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2008

Fermentation &
Distillation

Er. Raghvendra Sachan


RVS
1/1/2008
2008
Fermentation & Distillation

Er. Raghvendra Sachan


RVS
1/1/2008
Raghvendra Sachan 2
CONTENTS
1. INTRODUCATION............................................................................................................4
2. 5

3. ALCOHOLIC BEVERAGES:............................................................................................5
4. DISTILLED LIQUORS:.........................................................................................6

5. MANUFACTURE OF ALCOHOL ...................................................................................7


6. RAW MATERIAL FOR ALCOHOL INDUSTRY:...............................................7

7. ALCOHOL YIELD.................................................................................................8

8. PRODUCTION OF ETHANOL BY FERMENTATION OF SUGAR:.................9

9. BY PRODUCTS OF ALCOHOL MANUFACTURE .........................................10

10. FERMENTATION............................................................................................................11
11. DISTILLERY....................................................................................................................13
12. DISTILLATION................................................................................................................14
13. EFFLUENT TREATMENT PLANT................................................................................15
14. CALCULATION OF COD...................................................................................18

15. ENVIRONMENTAL SIGNIFICANCE OF DO...................................................19

16. BIOCHEMICAL OXYGEN DEMAND...............................................................19

17. EXPERIMENTAL DETAILS...........................................................................................20


18. BOTTLING UNIT.............................................................................................................22

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INTRODUCATION

An alcoholic beverage is a drink containing ethanol.


Ethanol is a drug, and depressant, and even though alcohol is a legal drug in most parts
of the world, many societies regulate or restrict the sale and use of it.

Ethanol (CH3CH2OH), the active ingredient in alcoholic


beverages, is almost always produced by fermentation - the metabolism of carbohydrates
by certain species of yeast in the absence of oxygen. The process of culturing yeast under
alcohol-producing conditions is referred to as brewing. Spirits are produced by
distillation of a fermented product, concentrating the alcohol and eliminating some of the
by-products.

Alcoholic beverages include low-alcohol-content


beverages produced by fermentation of sugar- or starch-containing products, and high-
alcohol-content beverages produced by distillation of the low-alcohol-content beverages.
Sometimes, the alcohol content of low-alcohol-content beverages is increased by adding
distilled products, particularly in the case of wines.

Most yeast cannot grow when the concentration of alcohol


is higher than about 18% by volume, so that is a practical limit for the strength of
fermented beverages such as wine, beer, and sake. Strains of yeast have been developed
that can survive in solutions of up to 25% alcohol by volume, but these were bred for
ethanol fuel production, not beverage production. Spirits are produced by distillation of a
fermented product, concentrating the alcohol and eliminating some of the by-products.

In many countries, alcoholic beverages are commonly


consumed at the major daily meals (lunch and dinner). Most early beers were in fact
highly nutritional and served as a means of calorie distribution

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ALCOHOLIC BEVERAGES:
Alcoholic beverages vary considerably in their ethanol
content and in the foodstuffs from which they are produced. Most alcoholic beverages
can be broadly classified as fermented beverages, beverages made by the action of yeast
on sugary foodstuffs, or as distilled beverages, beverages whose preparation involves
concentrating the ethanol in fermented beverages by distillation. The ethanol content of a
beverage is usually measured in terms of the volume fraction of ethanol in the beverage,
expressed either as a percentage or in alcoholic proof units.

• Undistilled Beverages:
These are produced by fermentation process from fruit juice or
grains. The beverages prepared from grape juice are called wines. Wines contain 18-20%
alcohol and produced by natural fermentation are called “Natural wines”. Weak natural
wines are made stronger by addition of pure alcohol from outside and are named as
Fortified wines. e.g. beer, champaigne.

• Distilled Beverages:
If the fermented liquids are distilled, most of the alcohol along
with other volatile products like flavor, essential oils, esters and higher alcohol pass over
as distillate. The distiller liquors have a high alcohol content that may go up to 50% or
more. e.g. whisky, brandy, rum, gin etc.
It implies that pure brandy, whisky will be made strictly
from their raw materials, which are cherries, malt respectively. But in the case of
blended, some part of alcohol is supplied by genuine raw material while the rest is
supplied through the spirit manufactured. While in the case of essence, only the essence
of brandy or whisky is mixed in rectified spirit. This is usually cheap and low in quality.

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DISTILLED LIQUORS:
COUNTRY LIQUOR: - Single distilled spirit
FOREIGN LIQUOR: - Double distilled spirit

COUNTRY LIQUOR is of two types

a) Plane country liquor:


It is produced by mixing alcohol (80-90%) strengthened
with DM water on a volume basis such that final strength of alcohol is 25%.

b) Spice (masala) country liquor:


It is made by mixing alcohol with water such that alcohol
is around 42.8%. Along with this, malt essence and caramel, which gives it the unique
brownish color, is also added.

FOREIGN LIQUOR is of following types:

∗ Whisky:
Made from malt spirit (malt is the technical name of germinated and dried
barley), has 40-50% alcohol.
∗ Brandy:
Made from grapes, litchis, cherries, apple has 40-50%alcohol.
∗ Rum:
Made from molasses spirit has 45-55% alcohol.
∗ Gin:
Made from maize, barley has 40-45% alcohol.

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MANUFACTURE OF ALCOHOL

In Mohan Meakin Ltd. the bulk of alcohol is being


produced from sugar cane molasses. Molasses is a thick viscous bye-product of the sugar
industry which is acidic in nature, rich in salts, dark brown in colour and it also contains
sugar which could not be crystallized. For manufacturing alcohol, the Molasses is diluted
with water into a solution containing 15-16 % of sugars. This solution is then inoculated
with yeast strain and is allowed to ferment at room temperature. The fermented wash is
distilled in a series of distillation columns to obtain alcohol of adequate/ requisite
strength and quality/ specification. This alcohol is used for various purposes including
potable and industrial. For manufacture of alcoholic beverages, the alcohol is, if
required, matured and blended with malt alcohol (for manufacture of whisky) and diluted
to requisite strength to obtain the desired type of liquor/ Indian Made Foreign Liquor
(IMFL). This is bottled in bottles of various sizes for the convenience of consumers.

RAW MATERIAL FOR ALCOHOL INDUSTRY:


In alcohol fermentation, glucose or sugar cane is the
fermentation materials. Therefore any natural product which contain this sugar can be
easily transformed into them, is a potential source of ethyl alcohol.

The raw material for alcohol industries are:

 stuff containing fermentable sugars:


e.g. Sugarcane juice, dry date molasses, fruit juice etc.
 Material containing starch or cellulose:
e.g. potato, Rice, barley, maize or wood

They are first treated to convert the starch or cellulose into the sugar’s that are then
fermented by yeast.

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ALCOHOL YIELD

If spirit=X (bulk liters) and it has Y% of alcohol in it then

ALCOHOL YIELD = (XY)/100


BASIS
For the manufacture of 1000 liters of 94.5% ethyl alcohol
Molasses 5000 g
Water 20000 lit
Yeast 2.5 kg
Sulphuric acid 0.125 lit
Urea 0.25 kg
Coal 500 kg
Plant capacity 20000 lit/day

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PRODUCTION OF ETHANOL BY FERMENTATION OF
SUGAR:

Ethyl alcohol is produced from sugar-containing material


such as molasses by fermentation process utilizing yeast enzymes to convert the sugar
into alcohol. alcoholic fermentation is the conversion of sugar into carbon dioxide gas
(CO2) and ethyl alcohol. This process is carried out by yeast enzymes. This is in fact a
complex series of conversions that bring about the conversion of sugar to CO2 and
alcohol
The most widely used molasses is obtained as a by product
in the sugar mill and contain glucose and fructose.

CHEMICAL REACTIONS:

invertase
C12H22O11 + H2O 2C6H12O6

invertase
C6H12O6 2C2H5OH + 2CO2

Side reaction
2C6H12O6 + H2O ROH + RCHO
(High mol. wt.)

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BY PRODUCTS OF ALCOHOL MANUFACTURE

i) Carbon-dioxide: large quantities are evolved during the fermentation process.


This is used in the solid form as ice.

ii) Fused oil: is a liquid with nauseating odour. It is used in confectionary and fruit
essences.

iii) Acetaldehyde: obtained during the alcohol distillation

iv) Spent wash: the residual liquor from which ethyl alcohol has been removed by
distillation. It contains nitrogenous matter which can be used as manure and
fodder.

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FERMENTATION
It involves slow decomposition of big molecules of certain
organic compounds into simpler ones under the catalytic influence of non living complex
substances called ferments. The majority of process requires oxygen and is classified as
aerobic. A few processes carried out in the absence of oxygen are called anaerobic.
Fermentation is in two parts.
Part 1
Aerobic (Oxygen is present)
This is the initial rapid process where the yeast is doubling its colony size every 4 hours.
(Usually 24-48 hours)
Part 2
Anaerobic. (No oxygen present)
Slower activity and the yeast focus on converting sugar to alcohol rather that
increasing the number of yeast cells.

ALCOHOLIC FERMENTATION:
The chief ethanol producers are fungi especially strain of
Saccharomyces cerevisiae. The yeast respires aerobically but in the absence of air they
ferment carbohydrates to ethanol and CO2. The by-product, CO2, bubbles through the
liquid and dissipates into the air. The other by-product alcohol, remains in the liquid
which is great for us but not for the yeast, as the yeast dies when the alcohol exceeds its
tolerance level.
The fermentation process has other limits such as
temperature. Greater than 27C kills the yeast less and than 15C results in yeast activity
which is too slow.
The conversion of glucose to ethanol can be represented as:

C6H12O6 2CO2 + 2C2H5OH

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The ability of yeast cells to convert sugar into Carbon
dioxide and Alcohol is down to enzymes. Several enzymes are involved each does its
step in the process. The final step is Zymase reduction which takes the end product of the
other enzymes (acetaldehyde/glycerol), and turns this into good old ethyl alcohol. Sadly
alcohol actually destroys enzymes and kills the yeast cell if in high concentrations. This
happens at different levels for different strains of yeast.. Brewers yeast cannot withstand
much beyond 5 or 6% Alcohol by volume. Wine yeast is more tolerant at a range of 10-
15%. Specially cultured strains of yeast with the correct environment can withstand
alcohol levels up to 21% alcohol.

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DISTILLERY

THERE ARE TWO TYPES OF DISTILLERISES:

1) Potable is prepared from raw material containing sugar. Firstly the alcohol is
produced from raw material and then liquor is prepared from alcohol.

2) Non potable alcohol is manufactured in the form of spirit.

The distillery industry today consists broadly of two parts,


one potable liquor and the industrial alcohol. The potable distillery producing Indian
Made Foreign Liquor and Country Liquor has a steady but limited demand with a growth
rate of about 8 per cent per annum. The industrial alcohol industry, on the other hand, is
showing a declining trend because of high price of Molasses which is invariantly used as
substrate for production of alcohol. The alcohol produced is now being utilized in the
ratio of approximately 52 per cent for potable and the balance 48 percent for industrial
use. Over the years the potable liquor industry has shown remarkable results in the
production of quality spirits.

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DISTILLATION
Distillation is the process of separation of two miscible
volatile liquids by vaporization, given that both the liquids exist in both the phases.
Distillation of raw alcoholic brews concentrates the alcohol and leaves behind many
chemicals that are not volatile at distillation temperatures
In practices distillation can be carried out by either of two
principle methods. The liquid mixture to be separated and condensing the vapor without
allowing any liquid to return to the still, and then there be no reflux.
The second method is based on the return of the part of the
condense to the still under such conditioned that this returning liquid is brought into the
condenser. Either of these methods can be conducted as a continuous or batch process.
Distillation unit consist of an analyzer (23 plates), aldehyde column and rectifier (56
plates).
The analyzer and the rectifier are connected via the 13th
plate called the adjust plate. In the rectifier section the heat is provided from the bottom
to the condenser heat exchange takes place between the vapors entering the water
flowing through condenser.

PROCESS DESCRIPTION:

In it the condensed liquid from the rectifier enters the


purification column. The steam is added to the condensed liquid and the alcohol rich
vapor is sent to the condenser that is further processed to the silent column. The silent
spirit produced from the silent column is also called E.N.A. or extra neutral alcohol,
which is double distilled alcohol generally used for making whisky.

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EFFLUENT TREATMENT PLANT
The main raw material of distillery molasses and when it is
distilled after fermentation to get alcohol, produce large quantity of liquid effluent called
“spent wash”. This spent wash contains organic matter in the effluent is therefore
required to be remove so that it can be discharged safely into the environment.
In the effluent treatment plant, set up by Mohan
Meakin ltd in March 1988, the treatment of the effluent takes place in the following
steps:
1. Anaerobic treatment i.e., biogas generation, two stage
2. Aerobic treatment i.e., secondary treatment
3. Clarification unit with chemical treatment
4. Second stage aeration unit with chemical treatment
5. Sludge decanter machine
6. Clarification by two methane separator clarifier
7. Ferti irrigation in the zeal of zero discharge
8. Fountain with atomization technique
9. Flocculation unit with R.C.C. clarifier for chemical treatment
10. Recycling of treated trade effluent for cooling purpose
Spent wash rich in organic matter from the distillery
having a temperature of 100-1020C, is cooled through heat exchangers to bring the
required temperature of 400C. This effluent is fed into METHANE REACTOR. Methane
reactor is the heart of effluent treatment plant. The biological process which includes the
degradation of higher organic compounds and reduction of BOD take place in this zone.
The methane (8, 000-9,000 NM 3/day) is recovered as a by product during the course of
BOD reduction. The methane reactor has been designed for 90% reduction in BOD.
The overflow of the methane digester is sent to the
anaerobic filter clarifiers and then to aeration basin having 3 surface aerators of 50 HP
each, to provide sufficient oxygen for the growth of aerobic bacteria responsible for
further decomposition of pollutants. The effluent of the brewery directly comes to

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aeration basin along with the anaerobic stream. This basin has been designed for 90%
reduction in BOD.
Effluent is then sent to clarifier where the sludge is
separated and dewatered through sludge decanter machine previously, sludge was been
dried by press deg dewatering machine and sludge drying beds. A part of sludge as
required is recirculated to the aeration basin. Separated sludge is used as manure in the
lawns and agricultural farms. The overflow effluent from the secondary clarifier is
further taken to the secondary stage aeration unit and clarifiers for further reduction of
the BOD value.
In this, chemical treatment is also added for the further
reduction in BOD value. The supernatant treatment trade effluent coming out from
methane separator clarifiers is partially sent to the fountain having an atomization
technique fro more natural aeration and it is used for ferti irrigation partially.
The F.L.D. and brewery bottle washing water of low BOD
value is mixed in second stage aeration for treatment with the help of chemicals, i.e.,
flocculants and polyelectrolyte.
The treated trade effluent thus coming out from the
clarifiers or flocculation unit is taken into the cooling tower and used for cooling purpose
in distillery condenser before being discharged. Ultimately treated effluent being
discharged top river Gomti is within the norms (i.e., 30pm) values led down by the
pollution control board.
Not only this, Mohan Meakins has a substantial saving of
coal in the form of biogas and reduced the coal consumption which is in the tune of 85-
90%.

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P.I Diagram of E.T. Plant

Mohan Meakin Ltd. Lucknow


Air Compressor
Spent Wash 7(a) 7(b)
P.H.E Digester 5

2
Vat Washing, 1 4 6
Distillery & Vat 3
washing brewery
Secondary treatment i.e. two stages
Bottle Washing of I.M.F.L
Anaerobic treatment i.e. two
stage followed by ClarifierBottle Washing of Country Liquor
Bottling
15 14
12 10 9 8
11

Tertiary treatment i.e.


chemical treatment

C.O.D. mg/L B.O.D mg/L T.S.S. mg/L Flow


Spent wash 60000-65000 25000-30000 4000-5000 300-350M3/D 13
1. New Digester 21000-22000 3500-4000 11000-12000
2. Old Digester Clarifier 16000-17000 2000-2500 1500-2000
3. Aeration Tank no. 1 13000-5000 600-700 2500-3000
4. Degassing Tank ..... ….. ….. ….. ….. …..
5. Secondary Clarifier 8000-10000 150-200 1200-1500 150-200M3/D
6. Aeration Tank no. 2 3000-4000 100-150 120-150
7. M.S. clarifier 7(a)-7(b) ….. ….. ….. ….. ….. …..
8. Atomization Tank ….. ….. ….. ….. ….. …..
9. Chemical Tank ….. ….. ….. ….. ….. ….. 250-300M3/D
10. Final Clarifier 300-350 50-55 100-120
11. Cooling Tower ….. ….. ….. ….. ….. …..
12. Discharge Point 200-250 30 60-90 800-900M3/D
13. Sludge Centrifuges & Sludge Beds….. ….. ….. ….. …..
14. Gas Holder ….. ….. ….. ….. ….. …..
15. Gas boiler ….. ….. ….. ….. ….. …..

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CALCULATION OF COD

FOUR SAMPLES FROM THE DIFFERENT STAGES OF E.T.P ARE TO BE TAKEN:


 0.25ml of spent wash , make volume up to 50 ml with DM water
and transfer to the conical flask, added 75ml conc. Sulphuric acid,
transferred the contents to the condenser heat exchanger for about
2-6 hours and after that 150ml DM water added followed by
cooling for about an hour.
 0.5ml from digester P1, make volume to 50ml with DM water and
transfer to the conical flask, added 75ml conc. Sulphuric acid,
transferred the contents to the condenser heat exchanger for about
2-6 hours and after that 150ml DM water added followed by
cooling for about an hour.
 0.5ml from digester outlet, make volume to 50ml with DM water
and transfer to the conical flask, added 75ml conc. Sulphuric acid,
transferred the contents to the condenser heat exchanger for about
2-6 hours and after that 150ml DM water added followed by
cooling for about an hour.
 1ml from aeration tank, make volume to 50 ml with DM water and
transfer to the conical flask, added 75ml conc. Sulphuric acid,
transferred the contents to the condenser heat exchanger for about
2-6 hours and after that 150ml DM water added followed by
cooling for about an hour.
Titrate all the 4 samples against ferrous ammonium sulphate with ferroin as an indicator.

8000(Blank titration – Sample titration) * Normality of Ferrous ammonium sulphate


COD =
ml Sample

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ENVIRONMENTAL SIGNIFICANCE OF DO

In liquid waste, DO is the factor that determine weather the


biological change are brought by anaerobic organism. It is used for oxidation of organic
and inorganic matter and produces innoculus end product.

CALCULATING DO
COLLECTION OF SAMPLE - entry of air should be avoided.
STANDARED REAGENTS FOR MEASURING DO-
Reducing agent used is 0.025N sodium thiosulphate.
Starch solution determines end point.
Standard reagent used is iodine.
End point-blue turns colorless.

BIOCHEMICAL OXYGEN DEMAND

Amount of oxygen required by bacteria while stabilizing


decomposable organic matter under aerobic condition. BOD test is used to determine the
pollutional strength of domestic and industrial waste in terms of oxygen that will require
if discharged into natural water.
How to find BOD
Adjust the sample to about 200c and aerate with diffused air to increase or decrease the
dissolved gas content of the sample to near saturation.
2 or more BOD bottles are then filled with the samples, at least one is analyzed for DO
immediately and then other one incubated for 5 days at 200C
After 5 days the amount of DO remaining in the incubated samples is determined and the
5 days BOD is calculated by subtracting 5 days results for those on day 0.

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EXPERIMENTAL DETAILS
Sugar testing:
In sugar testing two things are find out:

1) Brix:
It is the percentage of molasses solution in water by weight. Normally
available molasses has a brix is briolette. it consists of two parts, the upper part is
used to find brix, the bottom part gives the temperature, which is thus used to find
the correction to brix.

100gm molasses

900ml water

Mix

Check brix

Check the temperature

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2) Total reducing sugar (TRS)
100gm molasses

900ml water

Mix

Check brix

Check the temperature

Take 10ml solution in a pipette

Add HCl (2ml)

Boil to 70oC

Cool

Add sodium bicarbonate (neutralizer)

Titrate against fehling solution with methyl blue as indicator

Noted the reading

Formula for calculating the glucose in 100gm molasses:

Fehling factor * 100*100


Glucose in 100gm molasses = Burette reading

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BOTTLING UNIT

The rectified spirit that is obtained from the distillation


plant is stored in the storage tank and taken out according to the demand. The flavor
and essence are according the product nature. At the time of bottling strength
decreases to 42.8 % then after labeling they are packed and delivered.

Rectified spirit

Addition of essence and flavor

Filtration

Filling in the bottle capping

Sealing

Checking any particle impurity

Labeling security hologram

Packaging in cartons

Transportation unit

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