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N-10012-4-OPM-1601-1 Operation and Maintenace Manual Dehydration Section PDF
N-10012-4-OPM-1601-1 Operation and Maintenace Manual Dehydration Section PDF
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DISCLAIMER:
The purpose of the operation and maintenance manual (O & M manual) is to establish general
guidelines for the safe and proper use and maintenance of the Process Plant (as defined in the Supply
Agreement executed between the recipient and Praj Industries Limited) supplied by Praj Industries
Limited (PIL). These instructions are submitted with the implicit understanding that:
a) They are a guide to the recipient for the operation and maintenance of the Process Plant for
efficient operation.
b) The recipient has assigned skilled & competent maintenance and operating personnel for the
functioning of the Process Plant described herein.
c) The recipient has read, understood and thoroughly examined the aforesaid instructions prior to
abiding with the requirements.
The information contained in the O & M manual is confidential, and is meant solely for the use of the
recipient only and is not for circulation. This document is not to be reported or copied or made
available to others. The information contained herein is based on:
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TABLE OF CONTENT
1.0 INTRODUCTION 06
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3.0.6 Troubleshooting 75
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PART–I
THEORETICAL ASPECTS
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1.0 INTRODUCTION
This document being part of OPERATIONAL AND MAINTENANCE
MANUAL contains confidential and proprietary information belonging
exclusively to PRAJ INDUSTRIES LIMITED of Pune, India. VICENTIN
S.A.I.C. Argentina shall maintain confidentiality and take all necessary care to
ensure that the information shared in this document is used only by the
authorized and assigned representatives.
Under article (Secrecy and confidentiality), all data and information submitted
herein regarding design details, system operation, processing techniques should
not be divulged to others without the written consent from PRAJ INDUSTRIES
LIMITED, INDIA. Here after PRAJ INDUSTRIES LIMITED, INDIA shall be
called as PRAJ.
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1.0.1
.1 THEORY OF DEHYDRATION
The components of liquid / vapor mixture can be separated by distillation, but the
ethanol-water
water system forms a binary Azeotropic with 994-95% v/v alcohol water liquid
composition and a boiling point of 78.15 °C at 1.033 kg/cm2 (a) pressure. In order to
separate the components
nts of such cases following techniques can be used -
Azeotropic Distillation
Molecular Sieve Dehydration*
VICENTIN S.A.I.C. Argentina
* Technique used for “VICENTIN Argentina”.
Zeolite
Azeotropic Distillation:
The Azeotropic distillation of ethanol with an entrainer like benzene, cyclohexane, or
isopropyl ether may be used to break the azeotrope of ethanol and water. Since the ternary
azeotrope is richer in water than the binary ethyl alcohol water azeotrope,
azeotrop water is carried
over the top of the column. The azeotrope, when condensed, forms two phases. The
organic layer is refluxed to the column, while the aqueous phase is discharged to another
column for recovery of the entraining agent.
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CONSENT FROM
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to regeneration mode and the bed on regeneration mode will be switch over to
dehydration mode, with the help of automation system.
N-10012-1-PID1601 – P&I DIAGRAM FOR MSDH-I
Vaporizer Flash Tank (T-1603)
The 94-95% v/v Alcohol water liquid (hydrous alcohol) from Distillation section
and off-spec Alcohol water liquid (hydrous alcohol) from storage section are fed to
feed Preheater (H-1605) through Feed Filter (F-1601) to Vaporizer Flash Tank (T-
1603), which is provided with the Vaporizer Reboiler (H-1601). In Vaporizer Flash
Tank (T-1603) the alcohol is vaporised by supplying Low Pressure Steam to
Vaporizer Reboiler (H-1601). Flow of 94-95% v/v Alcohol water liquid (hydrous
alcohol) feed to Vaporizer is controlled by level control valve (LCV-160101) of
Vaporizer Flash Tank.
The Low Pressure steam condensate from Vaporizer Reboiler (H-1601) & Medium
Pressure steam Condensate from Superheater (H-1602) are collected in Steam
Condensate Tank (T-1604) and then return to Boiler through steam condensate
Transfer Pump (P-1604A/B).
N-10012-1-PID1602 – P&I DIAGRAM FOR MSDH-II
N-10012-1-PID1603 – P&I DIAGRAM FOR MSDH-III
Vaporizer Flash Tank (T-1603) alcohol water vapor flow to the Molecular sieve (V-
1601 A/B) through Superheater (H-1602).
Molecular Sieve I/II (V-1601A/B) removes excess water by the process of
“adsorption”. The Fuel Ethanol Plant performs the adsorption in vessels filled with
molecular sieve desiccant in combination with strictly controlled pressure and
temperature cycles. Each desiccant bed contains millions of tiny, uniform diameter
pores, which are established during the manufacture of the desiccant. A different
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purification application requires different size pores in the desiccant beds. In this
case, where water is adsorbed from ethanol, a desiccant with a pore size is selected
that selectively retains water. Because water molecules are smaller than ethanol
molecules, the water molecules are selectively adsorbed into the pores as the
mixture of ethanol / water vapor pass through the sieve beds. The ethanol
molecules are too large to fit into the selectively sized pores, so the purified ethanol
passes out the end of the sieve bed, stripped of the water it originally contained.
If this process continued indefinitely, the desiccant would eventually become
saturated with water molecules and would be unable to adsorb any more water.
Therefore, at regular intervals the sieve bed must be “regenerated”. This simply
means the adsorbed water must be removed from the desiccant so that the
desiccant can be reused. In the ECOMOL continuous, two Sieve Bed system one
bed dehydrates the ethanol stream during one half of the cycle while the other bed
is under regeneration. During the other half cycle, valves redirect the flow of
alcohol vapor so that the mode of operation (dehydration and regeneration) of
Sieve Bed is changed. The total time for one cycle is approximately 11 - 12 minutes,
depending upon the transition cycle time settings.
Cooling water is used as cooling media for Regeneration Condenser (H-1603),
Product Condenser (H-1608), PCV Condenser (H-1609), Product Cooler (H-1606)
and Regeneration Cooler (H-1607).
Molecular Sieve Dehydration System
The Dehydration System operates in series with the Vaporizer Flash Tank (T-1603),
to optimize ethanol recovery efficiency and reduce energy consumption. It is
designed to dry the ethanol vapor through adsorption of the water by synthetic
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This information permits the operator to monitor system operation and observe the
pressure drop across the beds.
CAUTION: If the vapor valves are improperly adjusted, a large uplifting pressure
drop (greater than 1.5 psi) can develop. A pressure drop of this magnitude can cause
the velocity of the vapor passing through the bed to be high enough to make the
sieve material become airborne or "fluidized". Once fluidized, the turbulence in the
bed will eventually cause a portion of the sieve desiccant material to abrade itself
into dust. The extent of the damage to the desiccant material will depend upon the
severity and frequency of the sieve bed “fluidizations.”
Temperatures are monitored at four (4) levels in each sieve bed vessel:
1) Near the top of the Sieve bed
2) Near the upper middle of the Sieve bed
3) Near the lower middle of the Sieve bed
4) Near the bottom of the Sieve bed
Local temperature gauges, provided to check sensor readings, are mounted close to
the temperature transmitters and at the same level in the bed.
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Water adsorption from the vapor stream occurs under an approximate pressure of
1.7 ~ 1.8 kg/cm2 (a) and temperature of 120-125 °C. The molecular sieve desiccant
material regeneration occurs at a pressure of 0.105 kg/cm2 (a) or less and a
temperature a few degrees cooler than the adsorption cycle in that sieve bed. The
molecular sieve desiccant heats up during adsorption and cools down during
regeneration. The duration of the adsorption and regeneration cycles is set short
enough to avoid significant fluctuations in the bed temperatures. The short cycle
means that only a small proportion of the molecular sieve's adsorption capacity is
used in the cycle before regeneration restores it. The short, closely controlled cycles
produce steady operating conditions, which result in a high and consistent purity
of the Fuel Ethanol produced.
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Dehydration Cycle
Wet or hydrous ethanol vapor is received from the Vaporizer Flash Tank (T-1603)
through valves (PCV-160201) or (PCV-160202). The Vaporizer Flash Tank pressure
is controlled by (PIC-160201). Alcohol water vapor from the Vaporizer Flash Tank
(T-1603) are heated in Superheater (H-1602) and fed to either of the Molecular
Sieve I/II (V-1601A or V-1602B) based on Sieve Sequence (UC 160201).
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Regeneration Cycle
In the ECOMOL “combined cycle” technique, a hard vacuum is first applied to
force water molecules to leave the sieve desiccant. A pulse of purge vapor is then
passed through the bed to sweep the water molecules up and out of the bed and
into the Regeneration Condenser (H-1603). This is accomplished by modulating the
Purge Control Valve (either FCV-160205 or FCV-160206, depending on which bed
is regenerating) between a "partially open” and “mostly closed" position at a
controlled frequency so that Fuel Ethanol vapor passes into the regenerating vessel
in a cyclic fashion. The oscillation frequency rate of the purge control valve cycle
and its percent open / closed settings are all adjustable from the computer
keyboard.
The vapor leaving the top of the regenerating sieve bed vessel is passes into the
Regeneration Condenser (H-1603), where it is condensed. The Regeneration
Condenser is a vertical shell and tube heat exchanger with tube side cooling water
condensing shell side regeneration vapor. Before returning to the Rectifier Column
(C-1461) for recovery of alcohol, the regeneration liquid is filtered by Regeneration
Filter (F-1602, 25-Micron Absolute) to remove any small particles of suspended
solids that are entrained as the purge stream passes through the molecular sieve
beds. A sample valve is provided to test the regeneration liquid alcohol
concentration (%).
System vacuum (0.106kg/cm2 (a) or less by the middle of the regeneration cycle) is
created by pumping cooled (less than 33°C) regeneration liquid at high pressure
through the Vacuum Eductor (J-1601). The Regeneration Pump (P-1602A/B) creates
the motive force, while the Regeneration Cooler (H-1607) maintains the required
liquid temperature.
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A flow indicator (FQI-160302) provides for visual verification of the motive fluid
flow to the Vacuum Eductor (J-1601). Sub cooling the regeneration fluid in the
Regeneration Condenser (H-1603) also helps create the regenerating sieve bed
vacuum. Non-condensable and regeneration liquid are discharged from the
Vacuum Eductor (J-1601) into the Regeneration Receiver (T-1602). The non-
condensable are vented to the atmosphere and the excess regeneration liquid is fed
to the Rectifier Column for further concentration. Flow of regeneration liquid going
to the Rectifier Column (C-1461) is controlled by Flow Totalizer Indicator &
Controller (FQIC-160207) using Flow control valve (FCV-160207).
Transition Cycle
The transition of the beds from pressure to vacuum and vice-versa is carefully
controlled through the computer to complete the transition while avoiding
bouncing or mechanical friction of the molecular sieve beads. If an adsorbing bed
under pressure were subjected to pressure decrease in the upward direction,
pressure release would fluidize (bounce) the sieve beads and the resulting
turbulence would damage them. Consequently, the switchover is carefully
sequenced by the control system to avoid extreme flow conditions in the beds by
always depressurizing beds at a slow, controlled rate.
The switching of the sieve bed vessels between adsorption and regeneration is done
through a network of valves and interconnecting piping at the vessels’ top and
bottom. The valves and their positions are listed below:
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Note: The following valves are used for more than one function as described below:
Valves PCV-160201 & PCV-160202 are used for
1) Feed flow (during dehydration cycle)
2) Pressure equalization (during transition cycles)
3) Pressure control on the Vaporizer Flash Tank.
Valves FCV-160203 & FCV-160202 are used for
1) Purge control (during regeneration cycle)
2) Pressure equalization (during transition cycles)
Summary of Valve Positions during Cycles
The pressure switching sequence duration is short (approx. 70 seconds) compared to
the adsorption / regeneration cycle (typically 300 seconds). The cycle times can be
adjusted at the computer for process optimization. A complete sieve bed vessel
cycle, from adsorption to regeneration and back to adsorption, will have valves
positioned as follows:
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TRANSITION 2: EQUALIZATION
(10 - 20 Seconds)
V-1601 A/ EQUAL V-1601 B/ EQUAL
VALVE POSITION VALVE POSITION
PCV-160201 OPEN PCV-160202 OPEN
FCV-160203 CLOSED FCV-160204 CLOSED
Equalization purge
FCV-160206 OPEN FCV-160205
position
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TRANSITION 2: EQUALIZATION
(10 - 20 Seconds)
* Valve is ramped to go from fully closed to fully open in approximately forty (40)
seconds.
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QUANTITY
TAG NO DESCRIPTION TECHNICAL DETAILS
OP. S/B
Type: Cylindrical/Vertical
T-1604 Steam Condensate Tank 1 0 Shell with Dished end
Capacity: 0.5 m3
Type: Cylindrical/Vertical
V-1601A/B Molecular Sieve Bed I/II 2 0 Shell with Dished End
Capacity: 10 m3
Product Pump with Type: Centrifugal
P-1601A/B 1 1
Explosion Proof motor Capacity: 7 m3/hr
Regeneration Pump with Type: Centrifugal
P-1602A/B 1 1
Explosion Proof motor Capacity: 50 m3/hr
Steam Condensate Pump
Type: Centrifugal
P-1604A/B with Explosion Proof 1 1
Capacity: 4 m3/hr
motor
Y-1601 Flame Arrestor for T-1602 1 0 -
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PART–II
PRE-START-UP ACTIVITIES
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1. The procedures and operating conditions listed here are guidelines only and
may be modified on start-up. The control system must be flexible enough to
accommodate these changes.
2. These instructions do not cover peripheral equipment, which may affect the
plant operation.
3. It is expected that the operator may be required to take some decisions and
actions not covered by this manual. The operator will be expected to monitor
the system during operation, and may need to intervene to assure safe
operation of the plant as and when required. The control system must be
flexible enough to allow operator intervention when necessary.
5. Operating personnel should follow the safety regulations as per factory rules
as well as factory acts and regulations.
Inspection is nothing but P&ID & Layout audit. It is necessary to conduct P&ID &
Layout audit to ensure that plant erection is done as per the recommended design.
Audit report should be made and if in case any work is pending it should be
brought to notice of project engineer and should be completed considering pre-
start-up and start-up schedule.
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Once physical inspection of all equipment is completed, open bottom most nozzles
for flushing purpose. Make temporary arrangements for putting water from top of
all equipment for flushing. Remember that these temporary arrangements made
should be removed after water flushing. Flush all the equipment till you get clear
water from bottom nozzles of the respective equipment.
B. Flushing of Piping
During erection there are chances that metal pieces, welding rod pieces, cotton balls
etc. may trap inside pipelines. It is necessary to flush piping to avoid problems like
chocking, damaging of instruments and pumps during pre-start-up and start-up.
Liquid lines can be flushed with water. Steam lines flushed with steam and airlines
can be flushed with air. Please remember that one end of the line should be open to
atmosphere and other end should be connected to flushing media. During flushing
please follow safety aspects also.
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F. Interlock testing
All interlocks should be tested before putting system on line. For interlock test
methods “Control Logic and Interlock Description (N-10012-4-ILD1601)”. Process
person should witness this test and joint report should be made.
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1. Power supply
2. Instrument air supply
3. Steam supply
4. Cooling water supply
5. Process water supply
6. Sealing fluid supply
7. Effluent treatment plant
8. Feed Stock handling section
Its Inspection report should be made and if any lacuna is there it should be brought
to the notice of project engineer to furnish it.
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Note – During initial start-up of cooling water circuit it is necessary to flush the
cooling water headers in order to avoid the unwanted material sent feed back
to the cooling tower. A temporary arrangement is required to do the same.
5. The cooling water flow to Product Cooler (H-1606) is Indicated by (FI-160303),
installed at cooling water supply line.
6. Open isolation valve on cooling water on Cooling Water Header Line.
7. Open cooling water valve slowly to product Cooler (H-1606) supply cooling
water. Ensure complete venting of air through vent valve.
8. After completed venting open cooling water Manual valve gradually up to
rated capacity by checking flow through FI-160303.
9. Ensure establishment of cooling water circuit for Dehydration Section. Ensure
the performance of temperature on cooling water lines.
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Water Flushing is nothing but cleaning of equipment and arresting the leakage. It is
very important to test the plant on water first to see its performance so as not to
face any problem during actual plant operation. During water trial itself it is
important to tune-up all the instruments and observe the performance of rotating
equipment too. Before starting actual water trial ensure there is sufficient Process
water stock available. Following are the equipment to be tested on water along
with allied rotating accessories:
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(T-1603) level control valve (LCV-160101) 25 % in MAN mode. Water will start
flowing to Vaporizer Flash Tank (T-1603) through feed Preheater (H-1605).
Ensure the flow through (FQI-160101). Open tube side drain point of Vaporizer
Reboiler (H-1601). Close the drain when clear water is observed. Vaporizer
Flash Tank (T-1603) level will start increasing. Calibrate (LIC-160101). When
Vaporizer Flash Tank (T-1601) level reaches 45% close level control valve of
Vaporizer Flash Tank (LCV-160101) and stop the Aldehyde bottom Pump (P-
1403A/B). Open Vaporizer Reboiler (H-1601) drain valve and drain the tank
completely. Close the drain valve.
4. Make temporary process water connection for flushing of Product Receiver (T-
1601) Regeneration Receiver (T-1602) and Steam Condensate Tank (T-1604).
5. Start process water to Regeneration Receiver (T-1602). Open Regeneration
pump (P-1602A/B) suction valve and open pump (P-1602A/B) suction drain
valve till clear water is observed. Level in Regeneration Receiver (T-1602) will
start to increase. Calibrate (LIC-160301). When Regeneration Receiver (T-1602)
level reaches 50%, start pump (P-1602A/B). Open manual inlet and outlet
valves of Regeneration Cooler (H-1607). Gradually open Regeneration pump (P-
1602A/B) discharge manual valve.
6. Water will start re-circulating to Regeneration Receiver (T-1602) through
Vacuum Eductor (J-1601). Open isolation valve on Regeneration Filter (F-1602).
Flow of regeneration liquid going to the Rectifier Column is controlled by Flow
Totalizer Indicator & Controller (FQIC-160207) using Flow control valve (FCV-
160207), in MAN mode 25% Water will start flowing to Rectifier Column (C-
1461). Ensure the flow through (FQIC-160207). Ensure the performance of
Regeneration Pump (P-1602A/B). After ensuring line flushing, close
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12. Remove temporary Process water connection to Product Receiver (T-1601) and
steam Condensate Tank (T-1604). Drain Product Receiver (T-1601) and Product
Cooler (H-1606) completely through drain valves. Close drain valves after
ensuring the complete draining.
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13. Ensure the healthiness of tight shutoff condition for PCV-160202, FCV-160205
and FCV-160203. Tight shutoff condition for PCV-160202 can be ensured from
PIT-160201, tight shutoff condition for FCV-160203 can be ensured from PIT-
160204 and PIT-160205.
14. After achieving maximum possible vacuum, check Molecular Sieve II (V-1601B)
system for air leakages. Close FCV-160204. Close Regeneration Pump (P-
1602A/B) discharge valve and stop the pump.
15. Check the rate of drop in vacuum and it should not be more than 5-10 mm of
mercury per hour. This will confirm the vacuum test for Molecular Sieve II (V-
1601B).
16. Make formal report for Dehydration section vacuum trial.
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11. Open top piping of the Molecular Sieve I/II (V-1601A/B) once vacuum test is
cleared.
12. Start loading of molecular sieves from top nozzle of the Molecular Sieve I/II (V-
1601A/B) by using crane.
Note: - While loading molecular sieves from top of the Molecular Sieve there
is no need of using buckets it can be inserted directly in the bed by guiding
the topside of the drum into top nozzle of the bed. Precaution is to be taken to
avoid ingress of any foreign material in the bed.
13. After loading of every 10-12 No. of molecular sieve drums, light pocking needs
to be done by using 1’’ steel pipe inside the Molecular Sieve to have better
compact-ability of molecular sieves and even distribution.
14. This way total molecular sieve is to be loaded in each bed. Physically level of the
molecular sieve will be just 1’’ above the top screen of the Molecular Sieve I (V-
1601A).
15. Start loading 1’’ ballast above the molecular sieves.
16. Fix the top 14’’ insert properly once loading is completed. Top insert of 14’’ to be
inserted at N1 nozzle body flange of the Molecular Sieve I (V-1601A) and
Repeat the same procedure for the Molecular Sieve II (V-1601B).
17. Once both the Molecular Sieve I/II (V-1601A/B).are ready after molecular sieve
loading take vacuum test of both the beds once again.
18. Successful vacuum test of both the Molecular Sieves will conclude the molecular
sieve loading activity.
NOTE: -MOLECULAR SIEVE LOADING PROCEDURE SHOULD BE CARRIED
OUT IN PRESENCE OF PRAJ ENGINEER ONLY.
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14” INSERT
1” BALLAST
MOLECULAR SIEVES
1'' ABOVE TOP
SCREEN
TOP SCREEN
MOLECULAR SIEVES
1/4” BALLAST
1/2” BALLAST
3” MULTIPLE
INSERTS
BOTTOM DISTRIBUTION
PLATE
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PART–III
PROCESS START-UP
AND
PROCESS PARAMETERS
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3. Good housekeeping is required and keeps the area clean and free of debris.
4. Be cautious from rotary / moving equipment.
5. No Smoking Zone.
6. Use safety goggle, gloves and follow safe practices.
7. For High temperature steam, juice and alcohol, use PPE.
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10. Keep Molecular Sieve I/II (V-1601A/B) purge position “0%” (Zero).
11. The Vaporizer Flash Tank (T-1603) Pressure Controller (PIC-160201) should be
set to the normal operating pressure, approximately 1.68 kg/cm2 (a).
12. The Sieve Pressure Controller (PIC-160204) should be set to the normal
operating pressure, approximately 1.0- 1.58 kg/cm2 (a).
13. Open temperature control valve (TCV-160209) to Super heater (H-1602), 10 %
open in MAN mode and start increasing gradually.
14. Take FST-160201 online and ensure its performance.
15. Line out Steam condensate by opening the Manual valve to Steam Condensate
(T-1604).
16. Open the Vaporizer Reboiler (H-1601) Steam Flow Control Valve (FCV-160103)
10% in MAN mode. Once stable flow is established, match the set point with the
process variable and put the steam Flow Controller FIQC-160103 in AUTO
mode, then raise the set point gradually as per process requirement.
17. Gradually increase steam Flow Control Valve (FCV-160103) to the Vaporizer
Reboiler (H-1601), level in Vaporizer Flash Tank (T-1603) will start dropping
and level control valve (LCV -160101) will open automatically to control the
level of Vaporizer Flash Tank (T-1603).
18. Gradually open Temperature Control Valve TCV-160209 in MAN mode to
100% for increase the output of the Superheater (H-1602) and continue to
periodically monitor the temperature on TIC-160209 until the temperature
reaches 123°C. Once this occurs, set the Superheater temperature controller TIC-
160209 in AUTO mode with 123°C set point.
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19. Gradually increase the Low Pressure Steam flow set point to Vaporizer Reboiler
(H-1601) till the water feed flow to Vaporizer Flash Tank (T-1603) FQI-160101
reaches approximately 10-20% of normal operating flow.
20. Increase the steam to Vaporizer Reboiler (H-1601) in such a way that the set
regeneration time is sufficient to remove the heat generated during adsorption
cycle.
21. Line out the steam condensate from steam condensate tank (T-1604) to Boiler
through Steam condensate transfer pump.
22. Level in Steam Condensate Tank (T-1604) will start increasing. When Steam
Condensate Tank (T-1604), LIC-160102 reaches 50% start Steam Condensate
Pump (P-1604A/B) and take Steam Condensate Tank (T-1604), LIC-160102 in
AUTO mode with 50% set point.
23. Line out regeneration liquid to Rectifier Column (C-1461) with Regeneration
Preheater (H-1604) and Regeneration Filter (F-1602) on line. Take FQIC-160207
in AUTO mode with the required set point based on level rise in Regeneration
Receiver (T-1602). Maintain Regeneration Receiver (T-1602) level 50%.
24. Water level if any in Product Receiver (T-1601) can be drained from Product
Pump (P-1601A/B) suction drain point.
25. Gradually temperature of bed starts increasing in adsorption mode where as
during regeneration mode it will decrease. Ensure the bed temperature on local
temperature gauges also.
26. Allow all sieve bed temperature to stabilize at 200 oC.
27. After ensuring stabilization of bed temperature at 200 oC, start reducing Low
Pressure Steam to Vaporizer Reboiler (H-1601) gradually. Take FIQC-160103 in
MAN mode and close the valve Steam Flow Control Valve (FCV-160103).
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28. Take Superheater TIC-160209 in Man mode and close the Temperature Control
Valve TCV-160209.
29. Stop sieve sequence (UC-160201). All high performance control valves will go to
shut-off position.
30. Close Vaporizer Flash Tank (T-1603) level control valve (LCV-160103).
31. Open manual drain valve at Vaporizer Flash Tank (T-1603) bottom and empty
out Vaporizer Flash Tank (T-1603) completely.
32. Steam conditioning will take approximately 8 – 12 hrs.
33. Gradually Open FCV-160203 and FCV-160204 to 100% in MAN mode. Keep
both the molecular sieve beds under vacuum for 24-36 hrs. During this cooling
period temperature of molecular sieve beds will drop below 100-120 oC.
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Preheater (H-1605) and Feed Filter (F-1601) on line and take 20% level in
Vaporizer Flash Tank (T-1603). Take level control valve (LCV-160103) in AUTO
mode with 20% set point.
10. Gradually open temperature control valve (TCV-160209) 10% open in MAN
mode to Superheater (H-1602), and Superheater outlet temperature TIC-160209
start increasing. Take Superheater temperature controller TIC-160209 in AUTO
mode with 123°C set point.
11. Gradually open Steam Flow Control Valve (FCV-160103) 10% in MAN mode the
Vaporizer Reboiler (H-1601). Once stable flow is established, take Low Pressure
steam Controller FIQC-160103 in AUTO mode, and then gradually increase the
set point as per requirement.
12. The Vaporizer Flash Tank (T-1603) Pressure Controller (PIC-160201) should be
set to the normal operating pressure, approximately 1.8-1.9 kg/cm2 (a).
13. The Sieve Pressure Controller (PIC-160204) should be set to the normal
operating pressure, approximately 1.7 - 1.8 kg /cm2 (a).
14. Initiate the sieve sequence (UC-160201) and ensure the Vaporizer Pressure
Controller (PIC-160201) is placed in AUTO mode and the Sieve Pressure
Controller (PIC-160204) is placed in AUTO mode.
15. Line out the steam condensate from Steam Condensate Tank (T-1604) to Boiler
through Steam Condensate Transfer Pump (P-1604A/B).
16. Level in Steam Condensate Tank (T-1604) will start increasing. When Steam
Condensate Tank (T-1604), LIC-160102 reaches 50% start Steam Condensate
Pump (P-1604A/B) and take Steam Condensate Tank (T-1604), LIC-160102 in
AUTO mode with 50% set point.
17. Take FST-160201 online and ensure its performance.
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Dehydration plant has been shutdown for an extended period of time and the sieve
beds have cooled down below 80°C, the manual heating procedure as described
below needs to be followed.
Note: Never use the normal start sequence in cold start-up situation, as a high
regeneration pressure drop will occur due to wet beds and cause possible
molecular sieve damage.
1. Verify that all cooling water valves are open and cooling water flow is
established.
2. Ensure the Distillation section is running.
3. Ensure continuous availability of alcohol water liquid to Vaporizer Flash Tank
(T-1603) from Aldehyde Recovery Column (C-1402) or off –spec storage tank.
4. Ensure all interlocks are offline/bypassed.
5. Ensure Aldehyde Recovery Column Reboiler (H-1404) is ready to accept vapor
from Dehydration plant.
6. Place all control loops in MAN mode with 0% output to ensure that all control
valves are in the closed position prior to start-up.
7. The Regeneration Pump (P-1602A/B) should be started if the Regeneration
Receiver (T-1602) level is greater than 50%. Once the pump starts, gradually
open the discharge valve.
8. Lineout alcohol water liquid with 95-96% v/v alcohol concentration from
Aldehyde Recovery Column (C-1402) or off- spec storage tank to Vaporizer
Flash Tank (T-1603) by opening LCV-160103, 5% in MAN mode. Ensure Feed
Preheater (H-1605) and Feed Filter (F-1601) on line and take 20% level in
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Vaporizer Flash Tank (T-1603). Take level control valve (LCV-160103) in AUTO
mode with 20% set point.
9. Gradually open temperature control valve (TCV-160209) 10% open in MAN
mode to Superheater (H-1602), and Superheater outlet temperature TIC-160209
start increasing. Take Superheater temperature controller TIC-160209 in AUTO
mode with 123°C set point.
10. Take FST-160201 online and ensure its performance.
11. Gradually open Steam Flow Control Valve (FCV-160103) 10% in MAN mode the
Vaporizer Reboiler (H-1601). Once stable flow is established, than take Low
Pressure steam Controller FIQC-160103 in AUTO mode and gradually increases
the set point to maintain the alcohol water feed flow to Vaporizer Flash Tank (T-
1603) reaches approximately 60-70% of normal operating flow.
12. Give openings to the control valves as shown in TABLE A
V-1601A V-1601B
PCV-160208 15-25 %*
* To be adjusted manually in order to control respective controller.
** To be open gradually to 100% with 10% increment after every 10 seconds.
13. The Vaporizer Flash Tank (T-1603) Pressure Controller (PIC-160201) to be
controlled at 1.8-1.9 kg/cm2 (a) by manually adjusting the PCV-160201.
14. The Sieve Pressure Controller (PIC-160204) to be controlled at 1.5-1.8 kg/cm2
(a) by manually adjusting the PCV-160208.
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V-1601A V-1601B
PCV-160208 15-25 %*
* To be adjusted manually in order to control respective controller.
** To be open gradually to 100% with 15% increment after every 10 seconds.
16. The sieve bed temperatures of V-1601B should be continuously monitored. V-
1601B top temperature TI-160206 will start increasing. When temperature at TI-
160206 reaches 120-125oC, switch over the adsorption manually to V-1601A by
giving opening to control valves as shown in TABLE A.
17. In order to prevent an overheat condition, the dehydration/regeneration cycles
should be shortened to 2.5 - 3.0 minutes during start-up with new sieve
material, until the sieve bed temperatures stabilize at about 120°C. The sieve
bed temperatures should be continuously monitored, and if they start to get
above 145°C, the cycle times should continue to be shortened until none of the
temperatures exceeds 145°C. The unit should be shutdown and allowed to cool
down for 6-8 hours if the Molecular sieve bed temperature exceeds 145°C.
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Bed Pressure
The operating pressure of the bed is controlled by the Pressure Controller PIC-
160204. The PID loop coefficients should be tuned to provide responsive control
of molecular sieve I/II (V-1601A/B) pressure.
Final Product proof
Product alcohol concentration is affected by many factors, including inadequate
vacuum, improper bed pressure control, improper purge adjustment, Lower
alcohol concentration in alcohol water liquid malfunctioning of high
performance valves, etc. If the system is mechanically sound and properly
adjusted, has sufficient vacuum in the regenerating bed and Product Alcohol
concentration is controlled by adjusting the purge parameters as follows.
Purge Max/ Min Set points
The purge valve does not fully open or close during the PURGE Max/Min
periods. Instead, it oscillates between two positions, Pmax and Pmin, which can
be set from the sieve parameters keyboard. During the Pmax period the valve
opens to around 14-19%, and during Pmin the valve is typically set to
approximately 6-9% open. The Pmin position slows the regeneration vapor
flow, allowing for a stronger vacuum to be developed across the regenerating
bed. The Pmin and Pmax positions should be set to pressure drop across the
Molecular Sieve I/II (V-1601A/B) should not exceeding a 0.098 kg/cm2 (a).
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Purge Adjustment
In general, the greater the purge rate, the higher the purity, or dryness of the
product. However, an excessive amount of purge can actually reduce product
dryness by overloading the vacuum system. This causes a loss of vacuum in the
regeneration bed which means that an inadequate amount of water will be
pulled out of the sieve bed during the regeneration cycle. This results in a loss of
drying capacity for that sieve bed when it is once again used for the
dehydration cycle. There may, however, arise some unusual conditions or
process upsets (i.e. drying out sieve beds which have gotten wet), where it may
be necessary to adjust Pmin and/or the Pmax position to a higher than normal
value to increase the ability to pull water from the sieve beds (Keep in mind that
the vacuum setting must be met during this exercise or the effect of an increased
purge will be counteracted by the loss of vacuum). When increasing the purge
valve MAX setting, closely watch the pressure drop across the regenerating bed.
If the valve is allowed to go too far open (greater than 0.098 kg/cm2 (a) pressure
drop across the sieve bed), the pressure drop can become sufficient to "fluidize"
the bed (bouncing the bed, which can physically damage the desiccant). If the
MAX position is set high enough where there is a 0.098 kg/cm2 (a) pressure
drop across the regenerating bed and still more purge is needed, the feed rate
should be reduced (which feeds less water to the beds) until the beds are dried
out enough that the feed rate can be increased without exceeding the 0.098
kg/cm2 (a) pressure drop across the regenerating bed.
If the product is dryer then needed, the max setting can be gradually reduced,
which gradually decreases the overall system energy until the desired product
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water content is obtained. It is best to adjust the purge to the lowest setting
possible where the final product still meets the desired specifications.
Frequency of Routine Analysis
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B) PRESSURE:
SR.NO. PARAMETER TAG NO. UNIT VALUE
1 Vaporiser pressure control PIC-160201 Kg/cm2 (a) 1.7
C) TEMPERATURE:
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D) LEVEL:
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NOTE –Above parameters are only guidelines. Actual operating parameters shall be fine-
tuned at site during normal operation of Commissioning.
3.0.6 TROUBLESHOOTING
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In this section some common cases were considered which guides the operating
personnel to arrive at the solution; troubles apart from the mentioned cases may
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PART–IV
PROCESS SHUTDOWN
AND
PROCESS START-UP
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CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
During instrument air failure condition of all on-off and control valve should go to
air failure position as mentioned with instruments on P&ID (FO: AIR FAIL TO
OPEN, FC: AIR FAIL TO CLOSE).
Operator and shift engineer has to ensure air fail position of control / solenoid
valves during instrument air failure. Due to instrument Air failure of control valve
Low Pressure Steam/ medium Pressure steam to all plant will get stopped and
concern section operator has to take actions accordingly.
During instrument air failure following actions to be taken by operator / DCS
sequence without time delay.
1. Put Vaporizer Flash Tank (T-1603) Level Control Loop, (LIC-160101) will be
forced to MAN mode with output 0%,
2. Put Low Pressure Steam control Loop (FQIC-160103) to Vaporizer Reboiler (H-
1601) in MAN mode and close it to zero.
3. Put Medium Pressure Steam control Loop (TIC-160209) on steam line to
Superheater (H-1602) in MAN mode and close it to zero.
4. Stop Molecular Sieve sequence (UC-160201) after 45 seconds. (PCV-160201,
PCV-160202, PCV-160208, FCV-160203, FCV-160204, FCV-160205 and FCV-
160206 will be forced to 0%).
5. Put Flow control Loop (FQIC-160207) on Alcohol water liquid from
Regeneration Receiver (T-1602) to Rectifier Column (C-1461) in MAN mode
close it to zero and Stop Regeneration Pump (P-1602A/B).
11. Put Level control Loop (LIC-160302) on Product receiver (T-1601) in MAN mode
close it to zero and Stop Product Pump (P-1601A/B).
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12. Put Level control Loop (LIC-160102) on Steam Condensate Tank (T-1604) in
MAN mode close it to zero and Stop Steam Condensate Pump (P-1604A/B).
Note: While shutdown of Dehydration plant, there will not be availability of
heat in the form of alcohol Vapor to Aldehyde Recovery Column Reboiler (H-
1404). During Low Pressure Steam / Medium Pressure Steam actions to be
taken by operator / DCS sequence without time delay.
THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
Apart from emergency shutdown like power failure, cooling water failure, steam
failure and instrument air failure as mentioned earlier, there are several number of
factors, which may lead to pre planned plant shutdown for short duration till the
affecting factor will get re-normalized.
It is assumed that power, cooling water, steam and instrument air and other
necessary utilities are available for safe short shutdown of the plant. It is also
assumed that the shutdown is not more than 12 hrs. If the shutdown is more than
12 hrs, follow normal plant shutdown procedure where it is necessary to empty out
the tanks.
Based on the leading factor for plant shutdown, operator has to take appropriate
and safe actions accordingly.
1. Put Vaporizer Flash Tank (T-1603) Level Control Loop, (LIC-160101) will be
forced to MAN mode with output 0%,
2. Put Low Pressure Steam control Loop (FQIC-160103) to Vaporizer Reboiler (H-
1601) in MAN mode and close it to zero.
3. Put Medium Pressure Steam control Loop (TIC-160209) on steam line to
Superheater (H-1602) in MAN mode and close it to zero.
4. Stop Molecular Sieve sequence (UC-160201) after 45 seconds. (PCV-160201,
PCV-160202, PCV-160208, FCV-160203, FCV-160204, FCV-160205 and FCV-
160206 will be forced to 0%).
5. Put Flow control Loop (FQIC-160207) on Alcohol water liquid from
Regeneration Receiver (T-1602) to Rectifier Column (C-1461) in MAN mode
close it to zero.
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6. Put Level control Loop (LIC-160302) on Product receiver (T-1601) in MAN mode
close it to zero and Stop Product Pump (P-1601A/B).
7. Put Level control Loop (LIC-160102) on Steam Condensate Tank (T-1604) in
MAN mode close it to zero and Stop Steam Condensate Pump (P-1604A/B).
8. Don’t stop Regeneration Pump (P-1602A/B) and keep it running depending on
shutdown.
9. Keep maintain the cooling water recirculation in Dehydration section.
10. Manually open valve (FCV-160203) & (FCV-160204) simultaneously (installed
between Molecular Sieve beds and Regeneration Condenser) gradually by 1%
up to 100%.
11. Maintain the Regeneration Receiver (T-1602) level (LIC-160301) by manually
opening of flow control Loop (FQIC-160207) on Alcohol water liquid to Rectifier
Column (C-1461).
Note: While shutdown of Dehydration plant, there will not be availability of
heat in the form of alcohol Vapor to Aldehyde Recovery Column Reboiler (H-
1404). During Low Pressure Steam / Medium Pressure Steam actions to be
taken by operator / DCS sequence without time delay.
THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
4.2 Plant Long Duration Shutdown and Start-up after Long Duration Shutdown
Long duration shutdown is generally planned shutdown for any reason there are
some planned maintenance jobs, which are to be carried out during shutdown; jobs
like hot jobs, vessel entries, and cold jobs etc.
SAFETY point of view it is important; not to have any alcohol traces in the plant
while carrying out any hot job or for vessel entries.
Therefore it is important to make plant alcohol free before taking the plant long
shutdown.
1. Put Vaporizer Flash Tank (T-1603) Level Control Loop, (LIC-160101) will be
forced to MAN mode with output 0%,
2. Put Low Pressure Steam control Loop (FQIC-160103) to Vaporizer Reboiler (H-
1601) in MAN mode and close it to zero.
3. Put Medium Pressure Steam control Loop (TIC-160209) on steam line to
Superheater (H-1602) in MAN mode and close it to zero.
4. Stop Molecular Sieve sequence (UC-160201) after 45 seconds. (PCV-160201,
PCV-160202, PCV-160208, FCV-160203, FCV-160204, FCV-160205 and FCV-
160206 will be forced to 0%).
5. Put Flow control Loop (FQIC-160207) on Alcohol water liquid from
Regeneration Receiver (T-1602) to Rectifier Column (C-1461) in MAN mode
close it to zero.
6. Put Level control Loop (LIC-160302) on Product receiver (T-1601) in MAN mode
close it to zero and Stop Product Pump (P-1601A/B).
THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
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THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
All safety norms to be follow before starting any hot / cold job after plant
shutdown.
Maintenance activities if any of mechanical activities to be carried out
during long shutdown.
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CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
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THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
CO NF I D EN T IA L CONSENT FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA