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OPERATION AND MAINTENANCE MANUAL

PROJECT REV. PAGE ISSUE


CLIENT SECTION DOCUMENT NO.
NO. NO. NO. DATE
VICENTIN
N-10012 DEHYDRATION N-10012-4-OPM 1601 0 1 OF 97 05.11.2012
S.A.I.C

OPERATION AND MAINTENANCE MANUAL


TITLE :
DEHYDRATION SECTION.

CLIENT : VICENTIN S.A.I.C.

140,000 OR 150,000 LITERS / DAY


PLANT :
ANHYDROUS ALCOHOL

LOCATION : AVELLANEDA, SANTA FE- ARGENTINA

PROJECT NO. : N-10012

DOCUMENT NO. : N-10012-4-OPM 1601

0 05.11.2012 NMP/HAK SBG/PKR VBJ FOR EXECUTION


REV.
PREPARED CHECKED APPROVED
DATE REMARKS
NO. BY BY BY

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

OPERATION AND MAINTENACE MANUAL DEHYDRATION SECTION


OPERATION AND MAINTENANCE MANUAL
PROJECT REV. PAGE ISSUE
CLIENT SECTION DOCUMENT NO.
NO. NO. NO. DATE
VICENTIN
N-10012 DEHYDRATION N-10012-4-OPM 1601 0 2 OF 97 05.11.2012
S.A.I.C

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:

a) the specifications and data provided by the recipient,


b) the input parameters provided by the recipient
The operating parameters and auxiliary / utility consumption mentioned in the O&M manual are to
be used as guidelines only and the same may change during Process Plant stabilisation as well as due
to change in input specification. PIL is not liable for any operational hazards or injuries caused to
anybody on account of the use of the processes mentioned in the O & M manual. During the
warranty period Praj Industries Limited shall not be liable for any claims, losses, and damages arising
out of the use of the Process Plants by the recipient on account of non-compliance with the terms of
this O & M manual.
The recipient shall comply with all applicable laws while using the Process Plants with respect to
which this operation and maintenance manual is provided.
Start-up assistance or field engineering service provided by PIL during the pre commissioning and
commissioning period or thereafter on the request of the recipient shall in no way relieve the
recipient of the responsibility for the proper maintenance and use of the Process Plant.
PIL reserves the right to alter, amend and / or modify the operation and maintenance manuals from
time to time.
In no event shall PIL be liable for any damages and /or liabilities on account of any indirect,
incidental, special, consequential or any other similar losses.
The information incorporated in the O & M manual is subject to copyright and must not be used,
disseminated, copied or disclosed to third parties without the written consent of PIL.
If you are not the intended recipient you should forthwith destroy all copies and inform PIL at
info@praj.net.
© Praj Industries Limited All Rights Reserved Registered Office: Praj Industries Limited, `Praj
House', Bavdhan, Pune- 411021 Maharashtra, 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

OPERATION AND MAINTENACE MANUAL DEHYDRATION SECTION


OPERATION AND MAINTENANCE MANUAL
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S.A.I.C

TABLE OF CONTENT

SR.NO. CONTENTS PAGE NO.

PART – I THEORETICAL ASPECTS

1.0 INTRODUCTION 06

1.0.1 Theory of Dehydration 08

1.0.2 Process Description 10

1.0.3 Control Logic & Interlock Description 26

1.0.4 Equipment Description 27

1.0.5 List of Pressure Safety Valves 28

PART – II PRE-START-UP ACTIVITIES

2.0 GENERAL INSTRUCTION 30

2.0.1 Cooling Water Loop Testing 34

2.0.1 a SOP for establishment of cooling water circuit 34

2.0.2 Water Flushing/Cold Water Trial 36

2.0.3 Valve Stoke Checking 40

2.0.4 Vacuum Trial 41

2.0.5 Molecular Sieve Loading 45

PART – III PROCESS START-UP AND PROCESS PARAMETERS

3.0 GENERAL INSTRUCTION 51

3.0.1 Steam Conditioning / AFTER TURNAROUND 53

THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
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3.0.2 Start-up after steam conditioning(Normal start-up) 60

3.0.3 Cold start-up 63

3.0.4 Process Monitoring 67

3.0.5 Process Parameters 71

3.0.6 Troubleshooting 75

PART – IV PROCESS SHORT SHUTDOWN AND PROCESS START-UP

4.0 GENERAL INSTRUCTION 79

4.0.1 Power Failure 80

4.0.2 Cooling Water Failure 82

4.0.3 Low Pressure Steam /Steam supply Failure 84

4.0.4 Instrument Air Failure 87

4.1 Plant Short Shutdown and Start-up after Short Shutdown 89

4.1.1 Plant Short Shutdown 89

4.1.2 Plant Start-up after Short Shutdown 91

4.2 Plant Long Duration Shutdown and Start-up after Long 92


Duration Shutdown

4.2.1 Plant long duration shutdown 92

4.2.2 Plant start-up after long duration shutdown 95

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

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S.A.I.C

PART–I

THEORETICAL ASPECTS

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

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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) Process license is nonexclusive, non-


transferable, for commissioning and operation of 140,000 OR 150,000 lit/day
anhydrous alcohol plant using partially Corn or Sorghum as a feed stock at
VICENTIN S.A.I.C. Argentina.

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.

Under annexure, VICENTIN S.A.I.C. Argentina shall be responsible for


procurement and installation of Process plant according to engineering software
provided by PRAJ. VICENTIN S.A.I.C. Argentina will provide feedstock data,
rotary equipment and heat exchanger details to PRAJ. Necessary laboratory
equipment, instrument and furniture shall be provided by VICENTIN S.A.I.C.
Argentina. Also, Vicentin S.A.I.C shall be responsible for arranging skilled
operating staff for plant operation and laboratory analysis VICENTIN S.A.I.C.
Argentina shall train operating staff for plant and personal safety and hazards

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

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under local statutory regulations before commencement of Pre-Commissioning


activity of process plant.
As per annexure of the contract, all chemicals, feedstock and utilities shall be
made available by VICENTIN S.A.I.C. Argentina and shall ensure readiness for
completion of mechanical work as detailed out in contract.
Under article (Warranty of Capacity), VICENTIN S.A.I.C. Argentina
acknowledges that PRAJ is providing the design engineering services for the
Process Plant to Produce 140,000 OR 150,000 lit/day anhydrous alcohol plant and
that PRAJ has not actually constructed the Process Plant. PRAJ warrants that after
acceptance of plant performance parameters, process plant will have the capacity
to perform in all material respects with the performance specification. VICENTIN
S.A.I.C. Argentina expressly acknowledges that the ability of the process plant to
actually perform in material compliance with the performance specifications is
conditioned upon several factors outside of the control of PRAJ, including but not
limited to proper construction of the process plant, proper maintenance of the
plant and machinery, use of chemicals as per specification, availability of utility,
proper operation of the plant as per operation and maintenance manual supplied
by PRAJ.

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

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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.

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 FROM,”PRAJ INDUSTRIES LTD, “PRAJ HOUSE”, BAVDHAN, PUNE 411021, INDIA
CONSENT FROM

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Molecular Sieve Dehydration:


The advantages of the molecular sieve unit over other processes for alcohol
dehydration are high product dryness, ease of operation, lower energy and
operating costs, and lower capital costs.
In this process beds of 3A zeolite are used. The 3A zeolite has 0.3 nm pores. The
water molecules can enter the sieve and are adsorbed. The larger ethanol molecules
are not retained and are passed through the sieve bed.
In the adsorption process one bed is the in dehydration service while the other bed
is regenerated. During regeneration, the pressure is lowered and the water is
desorbed and swept out of the sieve bed with product vapor from the bed in
dehydration service. The alcohol in the regeneration stream is recovered in the
distillation column. The product vapor is condensed and condensed ethanol is
collected in product receiver.

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

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1.0.2 PROCESS DESCRIPTION:


PRAJ’s ECOMOL - Molecular Sieve Dehydration Unit (MSDH) is a modularized, as
well heat integration with Distillation system. Equipment package composed of a
Vaporizer and a molecular sieve dehydration system, along with interconnecting
piping and support equipment.
The Vaporizer Flash Tank and distillation system utilizes the following functions –
1) Vaporize the 94-95% v/v alcohol water liquid feed in Vaporizer Flash Tank (T-
1603)
2) Ethanol liquid stream produced during regeneration of the dehydration bed is
fed to Rectifier Column (C-1461).
3) Molecular Sieve Dehydration system dehydrated ethanol from alcohol water
mixture by means of molecular sieve.
Alcohol water liquid containing at least 94 - 95% v/v alcohol water draw is taken
from Distillation to Dehydration section. Alcohol water liquid is preheated in Feed
Preheater by using product vapor then fed to Vaporizer Flash Tank (T-1603). The
objective of the Vaporizer is to evaporate Alcohol water liquid. Energy is supplied
to the Vaporizer Flash Tank (T-1603) by Vaporizer Reboiler (H-1601) by using Low
Pressure Steam condensing on shell side. Steam Condensate may be return back to
Boiler. The Vaporizer operates under pressure. Alcohol water vapor from
Vaporizer Flash Tank is then passed through Superheater where alcohol vapor is
superheated. Energy for superheating is supplied by medium pressure steam
condensation on shell side of the Super heater. Superheated Alcohol water liquid
vapor are sent to twin Adsorbent Beds. The twin Adsorbent Beds operate in cyclic
manner. Twin beds are provided to allow for bed regeneration in continuous
operation. While one bed is in dehydration mode, the other is in regeneration

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

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mode. Depending on feed and product specifications, dehydration regeneration


exchange takes place approximately every few minutes.
The feed alcohol vapor is passed through the bed under dehydration mode. The
Adsorbent Bed will adsorb moisture present in feed alcohol water vapor and
dehydrated product alcohol vapor (with moisture content less than 0.2% v/v) are
obtained from bottom of the bed.
The product alcohol vapor is passed through Regeneration Preheater and Feed
Preheater for heat recovery. Balance vapor are condensed in Product Vent
Condenser and Condensed product alcohol is collected in product receiver. The
Product alcohol from Product Receiver is pumped to Product Cooler where it is
cooled with the help of cooling water and transfer to Fuel Ethanol storage.
During regeneration mode, vacuum is applied to the bed under regeneration. A
small amount of product alcohol vapor are purged through the bed in regeneration
mode under high vacuum, to prepare the desiccant for cycle changeover when this
bed goes online. The purged alcohol vapor is act as carrier for removal of moisture
from the bed. Alcohol vapor along with moisture are obtained from the top of bed.
This alcohol-water vapor (regeneration stream) is condensed in Regeneration
Condenser, which is attached to Vacuum Eductor. Vacuum is generated in the
system with the help of Vacuum Eductor. Regeneration stream is used as motive
fluid for Vacuum Eductor. The regeneration stream coming from the Regeneration
Condenser is pumped, preheated in Regeneration Preheater and fed to the Rectifier
Column for recovery of alcohol. Moisture present in feed alcohol is removed from
the bottom of the Rectifier Column in the form of spent lees. After one cycle is over,
the bed are interchanged, that is, the bed on dehydration mode will be switch over

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

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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

THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
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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

THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
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zeolite molecular sieve desiccant (sometimes referred to as molecular sieve, mol


sieve, or MS). The dehydration operation involves two (2) cycles
1. Adsorption: the period during which water is removed from the wet ethanol
vapor by the desiccant.
2. Regeneration: the period during which the adsorbed water is removed from
the desiccant.
For continuous operation two molecular sieve dehydration bed is used. The
duration of the adsorption and regeneration cycles is approximately five (5)
minutes each, with one bed adsorbing while the other regenerates. Valve sequences
and other control loops are controlled by controlled system. Air operated valves on
the inlet and outlet of the molecular sieve bed vessels are opened and closed in a
programmed sequence to achieve the adsorption and regeneration cycles. The
control logic is also programmed to protect the molecular sieve beds from excessive
pressure changes during the transitions between regeneration and adsorption using
sequential valve controls.
The molecular sieve desiccant has the ability to selectively adsorb water molecules
from the ethanol as the hot vapor passes through it.
Pressures are monitored by the control system (as well as local indicators) near the
top and bottom of each molecular sieve bed as follows:

V-1601A Top PI-160208 and PIT-160204


Bottom PI-160210 and PIT-160205

V-1602B Top PI-160209 and PIT-160207


Bottom PI-160211 and PIT-160206

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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.

THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
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The locations and numbers are as follows:


V-1601 A Top TI-160202 & TI-160211
Upper Mid-Bed TI-160203 & TI-160212
Lower Mid-Bed TI-160204 & TI-160213
Bottom TI-160205 & TI-160214

V-1601B Top TI-160206 & TI-160215


Upper Mid-Bed TI-160207 & TI-160216
Lower Mid-Bed TI-160208 & TI-160217
Bottom TI-160201 & TI-160218

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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Molecular Sieve Regeneration System


The regeneration stream coming out from molecular sieve bed is taken from
Regeneration Condenser (H-1603) through vacuum Eductor (J-1601) to
Regeneration Receiver (T-1602). From Regeneration Receiver by means of
Regeneration Pump (P-1602 A/B), the regeneration stream is feed to Rectifier
Column (C-1461) through Regeneration Preheater (H-1604). 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).
Regeneration Filters (F-1602) (25-Micron Absolute) are provided to filter out any
suspended solids entrained in the regeneration liquid during the regeneration
cycle. Pressure indicators are provided to monitor the pressure drop across the
filters. A pressure drop in excess of 1 kg/cm2 indicates the need to clean the filter
bag. This filter will probably require frequent attention during the first week of
continuous operation as the dust from the new sieve desiccant is purged from the
beds. After a month of operation, this filter should rarely require servicing.
Note: A sudden increase in sieve dust collected in the filter indicates a possible
problem, and should be reported to PRAJ immediately so that the problem can be
expeditiously investigated and resolved.

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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Medium pressure steam flow to the Superheater (H-1602) is controlled by


Temperature Indicator & Controller (TIC-160209) using a Temperature control
valve (TCV-160209) located on the steam line to the Superheater (H-1602), where
the temperature is raised from about 90°C to approximately 120-125 °C. The sieve
beds function properly at any temperature within the 110 - 121°C range. The 120-
125 °C setting provides the best energy efficiency while the 121°C is more for
giving in the event of a process upset or operator error. It also gives operators more
time to take corrective action if bed temperatures start decreasing due to
condensation forming in the beds (sometimes known as wetting the beds).
The superheated wet ethanol vapor stream (typically at a pressure of 1.76 kg/cm2
(a)) goes to the particular sieve bed vessel, which is in the “dehydration” or
adsorption cycle. The molecular sieve desiccant adsorbs the water from the hot
vapor stream as it passes through the bed. The vapor then emerges from the bottom
as Fuel Ethanol vapor at about 118°C and 1.62 kg/cm2 (a). A portion of the
outgoing product vapor, typically 10- 15%, is passed back through the regenerating
sieve bed vessel.
The Fuel Ethanol vapor flows to the Regeneration Preheater (H-1604), Aldehyde
Recovery Column Reboiler (H-1404) and Feed Preheater (H-1605). The
Regeneration Preheater (H-1604) uses the thermal energy of the anhydrous vapor
to preheat regeneration liquid and Aldehyde Recovery Column Reboiler (H-1404)
uses the thermal energy of ethanol vapor for boiling liquid in Aldehyde Recovery
Column (C-1402). Excess vapor are condensed in Feed Preheater (H-1605) and
Product Condenser (H-1608). The Product condensate is collected in Product
Receiver (T-1601). The Product Pump (P-1601A/B) transfers the anhydrous alcohol
to storage through the Product Cooler (H-1606) which cools the product. The

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Product Receiver level is controlled by Level Indicator & Controller (LIC-160302)


through Level control valve (LCV-160302).
System pressure is dictated by the outlet pressure in the dehydrating sieve bed as
controlled by the Sieve Bed Pressure Controller (PIC-160204). The control computer
monitors a pressure transmitter (PIT-160204 or PIT-160207) at the top of the sieve
bed that is in the dehydration cycle, and sends signals to the Sieve Bed Back
Pressure Controller (PIC-160204) to regulate valve (PCV-160208) and maintain a
constant bed pressure.
The parts of vapor from sieve bed (V-1601A/B) are used as heating media for
Aldehyde Recovery Column Reboiler (H-1404). The alcohol vapor from sieve bed
(V-1601A/B) is condensed on shell side of Aldehyde Recovery Column Reboiler
(H-1404) by giving its thermal energy to tube side of the reboiler. The condensed
alcohol from Aldehyde Recovery Column Reboiler (H-1404) fed to Product
Receiver (T-1601), whereas non-condensable are fed to Product Condenser (H-1608)
and PCV Condenser (H-1609) through (PCV-160301). The Product Receiver (T-
1601) pressure is controlled by (PIC-160301). The condensed ethanol from Product
Condenser (H-1608) is fed to Product Receiver (T-1601), whereas condensed
ethanol from PCV Condenser (H-1609) is fed to Regeneration Receiver (T-1602).

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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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STREAM LOCATION V-1601A V-1602B


94 – 95%v/v Alcohol Water Vapor Inlet Top PCV-160201 PCV-160202
Regeneration Vapor Outlet Top FCV-160203 FCV-160204
Dehydrated Ethanol Vapor outlet Bottom FCV-160206 FCV-160205
Molecular sieve I/II Pressure Equalization - PCV-160208

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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MAIN CYCLE: V-1601A ON-LINE FOR DEHYDRATION


(300 Seconds)

V-1601 A - ADSORBING / PRESSURE V-1601 B– REGENERATING / VACUUM

VALVE POSITION VALVE POSITION


PCV-160201 OPEN PCV-160202 CLOSED

FCV-160203 CLOSED FCV-160204 OPEN

FCV-160206 OPEN FCV-160205 Pmax / Pmin

TRANSITION 1: VACUUM RELEASE


(10 - 20 Seconds)

V-1601 A / PRESSURE V-1601B/ VACUUM


VALVE POSITION VALVE POSITION
PCV-160201 OPEN PCV-160202 CLOSED
FCV-160203 CLOSED FCV-160204 CLOSED
FCV-160206 OPEN FCV-160205 Pmax

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 3: PRESSURIZE V-1601B/ DE-PRESSURIZE V-1601A


(30 - 50 Seconds)

V-1601 A / VACUUM V-1602 B/ PRESSURE


VALVE POSITION VALVE POSITION
PCV-160201 CLOSED PCV-160202 OPEN
FCV-160203 PART OPEN * FCV-160204 CLOSED
FCV-160206 CLOSED FCV-160205 OPEN

MAIN CYCLE: V-1601B ON-LINE


(300 Seconds)

V-1601A– REGENERATING / VAC V-1601B – ADSORBING / PRES


VALVE POSITION VALVE POSITION
PCV-160201 CLOSED PCV-160202 OPEN
FCV-160203 OPEN FCV-160204 CLOSED
FCV-160206 Pmax / Pmin FCV-160205 OPEN

TRANSITION 1: VACUUM RELEASE


(10 - 20 Seconds)

V-1601A/ VAC V-1601B /PRES


VALVE POSITION VALVE POSITION
PCV-160201 CLOSED PCV-160202 OPEN
FCV-160203 CLOSED FCV-160204 CLOSED
FCV-160206 Pmax FCV-160205 OPEN

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TRANSITION 2: EQUALIZATION
(10 - 20 Seconds)

V-1601A/ EQUAL V-1601B / EQUAL


VALVE POSITION VALVE POSITION
PCV-160201 OPEN PCV-160202 OPEN
FCV-160203 CLOSED FCV-160204 CLOSED
FCV-160206 Equalization purge position FCV-160205 OPEN

TRANSITION 3: PRESSURIZE V-1601A/ DE-PRESSURIZE V-1601B


(30 - 50 Seconds)

V-1601A/PRES. V-1601B/ VAC.


VALVE POSITION VALVE POSITION
PCV-160201 OPEN PCV-160202 CLOSED
FCV-160203 CLOSED FCV-160204 PART. OPEN *
FCV-160206 OPEN FCV-160205 CLOSED

* Valve is ramped to go from fully closed to fully open in approximately forty (40)
seconds.

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1.0.3 CONTROL LOGIC & INTERLOCK DESCRIPTION


Refer “Control Logic and Interlock Description (N-10012-4-ILD1601)” for Dehydration
section.

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1.0.4 EQUIPMENT DESCRIPTION


QUANTITY
TAG NO DESCRIPTION TECHNICAL DETAILS
OP. S/B
Type: Shell & Tube,
H-1605 Feed Preheater 1 0
Orientation :Vertical
Type: Shell & Tube,
H-1601 Vaporizer Reboiler 1 0
Orientation : Vertical
Type: Shell & Tube,
H-1602 Superheater 1 0
Orientation: Horizontal
Type: Shell & Tube,
H-1603 Regeneration Condenser 1 0
Orientation : Vertical
Type: Shell & Tube,
H-1604 Regeneration Preheater 1 0
Orientation: Horizontal
Type: Shell & Tube,
H-1608 Product Condenser 1 0
Orientation : Vertical
Type: Shell & Tube,
H-1606 Product Cooler 1 0
Orientation: Vertical
Type: Shell & Tube,
H-1609 PCV Condenser 1 0
Orientation : Vertical

H-1607 Regeneration Cooler 1 0 Type: Plate Heat Exchanger

Type: Bag Filter


F-1601 Feed Filter 1 0
Mesh Size 25 Micron
Type: Bag Filter
F-1602 Regeneration Filter 1 0
Mesh Size 25 Micron
J-1601 Vacuum Eductor 1 0 -
Type: Cylindrical/Vertical
T-1603 Vaporizer Flash Tank 1 0 Shell with Dished end
Capacity: 2.4 m3
Type: Cylindrical/Vertical
T-1601 Product Receiver 1 0 Shell with Dished end
Capacity: 1.5 m3
Type: Cylindrical/Vertical
T-1602 Regeneration Receiver 1 0 Shell with Dished end
Capacity: 1.5 m3

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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 -

Y-1602 Flame Arrestor for T-1603 1 0 -

Y-1603 Flame Arrestor for H-1609 1 0 -

1.0.5 LIST PRESSURE SAFETY VALVES

SR.NO. TAG NO DETAILS SET PRESSURE


Pressure Safety valve for Vaporizer
1 PSV-160101 2.2 kg/cm2(a)
(T-1603)

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PART–II

PRE-START-UP ACTIVITIES

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2.0 GENERAL INSTRUCTIONS


Operator must read and understand these instructions before operating the plant.

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.

4. Operator should read the bought-out items operation manual / safety


procedures received from respective vendors and follow the instructions as
mentioned in their manual before starting / stopping the respective item.

5. Operating personnel should follow the safety regulations as per factory rules
as well as factory acts and regulations.

A. Inspection and cleaning of Equipment

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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All instruments should be mounted at respective locations, tested, calibrated and


ready for use. Ensure that all equipment and instruments are properly tagged and
respective tag numbers and nameplates are visible to operators to avoid any
confusion during operation. Pipes should be colored and coded for proper
identification and ease of operation as per the codes prescribed by local legal body.
Once P&ID & Layout audit is completed and system is ready in all respects, carry
out internal inspection of all equipment. Ensure that there should not be any
foreign material inside. It should be free from all debris. Note that external process
area is equally important and it should be neat and clean. There should not be any
machinery lying inside the process area, which may create obstacle in operation.

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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C. Pressure Safety Valve & Pressure vacuum Relief Valves


All PSV should be tested for their accurate set pressures and proper functioning.
They can be tested at site if facilities are available or should get tested from outside
agency with its certification.
D. Box up of System
Once equipment’s inspection & cleaning is completed and piping flushing is
completed, box up the total system. Ensure that all pipe lines are properly
connected in place. All manholes / man-ways, drains, vents should be closed
properly and system should be made ready for use.

E. Control valve Stroke Checking


It is very important to conduct stroke trials of all control valves before putting them
in actual use, Process and Instrumentation person should witness the stroke
checking trial of all control valves. During stroke trial it is necessary to match valve
opening on control panel with valve opening in field. After complete stroke
checking its formal report should be made and problems faced should be reported
and rectified.

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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G. Utility and Allied System Checks


It is necessary to know readiness of the utilities and allied systems otherwise it may
create nuisance during pre-start-up and start-up. In utilities and allied system,
check followings should be ready and designed to supply required inputs to the
main plant and accept outputs from the main plant:

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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2.0.1 COOLING WATER LOOP TESTING

2.0.1a SOP FOR ESTABLISHMENT OF COOLING WATER CIRCUIT FOR


DEHYDRATION SECTION
Cooling water system is most important considering plant performance. Cooling
water should be available with desired flow and desired pressure at respective
user. Ensure that cooling water, which is being used, meets all specifications like
hardness, pH, phosphate, turbidity, alkalinity, etc. Better quality of cooling water
supply (CWS) definitely ensures better life of the exchangers and less maintenance
cost. Before starting cooling water pump is to be sure that all vents on Cooling
water lines are open to vent out the air. Vent at top most point should be open to
ensure complete removal of air from the Cooling water circuit. After venting out
air and once continuous supply of water starts close vents and establish the
desired flows through respective users with sufficient control valve opening in
MAN mode. Check the Cooling water supply pressure on respective header and it
should be sufficient enough to fulfil the requirement. Run the complete cooling
water circuit to ensure better performance.

1. Ensure Cooling Water supply is available.


2. Open Regeneration Condenser (H-1603) cooling water return manual valve.
Ensure complete venting of air through vent valve.
3. Open inlet and outlet cooling water side manual valves of Regeneration Cooler
(H-1606). Ensure complete venting of air through vent valve.
4. Open cooling water inlet manual valve for PCV condenser (H-1609).

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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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2.0.2 WATER FLUSHING / COLD WATER TRIAL

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:

a. Vaporizer Flash Tank (T-1603)


b. Regeneration Receiver (T-1602)
c. Product Receiver (T-1601)
d. Steam Condensate Tank (T-1604)
Before starting actual water trial ensure availability of Process water and other
utilities. All motors, pumps are to be operated remotely in coordination with field
personnel. It is presumed that instrument air line flushing, control valve stroking of
all control valves and instrumentation continuity has already been done. Flushing
of Sealing Water Header and utility headers has been done thoroughly.

1. Water flushing for Dehydration section to be taken in continuation with water


flushing of Aldehyde Recovery Column (C-1402) in Distillation section.
2. Open manual valve on Aldehyde Recovery Column bottom pump (P-1403A/B)
discharge line to Dehydration section.
3. Open Manual isolation valve on Feed Filter (F-1601). Open manual valve on
feed Preheater (H-1605) shell side inlet and outlet. Open Vaporizer Flash Tank

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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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regeneration flow control valve (FCV-160207) and Regeneration Pump (P-1602


A/B) discharge valve. Stop Regeneration Pump (P-1602A/B). Keep 50% level in
Regeneration Receiver (T-1602), which is required for vacuum trial of Molecular
Sieves.
7. Start process water to Product Receiver (T-1601). Open product pump (P-1601
A/B) suction valve. Open product pump (P-1601A/B) suction drain valve till
clear water is observed. Level in Product Receiver (T-1601) will start to increase.
Calibrate (LIC-160302). When Product Receiver (T-1601) level reaches 95%, start
product pump (P-1601A/B).
8. Ensure storage section is ready to receive water; open manual valve on product
pump (P-1601A/B) discharge to storage.
9. Open level control valve for product receiver (LCV-160302) 25% in MAN mode
and flush the line. Ensure flow through (FQI-160301). Ensure product pump (P-
1601A/B) performance. After ensuring the line flushing close level control valve
for product receiver (LCV-160302), stop product pump (P-1601A/B).
10. Start process water to Steam Condensate Tank (T-1604). Open Steam
Condensate Pump (P-1604A/B) suction valve. Open steam Condensate pump
(P-1604A/B) suction drain valve till clear water is observed. Level in steam
Condensate Tank (T-1604) will start to increase. Calibrate (LIC-160102). When
steam Condensate Tank (T-1604) level reaches 85%, start Steam Condensate
Pump (P-1604A/B).
11. Open level control valve for Steam Condensate Tank (LCV-160102) 25% in
MAN mode and flush the line. Ensure Steam Condensate Pump (P-1604A/B)
performance. After ensuring the line flushing close level control valve for Steam
Condensate Tank (LCV-160102), stop Steam Condensate Pump (P-1604A/B).

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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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2.0.3 VALVE STROKE CHECKING


As molecular sieve dehydration process is almost fully automated system where
Molecular Sieve changeover takes place after every 5 minutes through
programmable logic, it is necessary to check the valve stroking for following valves.
At the time of valve stroking check the actual opening on the field and set the
digital feedback signals (ZT) accordingly.
1. Vaporiser pressure control valves (PCV-160201& PCV-160202).
2. Molecular Sieve pressure control valve (PCV-160208).
3. Molecular Sieve vacuum generation valves (FCV-160203 & FCV-160204)
4. Molecular Sieve bottom flow control valves (FCV-160206 & FCV-160205)

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2.0.4 VACUUM TRIAL


Vacuum test has to be carried out for all the equipment which is subjected to
vacuum condition during the plant operation. Vacuum trial is to be carried out to
detect air leakage in the system as well as to ensure the tight shutoff condition of
high performance butterfly valves in Dehydration section.
Before staring the vacuum trials Regeneration Pump (P-1602A/B) should be tested
and its performance should be monitored.
• Ensure cooling water is available for the Regeneration Cooler (H-1607).
• Ensure the stroke checking of high performance butterfly valves completed.
• Ensure inspection & cleaning of equipment completed.
• Ensure pipeline flushing completed.
• All utilities are available in all respects.
Once these preliminary checks is over then start the Regeneration Pump (P-1602
A/B). Note the current, pump discharge pressure and flow. After satisfactory
operation for one hour check standby pumps in a same manner.
Isolate the system in such a way so that nothing should come in or nothing should
go out only it should be connected to vacuum system. Close all drains, vents,
manholes.
Following equipment will be under vacuum in Dehydration Section:
a. Molecular Sieve I (V-1601A)
b. Molecular Sieve II (V-1601B)
c. Shell side of Regeneration condenser (H-1603).

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NOTE: - VACUUM TRIAL BEFORE MOLECULAR SIEVE LOADING


1. Ensure Regeneration Receiver (T-1602) having 50 – 60% water level.
2. Ensure cooling water flow through Regeneration Cooler (H-1607).
3. Ensure following isolation & control valves position before starting the
regeneration pump.
3.1.Regeneration Pump (P-1602A/B) suction manual valve – OPEN.
3.2.Regeneration Pump (P-1602A/B) discharge manual valve – CLOSED.
3.3.Regeneration Cooler (H-1607) AWL side inlet and outlet manual valves –
OPEN.
3.4.Regeneration Cooler (H-1607) AWL bypass manual valve – CLOSED.
3.5.Regeneration Pump (P-1602A/B) discharges to Rectifier column (C-1461)
and manual valves on Regeneration Filter (F-1602) – CLOSED.
3.6.Manual valves on Feed Filter (F-1601) – CLOSED.
3.7.Pressure control valve PCV-160201, PCV-160202 & PCV-160208 – CLOSED.
3.8. Flow control valve FCV-160203, FCV-160204, FCV-160206, FCV-160205 –
CLOSED.
3.9.Manual valves on all pressure indicators and transmitters – OPEN.
3.10. Manual valve at Vacuum Eductor (J-1601) suction on line L160210 –
CLOSED.
4. After ensuring the above valve positions, start Regeneration Pump (P-
1602A/B). Gradually open Regeneration Pump (P-1602A/B) discharge valve.
Ensure Regeneration Pump (P-1602A/B) discharge pressure and flow.
5. Water will start flowing to Regeneration Receiver (T-1602) through Vacuum
Eductor (J-1601).

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6. Keep watch on temperature of cooling water return (TI-160307) in order to


ensure the performance of Regeneration Cooler (H-1607).
7. Vacuum will start developing on shell side of Regeneration Condenser (H-
1603). After achieving maximum possible vacuum check Regeneration
Condenser (H-1603) system for air leakages.
8. Open flow control valve FCV-160203, 5% in MAN mode. Gradually vacuum
will start developing in Molecular Sieve I (V-1601A). Gradually open FCV-
160203 to 100% and allow maximum possible vacuum in Molecular Sieve-I (V-
1601A).
9. Ensure the healthiness of tight shutoff condition for PCV-160201, FCV-160206
and FCV-160204. Tight shutoff condition for PCV-160201 can be ensured from
PIT-160201, tight shutoff condition for FCV-160204 can be ensured from PIT-
160207 and PIT-160206.
10. After achieving maximum possible vacuum, check Molecular Sieve I (V-1601A)
system for air leakages. Close FCV-160203. Close Regeneration Pump (P-
1602A/B) discharge valve and stop the Regeneration Pump (P-1602A/B).
11. 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 I (V-
1601A).
12. Ensure Molecular Sieve II (V-1601B) at atmospheric pressure condition. Start
Regeneration Pump (P-1602A/B) and gradually open pump discharge valve.
Open FCV-160204, 5% in MAN mode. Gradually vacuum will start developing
in Molecular Sieve II (V-1601B). Gradually open FCV-160204 to 100% and allow
maximum possible vacuum in Molecular Sieve II (V-1601B).

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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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2.0.5 MOLECULAR SIEVE LOADING


A. PREPARATION FOR MOLECULAR SIEVE LOADING
Molecular sieve loading is completely manual operation so manpower required
need to be considered before actual molecular sieve loading. Manpower required
will be 5 number of labours with one supervisor, one crane operator, and one safety
supervisor. All the people who are supposed to involve in this operation should be
aware of MSDS of molecular sieves & Ballast. (Refer Material Safety Data Sheet
for Molecular Sieve & Ballast) for proper handling and safety precautions. Risk
assessment need to be done before starting molecular sieve loading activity.
Following is the list of items required during molecular sieve loading
1. One crane for lifting ballast / molecular sieve drums up to molecular Sieve
top.
2. Require Personal Protection Equipment (PPE) for all the members involved
in loading operation.
3. One flameproof exhaust fan, which can be easily mounted on the top nozzle
of the Molecular Sieve.
4. One steel pipe of 1’’ diameter with length equivalent to bed height.
5. It is preferred to have engineering services department team for support
during molecular sieve loading.
6. Platform at the top of the Molecular Sieve for access to people and to guide
the drums while unloading in Sieve Bed.
7. 1 No. Topaz for proper distribution of ballast at the top of the Molecular
Sieve.
8. 1 No. Flame proof torch for internal inspection of Molecular Sieves.
9. Ballast and molecular sieves requirement will be as below –

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Molecular sieves (8400 X 2 beds kg)


1’’ Ballast (630 X 2 beds kg)
½’’ Ballast (280 X 2 beds kg)
¼’’ Ballast (280 X 2 beds kg)
10. Molecular Sieve I /II (V-1601A/B). inserts required will be
2’’ Inserts - 4 No.
14’’ Inserts - 2 No.
3’’ Multiple Inserts – 16 No.
11. 1 No. Ultrasonic vacuum detector.

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B. MOLECULAR SIEVE LOADING


Note: - Go through the pictorial representation before starting actual molecular
sieve loading
Following procedure is to be followed for molecular sieve loading in Molecular
Sieve I/II (V-1601A/B)
1. Confirm multiple inserts in both the Molecular Sieves are fully welded.
2. Confirm side inserts in both the Molecular Sieve I/II (V-1601A/B) are properly
fitted. Side inserts of 2’’ to be inserted at N3 & N4 nozzles body flange of the
Molecular Sieve I/II (V-1601A/B) with gasket on both sides of head of the
insert.
3. After successful completion of vacuum test release the vacuum in both the
molecular Molecular Sieves.
4. Open the manholes of both the Molecular Sieve I/II (V-1601A/B).
5. Open the drums of the ½’’ ballast and check the inside condition; it should be
neat & clean and completely dry. (Use the appropriate PPE before handling the
ballast and/ or molecular sieves).
6. By using the buckets spread these ½’’ ballast evenly in the Molecular Sieve.
7. By using topaz make top surface completely flat so that ballasts should get
uniformly distributed all over.
8. Then on ½’’ ballast spread ¼’’ ballast evenly up to top of the bottom insert.
9. On top of ¼’’ ballast spread 2 No. of molecular sieve drums evenly and make
top surface completely flat by using topaz and close the manhole and tight it.
10. Perform vacuum test of the above said Molecular Sieve I/II (V-1601A/B). If
vacuum test is perfect then proceed to next step. If not, check for the leakages
and get it rectified.

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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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C PICTORIAL REPRESENTATION OF MOLECULAR SIEVE BED

14” INSERT

1” BALLAST

MOLECULAR SIEVES
1'' ABOVE TOP
SCREEN

2'' INSERT FOR PT

TOP SCREEN

MOLECULAR SIEVES

2'' INSERT FOR PT

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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3.0 GENERAL INSTRUCTIONS


Operator must read and understand these instructions before operating the plant.
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’s intervention when necessary.
4. Operator should read the Operation Manual for bought-out items / safety
procedures received from respective vendors and follow the instructions as
mentioned in their manual before starting / stopping the respective item.
5. Operating personnel should follow the safety regulations as per factory rules as
well as factory acts and regulations.
6. Before plant start-up it is necessary to make detailed schedule so as to
understand sequence of start-up of individual sections and their
synchronization.
Safety Note
1. This is a hardhat and safety glasses area.
2. Never attempt to repair or replace the equipment in this area without prior
consent from authorized plant personnel. Never attempt to repair or replace any
equipment in this area without following Lockout-Tagout (LOTO) procedure

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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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3.0.1STEAM CONDITIONING / AFTER TURNAROUND*


Note: *Turnaround is defined as replacement of the sieve desiccant.
This activity to be carried out in continuation with stabilized water boiling of
Distillation section and at least two/ five days before availability of alcohol water
liquid. The intension is to ensure the continuous water supply to Vaporizer Flash
Tank (T-1603). Alternatively, temporary water arrangement from ethanol storage
tank to Vaporizer Flash Tank (T-1603) can also made.
STEAM CONDITIONING ACTIVITY IS REQUIRED ONLY ONCE IN THE
LIFETIME OF PARTICULAR MOLECULAR SIEVES. STEAM
CONDITIONING ACTIVITY IS REQUIRED ONLY AFTER REPLACEMENT
OF MOLECULAR SIEVES WITH NEW ONE.
The dehydration plant is a custom designed equipment system containing various
proprietary technologies developed by Praj. Since the dehydration plant is a
custom designed piece of equipment engineered specifically for the customer’s
ethanol liquid streams, it is not possible to know in advance the exact settings for
start-up and operating adjustments until the system can be operated for a few
weeks and fine tuned. The settings and parameters listed below and in other
sequence of operations described in this manual are subject to minor change.
1.Verify that all control valves identified in P&IDs are in closed position.
2.Verify that all pumps identified in P&IDs are stopped.
3.Plant personnel must ensure that a sufficient liquid level is available in the
Regeneration Receiver (T-1602) to operate the Regeneration Pump (P-1602A/B).
The tank must have a minimum of a 50% level. If the level is below this amount,
water can be added through the nozzle given to the Regeneration Receiver. Do
not fill the Regeneration Receiver above 70% level.

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4.Ensure all interlocks are off line/bypassed at a time of steam conditioning.


NOTE:
• At initial start-up (or following a turnaround) When water is absorbed by
new, completely dry desiccant, a significant amount of heat will be generated
in a short period of time in the sieve beds by this “heat of adsorption.” The
chemical reaction occurs in the reverse during the regeneration cycle, but the
cycle is not long enough for the regenerating bed to do any significant
cooling. During startup, temperatures in the dehydrating sieve bed can go
from ambient temperature to 230°C or hotter in a few hours or less. These
extreme temperatures can damage the equipment, instrumentation and
controls.
• In order to prevent an overheat condition, the dehydration/regeneration
cycles should be shortened to 2.5 - 3.0 minutes during startup with new sieve
material. The sieve bed temperatures should be continuously monitored, and
if they start to get above 205°C, the cycle times should continue to be
shortened until none of the temperatures exceeds 205°C. The unit should be
shut down and allowed to cool down for 6-8 hours if the bed temperature
exceeds 230°C.
• This heating problem will not reoccur on subsequent start-ups after the beds
have been “broken in” (unless a significant amount of new desiccant material
has been added). This is because once the new sieve beds stabilize during
start-up; they never again get completely dry. Even after regenerating during
normal operating cycles, the sieve beds still have residual water in them
which limits this “heat of adsorption” to the range of temperatures typically
seen in the sieve beds during the dehydration cycle.

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The following is a description of the start-up sequence


1. Ensure cooling water flow is established
2. Ensure Aldehyde Recovery Column Reboiler (H-1404) is ready to accept vapor
from Dehydration plant.
3. Ensure continuous availability of water to Vaporizer Flash Tank (T-1603) from
Aldehyde Recovery Column Bottom or make temporary water connection for
alcohol water line to Vaporizer Flash Tank (T-1603).
4. 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.
5. The Regeneration Pump (P-1602A/B) should be started if the Regeneration
Receiver level is greater than 50%. Once the pump starts, the operator should
open the discharge valve gradually. Starting the Regeneration Pump (P-
1602A/B) performs the two following functions:
a. Provides the liquid motive force for Vacuum Eductor (J-1601).
b. Pumps the excess regeneration liquid from the Regeneration Receiver (T-
1602) to the Rectifier Column (C-1461) where the ethanol is recovered.
6. Lineout process water to Vaporizer Flash Tank (T-1603) by taking Feed
Preheater (H-1605) and Feed Filter (F-1601) on line.
7. Keep manual valve on PCV condenser (H-1609) shell side vent 100% open.
8. Open Vaporizer Flash Tank (T-1603) level control valve (LCV-160103) 25% in
MAN mode and take 20% level in Vaporizer Flash Tank (T-1603). Take LIC-
160101 in AUTO mode with 20% set point.
9. 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.

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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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3.0.2 START-UP AFTER STEAM CONDITIONING (Normal Start-up)


After start-up of Distillation section, alcohol water liquid is line out to storage tank.
Dehydration plant is started after achieving 10-20% level in off-spec alcohol storage
tank for continuous supply of alcohol water liquid to Dehydration section. After
stabilization of Distillation plant line out alcohol water feed to Dehydration section.
Verify that all cooling water valves are open and cooling water flow is established.
1. Ensure the Distillation section is running.
2. Ensure the Molecular Sieve beds temperatures are below 100-120 o C.
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 Aldehyde Recovery Column Reboiler (H-1404) is ready to accept vapor
from Dehydration plant.
5. Ensure all interlocks are offline/bypassed.
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 level is greater than 50%. Once the Regeneration Pump start (P-
1602A/B), gradually open the discharge valve.
8. Open manual valve on vent line on L160107/15/HAL/KR2 to Vaporizer Flash
Tank (T-1603). Close the vent valve after ensuring the venting of water from the
line (This is required only during first start-up after steam conditioning in order
to remove water).
9. Lineout alcohol water liquid with 94-95% 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

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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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18. 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.
Note-At lower dehydration plant capacity, purge position of FCV-160206 and
FCV-160205 required to keep lower side. Actual purge position will be
decided at the time of commissioning.
19. 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 at 50%.
20. Level in Product Receiver (T-1601) will start increasing. When Product Receiver
(T-1601) LIC-160302 reaches 50%, start Product Pump (P-1601A/B) and take
Product Receiver (T-1601) LIC-160302 in AUTO mode with 50% set point.
21. PIC-160301 in AUTO mode with 1.5-1.6 kg/cm2 (a) set point.
22. Gradually temperature of bed starts increasing in adsorption mode whereas
during regeneration mode it will decrease. Ensure the bed temperature on local
temperature gauges.
23. Allow all sieve bed temperature to stabilize at 115 -125 oC.
24. After ensuring stabilization of bed temperature at 115-125oC, gradually increase
the Low Pressure Steam flow to Vaporizer Reboiler (H-1601) to be adjusted
based on the required production.

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25. Normalize the sieve sequence parameters.


26. Take all interlocks are online.
27. Check dehydrated ethanol concentration of product at regular intervals.
Note: Juice Vapour to Vaporizer Reboiler (H-1601) to be adjusted based on the
required production. Feed to Dehydration from Distillation is to be kept
constant.
Periodically inspect Regeneration Filter (F-1602) for abnormal differential pressure
readings. After initial start-up, this differential should remain low. These filters
should need some infrequent cleaning or changing, but a sudden increase in
cleaning frequency should be investigated immediately, as this may indicate some
possible system damage (any significant increase in cleaning frequency must be
immediately reported to PRAJ).

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3.0.3 COLD START-UP

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-160201 15-25 %* PCV-160202 0%

FCV-160203 0% FCV-160204 100 %**

FCV-160206 100 % FCV-160205 0%

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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15. In order to prevent an overheat condition, the dehydration/regeneration cycles


should be shortened manually to 2.5 - 3.0 minutes during cold start-up. The
sieve bed temperatures of V-1601A should be continuously monitored. V-1601A
top temperature TI-160202 will start increasing. When temperature at TI-160202
reaches 120-125 oC, switch over the adsorption to V-1601B manually by giving
opening to control valves as shown in TABLE B–

V-1601A V-1601B

PCV-160201 0% PCV-160202 15-25 %*

FCV-160203 100 % FCV-160204 0%

FCV-160206 0% FCV-160205 100 %

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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Note-At lower dehydration plant capacity, purge position of FCV-160206 and


FCV-160205 required to keep lower side. Actual purge position will be
decided at the time of commissioning.
18. 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 at 50%.
19. Level in Product Receiver (T-1601) will start increasing. When Product Receiver
(T-1601) LIC-160302 reaches 50%, start Product Pump (P-1601A/B) and take
Product Receiver (T-1601) LIC-160302 in AUTO mode with 50% set point.
20. PIC-160301 in AUTO mode with 1.5-1.6 kg/cm2 (a) set point.
21. Repeat the manual changeover of sieve beds till all temperature indicators of V-
1601A and V-1601B will stabilize at 115-120 oC.
22. 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.
23. Normalize the sieve sequence parameters as per normal operation and put all
interlocks are online.
24. Check dehydrated ethanol concentration of product at regular intervals.
25. After ensuring stabilization of bed temperature at 115-125 oC, gradually increase
the Low Pressure Steam flow to Vaporizer Reboiler (H-1601) to be adjusted
based on the required production.

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3.0.4 PROCESS MONITORING


This section describes the general principles that PRAJ INDUSTRIES LTD. has
developed to operate and adjust this type of equipment. The information needed to
program the control system (control logic, operating ranges, set points, etc.) is
given (Refer N-10012-4-ILD1601).
Even though the control system will continually control and monitor the
performance of the dehydration; Manual inspections, checks, and adjustments
should be made from time to time. The following adjustments are typically made
by, or in conjunction with, the control system to provide optimum performance.
Although the dehydration has been designed to practically run by itself for periods
at a time, there should always be an operator close enough to the control system
and/or the equipment to see or hear any alarms or other symptoms of trouble that
might be exhibited by the system. Also, the system should be thoroughly inspected
at least once every two hours by an operator. If problems are noted during the
inspection procedures, consult the troubleshooting guide (Refer Section 3.0.6).
 Bed Temperature
Bed operating temperature is controlled by the Superheater vapor discharge
Temperature Controller (TIC-160209).
 Vaporizer Flash Tank (T-1603) Pressure
The operating pressure of the Vaporizer Flash Tank (T-1603) is controlled by the
Pressure Controller PIC-160201 which modulates valve PCV-160201 or PCV-
160202 depending on which sieve bed is on-line.

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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

SR. No Parameters Frequency of analysis

1 Product alcohol concentration Every one Hour

2 Regeneration ethanol proof Every two Hours

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3.0.5 PROCESS PARAMETERS


A) FLOW:
A.1) Corn feed stock:

SR.NO. PARAMETER TAG NO. UNIT VALUE


Alcohol water liquid to Vaporizer Flash
1 FQI-160101 Lit/hr 9200
Tank (T-1603).
Low Pressure Steam to Vaporizer
2 FQIC-160103 kg/hr 2812
Reboiler (H-1601)
Medium Pressure Steam to Superheater
3 FQI-160201 kg/hr 315
(H-1602)
Regeneration liquid to Rectifier Column
4 FQIC-160207 Lit/hr 2180
(C-1461)
5 Dehydrated ethanol Liquid to Storage FQI-160301 Lit/hr 6400

6 Regeneration liquid to J-1601 FQI-160302 Lit/hr 42000

7 Cooling water supply header to MSDH FI-160303 Lit/hr 370000

A.2) Sorghum feed stock:

SR.NO. PARAMETER TAG NO. UNIT VALUE


Alcohol water liquid to Vaporizer Flash
1 FQI-160101 Lit/hr 8590
Tank (T-1603).
Low Pressure Steam to Vaporizer
2 FQIC-160103 kg/hr 2625
Reboiler (H-1601)
Medium Pressure Steam to Superheater
3 FQI-160201 kg/hr 292
(H-1602)
Regeneration liquid to Rectifier Column
4 FQIC-160207 Lit/hr 2035
(C-1461)
5 Dehydrated ethanol Liquid to Storage FQI-160301 Lit/hr 5973

6 Regeneration liquid to J-1601 FQI-160302 Lit/hr 39200

7 Cooling water supply header to MSDH FI-160303 Lit/hr 345330

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B) PRESSURE:
SR.NO. PARAMETER TAG NO. UNIT VALUE
1 Vaporiser pressure control PIC-160201 Kg/cm2 (a) 1.7

2 Bed A top pressure PI-160204 Kg/cm2 (a) 0.14*/1.7

3 Bed A bottom pressure PI-160205 Kg/cm2 (a) 0.14*/1.7

4 Bed B bottom pressure PI-160206 Kg/cm2 (a) 0.14*/1.7

5 Bed B top pressure PI-160207 Kg/cm2 (a) 0.14*/1.7

6 Differential Pressure across Bed A PDA-160205 Kg/cm2 (a) 0.1

7 Differential Pressure across Bed B PDA-160206 Kg/cm2 (a) 0.1

8 Seave Bed Pressure control PIC- 160204 Kg/cm2 (a) 1.7

9 T-1601 pressure PIC-160301 Kg/cm2 (a) 1.6


* Pressure during regeneration cycle

C) TEMPERATURE:

SR.NO. PARAMETER TAG NO. UNIT VALUE


1 Vaporizer vapors to H-1602 TI-160101 0C 93

2 Feed pre heater outlet temperature TI-160102 0C 88

3 Sieve Bed B Temperature TI-160201 0C 120

4 Sieve Bed A Temperature 0C 120


TI-160202
5 Sieve Bed A Temperature 0C 120
TI-160203
6 Sieve Bed A Temperature TI-160204 0C 120

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7 Sieve Bed A Temperature TI-160205 0C 120

8 Sieve Bed B Temperature TI-160206 0C 120

9 Sieve Bed B Temperature TI-160207 0C 120

10 Sieve Bed B Temperature TI-160208 0C 120

11 Superheater outlet Temperature TI-160209 0C 120

12 Regeneration liquid to distillation TI-160210 0C 65

13 Final product to storage TI-160301 0C


34

D) LEVEL:

SR.NO. PARAMETER TAG NO. UNIT VALUE


1 Vaporizer level LIC-160101 % 20

2 Steam condensate tank level LIC-160102 % 50

3 Regeneration Receiver Level LI-160301 % 50

4 Product Receiver Level LIC-160302 % 50

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E) SIEVE SEQUENCE PARAMETERS:


SR.NO. PARAMETERS TAG NO. UNIT VALUE

1 Maximum purge position Tmax Sec 15-20

2 Minimum purge position Tmin Sec 12-20

3 Bed A maximum purge position Pmax1 % 10-20

4 Bed A minimum purge position Pmin1 % 5-11

5 Bed B maximum purge position Pmax2 % 10-20

6 Bed B minimum purge position Pmin2 % 5-11

7 Main cycle time Tmc Sec 300

8 Vacuum release time Tvr Sec 10-20

9 Equalization time Teq Sec 10-20

10 Vacuum development time Tvd Sec 30-50

11 Equalisation factor Feq - 0.45

12 Equalisation purge position Peq % 40-70

13 Vacuum development ramp initial value RAMP_INITIAL % 0

14 Vacuum development ramp target value RAMP_TARGET % 100

15 Ramp time RAMP_TIME sec 40-50

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

Sr. No. Trouble Cause Corrective Action


1 No / low feed F-1601 clogged. Change over filter and Clean the
to Vaporizer filter.
Flash Tank Level control valve (LCV- Check and resolve the problem of
(T-1603) 160103) malfunctioning. Level control valve (LCV-160103).
2 High level in F-1602 clogged Change over filter and Clean the
Regeneration filter.
Receiver Low regeneration flow to Increase regeneration flow set
(T-1602) Rectifier Column (C-1461) point through FQIC-160207.
Regeneration Cooler (H- Clean Regeneration Cooler (H-
1607) clogged 1607).

3 High pressure PCV-160201& PCV-160202 Check valve feedback. Attain


of Vaporizer malfunctioning PCV-160201& PCV-160202.
Flash Tank High level in Vaporizer Ensure Vaporizer level through
(T-1603) LIC-160101.
Restriction for alcohol Ensure pressure setting for sieve
vapor flow through bed & Vaporizer thorough PIC-
Molecular Sieve I/II (V- 160204. Ensure pressure at local
1601A/B) pressure gauges on Molecular
Sieve.
Cooling water failure Ensure cooling water flow
through FI-160303.
High LP Steam flow Ensure & decrease Low Pressure
Steam flow through FQIC-160103.

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Sr. No. Trouble Cause Corrective Action


4 Low High level in Ensure Vaporizer level through
temperature of Vaporizer LIC-160101.
Superheater (H- Low Low Pressure Ensure proper steam flow and
1602) outlet Steam flow / pressure through FQIC-
pressure to 160103/PI-160101.
Superheater (H-1602)
Temperature Check and resolve the problem of
Control valve (TCV- Temperature Control valve (TCV-
160209) 160209).
malfunctioning
5 High pressure Cooling water Ensure and increase cooling water
during temperature high / flow through FI-160303. Ensure
regeneration flow low performance of Cooling Tower.
cycle Regeneration Cooler Clean Regeneration Cooler (H-
(H-1607) clogged 1607).
High Performance Check and resolve the problem of
Valve High Performance Valve.
malfunctioning.
More purging rate Ensure and decrease the purging
rate through FCV-160206 / FCV-
160205.
Air leakages Attain air leaks

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Sr. No. Trouble Cause Corrective Action


6 High moisture in Low alcohol water Ensure alcohol water liquid
final product liquid concentration in concentration by laboratory
feed to Vaporizer analysis.
Flash Tank (T-1603)
Less vacuum during Refer point no.5
regeneration cycle
Low / very high Ensure and correct the purging
Purging rate rate by monitor the regeneration
flow (FQIC-160207) to
distillation section.
Low temperature of Refer point no.4
Superheater outlet
7 High Cooling water Ensure and increase cooling
temperature of temperature high / water flow through FI-160303.
product flow low Ensure performance of Cooling
Tower.

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PART–IV

PROCESS SHUTDOWN
AND
PROCESS START-UP

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4.0 GENERAL INSTRUCTIONS


Short duration shutdown happens because of some breakdown or some emergency
or failure of any input to the Process plant like Low Pressure Steam/Medium
Pressure Steam, cooling water, power, instrumental air, Process water etc. Logic is
that after short duration shutdown it is necessary to go upon normal capacity and
stabilize the process in short time. Better shutdown planning can optimise the
breakdown time and increasing productivity.
It may not be possible to cover all the possibilities of short duration shutdown here
but it is operator’s skill and emergency planning technique to handle the situation
and recover fast and safe. Operator must give highest priority to ‘SAFETY’.

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4.0.1 POWER FAILURE

1. Inform concern section regarding the stoppage of Low Pressure Steam/Medium


Pressure steam in Dehydration section.
2. Put Vaporizer Flash Tank (T-1603) Level Control Loop, (LIC-160101) will be
forced to MAN mode with output 0%,
3. Put Low Pressure Steam Control Loop (FQIC-160103) to Vaporizer Reboiler (H-
1601) in MAN mode and close it to zero.
4. Put Medium Pressure Steam Control Loop (TIC-160209) on steam line to
Superheater (H-1602) in MAN mode and close it to zero.
5. 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%).
6. Put Flow control Loop (FQIC-160207) on Alcohol water liquid from
Regeneration Receiver (T-1602) to Rectifier Column (C-1461) in MAN mode and
close it to zero.
7. Put Level control Loop (LIC-160302) on Product Receiver (T-1601) in MAN
mode and close it to zero.
8. Put Level control Loop (LIC-160102) on Steam Condensate Tank (T-1604) in
MAN mode and close it to zero.
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 power failure actions to be taken by operator / DCS
sequence without time delay.

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Start-up after resumption of power


1. Ensure electrical power is available.
2. Ensure DCS Control system is ready for start-up.
3. Ensure Low Pressure Steam/Medium Pressure Steam is available.
4. Ensure Distillation section is running then start the Dehydration section.
5. Ensure Air Compressor and the auxiliaries and utilities sections are in ready
condition.
6. Ensure cooling water circuit established.
Note: During plant start-up, Dehydration section to be started with 94-95%
v/v alcohol concentration in alcohol water liquid from Aldehyde Recovery
Column (C-1402).
7. Refer dehydration normal start-up procedure for start-up of plant (Refer:
section 3.0.2).
Note: During plant start-up, Dehydration product to be diverted to off-spec
tank. Divert dehydrated ethanol liquid to ethanol storage tanks after
confirmation of quality.

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4.0.2 COOLING WATER FAILURE


1. The failure of cooling water supply in Dehydration Section will increase the
temperature and pressure. Dehydration section will be stopped through DCS.
2. At the time of cooling water failure, the vacuum during regeneration cycle as
well as pressure during adsorption cycle will get disturbed.
3. Inform concern section regarding the stoppage of Low Pressure Steam/Medium
Pressure steam in Dehydration section.
4. Put Vaporizer Flash Tank (T-1603) Level Control Loop, (LIC-160101) will be
forced to MAN mode with output 0%,
5. Put Low Pressure Steam control Loop (FQIC-160103) to Vaporizer Reboiler (H-
1601) in MAN mode and close it to zero.
6. Put Medium Pressure Steam control Loop (TIC-160209) on steam line to
Superheater (H-1602) in MAN mode and close it to zero.
7. 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%).
8. 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).
9. 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).
10. 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-

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1404). During cooling water failure actions to be taken by operator / DCS


sequence without time delay.
Start-up after resumption of cooling water
1. Ensure electrical power is available.
2. Ensure DCS Control system is ready for start-up.
3. Ensure Low Pressure Steam/Medium Pressure Steam is available.
4. Ensure Distillation section is running then start the Dehydration section.
5. Ensure Air Compressor and the auxiliaries and utilities sections are in ready
condition.
6. Ensure cooling water circuit established.
During plant start-up, Dehydration section to be started with 94-95% v/v
alcohol concentration in alcohol water liquid from Aldehyde Recovery
Column (C-1402).
7. Refer dehydration normal start-up procedure for start-up of plant (Refer:
section 3.0.2).
Note: During plant start-up, Dehydration product is to be diverted to off-spec
tank. Divert dehydrated ethanol liquid to ethanol storage tanks after
confirmation of quality.

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4.0.3 LOW PRESSURE STEAM / MEDIUM PRESSURE STEAM FAILURE

Failure of Low Pressure Steam/ Medium Pressure steam ultimately causes a


stoppage in Dehydration section, although it doesn’t affect Distillation directly.
Since Dehydration section is stopped, alcohol water liquid from distillation is to be
divert to off spec storage tank.
During Low Pressure Steam/ Medium Pressure Steam failure following actions is
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 and
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).
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
type of shutdown.
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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.
Start-up after resumption of Low Pressure Steam /Medium Pressure Steam
1. Ensure Medium Pressure Steam is available.
2. Ensure Low Pressure Steam is available.
3. Ensure electrical power is available.
4. Ensure DCS Control system is ready for start-up.
5. Ensure Distillation section is running then start the Dehydration section.
6. Ensure Air Compressor and the auxiliaries and utilities sections are in ready
condition.
7. Ensure cooling water circuit established.
During plant start-up, Dehydration section to be started with 94-95% v/v
alcohol concentration in alcohol water liquid from Aldehyde Recovery
Column (C-1402).
8. Refer dehydration normal start-up procedure for start-up of plant (Refer:
section 3.0.2).

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Note: During plant start-up, Dehydration product to be diverted to off-spec


tank. Divert dehydrated ethanol liquid to ethanol storage tanks after
confirmation of quality.

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4.0.4 INSTRUMENT AIR FAILURE

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.

Start-up after resumption of Instrument Air


1. Ensure Medium Pressure Steam is available.
2. Ensure Low Pressure Steam is available.
3. Ensure electrical power is available.
4. Ensure DCS Control system is ready for start-up.
5. Ensure Distillation section is running then start the Dehydration section.
6. Ensure Air Compressor and the auxiliaries and utilities sections are in ready
condition.
7. Ensure cooling water circuit established.
During plant start-up, Dehydration section to be started with 94-95% v/v
alcohol concentration in alcohol water liquid from Aldehyde Recovery
Column (C-1402).
8. Refer dehydration normal start-up procedure for start-up of plant (Refer:
section 3.0.2).
Note: During plant start-up, Dehydration product to be diverted to off-spec
tank. Divert dehydrated ethanol liquid to ethanol storage tanks after
confirmation of quality.

THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
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4.1 PLANT SHORT SHUTDOWN AND START-UP AFTER SHORT SHUTDOWN

4.1.1 PLANT SHORT SHUTDOWN

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.

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4.1.2 PLANT START-UP AFTER SHORT SHUTDOWN

1. Ensure Medium Pressure Steam is available.


2. Ensure Low Pressure Steam is available.
3. Ensure electrical power is available.
4. Ensure DCS Control system is ready for start-up.
5. Ensure Distillation section is running then start the Dehydration section.
6. Ensure Air Compressor and the auxiliaries and utilities sections are in ready
condition.
7. Ensure cooling water circuit established.
During plant start-up, Dehydration section to be started with 94-95% v/v
alcohol concentration in alcohol water liquid from Aldehyde Recovery
Column (C-1402).
8. Refer Dehydration section normal start-up procedure for start-up of plant (Refer:
section 3.0.2).
Note: During plant start-up, Dehydration product to be diverted to off-spec
tank. Divert dehydrated ethanol liquid to ethanol storage tanks after
confirmation of quality.

THIS DOCUMENT IS THE PROPERTY OF PRAJ INDUSTRIES LTD., INDIA AND SHOULD NOT BE REPRODUCED WITHOUT WRITTEN
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4.2 Plant Long Duration Shutdown and Start-up after Long Duration Shutdown

4.2.1 Plant 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).
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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 for 8 -12 hrs
for regeneration of Molecular Sieve.
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.
12. After ensuring 8-12 hrs regeneration of Molecular Sieve beds. Close FCV-160203
and FCV-160204.
13. If Distillation is running, transfer possible amount of alcohol water liquid level
from Regeneration Receiver (T-1602) to Rectifier Column (C-1461) and Stop
Regeneration Pump (P-1602A/B).
14. Close cooling water supply to Dehydration section.
Notes: Ensure all tanks / PHEs / lines emptied out completely.
 Isolate all equipment by manual valves.
 If the plant shutdown for long duration it is advisable to drain cooling
waterside of heat exchangers.

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 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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4.2.2 Plant Start-up after Long Duration Shutdown.


1. Ensure Medium Pressure Steam is available.
2. Ensure Low Pressure Steam is available.
3. Ensure electrical power is available.
4. Ensure DCS Control system is ready for start-up.
5. Ensure Air Compressor and the auxiliaries and utilities sections are in ready
condition.
6. Ensure cooling water circuit established.
7. Ensure the valve stroke is completed (Refer: section 2.0.3).
8. Ensure Vacuum trail is completed (Refer: section 2.0.4).
9. Ensure Distillation section is running then start the Dehydration section.
During plant start-up, Dehydration section to be started with 94-95% v/v
alcohol concentration in alcohol water liquid from Aldehyde Recovery
Column (C-1402).
10. Refer Dehydration section Cold Start-up Procedure for start-up of plant (Refer:
section 3.0.3).

------XXXX-------

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