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We thank to Almighty ALLAH the creator of earth and sky and all the
things in between and WHO has given us a chance to complete this
project. We would like to thank our teachers who helped us by teaching
us the aspects involved in chemical engineering due to which we become
able to design a chemical plant. We would like to thank specially our
supervisor Dr. Umar Manzoor who guided us towards the right path
throughout the project & our co-supervisor Dr. Sikandar Rafiq, who
helped us in the technical section. At end we would like to thank our
friends for their co-operation, which was really helpful.
ABSTRACT
This report includes the work done on a final year project named Production of 10
tons Zinc Stearate using Zinc Dust. Chapter one & two discusses the introduction &
literature reviewed about the project, which includes the current industrial techniques
and past practices and gives a detailed review about the product. Chapter 3 is the
detail of our selected manufacturing process and its process flow diagram. Chapter 4
is about the Material Balance, the balances around individual equipments and overall
balance. Chapter 5 calculates the duty requirements and energy balances for
individual equipments. Chapter 6 covers the design calculation & Selection criteria of
our key equipments which are reactors, centrifuge & dryer. Chapter 7 includes the
selection of construction material for our equipments. Chapter 8 is about
instrumentation and controllers needed for our process. Chapter 9 is giving estimate
cost for the production of zinc stearate on basis of our designing. Chapter 10 contains
the Safety approach. And chapter 11 covers the environmental aspects of zinc
stearate.
TABLE OF CONTENTS
CHAPTER # 1
Introduction......................................................................................................... 7
Chemical composition of zinc stearate ............................................................................................... 8
Physical properties of Zinc Stearate [2] .............................................................................................. 8
Scope ................................................................................................................................................................. 9
CHAPTER # 2
Literature Review ............................................................................................. 10
Stearate ......................................................................................................................................................... 11
Stearic Acid ................................................................................................................................................. 11
Commercial Stearic Acid [3].................................................................................................................. 11
Macro crystalline Stearic Acids [3] ..................................................................................................... 11
High Stearic Acids [3] ............................................................................................................................... 12
Economics and Performance [3] .......................................................................................................... 12
Metallic Stearates [3] ................................................................................................................................. 12
Chemistry of Metallic Stearates [3] .................................................................................................... 13
Melting Point:........................................................................................................................................ 13
Hydrophobic Nature: ......................................................................................................................... 14
Importance of Metallic Stearates [3] .................................................................................................. 14
Characteristics of Metallic Stearates ............................................................................................... 15
Lubricant................................................................................................................................................. 15
Gel .............................................................................................................................................................. 15
Inhibitor ................................................................................................................................................... 15
How Stearates are involved in Rubber Manufacturing [3] ................................................ 16
Dry Process: ........................................................................................................................................... 16
Water-cooled systems......................................................................................................................... 17
Water-Dispersible Forms ................................................................................................................. 18
Metallic Stearates:.................................................................................................................................... 19
Calcium stearate................................................................................................................................... 19
Magnesium stearates .......................................................................................................................... 20
Aluminum stearates ............................................................................................................................ 21
Lithium stearates ................................................................................................................................. 22
Sodium stearates and Sodium OleateS ....................................................................................... 22
Zinc Stearate .......................................................................................................................................... 23
Preparation of Zinc Stearate [1] .......................................................................................................... 24
Precipitation (or double-decomposition) reaction ................................................................. 24
CHAPTER # 3
Process Selection ............................................................................................... 31
Process Selection: ..................................................................................................................................... 32
Precipitation process:......................................................................................................................... 32
Process Flow DiagraM ........................................................................................................................... 35
Process Detail ............................................................................................................................................. 36
Reactor 1.................................................................................................................................................. 36
Settling Tank.......................................................................................................................................... 36
Plate & Frame Filter Press .............................................................................................................. 36
Reactor 2.................................................................................................................................................. 36
Washing Unit ......................................................................................................................................... 36
Centrifuge ............................................................................................................................................... 37
Dryer ......................................................................................................................................................... 37
High Shear Mill .................................................................................................................................... 37
CHAPTER # 4
Material Balance ............................................................................................... 38
Dryer .............................................................................................................................................................. 39
Centrifuge .................................................................................................................................................... 39
Reactor 2 ...................................................................................................................................................... 40
Filter press ................................................................................................................................................... 41
Reactor-1 ...................................................................................................................................................... 41
OVERALL BALANCE .......................................................................................................................... 42
CHAPTER # 5
Energy Balance ................................................................................................. 43
Reactor 1[11] ................................................................................................................................................. 44
Reactor 2 ...................................................................................................................................................... 45
Dryer: ............................................................................................................................................................ 46
CHAPTER # 6
Designing & Selection of Equipments............................................................. 47
Reactors ........................................................................................................................................................ 48
Reactor 1.................................................................................................................................................. 48
Reactor 2.................................................................................................................................................. 52
Centrifuge .................................................................................................................................................... 55
Dryer .............................................................................................................................................................. 58
Designing Specifications ........................................................................................................................ 62
CHAPTER # 7
Material Selection ............................................................................................. 63
CHAPTER # 8
Instrumentation & Process Control ................................................................ 66
Reactor 1 ...................................................................................................................................................... 72
Volume & Level Control .................................................................................................................. 72
Reactor 1 Composition Control ..................................................................................................... 73
Storage of Zinc Sulfate ........................................................................................................................... 74
Reactor 2 ...................................................................................................................................................... 75
Composition ........................................................................................................................................... 75
Level & Temperature......................................................................................................................... 76
Tray Dryer................................................................................................................................................... 77
CHAPTER # 9
Cost Estimation ................................................................................................. 78
CHAPTER # 10
HAZOP .................................................................. Error! Bookmark not defined.
REACTOR 1[21] ............................................................................................................................................ 83
FILTER PRESS[21] ................................................................................................................................... 84
REACTOR 2[21] ......................................................................................................................................... 86
TRAY DRYER[21] ..................................................................................................................................... 88
CHAPTER # 11
Environmental Aspects .................................................................................... 89
Routes of Exposure [9] ............................................................................................................................. 90
Effects on Humans [10] ............................................................................................................................. 90
Methods to control exposure [10] ......................................................................................................... 90
References .......................................................................................................... 91
CHAPTER # 1
INTRODUCTION
SAPOCIFICATION REACTION
Molten Form
Transparent
Density
1.095g/cm3
Metal Content%
10.0 - 11.5 %
Melting Point
120 - 130C
Boiling Point
Decomposes
Water Solubility
Insoluble
[2]
ZINC STEARATE
SCOPE
According to our market survey the total demand for year 2012 was 4500 tons;
according to custom report 4000 ton was imported from China, Germany and
Indonesia, which clearly shows us the potential of manufacturing zinc stearate locally.
Our aim is to capitalize this opportunity by erecting a plant of production capacity of
3000 tons per year initially which could be further increased depending upon the
market response. According to our cost analysis report done in the proceeding
chapters per ton cost of production is 200000 PKR and its selling in open market is
285000 PKR this clearly shows us that we have a good profit margin.
Pakistan offers quiet favorable conditions for erection of such plant because of
availability of all the raw materials locally i.e. cheap labor, skilled man power and
high demand of the product. By manufacturing it locally we will sell our product at
lower cost as compared to imported ones because we wont be paying duties and our
transportation cost would be much less.
USES [2]:
The main industries which use zinc stearate as a key component in their
manufacturing processes are:
Coating/anti block
Paints industry
Lubricant
Mold Release
Acid neutralization
Paper coating
CHAPTER # 2
LITERATURE
REVIEW
10
STEARATE
Stearates are anionic form of stearic Acid (C17H35COO), It is salt or ester of Stearic
Acid.
STEARIC ACID
Stearic Acid is long chain of hydrocarbons that contains on group of carboxylic & one
group of methyl at their both ends. The hydrocarbon chain can vary from 3 carbons to
24 carbons i.e. propionic acid to lignoceric acid resp. It is a saturated acid having
single bonds between there adjacent carbons, that is why the hydrocarbon chain is
flexible and we can roll it up like a ball or stretch it in zigzag manner.
Stearic acid is mainly found in animal oils or hydrogenated veritable oils are of length
16 20 carbons.
[3]
Stearic acid that is used commercially cannot be used in pure state, for making soap
stearic acid used contains 30-60% of palmatic acid. In their pure state, these acids are
solid crystalline, opaque white materials having a waxy feel. The main source of
Stearic acid is animal source; small quantity of it can also be obtained from cotton
seed, corn, soya, coco and palm oils.
[3]
Stearic acids whose weight ratio of stearic to palmatic acid is 9:11 are known as
Macro crystalline Stearic acids. Commercially they were firstly produced by pressing
the fatty acids gained from animal tallow. Oleic from crystalline solid acid was
squeezed out by using technique of hydraulic pressure. The greater number of
pressings, the less oleic remained in the solid portion.
11
[3]
Macro crystalline in which the ratio of stearic acid is 50% more than the other acid is
referred as High Stearates. Stearic Acid provides crystalline part a fineness and
softness so when the ratio of stearic acid is less than 50 i.e. 50:50 or 90:10, the acid
that is produces is hard, tough & microcrystalline solid.
[3]
Selection of stearic acid to make metallic crystals is done on the basis of their variety
of applications and cost.
In rubber industry, stearic acid used is made from triple pressed stearic process in
which stearic acid is up to 70 %. It is not possible to make weight ratio of stearic acid
more than 70% so the processes use to create high stearic content are more extensive
an add cost to the end product.
12
[3]
MELTING POINT:
The physical properties are all fairly similar between all three stearates.
The most significant property difference as it relates to the rubber release
agents is their melting points
Melting point defines the usage of product on the surface of uncured rubber.
When the rubber compounder is making stock for compression, transfer molding,
hoses or extruded profiles, the molding or cure temperature and time duration will
limit what can be used on the surface of the compound.
With the low melt point of zinc stearate, this has typically not been a problem. The
zinc stearate will melt during molding and be absorbed into the compound without
leaving discoloration or defects on the surface of the final molded rubber part.
13
HYDROPHOBIC NATURE
Metallic Stearates consists of long chain stable hydrocarbons. This hydrocarbon chain
structure is water insoluble so it gives hydrophobic nature of metallic stearates. The
solubility parameter values of these stearates are low, and are similar to the common
elastomers. TABLE below compares solubility parameters of these stearates to
elastomers.
Comparison of Solubility Parameters between steartes and elastomers:
[3]
14
[3]
LUBRICANT
Main property of metallic stearates as lubricants is that they can bear high
temperature as they have relatively higher meting points as compared to other
release agents & lubricants. So metallic stearates when present in fine dry powder
from can act as dry lubricant also, like graphite. In most cases, the hydrophobic
nature of metallic stearates is highly desirable.
Lubrication and release properties, as well as water repellency, are characteristics
of all metallic stearates. In order to determine that metallic stearate is providing
the lubrication property we need to study the properties related to cations, chain
length and water of crystallization.
GEL
Gelling mainly depends on the type, polarity, viscosity of stearates as well as
solvent properties of the liquid component used. Aluminum stearates are the main
metallic stearates used for gelling property.
INHIBITOR
Calcium stearate, magnesium stearate and zinc stearate have stabilizing and
processing aid effects in a wide range of thermoplastics. Aluminum and
magnesium stearates are used as foam inhibitors for various suspensions.
15
DRY PROCESS
[3]
In dry process, stearates are applied or dusted onto the surface of the rubber by
passing the rubber through a trough or box containing the stearate. This method is
dusty but provides effective dry lubricating properties to the surface of uncured
rubber.
16
WATER-COOLED SYSTEMS
Another way in which the powdered stearates are applied is in water-cooled
systems.
The stearate is mixed on the surface of dip tank on which it starts to float. The
hydrophobic nature of metallic stearates allows the powder to stay on the surface
without getting wet. This process is also effective but cause dust & health issues.
For water-cooled systems, stearates are normally provided in 20-30% active pastes.
[3]
The paste is made by combining stearates, water & little quantity of alcohol.
These formulations allow for stearates to be added to the dip tanks directly or can
be premixed in tanks which provide a more thorough dispersion.
[3]
17
It is advised to premix these all before adding to dip tank. The benefit of using this
method is that stearate is still floating and can be used in water-cooled take-off
units. Figure 2-3 shows how these products would appear in a slab dip tank.
In floatable stearate dispersions dust problem can be minimized.
Here again the hydrophobic nature of metallic stearates is especially important
because this property allows for the cooling of rubber by water. Normal or cold
water is mainly used for heat removal.
This helps prevent scorching of these compounds before they are cured.
WATER-DISPERSIBLE FORMS
The metallic stearates are available in water-dispersible forms. These products
are normally 30-50% active and have surfactant packages that allow for
dispersibility throughout a dip tank
[ 3]
18
METALLIC STEARATES:
CALCIUM STEARATE
Calcium stearates are considered as health friendly stearates so they are becoming
part of life with good speed. They are insoluble in many solvents. We need to
slightly heat them in aromatic compounds, chlorinated hydrocarbons or vegetable
and mineral oils and waxes to make them soluble. Calcium stearates are mainly
used as lubricants, mold release agents and acid scavengers by the plastics
industry. They are used as an anti-caking additive for powder and granules in
pharmaceutical and cosmetics industry and as an excipient for pressing tablets.
The building industry uses it as hydrophobic agent & as inhibitor for moisture
absorption and preservation of building materials and construction. Calcium
stearate when heated dehydrates and softens at temperatures between 120 C and
130 C and takes a viscous consistency at approx. 160 C. This state lasts whilst
the material is heated occurring some slight discoloration.
19
MAGNESIUM STEARATES
Magnesium stearates are almost insoluble in normal solvents. They can hold
large quantities of water and take on a creamy consistency. Magnesium stearates
are used to improve the retention power of creams and semi-rigid wax articles as
well as to produce waxes. Since they are also skin & body friendly, they are used
by the cosmetics and pharmaceutical industry.
Magnesium stearates improve the free-flowing properties and are added as anticaking agents to powders. One of the principle uses of magnesium stearate is as a
tablet excipient in pharmaceutical dosage forms. Thermo stable magnesium
stearates are used as lubricants and release agents for the processing of
thermoplastics and thermosets.
20
ALUMINUM STEARATES
Aluminum stearates are produced by the precipitation process only. There are
three possible combinations of aluminum with fatty acids:
There might be different ratios but the lies between 1:1 and 1:3. That is why there
are many varieties of aluminum stearates, generically known as aluminum mono, di- or tri-stearate, they have different physical properties such as melting point,
free fatty acid and particularly the gelling properties. Aluminum tri- and distearates are used for thickening less viscous oils, whilst very viscous oils form
stiffer gel when combined with aluminum di- or mono-stearates.
The dropping point of aluminum greases usually range from 110 C to 120 C,
but we are in a position to offer special stearates whose dropping point exceed
200 C. All aluminum greases are highly hydrophobic and are characterized by
outstanding transparency and good adhesion to metallic surfaces. Like every
metallic stearate, aluminum stearate is also good water repellent. So we can use
them in coatings and building industry materials as water repellent ingredients.
Aluminum mono-, di- and tri-stearates are insoluble in many solvents like water,
lower alcohols, esters and ketones.
In benzenes, aromatic compounds and halogenated hydrocarbons as well as in
natural and mineral oils, they dissolve to a gel when heated.
21
LITHIUM STEARATES
Lithium stearates are best known for their excellent swelling properties. They
work better than aluminum stearates because properties like dropping point
temperatures of greases containing lithium stearates are much higher than those
of aluminum stearates. Lithium stearates are mostly used to thicken natural as
well as synthetic oils and help to increase the melting point and flexibility of
micro-crystalline waxes and paraffins. They are also used during the production
of light weight metal moldings. The advantage of lithium stearates with long fatty
acid chain lengths is the minimal residue after thermal treatment.
LITHIUM STEARATE
SODIUM STEARATE
22
ZINC STEARATE
Zinc stearate is a chemical compound that is white in color, has a fluffy powdered
appearance and is usually formed from a combination of stearic acid and zinc
oxide. It does not have a strong odor, although traces of a slight fatty acid scent
are not uncommon. Zinc stearate is also known as octa-de-canoic acid or zinc
salt.
ZINC STEARATE
[1]
-It is insoluble in non polar solvents such as alcohol and ether but becomes soluble in
aromatic hydrocarbons (e.g., benzene and chlorinated hydrocarbons) when heated.
-It is the strongest mold release agent among all metal soaps. It contains no electrolyte
and has a hydrophobic effect like other metallic stearates.
-It is mainly applied in the plastics and rubber industry where it is used as a releasing
agent and lubricant which can be easily incorporated.
-Its hydrophobic nature also makes it suitable for many different kinds of
applications.
-In order to make plastics, zinc stearate is combined with a co-stabilizing soap called
Ba-Cd[2] that helps to stabilize the plastic. It does this by mixing with the liquid,
which helps make the material more fluid called a plasticizer.
In paint and coatings industry zinc stearates are used for pigment suspension and to
improve grind ability and matting. The building industry uses powdered, precipitated
zinc stearates as hydrophobic agents for plasters.
23
[1]
24
DIRECT REACTION
In this method, reaction between stearic acid and metal oxide, hydroxide or carbonate
takes place at an elevated temperature in presence of large excess of water. Particle
size, and thus particle surface and bulk weight are influenced by the relation of stearic
acid to water. The higher the dilution, the smaller the particles and the larger the
surface will be. The metallic stearates produced by direct reaction are also relatively
fine powders with a high degree of purity, being free of water-soluble salts.
The reaction takes place at atmospheric pressure, but an advantage of this method is
that it can also be run under pressure and at higher temperatures (> 100 C) to
produce certain types of metallic stearates, which cannot normally be obtained under
atmospheric conditions by the direct reaction process. The product must be filtered
and dried to the final desired moisture content. Direct reaction in water generally
produces a more rounded, agglomerated particle, with higher bulk density than
precipitated stearates.
25
FUSION PROCESS
In this method, metal oxides or hydroxides and stearic acid are heated under pressure
with continual stirring beyond the melting point of the metallic stearate product. As
the melting point of most metallic stearates is higher than 100 C, that is why water
resulting from the reaction escapes as steam and we get a dry product. A variety of
physical forms can be produced from this process, depending on the melting range of
the final product. For relatively low or sharp melting metallic stearates, all forms
(pastilles, prills, flakes and powder) are generally feasible. A very high degree of
purity is achievable with the fusion process.
This method is efficient because no drying is required
Improved processing
Complete reaction
26
AV PROCESS:
This method is the combination of direct reaction and fusion processes. Metal oxides
or hydroxides are heated with a fatty acid and a small quantity of water in a
pressurized reactor, with the final temperature corresponding more or less to the
melting point of the soap. The added water and the water resulting from the reaction
are removed under reduced pressure at the end of the reaction cycle.
The AV process allows the very efficient production of a variety of stoichiometries,
including very pure products. AV technology is generally used to produce metallic
stearates in free-flowing granule or powder forms
27
28
FIELDS OF APPLICATION
BUILDING INDUSTRY
HYDROPHOBIC AGENTS
LACQUER INDUSTRY
LUBRICANT INDUSTRY
RUBBER INDUSTRY
PAPER INDUSTRY
COATING AGENTS
METAL INDUSTRY
PHARMACEUTICAL AND
COSMETICS INDUSTRY
29
We have selected this project of producing zinc stearate because it is most widely
used stearate in paint, polymers, paper & rubber industry. It gives us a good profit
margin which makes its production feasible and it is required in our local market.
All the raw materials for manufacturing are easily available in local market.
Although all the stearates have their own uses but nowadays our major concern is
environment & safety of the labor, production of some stearates carrying heavy
metals like lead & cadmium is prohibited in many countries due to their cancer
causing tendencies.
30
CHAPTER # 3
PROCESS
SELECTION
31
PROCESS SELECTION:
Several factors affect making a decision for selecting a manufacturing process, the
most important factor is the end to which the metallic soap will be subjected.
For example; in the metallic soap used for making plastics & rubber needs almost
zero moisture & salt content is needed. For these requirements, Fusion process is the
best. On the other hand for the application in cosmetic industry, fine particle size and
fluffy product is needed & these requirements lead to the precipitation process.
Economics is also a major factor in choosing a process.
In our case we are choosing precipitation process, although it is a bit expensive than
the fusion process yet its merits are for more. We can obtain a very high quality
product by this method of we are using quality raw materials & are carefully
following the procedure.
PRECIPITATION PROCESS:
This is a 2 stage process
Sodium salt of fatty acid is prepared by treating caustic soda (at 800C) with stearic
acid that produces sodium salt. The stoichiometric amount of solid stearic acid is
mixed in caustic soda with vigorous stirring.
In other reaction 10-20% metallic salt solution is prepared; this salt is added gradually
in the precipitation tank. When the reaction is finished the resultant is filtered &
washed then can be dried in the tray dryer
The dried cake may be ground to fine powder; the resulting powder is fine, white &
light
C17H35COOH
NaOH
C17H35COONa
Stearic acid
Caustic Soda
Sodium Soap
C17H35COONa
ZnSO4
(C17H35COO)2Zn
Sodium Soap
Zinc Sulfate
H2 O
Na2SO4
Zinc Stearate
32
After approx half the water needed is run into the reaction vessel then caustic
soda is added
The barrel or drum containing the fatty acid is rolled over the dumping pit and
allowed to be drain
The steam is turned on slightly & the fatty acid is pumped to the reaction
vessel with the pumps throttled so that the fatty acid entering the lye in the
kettle is easily dispersed by swallowing liquid
After all the fatty acid is added steam agitation is continued until a clean liquid
is produced
The bottom valve in the tank is opened & the pump is started again to wash
out the lines still containing fatty acids, the soap in the kettle is tested with
phenolphthalein indicator, a slightly pink color shows neutral soap
The soap is diluted to a proper concentration while agitating. If the solid acid
is used they are added directly to control conc. of caustic soda
HYDROLYSIS:
If the sodium soaps are highly hydrolyzed one would expect to find much metal
hydrate as well as free fatty acid in the precipitated soap. Mc Bain and Hey found that
hydrolysis depends on the molecular mass of the fatty acid. The higher the soap in the
homologous series the higher will be hydrolysis. In conc. Solutions there is less
hydrolysis
PRECIPITATION OF METALLIC SOAP:
There are three different methods of precipitation of metallic soaps:
1- ADDITION OF SOAP TO SALT SOLUTION:
The solution of metallic soap is slowly added to the salt solution while agitating. If the
temperature of the soap is high enough and stirring sufficient, a very finely divided
suspension of metallic soap in the alkali soap slowly forms until much of the latter has
been precipitated at which point the mass coalesces. If salt solution is added too
quickly or if temperature is too low then very viscous, unworkable mass which is
certain to occlude large quantity of soap and alkali salt results. This alkali soap cannot
33
be removed even ob repeated washings. Because of this the finished metallic soap
tends to sludge when dissolved in hydrocarbons
2- ADDITION OF SALT TO SOAP SOLUTION::
The alkali soap solution may be slowly added to the metal salt solution while
agitating. If soap is slowly added and the temperature is high enough then a layer of
molten metallic soap which is quite workable and is not excessively hydrated forms a
precipitation progress. If the soap is added too quickly and temperature is kept low
then unworkable mass will be produced.
34
35
PROCESS DETAIL
REACTOR 1
In reactor # 1, Zinc Oxide along with 16% excess sulfuric acid are fed, reaction takes
place between them at room temperature but due to exothermic nature of this reaction
temperature of reactor rises up to (1700C). After 90% completion of reaction product
is formed that is zinc sulfate with water. This zinc sulfate is in form of slurry that
contains impurities & 10% unreacted reactants.
SETTLING TANK
The products are then entered in settling tank where the product cools down to room
temperature and settling occurs for about 3 to 4 hours. Due to density difference the
impurities and unreacted metal oxide settles and the zinc sulfate slurry is pumped to
plate and frame filter press
PLATE & FRAME FILTER PRESS
Zinc sulfate slurry is entered in filter press where the mud and unsettled impurities are
filtered; this feed contains 75% zinc sulfate and 25% of mud. It filters 95% of zinc
sulfate 5% is mud. Mud is separated here, Zinc sulfate is sent to a tank.
REACTOR 2
In reactor 2, two reactions are taking place. In first reaction caustic soda reacts with
17% excess stearic acid this reaction takes place at room temperature and 90% of
reactants converts into sodium stearate and water.
When the reaction is complete then zinc sulfate is added gradually in the reactor that
reacts with sodium stearate, heat is provided for starting the reaction and stirring is
done continuously for proper reaction. This second reaction also completes 90% and
then converts into zinc stearate of mass along with sodium sulfate.
WASHING UNIT
The products are allowed to cool down by adding cold water in the reactor. Sodium
sulfate, water and unreacted masses are dissolved in added water only zinc stearate
slurry is separated from reactor because it is hydrophobic by nature.
36
CENTRIFUGE
In centrifuge zinc stearate is entered that contains 60% moisture and 40% zinc
stearate. Centrifuge works on the principle of centrifugal force and helps to remove
the moisture and the zinc stearate at the end contains only 30% moisture.
DRYER
Zinc stearate containing 30% moisture is entered in tray and shelf dryer at room
temperature and air is used for purpose of drying. Air at 1300C is entered in the dryer,
this is basically batch drying process and drying is taking place by conduction.
Slurry is placed on hot trays at room temperature but due to contact with hot trays the
moisture starts to evaporate and after complete evaporation of moisture from initial
moisture temperature of zinc stearate raises up to 110oC; dried product contains 3%
inherent moisture which was not removed by evaporation.
Now zinc stearate is in form of solid granules which are stored in storage silo to cool
them down at room temperature
HIGH SHEAR MILL
Zinc Stearate in form of granules is entered in high shear mill which simply crush
them in to small size and final product in form of powder is collected.
37
CHAPTER # 4
MATERIAL BALANCE
38
DRYER
Product (F3) containing 70% Zinc Stearate and 30% moisture is entering to give
product (F1) containing 97% Zinc Stearate. Water (F2) is removed separately
F3 = F1 + F2
Applying balance on Zinc Stearate;
F1= 10000 kg
We get
F1
F2
F3
Zinc Stearate(kg)
9700
0
9700
Water(kg)
300
3857.142857
4157.14286
Total (kg)
10000
3857.142857
13857.14286
CENTRIFUGE
Product (F5) containing 40% Zinc Stearate and 60% moisture is entering to give
product of (F3) containing 70% Zinc Stearate. Water (F4) is removed separately
F5 = F3 + F4
We calculated F3 = 13857kg
We get
F5 = 24250kg product
F3
F4
F5
F4 = 10392.85 kg water.
Zinc Stearate(kg)
9700
0
9700
Water(kg)
4157.142857
10392.85714
14550
Total (kg)
13857.14286
10392.85714
24250
39
REACTOR 2
Stearic Acid (F7) and Caustic soda (F8) reacts to form Sodium stearate which
then reacts with zinc sulfate (F5) to form Zinc Stearate (F9), Sodium Sulfate
(F10) & water (F11)
2 C17H35COOH + 2 NaOH
2 C17H35COONa + ZnSO4
2 C17H35COOH + 2 NaOH + ZnSO4
2 C17H35COONa + 2H20
(C17H35COO) 2 Zn + Na2SO4
F5 + F7 + F8 F9 + F10 + F11
We get;
We have
= 9700/0.90
= 10777kg
=10777/631
= 17.08kgmoles
Taking Stearaic acid in excess 17% and 17000kg of water is added in the stearic acid
to provide reaction medium
Components
Moles
(kgmole)
Moles in
Reaction
(kgmole)
Molecular
mass
(kg/kgmol)
Mass in
Reaction(kg)
Inlet
F9
F6
F7
ZnSO4
NaOH
C17H35COOH
1
2
2
17.08047191
34.16094383
39.96830428
161
40
284
2749.955978
1366.437753
11350.99842
FM
C17H35COONa
34.16094383
294
9038.985737
945.9165346
18
17026.49762
H2 0
Total
Outlet
S.S
41532.87551
3031.100546
1
17.08047191
631
9700
F10
Reactants
(C17H35COO) 2
Zn
Na2SO4
17.08047191
142
2182.884311
F8
H2 0
34.16094383
18
17579.90491
FM
Total
C17H35COONa
34.16094383
294
9038.985737
F5
41532.87551
40
FILTER PRESS
Product (F12) containing 75% Zinc Sulfate and 25% Mud is entered in a filter
press that gives product (F9) containing 95 % Zinc Sulfate and Mud (F11) which
is separated.
F12 = F9 + F11
Applying balance on Zinc Sulfate;
where F9 = 2749.95kg
Mud (kg)
870.819393
137.4977989
733.3215942
Total(kg)
3483.277572
2749.955978
733.3215942
REACTOR-1
Zinc Oxide (F14) is reacted with Sulfuric acid (F15) to produce Zinc Sulfate
(F12) and Water (F13)
ZnO + H2SO4 ZnSO4 + H2O
We know F12= ZnSO4 = 2612.45 kg
Reaction conversion is 90 %
2612.45/0.90
=2902.722kg
2902.722/161
=18.02kgmoles
18.02*1.16
=20.9kgmoles
Inlet
F14
F15
Components
Moles
(kgmole)
Moles in
Reaction
(kgmole)
Molecular
mass
(kg/kgmol)
Mass in
Reaction(kg)
ZnO
H2SO4
1
1
18.02938702
20.91408894
81
98
1460.380349
2049.580716
MUD
Total
Outlet
S.S
F12
F13
Total
1393.311029
4903.272094
Reactants1
ZnSO4
H2O
MUD
18.02938702
161
18.02938702
18
605.4268161
2612.458179
292.0760697
1393.311029
4903.272094
41
OVERALL BALANCE
Components
Molecular
Mass
Mass In Reaction
(kg)
F14
ZnO
81
1460.380349
F15
H2SO4
98
2049.580716
F6
NaOH
40
1366.437753
F7
C17H35COOH
284
11350.99842
in R2
In
washing
unit
H2 0
18
17026.49762
Inlet
H2 0
14550
Mud
1393.311029
49197.20589
Total
Outlet
S.S(R1)
F13
F11
From
settling
Tank
SS(R2)
F10
MUD
522.4916359
Na2SO4
3031.100546
2182.884311
F8
H2 0
18
17579.90491
F4
F1
F2
Total
H2 0
(C17H35COO) 2 Zn
H2 0
18
631
18
10392.85714
10000
3857.142857
H2 0
Mud
18
605.4268161
292.0760697
733.3215942
49197.20589
42
CHAPTER # 5
ENERGY BALANCE
43
REACTOR 1 [11]
Zinc Oxide and Sulfuric acid are reacting, this reaction takes place at 300C but due to
exothermic reaction the reactor temperature rises up to 1700C, the product zinc sulfate
in the form of muddy solution is obtained
Enthalpy
Tref
T2
Cp
[13]
Mass
Moles
(kg)
Heat (Q)
Enthalpy
of
(kJ)
(kJ/kg)
Formation
(kJ)
zinc oxide
1460
18
25
30
0.52
3796
2.6
-348
sulfuric acid
2049
20
25
30
1.704
17457
8.52
-814
Heat IN
21433
zinc sulfate
2612
18
60
170
1.39
399374
152.9
-983
water
292
18
60
170
4.18
134261
459.8
-285.8
Heat OUT
533635
Products
Reactants
(-983-285)
(-348-814)
-1268
-1162
-106kJ
44
REACTOR 2
Stearic Acid is solid form it is mixed with hot water to convert in liquid form. Caustic
soda reacts with stearic acid and form sodium stearate, this sodium stearate reacts
with zinc sulfate produced in reactor 1 and gives our main product zinc stearate along
with sodium sulfate and water. The temperature of reactor rises up to 120oC
2 C17H35COOH + 2 NaOH
2 C17H35COONa + ZnSO4
2 C17H35COONa + 2H20
(C17H35COO) 2 Zn + Na2SO4
For Reaction 1:
Enthalpy of formation for C17H35COONa = -1978kJ
Hr
198.24Kj
So this is endothermic reaction and we have to provide heat to start this reaction
For Reaction 2:
Hr
-112kJ
So this is exothermic reaction and heat will be generated during this reaction
For Overall Reaction:
Hr
Mole
Tref
T2
Cp[13]
Heat
of
(kg)
(kmol)
(OC)
(OC)
(kJ/kg OC)
(kJ)
Formation
(kJ)
water
17026
945
25
120
4.18
6761024
caustic soda
1366
34
25
120
1.3
168701
-851.84
stearic acid
11350
39
25
120
1.8
1940850
-1896
zinc sulfate
2749
17
25
120
0.97
253320
-983
Heat IN
9123895
water
17579
976
25
120
4.18
6980620
-571.6
zinc stearate
9700
17
25
40
2.79
405945
-1686
sodium sulfate
2182
17
25
40
1.29
42221
-1387
Heat OUT
7428786
45
DRYER:
Moist Product is entering in the dryer at room temperature along with hot air
(1300C), dry product is obtained at 1100C along with water, and air is removed at
303K
Mass
(kg/day)
Tref
Cp[13]
zinc stearate
13857
30
air
8574
130
water
3857
60
zinc stearate
10000
60
air
8574
T2
50
Enthalpy
(KJ/kg)
Heat (kJ/day)
2.79
55.8
1.01
404
110
3.42
171
806113
110
2.79
139.5
1395000
30
303
3463944kg/day
773220
46
CHAPTER # 6
DESIGNING
&
EQUIPMENT SELECTION
47
REACTORS
We are producing 10 ton zinc stearate per day; it is not a very large quantity so batch
reactor is sufficient for our process. In batch reactor we can achieve high conversion.
Quality of product can be improved in batch reactor as after every batch we can clean
it and remove any impurities, which in case of continuous reactor is difficult to do.
As the reaction time is high (30-45 min) if we choose continuous reactor, its length
would be quite large and would require a large area for it.
Our drying time is high; if we choose a continuous process material will start
accumulating before the dryer.
REACTOR 1
Data:
Comp.
Density
Mass
(kg)
Volume
(kg/m )
Moles
(kgmole)
(m3)
Inlet
F1
ZnO
5606
18.0246914
1460
0.26043525
F2
H2SO4
1800
20.9081633
2049
1.13833333
3509
1.39876858
Total
7406
=12.89kmol/m3
Design equation:
d CA/ dt = -rA[15]
We have taken H2SO4 in excess & by assuming first order reaction
dCA/dt = -KCA
dCA/dt = -Kdt
When; t=0, CA = CAO;
We get
t[15]
As we know
CA
CA
=12.89(1-0.90)
CA
=1.289kmol/m3
assume X
=90%
48
Suppose K=0.05/min;
=(ln(12.89/1.289))/0.05
tr
=45min
Filling Time =
tf
Reaction time=
tr
=45 min
Cleaning Time =
tc
=120 min
TB
=4.75hrs
Vf = 1.129*1.30= 1.468m3
Dimensions:
H/D = 1.5
VF=3.14*L*(D2)/4)
D3= (1.468*4)/(1.5*3.14) =1.24m3
D=1.07m
H=1.5*1.07m
H=1.614m
Working pressure =
Total Pressure=
Ps=
7406*9.8*2.09/1000
Ps=
152.336kPa
Pw=
335kPa
=152+335=
487.46kPa
49
Outside diameter =
Di + 2(thickness)
= 1.07m+2(0.009) m = 1.09m
Mechanical Design:
Agitator Dimensions: [17]
Impeller Diameter =Da=
Dt/3
= 1.07/3
= 0.35m
=0.35m
Da/4
=1.07/4
=0.26m
Da/5
=0.35/5
=0.07m
As our reactor is not very big so 1 impeller will be enough for proper mixing or
stirring
Moles
(kmol)
T1 (OC) T2(OC)
Cp
Heat
(kJ/kg OC)
(kJ)
ZnO
1460
60
25
30
0.52
3796
H2SO4
2049
70
25
30
1.704
17457
Total
21253
Zn SO4
2612.5
60
60
170
1.39
399374
H2 O
292.07
60
60
170
4.18
134583
533957
50
= 1 in
OD
= 1.05 in
ID
=0.824 in
Flow area
= 0.534 in2
External surface/lin ft
=0.344ft2/ft
= 1.4 joule/s.m2.K
Q=UA*delta T[18]
A=Q/U*delta T
A= (heat transfer)
=18.403 ft2
=1.5 ft2
=12 turns
=3.5 ft
L= pie*D*no. of turns
=132 ft
Pressure drop
[18]
M= Q/cp(delta T)
M=506093/0.999(104-77)
=18777 lb/hr
V=M/density=18777/62.5
=0.08 ft3/s
Velocity=(V/Flow Area)
=5.71 ft/s
G=M/flow area
G=M/Flow Area
=1341214 lb/hr.ft2
Viscosity=u
=1.96lb/ft.hr
Equivalent diameter
=0.05
=34567
=0.006
=11.95 ft
Pressure Drop
=5 psi
51
REACTOR 2
Data; Reaction 1:
Density
Mass
(kg)
Volume
(kg/m )
Moles
(kgmole)
C17H35COOH
1103
39.9683028
11351
10.2910227
NaOH
water
2130
1000
3233
34.16075
945.888889
Comp.
Inlet
F1
F2
Total
CAO
(m3)
1366.43 0.64151643
17026
17.026
29743.43 27.9585391
=1.22kmol/m3
=34.16/27.958
Design equation:
d CA/ dt = -rA[15]
We have taken C17H35COOH in excess & by assuming first order reaction
dCA/dt = -KCA
dCA/dt = -Kdt
When; t=0, CA = CAO;
We get
As we know
CA=CAO (1-X)
assume X
=90%
CA=1.22(1-0.90)
CA =0.122kmol/m3
Suppose K=0.05/min;
Filling Time =
Reaction time=
tr =46 min
Cleaning Time =
TB1=3.76hrs
52
Data; Reaction 2:
Density
Comp.
(kg/m )
Moles
(kgmole)
Mass
(kg)
Volume
(m3)
Inlet
F1
C17H35COONa
1103
30.7448299 9038.98
F2
ZnSO4
3540
4643
11788.9 8.97173
Total
CBO
8.1949
=1.906kmol/m3
=17.08/8.97
Design equation:
d CB/ dt = -rA
We have taken C17H35COOH in excess & by assuming first order reaction
dCB/dt = -KCB
dCB/dt = -Kdt
When; t=0, CB = CBO;
We get
As we know
CB=CBO (1-X)
assume X
=90%
CA=1.906(1-0.90)
CA =0.1906kmol/m3
Suppose K=0.08/min;
Filling Time =
Reaction time=
tr =28 min
Cleaning Time =
tc =90 min
te= 120min
TB2=5hrs
53
Final Volume =
Vf = 14.20*1.4
Dimensions:
H/D = 1.5
= 19.88m3
VF=
3.14*L*(D2)/4)
D3=
(19.88*4)/(1.5*3.14) = 16.88m3
D=
2.56m
H=
1.5*2.56m
H=
3.84m
3233*9.8*4.23/1000
Ps=
134kPa
Pw=
295kPa
134+295 =
429kPa
Working pressure =
Total Pressure=
Outside diameter =
Di + 2(thickness)
= 2.56m+2(0.014) m = 2.58m
Mechanical Design:
Agitator Dimensions:
Impeller Diameter =Da=
Dt/3
= 2.56/3
= 0.85m
=0.85m
Da/4
=2.56/4
=0.64m
Da/5
=0.85/5
=0.17m
As our reactor is not very big so 1 impeller will be enough for proper mixing or
stirring
54
CENTRIFUGE
Zinc Stearate(kg)
Water(kg)
Total (kg)
F3
9700
4157.142857
13857.14286
F4
10392.85714
10392.85714
F5
9700
14550
24250
24250/24
1010.41kg/hr
Feed entering
1010.41kg/hr
Density of feed
1020kg/m3
Volume of feed
0.99m3/hr
Volume of centrifuge
1.25*0.99 = 1.23 m3
2
D H
4
H/D
0.625
D3
2.52m3
1.36m
&
0.85m
0.68 m
msolid
577.37 kg/hr
solid
1100 kg/m3
Vsolid
0.52 m3/hr
Vsolid
H (R2 IRC2)
IRC
0.52m
0.68 0.52
.16 m
16 cm
Thickness of Cake
R
D/2
H (R2 IRS2)
IRS
0.30m
55
0.000142 n2D
190.66 g
1
2 (R 2 IRS 2 )
2
2.205 106N.m2
Diameter of hole
5 mm
0.0000196m2
DH
3.14 1.36*0.85
3.63 m2
No. of holes
3.63
0.0000196
No. of holes/m2
2500
IF =
Where
Radius of Basket
R1
R e (e is thickness of liquid)
R1
0.56 m
70.51kg.m2
Ib = m2 R2
Where
m2
Mass of Basket
m2
D H S m
49 kg
Ib
22.93m2
IF + Ib
93.45Kg m2
RCF
Centrifugal Pressure
Pc
= 9094
Power Calculations
So
If
m1
(R 2 R 12 )
2
56
d
dt
93.45
161 104.67
16846 Watts
16.846 KW
23H.P
104 .67
= 161 N-m
60
SPECIFICATION SHEET
1.
Equipment
Centrifuge
2.
Type
3.
Method of operation
Batch wise
4.
No. Required
5.
Function
6.
Basket Diameter
1.36m
7.
Speed
1000 rpm
8.
190.66 g.
9.
23H.P.
10.
11.
2500
57
DRYER
Drying Operation:
Drying of solids means the removal of relatively small amounts of water or other
liquid from the solid material to reduce the content of residual liquid to an acceptably
low value. Drying is usually the final step in a series of operation and the product
from a dryer is often ready for final packaging.
Drying Selection [4]:
Our feed is slurry of zinc stearate containing 60% moisture, and we are producing this
in a batch process do we have the following options:
CLASSIFICATION OF DRYERS
We have selected atmospheric tray dryer because our required temperature is not very
high and also our feed is not heat sensitive, tray dryer works on the principle of
conduction, hot air heats the trays and when the slurry is spread on the trays heat
transfer operation takes place between slurry and trays. Feed takes sufficient time to
get dry so that maximum moisture is removed. Tray dryers have high labor costs but
they are good to handle small amount of feed. We can easily clean the trays by taking
them out of the shelves
58
DATA:
Amount of feed (ms)
13857kg/day
30oC
30% of ms 4157.143kg/day
10000kg/day
97% of mp 9700kg/day
Moisture in Product(X2)
3% of mp
300kg/day
Temperature of Product(Tp)
110oC
Cp of solids
2.79kJ/kgoC
Cp of water
4.18kJ/kgoC
Heating Medium
Air
130oC
404KJ/kg
251.5KJ/kg
2270KJ/kg
ms - mp
Total Evaporation
3857.14kg/day
100
700
200
load
100%
80%
60%
59
Zone
1
Operation
Solids temp.
o
Constant-rate
Heating
Steam temp.
o
Falling-rate drying
drying
130
130
130
130
130
30
70
70
70
100
100
60
60
60
30
Tm
LMTD. oC
(T t o ) (T t i ) [18]
ln[(T t o ) / (T t i )]
78
60
43
Heat Loads,
KJ/hr
(KJ/hr)
Day
kg-mol
24 hr
Day
= 45105 KJ/hr
Liquid heat
load
= 33828 KJ/hr
= 23695 KJ/hr
=1282.5 KJ/hr
Evaporation
heat load
251 .5 x3857
24
(KJ/hr)
=40419 KJ/hr
Totals of heat
=68800
load (KJ/hr),
Surface area,
m2
= 40419
Qh
Tmh . h h . L n
= 8.78m2
= 1.20 m2
Qc
Tmc . h c . Lc
=35111
=
Qf
Tm f . h f . Lf
= 6.76 m2
60
At
= 8.78+1.20+6.76
=16.74m2
Excess Area
20%
=1.2*16.74
=20.08m2
Qt
=68800+40419+35111
=144331 KJ/hr
Qt/HAir =144331/404
Drying Rate
mv
=2586.588kg/hr
h y (T Ti ) * A
=516.50kg/hr
ms
X c
=
X1 X c X c ln
v
m
X 2
At
=12.86hrs
=16.74m2
= .78+1.20+6.76
Width
[20]
= (A)^0.5
=4.09m
= (A)^0.5
=4.09m
=Atray
=0.7m2
=0.05m
= Aspace
=0.0025m2
=24
Number of Trays
=24/2
=Ht
=0.04m
=12(0.04+0.05)
=1.08m
=15% =1.15*1.08
=1.24.m
0.7m2 each
0.83
0.83
0.04
Drying Chamber
4.09
4.09
1.08
Dryer
4.48
4.48
1.24
61
DESIGNING SPECIFICATIONS
Equipment
No. Required
Centrifuge Separator
Tray Dryer
Specifications
Volume
1.46m3
Height
2.09m
Pressure
487KPa
Volume
19.88m3
Height
4.23m
Pressure
429kPa
Basket Diameter
1.36m
Rotations
1000rpm
Centrifugal Force
190.66g
No. of holes/m2
2500
357.25kg/hr
Throughput
516.50kg/hr
Area of Dryer
20.08m2
Height of Dryer
1.24m
Heat Required
144331kJ/hr
62
CHAPTER # 7
MATERIAL
SELECTION
63
Equipment
Material
Options
316 Stainless Steel
Storage Tank
H2SO4
Selection[21]:
316 SS is best material
to store sulfuric acid in
corrosion free
environment
316 SS is the selected
material because as
compared to Glass
Reactor 1
ZnO,
Lined Steel it is
H2SO4,
ZnSO4
Carbon Steel
Settling Tank
ZnSO4, H2O
& unreacted
ZnO, H2SO4
Carbon Steel
ZnSO4, H2O
PVC-coated iron
& Mud
Aluminum
Cast iron
Wood
64
Storage
Tank
ZnSO4, H2O
C17H35COOH,
Reactor 2
NaOH, ZnSO4
316 SS is best
material to store ZnSO4 in
corrosion free environment
Carbon Steel
using SS here
We can use 304 SS
Washing
Unit
(C17H35COO)2Zn
Na2SO4
H2 0
Carbon Steel
Centrifugal
(C17H35COO)2Zn
Filter
Tray Dryer
(C17H35COO)2Zn
Stainless steel
Carbon steel
65
CHAPTER # 8
INSTRUMENTATION
&
PROCESS CONTROL
66
67
A DP Cell will often include an internal mechanical feature which protects the central
sensing element from damage caused by high overpressure on one side of the DP
Cell. This high overpressure feature is often called a Mechanical Stop because it
limits the travel of the isolation diaphragm on either side of the DP Cell.
Flow measurement and control [7]:
Flow indicators are used to control the amount of liquid. Also all manually set streams
require some flow indication or some easy means for occasional sample measurement.
For accounting purposes, feed and product streams or metered. In addition utilities to
individual and grouped equipment are also metered. Most flow measures in the
industry are/ by Variable Head devices. To a lesser extent variable area is used as are
many types available as special metering situation arise.
Due to simplicity and dependability, the Venturi tube flowmeter is often used in
applications where it's necessary with higher Turn down Rates, or lower pressure
drops, than the orifice plate can provide. In the venturi meter the fluid is accelerated
through a converging cone of angle 15-20o and the pressure difference between the
upstream side of the cone and the throat is measured and provides a signal for the rate
of flow.
The pressure recovery is much better for the venturi meter than for the orifice plate.
The venturi tube is suitable for clean, dirty and viscous liquid and some slurry
services.
68
The globe valve must be installed in the proper relation to the media flow as indicated
by the flow direction arrow marked on the valve body. This valve is considered unidirectional and must be installed with the pressure side or inlet under the seat.
Butterfly valve:
Butterfly valve is used to control flow of material through a circular pipe or tube.
Certain dry materials may also be handled through butterfly valve. Valve body can be
made up of cast iron, ductile iron, aluminum, carbon steel, stainless steel and exotic
metals. They offer an excellent, economically priced, positive shut-off valve for
handling materials; they are easily displaced by valve disc as it closes. When handling
this type of material, butterfly valve provide a reliable, bubble-tight, bi-directional
shut off
Ball Valve [23]:
Ball valves are flow valves that are quarter-turn and straight through apparatuses.
These valves allow for shut-off or purposes of control. They have a round closure
element that contains a matching pair of rounded seats. These seats allow necessary
sealing to take place. The ball valve pressure rating and materials used determines
what kind of seat is required. Not all valve seats are the same. Some are of the single
molded variety while others have higher- pressure ratings, which often include a
design known as a "trunnion." This design means that each ball valve face is sealed
separately, not together.
Ball valves have many good points and are often considered superior to many other
kinds of valves. Ball valves are very easy to use and can both maintain and regulate
three things-high pressure, high volume and high flow of temperature. Other
advantages of ball valves are that they are sturdy devices that can be purchased for a
low price and they have a long service life. An added plus is that the regulating
element's design makes it easy for the ball valve to work without concern about side
loads, which often plague globe or butterfly valves. The ball valve design allows for
the easy ability to fix the seats if a problem arises and also seals without having to
take away the body of the valves from the line.
Ball valves can be found in a number of different styles. Some of these include onepiece, two-piece, three-piece and lastly, what is referred to as flanged body
69
construction. Each form of ball valve has its own good and bad points, all dependent
on what each application calls for. Ball valves are made using an assortment of
materials, some of which include brass, bronze, cast iron, copper ductile iron, metal
alloys, stainless and other steel types, and plastics (including CPVC and PVC). Ball
valves are to be found being used in a number of different industries.
Pressure Relief Valve [24]:
A pressure Relief Valve is a safety device designed to protect a pressurized vessel or
system during an overpressure event.
An overpressure event refers to any condition which would cause pressure in a vessel
or system to increase beyond the specified design pressure or maximum allowable
working pressure (MAWP).
The primary purpose of a pressure Relief Valve is protection of life and property by
venting fluid from an over pressurized vessel.
Many electronic, pneumatic and hydraulic systems exist today to control fluid system
variables, such as pressure, temperature and flow. Each of these systems requires a
power source of some type, such as electricity or compressed air in order to operate.
A pressure Relief Valve must be capable of operating at all times, especially during a
period of power failure when system controls are nonfunctional.
The sole source of power for the pressure Relief Valve, therefore, is the process fluid.
Once a condition occurs that causes the pressure in a system or vessel to increase to a
dangerous level, the pressure Relief Valve may be the only device remaining to
prevent a catastrophic failure. Since reliability is directly related to the complexity of
the device, it is important that the design of the pressure Relief Valve be as simple as
possible.
The pressure Relief Valve must open at a predetermined set pressure, flow a rated
capacity at a specified overpressure, and close when the system pressure has returned
to a safe level. Pressure Relief Valves must be designed with materials compatible
with many process fluids from simple air and water to the most corrosive media. They
must also be designed to operate in a consistently smooth and stable manner on a
variety of fluids and fluid phases.
70
Diaphragm pumps have good suction lift characteristics, some are low pressure
pumps with low flow rates; others are capable of higher flow rates, dependent on
the effective working diameter of the diaphragm and its stroke length. They can
handle sludges and slurries with a relatively high amount of grit and solid content.
Slurry Pump:
A slurry pump is a type of centrifugal pump, lobe pump or peristaltic hose pump
in physics principle that increases the pressure of liquid and solid particle mixture
(aka slurry), through centrifugal force (a rotating impeller) and converts electrical
energy into slurry potential and kinetic energy.
Slurry pumps are widely used to transport corrosive/abrasive and high concentration
slurry in many industries such as Gold, Silver, Iron ore, Tin, Steel, Coal, Titanium,
Copper, Mineral sands, Lead and Zinc. Various other industries include Molybdenum,
Electric Utilities, Oil Shale, Water & Sewage Utilities, Building areas, Sand &
Gravel, Tobacco and Agriculture (hog, poultry, dairy manure) and are grouped by:
shaft position from the horizontal: horizontal and vertical slurry pump
impeller suction way: single suction and double suction slurry pump
pump casing structure: solid casing, horizontal split-case, and vertical split-case
slurry pump
71
REACTOR 1
VOLUME & LEVEL CONTROL
In volume control, level measuring device measures the level in the reactor and then
compares it with the set value and then signal is transferred to the controller which
changes the flow rate with the help of final control element (valve) and maintains the
volume in the reactor.
In temperature control, thermocouple measures the temperature inside the reactor and
then it compares it with the set value and then signal is transferred to the controller,
which changes the flow rate of water to control the temperature inside the reactor.
72
COMPOSITION CONTROL
During filling time of reactor to control the composition in the reactor, composition
analyzer measures the composition of material inside the reactor and changes the flow
rate inside the reactor.
73
Level measuring device measures the level inside the storage tank and if the level is
about to exceed the volume of the storage tank, emergency drain will open and
material will go in another small tank to avoid wastage of material.
74
REACTOR 2
COMPOSITION
75
In case of volume control, level measuring device measures the level of material
inside the reactor and then signal is transferred to compare it with the set value and
then controller changes the flow rate with the help of the final control element (valve)
inside the reactor.
In temperature control, thermocouple measures the temperature inside the reactor and
the signal is then transferred to compare it with the set value, in case of any deviation
the controller changes the flow rate of steam with the help of final control element
(valve) to maintain the temperature inside the reactor at the desired value.
76
TRAY DRYER
In dryer, thermocouple measures the temperature inside the dryer and then signal is
transferred to compare it with the set value , in case of any deviation controller
changes the flow rate of air to maintain the temperature inside the dryer at the
required value.
77
CHAPTER # 9
COST
ESTIMATION
78
Equipment
Equipment
Specifications
[26]
Cost
2012
Materials of
Construction
Equipment
Cost in $, Jan
2013
CE index =
564.2
1*4000
4m3
32357
316 Stainless
Steel
1*46761
Reactor
Turbine single
impeller Agitator
2 m3
8 kW
30615
28862
Stainless steel
316 Stainless
Steel
1*44244
1*41710
4m3
32357
316 Stainless
Steel
1*32357
Horizontal
Centrifugal pump
6m3/s
8716
Cast Steel
Casing
1*12598
Plate-and-frame
filter
2.5 m2
7361
Rubber Covered
Iron
1*10638
Horizontal
Centrifugal pump
6m3/s
8716
Cast Steel
Casing
1*12598
4m3
32357
316 Stainless
Steel
1*46761
Hopper for
C17H35COOH
1*4000
1*4000
Reactor
Single Impeller
Agitator
20 m3
8 kW
118541
28862
Stainless Steel
Stainless Steel
1*1717313
1*41710
Washing Unit
30m2
321373
1*464443
Centrifuge
Bowl dia =
1.36m
20m2
266831
36312
304 Stainless
Steel
316 Stainless
Steel
Stainless Steel
200 kW
10019
Carbon steel
1kg/s
157843
1*14479
1*4000
1*228112
3140820
Atmospheric
Tray dryer
Heater
Storage
Shear Mill
Total
1*358619
1*52477
79
=E
= $3140820
Installation cost
= 40%E
=$1256328
=13%E
=$408306
Piping cost
=10% E
=$314082
Electric cost
=10%E
=$314082
=29%E
=$910837.8
Yard improvement
=10%E
=$314082
Land cost
=6%E
=$188449
= $6846988
Indirect cost:
Engineering and Supervision Cost
=32%E
=$1005062
Construction Expenses
=30%E
=$942246
Contractor fee
=18%E
=$565347
Contingency Cost
=30%E
=$942246
= $3454902
I.C
= $10301890
Working Capital
=18%F.C.I
= $1854340
W.C
F.C.I
=$12156230
80
CHAPTER # 10
SAFETY ANALAYIS
81
82
REACTOR 1 [21]
Study Node:
Reactor-1
Material:
H2SO4
Study Parameter:
Volume of H2SO4
Source:
H2SO4 Tank
No
Guide
Word
Deviation
Possible
Causes
Consequences
-No Level
sensor.
-Tank overflow.
-Greater Conc. of
More
More
-Operators
mistake.
runaway reaction as it
volume
is an exothermic
-Malfunction
reaction.
of pump.
-Overflow valve
provided on tanks
jacket.
-Pump shutdown.
provided on the
Less
-Malfunction
volume
of pump.
pipe.
remove choking.
-Operator
Re-establish H2SO4
provided on the
-Operator
mistake.
-Malfunction
No
of pump.
reactant leads to no
Volume
-Power failure.
reaction.
jammed.
-Blow pipe to
-Level sensor
sensor.
-Inlet vale
tanks jacket.
supply in tank.
-No level
No
tanks jacket.
sensor.
-Choking of
provided on the
-Level sensor
mistake.
Less
-Level sensor
-No Level
-Operator
Action Required
tanks jacket.
-Operator reestablishes H2SO4
supply in tank.
-Backup-generator.
Alternate inlet.
83
FILTER PRESS
Study Node:
Filter Press
Study Parameter:
No
Pressure
Guide
Possible
Word
Causes
1
More
[21]
Material:
ZnSO4
Source:
Settling Tank
Consequences
Actions Required
-Pump capacity
-Increased pressure of
is greater than
on ZnSO4 inlet.
required
rupture or damage.
-Automatic ZnSO4
-Operator
injection system.
mistake
-Pump to be of exact
-No automatic
specification to provide
system.
optimum pressure.
-Pipe leakage.
2
-Remove blockage of
pipe.
Less
-Partial
blockage in
-Alternate ZnSO4
pipe.
injection.
-Pump capacity
less than
required.
84
-Pipe block.
-No filtration
-Remove blockage.
-Pump
-Re-establish supply of
malfunction
further use.
ZnSO4.
-Impurities in
No
Other
pump casing.
material source
-Filter cloth damage due
-Impurities in
to reaction with
raw material
impurities.
removal of impurities.
85
REACTOR 2 [21]
Study Node:
Reactor-2
Material:
ZnSO4
Study Parameter:
Volume of ZnSO4
Source:
H2SO4 Tank
Guide
No.
Word
Less
No
Possible Causes
Consequences
Actions Required
-Malfunction of high
-Increased
-Re-establish
service pump.
concentration of
-Leakage of pipe.
sodium stearate in
supply.
-Partial Pipe
product rather
-Remove blockage.
Blockage
-Pipe repair.
stearate.
-Alternate pipe.
-Pipe blocked.
-Product only
-Remove blockage.
-Power failure.
stearate.
supply.
-Backup pump
86
Other
-Impurities from
-ZnSO4 not
-Re-filter if required
storage vessel
suitable for
-Impurities from
reaction.
to remove
filter press.
-Low Product
impurities
-Impurities from
purity.
pump casing.
to remove
impurities
More
-Greater conc. Of
-Level sensor
-Malfunction of
provided on the
pump
reactor.
tanks jacket.
-Operator mistake
-Un-reacted zinc
-Overflow valve
sulfate in product
provided on tanks
line
jacket.
-Low product
-Pump shutdown
quality
87
TRAY DRYER
Study Node:
Study Parameter:
No Guide
Flow Rate
Possible Causes
[21]
Material:
Air
Source:
Heat Exchanger
Consequences
Actions Required
Word
1
More
-Blower capacity
-Increased rate of
of required capacity.
automatic system.
material.
-Material might be
the flow.
Less
-Pipe leakage.
-Remove blockage of
-Partial blockage in
-Product containing
pipe.
pipe.
more than
-Alternate blower or
appropriate quantity
air inlet.
than required.
of water.
-Install a blower of
the appropriate
capacity.
-Impurities in
-Blow pipe to
-Impurities in blower
remove impurities.
casing.
quality of product.
-Impurities in pipe.
blower on regular
-Impurities due to
basis.
some leakage.
dryer.
88
CHAPTER # 11
ENVIRONMENTAL
ASPECTS
89
ROUTES OF EXPOSURE
[9]
Exposure to zinc stearate can occur through inhalation, ingestion, and eye or skin
contact.
EFFECTS ON HUMANS
[10]
[10]
STORAGE:
Zinc stearate should be stored in a cool, dry, well-ventilated area in tightly sealed
containers that are labeled in accordance with OSHA's Hazard Communication
Standard [29 CFR 1910.1200]. Containers of zinc stearate should be protected from
physical damage and should be stored separately from strong oxidizers or dilute acids
may cause reactions to occur.
90
REFERENCES
[1]- Baerlocher, Additives Metallic Stearates [Online]. Available:
http://www.baerlocher.com/fileadmin/media/0.5_Service/0.5.1_brochures/0.5.1.3_pro
duct_brochures/metallic_stearates.pdf
[2]-Zinc Stearate, Properties of Zinc Stearate [Online]. Available:
http://en.wikipedia.org/wiki/Zinc_stearate
[3]- Richard H. Morris and Stephen E. ORourke, Metallic Stearates [Online]:
http://www.hallstar.com/techdocs/metallic.pdf
[4]- Mujumdar A.S, (Third Edition), Handbook of Industrial Dryers [Online] at:
http://books.google.com.pk/books?id=uKOGg1vk61MC&printsec=frontcover
[5]- Thermocouple [Online] Available at:
http://science.howstuffworks.com/thermocouple-info.htm
[6]- DP Cell [Online] Available at: http://www.sensorsone.com/dp-cell/
[7]- Flow Meters [Online] Availbe at: http://www.engineeringtoolbox.com/orificenozzle-venturi-d_590.html
[8]- Nanyang, (28-04-2012); Zinc Stearate Production Technology [Online] at:
http://www.nypengmei.com/en/news_show.php?id=293
[9]- OSHA, Guideline for Zinc Stearate [Online]. Available:
http://www.osha.gov/SLTC/healthguidelines/zincstearate/recognition.html
[10]-TOXNET, Zinc Stearate Human Health Effects [Online]. Available:
http://toxnet.nlm.nih.gov/cgi-bin/sis/search/a?dbs+hsdb:@term+@DOCNO+212
[11]-Himmelblau D.M, & Riggs J.M, (Fifth Edition), Basic Principles and
Calculations in Chemical Engineering (pp 104-148)
91
[12]-Himmelblau D.M, & Riggs J.M, (Riggs (Fifth Edition), Basic Principles and
Calculations in Chemical Engineering (pp 362-480)
[13]- Sinnott R. K., Volume 6, (Fourth edition), Coulsons and Richardsons
Chemical Engineering Design (pp 322)
[14]-UC DAVIS CHEMWIkI, Heat of reaction [Online], Available at:
http://chemwiki.ucdavis.edu/Physical_Chemistry/Thermodynamics/State_Functions/E
nthalpy/Heat_of_Reaction
[15]- Fogler H.S (Fourth Edition), Elements of Chemical Reaction Engineering
[16]- Sinnott R. K., Volume 6, (Fourth edition), Coulsons and Richardsons
Chemical Engineering Design (pp 814)
[17]- McCabe W., Smith J. & Harriott P. (Fifth Edition), Unit operations of Chemical
Engineers
[18]- Kern D.Q, (International Student Edition), Process Heat Transfer
[19]-Richardson J.F& Harker J.H, Volume 2 (Fifth Edition), Coulsons &
Richardsons Chemical Engineering pp (901-912)
[20]- Perry R.H & Green D.W, (Eighth Edition), Perrys Chemical Engineers
HandBook, (Chapter # 12)
[21]-Timmerhaus K. & Peters M. (Fourth Edition), Plant Design & Economics for
Chemical Engineers
[22]-Globe Valves [Online] Available at:
http://www.ladishvalves.com/globe-valves-corrosion-resistant/
[23]-Ball Valves [Online] Available at:
http://www.thomasnet.com/about/ball-valves-90370206.html
[24]-Relief Valve [Online] Available at:
http://www.wermac.org/valves/valves_pressure_relief.html
92
93