University Of Khartoum

Faculty of Engineering
Chemical Engineering Department
Unit Operations Laboratory II

Distillation Experiment

GROUP (12)

Supervisor:
Eng. Nada
Prepared by:
Mohammed Ismail Abkar Bargo – 142043
Mazin Abuobida Mubarak – 142041
Amro Mohammed Osman Abdalla – 142036

August 2018
 Table of Contents
2.................................................................................................................... Objectives
3.............................................................................................................................. Aim
3................................................................................................................. Introduction
4......................................................................................................................... Theory
5.................................................................................................................... Procedure
6.................................................................................................................... Apparatus
6...................................................................................................................... Materials
6..................................................................................................... Readings and results
9.................................................................................................................... Discussion

Objectives
To study the operation of a packed bed batch rectification column under
constant or total reflux condition.

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 Aim
To operate the column under total reflux condition and estimate the minimum
number of theoretical stages required using both Fenske's equation.

Introduction
Distillation is one of the oldest and still most common methods for both the
purification and the identification of organic liquids. It is a physical process
used to separate chemicals from a mixture by the difference in how easily they
vaporize. As the mixture is heated, the temperature rises until it reaches the
temperature of the lowest boiling substance in the mixture, while the other
components of the mixture remain in their original phase in the mixture. The
resultant hot vapor passes into a condenser and is converted to the liquid, which
is then collected in a receiver flask. The other components of the mixture
remain in their original phase until the most volatile substance has all boiled off.
Only then does the temperature of the gas phase rises again until it reaches the
boiling point of a second component in the mixture, and so on.
The boiling point of a substance (determined by distillation) is a useful physical
property for the characterization of pure compounds.
At any given temperature a liquid is in equilibrium with its vapor. This
equilibrium is described by the vapor pressure of the liquid. The vapor pressure
is the pressure that the molecules at the surface of the liquid exert against the
external pressure, which is usually the atmospheric pressure. The vapor pressure
is a very sensitive function of temperature. It does not increase linearly but in
fact increases exponentially with temperature. The vapor pressure of a
substance roughly doubles for every increase in 10 °C.
When the vapor pressure of the liquid equals the applied pressure, the liquid
boils. Thus, the boiling point of a liquid is the temperature at which the vapor
pressure equals the applied pressure. The normal boiling point of a liquid is the
temperature at which the vapor pressure of a liquid equals atmospheric pressure
(1 atm).
The boiling point of a liquid is a measure of its volatility.
According to Seader (1998), distillation processes are a major component of
chemical processing with a great deal of scientific and economic significance.
A large amount of industrial distillation takes place in staged columns. Each
stage consists of a tray designed to contact rising vapor with descending liquid,
which increases the vapor composition of the more volatile component. This
process allows the separation of a wide variety of mixtures into separate
species.
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The relationship between the configuration of a distillation column and the
degree of separation achieved can be predicted using a combination of
theoretical and empirically derived models. Since complete equilibrium is
rarely achieved in any stage in distillation processes, experimental data must be
gathered in order to determine the efficiency of the column.
By collecting and analyzing samples from different stages, the efficiency of the
distillation operation can be calculated. These calculations can be used to
confirm the mathematical model for the distillation operation, and modify it for
the specific equipment being used.
A typical fractionating column usually contains between 2-4 theoretical plates,
while an industrial column can contain 20 or more theoretical plates. If the
number of equivalent plates, and the column length, are known, the height
equivalent to a theoretical plate (HETP or simply H) can be calculated. H is
defined as the length of a column divided by the number of theoretical plates in
a column.

Theory
Batch distillation with only a single still does not give a good separation unless
the relative volatility is very high. To obtain product with a narrow composition
range, a rectifying batch still is used that consist of a reboiler, a rectifying
column, a condenser, some means of splitting of a portion of condensed vapor
or distillate as reflux and the receiver. The operation of a batch still and column
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can be analyzed using the same operating line equation as for the rectifying
section of the continuous distillation:
R 1
y n+ 1= xn + x
R+1 R+1 D

For the binary system:

x 2=1−x 1 , y 2 =1− y 1

Since the slope of the operating line is R (R+1), the slope increases as the reflux
increases, until when reflux is infinite. Under total reflux slope is 1. The
operating line then coincides with the diagonal. The number of plate is
minimum at total reflux. Minimum number of plates required can be calculated
from the terminal concentration of xg and XD based on the relative volatility of
the components, which is defined in terms of equilibrium concentrations:
y2 e y1 e
α= /
x2 e x1 e

Minimum number of theoretical plates required:

xD(1−xB)
log ⁡[ ]
xB(1−xD)
N min = −1
logα

An ideal mixture follows Raoults's law, and the relative volatility is the ratio of
vapor pressure. Thus,
P1 = P'1 x1 , P2 = P'2 x2 , y1= P1/p , y2= P2/p
α = ( y 1/ x 1)/( y 2/x 2)=P' 1 /P ' 2

The final ratio does not change much over the range of temperature encountered
in a "typical column, so the relative volatility is taken as constant.

Procedure
Cooling water tank was filled with water. Then the reboiler was also filled but
with methanol-water solution with a composition in the range of 25% of
methanol by volume.
Using a digital temperature controller the process temperature was set, which
was in the range of 85 to 100 deg. C.

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The heaters and cooling water pump was started. Then Water flow rate was
adjusted to a moderate value (The bypass valve wasn't fully closed). After that
cyclic timer was set for total reflux. 25 or 30 minute later the system achieved
the steady state. Then the timer was closed for a short while, and a sample was
taken from the feed, bottom and distillate streams in order to be analyzed. Then
the samples cooled down to the room temperature, and the refractive indexes
were measured.
Cyclic timer was adjusted to desired reflux ratio for 10 to 15 min. After that
another samples was taken from both distillate and bottom product. Again the
refractive indexes was measured concur after cooling down to room
temperature. The experiment was repeated with differ set point temperatures
and reflux ratios.

Apparatus
1) Timer.
2) Packed bed batch rectification column.
3) Digital temperature controller.
4) Flask (250ml).
5) Glass test tubes.
6) Refractrometer ( Refractive index measuring device).
7) Water bottle.
8) Electricity Supply: 1 phase, 220V AC, 6.5 kW.

Materials
1) Water.
2) Ethanol.

Readings and results

Concentration of ethanol Refractometer reading (RI)
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 100 1.366
80 1.362
60 1.359
40 1.355
20 1.344
0 1.332

conc vs RI
1.37
1.36
1.36
1.36

1.34

1.33

100 80 60 40 20 0

B
Log(P) = A - C+T
For water:
A=8.07131
B=1730.62
C=233.426
For Ethanol:
A=7.68117
B=1332.04
C=199.2
Water at distillate :
1730.62
logP= 8.07131 - 1730.62+79.6 =348.81
water ethanol
Distillate 348.81 800.586
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 Bottom 509.46 1154,64

Pethanol 800.586
α top = = 348.81 =2.3
Pwater
Pethanol 1154,64
α bottom = = 509.46 =2.26
Pwater

α av =( α top∗α bottom)0.5=2.285

Nmin =log ⁡¿ ¿
Nmin=

Calculations
Water :-
B
A−
C+T
P=10

A=8.07131 , B=1730.63 , C= 233.426

T= 79.6 C ˚
P= 348.818833 mmHg
T= 89.2 C ˚
P=509.4612081 mmHg
Ethanol :-
B
A−
C+T
P=10

A=7.68117 , B=1332.04 , C=199.2

T= 79.6 C ˚
P=800.5863176 mmHg
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 T=89.2 C ˚
P= 1154.638423 mmHg

Pe
ἀ top = =2.295
Pw

Pe
ἀ Bottom= =¿ 2.266
Pw

ἀ av =(ἀ top∗ἀ Bottom )0.5= 2.280453902

x D ( 1−x B ) 0.47 ( 1−0.25 )

log( ) log( )
x B ( 1−x D ) = 0.25 ( 1−0.47 ) = 1.160119525
N min = N min =
log ( ἀ¿¿ av)¿ log( 2.280)

Discussion
Among this experiment the end compositions show that a reasonable separation
of the species in the feed stock was effected. However, data concerning the
steps within the process are not consistent with what one would expect from the
theory. Experimental data and defects within the equipment are both potential
causes of this inconsistency, and both should be addressed in order to ensure
accuracy in modeling this process.

Further experimentation is necessary to determine the steady-state

compositions. Vapor samples could be taken from every tray. Most of the
separation processes are occurring on a few trays, with the rest displaying little
performance. An additional testing regime to gather data over a wider variety
of operating conditions may be of use.

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Uncertainty and nonlinearity comes from the unsteady ambient conditions duo
to the need of adiabatic operation using an insulation.

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