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Industrial Training Project

Report
‘Understanding the
complete production
process of Urea prills’

In Production Department
An ISO 9001-14001-18001 Unit

Name of student- Gaurav Vinayak


Roll no. – 16112020
Discipline- B.Tech/Chemical Engineering
Name of the Organization- National Fertilizers Limited, Nangal Unit
Name of the Institute- Dr. B.R Ambedkar National Institute of
Technology, Jalandhar
National Fertilizers Limited,Nangal Unit
About NFL Plant:
Consequent upon the reorganization of FCI group of plants, Nangal
Plant was transferred to NFL & subsequently expansion plant of
Nangal Unit was commissioned with an installed capacity of 3.30
LMT. Further in order to sustain and enhance the company’s growth,
NFL successfully revamped Urea Plant of the Nangal Unit &
Commercial Production was commissioned after revamp w.e.f. 1st
Feb 2001 thus enhances the Annual installed Capacity from 3.30 LMT
to 4.785 LMT . As per guidelines of GOI, in order to reduce subsidy
burden & Carbon footprint, NFL revamped the Nangal Unit on LSTK
basis for changeover of Feedstock from LSHS/FO to Natural Gas and
commercial production on Gas was commenced during April 2013.

SALIENT FEATURES OF NANGAL UNIT:

 Installed capacity- 478500 MTPA


 Capital investment- 229.19 Crores
 Commencement of production- November 1,1978

Process Technology:

 Ammonia- KBR SMR (steam methane reforming) with purifier


technology.
 Urea- Technimont Total Recycle Process.
 Raw material- Coal, LNG/RLNG, Power, Water.

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Certificate of completing the Industrial training:

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Acknowledgement:
I’m very grateful to Dr. Rajeev Trehan (Head, Centre of Training and
Placement of NIT Jalandhar) and all the other staff at TPO who
helped me in preparing all the necessary documents for the training
at NFL, Nangal.

Further, I thank Dr. Sangeeta Garg (Associate Professor & Head) of


Chemical Engineering department of NIT Jalandhar, who always
motivated us in understanding the importance of an industrial
training. And Dr. Raj Kumar Arya (Associate Professor) the faculty
coordinator incharge of industrial training of Chemical Engineering
Department, who helped me in getting this, Training.

During this training I’ve learned alot, for which I pay my heaviest
gratitude to the HRD Assistant Manager Mr. Shubhankar Mitra and
other staff members of National Fertilizers Limited,Nangal, who
helped me in all aspects in fulfilling my cherished desire of getting a
successful industrial training.

I’m very thankful to all the supervisors and other officials for letting
me visit various plants of NFL and providing me complete process
details of their respective plants.

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Table of Contents
About NFL Plant: ..................................................................................................................................... 2
SALIENT FEATURES OF NANGAL UNIT: ................................................................................................... 2
Process Technology:................................................................................................................................ 2
Acknowledgement: ................................................................................................................................. 4
Benefits of NEEM COATED urea prills: .................................................................................................... 6
Elements/compounds needed: (Urea Production) ................................................................................. 7
Process description: ................................................................................................................................ 8
Urea synthesis section: ........................................................................................................................... 9
Urea vacuum concentration ................................................................................................................. 11
Ammonia recovery section: .................................................................................................................. 13
Prilling Tower: ....................................................................................................................................... 14
Complete process flow sheet of Urea synthesis plant:......................................................................... 17
Ammonia Synthesis Plant: .................................................................................................................... 18
PROCESS DESCRIPTION: ........................................................................................................................ 19
Feed Gas Compression, Preheating and Desulfurization:..................................................................... 20
PRIMARY REFORMER: ........................................................................................................................... 21
PROCESS AIR COMPRESSION: ............................................................................................................... 22
SECONDARY REFORMER: ...................................................................................................................... 22
SHIFT CONVERSION:.............................................................................................................................. 22
CARBON DIOXIDE REMOVAL:................................................................................................................ 23
METHANTION:....................................................................................................................................... 24
DRYING: ................................................................................................................................................. 25
CRYOGENIC PURIFICATION: .................................................................................................................. 25
SYNGAS COMPRESSION: ....................................................................................................................... 26
AMMONIA SYNTHESIS: ......................................................................................................................... 26
PURGE GAS AMMONIA RECOVERY: ...................................................................................................... 27
AMMONIA REFRIGERATION: ................................................................................................................. 27
PROCESS CONDENSATE STRIPPING: ..................................................................................................... 28
STEAM SYSTEM: .................................................................................................................................... 28
COOLING WATER: ................................................................................................................................. 28
Conclusion: ............................................................................................................................................ 29
Major engineering problems: ............................................................................................................... 29
References: ........................................................................................................................................... 31

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Benefits of NEEM COATED urea prills:

 Neem serves as a natural insecticide.

 The release of Urea is slow. (Slow nitrification of urea) which


ensures the use nutrients and plant’s yield increases.

 Earlier some industries like milk industry was mixing urea with
milk to gain profits but now, with the need coated urea it’s not
possible. (adulterated milk)

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UREA PRILLS MANUFACTURING
Elements/compounds needed: (basic)*

HYDROGEN

NITROGEN

CARNON DIOXIDE

PLANTS in service parallel to UREA production:

STEAM
generation
plant
AMMONIA CO2
production production
plant plant

UREA
production
plant

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UREA manufacturing plant
Process description:
This plant is divided into three main sections,

Urea synthesis section

Vacuum concentration section

Ammonia recovery section

Ammonium Carbamate

Urea

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Urea synthesis section:

 This section comprises synthesis loop and three decomposition


and recovery stages working at 70, 12 & 3 atm pressures
respectively.
 The CO2 coming from Rectisol unit of ammonia plant is fed to
urea plant by means of two separate headers at two different
pressures i.e. 11 & 1.2 atm .
 Then the CO2 is compressed at synthesis pressure of 220 atm by
two compressors.

Fig: stage 1 Fig: Stage 2

 The liquid ammonia coming from ammonia plant at pressure of


20-30 atm is compressed at synthesis operating pressure by
means of ammonia pumps.
 The ammonia is heated from about 20 °C to 70 °C in heat
exchanger by steam condensates.

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 All carbamate solution coming from 70 atm decomposition
stage is fed to the reactor by means of three of four carbamate
pumps operating in parallel.
 The fresh CO2 and NH3 and, the previous mixture are fed to
carbamate condenser where part of the ammonium carbamate
is formed and part of reaction heat is taken out generating
steam of about 7.5 atm.
 The hot carbamate from carbamate condenser flows to new
reactor where residence time is enough to convert 72% of
carbamate to urea.
 The urea solution produced in new reactor joins the one coming
from existing reactor.
 The resulting urea solution containing about 36% of urea,
unconverted carbamate, excess NH3 and water is depressurized
to about 70 atm and heated to 190 °C by means of saturated
HP steam.
 The vapours released by heating are separated from urea
solution concentrated up to 55% in existing first stage separator
and absorbed in first partial condenser.
 The resulting carbamate solution is recycled to existing reactor
by means of carbamate pumps.

 The urea carbamate solution from first stage separator


containing about 55% urea is heated to 155 °C in second stage
distiller.

 The 2nd carbamate solution from 2nd stage condenser is recycled


to 1st stage partial condenser & to the 1st stage washing
column.

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 The 66% urea solution from 2nd separator is heated in 3rd stage
distiller to 130 °C by saturated steam.

 The 3rd stage recycle carbamate is taken from discharge and


pumped to 2nd stage washing column.

 The unabsorbed NH3 with some inerts carried along in


outgoing gases from condenser top are absorbed in
washing column with the recycle solution.

 The inerts are vented to atmosphere through pressure


control valve.

Urea vacuum concentration:

 The urea solution at about 73% urea is pimped to first vacuum


stage distiller.

 In 1st vacuum stage distiller (divided in two parts) , the urea


solution is heated to 130 °C by 3.5 & 7.5 atm steam
respectively.

 Gases obtained are separated from urea solution at about 92%


in 1st vacuum separator.

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Fig: Vacuum section

 Vapours containing mainly steam with little NH3 and CO2 are
fed to 1st vacuum condenser where they’re condensed and
incondensable gases are sucked by ejector.

 The then concentration of urea solution at 1st vacuum stage


separator is about 92%.

 Urea solution is then pumped to 2nd vacuum stage distiller &


heated to 140 °C by 7.5 atm steam.

 Released steam with little NH3 & CO2 is separated from


melt urea in 2nd vacuum stage separator.

 The 99.7% melt urea from bottom of 2nd vacuum stage


separator is fed to top of prilling tower.
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Ammonia recovery section:
nd
 The process condensates obtained from 2 vacuum stage

condensers are collected into tank are pumped to:


 A small quantity to vent gas washing column C-7.

 Another small portion to PA-2 pumps flushing liquor

system as makeup.
 Another small part to vacuum system flushing.

 The greater part to inerts washing column C-6.

Fig: Part shown for Ammonia Recovery/Recycle section

 Condensates from 1st vacuum condenser HE-8 together with


the condensate coming from column C-7 are collected in 1st
vacuum stage condensate tank SR-6.
 The ammonia enriched condensate is fed to rectification column
C-4/N, the NH3 is stripped off from process condensate.
 The off gases containing mainly NH3 with some CO2 are fed to
partial condenser E-3/N.

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 The mixture of liquid carbamate solution and uncondensed
gases at 55 °C from condenser E-3/N flows into the recovered
vapour condensation column C-5 where vapours are absorbed
with weak carbamate solution under recirculation through
pump PC-10.
 The bottom of column C-4 containing small quantities of NH3,
CO2 and urea is sent to hydrolysis section where they’re
recovered under form of carbamate solution.
rd
 This carbamate solution is recycled to urea plant to 3

stage washing column C-3.

Prilling Tower:

Fig: Prilling Bucket

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 The 99.7% melt urea from bottom of SD-5 is fed to top of
prilling tower.
 It is a circular, natural draft and conical bottom type tower.
 Having two tuttle rotating prilling buckets at the top. One is
kept in operation & other one spare.

Fig: Louvers

 Speed of prilling buckets is varied to control prills size, having an


inverse relation.
 Melt urea comes out of holes of rotating bucket in form of fine
droplets.
 These droplets are distributed uniformly throughout the cross-
section of tower by centrifugal force imparted by rotation of
prilling bucket.

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 Ambient air enters the bottom of prilling tower through louvers
and rises upwards and cools the urea melt droplets to about 60
°C.

Fig: Belt conveyer

 Solidified prills fall on floor at bottom of tower which is


scrapped by double arm rotary scrapper to the belt conveyors
for packaging.

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Complete process flow sheet of Urea synthesis plant:

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Ammonia Synthesis Plant:

Fig: Block diagram of Ammonia Plant

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PROCESS DESCRIPTION:
The Ammonia production process takes place through following main
steps:

Feed Gas compression, Preheating and Desulfurization

Primary Reforming

Process Air Compression

Secondary Reforming

Shift Conversion

Carbon dioxide Removal

Methanation

Drying

Cryogenic Purification

Syngas Compression

Ammonia Synthesis

Purge Gas Ammonia Recovery

Ammonia Refrigeration

Process condensate Stripping

Steam system

Cooling Water System

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Feed Gas Compression, Preheating and Desulfurization:
 Natural gas is initially directed to Feed Gas Knockout drum
where any entrained liquids (or solids) are removed. Part of the
natural gas from the outlet of knockout drum is sent to primary
reformer furnace as fuel.
 The remaining natural gas is compressed to 57.32 kg/cm2 in
the feed gas compressor. After compression NG feed is mixed
with a small amount of syngas recycled from the synthesis loop
which provides the required hydrogen for the downstream
hydrotreater.
 The mixture of NG and hydrogen is heated to 371℃, first using
feed gas preheater, then in the fed gas coil located in the
convection section of the primary reformer.
 The hot gas then enters a two-step desulfurization system. In
the first step, the hot gas passes through a hydrotreater which
contains cobalt/molybdenum catalyst.
 The catalyst ensures hydrogenation of organic sulphur
compounds.

 In the second step, hydrogen sulphide in the feed gas is


removed in two Desulfurizer.
 Hydrogen sulphide reacts with the bed of zinc oxide contained
in each desulfurizer and is retained as zinc sulphide, thereby
producing an effluent stream containing less than 0.1 ppm of
sulphur.

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Fig- Horton sphere

PRIMARY REFORMER:
 Desulfurized feed gas is mixed with process steam from the
overhead of the process condensate stripper to give a steam to
organic carbon molar ratio 2.7:1.
 The mixture is preheated to about 495℃ in the convection
section of primary reformer.
 The preheated mixed feed is distributed over tubes packed with
reforming catalyst nickel and suspended in the radiant section
of reformer.
 Steam reforming reactions take place to form carbon monoxide,
carbon dioxide and hydrogen.

 The effluent gas from reformer at 48.0 kg/cm2 and 721℃


contains about 29.9 mol% of unreacted methane.
 This effluent is sent to secondary reformer.
 Heat for the above reaction is supplied by the combustion of
fuel gas in burners located at the top of the furnace.

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PROCESS AIR COMPRESSION:

 Process air is drawn through air filter and removes any dust
particles.
 It is then compressed in a process air compressor to a pressure
of 50.8kg/cm2.
 Compressed process air is then preheated to 510℃ in the air
preheated coil located in convection section of primary reformer
and sent to the secondary reformer.
 Steam is continuously added to the inlet of the coil.

SECONDARY REFORMER:
 Hot compressed process air and primary reformer effluent are
sent to the top section of secondary reformer where
spontaneous combustion occurs.
 The resulting hot gas mixture then flows down through a bed of
nickel based reforming catalyst in the lower section of
secondary reformer thus converting methane to more carbon
oxides and hydrogen.
 The unreacted methane content leaving secondary reformer is
about 1.8 mol%.

SHIFT CONVERSION:

 The secondary reformer effluent is sent to the High


Temperature Shift (HTS) Converter reactor.
 Here the gas flows over a bed of HTS catalyst and carbon
monoxide reacts with steam to form carbon dioxide and
hydrogen via the water gas shift reactions.

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 About 72% of the carbon monoxide is shifted to carbon dioxide
in the HTS converter.
 Carbon monoxide content in the HTS effluent is 2.9 mol%. The
gas leaving the HTS converter is cooled by generating HP steam
in the HTS effluent and by heating HP boiler feed water in the
HTS effluent /BFW preheater.
 The gas then passes through an LTS guard bed which is packed
with LTS catalyst.
 The LTS effluent is cooled and is then sent to the low
temperature shift converter at about 208℃.
 Most of the remaining carbon monoxide is shifted to carbon
dioxide in the LTS, leaving a residual carbon monoxide of about
0.25mol% in the LTS effluent.
 The gas is then sent to CO2 stripper reboiler and further cooled
in the LTS effluent/DMW Exchanger to about 70℃.
 The process condensate is separated out in the raw gas
separator and pumped to the process condensate stripper.
 The overhead of raw gas separator is sent to the carbon dioxide
removal unit.

CARBON DIOXIDE REMOVAL:

 The process condensate enters the bottom of CO2 absorber at


about 70℃.
 It is contacted counter current with semi-lean aMDEA solution.
 The gas then flows upwards into the top section of CO2
absorber where it is contacted with lean aMDEA solution.

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 The gas then passes through a water wash section, a demister
pad, and is sent to the CO2 Absorber Overhead Knockout Drum
to remove any traces of entrained aMDEA solution.
 The treated gas leaving the top of the absorber contains less
than 500 PPMV of carbon dioxide and is sent to the
Methanation section.
 Rich aMDEA solution is sent to HP flash where most of the
dissolved inlets are removed from the rich solution.
 The CO2 recovered from the above process is used in making of
urea.

METHANTION:

 The vapour from the CO2 absorber overhead Knockout Drum is


preheated to the Methanation reaction temperature, using
methanator effluent in the methanator feed/effluent
exchanger.
 And using condensing HP steam in the methanator start up
heater.
 The preheated gas then flows through the methanator where
carbon oxides in the gas are converted to methane over a nickel
catalyst.
 Residual carbon oxides leaving the methanator are less than 5
PPMV.

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DRYING:
 In preparation for drying, the methanator effluent is cooled by
heat exchange with methanator feed in methanator
feed/effluent exchanger to 79℃ and against cooling water in
the methanator effluent cooler to 38℃.
 This effluent then combines with recycle synthesis loop purge
gas from HP Ammonia scrubber and the mixture is chilled using
ammonia refrigerant in the methanator effluent chiller.
 And after this it is sent to methanator effluent separator where
process condensate is separated out.
 After this it is sent to molecular sieve dryer packed with zeolite
based desiccant and operates cyclically.
 These dryer remove traces of ammonia, residual carbon dioxide,
and water.

CRYOGENIC PURIFICATION:
 Dried raw synthesis gas is then sent to the cryogenic
purification section.
 The gas is cooled with make-up synthesis gas and with purifier
waste gas in the top section of the purifier feed/effluent
exchanger.
 The gas then flows through the purifier expander. The expander
effluent is further cooled and partially condensate in the bottom
of purifier exchanger and enters the rectifier at -171℃.
 Liquid from the bottom of the rectifier is partially evaporated
at reduced pressure in the shell side of the purifier rectifier
condenser and provides cooling for the condenser and reflux of
the column.
 The rectifier bottom contains the excess nitrogen, most of the
methane, and some of the inlet argon.

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 The partially evaporated liquid leaving the shell side of purifier
rectifier condenser is reheated and vaporized in purifier
feed/effluent exchanger and leaves as waste gas.
 The make-up Syngas from the top of purifier rectifier condenser
is reheated in purifier feed/effluent exchanger and sent to the
existing Syngas compressor at 1.8℃.

SYNGAS COMPRESSION:

 The purified Syngas is compressed in a four stage, steam


turbine driven synthesis gas compressor.
 Recycle gas is added to the synthesis gas before the fourth
stage suction, and the combined flow leaves the compressor at
about 197.2 kg/cm2.

AMMONIA SYNTHESIS:
 Ammonia is produced in a fixed bed, vertical converter.
 Make-up and recycle gas mixture from the synthesis gas
compressor is preheated by heat exchanger with converter
effluent in the Hot Exchanger.
 It then flows to the ammonia converter. Ammonia is
synthesised in two adiabatic beds provided with an inter cooler
and an after cooler.
 The converter effluent containing about 17.7 mol% ammonia is
at about 453℃.
 The converter effluent is cooled to 59℃. The converter effluent
is further cooled to 38℃ by cooling water in the converter
effluent cooler.
 It is then sent to the cold exchanger where it is chilled by heat
exchange with recycle gas.

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 The gas is finally chilled to about -4℃ against ammonia
refrigerant in the Ammonia Chiller.
 Liquid ammonia is separated out from the converter effluent in
the separator a small fraction of the vapour stream from the
separator.
 It is purged from the synthesis loop to control the inert
(methane plus argon) concentration inlet to the ammonia
converter at about 3.20 mol%.
 The high-pressure purge stream is sent to the purge gas
ammonia recovery section.
 Liquid ammonia is depressurized to about 37.0 kg /cm2 in the
flash drum to release dissolved gases in ammonia.
 Liquid ammonia from the above is mixed with recovered
ammonia is sent to the existing Horton sphere.

PURGE GAS AMMONIA RECOVERY:

 The high-pressure purge gas from the synthesis loop is sent to


the HP Ammonia scrubber in the ammonia recovery section.
 The gas is scrubbed with water to recover the ammonia.
 Flash vapour from flash drum is sent to the LP Ammonia
scrubber where it is scrubbed with water to recover most of the
ammonia.
 The bottom streams of both the scrubber contain water with
dissolved ammonia.
 These ammonia solutions are combined and sent to the
Ammonia Distillation Column.

AMMONIA REFRIGERATION:
 The ammonia refrigeration section supplies ammonia
refrigerant to two chillers:
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 The methanator effluent chiller
 The ammonia chiller.
 Ammonia refrigerant is stored in the Ammonia Refrigerant
Receiver. From here it is sub cooled.

PROCESS CONDENSATE STRIPPING:


 Process condensate from the Raw Gas Separator is sent to the
process condensate stripping section.
 Here the condensate is first preheated in the condensate
stripper feed/effluent exchanger.
 And is sent to the process condensate stripper.
 In process condensate stripper, the process condensate is
stripped of dissolved impurities, such as hydrogen, nitrogen,
methane, argon, carbon monoxide, carbon dioxide, methanol,
amines using MP stripping stream.
 The condensate free of impurities is cooled further and sent to
offsite polisher to recycle the water as demineralised water.

STEAM SYSTEM:
The ammonia plant uses steam at five pressure levels.

Pressure head type Pressure kg/cm2 Temperature °C


High pressure 90 500
Medium pressure 63 462
32 kg/cm2 32 386
10 kg/cm2 10 332
2.5 kg/cm2 2.5 146

COOLING WATER:
 The cooling water supply is at 33℃. The overall mixed return
temperature is limited to 43℃.
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Conclusion:

Major engineering problems:


 Carbamate decomposition and recycle
There are many processes that can be used for the manufacture
of urea. Main difference lies in the recycle section. Since,
conversion is only 40-50% per pass, the unreacted off gases
must be recirculated or used economically. Recompression of
off gases is virtually impossible because of corrosion and
formation of solid carbamate in compressors.

 Production of granular urea


Biuret formation is another problem. Vacuum evaporation of
urea from 80% to about 99%, spraying to air cool and
solidification must be done just above the melting point of urea
and with a minimum residence time in the range of several
seconds.

 Heat dissipation in autoclave


The exothermic heat of reaction can be removed by coils or wall
cooling.

 Corrosion
This has been the major reason why the Ammonia-Carbon
dioxide process was slow to develop. High cost silver or
tantalum liners are used in the autoclaves with Alloy C,
Titanium, Stainless steel (321 SS) and Al alloys used in other
parts of the plant. Minimum pressure and temperature
conditions with excess Ammonia are desirable to reduce the
severe corrosion rates. Under these conditions stainless steel
can be use in the autoclave.
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 Gradual leakages in the plant
This problem arises due to many factors but the plant in process
can’t be suddenly stopped in between so many parts of the
same component are in spare and are joined in series so as if
one goes off another can be used without shut down of plant.

 Heat controlling components


The bearings of motors or pumps are not designed to withstand
large temperature ranges so in between heat exchangers,
coolers are required to minimise the loss of bearings.

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References:

1. Urea CASALE Technology.


2. KBR Technology.
3. Mr. Darshan (Manager Urea production plant), NFL Nangal.

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