
lime as a binder is attractive when fluxed pellets are produced. Hydrate lime can actually play two roles
as both binder and fluxing agent. Substitution of hydrate lime by bentonite significantly decreased the
total energy requirement for the process, which provides direct cost savings.
The present paper describes the methodology and results on the beneficiation of iron ore dump slimes, as
first part of the total study. The sample of iron ore which were generated from the processing of Gua
(SAIL), dump slimes has been used for the present study. The sample was characterised through wet
chemical analysis and XRD. The beneficiation study was conducted using the Spiral Concentrator and
Mozley Mineral Separator. Mozley mineral separator was found to be more effective and efficient than
the spiral concentrator.
Keywords: Gua ore mines, Iron ore slimes, Spiral concentrator, Mozley mineral separator, Bentonite,
Lime, Pelletisation, Beneficiation.
1. Introduction
The present practice of beneficiation of iron ores in India produces slimes (below 150 micron) which are
not utilized and stored in tailings pond. It is estimated that the generation of slimes is 10-20% of the iron
507
Iron Ore Processing
ore mined and it amounts to 18 million tons per year (1, 6). The preferred route of their utilization is
through the agglomeration following their Fe enrichment through adopting intense beneficiation (1). As
the concentrate generated through the beneficiation route is in sub-sieve range, the pelletisation is the
preferred route for agglomeration compared to the sintering.
Binder plays an important role in the pelletisation as it holds the particles together while the water is
removed. Inorganic and organic binders are in use in the pelletisation process (1).
Bentonite is a good binder and can improve the properties of green balls, drop strength and compressive
strength. Bentonite binder is favourable in terms of mechanical and metallurgical pellet properties,
because of its acid constituent bentonite is considered as impurity especially for iron ores with high acidic
content (2). It is investigated that how insufficient preheated and fired pellets strength can be improved
when organic binders are used as binder (2).
Hydrate lime (Ca (OH)2) can be used with ores that already have some porosity for self agglomeration. It
acts as both a binder and a basic additive. It contributes no silica to the final product (1, 2). It acts as a
silica flux when the pellet is reduced in the blast furnace and improves the metallurgical performances of
the pellet. The use of hydrate lime as a binder is most attractive when fluxed pellets are being produced
(1, 2).
The present paper describes the methodology and results on the beneficiation of iron ore slimes which
was generated from the processing of the ores in Gua Iron Ore Mines, SAIL.
2. Materials
The sample of iron ore dump slimes generated from the processing of Gua mines (SAIL), has been
studied in the present work. It was courtesy of CSIR-National Metallurgical Laboratory, Jamshedpur,
from where the sample was collected. Grade of the collected Gua iron ore slimes was found to be 62.72%
with 7.44% of alumina.
3. Experimental study
About 0.5 gm of sample was taken and added 25 ml of concentrated HCl and cover with watch glass. Put
on the hot plate for about 3-4 hrs for digestion. After digestion, filter the solution in 250 ml measuring
flask and make volume of 250 ml stock solution. Take 25 ml stock solution and added 6-7 ml
concentrated HCl. The contents were boiled for 5 minutes and SnCl2 was added in hot condition till
yellow colour disappears completely. The solution was cooled then about 10 ml of HgCl 2 solution was
508
Iron Ore Processing
added. A silky white precipitate was observed. Added 95 ml water+5ml H2SO4, 3-5 ml H3PO4 and 8 drop
of Diphenyl amine indicator and shake properly. The solution was titrated against standard potassium
dichromate solution. The solution changes into violet colour.
About 0.5 gm of sample was taken in a conical flask and added 25 ml of concentrated HCl and cover with
watch glass. Put on the hot plate for about 3-4 hrs for digestion. After digestion, filter the solution in 250
ml measuring flask. After that there were 2 parts one was filter paper and another was liquid. Residue at
filter paper was silica content which can be found by burning the filter paper in platinum crucible for
about 1 hr at 900 C.
3.2 Calculations
Initial weight of empty platinum crucible=X
After burning final weight of platinum crucible=Y
Difference= X-Y
1gm iron ore= (X-Y)/0.5
100 gm iron ore= ((X-Y)/0.5)*100
About 100 ml stock solution was taken in a conical flask. Then 4-5 drops of methyl red was added to it. 3
gm of ammonium chloride was added to this solution. Then 20-25ml ammonia solution was added then
brown colour precipitate came out and then filtered it through wattman filter paper. The residue left in the
filter paper was burnt at 900 C for 1 hr with the help of platinum crucible.
3.3 XRD
The sample ground to -200 mesh size was analyzed for XRD using Co-K alpha radiation. Fig 1 shows the
results. It is apparent from the Figure that the sample consisted of hematite as major mineral phase.
Goethite, kaolinite and quartz minerals were present as minor mineral phases.
509
Iron Ore Processing
Head sample Gua ore slime ashwini 29_10_2015
d=4.83689
900
800
d=2.69732
700
600
d=4.17584
Lin (Counts)
500
d=2.51440
400
d=1.69430
d=6.29858
d=2.44418
d=3.67695
d=4.95812
d=2.20459
300
d=1.45261
d=1.84085
d=1.48578
d=2.57807
d=1.71167
d=3.34891
d=2.24537
d=1.59839
d=1.50841
d=2.28923
d=1.56203
d=1.31074
200
d=1.79976
d=0.96033
d=1.25802
d=0.90790
d=1.05469
d=1.28690
d=0.98466
d=0.96890
d=1.10063
100
2-Theta - Scale
Head sample Gua ore slime ashwini 29_10_2015 - File: Head sample Gua ore slime ashwini 29_10_2015.raw - Type: 2Th/Th locked - Start: 10.000 ° - End: 119.998 ° - Step: 0.020 ° - Step time: 36. s - Te
Operations: Import
The beneficiation of the iron ore slime samples crushed to -150 mesh sizes was carried out in Laboratory
spiral concentrator (Fig. 2). The pulp flows around the helix of the spiral concentrator in stratification
occurs in a vertical plane. This stratification is usually considered to be the result of a combination of
hindered settling and interstitial trickling. It is likely that the Bagnold force also plays a significant role
due to the relatively high rates of shear in the helical trough. The net result is that the heavier and lighter
mineral components of the streams are thus shifted laterally in opposite directions so that one is separated
from the other.
Slurry of 500 g slimes samples in 2.5 litre water was made. The slurry fed into the sump and starts the
feed motor. The splitter was set on narrow position and the system was run for 10 minutes. The
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Iron Ore Processing
concentrate and tailing generated through the separation were collected in two separate trays. These
fractions were decanted, dried, weighed and analysed for Fe radical.
385 g slimes samples ground to -150 mesh size was placed on the tray near the upstream side after proper
wetting. The separator was operated for about 5 minutes. The heavy mineral concentrate remained on the
tray while the light tailing was discharged through launder. All the variables were maintained at their
desired level. The heavier and lighter particles after the treatment were collected separately. The
concentrate and tailing generated through the separation were collected in two separate trays. These
fractions were decanted, dried, weighed and analysed for Fe radical.
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Iron Ore Processing
Radical Analysis%
Fe 62.72
Al2O3 7.44
SiO2 2.5
5. Conclusions
The Gua iron ore slimes, studied in the present work was highly aluminous It assayed 62.72% with 7.44%
of alumina. The beneficiation through Spiral improves Fe with grade in the concentrate 66.08%. The
beneficiation through Mozley mineral separator yielded the concentrate having Fe 67.2%. Mozley
mineral separator was found to be more effective and efficient than the spiral concentrator.
References
Singh, R. Singh and Mehrotra, S.P., Beneficiation of Iron Ores for Iron and Steel making, "Steel Tech".
Vol 1 No. 5, April 2007, p.17
Eisele T. C. and Kawatra S. K., “A review of binders in iron ore pelletization”, Mineral Processing &
Extractive Metallurgy Rev., Vol. 24:pp. 1-90, 2003.
512
Iron Ore Processing
Burt, R.O. "Development in Mineral Processing-gravity Concentration Technology" Elsevier Amsterdam,
1984.
Singh, R., Bhattacharyya, K.K. Bhattacharyya and. Maulik, S.C., "Gravity Concentration of Fines and
Ultrafines", in Processing of Fines, P. Bhattacharyya, R. Singh, K.V. Rao and N.G. Goswami, (Eds.), p.
40, NML Publication, Jamshedpur, 1997.
Chan, B.S.K., Mozley, R.H., Childs, G.T.C., " The Multi gravity Separator (MGS), - A mine scale
machine", In : Mineral Processing in the United Kingdom, London, P.A. Dowd (ed.), JIM Pub., p. 107,
1989.
Iron Ore: Mineralogy, Processing and Environmental Sustainability- Liming Lu - Technology &
Engineering - 2015
513
Iron Ore Processing
STUDIES ON CHARACTERIZATION AND BENEFICIATION OF LOW GRADE IRON ORE
FINES FROM GUA ORE MINES (SAIL), JHARKHAND
Rahul Ganesh Kotini* and Ram Pravesh Bhagat
Department of Fuel & Mineral Engineering, Indian School of Mines, Dhanbad
*Corresponding author: ganesh.rahul089@gmail.com
Abstract
Generation of iron ore fines while treatment of iron ore has become an issue environmentally and
economically. High grade iron ore is depleting day by day, so use of low grade iron ore fines is required for
good Indian economy. Sintering is an important technique amongst the agglomeration processes to produce
feedstock of the blast furnace. With the objective to make sinter, we have carried out the characterization and
beneficiation studies of low grade iron ore fines (80 wt. % passing through 10 mm screen) collected from
Gua Ore Mines of SAIL situated in Jharkhand.
Specific gravity of the sample ground to -0.25 mm size was 3.26. The sample analyzed 45.92% Fe, 5.74%Al
and 22.12% silica. The ore sample consisted of Fe bearing minerals namely, hematite as major phase and
goethite as minor phase. The ore also consisted of complex alumino-silicate (kaolinite) and quartz as gangue
bearing minerals. The thermal analysis of the sample shows 3- 4% weight loss at around 350-400 degree
Celsius indicating the transformation of goethite present in the sample. SEM with EDX point analysis
describes, at different points the weight% of different elements.
The ore sample ground to -0.25 + 0.15 mm size was subjected in the Davis tube having different
magnetization 1, 1.4, and 1.8 Amp at 16.34 %(v/v) pulp density. The concentrate analyzed Fe 60.48%,
62.72%, and 66.09% respectively having percent Fe recovery 10.14%, 12.23% and 13.43%. Poor recovery
has been attributed to the nature of ore, as it consisted of higher amount of alumina and silica. Separation
with higher magnetic intensity using WHIMS increased the Fe recovery to 49.10 % with Fe grade 62%
significantly at 5.2 amp magnetic current. The gravity separation using the spiral concentrator has given
encouraging results at pulp densities of 10%, 15% and 20% having recoveries of Fe content 35.74%, 49.11%
and 27.76%
Keywords: Iron ore fines, characterization, gravity and magnetic separation, Gua ore mines, sinter.
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Iron Ore Processing
1. Introduction
Indian iron ore contains high amount of clay and is brittle in nature which generates -10 mm fines as a major
fraction. Iron ore containing alumina as impurity is one of the important factor that effects crushing and
sizing the ROM ores, and had a common property to break down into fines as compared to hard ores which
leads to the slime being richer in alumina, and alumina content may vary from 4 - 8% in fines which in turn
produces 21 - 26% of slag [1]. Processing of these types of ores has brought solution for both environmental
and economic issue. These fines are of low grade which cannot be produced as feedstock (as charge) for the
blast furnace. Sintering is an important technique amongst the agglomeration processes to produce the charge
for the blast furnace. By the process of micro-balling, even -100 mesh particles are used as charge for
sintering[2]. Beneficiation/washing process is carried out to obtain products which have alumina less than
2% (lump and sinter fines) and fines of size less than 0.15mm (150 microns) accumulated with high
percentage of alumina(>4%) which cannot be used in the blast furnace [3]. Beneficiating the minerals by
gravity concentration has been recognised as low cost and high productive process. Spiral concentrator is one
of the gravity separation processes which have high separation efficiency for the particles below 30 micron
size [4-5]. It is more difficult to treat low grade ores which contain high amount of alumina. The spiral
concentrator does have low capital cost and high separation efficiency, especially in removal of silica
constituent of iron ore fines [5]. The complete beneficiation process invariably end up when enriched portion
as concentrate and the undesired minerals are obtained in the form of tailing [6]. The complete
characterization and amenability for beneficiation are studied for required quality of ore and to fulfill the
objectives [7]. Through the process, low grade iron ore fines can be utilized effectively, which makes the
overall process of iron-making profitable.
The test sample of iron ore fines about 135 kg of size -10mm was collected from Gua ore mines, SAIL,
Jharkhand. The sample was mixed thoroughly and the representative sample was drawn through simple
method of coning and quartering for the characterization and beneficiation studies.
The experimental procedure for the characterization of dump fines from Gua ore mines consists of
(a)chemical analysis (b)Specific Gravity measurement (c)SEM with EDAX (d)TGA (e)XRD studies.
515
Iron Ore Processing
(a) Chemical analysis:
The wet analysis method was followed for chemical analysis of radicals namely, Fe, SiO2 and Al2O3 present
in the iron ore sample. The sample contains 45.92% Fe, 5.24% Al and 22.12% silica. It is observed that
sample contains high alumina and silica which is not an acceptable grade for metallurgical industries. For this
concern the grade should be improved by rightful beneficiation techniques.
The specific gravity of sample was determined by a simple w/w technique depending on porosity of the
sample. The specific gravity of ore sample size (-72#) measured as 3.261.
(W4-W1) (W3-W1)
Specific gravity of solid= (W3-W1) - (W5-W4) (W2-W1)
Where W1= weight of empty bottle with lid
W2=weight of bottle +water (full)
W3= weight of bottle + kerosene (full)
W4=weight of bottle + 1/3rd sample
W5=weight of bottle +1/3rd sample + kerosene
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Iron Ore Processing
517
Iron Ore Processing
3. Beneficiation Studies
It is evident that the sample contains high alumina and silica content even at finer fraction from the
characterization studies, so the suitable beneficiation techniques should be provided so that sample can be
used further in metallurgical industries and also beneficiation should be of low operating and maintenance
cost. 20 g of ground sample having size -0.25+0.15 mm was subjected in the Davis tube having
magnetization 1, 1.4, and 1.8 Amp at 16.34% (v/v) pulp density. The concentrate analyzed Fe 60.48%,
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Iron Ore Processing
62.72%, and 66.09% respectively having good amount of Fe with recovery 10.14%, 12.23% and 13.43%.
Poor recovery has been attributed to the nature of ore, as it contains higher amount of alumina and silica.
Separation with higher magnetic intensity using WHIMS using steel wool matrix at 5.2 amp magnetic
current increased the Fe recovery to 49.10% with Fe grade of 62% .By using WHIMS the cost of operation
increases though with good recovery and grade but by using gravity separation the cost can be reduced.
Among gravity separation processes, the spiral concentrator is more affordable with low maintenance.
Insmart two product laboratory scale spiral concentrator was used for testing. The concentrate and tailing
were collected by changing the pulp density (w/w) significantly i.e. 10%, 15% and 20% which have good
recovery and Fe content. The ground sample of size (-0.1mm) was fed to the concentrator.
The experiments were carried out using the spiral concentrator to separate the concentrate of grade 60-62%
Fe content from ROM of Gua Ore Mines, Jharkhand. The experimental results of the test program along with
their condition are tabulated in Table (2). The splitter position was kept narrow and the product collected has
an influence on the quality of the concentrate fraction. It was possible to achieve the concentrate grade of
58.61% Fe2O3 at narrow splitter position. Similarly there was also the influence of feed pulp density varying
10%, 15% and 20% which showed that the concentrate fraction of spiral concentrate was enriched by grade
at higher pulp density. 53.76%, 59.36% and 62.72% Fe content are obtained from respective pulp density. By
increasing the pulp density of feed, the recovery of the concentrate fraction varied accordingly. 5 sec spiral
time was kept constant for all experiments.
Figure (4) represents the curve between the pulp density with concentrate Fe content and recovery, it is
observed that pulp density is directly proportional to concentrate grade but in case of recovery, at 15% pulp
density, the recovery obtained was 49.10% which is more than that with the 10% and 20% pulp density.
Figure (5) represents the variation between the ratio of concentration and pulp density which shows that at
15% pulp density the least F/C ratio was obtained. So the optimum pulp density was 15% by which we can
process for further work to achieve the objective
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Iron Ore Processing
70
60
50
Pulp density Vs
40
concentrate grade
30
Pulp density Vs
20 Recovery
10
0
0 10 20 30
6
5
concentration
4
3
ratio of
2
1
0
0 10 20 30
pulp density
4. Conclusions
On the basis of characterization studies on iron ore sample of Gua ore mines it can be described that sample
contains high alumina and silica content, and poor Fe content. Ore sample was treated in different equipment
for consistent feed recovery and grade. Davis tube test results in the poor Fe recovery which can be attributed
to the nature of ore, as it consisted of higher amount of alumina and silica. Separation with higher magnetic
intensity using WHIMS increased the recovery significantly with steel wool matrix. The gravity separation
using the spiral concentrator has given encouraging results with lower cost of operation producing the same
recovery as the WHIMS. The spiral concentrator was referable for these types of ores which consist of high
alumina and silica.
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Iron Ore Processing
References
M.P.Srivastava, S.K.Pan, N.Prasad, and B.K.Mishra, Characterization and processing of iron ore fines of
Kiriburu deposit of India, International Journal of Mineral Processing 61, 2001, 93-107.
C.Raghukumar, Sunil Kumar Tripathy, S.Mohanan, Beneficiation of Indian High Alumina Iron Ore Fines –
A Case Study, International Journal of Mining Engineering and Mineral Processing, 2012, 1(2), 94-100.
P.Ramsaywok, M.K.G.Vermaak, and R.Viljoen, Case study: high capacity spiral concentrators, The Journal
of the Southern African Institute of Mining and Metallurgy Volume 110.
G E Sreedhar and Dr. P C Naganoor, Process Development for Beneficiation of Iron Ore Slimes from
Donimalai Area, International Journal of Engineering Sciences & Research Technology, ISSN: 2277-96.
521
Iron Ore Processing
522
Manganese and Chromite Ores
523
Manganese and Chromite Ores
OPTIMIZATION OF SPIRAL CONCENTRATOR FOR BENEFICIATION OF CHROMITE
ORE
Gurudas Mustafi, Monomit Nandy, Ankur Kumar and Arpit Gupta*
MBE Coal & Mineral Technology India Pvt. Ltd.
*Corresponding author: arpit.gupta@mbecl.co.in
Abstract
With the present scenario of Indian Chromite ore industry, the utilization of low & medium grade
chromite ores have brought upon us new challenges and opportunities. To cater the demand of marketable
grade of chromite ore and utilization of low grade chromite reserves/dumps with the future prospects of a
sustainable chromite ore industry, India must improve the existing beneficiation industry as well as boost
the production capacity to emerge as new global leader. At Orissa Mining Corporation, existing Chrome
Ore Beneficiation Plant (COBP) at South Kaliapani; with a capacity to treat 150,000 TPA of low grade
chromite ore has been modified to produce saleable grade chromite concentrate.
MBE Coal & Mineral Technology India Pvt. Ltd. was awarded the modification project on a turnkey
basis for the existing COBP to generate 52% chromite content concentrate from the feed of 30-35%
chromite content. A flat bottom cyclone along with Hydroclassifier was installed in place of existing
classifying cyclone; and two parallel streams of spiral units were installed for coarse and fine concentrate
in place of existing gravity separation units. In addition, existing equipment maintenance, modification of
pipe routing and improvisation of operation parameters were also carried out to achieve the guaranteed
figures of the contract. This paper discusses the modification job carried out at the existing COBP and
their effects on the overall performance of the plant. A focused study has been detailed on the viability
and performance of Spiral concentrator units for the beneficiation of low grade chromite ore of Sukinda
region.
1. Introduction
Chromite is strategically an important source of chromium, which is widely used in metallurgy, refractory
and chemical industry. After South Africa, Kazakhstan, Zimbabwe and Finland, India has the 5th largest
reserves of the chromite ore. India is the third highest producer of chromite ore with 2.95 Million tonnes
(1)
per annum , which is 11.4% of the total world chromite production. Chromite deposits of Sukinda and
Nuasahi ultramafic belt constitute 93% of the country's chromite resources (2), which is estimated at 203
(1)
Million tonnes . Till now, the chromite ore beneficiation plants in India have been processing medium
524
Manganese and Chromite Ores
to high grade chromite ore reserves, which includes crushing, grinding, classification, conventional
gravity separation and thickening processes. To cater the demand of marketable grade of chromite ore and
utilization of low grade chromite reserves/dumps with the prospects of a sustainable chromite ore
industry, India must improve the existing beneficiation industry as well as boost the production capacity
to emerge as new global leader.
To achieve the guaranteed parameters of 52% chromite content product with optimum recovery, the
modified beneficiation circuit was conceptualized as shown in Fig-1. In the new scheme of beneficiation,
open circuit operation of the rod mill is converted to close circuit operation, replacing the existing
Hydrocyclone by a system of Hydrocyclone & Hydroclassifier of AKW, GmbH make. This combination
of classification is installed to provide an overflow of 150 microns with 80% passing. Two parallel lines
of Spiral circuits are installed in place of existing BM gravity separators to produce coarse and fine
concentrates. A single stage twin-start Spiral unit was placed for coarse beneficiation to produce
concentrate grade of 52% chromite content. A two stage beneficiation viz. rougher and cleaner stage
spiral units, both twin starts, are placed for fine beneficiation.
In addition, to assess the performance of individual existing equipment, samples have been collected from
different locations for a significant period inside the plant and the assessment of the results of the
collected samples has been done. Maintenance/improvisation of the existing equipment has been
simultaneously carried out and necessary changes in the pipe routing, attuning of operational parameters
such as solid feed rate, water dilution, and pressure have been carried out.
525
Manganese and Chromite Ores
526
Manganese and Chromite Ores
As shown in Table-1, the plant feed has been consistent at around 35% chromite content, however the
amount of -35µm was 26.97% of the total feed, which proves significant presence of ultrafines in feed.
The performance of the spiral concentrator units are shown in figure-2 and figure-3.
Figure 2: Graph for feed grade, concentrate grade and recovery for coarse spiral unit.
Figure 3: Graph for feed grade, concentrate grade and recovery for fine spiral units.
The individual tailing grade of all spiral units and their combined tailings grade have been shown in
Figure 4.
527
Manganese and Chromite Ores
i) The upgradation of more than 10% chromite content with an average metal recovery of 92.25% has
demonstrated the efficiency of the spiral concentrator for the beneficiation of the coarse chromite ore
with particles ranging from 150 µm to 75 µm in size.
ii) The results obtained from the fine spiral concentrator units have shown a matching performance with
an upgradation of 15.90% chromite content in two stages of spiral concentrator viz. rougher spiral and
cleaner spiral concentrator units.
iii) The metal recovery of the fine rougher spiral unit is 72.79%, which is relatively less as large amount
of ultrafines, both natural and generated, have affected the performance of the unit.
iv) Most of the ultrafines, irrespective of their specific gravity reported to tailings. Misplacement of high
grade particles to some extent was also noticed due to change in viscosity of fluid due to the same.
v) After the first stage of spiral concentrator in fine circuit, most of the ultrafines escaped through
tailings. The feed to fine cleaner spiral had lesser fraction of ultrafines, which also reflected in the
terms of metal recovery.
vi) The metal recovery of the fine cleaner spiral is 91.94% which shows that the application of the spirals
is very prolific for particles of 75µm to 25 µm size range.
5. Conclusions
With the constraints of designing the new beneficiation circuit with existing equipment and varying feed
quality, this performance seems promising (refer: Figures2, 3 and 4). The applicability of spiral for up-
gradation of chromite ore is a viable option for the processing of particles of 150 µm to 25 µm size range,
where optimum liberation of metal particles is achieved for such ore bodies.
References
Indian Minerals yearbook 2013 (Volume III, Chromite), Indian bureau of Mines.
528
Mineralogical characterization
529
Mineralogical characterization
CHARACTERISATION AND ASSESSMENT OF GOETHITE RICH IRON ORE FOR
BENEFICIATION FROM DEPOSIT 14 & 11C,
KIRANDUL COMPLEX, CHHATTISGARH, INDIA
Basant Rath, G. V. Rao* and Rajan Kumar
R&D Centre, NMDC Limited, Hyderabad, India
*Corresponding author: gvrao@nmdc.co.in
Abstract
Modern mining production faces a wide variety of operational challenges. While ore bodies are becoming
increasingly complex, both from mineralogical and textural perspective, as grades continue to decline, the
sustainability of mining requires that more care is to be taken with penalty elements. As a result,
elemental and mineral deportment is becoming a critical requirement for ore characterization projects.
Through study of process mineralogy of iron ore, it is possible to understand the behavior of the ore feed
during processing in the beneficiation plant and also later on agglomeration (Sintering and Pelletising). It
is required to know the kind of minerals and textures the ore possess, due to the fact that the liberation
characteristics are intimately related to the mineralogical texture. Optical microscopy identifies and
quantifies both mineralogical and textural properties.
The present study pertains to the mineralogical characterisation, mineral liberation studies,
photomicrographs and chemistry of goethite rich iron ore sample from deposit 14& 11C, Kirandul
Complex, Bailadila, Chhattisgarh using XRD, Optical microscopy and Chemical analysis.
The chemistry of the ‘as received’ sample reveals that the iron content (%Fe) in the ‘as received’ sample
is 55.00%, Silica (SiO2) 15.16%, 1.51% Al2O3, 3.60% Loss On Ignition (LOI) and all other critical
elements are within their critical limits. Detailed ore mineralogical studies suggest that the ‘as received’
sample consist approximately 64% of ore and 36% of gangue minerals by area of their distribution.
Hematite is the main ore mineral other than Goethite and Limonite, and gangue minerals are Quartz,
Pseudo Ore and Ferruginous Clay.
Keywords: Goethite rich iron ore, characterisation, geochemistry, mineralogy, beneficiation, specific
gravity, liberation studies, Bailadila.
1. Introduction
Bailadila range of mines is perched on the southern tip of Chhattisgarh in Dantewada District. The range
comprises of 14 iron ore deposits. Bailadila lies in the Survey of India toposheet no. 65F/2 within latitude
18o32'32" North and 19o36'5" North and longitude 81o13' & 81o14'30". "Bailadila" ranges of hills derive
530
Mineralogical characterization
its name from the shape of the hills. As the hills of the range look like 'the hump of an ox', it's named so
by the native inhabitants of this place [1].
The largest Iron ore deposit of the Bastar craton are in the thick, Banded Iron Formation (BIF) bearing
succession of the Bailadila Group in the Bailadila hill range (Fig. 1). The Bailadila group spreads 40 km
long and around 1 km wide range of hills. The north-south distribution of 14 deposits of Bailadila range
was presented in Figure 1[5]. Bailadila is at a mean sea level of 540m and its highest point stands out as
high as 1260 m above mean sea level. The easterly dipping eastern limb of the synclinorium is overturned
and the western limb is steeply easterly dipping to sub-vertical. The BIF unit is resistant to weathering
and forms a range of hills that hosts 14 individual ore bodies numbered for mining purpose as Deposit
No. 1 to Deposit No. 14 (Crookshank, 1938, 1963).
The association of very rich and extensive iron ores with hematite - quartzite in the Bailadila range has
first been made known to the world in 1898-1900 by Mr. P.N.Bose who was the first person to do
geological mapping of this region. A systematic geological mapping was done later during 1932-38,
through which 14 iron ore bearing hills have been chalked out from the range [1].
The Commercial discovery of Bailadila dates back to 1955-56 when Prof. Euemura of Japanese Steel
Mills Association, studying the memories of Geological Survey of India, draw the attention of the
Japanese Steel Mills to the richness of the vast deposits of iron ore and its proximity to the Eastern Coast
of India.
India is bestowed with large resources of iron ore, it occurs in different geological formations. These
deposits of iron ore are found to be associated with volcano sedimentary banded iron formations of
Precambrian age.
As per United Nations Framework Classification (UNFC) of mineral resources, total resources of iron ore
in the country is around 28.52 billion tonnes (National Mineral Inventory as on 01-04-2010). Hematite
and Magnetite are the principal ores of iron with 8.09 billion tonnes under reserve category and 9.79
billion tones under remaining resources category; accounting to 17.88 billion tonnes where as 10.64
billion tonnes under reserve category and 0.02 billion tonnes in reserve category with a total of 10.64
billion tonnes for magnetite [4].
With high grade iron ore reserves under the threat of depletion despite revision of threshold value of iron
ores to 45% Fe and 35% Fe (from hematite ore and siliceous hematite ore respectively), it is obligatory on
the part of mining industry to consider exploitation and utilisation of low/ lean grade iron ores which
hitherto were considered as waste for effective utilisation. A fresh exploration strategy would have to be
drawn with low grade as well as sub grade iron ores for beneficiation and utilisation. The role of
geochemical and mineralogical characterization is paramount to arrive at the process flow sheet
531
Mineralogical characterization
development for such complex ores. An attempt has been made to peep in to the geochemistry and
mineralogy of goethite rich iron ore available at Deposit 14 & 11C of Kirandul Complex, Bailadila which
will help to evolve an economically viable process flow sheet development for beneficiation.
Figure 1: Iron ore deposits of Bailadila range, south Bastar, Dantewada district, Chhattisgarh [5].
Geochemistry of banded iron formations of Singbhum region, Sandur schist belt Jharkhand- Orissa,
eastern India, granulitic terrain of north Arcot district of Tamilnadu, Orissa north-western Tamilnadu,
were studied by several scholars[6 to 17]. Whereas the Mineralogy, geochemistry and mineral liberation
studies of Goethite rich iron ore of Bailadila region are not available in the literature. Hence an attempt
has been made to study the geochemistry, mineralogy and mineral liberation studies of Goethite rich iron
ore from Bailadila Region.
532
Mineralogical characterization
2. Materials and methods
2.1 Sample and methodology
Around 16 tonnes of Goethite rich iron ore sample from Deposit No. 14 &11C, Kirandul Complex,
Bailadila, Chhattisgarh was collected for characterization and beneficiation studies. The sample was
designated as ‘as received’ sample for all practical purposes. Physically, the ‘as received’ sample is an
admixture of hard and soft lump, fines, powder and friable ore, in which fines contribute in higher
proportion. The ‘as received’ Goethite rich iron ore sample is highly altered lump, reddish brown to
yellowish brown in colour, porous in nature with a size range of 0 to 150mm. The sample was thoroughly
mixed and representative sub samples were drawn by standard sampling techniques for characterization
viz. head assay, evaluation of physical properties, mineralogy and mineral liberation studies.
Representative sub samples were drawn by standard sampling techniques and subjected to
characterization studies in order to investigate ore and gangue minerals, mineral liberation studies and
their distribution. Characterization studies include chemistry, physical properties, X-Ray diffraction
(XRD) studies, and mineralogy and mineral liberation studies. These steps were described in detail in the
following sections and corresponding observations were discussed.
A representative sub sample was drawn by adopting standard sampling techniques, stage crushed and
ground to 200mesh (75microns) for chemical analysis by adopting standard methods. The chemistry of
the ‘as received’ sample reveals that the iron content (%Fe) in the ‘as received’ sample is 55.00%, silica
(SiO2) is 15.16%, 1.51% Al2O3, 3.60% Loss On Ignition (LOI) and all other critical elements are within
their critical limits. The chemistry of ‘as received’ sample was presented in table 1. The chemical
analysis of major elements was done by standard wet chemical methods (volumetric and gravimetric),
loss on ignition by thermo gravimetric analyzer (model- Thermostep, make-Ultra) and trace elements by
induction coupled plasma (ICP, model JY2000-2, make JOBINYVON).
Table 1: Chemistry of ‘as received’ Goethite rich iron ore sample from deposit 14 & 11C, Kirandul
Complex.
Constitu-
Fe SiO2 Al2O3 LOI P S TiO2 CaO MgO MnO Na2O K2O
ent
533
Mineralogical characterization
Assay % 55 15.16 1.51 3.6 0.04 <0.01 0.48 0.10 0.03 0.03 0.07 0.043
The bulk density, specific gravity and angle of repose of ‘as received’ sample was determined by
adopting standard methods. The specific gravity, bulk density and angle of repose were found to be 3.90,
2.56 t/m3 and 34.7 degrees respectively. The energy required for grinding the sample from infinite size to
less than 150 micron (Bonds Ball Mill Work Index) was found to be 7.74kW/MT).
2.2.2 X-ray diffraction studies
X-ray diffraction technique (XRD) was extensively used for identification of various mineral phases for
assessing the abundance of each phase in an ore sample. The XRD was carried out on XRD machine supplied by
Pananalytical (Model - Xpert MRD) having automatic divergence slit, receiving slit and graphite mono-
chromator assembly. A diffraction pattern recording the angle 2θ against the intensity was obtained over a
range of 0˚ to 80˚ with scanning rate as 2˚ per minute with copper (Cu) anode. Each mineral phase exhibits a
characteristic reflection peak of its d-values. The mineral phases were identified by using the software
supplied with the equipment. The XRD difractogram of ‘as received’ sample was shown in figure 2. The
XRD studies reveal that goethite and hematite are the main ore mineral and quartz (SiO2) is the main
gangue mineral.
2.2.3 Mineralogical Studies
Required numbers of thin polished sections were prepared from various types of ore specimens by cutting
into smaller sizes by diamond wheel saw and isocut slow speed saw. Detailed ore microscopic studies
have been conducted to study the mineralogy, texture, micro structural aspects and mineral liberation
parameters in respect to various ore types by ore research microscope
Figure 2: X - Ray Difractogram of goethite rich iron ore from deposit 14 & 11C, Kirandul Complex,
Bailadila.
534
Mineralogical characterization
.Microphotographs were taken under reflected light, transmitted light, for detailed study of ore minerals,
gangue minerals and mineral liberation studies. The mineral phases were identified based on their
physical and optical properties. The mineralogical studies were done by using Lieca petrological
microscope (model: DMLP) and the quantity of various phases was identified by using software (Lieca
QWin V3).
3. Mineralogical studies
3.1 Ore mineralogy
The sample shows presence of low to moderate amount of ore minerals as hematite and high amount of
secondary mineral as goethite and limonite. The ‘as received’ sample is suggestive of moderate
distribution of ore minerals with considerably higher quantities of gangue minerals, mainly very fine
grains of altered products of ore and gangue minerals along with some pseudo ores. Detailed ore
mineralogical studies suggest that the ‘as received’ sample consist approximately 64% of ore and 36% of
gangue minerals by area of their distribution. Hematite(H) is the main ore minerals other than goethite(G)
and limonite (LIM), and gangue minerals are quartz(Q), pseudo ore(PSO) and ferruginous clay(FCL).
3.1.1 Hematite
Hematite (H) is the main ore mineral present in the ‘as received’ sample, which covers at around 20%
area by distribution. Coarsest grains are up to 1000 micron in size. All hematite grains occur in various
shapes and sizes and texturally it can be categorized into three groups as coarse, medium and small sized
grains. Coarse, medium and small size grains are in size range of 1000 to 100 micron, 100 to 30 microns
and less than 30 micron respectively.
Among the hematite grains, around 8% area is covered by coarse grains, out of which around 30% grains
are in fully liberated state and free from any gangue association. Remaining 70% grains are un-liberated
and show close association with other grains at less than 650 micron size. Among the medium sized
grains, which cover around 40% area of total hematite distribution, around 32% grains are in fully
liberated state. Remaining 68% grains are un-liberated and are associated with less than 75 micron sized
gangue minerals. Remaining 52% area of hematite is covered by fine grains, mainly less than 30 microns.
Among these, around 40% grains are in fully liberated state; whereas remaining 60% grains show very
fine, mainly less than 20 micron sized gangue minerals association. (Fig. 3, 4, 5, 6, 7 and 8).
3.1.2 Goethite
535
Mineralogical characterization
After hematite, goethite (G) is the ore mineral which occurs around 32% area as a whole in the ‘as
received’ sample. All goethite grains can be categorize into three classes as coarse, medium and small
based on their sizes. Coarse size grains are in size range of 350 to 100 micron size, medium size grains
are in size range of 100 to 30 microns size and small grains are at less than 30 micron size.
Coarse size grains which cover around 5% are as a whole of the goethite grains. Medium sized grains
cover around 22% area of total Goethite distribution and small size grains covers around 73% of the total
Goethite distribution. Among the coarse size grains, around 10% grains are in free-state and remaining
90% grains are in un-liberated state. All un-liberated grains in coarse size show close association with
other minerals at less than 180 micron size. Among the medium size grains, around 25% grains are in
fully liberated state and remaining 75% grains are in un-liberated state. All un-liberated grains show close
association with other ore and gangue minerals at less than 35 micron size. Among the small size grain,
which covers around 73% area, around 38% grains are in free-state and remaining 62% grains are in un-
liberated state and associated with other ore and gangue minerals at less than 20 micron size. (Fig.3, 4, 5,
6, 7 and 8).
3.1.3 Limonite
Limonite (LIM) is the mineral which covers around 12% area as a whole in the ‘as received’ sample. All
Limonite grains can be categorize into three classes as coarse, medium and small based on their sizes.
Coarse size grains are in size range of 130 to 100 micron size, medium size grains are in size range of 100
to 30 microns size and small grains are at less than 30 micron size.
Coarse size grains cover around 5% area as a whole are of the limonite grains. Medium sized grains cover
around 28% area of total Limonite distribution and small size grains covers around 67% of the total
Limonite distribution. Among the coarse size grains, around 15% grains are in free-state and remaining
85% grains are in un-liberated state. All un-liberated grains in coarse size show close association with
other minerals at less than 70 micron size. Among the medium size grains, around 30% grains are in fully
liberated state and remaining 70% grains are in un-liberated state. All un-liberated grains show close
association with other ore and gangue minerals at less than 50 micron size. Among the small size grains,
which cover around 67% area, around 35% grains are in free-state and remaining 65% grains are in un-
liberated state and associated with other ore and gangue minerals at less than 20 micron size. (Fig. 4, 5
and 8).
3.2 Gangue mineralogy
In the ‘as received’ sample, gangue minerals present are quartz(Q), pseudo ore(PSO) and ferruginous
clay(FCL).
3.2.1 Quartz
536
Mineralogical characterization
Quartz(Q) covers around 8% area as a whole by its area wise distribution. All quartz grains occur in
various shapes and sizes and texturally it can be categorized into three groups as coarse, medium and
small sized grains. Coarse sized grains are in size range of 130 to 100 micron size, medium grains are in
size of 100 to 30 microns; whereas small grains are less than 30 micron in size. Among the quartz grains,
around 10% area is covered by coarse grains, out of which around 15% grains are in fully liberated state
and free from any gangue association. Remaining 85% grains are un-liberated and show close association
with other grains at less than 70 micron size.
Among the medium sized grains, which cover around 30% area of total quartz distribution; around 35%
grains are in fully liberated state. Remaining 65% grains are un-liberated and are associated with less than
75 micron sized gangue minerals. Remaining 60% area of quartz is covered by fine grains, mainly less
than 30 microns. Among these, around 40% grains are in fully liberated state; whereas remaining 60%
grains shows very fine, mainly less than 20 micron sized gangue minerals association. (Fig. 3 and 4).
3.2.2 Pseudo ore:
Pseudo ore(PSO) is the another gangue mineral that occurs in the ‘as received’ sample. Pseudo ore is the
mineral which shows some properties of ore minerals but differs in other properties and hence termed as
pseudo ore. This mineral covers around 4% area as a whole. All pseudo ore minerals are in less than 70
micron size. None of the pseudo ore is in free-state. (Fig. 3,4 and 5).
3.2.3 Ferruginous clay:
In the ‘as received’ sample, ferruginous clay(FCL) is the gangue mineral which covers majority of area
after goethite(G) by its area wise distribution. It covers around 24% area as a whole. Ferruginous clay are
grains of minerals which are very fine in size, mainly less than 5 micron to sub microscopic in size which
occur as patches of variable sizes and shapes. Maximum size of the ferruginous clay patches is around
100 micron. All patches are in close association with other mineral grains by their margins. None of the
patch of this gangue is in free-state.(Fig. 3, 6, 7 and 8).
3.3 Mineral inter-locking & Liberation studies
The ‘as received’ sample shows very critical mineral interlocking and does not show clear trend. Major
ore mineral is hematite covering approximately 20% of the total area, followed by goethite and limonite
which covers around 32% and 12% areas respectively.
As a whole, with respect to the original hematite distribution i.e. 20%, around 7% grains are in free-state
whereas remaining 13% grains are in un-liberated state. Among the free grains i.e. 7%, around 3% grains
are in 1000 to 30 micron size whereas remaining 4% free grains are in less than 30 micron size.
537
Mineralogical characterization
Among the un-liberated grains i.e. 13%, around 7% un-liberated grains are in 1000 to 30 micron size
whereas remaining 6% grains are in less than 30 micron size. Liberation of these coarse to medium size
un-liberated grains would be possible at less than 100-75 micron size. Among the goethite mineral
distribution i.e. 32% area wise, with respect to original mineral distribution, around 11% grains are in
liberated state whereas remaining 21% grains are in un-liberated state. Among these liberated grains, only
around 2% grains are in 350 to 30 micron size whereas, remaining 9% grains are in less than 30 micron
size. Among the 21% un-liberated grains, only around 7% grains are in 350 to 30 micron size whereas
remaining 14% grains are in less than 30 micron size and liberation of these un-liberated grains would be
possible at less than 35-20 micron size.
Among the 12% limonite grain distribution, around 4% grains are in free-state and remaining 8% grains
are in un-liberated state. Among the 4% free grains, around 1% grains are in 130-30 micron size whereas
remaining 3%grains are in less than 30 micron size. Among the 8% un-liberated grains, around 3% grains
are in 130-30 micron size and remaining 5% grains are in less than 30 micron size. Among the un-
liberated grains, most of the coarse to medium size grains liberation would be possible at around 70
micron size whereas small size grains liberation would be possible at less than 20 micron.
Among the quartz distribution i.e. 8% area wise, with respect to original mineral distribution, around 3%
grains are in fully liberated state whereas remaining 5% grains are in un-liberated state. Among these
liberated grains only around 1% grains are in 130 to 30 micron size whereas remaining 2% grains are in
less than 30 micron size. Among the 5% un-liberated grains, around 2% grains are in 130 to 30 micron
size whereas remaining 3% grains are in less than 30 micron size and liberation of these coarse to
medium size un-liberated grains would be possible at less than 20 micron size. Pseudo ore covers around
4% area as a whole. None of the pseudo ore mineral is in free-state. All pseudo ores are masked by other
ultrafine ore and gangue minerals. Other gangue mineral present in the sample is ferruginous clay, which
covers around 24% area as whole and occurs as less than 100 micron size patches. None of the
Ferruginous Clay is in free-state. Summary of mineralogical and mineral liberation studies were presented
in table 3.
3.4 Photomicrographs
Photomicrographs exhibiting various features goethite rich iron ore under transmitted light and reflected
light at different magnifications were taken and the same were presented in figures 3 to 8.
538
Mineralogical characterization
539
Mineralogical characterization
Table 3: Summary of mineralogical study of goethite rich iron ore sample.
Overa
Lib Un- %, Un-
ll %,
Ore/ er- liber Distri liberat
Distri Distri
Gangu Area Fully ate a- b- ed
b- bu-
e Grain Size (µ) Cover Liberated d ted ution Gangu
ution, tion
Minera s (%) Grains (%) Gra grai Unlib. e size
Area (wrt
l ins ns Grain (micro
wise om)
(%) (%) s n)
(%)
1000- 1000- 3
Coarse 8 1.60 0.5 70 1.1 < 650
100 µ 100 µ 0
Hematit Mediu 100-30 100-30 3
20 40 8.00 2.6 68 5.4 < 75
e (H) m µ µ 2
4
Small <30µ 52 10.40 <30µ 4.2 60 6.2 < 20
0
350-100 350-100 1
Coarse 5 1.60 0.2 90 1.4 < 180
µ µ 0
Goethit Mediu 100-30 100-30 2 1.7
32 22 7.04 75 5.3 < 35
e (G) m µ µ 5 6
3 8.8
Small <30µ 73 23.36 <30µ 62 14.5 < 20
8 8
130-100 130-100 1 0.0
Coarse 5 0.60 85 0.51 < 70
µ µ 5 9
Limonit Mediu 100-30 100-30 3 1.0
12 28 3.36 70 2.35 < 50
e (LIM) m µ µ 0 1
3 2.8
Small <30µ 67 8.04 <30µ 65 5.23 < 20
5 1
130-100 130-100 1
Coarse 10 0.80 0.1 85 0.7 < 70
µ µ 5
Quartz Mediu 100-30 100-30 3
8 30 2.40 0.8 65 1.6 < 75
(Q) m µ µ 5
4
Small <30µ 60 4.80 <30µ 1.9 60 2.9 < 20
0
Pseudo
N
Ore 4 Small <70µ 100 4.00 <70µ Nil Nil Nil < 20
il
(PSO)
Ferrugi Occurs as patches of
n-ous N variable shapes and
24 Small <100µ 100 24.00 <100µ Nil
Clay il sizes in close association
(FCL) with other minerals.
4. Conclusions
The ‘as received’ sample is showing characteristics of low to moderate grade ore which comprises of
hematite, goethite and limonite as ore minerals and quartz, pseudo ore and ferruginous clay as gangue
minerals. Ore minerals distribution is around 64% as a whole and gangue minerals distribution is around
36% area as whole. Main ore mineral is hematite with 20% area out of which around 7% grains are in
540
Mineralogical characterization
free-state and remaining 13% grains are in un-liberated state. Around 6% un-liberated grains could be
liberated at around 75 micron size. Remaining un-liberated grains are in less than 20 micron size.
Goethite covers around 32% area as a whole out of which around 11% grains are in free-state and
remaining 21% grains are in un-liberated state. Around 6% un-liberated goethite can be liberated at
around 35 micron size whereas remaining 15% un-liberated grains can be liberated at less than 30 micron
size. Limonite covers around 12% area, out of which around 4% grains are in free-state and remaining 8%
grains are in un-liberated state. Among the un-liberated grains, around 3% grains liberation could be
possible at around 70 micron size whereas remaining 5% grains liberation would be possible at less than
20 micron. Quartz grain which is the main source of silica in the ‘as received’ sample covers around 8%
area as a whole, shows around 3% free Quartz grains whereas remaining 5% grains are in un-liberated
state. Out of these 5% un-liberated grains, around 3% grains could be liberated at around 70 micron size
and remaining 2% grains at less than 20 micron size. None of the pseudo ore and ferruginous clay are in
free-state. Liberation of these grains would be possible at less than 10 micron size. As a whole, around
80% ore minerals could be liberated at around 100-70 micron size.
Acknowledgements
The authors wish to thank Shri Narendra Kothari, Chairman cum Managing Director, NMDC Limited and
Shri Narendra Kumar Nanda, Director (Technical), NMDC Limited for approval to conduct studies and
permitting to publish this paper.
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Mineralogical characterization
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Eastern India; Econ. Geol. 72 90–98.
Chakraborty K L and Majumder T 2002 Some important aspects of the banded iron formation (BIF) of
eastern Indian shield (Jharkhand and Orissa); Indian J. Geol. 74(1–4) 37–47. Crookshank H, 1963,
Geology of southern Bastar and Jaypore from the Bailadila Range to the Eastern Ghats: Geological
Survey of India Memoir 87. p.50.
Roy Subrata and Venkatesh A S, Mineralogy and geochemistry of banded iron formation and iron ores
from eastern India with implications on their genesis, J. Earth Syst. Sci. 118, No. 6, December 2009, pp.
619–641
Gopinath P, Mohan S P and Magendran T, Structural, Mineralogical and ore grades of Banded Iron
deposits of North Western Tamilnadu, South India – A Comparative study, International Journal of
Emerging technology and Advanced Engineering, Volume 5, Issue 3, March 2015, pp 78-83.
Bhattacharya H N, Indranil Chakraborthy and Kaushik K Ghosh, Geochemistry of some banded iron
formations of the archean supracrustals, Jharkhand – Orissa region, India, Journal of Earth System
science Volume 116, Issue 3, June 2007, pp245-259.
Subrata Roy and A. S. Venkatesh, Mineralogy and Geochemistry of banded iron Formation and iron ores
from eastern India with implications on their genesis, Journal of Earth System Science, December 2009,
Volume 118, Issue 6, pp 619-641.
Nirlipta P Nayak, Mineralogical Constraints in beneficiation of Low grade Iron ores of Barsua, Eastern
India, International Journal of Engineering and Innovative technology, Volume 3, Issue 5, November
2013, pp109-113
Prasad K S S, D B Shankar and Y V Reddy, Geochemistry and Origin of Banded Iron formation from the
granulitic terrain of North Arcot district, Tamil Nadu, South India, Chemical Science Transactions, 2012,
Volume 1, issue 3, pp 482-493.
Manikyamba,C (1998) Petrology and geochemistry of mixed oxide-silicate facies banded iron formations
from Sandur schist belt, India. J.Geol.Soc.India 52, 651-661.
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Mineralogical characterization
Manikyamba,C and Naqvi,SM (1995) Geochemistry of Fe-Mn formations of the Archaean Sandur schist
belt, India - mixing of clastic and chemical processes at a shallow shelf. Precambrian Research 72, 69-95.
543
Mineralogical characterization
BAUXITE MINERALOGY AT MOMBI DEPOSIT SW IRAN
Abstract
The Mombi bauxite deposit is located in 165 km northwest of the Dehdasht city in the southwestern Iran.
From the bottom to top, the deposit is generally consisting of brown, gray, pink, pisolitic, red, and yellow
bauxite horizons. Boehmite, diaspore, kaolinite, andhematite are the major mineral components accompanied
by gibbsite, goethite, anatase, rutile. The brown and gray bauxites are characterized by the presence of some
textural elements, like spherical features, clay minerals and pyrite in the matrix. The spherical grains are
often pisoids and ooids with various shapes and sizes. Microscopic observations show spheroidal pisolites
with a boehmite core surrounded by a cortex of alternating hematite. In these horizons porous matrix filled
with calcite and fracture filled by kaolinite. The main textures of the brown and gray bauxites are including
pisolitic-ooide and ooide-spherical along with a pelitomorphic and microgranular matrix. The pink bauxite
layer at some parts of the profile consists of ooids and pisoliths of clay minerals. This layer characterized by
an increase in abundance and size of the pisolitic particles upwards. The main textures of the pink bauxite
include pisolitic-ooide, pelitomorphic and pisolitic along with a pelitomorphic and microgranular matrix. The
pisolitic bauxite layer with about 1 m thickness, containing pisolitic particles, has a boundary with the pink
bauxite. The pisolite grain size in this layer is larger than other bauxite layers. The main texture of the
pisolitic bauxite includes pisolitic grains along with a panidiomorphic matrix. The red bauxite contains iron
oxides, ooids with various shapes and sizes, and characterized by a decreasing in abundance of the pisolitic
particles. The main texture of the red bauxite includes oolitic–pisolitic along with a microgranular matrix.
The yellow bauxite layer contains oolitic particles and clay. Lack of pisolite particles is the important change
from the red bauxite to yellow bauxite layer. The main textures of the red bauxite include ooide-spheroid,
pelitomorphic and oolitic along with a microgranular matrix.
1. Introduction
Bauxite deposits are derived from alteration and chemical weathering of parent rocks which are rich in
alumosilicate minerals. Genetic models, mass changes, elements mobility and ore textures of bauxite deposits
544
Mineralogical characterization
in the world were studied by a number of authors (e.g., Bárdossy, 1982; Bardossy and Aleva; 1990). Some
studies have recognized a various range of ore textures such as oolitic, pisolitic, bedded and massive as well
as different genetic models like high and low level bauxites, laterite, tikhvin-types, and karst-type for bauxite
deposits (Bardossy and Aleva, 1990; Zarasvandi et al., 2010). The Mombi deposit is situated in the
southwestern Iran (Fig. 1a). Generally, karstification was a key diagenetic process that affected the formation
of bauxite deposits in the upper Sarvak carbonates. The bauxite horizon consists of a series of lenticular
bodies measuring 3 to 40 m in length and 75 cm to 9 m thick. The studied bauxite horizons in Mombi is
commonly consisted of (from top toward the bottom), (a) a yellow bauxite layer, (b) a red bauxite layer, (C) a
pisolitic bauxite layer, (D) a pink bauxite layer, (E) a gray bauxite layer, and (F) a brown bauxite layer (Fig.
1b). The brown and gray ores are characterized by the presence of some textural elements, like spherical
features, clay minerals and pyrite in the matrix. These layers with about 3 m thickness are situated on top of
the upper part of the sarvak limestone. The pink bauxite layer with approximately 1.5 m thickness is overlain
by pisolitic layer. The pink ores at some parts of the profile consists of ooids and pisoliths of clay minerals.
The pisolitic bauxite layer with about 1 m thickness, containing pisolitic particles, has a boundary with the
pink bauxite. The pisolith grain size in this layer is larger than other bauxite layers. The red layer with
approximately 1.5 m thickness covered pisolitic layer. This bauxite layer contains iron oxides, ooids with
various shapes and sizes, and characterized by a decrease in abundance of the pisolitic particles. The yellow
bauxite layer with about 1 m thickness is located in the upper part of the bauxite profile. The presence of the
oolitic particles and clay minerals are the most important characteristics of the yellow ores.
545
Mineralogical characterization
Figure 1: a) Study area and b) stratigraphic column section of the Mumbi bauxite deposit showing
different bauxite horizons.
The main textures of the different layers in the Mombi deposit include oolitic-pisolitic, ooide-spherical along
with a microgranular and pelitomorphic matrix (Fig. 2a and 2b). The spherical grains in the Mombi bauxite
include eooids and pisoids, which are important components in most ore samples. The presence of ooids and
pisoids within the ores can be attributed to the original heterogeneity of the initial colloids that were derived
from alteration and weathering of parent rocks. Microscopic observations show that the fractures within the
spherical grains of the ores can be classified in two different forms. Some of them are in irregular and radial
shapes and are often limited to within a component whereas some others cross the border of grains and
extend into the matrix. Various fractures, veinlet sand, joints are filled with materials such as kaolinite and
calcite (Fig. 2c and 2d).
546
Mineralogical characterization
Sample
Rock Major minerals Minor minerals Matrix Texture
no.
Quartz, Kaolinite,
SR-1 Sarvak Formation Calcite - Biomicritic
hematite, Montmorillonite
AL-1 Argillic limestone Calcite, kaolinite Quartz, goethite Micritic Biomicritic
547
Mineralogical characterization
Figure 2: a) Oolitic-pisolitic texture, b) ooide-spherical texture, c) fractures within the spherical grains, d)
fractures and joints are filled with materials such as kaolinite and calcite.
References
Bárdossy, G., 1982. Karst bauxites. Bauxite deposits on carbonate rocks. Dev. Econ. Geol., 14. Elsevier,
Amsterdam. 441 pp.
Bárdossy, G., Aleva, G.J.J., 1990. Lateritic Bauxites: Developments Economic Geology 27. Elsevier,
Amsterdam. 624 pp.
Chen, Q., Zeng, W., Chen, X., Gu, S., Yang, G., Zhou, H., Yin, Z., 1995. Investigation of the thermodynamic
properties of γ-Al2O3.ThermochimicaActa 253, 33–39.
Gu, J., Huang, Z., Fan, H., Jin, Z., Yan, Z. and Zhang, J., 2013. Mineralogy, geochemistry, and genesis of
lateritic bauxite deposits in the Wuchuan–Zheng'an–Daozhen area, Northern Guizhou Province, China.J.
Geochem. Explor.130, 44–59.
548
Mineralogical characterization
Peryea, F.J., Kittrick, J.A., 1988. Relative solubility of corundum, gibbsite, boehmite, and diaspore at
standard state conditions.Clays and Clay Minerals 36, 391–396.
Zarasvandi, A., Zamanian, H., Hejazi, E., 2010. Immobile elements and mass changesgeochemistry at Sar-
Faryab bauxite deposit, Zagros Mountains, Iran. J. Geochem. Explor.107, 77–85.
549
Mineralogical characterization
MINERALOGICAL AND GEOCHEMICAL EVOLUTION OF THE BAUXITE ORES FROM
GADHSISA GROUP OF MINES, KACHCHH, GUJARAT, INDIA
Abstract
Various bauxitic and lateritic samples were collected from drill cores, profiles (~2m depth) and surface in the
study area. Thorough field observations and mineralogical and geochemical analyses are carried out to
understand the process of lateritization and bauxitization. In the Permian lateritization and bauxitization, due
to highly mobile nature of alkali metals(K,Na) and alkaline earth metals(Ca,Mg) are removed from the parent
rocks during intense chemical weathering. Elements with a low mobility (Ti, Zr) are positively correlated
with Al. Mobility of the elements affected by intensity of leaching and drainage condition present in the
localization of bauxite deposits. Alumina(Al) is enriched by the removal of ferric (Fe) and silica (Si)
impurities from the bauxite profiles when exposed to surface. Mineralogical study reveals that gibbsite
(Al(OH)3) occurs as the major mineral and ranges between 76-87 vol.% with minor amount of boehmite (γ-
AlO(OH)) and diaspora (α-AlO(OH)) in the bauxite ore . Geochemical analysis yields Al2O3 (47-69wt.%),
Fe2O3 (3-21wt.%), SiO2 (3-12wt.%) with minor concentration of TiO2(rutile, anatase), CaO, MgO, Na2O,
K2O etc. Clay mineral like kaolinite was found to be present predominantly. The intensity of the leaching
process and the drainage conditions plays a major role in the enrichment of bauxite ore.
1. Introduction
Deccan Trap basalts of Kachchh region given rise to lateritic bauxite as one the major economic mineral in
the state of Gujarat. The lateritic bauxites occur mostly in tropical countries. They were formed by the
process of lateralization of basaltic parent rock under intense weathering conditions with very good drainage.
A detailed account of petrographic and mineralogical studies revealed the ore minerals in bauxite comprise of
hydrated aluminous oxide: gibbsite [Al(OH)3], boehmite [γ-AlO(OH)] and diaspore [α-AlO(OH)]. All three
550
Mineralogical characterization
are white when pure but always coloured by impurities in the natural state. Gangue minerals in bauxite
include iron oxides goethite and hematite, quartz (SiO2), anatase (TiO2) and water. Minor amounts of clay
mineral kaolinite, phosphate minerals, and unaltered bedrock are often present as contaminants.
2. Experimental Procedure
2.1 Study Area and Location
Extensive deposits of plant and non-plant grade bauxites are found in Gadhsisa group of mines in Kachchh
district. The study area is located between latitudes of 23°0'N to 23°13'N and longitudes of 69°11'E to
69°23'E. To the west of Ghadshisa lies Arabian sea and Mandvi beach is located at a distance of 20Km from
Ghadsisa. Kachchh railway station is around 200Km from the Ghadsisa region.
551
Mineralogical characterization
The samples of bauxite, associated clay and the host rock collected from eight working mines owned by
GMDC (Gujarat Mineral Corporation Development). Sample collected from various mines with prior
permission from GMDC(personal communication) include: Roha Kotada Jarjok Bauxite mine, Wandh
Bauxite mine, Naredi Nandra Bauxite mine, Daban - Wamoti Bauxite mine, Naredi-II Bauxite mine,
Mothala-Balachod Bauxite mine, Goniasar Bauxite mine and Ratadia-Nagrecha Bauxite Mines. All the mine
locations from where samples were collected has been shown in the geological map (Fig.1) (after
Biswas,1992). Opencast mining method is followed in all the mines to extract bauxite ore by drilling and
blasting. Sorting and stacking (Ref. Plate-1A-2) of ore is done by hand picking method. Hydraulic excavators
and trippers are used for transportation of ore minerals and waste materials during mining. Various other
important equipment like, dozer, water tanker and motor grader are used to keep the mine working.
Kachchh region is divided into various zones like coastal zone occurring along the south, Kachchh mainland
with hill ranges in the north, the Great Rann (North) and the Little Rann(East) comprising saline wasteland.
Mostly sedimentary rocks from Jurassic to Eocene age occur in the Kachchh area. Deccan trap volcanics
occur in these sediments found intercalated between Jurassic rocks of the northern part and Eocene sediments
in coastal belts of south. Most common rock types in Kachchh include limestone, sandstone and shale
(Krishnan, 1982). In the North, mainly Jurassic rocks are exposed and in the southern fringe, Eocene rocks
are found. Thick alluvium occurs in kachchh peninsula towards coast due to marine recession. In southern
part of the Kachchh peninsula, mainly Deccan Traps are exposed. Mesozoic rocks of Kutch occur along the
E-W trending ridges have been divided into various formations like Patcham(300m), Chari(400m),
Katrol(750m), Umia(550m) and Bhuj Formation. Marine transgression found to occur in Pathcham formation
and there is occurrence of fossils of ammonites in Chari Formation. In the Deccan trap, there is extensive
occurrence of basalt flows which has given rise to bauxite due to weathering under optimum paleoclimatic
conditions. The bauxite deposits are associated with laterites which separated underlying Deccan traps from
overlying Tertiary. Tertiary sequence of western Kachchh is given in (Fig. 2) (Biswas,1992).
3. Methodology
Various bauxite samples associated with clay minerals as well as its basaltic host rocks were studied by
preparing its thin section for petrographic and textural studies. Doubly polished thin sections (0.3 to 0.5mm)
and polished thick sections (around 10 mm) of each sample were prepared. Using X-ray Diffraction
technique and quantitative mineralogy of these bauxites have been made.
552
Mineralogical characterization
553
Mineralogical characterization
Optical properties of the samples were studied both under transmitted and reflected light using various
petrological microscopes like Leica Microscope, Leitz Microscope and Nikon Microscope. Common textures
found in the bauxitic sample under transmitted light, show oolitic and pisolitic textures (Ref. Plate-1B-3).
Important metallic phases like hematite and goethite are disseminated throughout the oolitic and pisolitic
bauxites. Big altered oolitic grains are surrounded by small grains. Larger oolites are observed in many
samples. At places there is association of iron oxides like hematite, goethite with bauxite as replacement
texture (Ref. Plate-1B-4). Iron oxides found to occur along the irregular fractures replacing bauxite. Irregular
inclusions of hematite occur along concentric zones of oolites. Concentration of metallic minerals found to
be very less inside oolitic grains than in the matrix. Commonly observed oolitic and pisolitic textures of
gibbsite occur in the clay minerals. There is preservation of basaltic textures in some samples with presence
of altered plagioclase feldspar grains disseminated in the matrix as well as in the oolites(Ref. Plate-
1D).Crosscutting tiny vein like structures of iron oxide occur in some lateritic bauxite samples.
1 2 Top Soil 3
(Alluvium)
Bauxite
Laterite Core STACKIN
G Lithomarge
4 5 6
Top Soil (Alluvium)
Plate-1A Field photographs from Kachchh. 1 - Laterite core sample at field. 2 - Stacking of Bauxite ores
done by sorting and sizing of the ores by hand picking method. 3 - Alluvium at the top layer followed by
high grade bauxite in the middle layer with lithomarge clay at bottom observed at Ratadia Mine. 4 - Top
554
Mineralogical characterization
layer with alluvium over burden due to marine transgression and then followed by bauxitic layer (Daban
Mine). 5 - Reddish outcrop represents laterite occurrence at Wandh Mine. 6 - Very high grade laterite
observed at field (Goniassar Mine)
1 2 3
4 5 6
Plate 1B (scale: 500px).Photomicrographs of bauxite ores from Kachchh. 1 -Thin section under reflected
light showing occurrence of hematite (white) in the interstial space between bauxite ooids (Balachod Mine).
2-Thin section under reflected light showing irregular, interconnected fractures on the large bauxitic grain
with minor occurrence of goethite (light grey) in the periphery (Balachod Mine).3-Thin section under
reflected light showing oolitic, pisolitic textures of bauxite (Balachod Mine). 4- Thin section under reflected
light showing occurrence of hematite (white) on the big bauxitix ooid as well as in the periphery. This shows
replacement texture where hematite replaced gibbsite (Naredi Mine). 5- Thin section under reflected light
showing distinct growth of goethite (bluish grey) along the periphery of the bauxite (Naredi Mine). 6- Thin
section under reflected light showing interconnected fractures are filled with hematite (white) in bauxite
(Naredi Mine).
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Mineralogical characterization
7 8 9
10 11 12
Plate 1C (scale: 500px).Photomicrographs of bauxite ores from Kachchh.7 - Thin section under reflected
light showing occurrence of hematite along the periphery of the oolitic grain in a concentric manner and the
goethite (grey) occurs irregularly surrounding the bauxitic oolite (Daban Mine). 8 - Thin section under
reflected light showing a distinct big fracture with precipitation of hematite and goethite along it (Roha-
Kotada Mine). 9 - Thin section under reflected light showing big oolitic grain where goethite(light grey)
occur almost over it. 10 - Thin section under reflected light showing concentric zoning in oolitic grains
(Roha-Kotada Mine). 11 - Hematite occurring between the oolitic grains as well as occurrence of iron oxide
(black) within the grain (Daban Mine). 12 - Big gibbsitic oolite in the ferruginous matrix (Ratadia Mine).
The use of radioisotope XRF for the analysis of major and minor elements in bauxite material has been found
to be accurate and precise. The technique and the instrumentation have been found to be reliable. In terms of
bauxite exploration this technique is therefore highly recommended, as it requires little sample preparation
and the added advantage of the speed of processing results when compared to that of wet chemical methods.
Each sample was ground into powder using mortar and pestle and screened until all material passed through
556
Mineralogical characterization
the screen of mesh aperture 200 mm (0.074 mm or 74 microns). The samples were oven dried at 105°C until
a constant weight is obtained for each sample. The sample is then pressed into a pellet of 25mm diameter by
mixing 4.0 g of the powdered sample with cellulose powder in a 1:4 weight ratio using SPEDAC hydraulic
press at a pressure of 15 tons. The cellulose serves dual purposes as a binder and also reduces absorption of
the target material. All the samples were analyzed (at XRF lab in SAIF,IITB) with respect to the international
standard of Darling Range Bauxite -206 B600,NIST-696 Suriname bauxite standard and Pune Bauxite
standard. Alumina contents of most samples are of commercially recommended level and good enough for
aluminum production.
Table 1. Major and minor oxide composition of bauxite samples analyzed by XRF(%)
Table 2. Major and minor oxide composition of bauxite samples analyzed by XRF(%)
557
Mineralogical characterization
P2O5 0.205 0.199 0.123 0.125 0.105 0.104 0.049 0.038
SiO2 18.306 17.482 0.314 0.457 5.633 6.007 3.050 4.067
TiO2 3.705 3.483 4.353 4.387 3.244 3.312 1.359 1.328
ZrO2 0.033 0.037 0.172 0.172 0.086 0.090 0.055 0.051
SO3 0.094 0.098 0.208 0.239 0.087 0.087 0.094 0.096
LOI 27.475 32.011 33.508 31.067 26.245 26.534 31.324 30.802
Sum 99.957 99.940 100.002 98.717 99.901 99.850 99.941 99.861
Table 3. Major and minor oxide composition of bauxite samples analyzed by XRF(%)
Table 4. Major and minor oxide composition of bauxite samples analyzed by XRF(%)
558
Mineralogical characterization
ZrO2 0.021 0.016 0.077 0.073 0.047 0.053 0.071 0.067
SO3 0.080 0.083 0.087 0.087 0.089 0.092 0.092 0.126
LOI 33.367 30.023 34.432 30.598 22.412 20.825 35.002 34.437
Sum 100.085 98.842 99.888 99.899 99.995 99.999 99.998 99.842
Table 5. Major and minor oxide composition of bauxite samples analyzed by XRF(%)
Table 6. Major and minor oxide composition of bauxite samples analyzed by XRF(%)
559
Mineralogical characterization
Sum 99.982 100.030 101.128 99.509 101.268 98.672
4. Conclusion
560
Mineralogical characterization
Deccan Trap eruption during Upper Cretaceous to Paleocene time in western margins of India has given rise
to basaltic flows in Kachchh region which is a pre-cratonic rift basin mainly comprised of sediments from
middle Jurassic to Recent (Biswas, 1971). According to Calvo et al. (1999), NE to SW trending basaltic
layers of Kachchh has undergone several phases of subsidence followed by marine transgression and
regression, which has led to the formation of a complete tertiary sequences in the western part of the
Kachchh region. Around eight mines were visited for the study of the bauxite ores. Bauxite ores occur above
the basaltic parent rock. The Ratadia mine falls in coastal zone. Daban, Goniassar, Wandh and Roha-Kotda
occur in the boundary between coastal plain and upland. Naredi, Nandra and Balachod Mines fall in to the
upland region. Ore petrography and quantitative mineralogical study of all the bauxite samples collected
from the field are done using various analytical techniques. Bauxite mainly occurs due to the extensive
weathering of the basaltic parent rocks under optimum rainfall and paleoclimatic conditions. Many fine sized
ore minerals are not identifiable under microscope. Most of the thin sections under reflected light show grey
colour of different shades. Again the study of the samples under transmitted light and/or reflected light and/or
under both lights, helped to identify them. Oolitic and/or pisolitic textures are shown by most of the bauxitic
as well as lateritic samples from all the mines under transmitted light as well as in reflected light (Ref. Plate
1B and 1C). Ore petrographic study revealed the presence of two main metallic phases like hematite (Fe 2O3)
and goethite (FeO.OH) which are disseminated throughout the oolitic and/or pisolitic structured bauxite
sections (thick/thin). Iron oxide also occurs along the fractures as well as along the concentric rings of
oolites. Iron oxides also occur as cementing materials. At some places there is iron oxides i.e. hematite
(white) and goethite (light grey) found associated with bauxite. At places replacement textures were seen,
where bauxitic minerals were being replaced by goethite and hematite along fractures, cavities and irregular
veinlets. In some samples basaltic texture are observed along with the presence of relict and less weathered
plagioclase feldspar laths. This occurrence of relict texture reveals basalt as its parent rock. In some samples,
absence of basaltic texture may be due to complete decomposition of basalt to kaolinite and gibbsite. The
XRD analysis confirmed, gibbsite occur as the major bauxitic mineral in all the mines with minor
concentration of boehmite, diaspore and anatase (TiO2). Clay mineral like kaolinite also detected at various
mines. In some mines also calcite has been observed which indicates the presence of limestone association
with basaltic parent rocks. Clay mineral like kaolinite also found to occur in many places. There are two
zones observed in the field associated with bauxitic profile; alucrete zone which is mainly Al dominant and is
the source of high grade bauxite and another ferricrete zone which mainly contains Fe as dominant element
with little occurrence of Al associated with it, giving rise to lateritic formations (Plate-1A-5). Replacement
561
Mineralogical characterization
textures occur due to diagenetic transformation in saprolite transition zone where hematite and goethite
replace the bauxitic minerals. As Fe is more mobile than Al, so the iron is leached out faster giving rise to an
Al rich Alucrete layer which is whitish high grade bauxite (Plate-1A-3). The diagenetic transformation in the
alucrete zone was characterized by the texture changing from relict to deformed, vesicular and brecciated
texture. Changes in mineralogy due to diagenetic change may have caused separation of Si, Al, Fe and
enhanced deposition of gibbsite. The basaltic parent rock mainly contains plagioclase feldspar. In the process
of weathering of the feldspar, the leaching of Si from feldspar given rise to kaolinite and further removal of
Si from kaolinite produced gibbsite (Al rich) as the dominant mineral. Due to weathering process through
solution, basalt changes to saprolite, ferralite and bauxite as stated by Jadhav et al. (2012). According to
Calvo et al. (1999), during the lateral textural evolution the massive hard bauxite- rich in iron, changed in the
seaward direction into yellow to white bauxite- relatively poor in iron with a bolder like structure. Similarly
hard and red coloured bauxites (lateritic bauxites) found in the Ratadia mine was due to iron concentration in
comparison to the white and pinkish white bauxite in the Roha-kotda mine. Concretions or nodules were
found in the in gibbsitic matrix.
The ores are mainly composed of Al2O3 (35.45–74.56 wt.%), SiO2 (0.15–18.57wt.%), Fe2O3(0.2–21.6 wt.%),
and TiO2 (1.3–7.8 wt.%) with LOI ranging from 15.7 wt.% to 38.3 wt.%. Alkalis and alkali earth elements
show low values, probably because these elements are highly mobile and are usually leached out during
chemical weathering. The enhanced Fe2O3contents in the lower horizon are attributed to the presence of iron
minerals like hematite and goethite formed under suitable Eh–pH conditions during the lateritic weathering
processes. Among the major elements, Al2O3 and TiO2showed the highest positive correlation, while Al2O3
and SiO2 display a negative correlation (Fig. 4 and Fig. 5). These patterns are consistent with leaching of
silica and residual enrichment of aluminum and titanium during chemical weathering. The triangular
variation diagrams of Al2O3–SiO2–Fe2O3 are commonly used to show the degree of lateritization, mineral
control and bauxite classification. Based on the mineralogical classification of Aleva (1994), most of the
bauxite samples in the studied areas fall within the bauxite and kaolinitic bauxitefields (Fig. 3). Calvo et al.
(1999), also pointed out that in near coastal areas with the subsiding tendency during bauxitisation a special
pisolitic and boehmite-diaspore facies occur. Below ground water table Eh and pH condition is low, so Fe is
more soluble than Al which enhances weathering of plagioclase feldspar found in the basalt by giving rise to
pisoliths composed of gibbsite and kaolinite.
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Mineralogical characterization
Acknowledgement
PSC is thankful to all the Mine managers and geologists especially Vijay Sumera at GMDC for their help in
carrying out geological field work and collecting samples. I am thankful to staffs of XRF Lab in SAIF,IIT-B
to carryout geochemical analysis of all the representative bauxite samples collected from the study area.I am
thankful to Vengu Lekar in sample preparation lab of Earth Sciences Department,IIT bombay for his constant
support to make thin section slides.
References
BALASUBRAMANIAM, K.S. (1987) Geomodelling of certain bauxite profiles from Kutch, Gujarat state,
India. In: Y. Ognra (Ed.), Proc. Internat. Sem. Laterite, .Tokyo, Japan. Chem. Geol., v.60, pp.121-130.
BALASUBRAMANIAM, K.S. and SABLE, S.G. (1976) Mineralogy, geochemistry andgenesis of certain
bauxite profiles from Kutch Dist., Gujarat. Proc. Symp. Deccan Traps and Bauxite, no.14, pp. 225-242.
BALASUBRAMANIAM, K.S. and NAMDAS, N.R. (1978) Geology and geochemistry and genesis of
sediments from Panandhro basin, Madh series, Kutch dist., Gujarat state. Mines Metals Fuels, pp.384-386.
BISWAS, S.K. (1971) Note on the geology of Kutch. Quart. Jour. Geol. Min. Metal. Soc. India, v.43,
pp.223-235.
BISWAS, S.K. (1992) Tertiary stratigraphy of Kachchh. Jour. Palaeont. Soc. India, v.37, pp.1-29.
CALVO, J.P., BLANC-VALLERON, M.M., RODRIGUEZ-ARANDIA, J.P., ROUCHY, J.M. and SANZ,
M.P. (1999) Authigenic clay minerals in continental evaporitic environment. Spec. Publ. Int. Assoc.
Sedimentologists, v.27, pp.129-151.
INESON, P.R. (1989) Introduction to practical ore microscopy. Longman Scientific and Technical, New
York, 181p.
JADHAV, G. N., SHARMA, N. and SEN, P. (2012) Characterization of Bauxite Deposits from Kachchh
Area, Gujarat. JOURNAL GEOLOGICAL SOCIETY OF INDIA Vol.80, September 2012, pp.351-362
KRISHNAN, J. (1987).An overview of the Mesozoic stratigraphy of Kachchh and Jaisalmer basins.
JOURNAL OF THE PALAEONTOLOGICAL SOCIETY OF INDIA VOL. 32, 1987, pp. 136-149.
ROBB, L. (2005) Introduction to ore forming processes. Blackwell Science Ltd. UK, 373p.
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MECHANISTIC MODELING OF AIR CORE IN HYDROCYCLONE
Chandranath Banerjee1*, Emmanuel Cid2, Eric Climent3, Florent Bourgeois2 and Arun Majumder1
1
Department of Mining Engineering, Indian Institute of Technology Kharagpur, Kharagpur, India
2
Laboratoire de Génie Chimique - Université de Toulouse, CNRS-INPT-UPS
Allée Emile Monso, BP 44362, 31432 Toulouse Cedex 4, France.
3
Institut de Mécanique des Fluides – Université de Toulouse, CNRS-INPT-UPS,
Allée Pr. Camille Soula – 31400 Toulouse, France.
*Corresponding author: for.chandramin@gmail.com
Abstract
Classification performances of a hydrocyclone are greatly influenced by the air core shape and
diameter. This study demonstrates the phenomenological characteristics of air core in a hydrocyclone
through a shadowgraph measurement technique. The oscillating nature of air core along the axial
direction has been quantified based on the image processing to detect the interface boundary.
Experimental observations of air core diameter exhibit oscillating nature throughout the cylindrical
and conical sections of hydrocyclone. Unexpectedly, the magnitude of oscillations is relatively higher
in conical section in comparison to that of cylindrical section. Moreover, this study offers an
approximated analytical solution of swirl flow behaviour for a viscous incompressible fluid to get a
general scaling relationship of air core diameter under a wide range of inlet Reynolds number. For
validation purposes, both concurrent experimental data and pertinent data from reported literature have
been used. Here, the theoretical model predictions versus the air core measurements leading to the
conclusion that the proposed model gives a conservative air core diameter but not definite towards the
modelling of the air core oscillating and elevation dependent shape. The oscillations can be forced by
several physical mechanisms, for example, by pressure fluctuations introduced into the hydrocyclone
through the feed. In this work, a relevant physical source of oscillations has been quantified by the
propagation of inertial waves induced in the air-water interface boundary through the principle of
Rankine vortex flow hydrodynamic.
1. Introduction
Understanding the role of the air core for analysing the hydrocyclone performance is an active research
domain in various engineering disciplines. It is worth emphasizing that the geometry of the air core is a
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Modelling & Simulation
significant parameter that characterizes the operational state of hydrocyclone (Ovalle and Concha, 2005;
Neesse et al., 2004; Concha et al., 1996). Inside the hydrocyclone, swirling motion is generated by the
tangentially introduced fluid which creates an air core along the axis, normally connected to the
atmosphere through the spigot opening. This phenomenological behaviour depicts that the axial position
of the air core diameter may have been related to the fluctuating operating conditions at the inlet. In-depth
review of the inherent flow field inside a hydrocyclone reveals the existence of a force-vortex flow near
the central region and free-vortex flow otherwise (Banerjee et al., 2015; Yao and Fang, 2012; Wang et al.,
2007). In general, air core commonly occupies the forced vortex region and intensify the turbulence
fluctuation leading to a poor performance. Subsequently, due to the formation of air core, the effective
cross-sectional areas of the two exits of cyclones will be reduced which will limit the transport rate of
solid particles and water in the form of slurry through those exits. As a result inside the hydrocyclone at a
given operating condition, the collection rate of particles through the exits may be hindered because of
non-availability of sufficient passage. This means, the accurate prediction of air core diameter at a given
operating condition is to be understood thoroughly.
Over the past few years, intense research investigations motivated by application consequences, the role
of air core on hydrocyclone performance have been produced (Krishna et al, 2010; Hararah et al., 2010;
Neesse and Dueck, 2007). Direct air-core measurements along the axis of a hydrocyclone were first
carried out by Heish and Rajamani (1991). This measurement showed that the air core diameter was
found to be almost cylindrical in shape. With the advent of advanced Electric resistance tomography
(ERT) techniques, air phase fraction is quantified with good prediction accuracy inside a hydrocyclone
(Rakesh et al., 2014; Gutiérrez et al., 2000; Williams et al., 1999, 1997). Further development of
tomography measurement techniques like Electrical impedance tomography, gamma-ray tomography etc.,
researchers gained more accurate information on air core shape in a hydrocyclone operating with slurry of
different pulp concentration. Formation of air core, however, controls the fluid film thickness and the
underflow discharge profile as well (Neesse et al., 2004). Xu et al. (1990) and Sripriya et al. (2007)
reported that eliminating the air core by solid rod hydrocyclone efficiency could be improved. From an
opposite viewpoint, investigators (Evans et al., 2008) reported that the hydrocyclone efficiency could be
improved by eliminating the air core through solid rod.
Though many convoluted studies exemplify the air core features inside a hydrocyclone through
experimental measurements and mathematical models, still comprehensive descriptions on axial variation
of air core shape and the corresponding physical arguments are limited in literature. To address this
overlooked research problem, the present study attempts to determine the elevation-dependent shape of
air core through experimental and theoretical approaches. In this study, we explicitly demonstrate the
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Modelling & Simulation
shadowgraph measurement of air core in a classifying hydrocyclone as well as the experimental
observations of air core characteristics with varying operating and designed parameters. Apart from these
experimental analyses, the phenomenological features of air core have been quantified from mathematical
aspects of Rankine vortex flow inside the hydrocyclone. This section also validates the implication of the
theoretical model with present experimental observations and other data reported in published literature.
The shadowgraph measurement technique has been adopted for visualization and characterization of free-
surface flows. Figure 1 shows the schematic of shadowgraph setup. The design and operating parameters
for the present experiment are given in Table I.
Table 1: Hydrocyclone dimensions and range of operating pressure used in shadowgraph experiment.
Cyclone diameter (mm) Vortex finder diameter (mm) Spigot diameter (mm) Inlet pressure (kPa)
75 25 13,15 50,75,100,125
The shadowgraph measurement technique has been adopted for visualization and characterization of free-
surface flows. Figure1 shows the schematic of shadowgraph setup. The design and operating parameters
for the present experiment are given in table 1. The boundary of the core at the air-water interface has
been enumerated using segmentation image processing routines developed under MATLAB environment.
In order to get a clear vision of air core, the hydrocyclone was made of transparent plexiglass material
(fig. 1b) with refraction index of 1.48. In order to reduce optical distortions, the outer face of cylindrical
and conical part of the hydrocyclone was designed flat. Shadowgraphy technique involves a backlighted
arrangement for image acquisition.
(a) (b)
Figure 1: (a) Experimental arrangement of shadowgraph setup (b) Image acquisition during
shadowgraph measurement.
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Modelling & Simulation
A Phlox white LED flat panel was used as illumination source in conjunction with a CCD camera Imager
Intense from LaVision, equipped with a 50 mm objective lens, as shown in fig. 1b. Images of resolution
1376x1040 pixels with 12 bit dynamic range were acquired. Image exposure time was set to 135 µs to
ensure no blur effect induced by the movement of air core. Fig. 1a represents the shadowgraph set up and
fig. 1b represent image acquisition procedure for shadowgraph measurement
Cylindrical
section
Conical section
Figure 2: Time lapse snapshot of instantaneous shadowgraph images at different time with spigot
diameter 13mm and inlet flow rate 0.001054 m3 s corresponding to inlet pressure 125 kPa .
Figure 3: Calculation of calibration factors by corner detection procedure in the checkerboard pattern.
Following automatic corner detection procedure (Bouguet, 2004), as seen in fig. 3 calibration factors
could be calculated.
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Modelling & Simulation
The boundary of the core at the air-water interface appears on images as a darker region on a brighter
background (fig. 2). These high contrasted images are well suited for outer edge detection of air core. As
a pre-processing step, an image was acquired only for hydrocyclone full of water (without air core) as a
background image.
Figure 4: (a) Air water interface predicted through edge detected boundary by image analysis (b) Mean
air core diameter obtained from conversion of pixel unit to metric unit.
This background image is substracted from each instantaneous raw image in order to eliminate optical
defects principally visible in the lower conical part. Thus binarization is applied with automatic
thresholding and morphological operations such as opening and closing are performed on binary images.
The Matlab function “bwtraceboundary” is then used to trace the outline of the air core in the binary
image. In order to transform the air core diameter from pixel unit to metric unit, calibrated checkerboard
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Modelling & Simulation
patterns were inserted into the cylindrical and conical parts of the hydrocyclone filled with water at rest
and images were acquired without changing the focus compared to dynamic conditions.
Figure 4(a) shows the air water interface (in green colour) detected through boundary trace methods in
order to quantify the mean air core diameter. From the calibration factor as obtained from the
aforementioned procedure, we extract the value of air core diameter at different axial locations of the
hydrocyclone, at different operating conditions as mentioned in table 1. Figure 4 (b) is the elevation
dependent shape of air core diameter obtained through the shadowgraph measurement.
3. Experimental observations
After the detailed discussion of experimental procedures, the experimental observations of air core
characteristics have been discussed in this section. We investigate the characteristics of air core with
spigot diameter 13mm and 15mm in a 75mm hydrocyclone. The axial variations of air core morphology
for these two spigot diameters are depicted in figs. 5(a) and 5(b) for inlet pressure 50 kPa and 125 kPa
respectively.
(a) (b)
Figure 5: Variations of air core diameter with spigot diameter for inlet pressures (a) 50 kPa, (b) 125 kPa.
We observe that air core diameter increases with increasing spigot diameter for fixed values of other
experimental parameters. This phenomenon is described by this way. The tangential velocity increases in
the prevailing swirling flow field with increasing spigot diameter; as such the increased magnitude of
maximum tangential velocity results in increasing pressure differential with ambient and this fact leads to
get increased air core diameter. Moreover, an observed interesting phenomenon is that the increased apex
diameter leads to the significant variation of air core diameter in cylindrical and conical sections at low
inlet pressure. In contrast to this view, at higher inlet pressure, cylindrical section shows increased air
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Modelling & Simulation
core diameter with increasing spigot diameter whereas conical section exhibits no variation of air core
diameter.
We illustrate the change in the air core diameter with varying inlet flow rate in fig. 6. Researchers
(Banerjee et al., 2015; Gupta et al., 2008) highlighted that the swirl flow pattern along any cross section
of the hydrocyclone exhibits a vortex structure which is composed by free and forced vortex components.
The matching region between these two components denotes the zone of maximum tangential velocity
denoted by 𝑢𝜃,𝑚𝑎𝑥 .
pressure drop created in the spigot region increases with increasing 𝐺𝑚𝑎𝑥 and results in an increase in air
core diameter.
The collection efficiency of a hydrocyclone depends on the available cross-sectional area at the two exit
openings. However, the air core at dynamic condition occupies significant cross-sectional area near the
vortex finder as well as spigot region. This observation can be explained by the fact that the diameter of
the air core near the vortex finder plays a crucial role to decide the water recovery rate in overflow.
Figure 7 depicts the variation of overflow water split as a function of inlet flowrate. It appears from the
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Modelling & Simulation
figure that the overflow water split increases initially with increasing inlet flow rate whereas it shows
very few variations in magnitude at higher values of inlet flow rate. The reason behind this phenomenon
might be due to negligible variations of air core diameter in cylindrical and conical sections at the higher
inlet flow rates.
0.90
0.85
Overflow water split
0.80
0.75
0.70
0.65
0.6 0.8 1.0 1.2 1.4 1.6
Figure 7: The observed trends of experimental water split data as a function of inlet flow rate. Here the
results are shown for vortex finder at 25 mm and spigot at 13 mm.
4. Theoretical analysis
dvf
z =0
Feed
Inlet
Dc
g
𝑢𝜃
R
𝑢𝑟
da
Cone angle
(100) 𝑢𝑧
dsp
(a) (b)
Figure 8: (a) Schematic representation of Hydrodynamic picture inside a hydrocyclone according to the
assumed theoretical model, (b) velocity component of the rotating fluid element in cylindrical coordinate.
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Modelling & Simulation
For the sake of analytical convenience in present study, a fixed cylindrical coordinate system (𝑟, 𝜃, 𝑧) has
been considered. Figure 8 (a) illustrate the hydrodynamic representation inside the hydrocyclone in
accordance to the present theoretical approach. Here, 𝐷𝑐 , 𝑑𝑣𝑓 and 𝑑𝑠𝑝 denote the diameters of the
hydrocyclone, vortex finder and spigot respectively and the 𝑧 axis is along the direction of gravity. Again,
in this figure, 𝛿𝑅 and 𝑑𝑎 represent the boundary layer thickness and air core diameter respectively. The
tangential, radial and axial components of the velocity are represented with respect to the cylindrical
frames by ur, uθ and uz respectively as shown in figure 8(b). The flow field inside a hydrocyclone is
essentially a swirling flow generated by tangentially introduced velocity; as such the phenomenological
aspects of air core would be evolved in a quantitative manner through analyzing the governing principle
of swirling flow behaviors inside the cylindrical and conical sections. For the sake of comprehensiveness,
we proceed by the following momentum integral equations which are derived from the solution of
momentum equation of laminar boundary layer based on the Pohlhausen’s method (Som and Mukherjee,
1980).
𝑑𝛿1 450𝐸1
𝑑𝑧1
=𝛿 2 (1)
1 (𝐸1 +105𝛿1 )
𝑑𝐸𝑅2 98 2𝐸𝑅2 𝐸2 𝑅′
𝑑𝑅 ′
= − 𝑅′ + 𝑅′
− 330 𝐸 𝑅𝛿2 (3)
𝑅 𝑅
Among eqs. (1) to (4), the first two equations are given for cylindrical section, whereas the remaining two
are provided for conical section. The dependent variables in eqs. (1) and (2) are given by 𝛿1 =
𝛿 ⁄𝑅𝑐 (𝛺 ⁄𝜈 )2/5 and 𝐸1 = 𝐸(𝛺 ⁄𝜈 )1/5 where 𝛿 and 𝐸 are functions of axial height z, 𝑅𝑐 is the radius of
hydrocyclone, Ω is the circulation parameter and 𝜈 is the kinematic viscosity of fluid. On the other hand,
the dependent variables in eqs. (3) and (4) can be expressed as 𝛿𝑅 = 𝛿 ⁄𝑅𝑐 (𝛺 ⁄𝜈 𝑠𝑖𝑛 𝛼 )1/2 and 𝐸𝑅 =
𝐸 𝑐𝑜𝑠 𝛼 where 𝛿𝑅 and 𝐸𝑅 determine the boundary layer at any axial position, 𝛼 is the half of the cone
angle of hydrocyclone and 𝑅 ′ = 𝑅 ⁄𝑅𝑐 in which 𝑅 is the radius of conical section at any axial location.
Equations (1) and (2) are solved analytically together with the boundary condition 𝛿1 =0 and 𝐸1 = 0 at 𝑧1 =
0, and the following solution is obtained.
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Modelling & Simulation
0.4
𝛿1 = 4.44 𝑧1 (6)
96(
On the other hand, eqs. (3) and (4) are solved with the boundary condition 𝛿𝑅 = (Ω⁄𝜈 )0.1 (sin 𝛼)0.5 and
𝐸𝑅 = 𝐸1 (𝜈 ⁄Ω)0.2 cos 𝛼 at 𝑅 ′ = 1 and we obtain the following equation.
(7)
𝐸𝑅 3 𝛿𝑅 2 = 𝑘𝑅 ′ - 22.5𝑅′2 + 24.5
From eq. (7), we calculate 𝛿𝑅 at different inlet Reynolds number as calculated from present experiments.
Finally, we calculate air core radius 𝑟𝑎 as
𝑟𝑎 = 𝑅𝑠𝑝 − 𝛿𝑅 (8)
where 𝑅𝑠𝑝 is the radius of spigot. Figure 9 exhibits comparative plots between measured air core
diameters as obtained from shadowgraph measurement and predicted air core diameters as perceived from
the solution of aforementioned theoretical model. It is obvious that the theoretical model provides a
cylindrical tube shape of air core located at the centre of the hydrocyclone.
14.0
Experimental value (volume
12.0
average)
10.0
8.0
6.0
4.0
4.0 6.0
Predicted8.0value ( Theoretical)
10.0 12.0 14.0
Figure 9: Comparison of the theoretical model with experimental data reported in published literature.
Apart from the observed real phenomenon of air core from the solution of theoretical model, its
rationality has been established by verifying with experimental observations reported in literature
(Krishna et. al., 2010; Heish, 1988). Figure 10 shows reasonable agreement with the observed trend of air
core diameter with varying inlet flow rate and spigot diameter.
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Modelling & Simulation
12
10
9
Theoritical trendline
Data Point -Hsieh[10]
Data Point - Krishna et al. [9]
8
0 20 40 60 80 100
3
Inlet Reynolds number x 10
Figure 10: Comparison of the theoretical model with experimental data reported in published literature.
5. Conclusions
A comprehensive analysis has been done to estimate the phenomenological characteristics of the air core
in a classifying hydrocyclone through experimental and mathematical approaches. Experimental
observations of the dancing nature of air core through the shadowgraph measurement have been
quantified. The boundary of the air-water interface has been predicted by using an image processing
technique based on edge detection algorithm. The surprising experimental observations are that the
oscillation characteristic of air core is relatively higher in conical section in comparison to that in
cylindrical section. This phenomenon occurs owing to the swirl flow around the central core region of the
hydrocyclone which originates a wave motion along the air water interface.
Moreover, theoretical investigations have been performed to compute the observed trend of air core
diameter measured from present experiment and the data reported in literature. Although the solution
theoretical model provides is a conservative air core diameter, but the model is not definite towards the
oscillation behavior and elevation dependent shape of the air core especially at the conical section. At the
end, it needs to mention that the prediction of dancing nature of air core through theoretical approach
together with the inclusion of other underlying physics is subjected to further verification.
Acknowledgements
This work was supported by the research federation Fermat (Fdration de recherche Fermat FR 3089,
www.federation-fermat.fr). Also, the authors gratefully acknowledge the support from Tega Industries,
Kolkata, India (www.tegaindustries.com) for providing hydrocyclone.
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Modelling & Simulation
References
[1] E. Ovalle, F. Concha, The role of wave propagation in hydrocyclone operations II: Wave propagation
in the air–water interface of a conical hydrocyclone, Chem. Eng. J. 111 (2005) 213–223.
[2] T. Neesse, M. Schneider, V. Golyk, H. Tiefel, Measuring the operating state of the hydrocyclone,
Miner. Eng. 17 (2004) 697–703.
[4] F. Concha, A. Barrientos, J. Montero, R. Sampaio, Air core and roping in hydrocyclones, Int. J.
Miner. Process. 44-45 (1996) 743–749.
[6] S. Yao, T. Fang, Analytical solutions of laminar swirl decay in a straight pipe, Commun. Nonlinear
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[7] B. Wang, K.W. Chu, A.B. Yu, Numerical Study of Particle−Fluid Flow in a Hydrocyclone, Industrial
& Engineering Chemistry Research. 46 (2007) 4695–4705.
[8] M.A. Hararah, E. Endres, J. Dueck, L. Minkov, T. Neesse, Flow conditions in the air core of the
hydrocyclone, Miner. Eng. 23 (2010) 295–300.
[9] V. Krishna, R. Sripriya, V. Kumar, S. Chakraborty, B.C. Meikap, Identification and prediction of air
core diameter in a hydrocyclone by a novel online sensor based on digital signal processing technique,
Chem. Eng. Process. Process Intensif. 49 (2010) 165–176.
[10] K.T. Hsieh, Phenomenological Model of the Hydrocyclone., University of Utah., 1988.
[11] A. Rakesh, V.T.S.R. Kumar Reddy, M. Narasimha, Air-Core Size Measurement of Operating
Hydrocyclone by Electrical Resistance Tomography, Chem. Eng. Technol. 37 (2014) 795–805.
[12] R. Williams, X. Jia, R. West, M. Wang, J, Cullivan, J. Bond, et al., Industrial monitoring of
hydrocyclone operation using electrical resistance tomography, Minerals Engineering, 12 (1999), 1245–
1252.
[13] J. Gutiérrez, T. Dyakowski, M. Beck, R. Williams, Using electrical impedance tomography for
controlling hydrocyclone underflow discharge, Powder Technol. 108 (2000) 180–184.
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[14] R.A. Williams, F.J. Dickin, J.A. Gutiérrez, T. Dyakowski, M.S. Beck, Using electrical impedance
tomography for controlling hydrocyclone underflow discharge, Control Eng. Pract. 5 (1997) 253–256.
[15] W.K. Evans, A. Suksangpanomrung, A.F. Nowakowski, The simulation of the flow within a
hydrocyclone operating with an air core and with an inserted metal rod, Chem. Eng. J. 143 (2008) 51–61.
[16] R. Sripriya, M.D. Kaulaskar, S. Chakraborty, B.C. Meikap, Studies on the performance of a
hydrocyclone and modeling for flow characterization in presence and absence of air core, Chem. Eng.
Sci. 62 (2007) 6391–6402.
[17] J. Xu, Q. Luo, J. Qui, Studying the flow field in a hydrocyclone with no forced vortex. Part I,
average velocity, Filtration & Separation, 27 (1990) 181-182.
[19] R. Gupta, M.D. Kaulaskar, V. Kumar, R. Sripriya, B.C. Meikap, S. Chakraborty, Studies on the
understanding mechanism of air core and vortex formation in a hydrocyclone, Chem. Eng. J. 144 (2008)
153–166.
[20] S.K. Som, S.G. Mukherjee, Theoretical and experimental investigations on the formation of air core
in a swirl spray atomizing nozzle, Applied Scientific Research. 36 (1980) 173–196.
578
Modelling
PREDICTION OF YIELD AND COMBUSTIBLE RECOVERY OF COAL USING & Simulation
ARTIfiCIAL
NEURAL NETWORK IN MULTI GRAVITY SEPARATOR
Ram Chandra Chaurasia* and Suresh Nikkam
Department of Fuel & Mineral Engineering, Indian School of Mines, Dhanbad, Jharkhand India
*Corresponding author: rcc.0761@gmail.com
Abstract
Yield and recovery of combustible matter are the two performance parameters commonly used in measuring
the performance of the plants treating coal. Assessment of these two parameters will indicate the operational
efficiency and the extent of separation taken place. In the present paper, attempts made to use multi gravity
separator (MGS) for the beneficiation of coal fines ground to finer than 75 micron has been discussed
elaborately. Effect of three important parameters like drum speed, drum inclination and its shake frequency
on the product quality has been analysed. To predict the ash content and combustible recovery in concentrate,
an attempt has been made through Artificial Neural Network. For this purpose different sensitivity analysis
approaches have been adopted to find out the significance of the most important parameter which influences
the product quality.
Keywords: MGS, Artificial Neural Network, Sensitivity Analysis, Coal, Fine particle
1. Introduction
Multi gravity separator (MGS) is one among the enhance gravity separators designed by M/s Richard Mozley
Limited, UK. This unit is used specifically for processing of fine particles below 75 microns from which
coal/minerals can be concentrated based on specific gravity difference of gangue and desired components.
Use of MGS is becoming increasingly important whenever, the surface property dependent techniques fail to
give the desired quality product. However, all these surface property dependent techniques, in practice are
found to be inappropriate owing to their poor separation efficiencies witnessed at finer sizes. Use of MGS
separator has many advantages in this respect, because it uses centrifugal force for separation of particles, no
chemicals are added during processing and therefore, does not create environmental hazards. To adopt MGS
for commercial coal cleaning, the extent of influence parameters on product quality and quantum need to be
considered. Their influences are to be understood thoroughly for a given material. The design parameters that
are involved are the Drum speed, Drum inclination, Shake frequency, Shake amplitude and whereas the
operating parameters are Pulp density, Wash water and Feed flow rate etc.,. In the present case effect of only
3 parameters viz., drum speed (DS), drum inclination (DI) and shake frequency (SF) have been considered
for the study.
There are articles on MGS treating plant rejects/fines to recover the clean coal from Turkey and India
(Majumder, Bhoi and Barnwal 2007, Özgen et al. 2011). More information on the applicability of MGS was
investigated from the literature. These are reported in the form of technical papers published elsewhere for
beneficiation of different ores and tailings using MGS (Cicek and Cöcen 2002; Aslan 2007, 2008a, 2008b
Aslan and Kaya 2009; Bandopadyaya 2000; Luttrell, Honaker and Phillips, 1995). Later studies, indicate that
MGS was also utilized for fine coal cleaning by several investigators (Erdem et al. 2008; Koca, H. Koca, S.
and Karaoglu, 2000; Oz, Koca, S. and Koca, H. 2009). However, in these studies the particles treated were of
579
coarser sizes and no attempts have been made to investigate the beneficiation possibilitiesModelling
of ultrafine & Simulation
coals.
In India, the proportion of ultra-fines is increasing pragmatically due to the advent of mechanization in
mining and material handling equipment. In coal processing, Combustible recovery and ash content are the
most important parameters which will decide the efficiency of the process with different variable conditions;
therefore optimization and modeling of process variables are essential in the concentration process. The
Multi-Gravity Separator (MGS) in the recent years is being used as a fine gravity separator, but its usage for
fine coals is scanty. The present paper outlines the use of this separator for treating ultrafine (d80p=30µ) coal
obtained from an operating washery in India.The Artificial neural network is a popular approach nowadays
most scientists adopts successfully as an alternate statistical method with high predictability. ANN has the
remarkable ability to derive meaning from complicated or imprecise data, which can be used to extract
patterns and detect trends with highly non-linear complex data sets. ANN gives an insight of separation of
particulate solids from discontinuous and incomplete data sets, and is highly advantageous. In view of this, in
the present work a feed forward back propagation neural network has been used to predict the combustible
recovery and ash content based on the input parameters such as drum inclination (DI), drum speed (DS) and
stroke frequency (SF). Different approaches to interpret the significance of input variables on the output
parameters are also deliberated in-depth.
The paper also outlines the significance of most important parameter which influence the product quality
generated out of MGS. Influence of design variables like drum speed, drum inclination and shake frequency,
for the prediction of combustible recovery and ash content of washed coal have been brought out explicitly.
2. Methodology
2.1 Artificial Neural Network
Artificial Neural Network (ANN) is a mathematical modelling tool which is basically concern to the
approach of statistical modelling, based similarly on the concept of Biological Neural Network (BNN) in the
human brain. The main objective of the neural network is to convert the different data input and streamline it
to get proper meaningful outputs. There are various kinds of neural network approaches available, such as
single-layer perception, multi-layer perception, and radial-basis function nets among which Multilayer
Perception (MLP); a feed forward back propagation neural network is the most commonly used ANN
approach. Back propagation is an algorithm which is commonly applied for training (Jorjani, Chelgani and
Mesroghli 2008; Kalyani et al. 2008; Wu and Jiang 2011; Liao, Liu and Wang 2011; Scott and Ray 1993;
Panda et al. 2012). Each neuron layer in ANN is associated to the next neighbouring layer of the neurons
system and all neurons are particularly connected with different weights. While training the data these
weights are adjusted to establish empirical correlation between input and output variables in the system. All
neurons are associated with different weights. ANN model has been developed using a total of 27
experimental data. Out of these 27 experiments, seventy percent data were used for training of the model,
thirty percent was used for testing of the model. The ANN has been implemented through using Matlab.
In the present study all the variables (inputs) are normalized in the range [-1, 1] before training. A
multilayer feed forward back propagation neural network was used with Tan-Sigmoid transfer function. The
network is trained (learning) with Levenberg-Marquardt (LM) algorithm. To further improve the
580
Modelling
generalization of the developed ANN model Bayesian regularization method has been adopted. It&also
Simulation
minimizes a combination of squared errors and weights, and then determines the correct combination. The
Bayesian regularization technique has been implemented using Matlab and the Connection weight and biases
are given in Table 1.
For proper selection of input variables that are critical and important in the process is of major
concern for sensitivity analysis. However, different approaches have been suggested to select the important
input variables such as Pearson correlation coefficient, Garson's algorithm and connection weights approach.
The Pearson correlation coefficient helps in selecting proper input variable for the ANN (Guyon and Elisseeff
2003, Wilby et al. 2003). Some investigators have used Garson's algorithm (Goh 1994, Garson 1991and
Shahin et al. 2002) in which the input-hidden and hidden-output weights of trained ANN model are separated
and the absolute values of the weights are taken for the selection of the important input variables, more
details on this aspect are presented elsewhere (Goh 1994). This was another method connection weights
approach was proposed by Olden et al. (2004) in which the actual values of input-hidden and hidden-output
weights are taken. It sums the products across all the hidden neurons, which is defined as S i. On the basis of
highest Si value selection of important input parameter is done. The results of these sensitivity analysis
obtained from the above approaches are showed in Tables 2 and 3.
Table 2 shows the cross correlation of inputs with the ash content and combustible recovery. From the table it
can be seen that ash content is highly dependent on rpm of the drum ascertained by the cross correlation
value of 0.81, followed by shake frequency (0.20) and drum inclination (-0.05). Here, negative sign is an
indicative indirect influence of the dependent variable. Similarly for recovery drum inclination is important
parameter followed by drum speed and shake frequency.
Weight Biases
Output Neurons
Input 1 Input 2 Input 3 Output bhk b0
Hidden neuron 1 (K=1) 0.8899 0.0993 -0.2887 0.8152 0.7833 -0.2003
Ash Hidden neuron 2 (K=2) -0.1107 -0.511 -0.6874 0.588 0.6644
Hidden neuron 3 (K=3) 0.7313 -0.494 0.2835 -1.1765 0.9933
Hidden neuron 1 (K=1) 0.659 -0.6654 0.353 0.8807 0.5687 -0.0853
Recovery Hidden neuron 2 (K=2) -0.57 -0.7185 0.0918 -0.9394 0.7032
Hidden neuron 3 (K=3) -0.0988 -0.0753 -0.9611 1.0568 0.1267
The sensitivity analysis for the important input parameters made for the model as per Garson’s method are
presented in Table 3. As per Garson’s approach, the extents of influence of each of the parameters indicate
that, the drum inclination to be the most important input parameter for ash with its relative share valuing at
42.18% in comparison to other inputs. Similarly for combustible recovery the relative importance of the input
variables were calculated and given in Table 3. The third approach of sensitively analysis viz., Connection
Weight approach, which also depicts and confirms that, the drum speed to be the most important input
parameter with Si value 0.97 followed by shake frequency and drum inclination. For this case also, where
negative Si values have appeared, mean that the parameter is indirectly related to output. From the above
results it can be seen that drum speed has found to be the most important parameter followed by shake
581
Modelling
frequency and drum inclination for ash content. Drum inclination has found to be the & Simulation
most important
parameter followed by drum speed and shake frequency for recovery based on all the sensitivity analysis
methods.
Table 2: Cross-correlation of input and output for the ash and recovery
DI SF DS Ash
DI 1 0 0 -0.0508
Ash SF 1 0 0.2019
DS 1 -0.8119
Ash 1
DI SF DS Rec.
DI 1 0 0 0.6699
Recovery SF 1 0 -0.0733
DS 1 -0.6201
Rec. 1
Table 3: Relative importance of different inputs as per Garson's algorithm and connection weight approach
3. Conclusion
Based on sensitivity analyses; Pearson correlation coefficient, Garson's algorithm and connection weight
approaches, it was observed that drum speed has found to be the most important parameter followed by shake
frequency and drum inclination for ash content. Drum inclination has found to be the most important
parameter followed by drum speed and shake frequency for recovery.
References
A.K. Majumder, K.S. Bhoi and J.P. Barnwal. Multi-gravity separator: an alternate gravity concentrator to
process coal fines, Minerals & Metallurgical processing, vol. 24, pp. 133-138, 2007.
Ozgen Selcuk, Malkoc Ozkan, Dogancik Ceyda, Sabah Eyup, Sapci Filiz Oruc, Optimization of a Multi
Gravity Separator to produce clean coal from Turkish lignite fine coal tailings, Fuel, vol. 90, pp. 1549-1555,
2011.
T. Cicek, and I. Cöcen. Applicability of Mozley multi gravity separator (MGS) to fine chromite tailings of
Turkish chromite concentrating plants. Mineral Engineering 15:91-93, 2002.
N. Aslan. Modeling and optimization of Multi-Gravity Separator to produce celestite concentrate. Powder
Technology 174:127-133, 2007.
582
Modelling
N. Aslan. Multi-objective optimization of some process parameters of a multi-gravity separator & Simulation
for chromite
concentration. Separation and Purification Technology 64: 237-241, 2008a.
N. Aslan. Application of response surface methodology and central composite rotatable design for modelling
and optimization of a multi-gravity separator for chromite concentration. Powder Technology 185: 80-86,
2008b.
N. Aslan, and H. Kaya. Beneficiation of chromite concentration waste by multi gravity separator and
High intensity Induced roll magnetic separator. The Arabian Journal of Science and Engineering 34:285-
297, 2009.
A. Bandopadyaya. Multi gravity separator - An equipment for separation of fines. Processing of Fines (2).
NML Jamshedpur 81-92, 2000.
G.H. Luttrell, R.Q. Honaker and D.I. Phillips. Enhanced gravity separators: new alternatives for fine coal
cleaning; Proceedings of the 12th International Coal Preparation Conference. Illinois. 1995.
A. Erdem, Z. Olgun, A.Gulmez, O. Altun, A. Gitmez, B. Oteyaka, and S. Koca. Beneficiation of Lignites by
Means of Shaking Table, MGS and Flotation, Project report 2, Project No. 106G056, MTA, Ankara. 2008.
H. Koca, S. Koca, and M. Karaoglu. Recovering of Fine Coal Particles from Tailing Ponds of Ankara-
Alpagut-Dodurga Coal Washing Plant. In Proceedings of the XI International Conference of Environmental
Issues and Management of Waste in Energy and Mineral Production SWEMP Calgary, Alberta, Canada, 117-
121, 2000.
D. Oz, S. Koca, and H. Koca. The Utilization of Unsaleable Lignite Fines at Eskisehir Koyunagli Region
Lignite Deposits. Falmouth, England. Physical Separation 16-17, 2009.
E. Jorjani, S.C. Chelgani, and Sh. Mesroghli. Application of artificial neural networks to predict chemical
desulfurization of Tabas coal. Fuel, 87: 2727-34, 2008.
V.K., Kalyani, Pallavika, Chaudhuri, S., D.D. Haldar, T. Gouri Charan, and K.P. Kamal, et al. Study of
laboratory scale froth flotation process using artificial neural networks. Mineral Processing ant Extractive
Metallurgy Review 29:130-42. 2008.
Y.F., Liao, J.T. Liu, and Y.T. Wang. Prediction of gas holdup in cyclonic static micro bubble flotation
column based on BP neural networks. Journal of China University of Mining and Technology 40(3): 443-37.
2011.
L. Panda, A.K., Sahoo, A. Tripathy, S.K. Biswal, and A.K. Sahu. Application of artificial neural network to
study the performance of jig for beneficiation of non-coking coal. Fuel 97:151–56. 2012.
A.J. Wu, and C.L. Jiang. Research on the propagation of shock waves from coal and gas outburst. Journal of
China University of Mining and Technology 40(6): 852-57. 2011.
G.M. Scott, and W.H. Ray. Creating efficient nonlinear neural network process model that allow model
interpretation. Journal of Process Control 3(3):163-78. 1993.
G.D. Garson. Interpreting neural-network connection weights. Artificial Intelligence Expert 6 (7): 47-51.
1991.
A.T.C. Goh. Seismic liquefaction potential assessed by neural network. Journal of Geotechnical Engineering
ASCE 120 (9): 1467-1480. 1994.
A.T.C. Goh, F.H. Kulhawy, and C.G. Chua. Bayesian neural network analysis of undrained side resistance of
drilled shafts. Journal of Geotechnical and Geo-environmental Engineering, ASCE 131 (1): 84-93. 2005.
I. Guyon, and A. Elisseeff,. An introduction to variable and feature selection. Journal of Machine Learning
Research 3: 1157-1182. 2003.
583
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J.D., Olden, M.K. Joy, and R.G. Death. An accurate comparison of methods for quantifying & Simulation
importance in artificial neural networks using simulated data. Economic Modelling 178 (3): 389-397. 2004.
M.A. Shahin, H.R. Maier, and M.B. Jaksa. Predicting settlement of shallow foundations using neural
network. Journal of Geotechnical and Geoenvironmental Engineering, ASCE 128 (9): 785-793. 2002.
R.L., Wilby, R.J. Abrahart, and C.W., Dawson. Detection of conceptual model rainfall-runoff processes
inside an artificial neural network. Hydrological Sciences 48 (2): 163–181. 2003.
584
Physical separation including gravity
separation
585
Physical separation including gravity separation
IMPACT OF VARIABILITY IN FEED DISTRIBUTION AND OPERATING VARIABLES ON
HIGH RATE THICKENER UNDERFLOW PULP DENSITY
Prateek Singh*, Vishal Shukla and D.P. Chakraborty
Process Technology Group, TATA Steel, Jamshedpur
*Corresponding author: prateek.singh@tatasteel.com
Abstract
Thickener is widely used as a dewatering device in various beneficiation plants for water recovery. In the
present scenario, due to shortage of hard ore, the iron ore beneficiation plant at Noamundi, Tata Steel is
facing innumerable challenges ranging from slime generation, slime management to scarcity of water
required for beneficiation. Thus, thickener plays a very crucial role and directly affects the plant
economics. This paper illustrates the effect of variation in feed distribution on thickener underflow pulp
density during low Hydrocyclone recovery. Relation of hard ore in feed with underflow pulp density is
established. Effect of rake arm torque on bed mass is also taken into account for effective operation of
thickener. It is observed that a high bed mass of 35-40% enabled to achieve 1.48 g/cc underflow pulp
density.
Keywords: Slime, Pulp density, Thickener, Hard ore, Bed mass, Rake arm torque.
1. Introduction
Iron ores are encountered in nature mostly as hard ore, friable ore, lateritic ore, blue dust and soft ore.
During the mining and processing of iron ores in India, around 10–12 million tons of slimes of below
0.15 mm size containing around 48–62% Fe with high silica and alumina are generated every year and
discarded into the tailing ponds. From decades the Noamundi plant is processing hard ore, friable ore and
soft ore but now due to the depletion of hard ore the ROM comprises of friable ore and soft ore.
Previously, the thickener was installed with respect to hard ore as feed but in present scenario due to
shortage of hard ore; the iron ore beneficiation is facing several problems ranging from slime generation,
slime management and consequently the scarcity of water required in the beneficiation. To cater the
above problems a High Rate Thickener (HRT) was commissioned in Noamundi process plant (Fig. 1) in
2012 to improve the recovery of water. HRT was installed since the ore characteristics changed and the
conventional thickener was unable to deal with the slimes. Use of HRT enabled hindered settling
classification.
586
Physical separation including gravity separation
2. Working principle of High Rate Thickener and study of its operational dynamics
The separation of suspended solid particles from a liquid stream by gravity settling is termed as
sedimentation, which is the working principle of thickener operations. The primary purpose of thickening
is to increase the solids concentration of the feed stream. Gravity settling is aided by addition of
chemicals called flocculants. The feed is pumped into the feed well, at the centre of the thickener, near the
top, which is normally dozed with flocculent. The thickened mass thus formed moves towards the bottom
centre of the thickener by large rakes which rotate around the tank. The raking arms convey the settled
solids from the entire area to the discharge cone. These are also equipped with the capacity to be raised to
reduce the drive torque. As a result, the clarified liquid formed at the top of the thickener overflows the
peripheral launder and goes for recycling, while the solids which settle over the entire bottom of the tank
are withdrawn as a thickened pulp from an outlet at the centre. During the thickener operation, the drive
torque is continuously monitored as high densities could cause failure of the rakes and drive equipment.
Basic components of high rate thickener include: Rake drive unit and lifting device, bridge and
walkway, lower shaft, feed well, deflector cone, deflector cone scrapper, rake arms, underflow cone
scrapper, instrumentation and flocculation facilities and rake position sensor.
Two forces that act upon particles inside the thickener are:
- Gravity Force (the force that the Earth exerts on every object)
587
Physical separation including gravity separation
- Buoyancy Force (dependent on the feed volume flow rate and the size of the thickener)
Volume dynamics involved in the thickener state that the volume of feed slurry must be equal to the sum
of thickener underflow volume and the overflow water volume, whereas according to Solid dynamics the
feed solid flow rate (tph) is equal to the thickener underflow solid tph.
As mentioned earlier, gravity settling in thickening operation is aided by the addition of chemicals called
flocculants. Flocculant is a long chain of negatively charged molecule that combines with the positively
charged ore particles to agglomerate into long chains and form a heavier colloid, which settles faster. The
amount of flocculant added to the thickener depends on the type of ore in feed. Hard ore tends to have a
coarser size distribution and therefore requires less flocculant addition, since coarse particles settle easily
and vice-versa for soft ore.
1.45
y = 0.0051x + 1.284
HRT U/F Pulp Density(g/cc)
R² = 0.3134
1.40
1.35
1.30
1.25
1.20
0 5 10 15 20 25
% Hard Ore (ROM feed)
High rate thickener process data during the span of April’14-Aug’14 was analysed. From Fig. 2 it can be
inferred that thickener underflow pulp density increases with increase in % of Hard Ore in ROM feed
(observed during low Hydrocyclone recovery). The O/F (overflow) of Hydrocyclone (H/C) reports to
high rate thickener as feed in the slime recovery circuit. Therefore, during low Hydrocyclone recovery i.e.
at lower separation efficiency of H/C the coarser particles in feed report to the H/C overflow which is
itself thickener feed. Thus, due to increase in hard ore% in ROM the amount of coarser particles in
thickener feed increases and as a result the thickener underflow pulp density increases.
588
Physical separation including gravity separation
1.45
y = -0.0048x + 1.3818
1.35
1.30
1.25
1.20
0 5 10 15 20 25 30
% Soft Ore (ROM feed)
It can be observed from Fig. 3 that thickener underflow pulp density decreases with increase in % of Soft
Ore in ROM feed (observed during low Hydrocyclone recovery). In slime recovery circuit the O/F of
Hydrocyclone is feed to high rate thickener. Therefore, during low Hydrocyclone recovery i.e. at lower
separation efficiency of H/C, the finer fraction in feed will report to the H/C underflow instead of
reporting in thickener feed, as a result the thickener underflow pulp density decreases.
40.0
Bed Mass (%)
30.0
20.0
10.0
0.0
9.0 10.0 11.0 12.0 13.0 14.0 15.0
Rake Arm Torque(N-m%)
589
Physical separation including gravity separation
A positive relationship can be observed from Fig. 4 between rake arm torque and the bed mass%.
Therefore, high bed mass can be achieved by controlling rake arm torque as the duty of rake arms is to
convey the entire solids towards the bottom centre of the cone for discharge. But rake arm torque should
be in a permissible limit because a high drive torque may cause the failure of thickener rake arms.
1.55
HRT U/F Pulp Density(g/cc)
1.50
y = 0.0045x + 1.2174
R² = 0.2965
1.45
1.40
1.35
1.30
1.25
1.20
0.00 10.00 20.00 30.00 40.00 50.00
Bed Mass (%)
The Fig. 5 indicates that High Rate Thickener U/F pulp density is a function of solids mass in the
thickener (Bed Mass%) and it follows an increasing trend. The ‘bed mass’ is effectively the density of the
settled sludge. The higher the density, the less process water is pumped out of the thickener’s underflow.
Bed mass is calculated based on the total volume of combined water and solids in the tank and the total
hydrostatic pressure measured near the bottom of the tank. This optimisation of water content in the
underflow allows for maximum recycling of process water while still keeping the underflow slurry
sufficiently liquid to be managed by the underflow pump.
4. Conclusion
From this investigation, we observed that during the period of low Hydrocyclone recovery the thickener
underflow pulp density is a function of ore type. The u/f pulp density increases with increase in hard ore%
and vice-versa. It was also established that by varying the bed mass% and rake arm torque, better control
of the thickener performance can be achieved.
Acknowledgement
590
Physical separation including gravity separation
The authors are grateful to all the persons who helped in this project directly or indirectly. The authors
would also like to thank the operations team of Noamundi Iron Mines (NIM) of TATA Steel Limited for
their assistance throughout the work. We are thankful to Tata Steel Ltd., management for all the support,
encouragement and permission to publish the paper.
References
Anderson, Corby G.; Dunne, Robert C.; Uhrie, John L., Metalliferous Mining – Processing, Thickening
Resource Book, 1-24, 2010.
Steve Tarleton, Richard Wakeman, Solid/Liquid Separation: Equipment Selection and Process Design, 2-
6, 2007.
Andrew L Mular, Doug N Halbe, Derek J Barratt, Mineral Processing Plant Design, Practice and Control
Volume 2, 1290-1298, 2002.
591
Physical separation including gravity separation
UNDERSTANDING OF CLASSIFICATION EFFECT IN STUB-CYCLONE: EFFECT OF
FLOW RATIO(RF) AND UNDERFLOW PULP DENSITY ON CYCLONE PERFORMANCE
Neeraj Kumar*, Vishal Shukla and D.P.Chakraborty
Process Technology Group, Tata Steel, Jamshedpur
*Corresponding author: neeraj.kumar8@tatasteel.com
Abstract
Stub-Cyclones, also known as water only cyclones, are used to beneficiate coal and iron ore worldwide.
This paper summarizes the classification effect in stub-cyclone at Joda iron ore processing plant, Tata
Steel. Stub-Cyclone is used to beneficiate classifier fines at Joda iron ore processing plant. The study was
done by analysing performance of cyclones at various cut-sizes. The effect of fraction of water reporting
to underflow on the imperfection of stub-cyclone was established and explained. The role of underflow
density on performance of stub-cyclone was understood and has been summarised in the paper.
Comparative study of Stub-cyclone at Joda and Hydrocyclone at Noamundi, Iron Ore Beneficiation Plant,
and Tata Steel is also done and described.
1. Introduction
Stub-Cyclones, also known as water only cyclones, are used to beneficiate coal and iron ore worldwide. It
utilizes the difference in gravity between concentrate and gangue. Lighter particles report to overflow
while the heavier particles report to underflow. These are used widely because of its low operating cost
and high capacity. It has stubby conical bottom unlike hydrocyclones which have long narrow conical
bottom. Due to this stubby bottom it behaves as a dense-medium cyclone as particles of intermediate or
high specific gravity collect and recirculate in the conical section of the cyclone. These particles then
form an autogenous dense-medium through which the sinks have to penetrate to enter the underflow, but
the lighter particles find it difficult to penetrate and report to the overflow.
Cyclone is key equipment at Joda processing plant, Tata Steel. It is intended to recover iron values from
slime. It beneficiates overflow of the classifier which operates at cut-size of 150 micron. Underflow of the
stub-cyclones is mixed with classifier underflow whereas overflow is discarded. There are two cyclone-
banks each having ten cyclones of diameter 10 inch.
592
Physical separation including gravity separation
To understand the classification effect, cut size of the stub-cyclone was calculated for the period of one
year. It was calculated by plotting partition curve & graph for the same is shown below (Figure 1)
Cut-Size of stub-cyclones
Weekly Data, Joda
70
60
50
d50c
40
30
20
Date
Bank-1 Bank-2
From the above graph it can clearly be seen that cut-size lies in the range of 40 micron to 60 micron.
Imperfection of stub-cyclone for the same period was also calculated. Graph for the imperfection is
shown below (Figure 2).
It was found that imperfection was on higher side and lies in the range of 0.45 to 0.55. But imperfection
of hydrocyclone at Noamundi is on the lower side and is generally below 0.45. Hydrocyclone at
Noamundi operates at generally lesser cut-size than stub-cyclones at Joda. In spite of that their
imperfection are on lower side which is better.
It was observed that for higher cut-size imperfection was on lower side but the yield of cyclone decreases
subsequently. Imperfection decreases significantly at higher cut-size and it can be clearly seen from the
graph shown below (Figure 3).
593
Physical separation including gravity separation
Imperfection of stub-cyclones
Weekly Data, Joda
0.60
0.55
Imperfection
0.50
0.45
0.40
0.35
0.30
Date
Bank-1 Bank-2
Stub-cyclone,Imperfaction vs cut-size
Joda, Weekly data
0.60
y = -0.0055x + 0.7691
R² = 0.8836
0.55
Imperfection
0.50
0.45
0.40
0.35
0.30
40 45 50 55 60
D50c
594
Physical separation including gravity separation
0.55
Imperfection
0.50
0.45
0.40
2 4 6 8 10
Flow Ratio
Figure 4: STUB-CYCLONE, IMPERFECTION VS. FLOW RATIO
At the same time it was also observed that fraction of water reporting to underflow decreases with
increase in cut-size. It can be clearly seen from the following graph (Figure 5).
5
4.5
4
3.5
3
2.5
2
40 45 50 55 60
Corrected Cut-Size(micron)
Figure 5: STUB-CYCLONE, FLOW RATIO VS. CORRECTED CUT-SIZE
Strong relationship between underflow density and yield of cyclone was observed. With increase in
underflow density yield of the stub-cyclone decreases significantly and it can be explained from the
following graph (Figure 6).
595
Physical separation including gravity separation
STUB-CYCLONE, YIELD% VS. U/F PULP DENSITY
JODA, Weekly Data
55.00
y = -1.2459x + 108.22
Yield of concentrate 50.00 R² = 0.4195
45.00
40.00
35.00
30.00
25.00
20.00
45.00 47.00 49.00 51.00 53.00 55.00 57.00 59.00
Pulp density of u/f(w/w)
3. Conclusions
Difference in imperfection of Stub-cyclones and hydrocyclone has been demonstrated in the paper. Stub-
Cyclone has higher imperfection than hydrocyclones which decreases significantly at higher cut-size.
Effect of flow ratio on imperfection has also been shown. Imperfection increases with increase in fraction
of water reporting to underflow. Fraction of water reporting to underflow decreases with increase in cut-
size. For better performance underflow density of stub-cyclone should be maintained just below the
underflow density at which roping occurs.
Acknowledgement
The authors would like to express his gratitude to Mr Ashok Kumar, CTO Process Technology Group,
Tata Steel for his support. Authors also wish to thank Team NRD, Joda for the experimental work.
References
Introduction to Mineral Processing Design and Operation. A.Gupta and D.S.Yan, Perth, Australia
An Introduction to the Practical Aspects of Ore Treatment and Mineral Recovery. Barry A. Wills, Tim
Napier-Munn
596
Science and technology of reagent design and
development
597
Science and technology of reagent design and development
Abstract
AEROPHINE® 3418A Promoter is a unique phosphine-based collector that has been an industry standard
in the global mineral processing industry since its first commercial use in 1980. Although originally
developed for the flotation of copper sulphide minerals and activated zinc minerals, its application soon
widened rapidly. It is now recognized for its excellent selectivity and efficacy in the processing of
complex polymetallic sulphide ores comprising Cu, Pb, Zn, Ag, and Au in various combinations, Cu-Au
and Cu-Ni ores. In addition to its high collector strength for the value sulphide minerals, it exhibits high
selectivity against gangue iron sulphides (pyrite, pyrrhotite, marcasite, and arsenopyrite), non-activated
sphalerite, and penalty element-bearing minerals.
This paper provides a brief history of its development and use, including a case study highlighting a
potential innovative application of AEROPHINE® 3418A Promoter for Cu-Pb-Zn ores. A plant
production update will also be given on the future supply of this collector.
Keywords: Froth flotation, collectors, AEROPHINE® 3418A, complex sulphide, precious metals,
copper, lead, zinc, gold, silver.
1. Introduction
Cytec Industries Inc. operates a phosphine derivatives plant in Niagara Falls, Ontario, Canada that
manufactures various products for their speciality chemicals division. The products from this site are
based on phosphine (PH3) chemistry and are used in a variety of markets including electronics,
agriculture, LED lighting, water treatment, metal extraction, and mineral processing. One of the major
products is the phosphine-based sulphide mineral collector, AEROPHINE® 3418A Promoter.
AEROPHINE® 3418A Promoter (Figure 1) was originally developed for the flotation of copper and
activated zinc minerals (Thomas, 2010).
598
Science and technology of reagent design and development
S
H 9C4
P S-Na+
H 9C4
Plant usage of AEROPHINE® 3418A Promoter indicates that it exhibits strong collecting power for
copper sulphide minerals, galena, nickel sulphide minerals, and activated sphalerite, while achieving
excellent selectivity against iron sulphide gangue minerals such as pyrite, pyrrhotite, marcasite, and
arsenopyrite. AEROPHINE® 3418A Promoter is recognized in the industry for the recovery of native
silver and silver sulphide minerals. Similarly, it has been shown to be very effective for gravimetric gold,
electrum, and other precious metal alloys. For many ores, the dosage required is typically considerably
lower than that needed for the traditional collectors such as a dithiophosphate and xanthate.
The following advantages have been demonstrated by plant use of AEROPHINE® 3418A Promoter over
the years:
599
Science and technology of reagent design and development
The idea of a phosphine based collector dates back to 1964-67 when the dithiophosphinates were found to
be effective in sulphide mineral flotation (Mingione, 1990; Farinato & Nagaraj, 2014). The technology
development work proved that this type of collector chemistry had many benefits over existing traditional
chemistries in the market at that time, including, xanthates, dithiophosphates, mercaptobenzothiazoles,
and thiocarbamates. Although not commercially available for most of the 1970s, three patents (Wystach
et al, 1964, 1966, 1967) were granted to American Cyanamid Company which describe the use of dialkyl
dithiophosphinate for the effective flotation of base metal sulphide ores. The flotation collector known
today as AEROPHINE® 3418A Promoter became commercially available for use in the mineral industry
in 1979 (Mingione, 1990), though with only limited capacity.
The first commercial plant test of Aerophine dates back to a major Cu/Au/Ag operation in British
Columbia, Canada. The collector’s first commercial use was in 1980 in a Cu-Zn-Ag operation in Ontario,
Canada. Results from the plant trial indicated that AEROPHINE® 3418A Promoter provided a significant
metallurgical advantage in terms of fast flotation rates for copper, selectivity against Zn and Fe in the Cu
circuit, controlled froth even at higher dosages and an overall stable circuit operation. This significant
achievement for this collector marked the beginning of a reputation for AEROPHINE® 3418A in the
industry. The success in Ontario encouraged the investigation, testing, and adoption of this collector for
the treatment of other Cu-Zn ore bodies. By the late 1980’s, it was commercially used in several
polymetallic processing facilities in Canada, and is still the collector of choice in several newer,
international operations.
With the growing number of successful applications of AEROPHINE® 3418A at many complex
sulphides ore bodies, other existing operational mines began investigating its use. In the early 2000’s,
several mine sites that historically used alternative collector chemistry began testing its effectiveness on
their ores (Zhou, et al., 2005). In many cases, operations switched to using AEROPHINE® 3418A and
many of these operations still use the chemistry today. AEROPHINE® 3418A has consistently
demonstrated improved selectivity for Pb and precious metals with rejection of pyrite in their bulk
flotation circuit.
Today AEROPHINE® 3418A use is widespread internationally for the processing of complex
polymetallic ores of Cu-Zn, Cu-Pb-Zn and Pb-Zn, which frequently have significant quantities of
associated Ag and Au. The majority of these operations have found the collector chemistry to bring
significant value to their operations by increasing secondary precious metal recoveries. This is a
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significant economic driver for many operations, which rely on the precious metals revenue streams
within their concentrates.
3. Case study
The following case study describes a trial of AEROPHINE® 3418A in a copper-lead-zinc operation.
Other case studies in different operations are available on request from the author.
This plant operates a sequential flotation circuit to produce three separate concentrates. This complex
sulphide ore body has many challenges to achieve a selective separation. The lead circuit was an area for
improvement, as the sole collector being used at the time was sodium isopropyl xanthate (SIPX) and was
achieving poor results. Flotation tests were conducted to improve selectivity in the Pb circuit.
AEROPHINE® 3418A Promoter was selected by the metallurgical staff for improved lead and silver
recoveries and grade.
The plant trial was run over a two week period to investigate AEROPHINE® 3418A performance in the
lead circuit. The average trial head grades in the lead circuit were: 1.31% Pb, 0.23% Cu, 9.89% Zn and
171-g/t Ag. AEROPHINE® 3418A was dosed at 20 g/t and the dosage was split into the lead
conditioning tank and lead mid-rougher bank to maximize its performance. The main objectives for the
trial were:
The plant trial was run in two blocks. Each of the two blocks operated with 6 shifts using SIPX and 6
shifts using AEROPHINE® 3418A Promoter. There were small but statistically significant differences in
grind, and Pb and Zn feed grades from one block to another. The results from the trial were very positive,
indicating that the use of AEROPHINE® 3418A was beneficial to the lead circuit. The Pb recovery
improved by 3% at the 95% confidence level, while maintaining grade (Figure 2). The Ag recovery in the
Pb concentrate improved by 3.5% at the 95% confidence level (Figure 3). The overall Ag recovery
increased by 4% compared to SIPX, with 3.5% reporting to the Pb concentrate and the remaining 0.5%
reporting to the Zn circuit. The Zn and Fe grades in the Pb concentrate remained similar to that of the
standard conditions (Figure 4). The AEROPHINE® 3418A dosage carried over into the zinc circuit had a
beneficial effect as well since the overall zinc recovery increased by 0.5% during the trial.
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Further mill evaluation found that the new chemistry increased Pb circuit performance and
AEROPHINE® 3418A is now used full time at the operation between 15-25 g/ton.
Figure 2: The Pb recovery and grade during the test shown by collector type.
Figure 3: The Ag recovery and Ag grade to the Pb concentrate by collector type during the test period.
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Figure 4: Zn and Fe grades in Pb concentrate by collector type during the test period.
The Niagara Falls plant is the only manufacturing site producing the AEROPHINE® 3418A Promoter
chemistry. Due to increasing global demand of phosphine chemistries, the facility has been operating
above capacity despite continuous debottlenecking and plant optimization. A significant capital
investment was dedicated to expanding the current onsite phosphine production capabilities with the
addition of a new standalone plant, which commissioned in October 2014. This facility provides security
of supply for the growing demand of phosphine based chemistries, including AEROPHINE® 3418A
Promoter.
The increased availability of AEROPHINE® 3418A will allow expansion into new mineral processing
operations, including Cu-Ni ores and large Cu-Au deposits.
AEROPHINE® 3418A has been used extensively in complex sulphide ore bodies since the 1980’s for
improved selectivity for Cu and Pb ores, particularly for improved recoveries of precious metals. The
many benefits of this collector chemistry have been well documented at a number of operations for
increasing performance of Cu, Pb, Zn and precious metal recoveries for both Au and Ag. There is also a
growing interest in AEROPHINE® 3418A in the research community as attested by the large number of
recent publications. These serve to not only support plant practice, but also enhance the knowledgebase
for the fundamental aspects of the dithiophosphinate chemistry.
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There will be an increasing need for selective and efficient flotation collectors as the number of new ore
bodies being discovered which contain lower head grades. This poses increased mineral separation
challenges in processing of these ores. AEROPHINE® 3418A usage should grow in the years to come.
The recent expansion of the Niagara Falls plant has increased the availability of AEROPHINE® 3418A
to meet market demands. This will allow for increased applications in other mineral segments, such as
Cu-Au, primary Au, and Cu-Ni ores.
References
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from their mixtures on chalcopyrite, Minerals Engineering, Volume 20, Issue 10, August 2007, Pages
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Basilio, C.I., Yoon, R.H, Nagaraj, D.R., & Lee, J.S. (1991). Adsorption mechanisms for modified thiol-
type collectors; SME Annual Meeting, Denver, Preprint 91-171.
Brinen, J.S., Greenhouse, S., Nagaraj, D.R., & Lee, J.S. (1993). SIMS and SIMS imaging studies of
adsorbed dialkyl dithiophosphinates on PbS crystal surfaces. Int. Journal of Mineral Processing, 38
(1993) 93-109
Farinato, R.S. & Nagaraj, D.R. (1992). Time dependent wettability of mineral and metal surfaces in the
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Electrochemical Society, NJ.
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interaction of diisobutyldithiophosphinate with copper, silver and gold surfaces: I. Raman and NMR
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Engineering Aspects, Volume 214, Issues 1–3, Pages 77-85,
Hope, G, Woods, R, & Watling, K, (2003). A spectroelectrochemical investigation of the interaction of
diisobutyldithiophosphinate with copper, silver and gold surfaces: II. Electrochemistry and Raman
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spectroscopy, Colloids and Surfaces A: Physicochemical and Engineering Aspects, Volume 214,
Issues 1–3, 12 Pages 87-97.
Mingione, P.A., (1990). Use of AEROPHINE® 3418A Promoter for sulphide minerals flotation, CMP
Proceedings – Paper No. 26, pp. 485-508, Ottawa, ON.
Pecina-Treviño, E.T, Uribe, A., Finch, J.A., Nava, F., (2006). Mechanism of di-isobutyl dithiophosphinate
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secondary dithiophosphinic acids or their salts or esters, DE 1214171 19660414
Wystrach, Vernon P.; Rauhut, Michael M.; & Freyberger, Wilfred L. (1967). Dithiophosphinate
promoters for improved flotation of sulfides, US 3355017 19671128
Zhou, J, Martin, C, Blatter, P, Bossé, P-A., & Robitaille, J, (2005). The process mineralogy of precious
metals in LaRonde flotation products and its effect on process optimization. Proceedings of
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Disclaimer
Cytec Industries Inc. in its own name and on behalf of its affiliated companies (collectively, "Cytec")
decline any liability with respect to the use made by anyone of the information contained herein. The
information contained herein represents Cytec's best knowledge thereon without constituting any express
or implied guarantee or warranty of any kind (including, but not limited to, regarding the accuracy, the
completeness or relevance of the data set out herein). Nothing contained herein shall be construed as
conferring any license or right under any patent or other intellectual property rights of Cytec or of any
third party. The information relating to the products is given for information purposes only. No guarantee
or warranty is provided that the product and/or information is adapted for any specific use, performance
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or result and that product and/or information do not infringe any Cytec and/or third party intellectual
property rights. The user should perform its own tests to determine the suitability for a particular purpose.
The final choice of use of a product and/or information as well as the investigation of any possible
violation of intellectual property rights of Cytec and/or third parties remains the sole responsibility of the
user.
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