Distillation

Objective:- to produce pure alcohol from fermented tela(wine)

Theory
Distillation is simply defined as a process in which a liquid or vapor mixture of two or
more substances is separated into its component fractions of desired purity, by the
application and removal of heat. The process is based on the fact that the vapor of a
boiling mixture will be richer in the components that have lower boiling points. Hence,
when this vapor is cooled and condensed, the condensate will contain more volatile
components. At the same time, the original mixture will contain more of the less volatile
material.

The primary equipment employed in the process of distillation are distillation columns,
which are designed to achieve this separation efficiently.

As stated, distillation is the process of heating a liquid until some of its ingredients pass
into the vapor phase, and then cooling the vapor to recover it in liquid form by
condensation. The main purpose of distillation is to separate a mixture by taking
advantage of different substances’ readiness to become a vapor. If the difference in
boiling points between two substances is great, complete separation may be easily
accomplished by a single-stage distillation. If the boiling points differ only slightly, many
redistillations may be required. In the simplest mixture of two mutually soluble liquids
with similar chemical structures, the readiness to vaporize of each is undisturbed by the
presence of the other. The boiling point of a 50-50 mixture, for example, would be
halfway between the boiling points of the pure substances, and the degree of separation
achieved by a single distillation would depend only on each substance’s readiness to
vaporize at this temperature.

Apparatus and chemicals used

apparatus

 Columns:- are used to separate the feed(tela) in to spent wash and

raw alcohol
 Heat exchangers(plate and shell and tube):- are used to to preheat
the tela and condense the top prodduct of the columns.
 Temperature sensors:- are used to measure temperature.
 Pressure gauge:- is used to measure pressure.
  Tubes:- are used to transport tela, steam,top product and bottom
products.
 Valves:- are used to control flow of the feed and steam in to the
column.
 Flow meter:- is used to measure the flow rate of produced alcohol

Chemicals

 Water:- used to dilute the raw alcohol in ED column.

 Tela:- the raw material for this unit operation.
 Steam:- used to separate the feed in to top and bottom product.
General Process description
In this company we use fractional distillation, separate based on temperature difference, it is
sieve tray type. Sieve tray is a metal sheet contain a number of performance that are provided
for vapor how the rising vapor can pass in the liquid flowing across the tray. The flow of vapor
must be sufficiently high to prevent weeping of liquid through holes. The “lightest” product
those with low boiling point exit from the top of column and the ‘heaviest’ product those with
highest boiling point exit from the bottom of column. This plant work using fermented wine or
mash from molasses as well as technical alcohol having alcohol strength in the range of 8-10%
GL alcohol content.
There are six columns which are degassing column, analyzer column, allied column, ED column,
stainless steel column and copper.
Mash/concentration/ degassing column
First fermented mash with 8-10% alcohol content fed from buffer tank in shell and tube
condenser in order to heat the fermented mash. The tube contains the mash and the shell
contain vapor from the analyzer column with Vapor. The fermented mash heated and the vapor
also condensate. Then the fermented mash adds to second condenser for further heating . then
the fermented mash is pumped and adds to degassing column.
Ethanol goes to top as a vapor form collect in the concentration section. There is reflux in the
degassing section to ensure quality of vapor. And minimize any eventual entrainment. Then this
vapor condenses in parallel plate heat exchanger with cooling water. Then by using pump reflux
to degassing column Used to improve quality of Ethanol product. At each reflux there is
Denature alcohol.

Process Descriptions of distillation

In Balezaf, alcohol and liquor factory the distillation process description is as follows:
Figure, Overall block diagram for distillery

1. Decanter
Decantation is a process for the separation of mixtures, by removing a layer of liquid,
generally one from which a precipitate has settled. Decanters are used to separate liquids
where there is a sufficient difference in density between the liquids for the droplets to
settle readily due to force of gravity. The fermented wine from the fermentation entered
into decantation tank where the precipitate settled after 24 hours. Then it is pumped and
passes through by flow meter and heat ex-changer then it exchange heat from spent
washes that comes from analyzer after that it feed into degassing column at a temperature
of 650c -800c.

2. Degasifying Column
Degasification is the removal of dissolved gases from liquids. The wine from the
decanter enters tangentially into this column at a temperature of 650c800c. Due to helical
motion caused by tangential injection of the feed, create sufficient time for the vapor and
the liquid phase to separate. The vapor leaves at the top of the column and passes
through plate heat exchanger. The condensing gas passes through a loop form and leaves
as degassing heads1(acetaldehyde) collected as 5L/h while the non-condensing gas
leaves as degassing vent.

The degassing vent and heads 1 are carbon dioxide and some other dissolved gases. From
the fermentation process, yeast uses sugar to produce alcohol and carbon dioxide. Carbon
dioxide is an undesired by product. The degasified wine leaves from the bottom of this
column send to analyzer column.

3. Analyzer column
It consists of a series of metal plates with hole punched in them and baffles to control the
liquid levels on the plates. The analyzer column operated under a temperature of 880c-
900c and pressure of 100-150 mbar.

It is a tray type distillation column, which contain sieve tray with two down comers in
one side. Since there might be scale fermentation in this column tray type is preferable
rather than packed type. In the fermentation process there is a formation of solid salts
from the addition of Sulphuric acid in the molasses that contain calcium ion. This
calcium sulphate forms a scale when heat is supplied in the analyzer column.

The degasified wine introduced from side of this column falls through the down comers
by gravity from one tray to another. Heat in the form of steam supplied to the base of the
column and rises via the openings on each tray. As the steam passes through the feed on
the tray, it transfers heat to the feed. Because of the heat, input from the steam the liquid
on the tray boils generating vapor that is richer in the more volatile component.

The continuous contacting between steam and liquid occurs on each tray brings about the
separation between alcoholic component with low boiling point and the spent
wash(nonalcoholic component)with higher boiling point. Some amount of alcohol
together with steam might leave with spent wash. In order to trap these steam the spent
wash water is send to 6 meter underground with larger tube and hits the ground this
made the steam to be released and send to the lower side of the analyzing column
through the pipe. Steam free spent wash water returned with a narrower tube with
increased pressure to preheat the fermented wine. The increased pressure reduces the
fouling formation in the plate heat exchanger. The vapor leaves through the top of

analyzing Column with improved alcoholic grade was sent to Aldehyde Column for
further purification.
4. Aldehyde Column
It is a packed type column operates under a temperature of 740c-760c and a pressure of
100mbar. It is used to separate highly volatile low boiling point components.

The vapor that leaves the analyzer column enters in to lower side of the aldehyde
column. The more volatile component rises into the overhead two consecutive heat
exchangers. The vapors that do not condense in the first pass to the next heat exchanger.
The non-condensing gas leaves off as a T5 vent from the last heat exchanger. The
condensing vapor in the two heat exchangers Aldehyde heads 1, amounting to about
100L/h, is drawn off from the two heat exchanger reflux loop and refluxed back to the
column. The raw alcohol portion of the feed tends to go down the column.

The product coming from this column is called raw alcohols (katikala) with alcohol
grade 35-75%v/v. It passes through plate type heat exchanger to be cooled and stored in
the shift tanker.

5. Extractive distillation column

Extractive distillation is a distillation in the presence of a miscible high boiling point
relatively non-volatile component, the solvent that forms no azeotrope with the other
components in the mixture. It used for mixtures having a low value of relative volatility,
nearing unity. It uses a separation solvent, which is generally non-volatile, has a high
boiling point and is miscible with the mixture, but does not form an azeotrope mixture.

The solvent interact differently with the components of the mixture there by causing their
relative volatilities to change. Extractive distillation column is a packed type column
operated at a temperature of 1300c-1370c and a pressure of 2.8-3 bars. The raw alcohol
that stored in a shift tanker pumped and preheated by heat exchanger passes through the
flow meter and fed into ED column. Hot water comes from striping section column that
used as a solvent pass through heat exchanger. It enters into the column at some height
above the raw alcohol for showering purpose. Steam comes from the re-boiler introduced
into the lower side of the column. It used to separate a high boiling component from the
non-volatile. The component with the greatest volatility separates out as the top and
enters into the condenser.
The vapor with a temperature of 1300c-1370c condenses by the water from the stripping
section column (T=700c), then the water recycled back to the striping section column as
re-boiler. Head3 (acetal aldehyde) is collected 100L/h from the condenser then pass
through heat exchanger and stored in the tanker. The rest refluxed back to the top side of
the column near the hot water. The bottom product consists of a mixture of the solvent
and the other component that is 8%v/v diluted alcohol, which can again be separated
easily because the solvent doesn’t form an azeotrope with it.

The diluted alcohol enters into the re-boiler and passes through the steam trap. The steam
trap holds the steam and allows the condensate to be discharged then pass through the
Heat exchanger. Both the raw alcohol from the shift tanker and the hot water from the
stripping section column preheated by the 6-8%v/v diluted alcohol in the heat exchanger.
The diluted alcohol enters into stainless steel rectification column.

6. Stripping process
The stripping section and the rectifying section can be built as a single vertical column.
However in order to make the total height shorter the two section built side by side
interconnected with tubing to return the output of the stripping unit to the rectifying
section and vice versa. However, it requires a pump to lift liquid from the bottom of the
second column to the top of the first.

It is a packed type distillation column with operating temperature of 750c820c and

pressure of 250450 mbar. The main objective of this column is to remove much of the
water contained in the feed and it separate light and fuel oil from the alcohol mixture.
Steam inters at the bottom and also the feed dilutes raw alcohol (8%v/v) inter at middle
in addition to that hot water comes from the condenser (it used as re-boiler for stripping
section) inter at the bottom parallel with steam

7.Rectification process
As the vapor moves out of the stripper, the rectifying section increases the alcohol
concentration by allowing the vapor flow to move up the column against some of the
final liquid product flow (reflux) moving down. This column operates under a
temperature of 720c-740c and a pressure of 250-450mbar.It used to upgrade the
concentration of more volatile component and it also used to separate methanol from the
mixture. In this column, the latent heat available increases the alcohol concentration as
the vapor rise. Vapor leaving from the top of the column feed in to the main condenser to
condense and the rest, which could not condense in the main condenser, passes through
vent condenser for further condensation to prevent vapor loss. The incoming water from
the cooling tower used as a cooling fluid in the condenser.

Then vapor which couldn’t condense in the two condensers released to atmosphere as
vent. Then 40L/hr of heads 2 main and 40L/hr heads 2 vents is collected from the reflux
loop and collected in a denature tank after passing through heat exchanger, while large
fraction refluxed (re circulated) into the top of the column to control the final
concentration of the product output. This reflux flow is required to produce a down ward
flowing liquid stream in the section of the column. Without the reflux stream, there can
be liquid in the rectifying section of the column, which means no separation would occur
in the rectifying section. The condensate with low grade of alcohol pumped from the
lower side of this column to the upper side of stripping column by feint pump to
strengthen its alcoholic content.

The product coming from this column, which is pure alcohol, having 96.8%v/v alcohol
grade collected at the upper side of the column and stored in pure alcohol storage tank.
The upper part of the column is made up of copper. Copper is preferable because it
improve the quality and taste of the alcohol by reacting with sulphate ion and form
copper sulphate.

Material balances
For steady process, there is no generation, consumption that means the equation becomes

Material out=Material in

Let us calculate in each column

Degassing coumn

Given wine(F)=11,000L/H, H1D=5L/H

Where F is the feed from the decanter

 Head1 (H1d)

tella (T1)
Fermented DDegasifying column

wine (F )

From the data F=11,000l/h and H1d=5l/h F=T1+H1d

T1=F-H1d=11,000l/h-5l/h=9,995l/h

Analayzer and aldehyde column

Head1a

Aldehyde column
Analyzer column
T1

Steam Spent wash Katikala

Let’s calculate the unknown variables from the above diagram

Input=out put
Thus,
T1=spentwash+head1+k
aticala
Spent wash (sw) =?
But head1a=100l/h and katikala=2000l/h
Then 10,995l/h=spent wash+100l/h+2000l/h

From this spent wash=10,995l/h-(100+2000) l/h

Spent wash=8895l/h

ED column

Head3
Hot water Diluted katikala
Extractive distillation column

Katikala

Solution steam

To calculated the amount of diluted katikala we will do both total mass balance and component
balance
Total balance
hot water(hw)+katikala(k)=head3+diluted katikala(Dk)
component balance of the alcohol
Rk*xk=Dk*xd+H3*x3 from this
Dk=(Rk*xk-H3x3)xd but from the grade reader xk=0.475 ,x3=0.8 and xd=0.125 now

Dk=((2000l/h*0.475)-(100l/h*0.8))/0.125,Dk=6960 or by using total balance

HW+Rk=H3+Dk from this HW=Dk+H3-Rk

HW=6960+100-2000

Hot water used in this column is 5060l/h

Striping section
Now to calculate the amount of leather water take the over balance of the alcohol component

Dk=diluted alcohol Lo=light oil Fo=fuse oil LW=Lease water M=mean=Vent

P=pure alcohol

From the data taken in the grade reader

Xkd=0.125, xlo=0.675, xfo=0.68, xm=xv=0.966 xp=o.97, xLw=0

M=40l/h,V=40l/h,p=800l/h,Fo=Lo=40l/h

General flow rate

Dk=Lo+Fo+M+V+Lw+P

Component balance

DK*Xd=LW*Xlw+Fo*Xfo+Lo*Xlo+M*Xm+V*Xv+P*Xp

P= ( DK*Xd-(LW*Xlw+FO*Xfo+Lo*Xlo+M*Xm+V*Xv))/XP

P=((6960*0.125)-(0*LW+40*0.68+40*0.675+30*0.966+40*0.966))/0.97
P=770L/h

Then the recycled lease water

LW=DK-(LO+FO+M+V+P)

=6960-(40+40+30+40+770)

=6040L/H