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Limited
VOCATIONAL TRAINING REPORT ON
SYNTESIS OF AMMONIA
May 17th 2016- June 26th 2016
(VT-247/16-17)
SUBMITTED TO-
SUBMITTED BY-
D. G. M. RAHUL
KUMAR VERMA
TRAINING DEPARTMENT
CHEMICAL ENGINEERING
IFFCO AONLA IIT
(BHU)
BAREILLY, UP
VARANASI, UP
Ammonia manufacturing plant (IIFCO)
ACKNOWLEDGEMENT
I extend my heart full gratitude to Mr. Harshil sharma for all the co-operation
rendered to me during the project.
I feel privileged to have completed my training in chemical department under the
experienced and able guidance of Mr. Rai. Sir who possess and exceptional
quality of simplifying my problem in a suitable and rational manner.
In last, I would like to thank the main person behind this training Dr. P K Mishra
(Officer Incharge, Head of department, Chemical Department, IIT BHU) who
permitted me to pursue training in winter vacations of Third Year.
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Table of content-
1. About IFFCO
2. IFFCO associates subsidiaries
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About IIFCO:
Initially IFFCO set up its plants at kalol and kandla in Gujarat which were
commissioned in 1975. Subsequently, it commissioned plants at Phulpur
and Anola in UP in the year 1981 and 1988 respectively. Capacity of all
these units have been enhanced to putting another plants in the same
complex in a phase wise manner. In order to argument its complex
fertilizers manufacturing capacity, IFFCO acquired DAP/NPK/NP plant in
Paradeep in September 2005. The Phulpur project consists mainly of
Ammonia plant, Urea plant and Offsite facilities like Water Treatment
System, Inert Gas Plant, Instrument Air Plant, Bagging Plant, Laboratory
and Storage for spares consumable and products.
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IFFCO has diversified its wings in other areas and across the globe by
putting plants in joint venture in India and abroad. The number of IFFCO's
Associates and Subsidiaries are 19. IFFCO has become a diversified entity
spreading its wings across the different continents. List of joint ventures &
subsidiaries is as below:
o) IFFCO Foundation
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Desulphurisation
The Traces of sulphur present in RLNG are removed in the
desulphurisation section before sending to the reforming section
following hydrogenation reactions are as under:
1) RSH + H2 = RH + H2S
2) COS + H2 = CO + H2S
3) C4H4S + 4H2 = C4H10 + H2S
Reforming Section
In the reforming section consisting of Pre-reformer, Primary reformer
& Secondary reformer, the sulphur free RLNG is reformed with steam
and air into raw synthesis gas (process gas) at a pressure of 30 - 37
kg / cm2. The gas contains mainly hydrogen, nitrogen, carbon
monoxide (CO) and carbon dioxide (CO2).
The steam reforming process can be described by the following
reaction:
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CO-Conversion Section
The reformed process gas enters into CO-conversion section
comprising the two CO-converters and equipment for process gas
cooling and condensate separation. The main part of the carbon
monoxide is converted into carbon dioxide by the shift reaction:
CO+H2O = CO2+H2+Heat
The heat evolved is primarily used for steam production and boiler
feed water preheating.
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Methanation Section
Following reactions take place in methanator.
The process gas from carbon dioxide removal section still contains
about 0.05 vol% CO2 and 0.30 vol % CO As the carbon dioxides are
poisonous to the ammonia synthesis catalyst, it is converted in the
methanator by use of hydrogen.
The outlet gas from Methanator contains around 73 % H2, 25 % N2,
0.7 % CH4.
Ammonia Conversion
The ammonia conversion is carried out in two converters installed in
series. One original converter and another (S-50) installed during
Energy Saving Project (ESP). Ammonia converter catalyst is promoted
Iron.
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Since the reaction is highly exothermic the waste heat is utilised for
generating steam and Boiler feed water heating. The gases are cooled
in a series of Chillers and the ammonia get condensed a series of
chillers and the ammonia get condensed and is separated. The
uncondensed gases are recycled back to Synthesis Gas Compressor.
The liquid NH3 separated out in a high pressure separator is taken to a
lower Pressure separator where the inerts are separated out. This
liquid NH3 is taken to another flash drum for removal of inerts and
liquid NH3 is sent to Urea plant or Ammonia Storage Tanks.
Fuel System:
Liquid Naphtha was used as fuel in burners of different location like
Primary Reformer Arch, Tunnel etc. Naphtha was pumped by Fuel Naphtha
Pump. Atomizing Steam at a pressure of 18 Kg/cm2g was used to atomize
naphtha in burners. For RLNG Fuel Conversion, total fuel Naphtha plus
atomizing steam facilities were dismantled and new RLNG fuel system
has been installed. RLNG Fuel system includes pressure let-down station,
flow control system for each furnace, their double block & bleed systems
to isolate the burners for any process requirement and necessary
modification in the Emergency Shut down System.
LNG specification at B/L:
Instrumentation:
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AMMONIA PLANT-I
The Plant is designed to produce 1215 tons per day liquid ammonia based
on Pullman Kellogg process with Natural Gas (RLNG) as raw material.
RLNG undergoes steam reforming in the catalyst tubes of the Primary
Reformer. Endothermic heat for reforming reaction is provided by firing
RLNG in Gas Burners. Further reforming takes place in the Secondary
Reformer where air is added to supply the nitrogen required for ammonia
synthesis. Hot reformed gases from Secondary reformer are cooled by
heat recovery in the waste heat boilers. Gases are then introduced in the
Shift Converters where most of the carbon monoxide gets converted to
carbon dioxide which is removed by the GV process.
In the GV Absorber, CO2 is absorbed in promoted Potassium Carbonate
solution (GV Solution). Solution is regenerated in the strippers and
recycled back to the Absorber. CO2 from the stripper is sent to the urea
plant. Residual oxides of carbon in the synthesis gas leaving the Absorber
are converted to methane in the Methanator. Pure synthesis gas from
methanator is compressed to about 150 Kg/Cm2 by Turbine driven
Synthesis Gas Compressor. Syn Gas is partially converted to Ammonia in
Syn Gas Converter. Recycled gas (containing H2 and N2) leaving the
synthesis converter re-joins the last stage of compressor. Product
ammonia is recovered by cooling the compressor discharge stream in the
series of Refrigeration Chillers where ammonia condenses. Liquid
ammonia is purified by flashing at lower pressures and then sent to the
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urea plant or storage tanks. All major pumps and compressors are steam
driven. Most of the high pressure steam is being generated in the waste
heat boilers by heat recovery from hot gases.
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OFFSITES FACILITIES:
Raw Water And Water Treatment Plant:
Entire Water requirement of our plant is being fulfilled by underground
water. IFFCO Phulpur Unit utilizes deep sub-soil water .Raw water is
collected in storage tank of 16000 M 3 capacity. This water under goes
extensive treatment to make it suitable for use as cooling tower make-up
and boiler feed. The temporary hardness of raw water is brought down in
line softener and softened water is used as cooling tower make-up. Water
for steam generation is treated in demineralization plant having
conventional ion exchange process. It consists of four stream of pressure
sand filter, primary and secondary cations, degasser, primary and
secondary anions and mixed bed units, each having a capacity of 70 M 3
/hr.
Cooling Towers:
Cooling water required to remove excessive process heat of ammonia,
urea and power plant is provided by three induced draft type cooling
towers .Hot water from various heat exchangers flow down the air in
circulation type cooling water system. An exhaustive cooling water
treatment system is followed to keep the circulating cooling water free of
scales, corrosion and natural growth. Blow down water from all cooling
towers is recycled back in lime softener. This reduces makeup water and
also results in considerable saving of chemicals required for treatment.
Ammonia Storage:
Product Ammonia is stored at-33C and at atmospheric pressure in
10,000 MT double walled insulated storage tank and a 5000 MT capacity
double integrity tank. Ammonia transfer pumps for transfer of liquid
ammonia to the urea plant, refrigeration package unit for maintaining
tank pressure, flare stack and loading/unloading facilities are provided to
meet the plant requirements safely.
Effluent Treatment:
All the liquid effluents generated from the various plants are subjected to
extensive treatment to ensure that the treated water quality conforms to
the specification laid down by the UPPCB and MINAS. For liquid effluent
control, deep hydrolyser, distillation column, stripper and ETP based on
steam stripping, disc. Oil separator, treatment cum recycle plant on
Reverse Osmosis technology. The treated water is completely recycled
and reused in plant itself and there is no liquid effluent discharge from
plant.
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AMMONIA PLANT-II:
Ammonia is produced using the Haldor Topsoe process with RLNG as raw
material. In the reforming section the RLNG is reformed with steam and
air into process gas. The gas contains mainly of hydrogen, nitrogen,
carbon monoxide (CO) and carbon dioxide (CO2).
In the shift section, CO2 is first converted into CO2 and H2 with steam
(shift reaction), in order to facilities removal of the carbon oxides and to
increase the H2 yield. Then CO2 is removed in the CO2 removal unit. The
residual CO and CO2 is converted into CH4 using H2, before the gas is
sent to the ammonia synthesis loop.
Pure synthesis gas from methanator is compressed to about 190 Kg/Cm2
by Turbine driven Synthesis Gas Compressor. Syn Gas is partially
converted to Ammonia in Syn Gas Converter. Recycled gas (containing H2
and N2) leaving the synthesis converter re-joins the last stage of
compressor. Product ammonia is recovered by cooling the compressor
discharge stream in the series of Refrigeration Chillers where ammonia
condenses. Liquid ammonia is purified by flashing at lower pressures and
then sent to the urea plant or storage tanks. All major pumps and
compressors are steam driven. Most of the high pressure steam is being
generated in the waste heat boilers by heat recovery from hot gases.
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Operating Conditions
Inlet Outlet
H2 36.59 24.45
N2 12.20 3.02
Ar 0.15 0.04
CO - 0.54
C3 + 50.25 -
Catalyst
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Operating Conditions
Pressure kg/cm2 34 46 39
Reactor Data
Ni 25%
Al2O3 11%
MgO Balanced
Ni 25 15-20
Al2O3 11 55-60
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S - <2000 ppm
Ni 8-10%
Al2O3 87-90%
SiO2 <0.05 %
S < 0.05%
Type C-14-02-RR
Volume 39 m3
Secondary Reforming:
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Mixing and combustion of reformed process gas with process air. Mixing
of N2 utilization of O2 by combustion temperature raised to 1200 oC.
Amount of air (nitrogen) addition depend on desired N 2 to H2 ratio. Normal
skin temperature 160 o C (designed 300o C).
Operating conditions
Inlet Outlet
CH4 13 0.45
H2 67.64 55.92
N2 0.55 23.29
Ar 0.01 0.28
CO 8.29 12.41
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Catalyst
Ni 8-10%
Al2O3 87-90%
SiO2 <0.05 %
S < 0.05%
Type C-14-02-RR
Volume 39 m3
Ammonia converter:
The main inlet low to the convertor R3501, introduce trough two nozzles
at the bottom. Higher Pressure and low temperature are favorable
conditions for reaction. From the annular space the non-converted gas
enters the tube side of interbed heat exchanger, where it is heated up to
the inlet temperature of the first catalyst bed. Temperature is adjusted by
the cold shot flow.
Operating Conditions:
Make-up Gas
Flow Rate: 199505
Temperature: 6 oC
Pressure: 25.9 kg/cm2g
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After Compression:
Temperature: 22.6 oC
Pressure: 181 kg/cm2g
R3502
Pressure
Catalyst
KM1 KM1
R
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R 3501
N2 20.76 16.79
H2 62.27 50.36
R 3502
N2 16.79 15.84
H2 50.36 47.51
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Refrigeration Circuit:
The purpose of the refrigeration circuit to carry out the various cooling
tasks in the ammonia synthesis loop. The primary task is to condense the
ammonia, which is produced in the convertor. Other cooling tasks are
cooling of make-up gas, purge gas, let down gas, and inert gas. The
chillers operated at different chillers temperature and pressure level
corresponding to the interstate pressure of the refrigeration compressor.
The letdown chiller E 3508, inert gas chiller E3509, and the purge gas
chiller E3511 operate at about 0.19 kg/cm2g and -30 oC. Evaporated
ammonia from these chillers combined with vapor from flash vessel
B3505, and enter the first stage of K3451. E 3507 operates at 4.6 kg/cm 2g
& 6.9 oC and the vapor enters at third stage of Compressor K3451. E 3506
and E 3514 operates at about 7.1 kg/cm2g & 17.8 oC and the vapor send
to the suction of 4th stage suction compressor K3451. The dissolved inert
gases released in B 3510 are sent through E 3509 and then to K.O. Drum
B3509. Inert gas from B3509 is mixed with let-down gas from KO drum, B
3508 and heated to approx. 25 oC in the inert gas heater, E 3513 which is
a coil integrated in B 3510. Letdown gas and inert gas send to off gas
absorber.
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M
ethanation:
To convert CO and CO2 in methane. Temperature increase across the
methanator shows conversion of CO and CO2 in CH4
Temperature: Inlet: 280
Outlet: 289
Catalyst
Volume 30.05%
Ni 20+1%
CaO 4.5-5.5%
Al2O3 69-72%
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Catalyst loading
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To fulfill the shortfall of Carbon dioxide after feed stock conversion, a 450
MTPD CO2 Recovery (CDR) Plant has been installed in Ammonia-II plant.
The CDR plant recovers CO2 from flue gases of Primary Reformer stack
which contain about 9 to 10% CO2 on dry basis.
The technology of CO2 Recover Plant is developed and supported by M/s
Mitsubishi Heavy Industries Ltd. Japan. The project was success fully
commissioned with an investment of Rs. 59.13 Crores
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STEAM GENERATION:
A Gas based boiler of capacity 200 MT/Hr. is installed. It has been
supplied by BHEL. And designed at 115 kg/cm2 at 510 C. This boiler is
equipped with force draft fans, feed water pumps, makeup water pump,
economizer, super heater, chimney (120 m high) to achieve maximum
efficiency in steam generation. This boiler is operated from a D.C.S.
control room.
POWER PLANT:
The power plant is designed to produce 18 MW of power at 11 KV, 50 HZ.
The power is produced by a turbo generator, driven by steam turbine. The
whole package has been supplied by BHEL, Hyderabad. The steam
turbine uses steam at 115 kg/cm2 and 515 deg. C as the motive fluid and
is an extraction cum condensating turbine. The TG set is DCS controlled.
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OFFSITES FACILITIES:
DM water plant:
Raw water from deep bore wells is collected into a raw water storage tank
of 16000 M3 capacity. Water for steam generation is treated in D.M. plant.
The plant has two streams each having a capacity of 140 M3/hr. The plant
has been designed and supplied by Indocan Engg. Systems Ltd., Pune.
This plant consists of sand filters, cation exchangers, anion exchangers,
mixed bed which are used to remove turbidity, cations and anions present
in water. This treated water is sent to power plant and other locations of
the plant for steam production.
Softening Plant:
This plant is designed to produce 800 M3/hr. of soft water for make up in
cooling Tower. The raw water is treated in a reactor clarifier to remove
hardness by using lime and alum.
Inert Gas:
To meet out the nitrogen requirement for ammonia plant, a nitrogen plant
producing 600 NM3/hr. of nitrogen at 7.5 kg/cm2 pressure, is installed.
The feed stock for generation of nitrogen is atmospheric air. Nitrogen
production is based on Pressure Swing Adsorption (PSA) system using
carbon molecular sieves. This unique adsorbent separates nitrogen from
compressed air and gets regenerated by depressurization to atmosphere.
This plant is designed and supplied by M/s Kinetic Technologies India Ltd.,
New Delhi.
Cooling Towers:
Cooling towers are of induced draft cross flow type and supplied by M/s
Paharpur Cooling Towers Ltd. Calcutta. These towers are designed to
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handle 24,500 M3/hr. C.W. flow to Ammonia plant, 18,400 M3/hr.C.W. Flow
to Urea plant and 5200 M3/hr. C.W. flow to Power Plant.
Air Compressor:
Tow nos of three stage centrifugal compressors supplied by M/s ELLIOT
Turbo machinery Ltd. USA have been installed to cater to the need of air
requirement of plant instruments and nitrogen generation. One
compressor is in running mode, while second one is standby. The capacity
of plant is 5000 NM3/hr. at 8.7 Kg/Cm2 out of which instrument air 3000
NM3/hr. is passed through air drying unit before use in plants. The speed
of the final stage impeller is increased up to 42642 R.P.M. in order to get
optimum efficiency.
AMF Set:
The set is designed to supply electricity during failure of main power and
its capacity I s 2.2 MW. It takes auto start in case of power failure and
keeps critical equipment/motors alive. DG set has been supplied by M/s
BHEL, Bhopal.
Product Handling:
Product handling plant of a capacity of 9600 bags/hr. has been installed
by TICB Bombay. Urea received from urea plant through conveyer belt is
either fed to bunker for direct bagging or into silo (Capacity 30,000 MT)
for storage. Stored urea from silo is sent to bagging through scrapper
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The design pressure drop across the primary reformer at 100% plant load
was 4.7 kg/cm2 but in actual practice this used to rise up to 4.5-8.0
kg/cm2 depending on the age of catalyst & load of plant. In the 4 to 6
months of a fresh catalyst charge, there used to be a gradual increase in
pressure drop, even at 90% load. After 5 to 6 months of operation 90%
load, the pressure drop used to reach to7.5 to 8.0 kg/cm2 and the plant
had to be shut down for steaming of catalyst. Steaming of catalyst had to
be repeated after every 6 weeks and a maximum of 4 to 5 steaming
operations had to be carried out before catalyst itself was replaced. The
aromatic slip from the reformer also exhibited the same characteristics of
gradual increase during the initial 4-6 months and accelerated in the
latter half of the year. Also the tube skin temperatures exhibited a general
upward trend after a few months of operation between 920-950 deg C
against the design metal temperature of 916 deg. C.
Primary Reformer was a bottleneck in achieving its rated capacity and
catalyst change was required after every 12 months. In April, 1984, a
ruptured tube was found. Reformer tubes at that point of time had been
operated for hardly for 30000 hours against a design life of 100000 hours.
After a survey of all naphtha based Indian Plants, a fact clearly emerged
that the catalyst loading, i.e., the amount of naphtha to be reformed per
hour per unit of volume of catalyst was the highest for Phulpur ammonia
plant.
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Thereafter the revamp task for primary tubes was undertaken with view
to provide more catalyst volume, improved metallurgy, improving feed
distribution by resizing pigtails, etc.
Revamping
Total catalyst volume was increased by about 35% (26 m3 from 20 m3) by
increasing I.D. of reformer tubes (95.2 mm from 81.3 mm) keeping same
O.D. by providing superior metallurgy Manurite 36X catalyst tubes in
place of original HK-40 tubes. As a result naphtha loading on catalyst
decreased from 1.04 to 0.76 kg / litre. The ratio of ICI catalyst 46-1S and
46-4S was changed to 65:35 from 75:25. The size of the inlet pigtails was
reduced to ensure uniform feed naphtha distribution in the catalyst. Also
material of inlet pigtail was changed to A 213 T11 from A 335 P11.
After revamping Pressure drop & Tube skin temperature got reduced and
the Plant could be operated in a consistent manner even at higher plant
load with reduced energy consumption.
1st Reformer revamping had been highly successful and the Primary
Reformer tubes could last more than their design life of 100000 hours.
Second reformer revamping was carried out in March 2000. This time
Catalyst volume was increased to 30 m 3 & naphtha loading on catalyst is
now 0.68 kg/litre which was quite comparable with other naphtha based
ammonia plants. The following modifications were carried out during
second reformer revamping:
I.D. of reformer tubes was increased to 100.2 mm from 95.2 mm. Material
of tubes and riser was changed to G 4852 Micro alloy. In place of
Manaurite 36X. Catalyst volume increase to 30 m3 from 26.3 m3.
Converter Catalyst:
High Temperature Shift Converter converts carbon monoxide to carbon
dioxide thereby generating the hydrogen in the process. Originally, there
was 64.28 M3 of conventional Iron Chromium catalyst. From the very
inception, it was experienced that the pressure drop in the reactor rose to
2.0 -2.5 kg /cm2 after six months of operation, though the initial pressure
drop used to be 0.5 2.5 kg / cm2. The design pressure drop of the
reactor is 0.5 kg /cm2 only. However the activity of the catalyst remains
normal and CO slip remains less than the design figure of 3.34 % High
pressure drop across the reactor results in to more power requirement in
the synthesis compressor.
To overcome the problem, the top grating and screen were removed from
the reactor in 1985 in consultation with the plant designer, MW Kellogg.
Analysis of the dust collected from the top of the reactor showed nearly
55% Fe3O4 and 10% Potash as K2O. The initial two catalyst charges were
conventional Iron Chromium catalyst supplied by M/s UCIL. In 1991,
copper promoted catalyst of M/s UCIL was charged but the problem of
high pressure drop still persisted. In year 1995, the copper promoted
catalyst of Topose make was loaded however the problem still remained
and after 2 years of operation, again UCIL catalyst was charged. The
same charge is in operation and at present the pressure drop is 2.5
kg/cm2.
In almost every annual shutdown, the dust from the top of catalyst was
removed in inert atmosphere which provided some temporary relief but
subsequently it regained the higher pressure drop value.
The unit was commissioned in July, 1985. With the addition of this unit,
the average increase in Ammonia production is 35 MTPD for the same
input of feed Naphtha and the energy saving is 0.11 GCal/MT of Ammonia.
Salient Features of PGR unit are given below:
Capacity
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a) Top Arch Burners (162 Nos.) of Primary Reformer having heat release
capacity of 578,900 kcal/h per burner.
b) Tunnel Burners (9 Nos.) of Primary Reformer having heat release
capacity of 922,600 kcal/hr. per burner.
c) Auxiliary Boiler Burner (5 Nos.) of Primary Reformer having heat
release capacity of 15,120,100 kcal/hr. per burner.
d) Hydrocarbon Feed Preheater (4 Nos.) having heat release capacity of
741,100 kcal/hr. per burner.
e) Start-up Heater Burner (4 Nos.) having heat release capacity of
741,100 kcal/hr. per burner.
All these burners were, earlier, steam atomized liquid naphtha burners.
New RLNG burners supplied by M/s John Zink were installed after
dismantling of earlier burners along with atomizing facilities.
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RLNG Preheater Coil to heat half of total RLNG Feed was installed in the
space available between LT Steam Super heater & Combustion Air
Preheater. Remaining RLNG is being heated through the existing
desulphurisers Feed Preheater. The total pressure drop in the preheating
section has reduced by 2.5 Kg/cm2g after this new arrangement .
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