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Operation and Trouble shooting in LP & Vacuum Section for M/S. Saipem Process
Presentation · July 2022
DOI: 10.13140/RG.2.2.33716.32641
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Prem Baboo
The Institution of Engineers (India)
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Operation and Trouble shooting in LP & Vacuum Section
for M/S. Saipem Process
By
Prem Baboo
Retired from National fertilizers Ltd. India
&
Dangote Fertilizers Ltd. Nigeria
Abstract
In Urea Process corrosion/Erosion also
observed in LP and vacuum section. The
paper indeed how to tackle this type of
problem? Root cause of corrosion in LP &
vacuum section. Construction of material
used in these sections. Operation of LP
section with trouble shooting How to
balance water in the process, Distillation
Tower Versus LP carbonate solution tank
with operation of LP decomposer. Water
balance in whole plant prilling rout as well
as granulation rout. How a small variation of
Pressure & temperature makes a drastic
change in the process including waste water
section? How Distillation tower feed related
to LP decomposer pressure & temperature?
The detail described in this article. The
intensity of corrosion is greatest in the
reaction section and the first recycle, where
pressures, temperatures and concentrations
are higher than downstream. The reactor
liner, pumps, decomposers, strippers and
condensers are more vulnerable to attack by
ammonium carbamate. But the corrosion is
also important in LP and vacuum sections.
The typical corrosion is observed in 2nd
stage of vacuum in some plants of urea.
Key words
Corrosion, erosion, water balance, trouble
shooting, vacuum section, Saipem,
Equilibrium. waste water.
Introduction
In M/S. Saipem Urea process the LP
decomposer is very important because the
water balances is related to either LP
carbonate solution or Distillation Tower
feed. In startup/shut down or any upset
condition of the process the 2nd
stage
vacuum section observed corrosion and
reduction of the vessel thickness. The sight
glasses are also given in the vessel for
seeing actual level in the field. The M/S.
Saipem process is the popular world famous
process and known as ammonia stripping
process. In capacity wise then there is no
comparison from other process. The HP loop
also very important for reactor and stripper
any variation in N/C & H/C ratio can cause
disturbances in downstream especially
vacuum section. Now 5000TPD plant is
ready and number of plants more than
4000TPD. Saipem is an advanced
technological and engineering platform for
the design, construction and operation of
safe and sustainable complex infrastructure
and plants. Saipem has always been oriented
towards technological innovation and is
currently committed, alongside its clients, on
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the frontline of energy transition with
increasingly digitalized tools, technologies
and processes that were devised from the
outset with environmental sustainability in
mind.
Description of the process
Snamprogetti ammonia stripping process is
characterized by a urea synthesis loop
operating at about 160 kg/cm2 (g) with
ammonia to carbon dioxide molar ratio at
urea reactor inlet of 3.3 - 3.6. This allows a
CO2 conversion into urea of 62 - 65% in the
reactor itself, also thanks to the perforated
trays which prevent back-flow and favor gas
absorption by the liquid. There are two kinds
of chemical reactions at the same time in the
urea reactor. Urea is produced by synthesis
from liquid ammonia and gaseous carbon
dioxide. Ammonia and carbon dioxide react
to form ammonium carbamate, a portion of
which dehydrates to form urea and water.
The reaction of ammonium carbamate
dehydration is influenced by the ratio of
various reactants, operating pressure,
temperature and residence time in reactor.
The reaction of ammonia and carbon dioxide
takes place in two stages to produce urea.
1. Formation of ammonium carbamate, at 25 0
C
2 NH3 (g) + CO2 (g) → NH4COONH2 (s) -38 086 cal/gmol
2. Dehydration of ammonium carbamate to urea, at 25 0
NH4COONH2 (s) → NH2CONH2 (l) + H2O (l) +10 330 cal/gmol
3. Overall reaction, at 25 0
C
2 NH3 (g) + CO2 (g) → NH2CONH2 (l) +H2O (l) -27 756 cal/gmol
The first reaction is highly exothermic and
heat is liberated as the reaction occurs. With
excess NH3, the CO2 conversion to
carbamate is almost 100%, provided
solution pressure is greater than
decomposition pressure. The decomposition
pressure is the pressure at which carbamate
will decompose back into CO2 and NH3 i.e.
,NH2 COO NH4 (s) → 2 NH3 (g) +
CO2 (g)
Decomposition pressure is a function of NH3
concentration in the feed and the solution
temperature and increases if either
temperature or NH3 recycle is increased. It is
desirable to operate at higher pressure and
high mole ratio of NH3 to CO2 provided
reactor operating pressure is quite high
enough to prevent carbamate from
decomposition into NH3 and CO2. This will
maximize CO2 conversion to urea towards
the reaction (ii). The second reaction is
endothermic; therefore heat is required for
this reaction to start. The heat for this
reaction comes from the heat of formation of
carbamate. This reaction is a function of
temperature and ammonia concentration in
the feed. The solution effluent from the
reactor being mixture of urea solution,
ammonium carbamate, un- reacted
ammonia, water and CO2 is extremely
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corrosive in nature. The subsequent stages of
process consist of decomposition
unconverted carbamate, recovery of
The decomposition of urea at temperatures
above 132 ◦C, some undesired parallel and
equilibrium intermediates and by
in liquid, solid and gaseous form are
produced , More than 23 possible reactions,
including urea and its numerous by
products, biuret, Triuret, cyanuric acid,
Fig-1
Description of LP & Vacuum section
Low pressure decomposer
Its function is to decompose residual
carbamate from M.P. decomposer, 10
02A/B, and separate it from the urea
solution. The final operating temperature is
determined by the concentration of urea
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corrosive in nature. The subsequent stages of
process consist of decomposition of
unconverted carbamate, recovery of
resulting ammonia and carbon dioxide for
recycle, concentration and prilling of urea
solution.
The decomposition of urea at temperatures
◦C, some undesired parallel and
equilibrium intermediates and by-products
in liquid, solid and gaseous form are
produced , More than 23 possible reactions,
including urea and its numerous by-
cyanuric acid,
ammelide, ammeline, melamine and others,
exist . In the whole reaction scheme,
isocyanic acid has been found to play a
major role. Nonetheless, it evaporates at
23.5 ◦C; reactions occurring at temperatures
exceeding 133 ◦C were formulated in the
condensed phase.As shown in the figure
& Vacuum section
Its function is to decompose residual
carbamate from M.P. decomposer, 10-E-
02A/B, and separate it from the urea
solution. The final operating temperature is
determined by the concentration of urea
solution needed at the outlet. NH3 content at
the outlet is between 1-3 % wt, CO2 is
between 0.3 -1.1 % wt and urea is around 70
% wt. These concentrations are obtained
with a temperature of approx. 144 °C and an
operating pressure of 3.7 kg/cm2 g.
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resulting ammonia and carbon dioxide for
recycle, concentration and prilling of urea
ammelide, ammeline, melamine and others,
exist . In the whole reaction scheme,
cid has been found to play a
major role. Nonetheless, it evaporates at
◦C; reactions occurring at temperatures
◦C were formulated in the
As shown in the figure-1.
at the outlet. NH3 content at
3 % wt, CO2 is
1.1 % wt and urea is around 70
% wt. These concentrations are obtained
with a temperature of approx. 144 °C and an
operating pressure of 3.7 kg/cm2 g.
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L.P. condenser 10-E-08
Its function is to condense mixture of gas
and liquid coming from L.P Decomposer
separator 10-V-03 and from Reflux
accumulator 27-V-17 . The L.P. condenser
10-E-08 receives the mixture of gas and
liquid from L.P Decomposer Separator 10
Carbonate solution accumulator 10
Fig-2
Normally it collects the diluted carbonate
solution coming from L.P. condenser, 10
08 and occasionally solution discharged
from M.P. absorber, 10-C-01 It is also used
for the recovery of NH3 and CO2 in case of
shut-down followed by emptying of the high
pressure equipment. By means of M.P.
carbonate pumps 10-P-03 A/B part of the
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Its function is to condense mixture of gas
and liquid coming from L.P Decomposer
03 and from Reflux
17 . The L.P. condenser
08 receives the mixture of gas and
liquid from L.P Decomposer Separator 10-
V-03 and from Reflux accumulator 27
through Reflux pumps 27
condensed solution flowing out of 10
is sent into carbonate solution accumulator,
10-V-06, at a temperature of 39 °C.
Carbonate solution accumulator 10-V-06
Normally it collects the diluted carbonate
solution coming from L.P. condenser, 10-E-
08 and occasionally solution discharged
01 It is also used
for the recovery of NH3 and CO2 in case of
emptying of the high
pressure equipment. By means of M.P.
03 A/B part of the
carbonate solution collected in 10
recycled into the M.P. absorber fed upstream
10-E-06. The operating temperature of 10
V-06 is about 39 °C and the
kept low in normal operation (20
max.) in order to recover all carbonate in
case of plant shutdown.
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03 and from Reflux accumulator 27-V-17
through Reflux pumps 27-P-17A/B. The
condensed solution flowing out of 10-E-08
is sent into carbonate solution accumulator,
06, at a temperature of 39 °C.
carbonate solution collected in 10-V-06 is
recycled into the M.P. absorber fed upstream
06. The operating temperature of 10-
06 is about 39 °C and the level must be
kept low in normal operation (20-30 %
max.) in order to recover all carbonate in
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Fig-3
L.P. inerts washing tower 10-C-04
Its function is to absorb with cold steam
condensate the NH3 vapors coming from
10-V-06. Non condensed vapours from L.P.
condenser, 10-E-08 are routed into 10-V-06,
and then absorbed with cold steam
condensate in L.P. inerts washing tower, 10-
C-04, where an ammonia solution is formed.
The ammonia solution is collected in
carbonate solution accumulator, 10-V06.
The released inert gases from 10-C-04 are
sent to the vent stack under pressure
controller that provides to maintain 10-V-06
at about 3.4 kg/cm2 g. Medium pressure
carbonate pumps 10-P-03 A/B Duty - Its
function is to pump carbonate solution from
carbonate solution accumulator, 10-V-06 to
medium pressure absorber, 10-C-01, through
M.P. condenser, 10-E-06. Operation - The
liquid is sucked from bottom of 10-V-06 at a
temperature of about 39 °C. The electrical
motor driven pumps have been designed to
recycle the dilute carbonate solution from
L.P. to M.P. Water is one of the products of
reaction during transformation reaction of
carbamate to urea. Its presence has a
depressing effect on the conversion. Any
addition of water with the feed reduces the
conversion. One mole of water is formed
when one mole of urea is produced.
Presence of excess water shifts the reaction
equilibrium in reverse direction and yield of
urea is reduced. However, water has to be
added for recycling unconverted ammonia
and CO2 back to the reactor. Lower the
amount of water concentration in low
pressure recovery section results in high
concentration of carbamate and this causes
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pumping and choking problem in piping
system. Excess water in reactor reduces
effective volume for urea formation and
additional energy is required in evaporation
section. Study shows that presence of one
mole of excess water per mole of carbamate
reduces the equilibrium yield of urea by
nearly one half.
Rate of transformation on CO2 to urea
with excess water
Fig. No. -4 shows the depressing effect of
water on conversion. The presence of water
limits the concentration of the product to an
aqueous solution containing not more than
76.93 % urea by weight. When the desired
product is a solid urea, all water must be
removed by either crystallization or
evaporation, which means expenditure of
energy and labour. Extra water from any
other source has an adverse effect upon the
concentration of urea. First, extra water
occupies volume in the autoclave, thereby
decreases its productive capacity. Second,
extra water dilutes the urea solution,
increases the load on the evaporation and
increases energy consumption. But most
important of all, excess water decrease the
yield of urea. The presence of one mole of
excess water per mole of carbamate cuts
down the yield of urea by nearly half. The
presence of excess ammonia over the
NH3:CO2 ratio of 2:1 counter acts to a great
extent the adverse influence of water. The
formation of urea in homogeneous solutions
is in no case dependant on the partial
pressure of carbon dioxide, but that the
conversion of carbamate into urea is directly
proportional to the partial pressure of
ammonia and inversely proportional to the
partial pressure of water.
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Fig-4
Low Pressure Section This section includes:
L.P. Decomposer, L.P. Condenser,
Carbonate Solution Accumulator and L.P.
inerts washing tower. Proceed with seal test
with condensate as follows:
1. Close all drains and vents on
lines and equipment. Open all
block valves and in
connections so that it is possible
to pressurize all lines and
equipment at the same time.
2. Isolate the loop by closing the
following valves: Discharge
valves of M.P. carbonate solution
pumps, Level control valve (10
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Section This section includes:
L.P. Decomposer, L.P. Condenser,
Carbonate Solution Accumulator and L.P.
inerts washing tower. Proceed with seal test
Close all drains and vents on
lines and equipment. Open all
block valves and instrument
connections so that it is possible
to pressurize all lines and
equipment at the same time.
Isolate the loop by closing the
following valves: Discharge
valves of M.P. carbonate solution
pumps, Level control valve (10-
LV-1014) of solution outlet fr
the Medium pressure
decomposer, Level control valve
10-LV-1022 of solution outlet
from low pressure decomposer,
10-HV-1012 from M.P. absorber
to the carbonate solution
accumulator.
3. Isolate this section from the
process condensate system by
closing the isolation valve on line
3”-10-P2722 which will be tested
separately.
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1014) of solution outlet from
the Medium pressure
decomposer, Level control valve
1022 of solution outlet
from low pressure decomposer,
1012 from M.P. absorber
to the carbonate solution
Isolate this section from the
process condensate system by
isolation valve on line
P2722 which will be tested
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4. Keep open the high point vent
on LP decomposer vapour line
and keep open 10-PV-1033,
5. If the steam headers are live,
isolate steam to all tracings, PSV
jacket and control valve jacket,
6. Admit condensate to the system
through the lowest points (10-
LV1022 upstream, 10-LV-1014
downstream,10-P-03 A/B
suction),
7. Close the vents when the
condensate is coming out,
8. Slowly increase the pressure in
the system up to the test value
(3.7 kg/cm2 g), keeping the
pressure controller 10-PIC-1033
on 10-V-06 in automatic mode.
9. Check all flanges and
connections in order to identify
leaks and eliminate them. If no
losses are found, keep the
pressure in the circuit over a
period of minimum 4 hours.
10. If pressure does not fall
appreciably the test can be
considered satisfactory,
otherwise it will be necessary to
look for the losses, to eliminate
them and then repeat the test.
Low Pressure Decomposer is Prime role
of Ammonium Carbonate Solution Tank
and (V-3) & Distillation Tower (C-2) for
Ammonia CO2 Load and water Balance
The LPD pressure and temperature are the
prime role of Ammonia and CO2 load on
Carbonate solution and distillation tower
Feed. As per attached figure No-5. If you
maintain the design pressure and
temperature according to equilibrium then
V-3 & C-2 load will be ok. If you raised the
temperature ad reduced the pressure then V-
3 level will be increased. Another case if
you increase the pressure and reduced the
temperature then C-2 feed concentration in
terms of Ammonia & CO2 will be increased.
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Fig-5
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Water Balance for 3850 TPD Urea Plants (Prilling Rout)
T/H
1 Water from 3850 Urea production 48.125
2 Steam added in Pre-Concentrator Ejectors 3.2
3 Steam added in 1st
stage Ejector of Vacuums 3.8
4 Steam added in 2nd
stage Ejector of Vacuum
with Booster Ejector
14.5
5 Condensate to Carbonate Solution Tank 0.9
6 Condensate to MP Inerts washing column 2.276
7
Condensate to HP ammonia Feed Pump
sealing
1.0
8
Condensate to HP Amm. carbamate pump
sealing
1.0
9
Condensate to Flushing of Pre Conc,
Vacuum, MP absorber Intermittently
1
10 Condensate to different types of FT 1
11 Condensate from Vent stack 1.5
12 Water recycle from waste water section 5.535
Total Water in Urea Process 85.036
Distillation Tower Feed
NH3 4.831
CO2 0.966
Urea 0.95
Water 85.036
Total Feed 91.783
Table-1
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Water Balance for 3850TPD Urea Plants(Granulation Rout)
T/H
1 Water from 3850 Urea production 48.125
2 Steam added in Pre-Concentrator Ejectors 3.2
3 Steam added in Ejector of Vacuums 3
4 Condensate to Vacuum Scrubber 5
5 Condensate to Crabonate Solution Tank 0.9
6 Condensate to MP Inerts washing column 2.276
7
Condensate to HP ammonia Feed Pump
sealing
1.5
8
Condensate to HP Amm.Carbamate pump
sealing
1.5
9
Condensate to Flushing of Pre Conc, Vacuum,
MP absorber Intermittently
1.5
10 Condensate to different types of FT 1.5
11 Condensate from Vent stack 2.1
12 Water recycle from waste water section 13.499
Granulation
1 Process water to Cooler Scrubber( C-51) 35.133
2 Process water to Granulation Scrubber( C-55) 31.8
3 LS to Ejector Urea solution Tank 2.0
4 water from waste basin 2.0
5 LS to X-53 (Ejector) 2.544
Total Water in Urea Process 157.577
Distillation Tower Feed
NH3 9.777
CO2 1.916
Urea 0.88
Water 145.004
Total Feed 157.577
Table-2
Waste Water Section Water Balance, in T/Hr(Prilling Rout)
Input water Outlet water
C-2 Feed water 85.036 Water from C-2 Bottom 105.556
Steam(LMS) to C-2 20.7 Water from C-2 Top 5.573
Steam(HS) to R-2 6.5 Water from R-2 Top 1.107
Total 112.236 Total 112.236
Table-3
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Waste Water Section Water Balance, in T/Hr (Granulation Rout)
Input water Outlet water
C-2 Feed water 145.004 Water from C-2 Bottom 176.524
Steam(LMS) to C-2 35.3 Water from C-2 Top 13.499
Steam(HS) to R-2 12.9 Water from R-2 Top 4.6
Total 193.204 Total 194.623
Table-4
After completion of seal test the section will
be depressurized and all the water will be
drained by keeping the high points open.
Keep the level around 50% in Carbonate
solution accumulator 10-V-06.Vacuum
Evaporation Section This section includes:
Vacuum Concentrator and Separator,
Ejectors and Vacuum Condensers. The seal
test might be performed with air as follows
or filling the system with water. Isolate the
loop as follows:
1. Place adhesive tape on all
flanged connections making sure
that it is firmly sealed to the
flange edges, and then make a
small hole on the tape for leak
check by using soapy water.
2. Install blinds on the discharge
lines to the hydraulic seals at 10-
T02.
3. Close all drains and vents on
lines and equipment.
4. Open the block valves to
pressurize all the lines and
equipment simultaneously.
5. Close the level control valve 10-
LV-1022 on the L.P. decomposer
solution outlet line,
6. Close 10-P-08A/B suction
valves,
7. Close the Ejector steam isolation
valves,
8. Isolation valves on recovered
solution lines to vacuum
concentrator (from 10-P-09 A/B,
Granulation)
9. Close pressure control valves 10-
PV-1034 A/B and vent lines
from vacuum system packages.
10. Connect air hose at a suitable
location and admit air into the
system pressurizing up to 0.5
kg/cm2 g.
11. Check all flanges and
connections using soap solution
to identify leaks and eliminate
them.
12. If pressure does not fall
appreciably the test can be
considered satisfactory,
otherwise it will be necessary to
look for the losses, to eliminate
them and then repeat the test.
13. When the test has been carried
out successfully, depressurize by
opening the high point vents,
remove the blinds installed on the
discharge of the hydraulic seals
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and adjust the valves as described
later under start-up procedure.
14. during the leak test isolate steam
to all the steam tracings and
jacketing
1. Alternative by water filling Follow
operations of first nine points
mentioned above, then proceed as
follows.
2. Admit condensate to the system
through the lowest points and keep
the vent at highest point opened.
3. Stop the water injection when
condensate is coming out from
highest point.
4. Check all the flanges and valves for
leaks and attend them. When no
more leaks are detected the test can
be considered completed and the
system emptied.
Trouble Shooting of LP Decomposer
Variables Change Effect Corrective action
Bottom
temperature
decrease Overload of the down-
stream section
Check the M.P. decomposer
holder 10-L-02 temperature.
Check the L.P. decomposer 10-L-
03 holder level. Check the steam
flow to L.P. decomposer. Check
level in steam condensate
separator 10-V-24
Increase Level of carbonate
solution accumulator
10-V-06 increases due
to excessive off-gas
production in L.P.
decomposer.
Decrease the temperature by
reducing the steam flow at L.P.
decomposer.
Pressure
Decrease 10-P-03 A/B may begin
to cavitated.
Reduce water recovery from
process condensate treatment by
reducing, if possible, the steam
flow rate to the column 27-C-02
or to the Hydrolyzer 27-R02; an
option is to increase the reflux to
27-C-02. Last, reduce CW flow to
L.P. condenser 10-E-08; this may
cause
Increase Overload of the down-
stream section.
Check the M.P. decomposer
holder level controller and restore
the normal condition
Decrease Vapours can pass to the
downstream section and
there is the possibility
to break the vacuum
Close slightly L.P decomposer
level control valve or open
temporarily the M.P. decomposer
holder level control valve. Check
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Level conditions in vacuum
concentration section.
the correct functioning of L.P.
decomposer holder level control
valve and M.P. decomposer
holder level control valve.
Increase Flooding of L.P.
decomposer and
consequently urea carry
over to accumulator 10-
V-06.
Increase the steam flow to LP
Decomposer .Check the level and
restore the normal situation
without disturbing
Table-5
Corrosion Reported in 2nd
stage of
Vacuum in Many Plants
Number of plants reported corrosion in 2nd
stage of vacuum and part ion plate crack in
vacuum waste water tank (V-09).Some
plants reported erosion problem in 2nd
stage
of inlet nozzle. But question arise why in 1st
stage of vacuum? Following are the reason
for above problems. Urea itself is considered
as non-corrosive for stainless steel, while
some of its decomposition products at high
temperature may lead to corrosion. The urea
decomposition process plays a role in the
corrosion of stainless steel. All
corresponding decomposition products,
which exist in the solid, liquid and gaseous
state and correlate with temperature and pH
value at which they may lead to uniform
corrosion. In start up the urea concentration
is less means the ammonium
Carbamate/carbonates are there and it is
very highly corrosive to SS-304 L. The urea
solution from LPD/Pre concentrator to be
lined up to vacuum section when proper
temperature and concentration achieve
during start-up of the plant.
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Fig-6
1. In startup/ shut down, No Vacuum in
both vacuum separators, the quantity
wise 1st
vacuum inlet and 2nd
vacuum
inlet feed is about the same the first
vacuum separator area is more very
large vessel and 2nd
vacuum separator is
to small as compare to first and the
liquid/vapour load per square meter is
more so the corrosion is more in 2nd
vacuum separator.
2. The 1st
vacuum separator has large
volume and two number vacuum control
valves (PIC 140A/B) are there, one is
for sudden vacuum breaker (Large
capacity) other is less capacity for
controlling of vacuum. These valves are
air failure to open.
The 1st
stage vacuum design is 0.33 ata.
But practical point of view this vacuum
maintain about 0.4 ata for maintaining
the temperature to avoid crystallization.
Because of large volume the vacuum
breaker valve (B) is always open and air
introduces into the vessel this air act as a
passivation for SS 304 L.
3. In case of 2nd
separator the vacuum
maintain about 0.03 ata , it is high
vacuum booster ejector is required to
pull of vacuum and control valve (PIC
141) is always closed.
4. Due to high vacuum the velocity of
solution inlet of nozzle is high the
erosion also observed.
5. The 2nd
vacuums also have Skirt inside
the deposition of polymer always there
inside and outside. However some plants
have removed the skirt. This skirt is the
reason of corrosion.
6. The temperature in 2nd
stage separator is
more 135-1400
C.more temperature more
corrosion see fig-6
7. The 1st
stage having more water and
about all the water removed by 1st
stage.
www.researchgate.net
This is an open access article, Research Gate
water is not corrosive . Corrosive is
mixture of NH3/CO2 mixture.
8. The water balance as shown in the
following figure-9
Fig-7
16th
July. 2022
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This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers
water is not corrosive . Corrosive is
mixture.
The water balance as shown in the
9. Corrosion is the function of
fig-6
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is a European commercial social networking site for scientists and researchers
Corrosion is the function of temperature
www.researchgate.net
This is an open access article, Research Gate
Fig-8
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July. 2022
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Research Gate is an academic social networking site
is a European commercial social networking site for scientists and researchers
www.researchgate.net
16th
July. 2022
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This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers
Fig-9
Waste Water Treatment Section
The distillation tower is divided into two parts:
the lower part consists of 38 trays and the upper
part of 17 valve trays. The feed is placed on the
51st
or 45th
tray. The wastewater containing
NH3, C02 and urea after a first stripping of the
ammonia in the upper part of the lower is sent to
the hydrolyser for the decomposition of urea.
The treated water from the hydrolyser comes
back to the lower where the top of lower part
where the remaining ammonia is stripped out by
means of 6.5 Ata saturated steam directly fed to
C-2 bottom. The vapors leaving the top of the
tower are condensed in 11-E-17 by cooling
water and the carbonate solution produced is
recovered in the reflux accumulator 11-V-5.The
process condensate containing NH3-CO2 and
urea coming out from vacuum system of both
urea units, 10 & 20 is treated in this section to
make free of contaminants before sent to utility
unit. The contaminated water of each urea unit is
collected in the process condensate tank 10-T-
02. From this tank the process condensate is
pumped, by means of 10-P-14 A/B, to a
common buffer off spec tank, 27-T-05, then the
mixed solution is sent to the upper part of
distillation tower 27-C-02. The Tank 10-T-02
also receives the drain solutions accumulated
into underground carbonate close drain tank 10-
T-04, and fed to process condensate tank by
means of pump 10-P-16 A/B. Before entering
the distillation column, the process condensate
picks up heat from the purified condensate
leaving the bottom of the column itself, by
means of pre heater 27-E-16. The column 27-C-
02 is provided with trays and is divided in two
main sections by a chimney tray. Column
process conditions are: - Pressure (top): 2.5
kg/cm2 (g) - Temperature (top): 118 °C The
condensate from the chimney tray is drawn and
pumped, by centrifugal pump 27-P-15 A/B/C, to
urea hydrolyzer 27-R-02, where process
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16th
July. 2022
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conditions are suitable to decompose urea into
CO2 and NH3.The necessary decomposition heat
is provided by adding steam at 44 kg/cm2 (g)
and 380 °C. Hydrolyzer
process conditions are: - Pressure: 34 kg/cm2 (g)
- Temperature: 235 °C The out coming vapours
from the hydrolyzer as well as the vapours from
the top of the distillation tower are mixed and
condensed in the overhead condenser, 27-E-17,
then collected in the reflux accumulator, 27-V-
17 and split to LP section of urea unit 10 & 20
by reflux pumps, 27-P-17A/B. The recycle
stream is mixed upstream of 10-E-08 with the
LP Decomposer overhead vapors. The
hydrolyzed condensate leaving the bottom of the
27-R-02, after having decreased its temperature
passing through hydrolyser preheated, 27-E-18,
enters the distillation tower immediately under
the chimney tray where the final NH3 and CO2
stripping takes place. Saturated steam at 5.3
kg/cm2 (g), injected directly at the column
bottom, and provides the necessary stripping
force. The purified process condensate leaves
the column bottom at 143°C and it is cooled at
45°C by means of : - Distillation tower feed
preheating by means of 27-E-16 - Process
condensate cooler 27-E-23
www.researchgate.net
This is an open access article, Research Gate
Fig-10
Impotence of Reflux and Steam to
Distillation Tower
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July. 2022
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Impotence of Reflux and Steam to The reflux to distillation column decide
concentration of reflux accumulator section
.How much steam is required? Increasing
Research Gate is an academic social networking site
is a European commercial social networking site for scientists and researchers
The reflux to distillation column decide
concentration of reflux accumulator section
.How much steam is required? Increasing
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16th
July. 2022
Research Gate is an academic social networking site
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/decreasing of steam can cause the
distillation column disturbed. Inside the
column, the down flowing reflux
liquid provides cooling and condensation of
the up flowing vapors thereby increasing the
efficiency of the distillation column. The
purpose of reflux is to provide down-
flowing liquid throughout the rectification
section to contact with the up-flowing vapor
in order to achieve stage-by-stage
equilibrium heat and mass transfer and,
hence, purification of the top product. The
utility cost includes Steam to distillation in
bottom and cooling water cost in overhead
condenser. As reflux ratio increases more of
the steam heat is consumed to vaporize the
incoming liquid which results in energy loss.
Also more of the steam for heating purpose
will be wasted. Because of the higher steam
duty as the more volatile component reaches
the condenser with higher rate thus more of
the cooling water will be required which
again results in a loss of energy. If you give
more steam in bottom then concentration of
reflux accumulator will be decrease because
at certain point that steam will condense in
accumulator. A practical curve for 4000
TPD Plant as figure No-11
Fig-11
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16th
July. 2022
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This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers
Conclusion
It has been observed the water balance of the
plant is main key factor. It must be balance
and optimized otherwise conversion of urea
will be disturbed. The safe plants operation
is the technical art. A small mistake can
make big incident. The operations of this
activity implies a unit shut-down duration of
not more than 48 hours (24 hours during 1st
start-up of the unit), leaving the H.P. loop
bottled before corrosion problems can take
place. If maintenance jobs have to be
performed on the unit (excluding the
synthesis loop) it is possible to separately
depressurize and drain the required
equipment, leaving the reactor full and ready
to restart. It is suggested, before starting any
maintenance job, isolate NH3 and carbonate
solution vessels from the remaining unit,
controlling the pressure by the respective
PIC in automatic mode. It is not advisable to
carry out series of inlet contacts to interlock
system, exception Consist of push button
and selector switches on the control board
and particular cases which must be
considered one by one. The push buttons for
shut down shall be protected from accidental
operation. The analysis points and the
frequency with which they have to be
carried out, during start-up and under normal
running conditions. Number of the
instruments in the plant are equipped with
passive alarms to warn the operators in the
control room against deviating operating
conditions which may lead to dangerous
situations or which may cause damage to the
equipment. A leakage detection system
should be developed due to impurities in
steam-damaged steels. The barrier of having
an effective start-up procedure was totally
ineffective as this not apply to the specific
conditions applicable on the day. The water
balance must be checked day by day.
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OPERATION AND TROUBLE SHOOTING IN LP AND VACUUM SECTION FOR MS SAIPEM PROCESS (1).pdf

  • 1. See discussions, stats, and author profiles for this publication at: https://www.researchgate.net/publication/362034614 Operation and Trouble shooting in LP & Vacuum Section for M/S. Saipem Process Presentation · July 2022 DOI: 10.13140/RG.2.2.33716.32641 CITATIONS 0 1 author: Some of the authors of this publication are also working on these related projects: Silo (UREA) level measurement View project Comparison Stamicarbon Saipem View project Prem Baboo The Institution of Engineers (India) 85 PUBLICATIONS   26 CITATIONS    SEE PROFILE All content following this page was uploaded by Prem Baboo on 16 July 2022. The user has requested enhancement of the downloaded file.
  • 2. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Operation and Trouble shooting in LP & Vacuum Section for M/S. Saipem Process By Prem Baboo Retired from National fertilizers Ltd. India & Dangote Fertilizers Ltd. Nigeria Abstract In Urea Process corrosion/Erosion also observed in LP and vacuum section. The paper indeed how to tackle this type of problem? Root cause of corrosion in LP & vacuum section. Construction of material used in these sections. Operation of LP section with trouble shooting How to balance water in the process, Distillation Tower Versus LP carbonate solution tank with operation of LP decomposer. Water balance in whole plant prilling rout as well as granulation rout. How a small variation of Pressure & temperature makes a drastic change in the process including waste water section? How Distillation tower feed related to LP decomposer pressure & temperature? The detail described in this article. The intensity of corrosion is greatest in the reaction section and the first recycle, where pressures, temperatures and concentrations are higher than downstream. The reactor liner, pumps, decomposers, strippers and condensers are more vulnerable to attack by ammonium carbamate. But the corrosion is also important in LP and vacuum sections. The typical corrosion is observed in 2nd stage of vacuum in some plants of urea. Key words Corrosion, erosion, water balance, trouble shooting, vacuum section, Saipem, Equilibrium. waste water. Introduction In M/S. Saipem Urea process the LP decomposer is very important because the water balances is related to either LP carbonate solution or Distillation Tower feed. In startup/shut down or any upset condition of the process the 2nd stage vacuum section observed corrosion and reduction of the vessel thickness. The sight glasses are also given in the vessel for seeing actual level in the field. The M/S. Saipem process is the popular world famous process and known as ammonia stripping process. In capacity wise then there is no comparison from other process. The HP loop also very important for reactor and stripper any variation in N/C & H/C ratio can cause disturbances in downstream especially vacuum section. Now 5000TPD plant is ready and number of plants more than 4000TPD. Saipem is an advanced technological and engineering platform for the design, construction and operation of safe and sustainable complex infrastructure and plants. Saipem has always been oriented towards technological innovation and is currently committed, alongside its clients, on
  • 3. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers the frontline of energy transition with increasingly digitalized tools, technologies and processes that were devised from the outset with environmental sustainability in mind. Description of the process Snamprogetti ammonia stripping process is characterized by a urea synthesis loop operating at about 160 kg/cm2 (g) with ammonia to carbon dioxide molar ratio at urea reactor inlet of 3.3 - 3.6. This allows a CO2 conversion into urea of 62 - 65% in the reactor itself, also thanks to the perforated trays which prevent back-flow and favor gas absorption by the liquid. There are two kinds of chemical reactions at the same time in the urea reactor. Urea is produced by synthesis from liquid ammonia and gaseous carbon dioxide. Ammonia and carbon dioxide react to form ammonium carbamate, a portion of which dehydrates to form urea and water. The reaction of ammonium carbamate dehydration is influenced by the ratio of various reactants, operating pressure, temperature and residence time in reactor. The reaction of ammonia and carbon dioxide takes place in two stages to produce urea. 1. Formation of ammonium carbamate, at 25 0 C 2 NH3 (g) + CO2 (g) → NH4COONH2 (s) -38 086 cal/gmol 2. Dehydration of ammonium carbamate to urea, at 25 0 NH4COONH2 (s) → NH2CONH2 (l) + H2O (l) +10 330 cal/gmol 3. Overall reaction, at 25 0 C 2 NH3 (g) + CO2 (g) → NH2CONH2 (l) +H2O (l) -27 756 cal/gmol The first reaction is highly exothermic and heat is liberated as the reaction occurs. With excess NH3, the CO2 conversion to carbamate is almost 100%, provided solution pressure is greater than decomposition pressure. The decomposition pressure is the pressure at which carbamate will decompose back into CO2 and NH3 i.e. ,NH2 COO NH4 (s) → 2 NH3 (g) + CO2 (g) Decomposition pressure is a function of NH3 concentration in the feed and the solution temperature and increases if either temperature or NH3 recycle is increased. It is desirable to operate at higher pressure and high mole ratio of NH3 to CO2 provided reactor operating pressure is quite high enough to prevent carbamate from decomposition into NH3 and CO2. This will maximize CO2 conversion to urea towards the reaction (ii). The second reaction is endothermic; therefore heat is required for this reaction to start. The heat for this reaction comes from the heat of formation of carbamate. This reaction is a function of temperature and ammonia concentration in the feed. The solution effluent from the reactor being mixture of urea solution, ammonium carbamate, un- reacted ammonia, water and CO2 is extremely
  • 4. www.researchgate.net This is an open access article, Research Gate corrosive in nature. The subsequent stages of process consist of decomposition unconverted carbamate, recovery of The decomposition of urea at temperatures above 132 ◦C, some undesired parallel and equilibrium intermediates and by in liquid, solid and gaseous form are produced , More than 23 possible reactions, including urea and its numerous by products, biuret, Triuret, cyanuric acid, Fig-1 Description of LP & Vacuum section Low pressure decomposer Its function is to decompose residual carbamate from M.P. decomposer, 10 02A/B, and separate it from the urea solution. The final operating temperature is determined by the concentration of urea 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers corrosive in nature. The subsequent stages of process consist of decomposition of unconverted carbamate, recovery of resulting ammonia and carbon dioxide for recycle, concentration and prilling of urea solution. The decomposition of urea at temperatures ◦C, some undesired parallel and equilibrium intermediates and by-products in liquid, solid and gaseous form are produced , More than 23 possible reactions, including urea and its numerous by- cyanuric acid, ammelide, ammeline, melamine and others, exist . In the whole reaction scheme, isocyanic acid has been found to play a major role. Nonetheless, it evaporates at 23.5 ◦C; reactions occurring at temperatures exceeding 133 ◦C were formulated in the condensed phase.As shown in the figure & Vacuum section Its function is to decompose residual carbamate from M.P. decomposer, 10-E- 02A/B, and separate it from the urea solution. The final operating temperature is determined by the concentration of urea solution needed at the outlet. NH3 content at the outlet is between 1-3 % wt, CO2 is between 0.3 -1.1 % wt and urea is around 70 % wt. These concentrations are obtained with a temperature of approx. 144 °C and an operating pressure of 3.7 kg/cm2 g. Research Gate is an academic social networking site is a European commercial social networking site for scientists and researchers resulting ammonia and carbon dioxide for recycle, concentration and prilling of urea ammelide, ammeline, melamine and others, exist . In the whole reaction scheme, cid has been found to play a major role. Nonetheless, it evaporates at ◦C; reactions occurring at temperatures ◦C were formulated in the As shown in the figure-1. at the outlet. NH3 content at 3 % wt, CO2 is 1.1 % wt and urea is around 70 % wt. These concentrations are obtained with a temperature of approx. 144 °C and an operating pressure of 3.7 kg/cm2 g.
  • 5. www.researchgate.net This is an open access article, Research Gate L.P. condenser 10-E-08 Its function is to condense mixture of gas and liquid coming from L.P Decomposer separator 10-V-03 and from Reflux accumulator 27-V-17 . The L.P. condenser 10-E-08 receives the mixture of gas and liquid from L.P Decomposer Separator 10 Carbonate solution accumulator 10 Fig-2 Normally it collects the diluted carbonate solution coming from L.P. condenser, 10 08 and occasionally solution discharged from M.P. absorber, 10-C-01 It is also used for the recovery of NH3 and CO2 in case of shut-down followed by emptying of the high pressure equipment. By means of M.P. carbonate pumps 10-P-03 A/B part of the 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Its function is to condense mixture of gas and liquid coming from L.P Decomposer 03 and from Reflux 17 . The L.P. condenser 08 receives the mixture of gas and liquid from L.P Decomposer Separator 10- V-03 and from Reflux accumulator 27 through Reflux pumps 27 condensed solution flowing out of 10 is sent into carbonate solution accumulator, 10-V-06, at a temperature of 39 °C. Carbonate solution accumulator 10-V-06 Normally it collects the diluted carbonate solution coming from L.P. condenser, 10-E- 08 and occasionally solution discharged 01 It is also used for the recovery of NH3 and CO2 in case of emptying of the high pressure equipment. By means of M.P. 03 A/B part of the carbonate solution collected in 10 recycled into the M.P. absorber fed upstream 10-E-06. The operating temperature of 10 V-06 is about 39 °C and the kept low in normal operation (20 max.) in order to recover all carbonate in case of plant shutdown. Research Gate is an academic social networking site is a European commercial social networking site for scientists and researchers 03 and from Reflux accumulator 27-V-17 through Reflux pumps 27-P-17A/B. The condensed solution flowing out of 10-E-08 is sent into carbonate solution accumulator, 06, at a temperature of 39 °C. carbonate solution collected in 10-V-06 is recycled into the M.P. absorber fed upstream 06. The operating temperature of 10- 06 is about 39 °C and the level must be kept low in normal operation (20-30 % max.) in order to recover all carbonate in
  • 6. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Fig-3 L.P. inerts washing tower 10-C-04 Its function is to absorb with cold steam condensate the NH3 vapors coming from 10-V-06. Non condensed vapours from L.P. condenser, 10-E-08 are routed into 10-V-06, and then absorbed with cold steam condensate in L.P. inerts washing tower, 10- C-04, where an ammonia solution is formed. The ammonia solution is collected in carbonate solution accumulator, 10-V06. The released inert gases from 10-C-04 are sent to the vent stack under pressure controller that provides to maintain 10-V-06 at about 3.4 kg/cm2 g. Medium pressure carbonate pumps 10-P-03 A/B Duty - Its function is to pump carbonate solution from carbonate solution accumulator, 10-V-06 to medium pressure absorber, 10-C-01, through M.P. condenser, 10-E-06. Operation - The liquid is sucked from bottom of 10-V-06 at a temperature of about 39 °C. The electrical motor driven pumps have been designed to recycle the dilute carbonate solution from L.P. to M.P. Water is one of the products of reaction during transformation reaction of carbamate to urea. Its presence has a depressing effect on the conversion. Any addition of water with the feed reduces the conversion. One mole of water is formed when one mole of urea is produced. Presence of excess water shifts the reaction equilibrium in reverse direction and yield of urea is reduced. However, water has to be added for recycling unconverted ammonia and CO2 back to the reactor. Lower the amount of water concentration in low pressure recovery section results in high concentration of carbamate and this causes
  • 7. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers pumping and choking problem in piping system. Excess water in reactor reduces effective volume for urea formation and additional energy is required in evaporation section. Study shows that presence of one mole of excess water per mole of carbamate reduces the equilibrium yield of urea by nearly one half. Rate of transformation on CO2 to urea with excess water Fig. No. -4 shows the depressing effect of water on conversion. The presence of water limits the concentration of the product to an aqueous solution containing not more than 76.93 % urea by weight. When the desired product is a solid urea, all water must be removed by either crystallization or evaporation, which means expenditure of energy and labour. Extra water from any other source has an adverse effect upon the concentration of urea. First, extra water occupies volume in the autoclave, thereby decreases its productive capacity. Second, extra water dilutes the urea solution, increases the load on the evaporation and increases energy consumption. But most important of all, excess water decrease the yield of urea. The presence of one mole of excess water per mole of carbamate cuts down the yield of urea by nearly half. The presence of excess ammonia over the NH3:CO2 ratio of 2:1 counter acts to a great extent the adverse influence of water. The formation of urea in homogeneous solutions is in no case dependant on the partial pressure of carbon dioxide, but that the conversion of carbamate into urea is directly proportional to the partial pressure of ammonia and inversely proportional to the partial pressure of water.
  • 8. www.researchgate.net This is an open access article, Research Gate Fig-4 Low Pressure Section This section includes: L.P. Decomposer, L.P. Condenser, Carbonate Solution Accumulator and L.P. inerts washing tower. Proceed with seal test with condensate as follows: 1. Close all drains and vents on lines and equipment. Open all block valves and in connections so that it is possible to pressurize all lines and equipment at the same time. 2. Isolate the loop by closing the following valves: Discharge valves of M.P. carbonate solution pumps, Level control valve (10 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Section This section includes: L.P. Decomposer, L.P. Condenser, Carbonate Solution Accumulator and L.P. inerts washing tower. Proceed with seal test Close all drains and vents on lines and equipment. Open all block valves and instrument connections so that it is possible to pressurize all lines and equipment at the same time. Isolate the loop by closing the following valves: Discharge valves of M.P. carbonate solution pumps, Level control valve (10- LV-1014) of solution outlet fr the Medium pressure decomposer, Level control valve 10-LV-1022 of solution outlet from low pressure decomposer, 10-HV-1012 from M.P. absorber to the carbonate solution accumulator. 3. Isolate this section from the process condensate system by closing the isolation valve on line 3”-10-P2722 which will be tested separately. Research Gate is an academic social networking site is a European commercial social networking site for scientists and researchers 1014) of solution outlet from the Medium pressure decomposer, Level control valve 1022 of solution outlet from low pressure decomposer, 1012 from M.P. absorber to the carbonate solution Isolate this section from the process condensate system by isolation valve on line P2722 which will be tested
  • 9. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers 4. Keep open the high point vent on LP decomposer vapour line and keep open 10-PV-1033, 5. If the steam headers are live, isolate steam to all tracings, PSV jacket and control valve jacket, 6. Admit condensate to the system through the lowest points (10- LV1022 upstream, 10-LV-1014 downstream,10-P-03 A/B suction), 7. Close the vents when the condensate is coming out, 8. Slowly increase the pressure in the system up to the test value (3.7 kg/cm2 g), keeping the pressure controller 10-PIC-1033 on 10-V-06 in automatic mode. 9. Check all flanges and connections in order to identify leaks and eliminate them. If no losses are found, keep the pressure in the circuit over a period of minimum 4 hours. 10. If pressure does not fall appreciably the test can be considered satisfactory, otherwise it will be necessary to look for the losses, to eliminate them and then repeat the test. Low Pressure Decomposer is Prime role of Ammonium Carbonate Solution Tank and (V-3) & Distillation Tower (C-2) for Ammonia CO2 Load and water Balance The LPD pressure and temperature are the prime role of Ammonia and CO2 load on Carbonate solution and distillation tower Feed. As per attached figure No-5. If you maintain the design pressure and temperature according to equilibrium then V-3 & C-2 load will be ok. If you raised the temperature ad reduced the pressure then V- 3 level will be increased. Another case if you increase the pressure and reduced the temperature then C-2 feed concentration in terms of Ammonia & CO2 will be increased.
  • 10. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Fig-5
  • 11. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Water Balance for 3850 TPD Urea Plants (Prilling Rout) T/H 1 Water from 3850 Urea production 48.125 2 Steam added in Pre-Concentrator Ejectors 3.2 3 Steam added in 1st stage Ejector of Vacuums 3.8 4 Steam added in 2nd stage Ejector of Vacuum with Booster Ejector 14.5 5 Condensate to Carbonate Solution Tank 0.9 6 Condensate to MP Inerts washing column 2.276 7 Condensate to HP ammonia Feed Pump sealing 1.0 8 Condensate to HP Amm. carbamate pump sealing 1.0 9 Condensate to Flushing of Pre Conc, Vacuum, MP absorber Intermittently 1 10 Condensate to different types of FT 1 11 Condensate from Vent stack 1.5 12 Water recycle from waste water section 5.535 Total Water in Urea Process 85.036 Distillation Tower Feed NH3 4.831 CO2 0.966 Urea 0.95 Water 85.036 Total Feed 91.783 Table-1
  • 12. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Water Balance for 3850TPD Urea Plants(Granulation Rout) T/H 1 Water from 3850 Urea production 48.125 2 Steam added in Pre-Concentrator Ejectors 3.2 3 Steam added in Ejector of Vacuums 3 4 Condensate to Vacuum Scrubber 5 5 Condensate to Crabonate Solution Tank 0.9 6 Condensate to MP Inerts washing column 2.276 7 Condensate to HP ammonia Feed Pump sealing 1.5 8 Condensate to HP Amm.Carbamate pump sealing 1.5 9 Condensate to Flushing of Pre Conc, Vacuum, MP absorber Intermittently 1.5 10 Condensate to different types of FT 1.5 11 Condensate from Vent stack 2.1 12 Water recycle from waste water section 13.499 Granulation 1 Process water to Cooler Scrubber( C-51) 35.133 2 Process water to Granulation Scrubber( C-55) 31.8 3 LS to Ejector Urea solution Tank 2.0 4 water from waste basin 2.0 5 LS to X-53 (Ejector) 2.544 Total Water in Urea Process 157.577 Distillation Tower Feed NH3 9.777 CO2 1.916 Urea 0.88 Water 145.004 Total Feed 157.577 Table-2 Waste Water Section Water Balance, in T/Hr(Prilling Rout) Input water Outlet water C-2 Feed water 85.036 Water from C-2 Bottom 105.556 Steam(LMS) to C-2 20.7 Water from C-2 Top 5.573 Steam(HS) to R-2 6.5 Water from R-2 Top 1.107 Total 112.236 Total 112.236 Table-3
  • 13. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Waste Water Section Water Balance, in T/Hr (Granulation Rout) Input water Outlet water C-2 Feed water 145.004 Water from C-2 Bottom 176.524 Steam(LMS) to C-2 35.3 Water from C-2 Top 13.499 Steam(HS) to R-2 12.9 Water from R-2 Top 4.6 Total 193.204 Total 194.623 Table-4 After completion of seal test the section will be depressurized and all the water will be drained by keeping the high points open. Keep the level around 50% in Carbonate solution accumulator 10-V-06.Vacuum Evaporation Section This section includes: Vacuum Concentrator and Separator, Ejectors and Vacuum Condensers. The seal test might be performed with air as follows or filling the system with water. Isolate the loop as follows: 1. Place adhesive tape on all flanged connections making sure that it is firmly sealed to the flange edges, and then make a small hole on the tape for leak check by using soapy water. 2. Install blinds on the discharge lines to the hydraulic seals at 10- T02. 3. Close all drains and vents on lines and equipment. 4. Open the block valves to pressurize all the lines and equipment simultaneously. 5. Close the level control valve 10- LV-1022 on the L.P. decomposer solution outlet line, 6. Close 10-P-08A/B suction valves, 7. Close the Ejector steam isolation valves, 8. Isolation valves on recovered solution lines to vacuum concentrator (from 10-P-09 A/B, Granulation) 9. Close pressure control valves 10- PV-1034 A/B and vent lines from vacuum system packages. 10. Connect air hose at a suitable location and admit air into the system pressurizing up to 0.5 kg/cm2 g. 11. Check all flanges and connections using soap solution to identify leaks and eliminate them. 12. If pressure does not fall appreciably the test can be considered satisfactory, otherwise it will be necessary to look for the losses, to eliminate them and then repeat the test. 13. When the test has been carried out successfully, depressurize by opening the high point vents, remove the blinds installed on the discharge of the hydraulic seals
  • 14. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers and adjust the valves as described later under start-up procedure. 14. during the leak test isolate steam to all the steam tracings and jacketing 1. Alternative by water filling Follow operations of first nine points mentioned above, then proceed as follows. 2. Admit condensate to the system through the lowest points and keep the vent at highest point opened. 3. Stop the water injection when condensate is coming out from highest point. 4. Check all the flanges and valves for leaks and attend them. When no more leaks are detected the test can be considered completed and the system emptied. Trouble Shooting of LP Decomposer Variables Change Effect Corrective action Bottom temperature decrease Overload of the down- stream section Check the M.P. decomposer holder 10-L-02 temperature. Check the L.P. decomposer 10-L- 03 holder level. Check the steam flow to L.P. decomposer. Check level in steam condensate separator 10-V-24 Increase Level of carbonate solution accumulator 10-V-06 increases due to excessive off-gas production in L.P. decomposer. Decrease the temperature by reducing the steam flow at L.P. decomposer. Pressure Decrease 10-P-03 A/B may begin to cavitated. Reduce water recovery from process condensate treatment by reducing, if possible, the steam flow rate to the column 27-C-02 or to the Hydrolyzer 27-R02; an option is to increase the reflux to 27-C-02. Last, reduce CW flow to L.P. condenser 10-E-08; this may cause Increase Overload of the down- stream section. Check the M.P. decomposer holder level controller and restore the normal condition Decrease Vapours can pass to the downstream section and there is the possibility to break the vacuum Close slightly L.P decomposer level control valve or open temporarily the M.P. decomposer holder level control valve. Check
  • 15. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Level conditions in vacuum concentration section. the correct functioning of L.P. decomposer holder level control valve and M.P. decomposer holder level control valve. Increase Flooding of L.P. decomposer and consequently urea carry over to accumulator 10- V-06. Increase the steam flow to LP Decomposer .Check the level and restore the normal situation without disturbing Table-5 Corrosion Reported in 2nd stage of Vacuum in Many Plants Number of plants reported corrosion in 2nd stage of vacuum and part ion plate crack in vacuum waste water tank (V-09).Some plants reported erosion problem in 2nd stage of inlet nozzle. But question arise why in 1st stage of vacuum? Following are the reason for above problems. Urea itself is considered as non-corrosive for stainless steel, while some of its decomposition products at high temperature may lead to corrosion. The urea decomposition process plays a role in the corrosion of stainless steel. All corresponding decomposition products, which exist in the solid, liquid and gaseous state and correlate with temperature and pH value at which they may lead to uniform corrosion. In start up the urea concentration is less means the ammonium Carbamate/carbonates are there and it is very highly corrosive to SS-304 L. The urea solution from LPD/Pre concentrator to be lined up to vacuum section when proper temperature and concentration achieve during start-up of the plant.
  • 16. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Fig-6 1. In startup/ shut down, No Vacuum in both vacuum separators, the quantity wise 1st vacuum inlet and 2nd vacuum inlet feed is about the same the first vacuum separator area is more very large vessel and 2nd vacuum separator is to small as compare to first and the liquid/vapour load per square meter is more so the corrosion is more in 2nd vacuum separator. 2. The 1st vacuum separator has large volume and two number vacuum control valves (PIC 140A/B) are there, one is for sudden vacuum breaker (Large capacity) other is less capacity for controlling of vacuum. These valves are air failure to open. The 1st stage vacuum design is 0.33 ata. But practical point of view this vacuum maintain about 0.4 ata for maintaining the temperature to avoid crystallization. Because of large volume the vacuum breaker valve (B) is always open and air introduces into the vessel this air act as a passivation for SS 304 L. 3. In case of 2nd separator the vacuum maintain about 0.03 ata , it is high vacuum booster ejector is required to pull of vacuum and control valve (PIC 141) is always closed. 4. Due to high vacuum the velocity of solution inlet of nozzle is high the erosion also observed. 5. The 2nd vacuums also have Skirt inside the deposition of polymer always there inside and outside. However some plants have removed the skirt. This skirt is the reason of corrosion. 6. The temperature in 2nd stage separator is more 135-1400 C.more temperature more corrosion see fig-6 7. The 1st stage having more water and about all the water removed by 1st stage.
  • 17. www.researchgate.net This is an open access article, Research Gate water is not corrosive . Corrosive is mixture of NH3/CO2 mixture. 8. The water balance as shown in the following figure-9 Fig-7 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers water is not corrosive . Corrosive is mixture. The water balance as shown in the 9. Corrosion is the function of fig-6 Research Gate is an academic social networking site is a European commercial social networking site for scientists and researchers Corrosion is the function of temperature
  • 18. www.researchgate.net This is an open access article, Research Gate Fig-8 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Research Gate is an academic social networking site is a European commercial social networking site for scientists and researchers
  • 19. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Fig-9 Waste Water Treatment Section The distillation tower is divided into two parts: the lower part consists of 38 trays and the upper part of 17 valve trays. The feed is placed on the 51st or 45th tray. The wastewater containing NH3, C02 and urea after a first stripping of the ammonia in the upper part of the lower is sent to the hydrolyser for the decomposition of urea. The treated water from the hydrolyser comes back to the lower where the top of lower part where the remaining ammonia is stripped out by means of 6.5 Ata saturated steam directly fed to C-2 bottom. The vapors leaving the top of the tower are condensed in 11-E-17 by cooling water and the carbonate solution produced is recovered in the reflux accumulator 11-V-5.The process condensate containing NH3-CO2 and urea coming out from vacuum system of both urea units, 10 & 20 is treated in this section to make free of contaminants before sent to utility unit. The contaminated water of each urea unit is collected in the process condensate tank 10-T- 02. From this tank the process condensate is pumped, by means of 10-P-14 A/B, to a common buffer off spec tank, 27-T-05, then the mixed solution is sent to the upper part of distillation tower 27-C-02. The Tank 10-T-02 also receives the drain solutions accumulated into underground carbonate close drain tank 10- T-04, and fed to process condensate tank by means of pump 10-P-16 A/B. Before entering the distillation column, the process condensate picks up heat from the purified condensate leaving the bottom of the column itself, by means of pre heater 27-E-16. The column 27-C- 02 is provided with trays and is divided in two main sections by a chimney tray. Column process conditions are: - Pressure (top): 2.5 kg/cm2 (g) - Temperature (top): 118 °C The condensate from the chimney tray is drawn and pumped, by centrifugal pump 27-P-15 A/B/C, to urea hydrolyzer 27-R-02, where process
  • 20. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers conditions are suitable to decompose urea into CO2 and NH3.The necessary decomposition heat is provided by adding steam at 44 kg/cm2 (g) and 380 °C. Hydrolyzer process conditions are: - Pressure: 34 kg/cm2 (g) - Temperature: 235 °C The out coming vapours from the hydrolyzer as well as the vapours from the top of the distillation tower are mixed and condensed in the overhead condenser, 27-E-17, then collected in the reflux accumulator, 27-V- 17 and split to LP section of urea unit 10 & 20 by reflux pumps, 27-P-17A/B. The recycle stream is mixed upstream of 10-E-08 with the LP Decomposer overhead vapors. The hydrolyzed condensate leaving the bottom of the 27-R-02, after having decreased its temperature passing through hydrolyser preheated, 27-E-18, enters the distillation tower immediately under the chimney tray where the final NH3 and CO2 stripping takes place. Saturated steam at 5.3 kg/cm2 (g), injected directly at the column bottom, and provides the necessary stripping force. The purified process condensate leaves the column bottom at 143°C and it is cooled at 45°C by means of : - Distillation tower feed preheating by means of 27-E-16 - Process condensate cooler 27-E-23
  • 21. www.researchgate.net This is an open access article, Research Gate Fig-10 Impotence of Reflux and Steam to Distillation Tower 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Impotence of Reflux and Steam to The reflux to distillation column decide concentration of reflux accumulator section .How much steam is required? Increasing Research Gate is an academic social networking site is a European commercial social networking site for scientists and researchers The reflux to distillation column decide concentration of reflux accumulator section .How much steam is required? Increasing
  • 22. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers /decreasing of steam can cause the distillation column disturbed. Inside the column, the down flowing reflux liquid provides cooling and condensation of the up flowing vapors thereby increasing the efficiency of the distillation column. The purpose of reflux is to provide down- flowing liquid throughout the rectification section to contact with the up-flowing vapor in order to achieve stage-by-stage equilibrium heat and mass transfer and, hence, purification of the top product. The utility cost includes Steam to distillation in bottom and cooling water cost in overhead condenser. As reflux ratio increases more of the steam heat is consumed to vaporize the incoming liquid which results in energy loss. Also more of the steam for heating purpose will be wasted. Because of the higher steam duty as the more volatile component reaches the condenser with higher rate thus more of the cooling water will be required which again results in a loss of energy. If you give more steam in bottom then concentration of reflux accumulator will be decrease because at certain point that steam will condense in accumulator. A practical curve for 4000 TPD Plant as figure No-11 Fig-11
  • 23. www.researchgate.net 16th July. 2022 Research Gate is an academic social networking site This is an open access article, Research Gate is a European commercial social networking site for scientists and researchers Conclusion It has been observed the water balance of the plant is main key factor. It must be balance and optimized otherwise conversion of urea will be disturbed. The safe plants operation is the technical art. A small mistake can make big incident. The operations of this activity implies a unit shut-down duration of not more than 48 hours (24 hours during 1st start-up of the unit), leaving the H.P. loop bottled before corrosion problems can take place. If maintenance jobs have to be performed on the unit (excluding the synthesis loop) it is possible to separately depressurize and drain the required equipment, leaving the reactor full and ready to restart. It is suggested, before starting any maintenance job, isolate NH3 and carbonate solution vessels from the remaining unit, controlling the pressure by the respective PIC in automatic mode. It is not advisable to carry out series of inlet contacts to interlock system, exception Consist of push button and selector switches on the control board and particular cases which must be considered one by one. The push buttons for shut down shall be protected from accidental operation. The analysis points and the frequency with which they have to be carried out, during start-up and under normal running conditions. Number of the instruments in the plant are equipped with passive alarms to warn the operators in the control room against deviating operating conditions which may lead to dangerous situations or which may cause damage to the equipment. A leakage detection system should be developed due to impurities in steam-damaged steels. The barrier of having an effective start-up procedure was totally ineffective as this not apply to the specific conditions applicable on the day. The water balance must be checked day by day. View publication stats View publication stats