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A Report on:
Distillation Section: An in depth study of most crucial stage in
production of extra neutral alcohol in a distillery
By:
Nidhi Jaiswal
MBA Tech Chemical Engineering
Duration: 1st May 2019 – 22nd June 2019
Rajasthan Liquors Limited
1
A REPORT ON
Distillation section: An in depth study of most crucial stage in the
production of extra neutral alcohol in a distillery
By
Nidhi Jaiswal
L009
Distribution List:
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ACKNOWLEDGEMENT
I would like to express my sincere gratitude to all the mentors who helped provide me
with the opportunity to work on this project. I would like to extend my sincere &
heartfelt appreciation towards one and all who have helped me in this endeavor.
Without their constant guidance, help, support, cooperation, motivation and
encouragement, the difficulty levels of the project would’ve been insurmountable.
I would like to mention a special thanks to my project mentor, Mr. Pavan Kumar
Dubey, who has taken great efforts in involving me in multiple everyday plant
operations and has guided and monitored my everyday progress. Without his constant
help and guidance completing the primary project on distillation section would not
have been possible. I would also like to extend my sincere thanks to Mr.Vivek, who
has taught and guided me on the various methodologies required for lab analysis. I
shall remain indebted to Mr. Ravi Kumar Rana who has allowed me to intern at
Rajasthan liquor limited. I am extremely thankful to all the Production, Human
Resources, Maintenance, Safety, Utility and QA personnel for their valuable guidance
and support and aiding me throughout the project tenure. I am grateful to the entire
team at Rajasthan liquor limited for having allowed me this enriching opportunity and
for their day to day support and giving me access to resources that I required for the
project.
The first big step for any venture / project is opportunity. I would like to thank my
college, Mukesh Patel School of Technology Management and Engineering, NMIMS
for giving me this opportunity and allowing me to pursue my technical internship
program at Rajasthan liquor limited.
Request the concerned to overlook any omission in this brief acknowledgement. This
is only inadvertent and not by design. I remain grateful to all concerned for the help
and support in completing the projects successfully.
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INDEX
I. ACKNOWLEDGEMENT .................................................................................................. 5
II. ABSTRACT ...................................................................................................................... 10
III. ABOUT THE COMPANY ............................................................................................... 11
IV. ABOUT THE PRODUCTS .............................................................................................. 13
V. ABOUT THE BYPRODUCTS ........................................................................................ 13
VI. OVERVIEW OF THE PLANT ........................................................................................ 14
VII. PROCESS BLOCK DIAGRAM....................................................................................... 14
➢ GRAIN HANDLING AND MILLING SECTION .................................................... 15
➢ LIQUEFACTION AND FERMENTATION SECTION............................................ 15
➢ MULTI-PRESSURE DISTILLATION SECTION .................................................... 18
➢ DRIER & DECANTER SECTION ............................................................................ 20
➢ CARBON DIOXIDE AND DRY ICE PRODUCTION SECTION ........................... 21
➢ BOILER AND POWER PLANT SECTION .............................................................. 22
VIII. IN DEPTH STUDY OF DISTILLATION PROCESS OF THE PLANT ........................ 30
➢ HISTORY OF DISTILLATION................................................................................. 30
➢ DISTILLATION ......................................................................................................... 30
➢ MULTI PRESSURE DISTILLATION....................................................................... 31
➢ DEFINITIONS INVOLVED IN PROCESS .............................................................. 31
➢ UTILITIES STUDY ................................................................................................... 34
➢ PRODUCT PROPERTIES ......................................................................................... 35
➢ EXTRA NEUTRAL ALCOHOL .............................................................................. 35
➢ RECTIFIED SPIRIT ................................................................................................... 36
➢ FUSEL OIL................................................................................................................. 37
IX. DISTILLATION FLOW DIAGRAM............................................................................... 38
➢ ANALYSER COLUMN ............................................................................................ 38
➢ PRE-RECTIFIED COLUMN ..................................................................................... 39
➢ EXTRACTIVE DISTILLATION COLUMN............................................................ 40
➢ RECTIFIED COLUMN ............................................................................................. 41
➢ SIMMERING COLUMN .......................................................................................... 42
➢ RECOVERY COLUMN ............................................................................................ 43
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X. PROCESS DESCRIPTION .............................................................................................. 44
➢ ANALYSER COLUMN ............................................................................................. 44
➢ PRE RECTIFIER COLUMN ...................................................................................... 46
➢ EXTRACTIVE DISTILLATION COLUMN (E.D.)................................................. 48
➢ RECTIFIED COLUMN(R.C.) .................................................................................... 49
➢ RECOVERY COLUMN ............................................................................................. 50
➢ SIMMERING COLUMN: .......................................................................................... 51
XI. OTHER IMPORTANT EQUIPMENT: ............................................................................ 52
➢ FLASH TANK ............................................................................................................ 52
➢ ALCOHOL SCRUBBER ........................................................................................... 53
➢ PRESSURE CONTROL VALVE .............................................................................. 53
➢ PUMPS ....................................................................................................................... 53
➢ CLEANING PROCESS .............................................................................................. 62
➢ INSULATION: ........................................................................................................... 63
XII. INSPECTION OF VESSELS: .......................................................................................... 63
➢ VACUUM TEST: ....................................................................................................... 63
➢ WATER TRIAL RUN: ............................................................................................... 65
XIII. SCADA( SUPERVISORY CONTROL OF THE DISTILLATION PLANT) ................. 68
➢ ANALYSER COLUMN ............................................................................................. 69
➢ PRE-PRECTIFIER COLUMN ................................................................................... 72
➢ EXTRACTIVE DISTILLATION COLUMN............................................................. 73
➢ RECTIFIER COLUMN .............................................................................................. 74
➢ RECOVERY COLUMN ............................................................................................. 75
➢ SIMMERING COLUMN ........................................................................................... 76
XIV. ADVANTAGES OF MULTIPRESSURE DISTILLATION UNIT: ............................... 77
XV. LAB TESTING FOR RAW MATERIAL AND DISTILLATION UNIT PRODUCTS . 78
➢ TEST 1: ALCOHOL STRENGTH IN EXTRA NEUTRAL ALCOHOL.................. 78
➢ TEST 2: ALCOHOL STRENGTH IN EXTRACTIVE DISTILLATION BOTTOMS
WHICH ARE BEING SEND TO RECTIFIER COLUMN. ...................................... 79
➢ TEST 3: ALCOHOL STRENGTH IN EXTRACTIVE DISTILLATION TOP
VAPOURS WHICH ARE BEING SENT TO RECOVERY COLUMN. .................. 79
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➢ TEST 4: ALCOHOL STRENGTH IN LIGHT FUSEL OIL FROM RECTIFIER
COLUMN. .................................................................................................................. 80
➢ TEST 5: ALCOHOL STRENGTH IN HEAVY FUSEL OIL FROM RECTIFIER
COLUMN. .................................................................................................................. 81
➢ TEST 6: ALCOHOL STRENGTH IN REFLUX OF RECTIFIER COLUMN. ........ 82
➢ TEST 7: ALCOHOL STRENGTH OF REFLUX OF PRE RECTIFIER COLUMN. 83
➢ TEST 8: ALCOHOL STRENGTH IN RECTIFIED COLUMN DRAW. .................. 83
➢ TEST 9: FUSEL OIL TEST IN FINAL PRODUCT .................................................. 84
➢ TEST 10: LOSS OF ALCOHOL IN THE PROCESS OF OBTAINING E.N.A. ...... 84
➢ TEST 12: POTASSIUM PERMANGANATE TEST. ............................................... 86
XVI. WEEKLY REPORT ......................................................................................................... 88
➢ REPORT 1: INTRODUCTION TO THE FACTORY ............................................... 88
➢ REPORT 2: PROCESS FLOW FROM MILLING SECTION TO DISTILLATION
INCLUDING BYPRODUCT FORMATION ............................................................ 90
➢ REPORT 3 : STUDY ON 1ST THREE COLUMN ................................................... 92
➢ REPORT 4: STUDY ON THE LAST THREE DISTILLATION COLUMN ........... 94
➢ REPORT 5: LAB ANALYSIS ................................................................................... 95
XVII. REFERENCES ................................................................................................................. 96
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LIST OF TABLES
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ABSTRACT
Rajasthan liquors limited (RLL) is a grain based distillery at the cited location
in Derabassi, Punjab, thereby diversification towards new development and
market penetration by new product. This distillery is major producer of Extra
Neutral Alcohol along with rectified spirit, technical or impure alcohol. Major
by products are carbon dioxide and distilled dried grain with soluble (DDGS/
cattle feed).
Major product of the company is extra neutral alcohol i.e. purified grade of
ethyl alcohol. The E.N.A. produced is of strength 96% v/v. To achieve this
strength and quantity per day a multi pressure distillation section having 6
columns has been set up in the plant. The project aim is to analyse and study
the whole distillation section separately and prepare a study report
accordingly. Physical, chemical and operating conditions need to be outlined.
Along with this I need to work on the problems which can arise in the section
with appropriate solutions for the same.
The study of the products which are being produced , equipment description,
process flow diagram, process flow description, cleaning process, insulation,
material of construction and other major equipment used other than the 6
columns need to be defined.
The study also included inspection of vessel tests, lab analysis of all the
products being produced, and time to time recording results for the same, along
with importance of result. Simultaneously study of the properties of the column
product has been done
Apart from this key accomplishment achieved was through the training and
understanding at every stage in the distillation process. This understanding has
added enormously to the technical knowledge gained at college. The chemical
process involved in the various stages in the distillation process used by the
organization has been studied and the finer details analysed.
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ABOUT THE COMPANY
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distillers, we are committed to achieve our vision by contribution through hard
work, commitment and honesty.
RLL has also installed a 120 Kilo Litre per day (KLPD) Grain based Distillery at
the above cited location in Derabassi, Punjab, thereby diversification towards
new development and market penetration by new product.
RLL, a top brand amongst the Indian IMFL bottler, is a company whose
promoters have more than 20 years’ experience in Liquor industry and belongs to
a leading group of distribution and retailing business of Liquor having
nationwide network in India. We are committed towards the vision of the
company which compels us to make RLL a leading liquor company in India. The
company has set its mission by defining the goals and objectives to achieve its
vision and continual developments thereof.
Our Vision!!!
“To be the preferred and leading Liquor Industry”
Our Mission!!!
“ To boost business, by providing quality product using state of the art
technology and methodology with minimum
exploitation of natural and energy resources
focusing more on environmental status. ”
Our Quality Product!!!
“We, at Rajasthan liquors Limited are committed
to customer Satisfaction through on time delivery
of cost effective quality products by continual
improvement of processes and skills of our
Employees.”
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ABOUT THE PRODUCTS
1. ENA: extra neutral alcohol is a clear, colorless, flammable liquid that has
been distilled from the grain based mash to a very high concentration of
ethanol. The word neutral refers to lacking of flavor. Used to manufacture
whisky. Ethanol v/v in the liquid is 96%.
2. RS: rectified spirit is ethyl alcohol of agricultural origin with high
concentration of ethanol which is purified with the means of repeated
distillation called rectification. A neutral spirit with the strength of 95.6%.Used
in manufacturing of blended whisky, cut brandy and some bitters.
3. Fusel oil: A mixture of volatile oily liquids having pungent smell and taste,
produced during alcoholic fermentation. They are considerable less volatile
than alcohol. A simple distillation with steam usually results in their complete
carry over in to the distillate, but in rectification to produce a high proof product
allow the separation of fusel oil.
4. SDS: Denatured alcohol is ethanol that has additives make it poisonous,
extremely bad tasting, and foul smelling to discourage recreational
consumption. It is used as solvents and as fuel for alcohol burners. In some
cases it is also dyed. It is used as solvent or as fuel for alcohol burner or
camping stoves.
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OVERVIEW OF THE PLANT
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1) GRAIN HANDLING AND MILLING SECTION
The broken rice i.e. raw material coming to the factory is sent for storage to 3
silo tanks. The tanks storage capacity is about 9000 metric ton. From here grain
is passed via belt conveyer to chain conveyer and via elevator bucket to the
grain buffer bin.
Grain is fed to the 3 classifier for separation of oversize and undersize particles.
Classifier are sieve type classifier with 2 sieve trays. The top tray sieve size is
5.5mm whereas bottom tray size is 0.5mm. Undersize particles are sent to
destoner for the removal of stones present in the grain. Destoner is a 14 mesh
machine. After removal of stones grain is sent to buffer bin for storage.
From the buffer bin grain is fed to the flour mill. Flour mill is a hammer mill
with 48 hammers running at 1400 rpm with sieve size 2.5mm. It is used to grind
rice to flour. Flour is fed to the conveyer belt and then passed through sieving
machine of size 2.5 mm. The oversize particles are fed back to the flour mill
whereas undersize particles passed through bucket elevator to conveyer belt to
flour silo.
From flour silo flour is passed through flour screw conveyer and then to
weighing scale. Approximately 9702 kg per hour flour is weighed and the
passed to liquefaction section.
On top of both the destoner blower is connected. It sucks in the dust particles
and feed it to the cyclone separator. In cyclone separator air is passed and it
separated dust particles from the air. Blower – cyclone system helps to prevent
dust accumulation which may pollute the grain.
15
Initial liquefaction tank is filled with slurry. The temperature of the tank is
maintained at 88-90oC. To maintain the temperature low pressure steam is
passed through the tank. For the conversion of starch to sugar alpha amylase
approximately 30% is added from enzyme tank 1. In ILT around 22% starch
and 5% sugar is produced.
The contents from here are pumped through jet cooker. In jet cooker
temperature of the contents is raised to 112 to 120oC and a pressure of around
7.5kg/cm2 is build up. As the slurry is pumped, at the same time steam at
7.5kg/cm2 is pumped in too. Jet cooker is used for starch liquefaction into
glucose and fructose production. Jet cooker also helps in opening of starch
molecule and gelatinization of starch.
He gelatinized liquid is fed to the retention vessel. There it is kept for around 5
to 10 minutes. Here pressure is reduced to around 2.5 kg/cm2 and temperature
to around 108 -110oC. It is used for conversion left over starch to sugar.
Cooked slurry is flashed in the flash tank; this reduces the temperature of slurry.
The vapours coming out from the flash tank are sent to the condenser and the
condensate is sent to the hot water tank. Here the slurry is kept for around 2 to 5
minutes.
From flash tank flash slurry is fed to the final liquefaction tank. Here 70 to 75%
enzyme is added which is prepared in the enzyme tank. The temperature of the
tank is maintained at 85oC. FLT tank has approximately 10 to 15% starch and
5% sugar.
Yeast vessel is being used to metabolize dry inactive yeast to active state. This
is done by feeding the vessel with dry yeast, processed water, air, enzyme (beta
amylase) and some source of nitrogen along with catalyst alcozyme. The yeast
vessel is internally cooled to maintain the temperature of vessel around 34-
35oC. It takes around 6 hours for once batch to get activated.
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Pre-fermentor is a tank with volume 19.5 kiloliters. It is used for preparation of
wash before sending it to fermentation tank. With the presence of pre-fermentor
tank, the time tank for the fermentation to complete gets eventually reduced.
Feeding of the tank is done by using 12 liters of enzyme( beta-amylase) ,
catalyst( alcozyme) approx. 1 kg , wash from FLT is taken , air is in continuous
circulation and yeast from yeast vessel is taken once matured as well as some
quantity of dry yeast.
The yeast vessel and the pre-fermenter are made ready before the dosing is done
to the fermentation tank. The materials from both yeast vessel and pre-
fermenter are transferred to the fermentation tank along with continuous input
from the Final Liquefaction Tank. The temperature in the fermentation tanks
should not exceed 35oC. The total time which is required to fill up the fermenter
is approximately around 22 to 24 hours. After this the slurry is kept in the
fermenter for 12 to 13 hours for the reaction to take place. The total time
required from the filling to the reaction to get completed is 38 hours.
After 30-34 hours sample is taken and tested to check the gravity of wash. If
gravity of wash is decreased to 1.000 it signifies completion of the reaction/
fermentation process if not then wash need to be kept in tank for more time. In
fermentation tank around 49% carbon dioxide is produced which is sent to
carbon dioxide plant for processing as it is a valuable by-product.
After the gravity in the fermenter drops to 1.000 the contents are passed to beer
well for storage. The bell has a top mounted agitator which is in continuous
motion so that the solid particles do not settle down and remain suspended in
the wash.
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nC6H10O5 + nH2O nC6H12O6
(Starch) (Glucose)
C6H12O6 2C2H5OH + 2CO2
(Glucose) (Ethanol)
Fermented wash from beer well is fed to the top of the degassifier column.
Alcoholic vapours approximately 45-50% sent to 1st multiple effect evaporators
from where condensate is sent to the PRC feed tank. The distillate comprising
of left over impure alcohol is sent to the alcohol scrubber via passing through 3
condensers. The bottoms comprising of spent wash is sent to the decanter for
production of DDGS and thin slope. Column doesn’t have any reboiler.
The contents from PRC feed tank is feed to the pre-rectifier column. The cut of
light fusel oil and heavy fusel oil is taken from plate 17/18, 15 respectively.
Rectified spirit of strength 95% is drawn from plate 51. Distillate comprising of
vapours is sent to the simmering and extractive distillation reboiler for heating
the column. The spent wash from bottom is sent to liquefaction section.
The rectified spirit drawn from PRC is fed to extractive distillation column.
Demineralizes water and spent wash from rectified column is fed to the column
on top most tray. The bottoms with the strength of 14% alcohol is passed
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through plate type heat exchanger and then to the rectified column. Distillate
has 7% impure alcohol passed through 3 condensers then to alcohol scrubber.
PRC vapours are fed to the reboiler to supply heat to the column.
The bottoms from E.D. column are fed to the rectified column on plates 14 to
18. Light fusel oil and heavy fusel oil are drawn from plate 10 and 17 to 22
respectively. Vapours as distillate fed to flash tank reboiler. Steam is passed
through R.C. reboiler to supply heat to the column and maintain the pressure of
column. The bottoms i.e. spent lees is sent to cooling tower. The extra neutral
alcohol with other lighter alcohol is drawn from plate 70 and fed to simmering
column.
Rectified column drawn and rectified spirit is fed to the simmering column.
Vapours containing impure or technical alcohol are passed through the 3
condensers whereas E.N.A. 96% v/v strength is collected as bottoms and sent
for storage. PRC vapours are fed to the reboiler to supply heat to the column.
Rectified column fusel oil and E.D. top vapours are fed to the recovery
column. Flash steam is fed to the bottom tray to heat up the column. A low
grade RS (rectified spirit) is drawn from plate 45 and larger portion is refluxed
back whereas smaller portion is sent to the PRC feed tank. The vapours are
passed through the 2 condenser. From the 2nd condenser trial or technical
alcohol is obtained which is sent to warehouse for packing. Bottom or lees is
taken out from bottom and sent to spent wash tank.
Apart from this section has alcohol scrubber. Condensate from 3 rd E.D.
condenser, 2nd degassifier condenser and analyser vent condenser are fed to the
scrubber from bottom and water from the top. Water absorbs left over alcohol
and sent to PRC feed tank where as other insoluble impurities vented out.
Vacuum pump is attached to the alcohol scrubber from here only the vacuum
in the analyser column, degassifier column and extractive distillation column is
achieved.
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4) DRIER & DECANTER SECTION
In this section one of the main by product is formed i.e. DDGS (Dried Distillers
Grains with soluble). Feed i.e. bottoms from analyser column are fed to the
three decanter. The liquid and solid are separated. The liquid is the thin slope
fed to the multiple effect evaporators for further production of thick slope
which can be recycled in the plant. The solids are called wet cake.
The wet cake is sent to the ribbon mixer through a conveyor belt. The ribbon
consists of outer and inner helical agitator. The outer ribbon moves material in
one direction and inner ribbon moves material in opposite direction. Thick
slope is also added in the mixer which ensures better mixing.
The contents are passed through the distributor to the double shaft mixer. The
contents are mixed to decrease the amount of moisture in the cake.
Approximately 30% cake from drier is fed to the double shaft mixer for
recycling. After the mixing the contents are passed through the feed screw
conveyor to the drier.
There are 2 drier installed in the plant. They are operated at around 60-65oC
temperature and at about 65-70% capacity. It is a tube bundle drier with 600
tubes and for heating steam is supplied to the drier. After the wet cake is dried
the dried cake is fed to the hopper tank from where dust particles are removed
by the help of cyclone dust remover which is attached on the top of hopper
tank. The dust particles are recycled back to the double shat mixer.
From the hopper contents are passed through the silo tank. Here temperature is
reduced to 60oC. From here they are sent to the hammer mill. In the mill the
solid accumulated particles are broken down into powder form. The hammer
mill contains 72 hammers and run at a speed of around 1200-1400rpm.
The particles are the main byproduct DDGS stored in hopper tanks at room
temperature.
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5) CARBON DIOXIDE AND DRY ICE PRODUCTION
SECTION
Carbon dioxide from fermentation tank is passed through a pipe and fed to the
bottom of water scrubber. Water is fed from top it absorbs the impurities and
takes the solid particles which are drained out, whereas carbon dioxide being
insoluble in water is collected from top and fed to the foam trap at a pressure of
about 0.05kg/cm2.
The pure carbon dioxide gas is passed through a blower to increase it’s pressure
to 0.5kg/cm2. From here gas is fed to low pressure scrubber.
The low pressure scrubber helps to remove bulk water soluble impurities. The
temperature of gas is reduced to 40oC. The gas is passed through moisture
separator. The plates are present in zigzag manner. The moisture picked up by
gas from the scrubber is removed when gas strikes the plates as the heavy
molecules get settled down whereas gas keeps on moving in the upward
direction. The moisture free gas is fed to the multistage compressor.
1st stage
2nd stage
3rd stage
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Outlet pressure: 16 kg/cm2
After each compressor there is moisture separator and a heat exchanger. From
the final stage gas leaves at temperature of around 20oC. The gas coming out at
16 kg/cm2 is passed through high pressure scrubber. The remaining impurities
are removed and pure gas is fed to activated carbon filters for removal of traces
of oil and odour. There are 2 activated carbon filters installed. One is under
process will other one under regeneration. For around 150 hours 1 filter can
work without any disturbance then it undergoes regeneration.
The odour and oil free gas is passed through a plate type heat exchanger to
reduce the temperature of the gas from 38oC to 6oC. This gas is passed through
the dries to remove water molecules. This gas is passed through a chiller unit
which is a shell and tube heat exchanger. Carbon dioxide is present on the tube
side where as liquid ammonia is present on the shell side. The gaseous carbon
dioxide is converted into liquid carbon dioxide and sent for storage. The
temperature of liquid carbon dioxide which is stored is about -32oC.
Liquid carbon dioxide held under pressure (300 psi) in bulk storage vessels. Is
sent through an expansion valve into an empty chamber where under normal
atmospheric pressure it flashes into C02 gas. This change from liquid to gas
causes the temperature to drop quickly. About 46% of the gas will freeze into
dry ice snow. The rest of the C02 gas is released into the atmosphere or
recovered to be used again. The dry ice snow is then collected in a chamber
where it is compressed into blocks. Then it is kept at -180 degree Celsius.
22
district heating, or for desalination of water as well as delivering electrical
power.
BOILER:
Type: Water tube and internally fired boiler.
Pressure: 46 kg/cm2
Capacity: 36 TPH
The four main circuits come across in any thermal power plant are:-
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Air and Gas Circuit
Air from the atmosphere is directed into the furnace through the air preheater by
the action of a forced draught fan. Forced Draught Fan helps for proper
Combustion of fuel and increases combustion Efficiency of Boiler. The exhaust
gases from the Furnace, heat the air, in air preheater, Feed Water in Economizer
and their remaining Ash Particles are collected in ESP and is finally let off into
the environment through Chimney with the help of Induced Draught Fan.
All these circuits are integrated to form a thermal power plant that generates
electricity to meet our Electrical and Steam demands.
24
TURBINE:
Steam generated from the boiler is admitted to the turbine, this heat energy is
converted into mechanical energy and further this mechanical energy is
converted in electrical energy with the help of alternator and then this energy is
used for the operation in the plant.
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PLATE TYPE HEAT
EXCHANGER-2
CAPACITY- 40KL/HR
4 FERMENTER MAKE – PRAJ
PRE-FERMENTOR-1
CAPACITY-192000L
YEAST VESSEL -1
CAPACITY-20KL
FERMENTOR TANK-3
CAPACITY-1000KL
BEER WELL-1
CAPACITY-1000KL
5 DISTILLATION MAKE PRAJ
PRODUCTION CAPACITY-
120KLPD
TOTAL 7 COLUMNS
1) DEGASSIFIER
COLUMN
2) ANALYSER COLUMN
3) PRE-RECTIFIER
COLUMN
4) EXTRACTIVE
DISTILLATION
COLUMN
5) RECTIFIER COLUMN
6) SIMMERING COLUMN
7) RECOVERY COLUMN
6 EVAPORATION MAKE PRAJ
EVAPORATION DUTY-
454M3/HR
NO. OF EFFECTS-4
TYPE OF EFFECT- FALLING
FILM
7 DECANTER MAKE-ALFA
26
TYPE-CENTRIFUGE
NO. OF DECANTER-4
CAPACITY-15 M3/HR (EACH)
8 DRYER MAKE-PRAJ
TYPE- TUBE BUNDLE
NO. OF DRYER-2
CAPACITY-40MT EACH
28
6 FERMENTATION MAKE- PAHARPUR
COOLING COOLING TOWER
TOWER SERVICES
CIRCULATION RATE-750
m3/hr
HOLDING CAPACITY-200
m3
7 TURBINE MAKE- MIHIR COOLING
COOLING TOWER
TOWER
CIRCULATION RATE-125
m3/hr
HOLDING CAPACITY-15
m3
8 CO2 COOLING MAKE- MIHIR COOLING
TOWER TOWER
CIRCULATION RATE-220
m3/hr
HOLDING CAPACITY-20
m3
29
IN DEPTH STUDY OF DISTILLATION PROCESS OF THE
PLANT
• HISTORY OF DISTILLATION
The Chinese were believed to have distilled a rice drink as early as 800 B.C. In
Europe the first documented case of alembics being used to distill alcohol as
around 10th century A.D. Early distilled alcohol had medicinal value and
was called “spirited water” because it altered the state of those who drank it. In
Europe, honey was distilled into mead and grapes were distilled into mead and
grape brandy.
In our Indian distilleries before year 2002 used generally atmospheric
distillation system. The year 2002 was a golden year for Indian distilleries for
first time adopting a new technology i.e. “multipressure distillation system”.
The first plant installed in India at shree chatrapati shahu SSK Kagal Dist.-
Kolhapur (Maharashtra) supplied by Praj Industries Ltd.Pune.
In India, molasses or grain based distilleries having so many different
technologies used for fermentation and Distillation, which were helpful for high
efficiency, yield & quality of spirit.
Molasses or grain based fermented wash having so many impurities i.e. low
boiling &high boiling impurities with ethanol. Our main product ethanol is
straightening out by distillation of fermented wash. The quality of ethanol is
decided by how much impure spirit is presented in the spirit and sensory
analysis. The sensory of alcohol is mainly dependent on impurity present in it.
• DISTILLATION
Distillation is the process of separating the components or substances from a
liquid mixture by using selective boiling and condensation. Distillation may
result in essentially complete separation (nearly pure components), or it may be
a partial separation that increases the concentration of selected components in
the mixture. In either case, the process exploits differences in the volatility of
the mixture's components. In industrial chemistry, distillation is a unit
operation of practically universal importance, but it is a physical separation
process, not a chemical reaction
30
• MULTI PRESSURE DISTILLATION
As the name suggest Distillation process are carried out in different pressure i.e.
columns work under vacuum, atmospheric pressure and high pressure. “The
separation of components by cascading of pressure and vacuum concept to
achieve overall steam consumption by means of thermal integration or coupling
of distillation columns”.
1. Distillation
The word distillation is from Latin, “Destillare” which means to drop or to
trickle down .Distillation is a method of separating the components of a
miscible solution, separated on the basis of difference in there boiling point.
Distillation is a process of evaporation and re-condensation used in separating
liquid in to vapour fraction according to boiling point.
2. Reboiler
A device for supplying heat to a distillation column without introducing
live steam. It generally consists of a shell and tube heat exchanger connected to
the base of the column, liquid from the column entering inside the tubes to be
heated indirectly by steam on the shell side.
3. Condenser
A heat exchanger device connected to the vapour discharge pipe of a column to
permit the vapour to the cooled and condensed to a liquid. Condenser is
commonly cylindrical vessels. Containing tubes through water is passed.
4. Distillation column
A vertical cylindrical vessel containing a series of perforated plates or other
contact devices through which vapours may pass to effect a separation of liquid
mixture by distillation.
5. Decanter
Vessel used for the separation of 2 phase liquid. In a fusel oil decanter an upper
fusel oil phase is separated from lower water.
31
6. Cooling tower
This is a tower or other type of structure where air (the heat receiver) circulates
in direct or indirect contact with warmer water (the heat source) to cool the
water. Cooling towers are used in industries to cool the process streams.
7. Pressure
The portion of the condensed overhead vapours returned to a distillation column
to maintain the liquid-vapours equilibrium.
8. Reflux ratio
The ratios of the amount of condensate refluxed to the amount withdrawn as the
product.
9. Boiling point
This is the temperature at which the vapour pressure of a liquid equals the total
pressure of the atmosphere above it. Bubble of vapour can be formed when
vapour pressure slightly exceeds atmosphere pressure.
32
13. Anhydrous alcohol
Anhydrous literally means ‘without water’. The term used for a substance that
does not contain water. Ethanol for fuel use is commonly referred to as
anhydrous, because it has almost all water removed.
14. Heads spirit
Heads term used to describe the impurities produced in ethanol fermentation
that has lower boiling point than ethanol (by distillation).
33
UTILITIES STUDY
1. Soft water/DM water:
Filtered water, free from algae, bacteria, suspended solid, non-corrosive and
commercial zero hardness for soft water.
2. Cooling water:
Cooling water coming at 2kg/cm2 at the inlet water header at the operating
floor. Approximately 60,000ltr/ hr. water is utilized.
3. Steam
Dry, suspended, regulated saturated steam at pressure 3.5 kg/cm2 and
temperature 150oC
Table 4: NORMAL CONSUMPTION FIGURES
FOR ENA
PARAMETERS UNIT PER DAY
FERMENTED Bulk litre(BL) 750000
WASH
STEAM ton 314
SOFT WATER KL 50000
FOR FLASH
TANK AND
ALCOHOL
SCRUBBER
…..ETC
DM WATER TO KL 200
ED COLUMN
WITH SPENT
LESS RECYCLE
COOLING KL 14,400
WATER
CIRCULATION
34
In this plant multi pressure distillation system. The process
utilizes 6 columns, they are-:
➢ Analyser column
➢ Pre-rectifier column
➢ Rectifier column
➢ Extractive distillation column
➢ Recovery column
➢ Simmering column
This system is used in ideal heat integration format in order to reduce the
energy consumption. The analyser and extractive distillation column is used
under vacuum, whereas simmering and recovery column operated under
atmospheric condition. The pre-rectifier and rectifier column is operated under
pressure. Extra neutral alcohol as product is removed from simmering column,
cooled and then transferred to spirit storage section.
PRODUCT PROPERTIES
2) RECTIFIED SPIRIT
Rectified spirit is also known as neutral spirits, rectified alcohol, or ethyl
alcohol of agricultural origin is highly concentrated ethanol which has been
purified by means of repeated distillation, a process that is called rectification.
It typically contains 95% alcohol by volume (ABV) (190 US proof). The purity
of rectified spirit has a practical limit of 95.6 % ABV when produced using
convential distillation processes, because a mixture of ethanol and water
becomes anazeotrope
Neutral spirit is used in the production of blended whiskey, cut brandy, some
liquor, and some bitters. As consumer products, it is almost always mixed with
other beverages to create such drinks as punch, or is sometimes added to
cocktails in place of vodka or rum and is used in Jello shots. Rectified spirits
are also used for medicine tinctures, and as a household solvent. It is sometimes
drunk undiluted.
Table 6 : RECTIFIED SPIRIT PROPERTIES
Parameter Specification
Strength 95.6%
Specific gravity 0.817
Proof 66
Appearance Colourless, volatile liquid
Smell Characteristic odour
Boiling point 78.2oC
Melting point -114oC
Flash point 16.6oC
Solubility - water Miscible in all proportions
36
3) FUSEL OIL
Fusel Oil is a mixture of volatile oily liquids having pungent smell & taste,
produced during alcoholic fermentation. They are considerable less volatile
than alcohol. A simple distillation with steam usually results in their complete
carry over in to the distillate, but in rectification to produce a high proof product
allow the separation of fusel oil. The % of amyl alcohol is 70 to 80%, butyl
alcohol 15 to 20% and 5 to 10% other higher alcohol like Propyl alcohol. This
is produced in the metallic pathway between carbohydrate and amino acids,
generally yield of fusel oil is 0.2% of alcohol produced but it depends on
fermentation cycle. Amyl alcohol gives commercial value. It used as an
industrial solvent for resins, hydraulic fluids, printing ink, several of its esters
are also made commercially amyl acetate for essence.
37
DISTILLATION FLOW DIAGRAM
1) ANALYSER COLUMN
Fermented DEGASIFIER
wash Alcoholic 1st
COLUMN
vapours effect ALCOHOL
evapor SCRUBBER
-ator
GAS
SEPARA
TOR CONDENSATE
ANALYSER
COLUMN
(vac)
PRC FEED
FLASH STEAM TANK
SPENT WASH
TO DECANTER
38
2)PRE-RECTIFIED COLUMN
VAPOURS GO TO
SIMMERING AND E.D.
COLUMN REBOILER
FUSEL OIL
TANK
REFLUX
RECTIFIED
SPIRIT TO
LFO
E.D.
COLUMN
DECANTER
HFO
PRC COLUMN
PRC FEED
(under LIQUID +
pressure) WASHING
ANALYSER WATER FED TO
PRC FEED TANK
VAPOUR
SPENT WASH TO
LIQUEFACTION
SECTION STEAM
REBOILER
CONDENSATE
TO BOILER
39
3) EXTRACTIVE DISTILLATION COLUMN
VAPOURS GO TO E.D.
CONDENSER THEN TO
RECOVERY COLUMN
(vac)
PRC
PHE
VAPOUR
REBOILER
CONDENSATE
TO PRC
REFLUX TANK
PUMPED TO
RECTIFIED
COLUMN FEED
TRAY
40
4) RECTIFIED COLUMN
VAPOURS GO TO
FLASH TANK
REBOILER
REFLUX
ENA TO GO TO RECOVERY
SIMMERING LFO & HFO
COLUMN
COLUMN
RECTIFIED
COLUMN
(under
pressure) E.D. BOTTOM AS
FEED
BOTTOM TO
COOLING TOWER STEAM
REBOILER
CONDENSATE GO
TO BOILER
41
5) SIMMERING COLUMN
VAPOURS
CONDENSER CONDENSER
1 2
REFLUX
CONDENSER
3
R.S DRAWN
ENA FROM RC
SIMMERING TECHENICAL
(R.S.) ALCOHOL
COLUMN
(METHENOL)
(atm)
PRC
VAPOURS
REBOILER
EXTRA NEUTRAL
ALCOHOL (ENA)
GO FOR COOLING PRC REFLUX
THEN TO WARE TANK
HOUSE
PCV (PRESSURE
CONTROL VALVE)
TO REMOVE
IMPURITIES
42
6) RECOVERY COLUMN
CONDENSER 1 CONDENSER
2
TRIAL
REFLUX
ALCOHOL
RECOVERY
R.C. FUSEL OIL
COLUMN
E.D. TOP VAPOUR
(atm)
TO SPENT
WASH
FLASH STEAM
43
PROCESS DESCRIPTION
1. ANALYSER COLUMN
Analyser column strips of all the alcohol from the fermented wash before
discharging the rest of the material as spent wash. Analyser column is operated
under vacuum; vacuum in the column is created by using vacuum pump which
sucks air via alcohol scrubber which is connected to the vent condenser of
degassifier column and analyser column. This is how all the air from the
analyser column is pumped out and vacuum pressure in the column is
maintained at 0.42 to 0.425 kg/cm2.
The analyser column is a tall column with 22 trays. It has a short column with 5
trays mounted on top called degassifier column. This tower is also under
vacuum. The column is called degassifier column.
The fermented wash coming from the beer well is fed on the top most tray of
the degassifier column. The alcoholic vapours are obtained from top tray of
analyser. And fed to 1st effect of multiple effect evaporators. From here
alcoholic condensate is received which is fed to the PRC feed tank whereas
balance vapours are fed to the analyser vent condenser.
The bottoms from the analyser column are fed to the decanter as spent wash.
For manufacturing of DDGS (cattle feed) and thin slope which can be recycled.
The vapour concentration at the top will be in the range of 45-50% w/w.
Alcohol concentration in the top vapours depends upon the alcohol % in the
fermented wash. Analyser column is heated by the flash vapours coming from
flash tank which are fed at the bottom.
44
TABLE 8: TECHNICAL SPECIFICATION OF ANALYSER
COLUMN
1.No. of trays 22 +5(DEGASSIFIER)
2.Type of tray Sieve tray
3.Tray spacing 750mm
4.analyser Column height 19.4m
5.analyser Internal diameter 2150mm
6.Degassifier column height 6.750m
7.Degassifier column internal 1100mm
diameter
6.MOC SS 304
OPERATING PARAMETERS
ANALYSER COLUMN:
DEGASSIFIER COLUMN:
45
2. PRE RECTIFIER COLUMN
Light fusel oil as well as high fusel oil is drawn from PRC column. Light fusel
oil is drawn from plate 17th,18th tray at temperature 106- 107oC. High fusel oil
is drawn from plate 15th and at temperature 108-109OC. The fusel oil water
solution is fed to decanter where water alcohol mixture is separated from fusel
oil. Fusel oil is sent to storage tank whereas water alcohol solution recycled
back to PRC tank.
46
5.Column height 17.1 m
6.MOC SS 304
OPERATING PARAMETERS
% alcohol: 45-50%
Extract % - 94-95%
47
3. EXTRACTIVE DISTILLATION COLUMN (E.D.)
Extractive distillation column is operated under vacuum of 0.5to 0.51 kg/cm2.
Vacuum in the column is created by using vacuum pump which sucks air via
alcohol scrubber which is connected to the vent condenser of extractive
distillation column. This column serves to remove the impurities based on
principle of hydro extraction. Rectified spirit from PRC column is fed to the
extractive distillation column at plate 38 at temperature 70.5 OC and pressure
0.5to 0.51 kg/cm2. Demineralized water and rectified column spent wash
(bottom) is fed to E.D. column on the topmost plate. Whereas vapours from
PRC column are fed to the reboiler to provide heat to the column. The
condensate from the reboiler is sent to PRC feed tank.
The bottoms with 14% alcohol are passed through plate type heat exchanger
and then fed to rectified column. The vapours coming out from E.D. column
containing 7% impurities are passed through the condenser and fed to recovery
column to obtain left over alcohol.
There are 3 condensers for E.D. Column 1st used for beer heating (ferment
wash) 2nd and 3rd are used for condensing its own column vapours and then fed
to recovery column.
48
OPERATING PARAMETER:
4. RECTIFIED COLUMN(R.C.)
Rectified column is a tall column with 72 trays. The E.D. bottoms are fed to the
rectified column on tray 14 to 18 at temperature 113.9oC and pressure
2.2kg/cm2. A small amount of portion of extra neutral alcohol, in the ratio of
1:4.2,is refluxed back where as E.N.A.is drawn from plate 70th temperature
104.5oC and pressure 2.2kg/cm2 and fed to simmering column for the separation
of ethyl alcohol rom methyl alcohol. Vapours are sent to the flash tank reboiler
from where condensate is fed to the flash tank and vapours are sent to the vent
condenser from where technical alcohol or trial alcohol is obtained.
The light fusel oil and heavy fusel oil are drawn from trays 10th and 17th to 18th
plate respectively at temperature 106.5oC & 108.1oC pressure 2.2kg/cm2
respectively.
The LFO &HFO are fed to recovery column to separate ethyl alcohol from
them.
The bottoms or lees is sent to the cooling tower along with the condensate from
the reboiler.
The column is heated by controlled supply of steam at temperature 147.7 oC
&pressure 3.5kg/cm2
49
Table 11:TECHNICAL SPECIFICATION OF RECTIFIED COLUMN
1.No. of trays 72
2.Type of trays sieve tray
3.Tray spacing 250mm.
4.column height 22.4m
5.Column diameter 2050mm
6.MOC SS 304
OPERATING PARAMETERS
Top temperature: 98-102oC
Bottom temperature: 131-132oC
R.C. feed plate: 14 to 18
R.C. feed temperature: 113.9oC
LFO drawn temperature: 106.5oC
LFO drawn plate: 10
HFO drawn temperature: 108.1oC
HFO drawn plate: 17 to 18
5. RECOVERY COLUMN
Recovery column is operated at atmospheric pressure. Feed is from rectified
column and extractive distillation column they are fed on plate 20th & 23rd
respectively. Flash steam is fed to the bottom tray to heat up the column. A low
grade RS (rectified spirit) is drawn from plate 42nd and larger portion is
refluxed back whereas smaller portion is sent to the PRC feed tank
The vapours are passed through the 2 condenser. From the 2nd condenser trial or
technical alcohol is obtained which is sent to warehouse for packing.
Bottom or lees is taken out from bottom and sent to spent wash tank.
50
Table 12:TECHNICAL SPECIFICATION OF RECOVERY COLUMN
1.No. of trays 50
2.Type of trays sieve tray
3.Tray spacing 250mm
4.column height 14.650m
5.Column diameter 750mm
6.MOC SS 304
OPERATING PARAMETERS
6. SIMMERING COLUMN:
Main product of the factory i.e. extra neutral alcohol is obtained from this
column. The column is operated at atmospheric pressure. Here E.N.A from
column is fed at plate 27th at temperature 104oC and at atmospheric pressure.
Rectified spirit is drawn from tray 38th and fed to rectified column; a larger
portion is refluxed back on top most trays.
PRC vapours are supplied to the reboiler for heating the column, condensate is
sent to PRC reflux tank. Vapours are passed through the 3 condensers, technical
alcohol or trial alcohol is obtained from the 3 rd condenser from where it is sent
to warehouse.
51
The main product extra neutral alcohol of strength 96% is drawn from bottom,
cooled and sent to warehouse for packing.
1.No. of trays 50
2.Type of trays sieve tray
3.Tray spacing 250mm
4.column height 15.850m
5.Column diameter 1250mm
6.MOC SS 304
OPERATING PARAMETERS
Bottom temperature:80oC
1. FLASH TANK
Flash tank is a container with 2 reboiler attached to it. It has an inlet for thin
slope coming from decanter and outlet for vapours which are fed to analyser
reboiler to heat the column. The vapours are fed at temperature of 103 to 105oC
at pressure of 0.425kg/cm2.
There are 2 reboiler connected to the flash tank. 1st is R.C. vapour reboiler, 2nd
is normal reboiler. The vapours from rectified column are fed to the reboiler
condensate is fed to the tank whereas vapours are sent to vent condenser from
where trial alcohol is collected.
52
2. ALCOHOL SCRUBBER
It is a water column in which vapours from E.D. , degassifier and analyser vent
condenser are fed from bottom and water is sprinkled from the top. Water
absorbs the alcohol from the vapours drained out to PRC storage tank whereas
insoluble non-hazardous impurities are thrown out.
Vacuum pump is attached to the scrubber which sucks out the air from scrubber
which further sucks out the air from the three condenser thus creates vacuum of
0.42 to 0.425kg/cm2 in the columns.
4. PUMPS
There are 36 pumps in the distillation section. 18 pumps are in working state
whereas 18 pumps are on standby. They are centrifugal type of pump
manufactured by company micro finish. There are 2 vacuum pumps whereas
rests are pressure pump. Among the 2 vacuum pump one is on standby. The
rpm for vacuum pump is 1440 and for normal pressure pump 2900 rpm.
Pressure head for reflux pumps, spent wash pump, lees pump, feed pump are
50m.
53
IMPORTANT DATA TABLES
Table 14: STEAM FLOW RATES
STEAM QUANTITY kg/hr
Steam to PRC COLUMN 5300
Steam to RC COLUMN 7800
54
Extractive distillation 44-45
Simmering 42-44
Recovery column 50
55
Table 19: CONDENSER –REBOILER FLUID TABLE
56
20)Simmering column Vapours from analyser Fermented wash
condenser 1(fermented column
wash heater
21)Simmering column Vapours from analyser Cooling water
condenser 2 column
22) Simmering column Vapours from analyser Cooling water
condenser 3 column
23)Simmering column PRC vapours Alcohol(E.N.A)
reboiler
24)Simmering column PRC vapours Cooling water
vent condenser
25)E.N.A. cooler E.N.A. solution Cooling water
57
7)Rectifier 3 20 25.4 1.2 2000
PCV
condenser
8)Pre-Rectifier 451.97 1888 25.4 1.2 3000
column
reboiler
9)Extractive N.A N.A. N.A. N.A. N.A.
distillation
(E.D.) column
feed cooler
10) Pre- 2 13 25.4 1.2 2000
rectifier fusel
oil cooler
11)E.D. 500 1700 25.4 1.2 3000
condenser 1
(fermented
wash heater)
12)E.D. 61 264 25.4 1.2 3000
condenser 2
13)E.D. 51 216 25.4 1.2 3000
condenser 3
14)E.D. 60 301 25.4 1.2 2500
reboiler
15)Rectifier 2 13 25.4 1.2 2000
column
reboiler
16)Rectifier 5 21 25.4 1.2 3000
column E.N.A
cooler
18)Recovery N.A. N.A. 25.4 N.A. 3000
column
condenser 1
19)Recovery 1.5 N.A. N,A. N.A. N.A.
column
condenser 2
20)Simmering 67.03 280 25.4 1.2 3000
column
condenser
1(fermented
58
wash heater)
21)Simmering 25 62 25.4 1.5 2400
column
condenser 2
22) Simmering 5 31 25.4 1.2 2500
column
condenser 3
23)Simmering 95 476 25.4 1.2 2500
column
reboiler
60
bottom temperature column bottom
temperature through
steam to the reboiler.
7) Low fusel oil plate Low bottom temperature Check and adjust steam
temperature in flow
rectifier column
Low spirit draw Check and adjust draw
8) Higher temperature Higher dilution ratio Check and adjust dilution
of E.D. column ratio
bottom
61
12)Loss through spent Check the rectifier Increase the steam flow to
lees column bottom column and maintain
temperature bottom pressure.
Low impure Increase draw. Check
spirit/RS/ENA analyser column vacuum
CLEANING PROCESS
Occasional cleaning of the columns, condenser and reboiler is necessary. In
Rajasthan Liquor limited (distillery) cleaning of distillation unit is done once in
100 days. If losses are taking place or there is some disruption in the process
than cleaning can be done earlier to ensure proper functioning of the unit.
Disruption in the process may be caused because of air leakages in the vessel,
scaling of trays or malfunction of pumps, valves.
For cleaning of the column caustic (NaOH) solution and sulphonic acid solution
is used.
Once CIP is completed unit undergoes inspection of vessel, vacuum test and
water trial test.
62
INSULATION:
• A layer of 40-50mm glass wool is provided around stainless steel columns.
• The glass wool are covered by the aluminum sheets.
INSPECTION OF VESSELS:
Before vessels are closed for testing and operation ,they should be inspected,
washed free of residue and the internals checked for proper installation .The
points checked should include the location and length of thermo wells ,location
and fabrication details of sparger piping and the range and location of level
transmitter.
VACUUM TEST:
Vacuum test has to be carried out for the columns ,related accessories and
piping. This has to be carried out to detect air leakage into the system.
Before starting the vacuum trials following points are to be taken care of:
1) Isolate all the instruments like Pressure gauges, Pressure transmitters, Level
transmitters, Control valves etc.
2) Check the pressure of sealing water to the Vacuum Pumps.
3) Check the Vacuum Pumps for free rotation , direction of rotation and
lubrication.
4) Check the suction and discharge piping of Vacuum Pumps.
Once the preliminary checks are over-
1) Close the valve on the suction line of the vacuum pump and start the vacuum
pump.
2) Open the valve on the sealing water line to the vacuum pump and regulate
the flow of water by means of plug.
3) Check the pressure on the pressure gauge.by opening the isolation valve
63
slowly.
4) Let the pump run for 1 hr in this condition. Check for unusual sound and
Vibration . If the pump performance is satisfactory ,stop the pump.
5) Always stop water first then pump.
Repeat the above steps for the second pump
By carrying out the above steps, the following equipment will be under vacuum
and have to be tested for air leakages:
Once the air leakage is arrested. Isolate the whole system by closing the valve
on suction line of the vacuum pump and stop the vacuum pump. Check the rate
of drop in pressure.
64
After the successful vacuum test of the column following steps water trial test
need to be carried out:-
It is the final check of any equipment and apparatus that helps the operator to
understand the process flow and correlation of different equipment. It also helps
to set the instrumentation equipment ready for the start-up with the appropriate
material.
1. All the equipment in the plant and processing area has to be cleaned
mechanically(tanks ,pipes ,valves ,pumps etc.).
2. After mechanical cleaning ,all equipment should be flushed with water to
remove metal-dust, and other residues .Be careful ,not to block the sewerage
system with this residuals.
3. The following utilities have to be set in function and all the lines have to be
cleaned and checked carefully:
Electricity
Soft water and Cooling water
Steam
Instrument air
After the above steps has been fulfilled one must proceed as follows:
2) Open all vents on the condenser to vent out air. Establishing cooling water
circuit in condensers and coolers through cooling water pumps.
3) Fill the pre-rectifier RS draw tank with soft water and ensure that level of
water in the tank is 40% of total.
65
4) Start DM water to extractive distillation Feed column from DM water line.
Continue draining-water till clean water is observed. Stop soft water to feed
pipe by closing valve. Box up the blind flange on loop drain line. Open
extractive distillation Column bottom drain valve. Start DM water to column
through feed line. Let water drain through extractive distillation Column bottom
drain till clear water comes. Close the drain line valve and build water level .
Stop soft water supply.
5) Connect water hose to suction line of Fermented Wash Pump. Open by-pass
valve .Close suction valve and discharge valve on Fermented Wash Pump. Start
Fermented Wash Pump. Gradually open discharge valve and start feeding
water through flow meter. Ensure flow of water through Fermented Wash Pre-
heaters to Analyser Column & Degasifying Column .Allow water to drain
through the Degasifying Column bottom to Analyser Column till clear water
comes through. Analyser Column bottom. Open the valve on suction line of
Spent Wash transfer Pump and the drain valve on the suction line of the pump.
Drain water until clear water comes through it. Close drain. Open the bypass
valve. Start the pump and open the discharge valve slowly. Maintain 40% level
in the Analyser Column; continue the pump till all system get flushed.
6) Open the Reflux nozzle of the Pre-rectifier column.at top. Put water hose to
the top of the column, let the water come down, open the drain valve at bottom
of the pre-rectifier Column till clear water comes from it. When clear water
comes on Suction of the close the drain and stop feeding water at top and finally
close the top reflux-nozzle.
7) Start soft water feed to Fusel Oil Decanters by opening the respective
isolation valves. Start collecting the soft water in FO washing holding Tank.
Level will start building up in the tanks. As soon as the level reaches the 40% ,
open the drain valve on the suction line of feed pump and start draining the
water. Once clear water starts flowing, close the drain valve on the suction line
and attain the level in the tank. Once sufficient level is attained, open the
suction valve and start pump and slowly open the discharge valve. This will
start water feed to Recovery column. Allow the water to drain through the
66
recovery column bottom until clear water comes through it. Close drain. Open
the valve on suction line of recovery bottom. Drain water until clear water
comes through it. Close drain. Once flow is ensured stop the pump.
8) Open the reflux nozzle of rectifier column. Put water hose to the top of the
column, let the water come down, open the drain valve at the bottom of the
column to rectifier flash tank till clear water comes from it. When clear water
come close the drain and stop feeding water and finally close the reflux nozzle.
9) Open reflux nozzle of the simmering column. Put water hose to the nozzle
and let the water come down, open the drain valve at bottom of the simmering
column till clear water comes from it. When clear water comes in the suction
line close the drain , stop feeding water supply and close reflux nozzle valve
10)Check the respective draw/ transfer lines of all the columns accordingly.
67
SCADA( SUPERVISORY CONTROL OF THE DISTILLATION
PLANT)
68
1) ANALYSER COLUMN
69
EQUIPMENT TAG EQUIPMENT NAME
T-1413 Pre rectifier feed tank
T-1497 Sealing water storage tank
P-1413A Pre rectifier feed pump
P-1413B Pre rectifier feed pump
P-1437A Sealing water transfer pump
P-1437B Sealing water transfer pump
H-1497 Sealing water cooler vacuum pump
70
EQUIPMENT TAG EQUIPMENT NAME
H-1462 Rectifier pressure control valve
condenser
H-1405 Vent condenser for analyser reboiler
K-1462 Vapour bottle collector
K-1405 Vapour bottle collector
H-1401A Analyser reboiler column A
H-1401B Analyser reboiler column B
K-1401A Vapour bottle collector( gas liquid
separation)
K-1401B Vapour bottle collector
T-1462 Rectifier reflux tank
T-1402 Analyser flash tank
71
2)PRE-PRECTIFIER COLUMN
72
3)EXTRACTIVE DISTILLATION COLUMN
73
4)RECTIFIER COLUMN
74
5)RECOVERY COLUMN
75
6)SIMMERING COLUMN
76
ADVANTAGES OF MULTIPRESSURE DISTILLATION UNIT:
77
LAB TESTING FOR RAW MATERIAL AND DISTILLATION
UNIT PRODUCTS
Process:
Sample calculation:
Sample : 250 ml
Temperature: 93oF
Overproof: 68
% v/v= 96%
Result : The strength of E.N.A coming out from simmering column is 96% v/v.
78
Test 2: Alcohol strength in extractive distillation bottoms which are being
send to rectifier column.
Aim: to calculate alcoholic % v/v in bottoms of extractive distillation column
Process:
Sample calculation:
Sample : 250 ml
Temperature: 94oF
underproof: 74.4
% v/v= 14.62%
Process:
Sample calculation:
Sample : 250 ml
Temperature: 93oF
Hydrometer reading: 92
underproof: 85.8
% v/v= 8.11%
Process:
80
Inference: % strength of light fusel oil from rectifier column v/v is determined
.
Sample calculation:
Sample : 250 ml
Temperature: 90oF
underproof: 46
% v/v= 83.42%
Result : The strength of light fusel oil from rectifier column is 83.42% v/v.
Process:
Sample calculation:
Sample : 250 ml
81
Temperature: 91oF
underproof: 42.8
% v/v= 81.6%
Result : The strength of heavy fusel oil from rectifier column is 81.6% v/v.
Process:
Sample calculation:
Sample : 250 ml
Temperature: 91oF
overproof: 68.4
% v/v= 96.22%
82
Test 7: Alcohol strength of reflux of pre rectifier column.
Aim: to calculate alcoholic % v/v in reflux of pre rectifier column
Process:
Sample calculation:
Sample : 250 ml
Temperature: 91oF
Overproof: 63.8
% v/v= 93.6%
Process:
Sample calculation:
Sample : 250 ml
Temperature: 90oF
Overproof: 68
% v/v= 95.99%
Process:
Inference:
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Titrate the solution against ferrous ammonia sulphate with
few drops of ferroin indicator and note the reading.
Sample calculation:
Blank reading:30.5mm
Result: the total loss in the distillation unit for that sample was 0.393.
Process:
Inference:
a) If tip of tongue feel the maximum sensation then gases are present.
b) If it taste sweet it signifies presence of esters as impurities.
c) If side of tongue burns on tasting the solution then fusel oil present in final
product.
Process:
Inference:
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a) If time need for disappearance is more than 40-45 minutes then our product
sample is free from impurities.
b) If time for disappearance is less than 40 minutes then our sample has some
amount of impurities.
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WEEKLY REPORT
RLL has also installed a 120 kilo litre per day (KLPD) grain based distillery at
the above cited location in Derabassi , Punjab ,thereby diversification towards
new development and market penetration by new product.
1) SPIRITS
• EXTRA NEUTRAL ALCOHOL – A colourless clear flammable liquid
lacking flavor used to manufacture whisky. Ethanol v/v in the liquid is 96%.
• RECTIFIED SPIRIT - A neutral spirit with the strength of 95.6%. It is
highly concentrated ethanol with distilled by the process of rectification.
Used in manufacturing of blended whisky, cut brandy and some bitters.
• IMFL ( Indian manufactured foreign liquor)
• DENATURED ALCOHOL- ethanol that has additives to make it poisonous,
extremely bad tasting , foul smelling or nauseating. In some cases it is also
dyed. It is used as solvent or as fuel for alcohol burner or camping stoves.
2) BY-PRODUCT
• DISTILLED DRIED GRAINS WITH SOLUBLES - Kind of high protein
fodder/feed made from grain through fermentation, distillation , evaporation
and drying. The fodder contains not only rich proteins but also amino acids,
vitamins and mineral matters favorable to the growth of animals.
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• CARBON DIOXIDE- Alcoholic fermentation is the conversion of sugar to
alcohol and carbon dioxide. Around 49% CO2 is evolved which is processed
and sold out to other companies.
• DRY ICE- dry ice is produced from CO2 by changing the operating condt.
I was also given safety instruction and precautions which I need to follow
during my 2 month internship at the factory.
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REPORT 2: PROCESS FLOW FROM MILLING SECTION TO
DISTILLATION INCLUDING BYPRODUCT FORMATION
The process of manufacturing of E.N.A starts for milling section.
1) MILLING SECTION- In this grain i.e. rice is stored in silo tanks from
where via grain handler and elevator bucket they are sent for cleaning.
Cleaning is done in 3 classifier to separate oversize particles then it is fed to
destoner to separate stone and from here product is sent to flour mill (
hammer mill). Flour formed from here is stored in flour silo.
2) Liquefaction & Fermentation – In liquefaction section starch is converted
into sugar. Weighed amount of flour is taken and added to pre masher along
with water to form slurry. This slurry is fed to the initial liquefaction tank
along with enzyme alpha amylase in controlled quantity. The enzyme start
breaking starch into sugar the mixer is fed to jet cooker which maintains the
temperature and enhances the conversion. From here it is fed to retention
vessel and then to flash tank. From here mixer is fed to final liquefaction
tank where 75% enzyme is added which increases the breakdown of starch
to sugar.
A portion of wash from final liquefaction tank (FLT) along with water, air,
enzyme and dry yeast I added to yeast vessel to activate dry yeast. The
activated yeast from yeast vessel , air, enzyme, catalyst and wash from FLT
is added to pre fermentor tank. From here the contents are fed to the
fermentation tank along with wash from FLT. It take around 22-24 hours to
fill the tank and in this time only dosing of nitrogen source, enzyme and
catalyst takes place. Around 4 dosing takes place in 24 hours. And after that
in around 12- 13 hours sugar breaks down into ethyl alcohol and carbon
dioxide. Carbon dioxide is sent to carbon dioxide plant and alcohol is sent to
beer well.
3) Distillation unit- distillation unit comprises of 6 columns. They are analyser
column, pre- rectifier column, extractive distillation column, rectifier
column, simmering column and recovery column. This is a multi pressure
distillation unit. The purpose of this unit is to purify ethyl alcohol by
distilling is multiple time. In this analyser column and extractive distillation
column are kept under vacuum whereas pre- rectifier and rectifier column
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are kept under pressure. Simmering column and recovery column are under
atmospheric pressure. The pure E.N.A. obtained from the simmering column
is of strength 96%v/v.
My factory mentor assigned me to go for an in depth study of the distillation
unit. My work is to study each and every column there operating conditions,
physical measurements and chemical compositions. I have to figure out
about the problems which can be faced and give appropriate solutions along
with this suggestions for improvement if any.
4) By product section
Carbon dioxide plant- Approx. 49% of carbon dioxide is formed it is
purified, compressed , dried and then passed through chilling unit to convert
carbon dioxide from gaseous to liquid form for easy transportation and
storage. The carbon dioxide liquid is used to form dry ice.
DDGS ( distilled dried grain with soluble/cattle feed)- bottoms from
analyser column are fed to the 3 decanter. Thin slope is sent to multiple
effect evaporator whereas wet cake is sent to converyer belt from where fed
to ribbon mixer along with thick slope. Distributor is used to send the
product to double shaft mixer for breaking down large globules to smaller
particles and then fed to drier. From here dried product passed to bag filter
hopper to remove large particles whereas product fed to silo tanks and from
there sent for packing .
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REPORT 3 : STUDY ON 1ST THREE COLUMN
I have been assigned to study the multi pressure distillation section completely
and provide a detailed report on it. The steps taken so far for the fulfilment of
the project is detailed study of the 3 columns among 6. The study includes:
Similarly data for pre-rectifier column and extractive column has been taken
down along with there block diagrams.
By the end of this week I’ll be done recording data for the remaining 3 columns
rectifier column, simmering column and recovery column.
Along with this study need to be done on alcohol scrubber, pressure control
valves and flash tank.
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Cleaning of the section, insulation and material of construction study is going
on simultaneously.
SCADA observation will start from this week onwards. Depending on my
observations problem being faced are also being recorded and I have started
working on the solution for the same.
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REPORT 4: STUDY ON THE LAST THREE DISTILLATION
COLUMN
For the fulfillment my project I need to complete study all the distillation
columns. Last week I completed the study of remaining 3 columns. Those were
rectifier column, simmering column and recovery column. The study included:
Rectifier column:
Feed: Bottoms from extractive distillation column
Distillate: vapours to flash tank reboiler
Bottom: lees to cooling tower
Upper cut: 96% E.N.A along with ethyl and methyl alcohol
Middle cut: L.FO. AND H.F.O
Pressure of the column: 2.2kg/cm2
RECTIFIER COLUMN:
Top temperature : 98-102oC
Bottom temperature: 131-132oC
No. of trays: 72
Height of column: 22.4m
There is a reboiler, E.N.A cooler, D.M. water preheater and rectifier fusel oil
cooler.
Rectifier column reboiler No. of tubes: 727,Internal diameter:25.4mm;
E.N.A cooler No. of tubes: 21,Internal diameter:25.4mm;
Fusel oil cooler No. of tubes:13,Internal diameter:25.4mm;
Similarly data for simmering column and recovery column has been taken down
along with their block diagrams.
Along with this study on alcohol scrubber, pressure control valves and flash
tank has been done.
Cleaning of the section, insulation and material of construction study is going
on simultaneously and will be completed by the end of this week.
SCADA observation has been started from this week onwards. Depending on
my observations problem faced are also being recorded and I have started
working on the solution for the same.
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REPORT 5: LAB ANALYSIS
Last week I was assigned lab testing of quality check of the products from the
distillation unit.
I was briefed about the equipments used in the lab, was given information about
all he test which were being carried out. In total there are around 18 tests we are
being performed in the laboratory everyday out of which I was assigned to
perform 9 tests on daily basis.
The lab test which I have been assigned quality check of the products from
distillation unit includes test involving calculation of strength of products,
potassium permanganate testing, fusel oil presence testing and test to calculate
losses.
The test which I practically carried out was calculations involving analysis of
strength of the products. Steps to calculate ethanolic % v/v in E.N.A from
simmering column were:
Test reading for the same was recorded. Similarly test for other column
products were carried out.
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REFERENCES
www.sigmaaldrich.com/catalog/product/aldrich/w249715?lang=en®ion=IN
www.rll.co.in
https://eur-lex.europa.eu/legal-content/EN/ALL/?uri=CELEX:32008R0110
http://www.diamondspirit.net/adunk/metho.html
https://www.pharmaceuticalonline.com/doc/multiple-effect-distillation-unit-0001
http://www.shankerinternational.in/extra_netural_alcohol.html
https://pdfs.semanticscholar.org/d825/d06b3e068f1d945750f65e56a7f116af0f28.p
df
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