REPORT

FOR
INPLANT TRAINING
OF
Diploma in Industrial Fermentation and Alcohol Technology

In
M/S BALRAMPUR CHINI MILL (CHEMICAL DIVISION)
Duration of Training 01/12/2017 to 31/03/2018

Date of Submission:
Submitted to,
Director
National Sugar Institute,
Ministry of Consumer Affairs, Food & Public Distribution
Department of Food & Public Distribution
(Government of India)
KALYANPUR KANPUR-208017
2018
 INDEX
1. Introduction

2. Organizational Setup

3. Definition involved in process

4. The Process (Fermentation Section)

 
 The Raw material: Cane molasses
 
 Molasses management
 
 Propagation in lab scale
 
 Propagation in plant
 
 Fermentation and the fermentor
 
 Wash and sludge management
 
 Typical calculation of fermentation efficiency

 
Overview flow diagram of fermentation process

4. The Process (Distillation Section)

 
 Distillation Overview
 
 Azeotropic distillation of Ethyl alcohol and water
 
 Industrial distillation

 
 Definition involved in process
 
 R.S./E.N.A. Plant (Column)

Overview flow diagram of R.S./E.N.A. PLANT

 
Typical calculation of distillation efficiency

5. The Process (Effluent Treatment)
 
 Definition involved in process
 
 Introduction of ETP
 
 Bio-gas Digester
 
 Falling film Multiple-effect evaporator

 
Flow diagram of ETP

6. Demineralization plant (D.M. Plant)
 
 D.M. water and D.M. Plant
 
Soft water and Soft water Plant

7. Lab analysis

8. Ware house

9. Denaturation tank

10. By-products
12. Plant Setup and configuration information
 
 Molasses supply during production season in %
 
 Molasses storage tanks
 
 Fermentation house
 
 Distillation house
 
 Ethanol plant
 
 Instrumentation and control
 
 Receiver house and storage
 
 Bio-gas digester
 
 Multiple-effect evaporators
 
 Lagoon

 ABBREVIATIONS
R.S-Residual sugar
T.R.S-Total reducing sugar
T.V.A- Total volatile acid
R.S- Rectified spirit
V.F.A- Volatile fatty acid
D.S.I- Direct steam injection
V.L.S- Vapour liquid separator
P.R.V- Pressure reducing valve
E.N.A- Extra neutral alcohol
T.A- Technical alcohol
P.R.C- Pre- rectifier column
R.C- Rectifier column
D.C.- Distillation column
L.F.O- Low Fusel oil
H.F.O- High Fusel oil
 Process Principle In Details
Fermentation process-
The term fermentation was obtained from the Latin verb ‘fervere’, which describes
the action of yeast or malt on sugar or fruit extracts and grain. The boiling is due to
the production of carbon dioxide bubbles from the aqueous phase under the
anaerobic catabolism of carbohydrates in the fermentation media. However,
fermentation has come to have different meanings to biochemists and to industrial
microbiologists. Its biochemical meaning relates to the generation of energy by the
catabolism of organic compounds, whereas its meaning in industrial microbiology
tends to be much broader. The catabolism of sugars is an oxidative process which
results in the production of reduced pyridine nucleotides which must be re-oxidized
for the process to continue. Under aerobic conditions, re-oxidation of reduced
pyridine nucleotide occurs by electron transfer, via the cytochrome system, with
oxygen acting as the terminal electron acceptor. However, under anaerobic
conditions, reduced pyridine nucleotide oxidation is coupled with the reduction of
an organic compound, which is often a subsequent product of the catabolic
pathway. In the case of the action of yeast on fruit or grain extracts, NADH is
regenerated by the reduction of pyruvic acid, to ethanol. Different microbial taxa
are capable of reducing pyruvate to a wide range of end products. Thus, the term
fermentation has been used in a strict biochemical sense to mean an energy-
generation process in which organic compounds act as both electron donors and
terminal electron acceptors. The production of alcohol by the action of yeast on
malt or fruit extracts has been carried out on a large scale for very many years and
was the first 'industrial' process for the production of a microbial metabolite. Thus,
industrial microbiologists have extended the term fermentation to describe any
process for the production of product by the mass culture of a micro-organism.
Brewing and the production of organic solvents may be described as fermentations
in both senses of the word but the description of an aerobic process as fermentation
is obviously using the term in the broader, microbiological, context.

Organizational setup:
Since this Distillery is based on molasses as a raw material, a liquid saccharine
source for fermentation, it imposes several key factors which influence the type
of organizational setup and design both directly and indirectly. The essential
bodies that are integral to such kind of distillery that were present are namely:
1. A water source such as a rever water supply

2. A DM water plant and softener

3. A Fermentation house with laboratory

4. A Distillation house with Control room

5. A Receiver house

6. Product storage tanks

7. Product supply station

8. Molasses storage tanks

9. A molasses receiving pit

10. A molasses day tank

11. Bio-digesters for biogas production from effluent spent wash

12. A multiple effect evaporator for decreasing the volume of effluent

13. Spent wash lagoons for buffer storage

14. Cooling towers for temperature control

15. A general store house and workshop

DEFINITIONS INVOLVED IN PROCESS-

 
Molasses-
Molasses is the mother liquor left after removal of sugar crystals &
usable as a raw-material of Alcohol production. It contains fermentable
sugars 40-50 %, unfermentabe sugars 4-6 %, organic acids, vitamins,
pigments, nitrogenous matter and non nitrogenous matter. It is a dark
brown colour, thickly mass. Its specific gravity is 1.40 to 1.47.
 
Total Reducing Sugars (TRS)-
Total reducing sugars denote the content of total sugars (like sucrose,
glucose, fructose etc) in molasses in terms total reducing substances. It is
generally determined by “Lane” and “Eynon” method.

TRS = Fehling Factor X Dilution Factor X 100

Burette reading

 
Fermentable Sugars (FS)-
Simple sugars such as glucose and fructose are converted into
ethanol by the process fermentation in the presence of Yeast. They may
be derived by the hydrolysis of sucrose, starch or cellulose. These
converted sugars are known as fermentable sugars.
FS = TRS - UFS
 
Specific gravity-
It is the ratio between the mass of the substance and mass of a reference
substance (water) for the same given volume and temperature (at 40c).

Mass of the substance

Specific gravity =
Mass of equal volume of water
 
Brix-
A scale used to measure the specific gravity of a liquid in relation to
that of a solution of sugar in water. The measurement is accomplished by
use of a brix hydrometer or refract meter.

 
pH-
 This is value measuring the acidity or alkalinity of an aqueous
solution. Defined as the logarithm of the reciprocal of the hydrogen ion
concentration. Pure water at room temperature has a pH of 7.0 solution
with a pH of less than 7.0 are acidic, and greater than 7.0 are alkaline.
Control of pH is important in ethanol production both for obtaining
optimal enzymatic activity and in controlling the growth of bacterial
contamination.
pH= - log [H+]
 
Metabolism-
The chemical process in living cells by which energy is derived for
vital processes, growth and activities.
 
Sterilization-
Sterilization is complete destruction of all organisms including viruses
and spores.
 
Fermentation-
The process by which certain organism such as bacteria and yeast
degrade organic compounds in absence of oxygen in order to release
energy. It is a form of anaerobic respiration.
 
Microorganisms-
Microorganisms are collective term for microscopic organisms
including bacteria, Yeast, viruses, algae and protozoa.
  Yeast -
 A fungus capable of converting sugar into alcohol and carbon dioxide.
 
Propagation-
The process is increasing numbers of organisms by natural
reproduction. In case of yeast propagation occurs by budding and by
fusion to form new cells in both aerobic and anaerobic conditions.
 
Inoculum-
The portion of a culture of yeast or bacteria used to start a new
culture or fermentation.

 
Bacterial contamination-
 The condition occurring when undesirable bacteria become established
in a fermenting mash and reduce the ethanol yield.
 
Sludge-
The residual remains at the bottom of fermenter after fermentation. It
contains cell mass and other materials.
 
Antifoam-
A preparation composed of substance such as silicones, organic
phosphates and alcohol that inhibits for motion bubbles in a liquid during
agitation by reducing the surface tension.
 Fermentation house

Process of fermentation :
The Raw material: Cane Molasses
The third boiling of the sugar syrup yields dark, viscous final molasses, which is
the mother liquor from which no more sugar can be extracted commercially since
the majority of sucrose from the original juice has been crystallised and removed.
The calorific content of final molasses is mostly due to the small remaining sugar
content. This turns out to be a waste product for the sugar industry, but is
conveniently used as a cheap raw material for the production of alcohol either as
absolute alcohol (Ethanol), extra neutral alcohol (ENA) or for Indian made foreign
liquor (IMFL). Certain key factors that come into play while using final molasses
as the raw material is tightly controlled by the excise as well as sets the basic raw
material handling capacity of the plant from a design perspective. Since the sucrose
content of the molasses is of key interest, more specifically the fermentable sugar
content, it is commercially valued accordingly
COMPOSITION OF MOLASSES-
Composition of molasses quality is referred to the variety of molasses and also
varied in the wide range as follows-
ConstituentsNormal Range
Water 17-25 %
Sucrose 30-40 %
Glucose 4-9 %
Fructose 5-12 %
Ash 7-15 %
Other reducing substance 1-4 %
Nitrogenous substance 2.5-4.5 %
Amino acids 0.3-0.5 %
Non nitrogenous organic acid 1.5-6.0 %
Wax sterols 0.1-1.0 %
Vitamins very less in amount
GRADATION OF MOLASSES:
Gradation of molasses is generally based upon Brix, TRS, and Ash % in the
molasses.

Sr. No. Parameter Grade A Grade B Grade C

1. Brix (at room 88-90 85-88 Below 81
temp.)
2. Ash (% by 12-13 14-15 More 17-18
weight)
3. TRS(% by Above 50 % 44-49.9 % Below 44 %
weight)

Molasses management:
Molasses can be either retrieved from the organization’s own adjacent sugar
section or can be bought from other bodies. When bought from other bodies, its
commercial value is decided by its grade as discussed before. During the plant
operation, molasses was purchased from the organization’s own adjacent sugar
section The Ugar Sugar Works Ltd. Ugar Khurd, Belagavi, Karnataka to meet
production goals. Since Alcohol is an excisable product, the raw material and its
management (molasses) is done in a predefined manner in almost every
distillery. This includes the use of storage tanks and a day tank. The
construction of the day tank is necessary according to excise as one cannot
consume the raw material directly from storage. It is weighed at a weighing
station which is equipped to weigh 275 tonns of molasses in a single batch.
 MOLASSES STORAGE TANK
The molasses pit provides convenience when molasses in bought from outside
and tankers are usually ramped backwards slightly to dump the molasses
directly in it without the requirement of pumping it.
A similar weighing station is present at the fermentation house to cross check
the amount of molasses actually being fed to the process. Therefore the TRS of
the molasses is monitored at two points i.e. at the storage location and at the
fermentation section where it is called “process molasses”.
Pulley driven screw pumps are used for transfer of molasses from one location
to the other as it is a highly viscous material.
Propagation in lab scale:
This is the core of the process since the raw material is converted in the bulk
product here. From a microbiological perspective the key organism yeast,
(Saccharomyces cerevisiae) is cultured in the laboratory and the strains being
used are carefully propagated by increasing the biomass of the yeast (yeast
population) also at this stage, conditioning is done from lab culture media to
molasses via a jaggery medium (gur) that bears resemblance to molasses media
that is ultimately utilized.
Initial lab media is a simple YEPD (Yeast extract potato dextrose) media which
is prepared in agar slants to preserve efficient yeast strains. An alternative is to
use commercially available active dry yeast to initiate yeast biomass
development. In the jaggery media, 1.5 gram of peptone and albumen is added
along with 1 gram of Yeast extract. The jaggery is boiled and strained to
remove suspended or insoluble impurities and mixed in a 1:1 ratio with
molasses. The pH and specific gravity is adjusted to 4.5 and 1.05 respectively
and then autoclaved. Inoculation volumes is increased roughly by a factor of
five which starts from 10ml of media to 25, 50, 100, 500, and 1000 to finally
5000ml flasks. Three such flasks are fed in every batch of fermentation (a total
of 15 litres) to the initial yeast vessel.

Propagation in plant:
A) Yeast vessels (culture vessels) :These are stainless steel vessels with a
consecutive increase in capacity and three vessels with its pair is installed, with
a particular set of three operating at a time and the other set on standby. Yeast
vessels have got aeration system via sparging of air filtered by HEPA (High
efficiency particulate air filter). Also cooling coils and steam line is connected
for sterilization with steam in each batch.
 Yeast Vessels

vessels noumber Quantity Capacity Material

Yeast vessels 1. 1 500 L. Stainless steel
Yeast vessels 2. 1 1200 L. Stainless steel
Yeast vessels 3. 2 6000 L. Stainless steel
Pre-fermenter 2 55000L. Mild steel
Fermenter in new
plant 4 405006 L. Mild steel
C.W.T 1 162666L. Mild steel
Fermenter in old
plant 5 363000L. Mild steel

Add chemicals YV 1 YV 2 YV 3
Urea 500 gm 60 gm 600 gm
DAP 200 gm 25 gm 250 gm
Acid 250 ml 400ml 1.5 lit.

B) Pre-fermentor: They are two pair of mild steel vessels, one pair for old
plant and another one pair used for new plant (one at standby) in which the final
aeration stage is completed to obtain optimum cell population. This is also the
stage in the process where apart from molasses other nutritional and disinfecting
compounds are added for efficient fermentation.
The compounds added at this stage are as follows:
  
Urea: 1.5 kg
 
Di-ammonium phosphate: 1 kg
  
Turkey red oil antifoaming agent: as and when required ~2 kg in a batch
  
Sulphuric acid: 1.5
 
Commercial enzyme additive: 110gm

Both Yeast vessels and Pre-fermentor have dedicated molasses supply lines that
is combined with the water supply line such that molasses is diluted internally
and mixed in the piping with water with controlled flow rate to obtain “wort” at
a specific gravity of 1.05. This specific gravity is monitored during the filling of
these vessels and pre-fermentor. Aeration is also monitored.

Fermentation and the fermentor:

Unlike in the previous stages of the process, fermentation is in contrast an
anaerobic process and it is here where the bulk product is formed. The principle
biochemical process includes the Embden-Meyer pathway or glycolysis and the
implication of anaerobic biochemical transformation of pyruvate to yield ethyl
alcohol.
In the first step of alcoholic fermentation, the enzyme invertase in yeast cleaves
the glycosidic linkage between the glucose and fructose in the bulk sucrose
molecules present in the molasses.
C12H22O11 + H2O + invertase C6H12O6 + C6H12O6

Next, each glucose molecule is broken down into two pyruvate molecules in a
process known as glycolysis. Glycolysis is summarized by the equation:

C6H12O6 + 2 ADP + 2 Pi + 2 NAD+ → 2 CH3COCOO− + 2 ATP + 2NADH +

2 H2O + 2 H+
Pyruvate (CH3COCOO) usually finds its way into the Citric acid cycle in an
aerobic environment; however in anaerobic conditions the fate of pyruvate is
different. NADH generated by glycolysis cannot be re-oxidized by O2.

Failure to regenerate NAD+ would leave the cell with no electron acceptor for
the oxidation of glyceraldehyde 3-phosphate, and the energy-yielding reactions
of glycolysis would stop. NAD+ must therefore be regenerated in some other
way. The earliest cells lived in an atmosphere almost devoid of oxygen and had
to develop strategies for deriving energy from fuel molecules under anaerobic
conditions. Most modern organisms have retained the ability to constantly
regenerate NAD+ during anaerobic glycolysis by transferring electrons from
NADH to form a reduced end product such as lactate or ethanol. Yeast and
other microorganisms ferment glucose to ethanol and CO2, rather than to
lactate. Glucose is converted to pyruvate by glycolysis, and the pyruvate is
converted to ethanol and CO2 in a two-step process:

The fermentor is the essential vessel in which the raw material (molasses) is
converted into product (Ethyl alcohol). Wort is filled in the fermentor at this
stage at a specific gravity of 1.5 (more than that in propagation stages). This is
because in anaerobic conditions pyruvate is unable to enter the Calvin cycle and
much less energy is obtained from a single glucose molecule, therefore the
anaerobic process demands a higher sugar load.
The reaction shown above is the major reaction that takes place making Ethyl
alcohol as the major product, however since it is a biological process, involving
several key parameters and organic compounds, many other alcohols are also
formed which comprise of compounds both lighter/ more volatile and heavier/
less volatile than Ethyl alcohol. Thus a mixture of alcohols is the bulk product
in the fermentor after the fermentation process is complete. It was noted that
instead of intermittent aeration in the pre-fermentor, an hour of low pressure
aeration is done in the fermentor itself which serves as both conditioning of
cells for anaerobicenvironment as well as re-suspending of the yeast cells in
the fermentor volume via sparging. Since the anaerobic process leaves energy
rich pyruvate molecules unutilized, the two ATPs generated in the glycolysis
step appear as waste heat and tend to raise the temperature of the vessel. Since
the optimum temperature of the process is 30-320C, the reaction volume has to
be cooled intermittently.

here this is done by circulation of the reaction volume through a plate type heat
exchanger via a powerful direct driven centrifugal pump.

The fermentation is said to be complete, when no carbon dioxide is liberated and

the yeast settles down at the bottom. Fermentation time is roughly around 12-13
hours. The fermentor vessel (four pairs) are operated in such a manner that in one
fermentation is in progress, another one is final, ready to be processed further, one
is under filling condition and the final one is under cleaning. This process is
repeated within the eight fermentors in both plants. The design of the fermentor is
such that it has a sloping bottom which aids as a sloping sedimentation surface for
removal of waste sludge (dead yeast biomass). The carbon dioxide evolved in the
process
is sent through an exhaust outlet, no CO2 plant is established here to
commercialize pressurized CO2.
The compounds added at this stage are:
  Turkey red oil antifoaming agent: when required
 
Commercial enzyme additive: 1 kg

Wash and yeast sludge management:

Wash, i.e. the final liquid fraction of the fermentation reaction mixture contains the
alcohol in it and is subjected to distillation. Prior to that, it is held in a clarified
wash tank and this acts as a buffer feed system to the distillation section.
Yeast sludge generated in each fermentor is subjected to repeated sedimentation
(no decanting step involved). This is done with the help of a sludge pump which
intermittently pumps away the sludge settling at the bottom of the fermentors
and the clarified wash tank and collects it in two sludge settling tanks (one stays
on standby). The overflow of this tank is sent back to the clarified wash tank.
The sludge is periodically sent to the ETP section for treatment process.

Typical calculation of fermentation efficiency:

Theoretically the amount of alcohol that can be produced from 1 gram of
glucose can be stoichiometrically determined from the overall summarized
reaction of fermentation, known as Gay Lussac’s equation:
C6H12O6→ 2 C2H5OH + 2 CO2
180 grams of glucose gives 92 grams of ethyl alcohol and 88 grams of carbon
dioxide. Therefore1 gram of glucose will yield 0.51 gram of alcohol.
Assuming the molasses being fed has a typical total reducing sugar content of
48% with a unfermentable sugar content of 4.5% in a typical 1080 quintals of
molasses being fed to the process, then fermentable sugar content = 43.5% of
1080
= 469.80 quintals
Hence by the Gay Lussac’s equation 440.64 quintals of sugar can yield (469.80
X 0.51) = 239.598 quintals of alcohol, = 23959800 grams of alcohol.
Since ethyl alcohol has a density of 0.789 gram/cm3 at 200C or 789000
grams/m3. Therefore volume of alcohol produced is 30.3673 m3 or 30367.300
litres. This is the theoretical yield.
However, in actual a typical 9.5% alcohol is observed, fermentor volume being
285120 litres.
i.e. 27086.4 litres of alcohol is produced.
Therefore the fermentation efficiency is (27086.4/30367.300) = 0.89195 or
89.1959%.
 DISTILLATION HOUSE
Distillation
Distillation is a process of separating the component substances from a liquid
mixture by selective evaporation 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 of the mixture.
In either case the process exploits differences in the volatility of mixture's
components. In industrial chemistry, distillation is a unit operation of practically
universal importance, but it is a physical separation process and not a chemical
reaction. For many cases, the boiling points of the components in the mixture will
be sufficiently close that Raoult's law must be taken into consideration. Therefore,
fractional distillation must be used in order to separate the components by repeated
vaporization-condensation cycles within a packed fractionating column. This
separation, by successive distillations, is also referred to as rectification.

Azeotropic distillation of Ethyl Alcohol and Water:

Interactions between the components of the solution create properties unique to the
solution, as most processes entail non-ideal mixtures, where Raoult's law does not
hold. Such interactions can result in a constant-boiling azeotrope which behaves as
if it were a pure compound (i.e., boils at a single temperature instead of a range).
At an azeotrope, the solution contains the given component in the same proportion
as the vapour, so that evaporation does not change the purity, and distillation does
not affect separation. For example, ethyl alcohol and water form an azeotrope of
95.6% at 78.1°C. If the azeotrope is not considered sufficiently pure for use, there
exist some techniques to break the azeotrope to give a pure distillate. This set of
technique is known as azeotropic distillation. Some techniques achieve this by
"jumping" over the azeotropic composition (by adding another component to
create a new azeotrope, or by varying the pressure). Others work by chemically or
physically removing or sequestering the impurity. For example, to purify ethanol
beyond 95%, a drying agent or a (desiccant such as potassium carbonate) can be
added to convert the soluble water into insoluble water of crystallization.
Molecular sieves are often used for these purposes which are packed beds of
desiccant operating in cycles of moisture removal.

An insight into modern day Multi-pressure distillation (MPR):

The boiling points of components in an azeotrope overlap to form a band. By
exposing an azeotrope to a exploiting the differing vapour pressure curves of each;
the curves may overlap at the azeotropic point, but are unlikely to be remain
identical further along the pressure axis either side of the azeotropic point. When
the bias is great enough, the two boiling points no longer overlap and so the
azeotropic band disappears. This method can remove the need to add other
chemicals in distillation. This can be done either using positive or negative
pressure or both. In modern day distillation columns, both positive and negative
pressure is employed as suited to application. This characteristic of having multiple
columns with different pressure profiles is known as multi-pressure re-
distillation (MPR) and provides efficiency to the process handling fluids with
diverse components. Essentially modern day distilleries have this application.

Industrial distillation:
Industrial distillation is typically performed in large, vertical cylindrical columns
known as distillation towers or distillation columns with diameters ranging from
about 65 centimetres to 16 meters and heights ranging from about 6 meters to 90
meters or more. When the process feed has a diverse composition, as in distilling
fermented wash, liquid outlets at intervals up the column allow for the withdrawal
of different fractions or products having different boiling points or boiling ranges.
The "lightest" products (those with the lowest boiling point) exit from the top of
the columns and the "heaviest" products (those with the highest boiling point) exit
from the bottom of the column and are often called the bottoms. Industrial towers
use reflux to achieve a more complete separation of products. Reflux refers to the
portion of the condensed overhead liquid product from a distillation or
fractionation tower that is returned to the upper part of the tower. Inside the tower,
the Down-flowing reflux liquid provides cooling and condensation of the Up-
flowing vapours thereby increasing the efficiency of the distillation tower. If more
reflux is provided for a given number of theoretical plates, the better the tower's
separation of lower boiling materials from higher boiling materials. Alternatively,
the more reflux that is provided for a given desired separation, the fewer the
number of theoretical plates required. Chemical engineers must choose what
combination of reflux rate and number of plates is both economically and
physically feasible for the products purified in the distillation column.

For a multi-component feed, simulation models are used both for design and
operation. Moreover, the efficiencies of the vapour–liquid contact devices
(referred to as "plates" or "trays") used in distillation towers are typically lower
than that of a theoretical 100% efficient equilibrium stage. Hence, a distillation
tower needs more trays than the number of theoretical vapour–liquid
equilibrium stages. A variety of models have been postulated to estimate tray
efficiencies. In modern industrial uses, a packing material is used in the column
instead of trays when low pressure drops across the column are required. Other
factors that favour packing are:
 
 vacuum systems
 
 smaller diameter columns
 
 corrosive systems
 
 systems prone to foaming
 
 systems requiring low liquid holdup and
 
batch distillation

Definitions involved in process-

  Distillation:-
The word distillation is from the Latin, “destillare” which means to
drop,or to trickle down. Distillation is a method of separating of the
components of a miscible solution having different boiling points are
 separated on the basis of their boiling point.
“Distillation is a process of evaporation & re-condensation used in
 separating liquid in to vapours fraction according to boiling point.”
  Reboiler:-
A device for supplying heat to a distillation column without introducing
live steam. It generally consist 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.
  Condenser:-
A heat exchange device connected to the vapour discharge pipe of a
column to permit the vapour to the cooled and condensed to a liquid.
Condensers are commonly cylindrical vessels. Containing tubes
 through which cooling water is passed.
 
Distillation column:-
 A vertical cylindrical vessel containing a series of perforated plates or
other contact device through which vapours may pass to effect a
separation of liquid mixture by distillation.
  Decanter:-
Vessels used for the separation of two phase liquid. In a fusel oil decanter
 an upper fusel oil phase is separated from lower water.
  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.
  Pressure:-
Pressure is defined as the force per unit area. The various units for the
pressure measurement are kg/cm2, psi, mmHg, Bar.
  Reflux:-
The portion of the condensed overhead vapours returned to a distillation
 column to maintain the liquid-vapour equilibrium.
  Reflux ratio:-
The ratio of the amount of condensate refluxed to the amount withdraw
 as product.
  Boiling point:-
This is the temperature at which the vapour pressure of a liquid equals
 the total pressure of the atmospheric above it.
  Proof:-
This is the measure of the absolute ethanol content of a distillate
containing ethanol and water. In the US system, each degree of proof is
 equal to 0.5714% ethanol by volume.
  Rectified sprit:-
Rectified sprit (R.S.) is produced from molasses by distillation. Rectified
spirit is not completely neutral as it a lot of impurities. Rectified sprit is
redistilled to produce neutral alcohol (ENA).

 
Neutral spirit:-
 Neutral spirit is purified, odourless, tasteless and colourless ethanol
produced by distillation from rectified spirit. It is used in the production
of IMFL such as rum, gin, vodka.
  Anhydrous alcohol:-
Anhydrous literally means “without water”. The term used for a
substance that does not contain water. Ethanol for fuel is commonly
 referred to as anhydrous, because it has had almost all of water removed.
  Denatured sprit:-
Denaturant mixed with spirit then it is called as denatured spirit.
 Denaturant addition makes the material unpleasant and unfit to drink.
  Fusel oil:-
Fusel oil term used to describe the higher alcohols, generally the various
forms of propanol, butanol, and amyl alcohol that are by-products of
ethanol fermentation. Their presence in alcoholic beverage is known to be
a cause of headaches and hangovers. The fusel oils have higher boiling
 points than ethanol.
  Spent wash:-
Distillery effluent known as spent wash. It is a source of organic matter
 nutrients such as iron, zinc, copper, manganese, boron and molybdenum.
 
Scale formation:-
A deposit formed on the surface of equipment due to formation of
insoluble inorganic compounds. Scaling problems are more common in
ethanol distillation (distillation column and heat exchanger)
  Soft water / DM water:-
Filtered water, free from algae, bacteria, suspended solid, non corrosive
and commercial zero hardness for soft water.

Here, the plant is designed for the manufacture both Ethanol and ENA as end
products; however this season only Ethanol production was undertaken. The
related sections are shown below:

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, by create vacuum with pump. Fermented wash feed to the
Analyser column through the fermented wash beer-heater. The vapours form the
top of Analyser column are fed to the PRC column .the vapours concentration at
the column top will be in the range of 40-45%w/w. Alcohol concentration in the
top vapours depend upon the alcohol % in FW Feed and efficiency of Analyser
column reboiler. Spent wash from the Analyser column bottom is used to
preheat the fermented wash and sent to the effluent treatment plant. ETP for
further treatment. RC column vapours is used to heat the Analyser column
through Analyser column reboiler.

Technical specification of Analyser column-

  No. of trays- 23
   Sieve plate
Type of trays-
   0.35m
Tray spacing-
  Stainless steel
MOC-

Operating parameters-
  Top temperature-
  Bottom temperature-
  Top pressure-
 
Bottom pressure-
76 to 770C
86.5 to 87.50C
-0.52 to -0.57 kg/cm2
-0.45 to -0.47 kg/cm2

PRE RECTIFIER COLUMN (PRC):-

 Pre rectifier column is operated under vacuum. The primary motive of this
section is to separate the heavier alcohols (fusel oil) from lighter components
that include ethyl alcohol. The purpose of this column is to concentrate low
boiling impurities and also to concentrate alcohol this will be fed to pre-
distillation column for further processing. Analyser column vapours are fed to
the bottom of the PR column.PR column is heated with the help of exhaust with
steam. In PR column vapours are condensed in beer heater, uncondensed
vapours then condensed in condenser then remaining condensed in vent
condenser. From these condensers the part of condensed liquid is collected in
PR Reflux tank, then condensed is re-feed PR column for reflux. When
temperature is reached optimum which is necessary then PR draw is feed into
pre-distillation column for further process. In PR column several cuts are found
by which fusel oil is separate which go in PR cut.

Technical specification of Pre-rectifier column-


No. of trays- 45

Type of trays- Sieve plate

Tray spacing- 0.35m

MOC- Stainless steel
Operating parameters-

Top temperature- 53.7 to 54.70C
 
Bottom temperature- 81.8 to 82.20C
Top pressure- -0.72 to -0.73kg/cm2
Bottom pressure- -0.42 to -0.43 kg/cm2

PRE-DISTILLATION COLUMN:-
 Pre-distillation column is operated under atmospheric pressure. The
column is principally used for removal of low boiling impurities and it is
operated with extractive mode of operation. The rectified spirit from the
PRC column is fed in the middle part of the column. DM water and spent
lees form the Rectifier column bottom are used for the dilution of
alcohol. These water and spent lees feed on the top tray of PD column.
Steam is provided to heat the column through thermo-siphon reboiler.
Alcohol vapours form PD column are used to heat head column. PD
draw which draw from bottom are fed in Rectifier column at the top. RC
lees drain when ENA made.

Technical specification of Predistillation column.


No. of trays- 50

Type of trays- Sieve plate

Tray spacing- 0.35m

MOC- Stainless steel
Operating parameters
 105 to 105.80C
Top temperature-

Bottom temperature- 86 to 870C

Pressure- atm

RECTIFIER CUM EXHAUST COLUMN (RC COLUMN):-

 Rectifier cum exhaust column is operated under pressure. The column is used
to concentrate the alcohol. The pre-heated feed from PD column is feed to rectifier
column. The feed is heated with the spent lees coming out from the RC bottom
with the help of PHE. Steam is fed to the RC reboilering a controlled manner. The
alcohol vapour from RC top used to heat analyser reboiler. These vapours
condensed and go to reflux tank. After reflux when acquired temperature achieved
then RS product draw and it receive in receiver by PHE. Rectifier cut (i.e. fusel oil)
draw several cuts which go RC cut and then fed into Head column.

Technical specification of Rectifier column-

  No. of trays- 70
   Bubble caps
Type of trays-
   0.17m
Tray spacing-
  Stainless steel
MOC-

Operating parameters-
  Top temperature-
  Bottom temperature-
  Top pressure-
 
Bottom pressure-
91.5 to 920C
122 to 1230C
0.72 to 0.98 kg/cm2
1.18 to 1.25 kg/cm2

HEAD COLUMN:-
 The motive of this column is to achieve the ENA end product by removal of
aldehydes, fusel oil and acids from ethyl alcohol. This column is operated under
atmospheric pressure. This column is heated with the help of PD top vapours.
All fusel oil cuts (PR cuts and RC cuts) are fed in head column by pump.
Vapours of head column are used to heat methanol reboiler. After heated these
vapours go to head condenser and vent condenser. The condensed part is go into
head reflux tank for reflux. When the acquired temperature achieved the TA
(technical alcohol) is removed by head condenser and store. Head cuts i.e. fusel
oil is removed by cuts and go into fusel oil decanter. In fusel oil decanter fusel
oil is separated by soft water, after separation fusel oil is store.
Head column top are joined with aldehyde column which are used for
separation of aldehydes. Separated aldehydes are fed in wash charger for
reduction after reduction aldehydes convert in to alcohol.
Head column bottom are joined with water stillage. It works atmospheric
conditions. It heated with the help of steam. It used for extract for remaining of
alcohol which remain.
Technical specification of Head column-

No. of trays- 40

Type of trays- Sieve plate

Tray spacing- 0.17m

MOC- Stainless steel
Operating parameters-
 78.2 to 78.60C
Top temperature-

Bottom temperature- 101 to 1020C

Pressure- atm
Water stillage:
METHENOL COLUMN:-
Methanol column (Simmering column) is operates under atmospheric
pressure. The column is principally used for removal of methanol form ENA.
Methanol column is manufactured with copper metal to separation of sulphur
containing components and mercaptans. Methanol column is operating at very
high reflux ratio to increase the purity of top product which is separation form.
PD column top vapours are provided through thermos siphon reboiler to heat
the methanol column low pressure steam is used as a heating media whenever
column PD column is not working. Methanol column top vapours are
condensed in condenser and vent-condenser. Condensed vapours sent to reflux
tank for reflux. After reflux it transfer receiver for storage.

Technical specification of Methanol column-

  MOC- Stainless steel
 
Chip division

Operating parameters-
  Top temperature-
  Bottom temperature-
  Top pressure-
 
Bottom pressure-
51 to 520C
53 to 540C
-0.72 to -0.73 kg/cm2
-0.42 to -0.43 kg/cm2
OVERVIEW FLOW DIAGRAM OF R.S. / E.N.A. PLNT
 MOLICULER SIEVE DEHYDRATION
PLANT (M.S.D.H. PLANT)-
Absolute alcohol (Ethanol) plant:-
Since ethyl alcohol and water form an azeotrope as discussed before, the
requirement of obtaining high purity alcohol also known as anhydrous alcohol
as a final product is achieved by the installation of a separate plant. Here, the
popular choice of using molecular sieves for dehydrating is used.
As the name indicates, molecular sieves serve the function of sieving at a
molecular level. This is achieved by using suitable materials which are porous
at a molecular level. For dehydrating alcohol at an industrial level, zeolite
packed beds (micro-porous aluminosilicates) are used. The operation involves
using a pair of sieves that alternately function in the dehydrating process.
Usually alcohol is superheated to a temperature of 135-1450C in vapour phase
and passed through the sieve where the smaller water molecules are adsorbed in
the packed bed and the ethanol molecules are retained back which is then
condensed further to obtain anhydrous alcohol. The hydrated bed is dehydrated
by the application of vacuum. This process of dehydration and vacuum
application is repeated in alternated cycles within the pair of molecular sieves to
achieve an effectively continuous process.
The basic roles of these two sections are as follows:

1. Rectification Section:
An additional rectifier ensures that the alcohol to be dehydrated has only 3%
moisture or less before being fed to the molecular sieves. Since the Excise
requires storage of initially produced rectified spirit before being used as feed to
the Absolute alcohol (Ethanol) plant, the alcohol gains moisture during storage
and transfer. But because the sieves can remove only 3% moisture in a cycle, it
is important that the plant has its own rectifier.

2. Molecular Sieve and Vacuum Section:

This section as stated previously has two molecular sieves for dehydration
working alternately to provide a continuous supply of anhydrous alcohol as the
final product.

Ethanol plant:
 
 Molecular sieve capacity: 340 litres
 
 Sieve composition: Zeolite packed bed
 
Feed rate to molecular sieve: 42-48 litre/minute
  
 Steam pressure: 5.5kg/cm2
 
 Vacuum: - 0.9kg/cm2
 
 Operating cycle time: 420 seconds
 
Number of vacuum pumps: 2

Process description:-
Condensed rectified spirit first feed pre-heater through pump. The feed is
preheated in this heat exchanger against steam condensate coming from
reboiler. The preheated feed enters the Rectifier column. The rectifier is
pressurized, and its purpose is to vaporise the ethanol feed and to process the
recycle liquid coming from the molsieve regeneration system.
Since the ethanol feed has already rectified and only needs to be vaporized, it
can be fed near the top of the Rectifier.
Energy is provided to the bottom via the reboiler using steam under flow
control. After heated vapours of rectifier is feed into condenser. In condenser
these vapours are condensed and returns receiver and recycle process. When
super heater achieved necessary temperature, control valve open and vapour of
rectifier fed super heater. Super-heater heater heated directly with steam. From
super heater vapours are fed in molsieve units. (Mol-A and Mol-B). The vapour
passes up through one bed of molecular sieve beds at a defined pressure.
Incoming water is adsorbed on the molecular sieve beds. Anhydrous ethanol
vapour exists the molsieve units.
The molsieve units are cycled so that one is regeneration while the other is
adsorbing water from the vapour stream. The regeneration is accomplished by
doing two things. First a vacuum is applied to the bed undergoing regeneration.
Second, a portion of the anhydrous ethanol vapours stream is directed down
through the bed. This combination caused water to adsorb the molecular sieve
beads and transfer into the ethanol vapour stream. This mixture of ethanol and
water is condensed in the mol sieve regeneration condenser against cooling
water. Any uncondensed vapour leaving the vent of the mol sieve regenerate
condenser enters the mol sieve regenerate drum where it is contacted with
cooled regenerate liquid.
The liquid regenerate stream collects in the mol sieve regenerate drum. A
portion of regenerate liquid is fed to the rectifier.
Anhydrous ethanol vapour from the mol sieve units passes through the pressure
control valve into the mol sieve condenser where it is condensed against cooling
water. After condensation it receive in receiver and store.
Typical calculation of distillation efficiency:

Suppose the alcohol% in the wash achieved in fermentation is 9.5% and

fermentor volume being 285120 litres = 27086.4 litres of alcohol
After being fed to the plant, the amount of rectified spirit obtained after the
distillation process is calculated by a flow-meter called a totalizer. Typically for
a particular fermentor volume handled, it is 26680.1 litres. Therefore distillation
efficiency = (26680.1/27086.4) = 0.98or 98.1%
The strength of alcohol is calculated by an instrument called the Karl-Fisher
titrator in the laboratory and typically rectified spirit has a strength of 95.4%
which means the bulk volume of 25198 litres represents (0.954 X 26680.1) =
25452.81 litres (absolute volume).
The overall efficiency of the entire plant is given by:
Overall efficiency = (D.E.X F.E.)/100
Therefore typically, overall efficiency stands as: (98.1 X 89.19)/100 = 87.49%.
 Effluent treatment plant

DEFINITIONS:-

Chemical oxygen demand (COD):-

Oxygen required for the complete oxidation of biological degradable and
non-biodegradable organic matter. The organic matter in reduced state such as
Cl, CN, and NO3 also get oxidized.

Biological oxygen demand (BOD):-

It is the oxygen quantity demanded by the aerobic micro-organisms (bacteria) to
stabilize the organic matter. Since BOD is directly proportional to the organic
matter concentration.

Total solids:-
The amount and nature of dissolved and undissolved matter present in liquid
very gently. It potable waters most of the matter is in dissolved from and
consists mainly of inorganic salts and small amount of organic matter. The
amount of undissolved colloidal and suspended matter increases with pollution.

Anaerobic Digester:-
Organic materials are decomposed biologically by various species of bacteria.
Bacterial decomposition can occur without air in anaerobic digester. These
bacteria are Acetogenic bacteria and Methogenic bacteria.

Acetogenic Bcteria:-
Acetogenic bacteria are described as non-methanogenic or simply they are
called as acid formers.
Among the non-methanogenic bacteria that have isolated from anaerobic
digesters are clostridium, lactobacillus, etc.

Methanogenic Bacteria:-
Methanogenic bacteria are simply called as methane formers. They are strictly
called anaerobes. Methanogenic bacteria are H2 utilizing bacteria
(methnospirillum hungares) and acid utilizing bacteria.

Biogas:-
Biogas produced from anaerobic digester consists of C02 (38-48 %), CH4 (50-60
%), H2S (1-2 %). The biogas has a high calorific value 4500 Kcal/m3. This is
directly sent to the boiler as fuel for steam generation.
Bio-composting:-
Composting is the biological decomposition of organic solid wastes or
mixture of solids and liquid wastes at between 50 to 70 % moisture content to a
relatively stable and product. Decomposition proceeds in the thermophilic
temperature range 500C.

Mixed culture:-
This is used for Bio-compost process. Several micro-organisms are
mixed with yeast, bacteria and molds.

Introduction of effluent treatment:-

The alcohol industry like any other industry has certain characteristic processes
that result in the development of various by products from mainstream
production of alcohol. A few of these by products have commercial value if
channelled properly into the consumer market. Others result as waste by
products or effluents. A molasses based distillery develops the following by
products while the production of ethyl alcohol is carried out:
  
Carbon dioxide
  
Yeast sludge
  
Spent wash
 
Fusel oil and Impure spirit

Among the above by products, apart from spent wash every other by product
has the potential of a commercial value. Many distilleries have expanded their
profit margin by installing proper machinery to handle these by products, these
are namely:

o Use of CO2 scrubber and compressor to commercialize CO2 for

carbonation of soft drinks, packaging with inert CO2.

o Use of Yeast sludge in dried form for manufacture of yeast

extracts, baker’s yeast or for poultry feed purpose.

o Use of fusel oil and impure spirits in alcohol based perfumes and
colognes or as industrial solvents.

Only spent wash is the type of by product that requires being properly treated,
and is otherwise considered to be an effluent. The treatment of spent wash has
been a heated topic of research and development over recent years and
technologies to do so are debated and tested across the country. Most recently,
the CPCB (Central Pollution Control Board) government of India has mandated
the ZLD/ZSD norms (Zero liquid/spent wash discharge) to enforce strict
pollution regulation caused by spent wash discharge. Here spent wash treatment
is done with the following objectives:

1. To reduce the volume of spent wash volume with the help of multi-effect
evaporator setup.
2. To reduce the BOD and COD value of raw spent wash by anaerobic digestion
done with bacteria releasing biogas consisting of mainly methane.

The treatment of spent wash is important because it is a liquid effluent with a lot of
organic carbon load, apart from the usual concern of BOD and COD increasing
characteristic, its pH also stands as a reason why it cannot be directly applied to
land areas with low carbon content, which tends to make the soil acidic. Therefore
raw spent wash discharge from the industry can have both water and land pollution
concerns. The spent wash generated in the Analyser column is pumped out in a
lagoon that holds the spent wash as a buffer stage. From there, it is pumped to the
bio-gas digester, while the multiple effect evaporators continuously functions to
reduce the buffered volume of spent wash in the lagoon. Another fraction of the
spent wash is pumped to the bio-composting area, where it is sprayed over press
mud to maintain a moist consistency of the compost.

Bio-gas Digester:-
The distillery has a bio-gas digester which is a cylindrical vessel made of mild
steel, with a large diameter. More precisely it is a continuous stirred tank reactor
(CSTR).

DIGESTER
Here, the raw spent wash is continuously stirred inside to maintain a homogenous
profile of biomass. This is also an anaerobic fermentation process, which is done
with bacterial strains instead of yeast as in the fermentation house. Effectively,
the purpose is to produce bio-gas which mainly consists of methane, while
simultaneously decreasing the organic carbon load of the feed. The CSTR has 6
agitators at the bottom around the circumference of the tank and one central
agitator. Raw spent wash fed to the bio-gas digester has a COD of about
120000mg/litre and is taken out at around 35000mg/litre from the manhole
openings. This is known as bio-methanated spent wash, which is sent further for
composting. Some micronutrients such as ZnCl2, CoCl2 and FeCl3 are added in
the digester. The bio-methanation takes place with the successive action of the
following kinds of bacterial strains:


Hydrolytic bacterial strains break down complex carbohydrates, fats and
 proteins into simpler soluble compounds which are further fermented to
volatile organic acids, carbon dioxide and hydrogen.
 
 Acidogenic bacterial strains process the organic acids to acetate.

 
Methanogenic bacteria process the acetate into methane and carbon dioxide.

When the methane produced develops a pressure head of around 1.2 kg/cm2 it
is sent to the boiler with the help of a blower, for combustion and generation of
steam.

Falling film type Multiple-effect evaporator:

A five effect falling film evaporator is installed here for the purpose of reducing
the effective volume of spent wash in the buffering lagoon.
This is done by film evaporation by indirect contact of steam which heats long
cylindrical calendrias through which the spent wash is passed. The evaporation
reduces the volume of the spent wash as a concentrate which is pumped back as
reflux to the lagoon simultaneously increasing its viscosity, while the
condensate obtained from evaporation and heat exchange with steam is drained
out or can be used for cleaning and washing purposes in the industry

Multiple-effect evaporator (MEE)

Bio-composting:-
A bio-composting yard, (not shown in the organizational setup schematic)
located in a separate area away from either the sugar mill or distillery, is the site
where all the organic effluent/ by product from the organization is composted in
rows of tilled biomass, largely consisting of press mud from the sugar mill and
yeast sludge from the distillery. Press mud and yeast sludge are sprayed ad
mixed with both bio-methanated as well as raw spent wash to give a continuous
moist consistency. This mixture of organic effluents is aerobically digested by a
variety of naturally growing bacteria as well as added rhizobium and
actinomycetes strains. The compost gives off a foul odour as the biomass
degrades into simpler organic compounds, which is why is remotely located.
Composting is done for 45 days where the biomass is periodically tilled using
tractors to provide a homogeneous profile. After composting, this is sold as a
form of organic fertilizer.

Raw material & Land requirement for bio-composting process of 60 KL/Day

Rectified spirit of this plant:-

Proposed capacity of the plant 60 KL/Day

Total spent wash @ KL per KL of product 05 X 60 = 300 KLPD

Number of working days in a year 270 days

Spent wash generated per year 300 X 270 = 81000
KL

Press-mud : spent wash ratio 1 : 3.5

Press-mud required per year 81000/3.5 = 23142
MT/year

Compost produced per year 23142 X 35 % = 8100
MT/year

Land required for compost plant23142 / 850 X 3 = 9.07

acres (Land required @ 850 MT/Acre per cycle)

Land required for storage of finished product

33% of annual production of compost = 2.73 acres.

Total land required for 60 KLPD project = A+B = 9.07+2.73 =11.3 Acres.

BIO-COMPOST : DISTILLERY
STANDRAD OPERATING PROCEDURE:-
1. Press-mud with maximum 75%moisture is shifted to “compost yard”
form storage yard press mud is stored (3.0 metes width and 1.00-1.10
meters height) in triangular form is called windrows the length of
windrows is depend upon requirement.
2. Turning of the windrow is done using “ compost machine” (Tractor
coupled with aerotiller machine) to homogenize the windrow& regulate
moisture in the windrow and culture is added as per requirement (solid
culture: 1Kg/MT and liquid culture :1 list/7MT.
3. Moisture content of the windrow is measured and maintains up to 50
to55%with turning and spraying of effluent if required .keep the windrow
undisturbed for 8Hrs and record the windrow temperature and pH.
4. Attached the effluent spraying hose with aerotiller machine. Start the bio-
compost lagoon pump and adjust effluent header. Spraying of effluent is
started using the compost machine after the retaining the windrow temp
60-65 0C is maintained for 20 days.
5. Effluent spraying on windrow and turning of windrow is continued for 35
days.
6. Take the temperature, moisture, C:N ratio and pH according to schedule
random sampling is done of 20% of the windrow.
7. After 35 days windrow height reduces to 0.75-1.0 meters for 60 days cycle,
effluent spraying is stopped and turning is continued without spraying. This
is done till the windrow moisture reaches to 30-35% moisture content.
8. Collect the finish product sample of ready compost for process control
analysis, at this stage two windrows can be clubbed to form one windrow
so as to make space.
9. When the material is found s per requirement, a lot no. is allotted to the
material for approximate qty of 500 MT.
10.Product analysis request for approval of each lot is given to QA
department mentioning the windrows numbers.
11.Collect the finish compost of separate lot from the windrows and make
heaps in the finish product storage shed.
12. When the material is approved by QA, dispatch the finished product
according to demand.

13.Quality of Bio-compost should be as under-


Moisture content 30-35%


Nitrogen content 1.8-2.5%

Potassium content 1.5-2.0%

Phosphorous content 2.0-2.6%

Organic carbon content 20-25%

pH 7.0-7.5

Digester performance is analysed by following factors:-


Percentage COD removal Normally COD reduction is 65-75%

Volatile acid Less volatile is good for process.

Alkalinity Alkalinity related with volatile acid formation
and CH4 gas production.

Gas generation rate Methane generation per unit volume
per day per kg COD removed.

Methane content in Bio-gas normally CH4 content in Bio-gas 55-60%.

The Process (Automation and Instrumentation control)

Overview of Automation and continuous control systems:-
Automation or automatic control is the use of various control systems for
operating equipment such as machinery, processes in factories, boilers and
switching on telephone networks, steering and stabilization of ships, aircraft and
other applications with minimal or reduced human intervention. The biggest
benefit of automation is that it saves labour; however, it is also used to save
energy and materials and to improve quality, accuracy and precision. The
advanced type of automation is feedback control, which is usually continuous
and involves taking measurements using a sensor and making calculated
adjustments to keep the measured variable within a set range. This is known as
a continuous control system.

Programmable Logic Controllers (PLC):

A programmable logic controller, (PLC) is a digital computer used for
automation of typically industrial electromechanical processes, such as control
of machinery on factory assembly lines. PLCs are used in many machines, in
many industries. PLCs are designed for multiple arrangements of digital and
analog inputs and outputs, extended temperature ranges, immunity to electrical
noise, and resistance to vibration and impact. Programs to control machine
operation are typically stored in battery-backed-up or non-volatile memory. A
PLC is an example of a real-time system since output results must be produced
in response to input conditions within a limited time. PLC architecture typically
looks like as shown below:

The functionality of the PLC has evolved over the years to include sequential
relay control, motion control, process control, distributed control systems
(DCS), and networking. The data handling, storage, processing power, and
communication capabilities of some modern PLCs are approximately equivalent
to desktop computers. PLC-like programming combined with remote I/O
hardware, allow a general purpose desktop computer to overlap some PLCs in
certain applications, but are usually used as a human interface for simulation
and display. PLCs are armoured for severe conditions (such as dust, moisture,
heat, cold), and have the facility for extensive input/output (I/O) arrangements.
These connect the PLC to sensors and actuators. PLCs read limit switches,
analog process variables (such as temperature and pressure), and the positions
of complex positioning systems. On the actuator side, PLCs operate electric
motors, pneumatic or hydraulic cylinders, magnetic relays, solenoids, or analog
outputs. The input/output arrangements may be built into a simple PLC, or the
PLC may have external I/O modules attached to a computer network that plugs
into the PLC, commonly known as a field bus as shown below:

Industrial sensors:-
As stated above, sensors are used to measure individual variables and are
located at different places throughout the plant machinery. Here, since the
process of distillation handles fluids and involves both heat and mass transfer,
following types of sensors are used:
 
 Temperature sensors mostly RTDs
 
 Pressure sensors both bourdon tube type and diaphragm types
 
 Flow meters; magnetic, orifice, nozzle and rotameter types
 
Level control valves
  
 Flow control valves
 
 Pressure control valves
 
 Temperature control relays
 
Timers

DEMINERALIZATION PLANT
DM Water:-
Demineralised water is specially purified water that has had most all of its
minerals and salts such as Calcium, Magnesium, Sodium, Chloride, Sulphate,
Nitrate, and Bicarbonate. It is also known as Deionised Water.

Demineralised water is used for industrial and scientific purposes. In this

factory it is used for preparation of reagents, distillation process and boiler.

DM Plant:-
The capacity of DM water plant is15kl. Rawwater is taken from Bore
well and it is passed through DM Plant. DM Plant is divided in to four parts-

1. Cation- here pH is adjusted to 3 by adding HCl.

2. Anion- here pH is adjusted to 8.5 by adding NaOH.
3. Degasser- it is section CO2 and unwanted gasis removed.
4. Mixed bed- (NaOH +HCl) is added here which removes total chemicals
substances.
Raw water is passed via two small polystyrene bead filled (ion exchange resins)
beds. While the cations get exchanged with hydrogen ions in first bed, the
anions are exchanged with hydroxyl ions, in the second one.

There are two basic types of resin, cation exchanger resin and anion exchanger
resin.
Cation exchanger resins will release Hydrogen ions (H+) or other positively
charged ions in exchanger for impurity cations present in the water.
Anion exchanger resins will release Hydroxyl ions (OH-) or other negatively
charged ions in exchanger for impurity anions present in the water.

Soft Water Plant:-

There are a soft water plant is stabilised. Soft water is water which has
relatively low concentration of calcium carbonate and other ions.
Soft water is used for cooling tower makeup water & process.
Soft water plant contains R Na+ resins. Here Mg+ and Ca + ions are removed
from raw water by addition of Na+. Outlet water is called Soft water.
This resin regenerated with NaCl solution.
Softener Plant capacity
Reactions:-when soft water is prepared-

R.Na+ + CaCl2 R.Ca + NaCl R.Na+

+ MgSO4 R.Mg + NaSO4 Reactions:-when

regeneration process occurs-R.Ca + NaCl

R.Na+ + CaCl2 R.Mg + NaSO4 R.Na+ +

MgSO4

D.M. PLANT
 LAB ANALYSIS PROCESS
1. Determination of brix, specific gravity and pH of the molasses:-
Brix-

Take 50 gm of molasses sample and 
add 450 ml of distilled water, mix it
till a homogenous mixture prepared.
  
The prepared sample take in jar or measuring cylinder.

Take Brix hydrometer and deep in jar or measuring cylinder and keep
floats freely and 
does not touch the bottom of the jar. Take the reading
and temperature.

Calculation-
Brix= (spindle reading + correction factor) X 10

Specific gravity-

  add 450 ml of distilled water, mix it till
Take 50 gm of molasses sample and
a homogenous mixture prepared.
  
The prepared sample take in jar or measuring cylinder.

Put the hydrometer in jar and keep freely floats, does not touch the
bottom ofthe jar and take the reading. This is the Specific gravity of
molasses.

pH-

Take prepared sample in a beaker and deep the pH paper, after
removing pH paper from sample match the colour which show on
the pH paper cover.
 
Which reading is match, is the pH of sample.

2. Determinations of Fehling factor:-
Glass ware required: Conical flask, Burette, Hot plate, Pipette,
Volumetric flask and Beaker.
Reagents required: Fehling’s A, Fehling’s B, and Methyline blue.
Procedure: Take 5gm glucose accurately and dissolve it in 500ml distill water
in volumetric flask.

 Take 5ml Fehling’s A and 5ml Fehling’s B in conical flask, Add 20 ml of
water and heat up to boiling.T

methylene blue as indicator. End
Then titrate with above solution by using
point is brick red. Take burette reading.

Calculation:-
Fehling factor = dilution factor x burette reading
 3. Determinations of TRS content of Molasses:-

Glass ware required: Conical flask, Burette, Hot plate, Pipette, Volumetric
flask andBeaker.
Reagents required: Fehling’s A, Fehling’s B, HCl, 6N NaOH, Methylene blue
and phenolphthalein indicator.
Procedure:

 Weigh 50 gm of molasses in small beaker, dissolve it and make up to 500 ml
volume in volumetric flask.

 Take  flask and add 5 ml of HCl
10 ml of above solution in another volumetric
then heat in water bath at 70°C for 15 minutes.

 Cool 
the above solution and add few drops of phenolphthalein indicator then
neutralize it with 6N NaOH, pink colour appears.
  Make up the solution to 100ml with distilled water.

Take 5ml Fehling’s A and 5ml Fehling’s B in conical flask, Add 40 ml of
 water and heat up to boiling then titrate with above pink solution by using
methylene blue as indicator . End point is brick red.
 
Take the burette reading.

Calculation-
TRS= Fehling factor X dilution factor X 100
Burette reading.

4. Determinations of RS (Residual Sugar) content of Fermented wash:-

Glass ware required: Conical flask, Burette, Hot plate, Pipette, Volumetric
flask and Beaker.
Reagents required: Fehling’s A, Fehling’s B, Methylene blue indicator.
Procedure:

Take 10 ml fermented wash sample. Makeup to 100 ml with distilled water and
filled in burette.

Take 5ml Fehling’s A and 5ml Fehling’s B in conical flask, add 40ml of water and
heat up to boiling

Then titrate with Fermented wash by using methylene blue as indicator. End point
is brick red. Take the burette reading.

Calculation-
R.S. = Fehling factor X dilution factor X 100
Burette reading

5. Determination of Unfermentable sugars in Molasses sample:-

Reagents required: Fehling’s A and Fehling’s B.
Requirements: Molasses, Yeast, Urea, DAP, and H2SO4.
Procedure:
  Weigh 12 gm of molasses and dilute with 125ml distilled water in a beaker.
  Transfer into 500 ml capacity conical flask adjusts pH to 4.5 with H2SO4.
Add 0.025gms of urea and 0.025gms 0f DAP. Then add 20 gm of Baker’s
yeast.
  Mix well and put cotton plug to flask. Keep for 24 hrs at 32°C.

After 48 hrs make volume upto 250ml with water. Mix well and filter to get 
 clear filtrate. Take 25 ml of filtrate and dilute to 100 ml then fill in burette.

Titrate with Fehling’s
A & B solutions as mentioned in Eynon and lane method.
Note burette reading.

Calculation-
U.F.S. = Fehling factor X dilution factor X 100
Burette reading

6. Determination of Alcohol loss in spent wash:


 Take 10 ml spent wash in distillation unit and distilled with
the help of 10
ml K2Cr2O7 (Potassium dichromate) and 5 ml cons. H2SO4.

 Then it titrate with ferrous ammonium sulphate and add few drops of indicator
ferroin.
 
End point is Red colour, Note the burette reading and calculate.

Calculation-
Alcohol loss%= blank reading – sample reading
Blank reading

7. Determination of Alcohol loss in head lees and PR lees:-

  Take 10 ml K2Cr2O7 (Potassium dichromate) and 5 ml cons. H2SO4 and cool it.
 
Add 10 ml sample.
If no colour change - no alcohol loss.
If colour change - alcohol loss.

it titrate with ferrous ammonium sulphate and add few
 For determination of loss %
drops of indicator ferroin.
 
End point is Red colour, Note the burette reading and calculate.

Calculation-
Alcohol loss%= blank reading – sample reading
Blank reading
8. Alcohol % in fermented wash:-
  
Take 10 ml fermented wash and maintain 100 ml with distilled water.

Take 10 ml from prepared sample and it distilled with the help of
 10 ml K 2Cr2O7 (Potassium dichromate) and 5 ml cons. H2SO4 and
cool it.

 ammonium sulphate and add few drops of
It titrate with ferrous
indicator ferroin.
 
End point is Red colour, Note the burette reading and calculate.

Calculation-
Alcohol %= blank reading – sample
reading Blank reading

9. Determination of alcohol strength and moisture:-

  
It is determination by “Karl Fisher Titrator”.
  
Switch on the titrator and start the process.
  
Add 3ml sample.
  
Note the reading and click the ppm.
  
This show the moisture content of given sample.
 
For alcohol strength = 100 – moisture reading
 Ware house
Introduction-
  The storage where alcohol is kept in distillery is called ware house.
  Ware house consists of nine receiver tank and six storage tank.

  in receiver tank. After quantifying the spirit
Daily production of spirit is collected
is pumped to main storage tanks.

 Ware house section all operation visualized by state prohibition and excise
department.

 of spirit and issue of spirit are maintained
Wash made, wash distilled, production
as per excise rules and regulation.

Capacity of receivers and storage tank:-

  Receiver material of construction: mild steel
  Number of receivers (RS): 3 capacity: 74425, 76458 and 75696 litres
  Number of receivers (ENA): 3 capacity: 75784, 75992 and 74906 litres
  Number of receivers (Ethanol): 3 capacity: 76522, 76578 and 76399 litres
  Number of storage tanks (RS): 2 capacity: 713551 and 713683 litres
  Number of storage tanks (ENA): 2 capacity: 718569 and 718389 litres
  Number of storage tanks (Ethanol): 2 capacity: 713432 and 716560 litres
 
Number of receivers (technical alcohol): 2 capacity: 45557 and 45669 litres
Denaturation:-
When the power alcohol is loaded in the tanker for selling then two chemical
are used that is Denatonium(0.04%) and Crotonaldehyde (0.02%) to give the
bitterness to power alcohol so that it cannot be used as a potable form.

BY– PRODUCTS-
  CO2:-
It is a one of the important by product in fermentation industry. Which is
produced by yeast conversion of sugars into alcohol and carbon-di-oxide.
With the help of CO2 scrubbing it collects and sent into bakery and
drinking product factory for storage.

C6H12O6 + Yeast 2C2H5OH + 2CO2 + Heat

  Fusel oil:-
Fusel oils are produced in distillation process. It is a mixture of higher
alcohol. It is used in pharmacy industry, cosmetics, perfumes, and
 chemical industry.
Fusel oil composition-
  
n-propyl alcohol
  
iso-propyl alcohol
  
n-butyl alcohol
  
iso-butyl alcohol
  
amyl alcohol
 
iso-amyl alcohol


  Bio Gas:-
It is produced in bio-digester by Methanogenic bacteria. Bio gas is used
for boiler fuel and for other cocking processes. It contains mainly
 Methane 65% and CO2 30%.
 
Bio compost:-
It is prepared with mixer of spent wash (40000-45000 COD), Press-
mud with maximum 75%moisture and culture media. It distribute to
formers as fertilizer.
Plant setup and basic configuration information
Molasses supply during production season in %
 
 Tankers (purchased from other area ): 0%
 
From Sugar section of the organization: 100%

Molasses storage tanks:

 
 Material of construction: SS-304
 
 Storage tank 1 capacity: 80000 quintals number: 1
 
 Storage tank 2 capacity: 65000 quintals number: 1
 
Day tank capacity: 200 MT number: 1


Fermentation House:
 
 Supplier: Praj Pvt. Ltd. Pune
 
 Total molasses used per fermentor: 85 tonns
 
 TRS range:47-50%
 
 Yeast vessel material of construction: stainless steel
 
 Yeast vessel 1 capacity: 80 litres number: 1
 
 Yeast vessel 2 capacity: 600 litres number: 1
 
 Yeast vessel 3 capacity: 4000 litres number: 1
 
 Pre-fermentor material of construction: stainless steel
 
 Pre-fermentor capacity: 28000 litres number: 2
 
Fermentor material of construction: Miled steel
  
 Fermentor capacity: 18000 litres number: 3
 
 Type of fermentation: Fed batch type
 
 Filling time: 11-12 hours
 
 Fermentation time: 11-12 hours
 
 Initial brix : 22.5
 
 Final specific gravity: 13-14
 
 Alcohol%: 9.5-11%
 
Sludge % in molasses : 10-12%
 
Lab Analysis procedures:

1. Lane-Eynon method of determining TRS

2. Dichromate method of determining Alcohol %

3. Strength of alcohol in product measured by: Karl-Fischer titrator

4. Unfermentable sugar% determined by yeast growth followed by Lane-

Eynon method.

5. Measurement of BOD and COD of effluent in regular time intervals.

 
 Sludge holding tank material of construction: mild steel
 
 Sludge holding tank capacity: 40981 bulk litres number: 2
 
 Clarified Wash tank material of construction: mild steel
 
Clarified Wash tank capacity: 18000 L

Distillation House:
  
 Supplier: Praj Pvt. Ltd.

  Plant feed rate and production capacity: capacity: 15000 L /H and 75KL/D
 
 Overall steam consumption rate: 310-321 tons/day

  Steam pressure: 3.9 kg/cm2

 
Number of heat exchangers: 11

 
Number of beer heaters: 2
Bio-gas Digester:
 
 Supplier: M.M. Enviro Ltd.
 
 Material of construction: mild steel type: Continuous stirred tank reactor
 
 Feed rate: 1060000L/day
 
 Feed COD initial: 100000-120000 mg/litre
 
 Feed COD final: 35000 mg/litre
 
 Number of agitators: 6

 
Methane production: 30000m3/day

Multiple-effect evaporators:
 
 Supplier: SSP ltd.
 
 Material of construction: stainless steel
 
 Number of evaporators: 5
 
 Feed capacity: 750m3/day

 
 Feed rate: 30m3/hour

 
 Feed composition initial: 4% solids
 
 Concentrate composition final: 40% solids
 
 Steam consumption rate: 12 tons/hour
 
Operating cycle time: 20 hours


 
Power consumption: 250 kW

THANK YOU
X