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CHAPTER ONE

1.Introduction
Alcohol is among the most common organic compounds. They are characterized by one or
more hydroxyl (‐OH) groups attached to a carbon atom of an alkyl group (hydrocarbon chain).
Alcohols may be considered as organic derivatives of water (H₂O) in which one of the hydrogen
atoms has been replaced by an alkyl group. Alcohols may be classified as primary, secondary, or
tertiary, according to which carbon of the alkyl group is bonded to the hydroxyl group. Most
alcohols are colourless liquids or solids at room temperature. They are used as sweeteners and in
making perfumes, are valuable intermediates in the synthesis of other compounds, and are
among the most abundantly produced organic chemicals in industry. The two best-known
alcohols are ethanol and methanol or(methyl alcohol).

1.1 Ethyl Alcohol (Ethanol)

Ethyl alcohol, also called ethanol, grain alcohol, or alcohol, a member of class of organic
compounds that are given the general name alcohols. Its molecular formula is C₂H₅OH. Ethyl is
an important industrial chemical. It is used as a solvent, in the synthesis of other organic
chemicals, and as an additive to automotive gasoline (forming a mixture known as a gasohol).
Ethyl alcohol is also the intoxicating ingredient of many alcoholic beverages such as beer, wine,
and distilled spirits. There are two main processes for the manufacture of ethyl alcohol the
fermentation of carbohydrates (the method used for alcoholic beverages) and the hydration of
ethylene. Fermentation involves the transformation of carbohydrates to ethyl alcohol by growing
yeast cells. After the fermentation process, the ethanol is purified by a multiple distillation and
rectification process. It is the principal type of alcohol found in alcoholic beverage. Hydration of
ethylene is achieved by passing a mixture of ethylene and a large excess of steam at high
temperature and pressure over an acidic catalyst.

1.2 BACKGROUND OF THE COMPANY

National Alcohol & Liquor Factory is a pioneer sole government owned state enterprise in
manufacturing & selling Liquors and Alcohol products in our Country. The factory is established
in 1928 E.C by private company and transferred to the government institute in 1969 E.C. The
factory comprises four branch factories which was once established and owned by individuals in
different period. Three of them are in Addis Ababa and the other is in Sebeta town far away from
Addis by 25 K.M. The branch factories are named as:

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 Maichew Branch Factory,
 Mekanisa Branch Factory ,
 Sebeta Branch Factory, and
 Akaki Branch Factory.

Maichew Branch Factory: The former name of this factory was “Elias Papasinos” but now
it’s named as Maichew branch Factory (head office). This factory was established and owned by
individual/ private since 1906 G.C.

Mekanisa Branch Factory: This factory is the biggest pure alcohol producer of NALF at
this moment.It‘s time-honored since 1949 E.C under Awash Wine Factory. But the factory was
not on the process for the long period of time. Since 1971 E.C through the decision of Ethiopian
government Beverage Corporation it was separated from Awash Wine Factory to join National
Alcohol and Liquor factory. On 1974 E.C the factory have got a big investment to produce Pure
Alcohol.

Sebeta Branch Factory: This factory was established and owned by individual/private in
1898 E.C to produce pure alcohol from cereal crops used by wood boiler technology. But now
the factory uses modern technology and extracts alcohol from molasses.
The Factory produces three products, namely pure alcohol, denature alcohol, and different types
of Liquors.

Akaki Branch Factory: This branch also established on 1930 E.C. The Factory used to
produce two products, namely pure alcohol & denatured alcohol from cereal crops. But now this
factory is not on the process/production. the factory comprises four branch factories which was
once established and owned by individuals in different period.

In 1976 G.C the Ethiopian Government nationalized & owned the factories under National
Alcohol & Liquor Factory. The factories, before they were nationalized by NALF, they have no
qualified personnel and enough capital. And they were on a problem. But the factories since they
were nationalized by NALF problems were solved and have got qualified personnel and capital.
Now the company is highly profitable and produces quality and competitive products with fair

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price. At present the company has 469 permanent, 92 temporary & contract employee. This
popular factory had been consistently mining a wealth of experience in industrial production and
marketing of a mix of alcohol and liquor. The present National Alcohol and Liquor Factory have
grown in to far-reaching reputation for mounting quality and taste of its variety products among
the public all over the country. The head office of the factory is located in Mexico square behind
Addis Ababa industrial Technology College the former “Tgebared”.

1.2.1 VISION OF THE FACTORY

 To maintain its leadership in the liquor industry of the country


 To improve the quality of its products
 To expand its market share
 To make at most effort to enter foreign markets and to be competent internationally

1.2.2 MISSION OF THE FACTORY

 To produce internationally recognized quality products and to satisfy and exceed


customer requirement
 The company strive to produce high quality pure alcohol, denatured alcohol and liquors
 applying modern management system and employing experienced and qualified
professionals
 Building a business based on sound customer values and principles
 Maximizing the benefits of customers needs attempt to must be strong competitor and
profitable
 To produce internationally recognized quality liquor products to the taste of costume
 Enable to contribute for the national economic development
 Protecting the environment to contribute our share of the growth of our country.

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1.2.3 PRODUCTS OF THE COMPANY

Currently National Alcohol & liquor Factory produces and distributes the following products:

 Pure Alcohol: it is the main product in the distillation process of this factory; it has 97%
alcoholic content

 Denature Alcohol: is also one of the products with an alcoholic content of 95%. It is a
by-product obtained when potable alcohol is distilled from molasses in the distillation
process. It is an ethyl alcohol made unfit for drinking but still this product uses for many
purposes. To mention few of them are: Clinical purpose, Beauty salons and barberries,
Cleaning electrical equipments & Cooking purpose.
 Liquors: Different 14 varieties of liquors are produced from pure alcohol in bottling
plant section. In the bottling plant each bottle is filled with 890ml of liquor except the
mini bottles with 250ml of liquor.

Types of liquors Concentration of Alcohol(%v/v)


Ouzo 41
Double Ouzo 43
Baro’s Dry Gin 41
Fernit 37
Bitter 15
Apretife 32
Cognac 37
Brandy 41
Coffee 30
Lemon 30
Pineapple 30
Orange 30
Pernod 45
Supermint 24

Table 1. Different variety of liquors and their alcohol concentration

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1.3 Quality control practices

There are two quality control systems:

A) Organoleptic taste: odour, taste, colour,

B) Qualitative taste: fusel oil taste, permanganate taste, apparent grade.

A) Organoleptic taste

This quality controlling system is mainly based on physical means of controlling which are
basically odour, taste and colour of the alcohol as well as the liquor

 Odour:- Should have alcoholic smell if it is pure alcohol and it should have the desired
smell of a liquor which is the same or nearly the same odor of the essence used
 Colour:- Must be colourless if it is pure alcohol and it should have the desired liquor
colour according to the liquor produced
 Taste;- Mixing 25 ml of pure alcohol 25 ml of water then taste it. If it is pure alcohol it
will have the common alcohol taste where as if it is in liquor stage it will have different
tastes according to the liquor type.

B ) Qualitative taste

This quality controlling system undergoes different chemical changes which are tested in
laboratory experiments.

 Fusel oil taste:- 25 ml of pure alcohol put on stove until evaporated (reached drop of
alcohol) then add 1ml of H₂SO₄ then must out of red & black if there is oil look red &
black.
 Permanganate taste:- add 2 ml of permanganate to 50 ml of pure alcohol then must >25
min to change colour. Apparent grade;- check the grade of alcohol to be >96.2% by
Alcohol metric measurement.

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CHAPTER TWO

2. MOLASSES TREATMENT

2.1 Raw materials used in National Alcohol & Liquor Factory:

 Molasses
 Water (soft water)
 Steam
 Sulphuric acid

Molasses:-Molasses is the by product of sugar factories. It has a brownish black color, sugar
content 78-83% brix and having 1.4-1.5 true density. It is the principal ingredient for liquor
production. In reality; the Molasses used in liquor production is a highly viscous material with
approximately 45% sugar content & it also have a lot of impurities. the amount of sugar in the
raw molasses will have a significant influence on the quality of the finished product. Molasses is
obtained from sugar factories such as Metehara,Wenji and Fincha sugar factories; it costs 70
birr/Tone. It is transported to Alcohol factories by trucks then its brix is measured and stored in
underground concrete tank.

Components Amount ( % w/w)


Sucrose 30-40
Fructose 5-12
Glucose 4-9
Reducing sugar 10-15
Water 20-30
Ash 10-12
Total sugar % dry solids 55-60
Non sugar substances 15-20
Unfermentable sugars 3-5
Table 2: composition of molasses

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Water:-Water is also another principal ingredient in the liquor production process. in order to
get rid of scale formation on the equipments soft water is used in the whole process. the main
purpose of water in the process is to dilute the raw molasses until it reaches the desired viscosity
(◦brix).

Steam:-The steam is generated from the boiler by using soft water. Furnace or benzene is used
as a source of heat to boil the water and convert it to steam. the main purpose of steam is melt
down the raw molasses to facilitate the dilution.

Sulphuric acid:-It is added in different sections of the production process. it mainly used to
kill the microorganisms in the molasses & also it provides acidic media which is suitable for the
yeasts during the yeast propagation stage.

2.2 MOLASSES TREATMENT

When molasses is the raw material for fermentation, pre-treatment improves the overall
process efficiency and also the quality of product ethanol.Raw molasses from bulk storage is
diluted with water, heated and mixed with sulphuric acid. The hot mixture is held in a retention
tank for a sufficient time to ensure production of fine-grain crystal sludge.The clarified effluent
obtained, is further diluted with water and cooled to fermentation conditions. The sludge is
washed to recover residual sugar that is recycled in the system, and then discharged to waste.
Heat is recovered by exchange between process water (mashing) and hot clarified molasses.

The advantages of molasses pre-treatment clarification are: Faster fermentation,Higher


ethanol yield during fermentation,Improved heat transfer in cooling fomenters,Reduced scaling
problems in distillation,Reduced BOD of distillers effluent. Molasses Treatment is the first step
process in National Alcohol & Liquor Factory. It is mainly concerned on killing the
microorganisms in the raw molasses, separating different dust particles from the raw molasses &
lowering the viscosity (◦Bx) of the raw molasses. this process takes place in 5 different types of
tanks:

Dilution tank 1(D-1201):- the raw molasses with 78 to 80 (◦Bx) coming from bulk storage is
pumped in this dilution tank. Mass flowmeter permits the flow control adjusting the speed
controller of pump. In this tank dilution occurs by using with white stillages coming from
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distillation unit and fresh water as integration.temperature in this dilution tank is maintained at
85°C by steam control valve and pH value is corrected at 5 by adding of sulphuric acid:sulphuric
acid injection dose is adjusted by pH control. after mixing the solution for some time then the
hot and diluted molasses with 40-45◦Bx is fed into the next treatment tank which is static
decanter(D-1202).

Static decanter 1(D-1202):-Due to the help of centrifugation caused by the movement of the
extractor inside this tank as a result sedimentation of fine-grain crystal sludge occurs. over flow
liquid molasses(treated liquid molasses)goes to the storage tank(D-1205) while under flow(semi-
sludge) is collected on the bottom and pumped to the sugar recovery tank (D-1203).

Sugar recovery tank(D-1203):-the under flow of tank 1202 which is sludge is transferred in this
tank in order to recover a part of residual sugar. then after the liquid from D-1203 goes to static
decanter 2(D-1204).

Static decanter 2(D-1204):-At this stage the waste sludge removed to the drainage while the
sugar containing liquid goes back to dilution tank 1(D-1201) & proceed the continuous process.

Storage tank(D-1205):- the over flow liquid which comes from D-1202 cooled down to 30◦c by
passing through plate type heat exchanger by the help of cooling water then Molasses is sent to
static mixer where second dilution occurs by process water in line addition. Mass flow meter
adjust the water flow rate in order to achieve the wanted final value of 26-23 ◦Bx it goes to the
storage tank(D-1205). finally treated and diluted molasses is sent to fermentation unit from this
storage tank.

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Soft water or white stilag steam

Over flow

H2SO4 1201 1204 1203


MX EX MX
Steam

Over flow

40-50°Brix Discharged sludge

T°=80-85°C

T°=31-34°C
1202
EX 1205
Process water MX

Under flow to be recycled

Static mixer 26°Brix mash

Figure 1 Process flow chart for molasses treatment

CIP CLEANING consists basically of 3 steps: wash with water, wash with caustic solution and rinsing.

In order to avoid damages of the plant due to impermissible thermal stress, cold products must not be
introduced into the hot plant. It has to be ensured that the difference between the temperature of
apparatus and the temperature of the product will not exceed 30°C After “moving” of mash (provided
during shutdown) tank is washed by process water using the CIP line that terminates with sprinkler.

 CIP solution is fed, usually for a time depending from tank dimensions. Wash one by one D-
1201, D-1203, D-1205 using dedicated manual valves
 For D-1205 provide filling at 5% and provide circulation with pump to clean recycling line

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 For decanters, cause their geometry, cleaning must be provided with mobile pipe of water
and if required by mechanical removal of dust in the bottom
 Provide washing of pumps and their lines also
 Rinse solution by process

2.3 Material balance on molasses treatment


X1 3040lt/hr
X2
.
D-4 D-3
steam@80◦C

334kg/hr

Discharge (D4) 625kg/hr

3360lit/hr

50◦bx 26˚Bx
Molasses@80˚ D-2 D-5 On line
.
3040kg/hr D-1 X3
X4 X5 X6@32˚c
3024lt/hr 50˚Bx

Steam 80˚c
Given

 Water for first dilution 3024lt/hr.(60% white stillage and process water from heat
exchanger)
 Molasses feed to D -1 =3040kg/hr.
 Recovery sugar to D-3=625kghr
 Water for second dilution =3360lt/hr.
 Density of water=1000kg/m3
 Density of molasses=1103kg/m3
 Discharge from D-4=334kg/hr.

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Assumption

 Steam is negligible
 Steady state

Material balance in D-3

X1 625 kg/hr
D-3

3024 lit/hr

Material balance in D-4

X2 3649kg/hr
D-4

Discharge = 334kg/hr

Material balance in D-1

3040kg/hr
X3
D-1
3315kg/h

80◦c
11
635kg/hr

6355KG X4
D-2

5730kg/h X5
D-5

5730kg/hr
D-1301 X6
3301kg/hr

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CHAPTER THREE
3.1 Propagation and fermentation

3.1.2 Propagation
Propagation is the production of yeast in a controlled environment. There are two propagation
tanks. In this tank low brix preparation are prepared to be suitable for yeast growth. To reduce
the brix we use water so molasses fed from online mixer to propagation and fermentation tank.
Propagation is aerobic stage.

Objective
Objective of propagation is Production of activated yeast.

3.1.3 Raw material


The raw materials used at the start of the process are as follows:

 Molasses with 26◦bx


 Process Water
 Raw yeast (saccharomyces cerevisiae)
 Di ammonium phosphate (DAP)
 Sulfuric acid (H2SO4)
 Anti-foam
 Air

Treated molasses: used to produce high amount of alcohol.


Water: used for dilution, cleaning, cooling purposes, and steam production.
Yeast- can produce alcohol from molasses (sucrose) by the way of biochemical process.
Saccharomyces scescrevices: is a type of yeast that we use during fermentation for the fast
and good production of alcohol.
Yeast select based on –fast fermentation process
_resist high alcoholic content during propagation
_produce high alcoholic product

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DAP (Di Ammonium phosphate) – main food or nutrient for yeast dilute with water and
reduce the amount up to 10%.
Anti foam – is bought from factories or mix food oil and sulfuric acid. Anti-foam is created in
the micro bio chemical reaction because of existence of protein. When foam is formed the yeast
cell is also drifted out with foam and the amount of alcohol production decrease because yeast
depopulation occurs. So we use anti foam to inhibit loss of yeast. Anti-foam agents are esters,
fatty acid, fat etc.
H2So4- use because yeasts need acidic media so by using this chemical create good and
comfortable pH and protect from microorganism such as bacteria
Air – is necessary for yeast growth and volatilities because it is aerobic reaction. Air is provided
by the air compressor before fed to propagation tank filtered and cool with cooling water from
40-50◦C to 25◦C and injected through distributor there for yeasts are doing their function actively.

3.2 Composition

Most raw materials fed are similar but differ in water and yeast amount as describe as follow:-

Raw material For first case, When there is


use dry yeast starter
Molasses 30%@26◦bx 30%@26◦bx
Process water 32% 22%
Raw yeast 5kg 10% (propagated
yeast)
DAP 230kg @10% 230kg @10%
Sulphuric acid PH from3.5-4.5 PH from 3.5-4.5
Anti-foam If it is necessary If it is necessary
Air Present Present

Table 3-1 Raw material list and its composition

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molasses

water
sulfuric acid
yeast

Propagation tank
jacketed vessel

air

3.3 FERMENTATION

Fermentation is a process in which the yeast converts the sugars from the molasses into alcohol,
carbon dioxide and heat.Alcoholic.Fermentation is a type of exothermic reaction that release heat
energy and is catalyzed by enzymes secreted by yeast as shown in the theoretical equation:

C₁₂H₂₂O₁₁ + H₂O 2C₆H₁₂O₆

C6H12O6 2C2H5OH+2CO2+heat

The alcoholic fermentation is obtained by means of two main process steps, namely the "aerobic
stage" and the "anaerobic stage". The aerobic stage basically realizes the growth of the yeast,
necessary conversion of sugar to ethanol which takes place in the anaerobic stage.

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Mash feeding: Fermentation tank 1 will be fed with 26◦Bx molasses till it reaches 20% then
7.7 m3 propagated yeast is added in a proportion of 8,000 Litter of propagated yeast for 35,000
Litter tank and again molasses is fed until the fermenter has been fed to its full operating
capacity(70%). Side entering mixers allow for homogenization of the fermenting mash, and
improve the removal of the CO2 produced, thus resulting in optimum reaction development.
When the fermenter has been fed to its full operating capacity, the feed is switched to the next
fermentation tank and the solution is leaved for 48 hours to complete the conversion. Because
fermentation is exothermic reaction there will be heat loss; in order to maintain the temperature
from 30-33◦c a jacketed vessel is used to circulate cold water. During fermentation the sugar
found in molasses is used as food for yeast as a result CO₂ is released & foam is formed.
Whenever there is foam(bubble) formation anti foam is used to settle down the solution. If the
CO₂ increased and foam thickness is increased. High chemical reaction take place during this
alcoholic content is increased. The end of fermentation there is no sign of movement except at
the sides of the tanks. Since at the end of fermentation Ale is well fermented it stays for a short
period of time. In three hours we measure for two consecutive times if the brix of the ale is
reaches 8-11 brix, transfer to the decantation tank. The two mild steel decantation tankers have a
total capacity of 60,000liters each. In the decantation tank it gives the ale more time to settle
down before transfer it to distillery when decanted ale is transferred to Distillery there is no
scaling formation this facilitates the time& product formation during Alcohol Production. The
CO2 produced in the fermentation process is sent to a scrubber where the ethanol is recovered
by absorption with water then the weak alcoholic solution recovered is fed to the fermented
mash tank, and sent to the distillation unit while scrubbed CO2 is partially released to the
atmosphere. After emptying the fermentation & propagation tanks are cleaned by caustic soda
solution and rinse by water.

3.3.1 FERMENTATION PROCESS CONTROLING METHODS


Performing physical and chemical tests to check whether the wine reaches at good fermented
stage or not and help to know at what stage the process is found and also what is its shortages.
Fermentation process controlling methods include molasses brix checkup, temperature of the
process, fermentation period, microscopic checkup, wine odor, etc…

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A) Molasses Brix
During fermentation process the sugar content of the solution should be measured within two
hours gap consecutively. If the brix decrease, the sugar is in the process of changing in to alcohol
and the remark is good. If not, we understand that the process is not in good condition. This may
happen due to an abrupt temperature change or some other reasons to traced.
B) Temperature
Due to high fermentation movement in the process, the temperature of wine will increase. To
avoid this, wine tank should be cooled with cold water, unless it may lead the process to useless.
Very slow as well rapid lift of temperature is not the sign of good fermentation process.
 Amount of yeasts transferred to fermentation is low
 There is bacterial infection
 Yeasts are very weak, etc…
 The sugar content of the molasses syrup is maximum
 The entrance temperature of the molasses syrup to fermentation tank is high, etc…

C) Fermentation period
Another fermentation controlling mechanism is the time duration that the process takes. If the
time is short, the process is fast and the reverse is true. When the fermentation process requires
longer time than the normal time, one of the following might be happened:
 Either the number of yeasts is below sufficient or highly thick molasses brix is supplied
 Micro-biological infection may happen
 Environmental temperature decrease
 Selected type of yeast cannot perform their function properly, etc…
In other case, when the fermentation process requires very short time, one of the following might
be happened.
 Less sugar containing molasses is supplied
 The environmental temperature may be maximum
 Selected types of yeast are doing their function actively, etc…

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CHAPTER FOUR
4.1 DESTILLATION SECTION

4.1.1 Process description


Distillation is the most common method of separating chemical substances based on
differences in their volatilities. It is typically performed in vertical cylindrical columns known
as “distillation towers” or “distillation columns” and is operated at continuous steady state.
Heat duty to distillation column is provided by direct injection of steam in the column bottom
or reboiling part of liquid of column bottom in a heat exchanger (called reboiler) using the
steam as hot fluid. Overhead vapors are condensed in another heat exchanger (called
condenser) that is cooled with water or chilled on depending from vapors conditions. A part of
liquid obtained in condenser is returned to upper part of column as reflux to provide cooling
and condensation of up flowing vapors thereby increasing efficiency of column and purity of
product.
When the feed has diverse compositions, liquid outlets at intervals along the column
allow 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.
The alcohol in mash produced in fermentation section is mainly ethanol, but other
minor components such as methyl alcohol, Esters, Acids, Aldehydes, can be contained in the
mash. In this case, main aim of the distillation columns is to separate the ethanol from the other
products. Distillation process of national alcohol & liquor factory produce pure alcohol &
denature alcohol. In this process the more volatile component is collected as the top product &
spent wash as the bottom product. In national alcohol & liquor factory there are four stages of
distillation process. These are analyzing or mesh column, pre distillation column, filter column,
rectification column & oil column.

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4.2 PLANT DESCRIPTION

The plant is work using fermented sugar cane molasses having an alcohol strength in the range 8-
10% vol.
In the distillation train, the following main columns may be then identified:
 C - 1510 / 1520 / 1530 Mash / Degassing / Concentration
 C - 1540 Rectification
 C - 1550 Hydro selection
 C - 1560 Fusel Oil
 C - 1570 Demethylizer

4.2.1 MESH COLUMN (distillery column) (C-1510)


Fermented mash from buffer tank enters to condenser (E-1531) for preheating by the vapour
which comes from Concentration section of Mesh column and sent to the second condenser (E-
1561) for further heating by the vapour which comes from Fusel oil column then hot mash is
pumped to the degassing column (C-1520), where the elimination of carbon and sulphur dioxide
is achieved by means of heating under vacuum conditions.
In this section the selection of copper as tray construction material has been made in order to
facilitate the removal of the volatile sulphur compounds which have a negative effect on
distillate quality: these compounds undergo a chemical reaction in presence of copper which acts
as a catalyst, renders them insoluble and removes them from the product vapour thereby
improving distillate quality.
Alcohol contained in the mash is then stripped in the mash column C-1510 and collected as
vapour in the concentration section C-1530, which operate with a minimum reflux to ensure a
cleaning of vapours and minimize any eventual entrainment. Overhead vapours feed the hydro
selection column C-1550.
The spent wash, with a residual alcohol content lower than 100 ppm which is almost zero
amount of drain discharged as slop from the mash column bottom.

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fermented Excess vapour
Condenser Heat Condenser
Mash E-1531 exchanger E-1561
1532

Vapour Condensate

1530
Vapour E-1531
E-1521 Degazing
Reflux
1520 C-1550
reboiler
1510
Mash 8m3/hr hot mash
Drainage
4.2.2 HYDROSELECTION COLUMN (C-1550)
After condensation, recovered alcohol, with an alcoholic strength variable from (40-50) °G.L is
still rich of impurities and is refined in the hydro selection column C-1550. Within this column
an extractive distillation takes place and the congeners are removed within the overhead stream.
The extractive distillation is obtained by diluting the alcohol stream with softened water and part
of the spent lees coming from rectification column bottom product.
The alcohol is recovered, at a dilution of about 10%vol, from the bottom of C-1550 and is then
sent to the rectifying column C-1540. The hydro selection column C-1550 is heated by direct
steam injection.
Vapour

Heat exchanger C-1570


D-1531 Hydros
election E-1570
Steam Excess vapour E-1551
White wash C-1550 Condensate D-1551
from rectification Condensate
Condensate reflux

10% Alcohol

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4.2.3 RECTIFYING COLUMN (C-1540)
The rectifying column C-1540 has 8 segments (stages). The feed is entered in the third 3rd stage.
The 10% alcohol feed is refluxed from its two condensers until the ethanol is concentrated up to
96.2 °G.L., extracted as a side draw few trays below the top of the column and sent to the final
demethylization stage. The rectifying overhead is condensed within plate type heat exchanger
(E-1510), mash column reboiler. The reboiler heats indirectly the mash column C-1510
vaporizing the white stillage coming from pump (P-1562) (discharge of flash drum D-1560). The
guard condenser (E-1541) achieves the condensation of any excess vapour and provide pressure
regulation for rectification column. All condensates are then collected in the reflux drum D-1541
and recycled to the rectifier as reflux and a part is sent to technical alcohol storage. The spent
lees from the bottom of rectifying column under level control, is flashed in the drum (D-1560)
for heat recovery in demetlyizing column.
First condenser:-returns the semi refluxed alcohol on the upper part of column & separate the
pure alcohol from denature.

Final condenser:-cool the denature alcohol and transferred to temporary storage.

The spent from the bottom of drum (D-1560) is partially recycled, after cooling, for dilution in
the fusel oil decanter (DS-1560) and washing column C-1580 while the remainder is then
discharged to D-1510 for vaporization and then C-1510 heating.

Denature Alcohol
Rectifying
10% Alcohol column C-1540 HHT HX E-1510
HT E-1541
Works over
C-1560
pressure >1 bar
D-1541
Steam LT
Reflux to rectification

D-1560 C-1560
White silage Hot water to

Heat
White sillage to treatment & fermentation exchanger
Pure Alcohol (96.2% Alc) Soft water
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4.2.4 DEMETHLIZING COLUMN (C-1570)
The alcohol extracted from the rectifier is fed to the demethylization column C-1570 where
practically any trace of methanol is removed. Ethanol stream rich in methanol is withdrawn from
the top of the column, and sent to the heads storage after final cooling. Purified alcohol is
removed from the bottom and also sent to the storage after final cooling.
The demethylizing column C-1570 is indirectly heated by reboiler (E-1570).
The main route of the alcohol product is then ended.
Vapour E-1571 CW
Pure Alcohol(96.2) Demithlizing
From rectification column E-1571

C-1570
Condensate
Denature Alcohol
to daily storage
4.2.5 FUSEL OIL COLUMN (C-1560)
The processing of the congeners is carried out in the fusel oil concentration column C-1560.
The feed to this column, coming from C-1550 top, contains both fusel oils and heads congeners,
which undergoes one more stage of concentration. The fusel oils are extracted as a side stream
which is fed to the decanter (DS-1560). The fusel oils from the decanter are sent to the storage,
while the heavy layer, still containing ethanol, is recycled back to the column.
The overhead vapour of the this column, after condensation is partially refluxed while the
remaining is fed to technical alcohol storage; to this storage are also sent top products of
degassing( C-1520), C-1540, high and high high tails of C-1540 and C-1560. A side stream near
to the top of C-1560 is recycled to hydro selection C-1550.
 In order to reduce the emission to the atmosphere as well as the alcohol losses, the vents
from vacuum pumps are washed in a vent scrubber C-1580. Washing liquid is white
sillage that comes from oils column bottom, after cooling, and alcohol is recovered in oils
column C-1560.

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E-1562

E-1561

HHT HHT Denature Condensate


Fusel oil
HT column HT
LT oily material to oil recovery DS-1560
LT C-1560

Congeners from WS Weak Alcohol


C-1550,10% Alc Feed back to Fusel oil column
Reflux

Denature Alcohol

4.3 Overall Distillery flow diagram


Denature alcohol

C- C-1540 C-1550 C- C-
1530 1570 156
fermented C- 0
1520
mash @8GL

=10000lit/hr

10%alc congeners
D-1531
ENA(pure

reboiier Tails

oil extracted Decanter

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CHAPTER FIVE
5.1 LIQUORS PREPARATION AND BOTTELING

5.1.1 Raw materials:-materials that are used in alcoholic liquor production of national
alcohol and liquor factory are listed below

 Pure alcohol
 Soft water
 Sugar
 Essences

5.2 PROCESS DISCRIPTION

Mixing:- First wash and clean the preparation tanks, pumps, hose, filter and preparation house.
Then transfer the pure alcohol to preparation tank and add 25% soft water then mixed by stirrer
for 45min. to prepare the selected liquor add the essence which measured by the operators and
homogenized for 45min. after 45min add soft water which 10% of the preparation pure alcohol
and wait for 30min to homogenize. By the recipe add the measured syrup and homogenize for
30min. then add soft water when the alcohol grade come good condition and homogenize for
1hr.

Filtration:- After the liquor is produced in the preparation tank, it is filtered and goes to
holding tank for temporary storage till it is filled in bottles.

Bottle washing:- Returnable empty bottles comeback from customers dirty and still labelled.
Moreover many bottles still have remains of metal closures on the bottle’s neck. For reuse, the
bottle labels and remaining part of the metal closures must be removed and the bottles are to be
thoroughly cleaned. The aim of bottles cleaning is not only to remove all visible dirt from the
inside and out of the bottles but also to ensure that the bottles have been sterilized. Cleaning
agents are alkaline and also kill micro-organisms particularly at higher temperature. Caustic soda
is used with a concentration of 1% Sodium hydroxide to which additives are added in order to
achieve better cleaning. To make this cleaning process efficient, the effective use of the
following factors has to be considered:

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A) Effect of soaking;- Removal of dirt requires a dissolving and soaking time, which is
affected by various factors. This also applies to removal of labels. The soaking time is
10-30 minutes.
B) Mechanical effect of the bottle washer:- Cleaning is reinforced by mechanical effect of
rinsing the flasks in the upper part of the bottle washer.
C) Washing temperature:- Higher temperature always speeds up removal of dirt.
Temperature of 60-85◦c is used to obtain a good biological cleaning.

Filling and capping:- Here prepared liquor is filled in washed bottles and closed up by
aluminium closures. The filled bottles are inspected manually (visually by light inspection
method) for any foreign matter before it is labelled.

Labelling:- The filled bottles are labelled manually and are inserted manually into the plastic
crates in the liquor section where as in the Mini Gin section The filled bottles are labelled using
cold glue labelling machine and go right to the filled bottle warehouse after they are inserted
manually into the plastic crates.

25
Water
Pure Alcohol
Sugar
Flavour
Colour

Mixer Storage tank


Filter press Ageing tank

Labelling Capping Filler machine


machine machine

Steam
Bottled Bottle washing
liquor Water section
demandin
g markets. Caustic soda

Bottles (recycled from markets)

figure. liquor preparation and bottling flow diagram

26
27
5.3 Utility and Application

equipment(s) Application
Mixer To control homogeneity
Extractor To extract over and under flow
Tanker(s) To dilluting‚mixing‚extracting and CIP
Heat exchanger To reduce/increase temperature
Valve(s) To control PH‚ temperature and back flows
Nozzle To transfer over and under flow
Pump To transfer heat and solution
Table 1 Types of equipment and their use in molasses treatment

Equipment Application
Tanks and drums To fermentation and propagation and as
decanter
Compressor To providing air to propagation
Fan To fermentation process
Valves To control flow
Mixer To homogenize the solution
Pump To transferring the solution
Spraying device To CIP system
Scrubber To scrub Ethanol from CO2
Table2 types of equipment and their use in fermentation

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Equipment Application
Boiler/reboiler Steam providing/reboiling
Pump Transferring of solution
Condenser Condensation and heat exchanging
Valves Control flowing
Distillation towers Distillation process
Decanters Storage purpose
Vent scrubber Washing of vent
Generator Main power source

Table 3 types of equipment and application in distillery

Equipment Their application


Boiler Steam production
Compressor Air compressor
Softener Water softening(water treatment)
Preheater Heating
Pipes and valves Transferring and controlling flows
Caramel machine Melting sugar
Filler Filling the bottles
Bottle machine Washing the bottles
Capping machine Capping the bottles
Pump Transferring liquors
Filter press Filtration of liquors

Table 4 types of equipment and their application in liquor section

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PROBLEMS INVESTIGATED IN THE OVER ALL PROCESS

 Lack of organized laboratory


 Lack of sludge treatment plant
 Safety first!!!!

 Installing CO2 recovery plant is very profitable and safe way of waste management; it is
very economical, even if it isn’t, it is not ethical to release Such amount of green house
gas(over 10,000kg/day of CO2) to the environment especially in plant(consumers of
CO2) lacking environment

 High labour request around the packaging area to lode bottles

RECOMMENDATIONS FOR THE PROBLEMS


 Properly organised laboratory which have all the equipments for the taste of:
 Sugar content analysis of the molasses and the waste sludge
 Waste composition analysis
 Molasses specialization
 Acetic and Lactic acid analyser
 Sludge treatment plant should be installed with regard to environmental protection and
additional economical benefit to the industry
 All the workers must get mouth cover because of the bad smell around the factory
 Using mechanical system to loaded the bottles.

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Conclusion
The NALF produce alcohol and denature alcohol. The alcohol use for directly to drinking and
the denature is for different purpose like beauty salon, perfume etc… the row material of the
company is molasses, it’s a byproduct of sugar factory. The factory have a four section, these are
treatment section, fermentation and propagation section, distillation section and liquor and
packaging section. There are also side plants that are cooler tower and boiler room. The factory
produce around sixteen types of alcohol.

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Reference

 Company profile
 Distillation hand books
 Internet (www.wekipedia.com)
 Personal short notes taken during the internship visits

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