HERIOT - WATT UNIVERSITY/BAKU HIGHER OIL SCHOOL

School of Engineering & Physical Sciences

3rd Year Chemical Engineering Laboratory

Laboratory Report

Name

Mehran Isgandarli

Group Number

CE-01

Experiment Title

Batch and Continuous Distillation

Date of Experiment

11.03.2016

Supervisor

Sanan Eminov

Contents
Abstract...........................................................................................................3
Introduction.....................................................................................................3
Basic theory.....................................................................................................3
Batch distillation...........................................................................................3
Continuous distillation..................................................................................4
Procedure.........................................................................................................5
Schematic drawing of batch distillation......Error! Bookmark not defined.
Results.............................................................................................................6
Batch process...............................................................................................6
Continuous process......................................................................................8
1.

Discussion of results..................................................................................9
1.1. Batch process.......................................................................................9
Continuous process......................................................................................9

Conclusion.....................................................................................................10
Appendix A....................................................................................................11

Abstract
Aim of this experiment is to investigate two types of distillation columns, namely
batch and continuous distillation. Dependence of the composition of distillate on reflux is
the matter of interest here, and first part of experiment will us various reflux ratios to see
the effect on the distillate. In continuous distillation flow rate and reflux ratio values are
set at certain value then it will be estimated how many plates this column has
theoretically. Values obtained from experiment will be compared with theoretical ones
and any reason for difference between them will be justified.

Introduction
The main objective of chemical engineering is to get useful products from raw
materials. This usually is done in reactors, but unfortunately product in most cases
contains undesirable components as well. In most chemical processes getting pure
product right after the reactor is difficult and sometimes even impossible. For this
reason there must be a chemical unit which separates components from each other.
This can be done by several methods and distillation is one of them. For distillation we
need distillation column and this experiment has been based on distillation column
working principles. Distillation columns has two types for flow: batch and continuous
distillation columns. There are some factors which affects to distillation rate and extent.
Pressure of column, reflux ratio, sieve type, size and etc. Some of these effects will be
used in this experiment and effect of them will be clarified. To design a distillation
column and to determine the size of it is key factor which is done by setting the number
of plates. In practice usually there is more plates than in theory to get most from
distillation. To sum up objective of this report can be summarized as, visualizing
distillation process, time dependence of composition in batch distillation while
composition depends on the reflux ratio and feed flow rate.

Basic theory
Distillation is a process in which a mixture of two or more substances are
separated into its component to the fractions of desired purity. Components which have
lower boiling point will be more in vapour phase and when this vapour is condensed,
liquid will contain components which have high volatility. This is the basic principle of the
distillation column. Distillation is done in two modes about which information is given
below.

Batch distillation
Some amount of mixture is fed to the batch column which is being heated up.
After sufficient heat is supplied mixture starts to vaporize and vapor leaves the column
and enters into the condenser. Liquid after the condenser is reach with high volatile
components. Some of the liquid is sent back to the column as reflux. Below basic
diagram for batch distillation is shown.

Figure 1: Illustration of batch distillation system

Continuous distillation
During continuous distillation, unlike batch process, feed is supplied to the
optimum plate of the column continuously. Entrance point is the point where
composition of feed is same with the mixture composition. Vapour from the top plate is
fed to the condenser while from the bottom plate to the reboiler. Diagram below is the
scheme of the continuous distillation system.

figure 2: continuous distillation

For designing a distillation column number of plates is the main parameter should
be considered. Composition of the mixture is used to estimate theoretical number of
plates. To find this value McCabe-Thiele diagram is used. Steps which is drawn on
diagram shows the number of steps and they are on two lines so called operating lines.
Top and bottom operating lines for which equations are given below.
Top operating line
x
R
y n=
x n+1 + d
R+1
R+1

Bottom operating line

y m=

Lm
B
x m +1
x
Vm
Vm b

Where
Lm- liquid at the bottom plate
B- bottom product
xd- distillate composition
R is reflux ratio and can be found using equation below
Ln=RD
Where

Lnamount of liquid flow at thetop of thecolumn ;

Damount of distillate ;

Bamount of bottom product .

Procedure
As mentioned before, experiment consists of two parts. First one is batch process
for which diagram is shown below.

Figure 3: Batch distillation block diagram

As it can be seen from the diagram above the process is batch, there is no constant
feed stream. Some amount of mixture is charged to the column as feed and it Is not
shown on diagram as it is not our interest here. For measuring density sample is used
before entering the column. When sufficient and desired amount of mixture is in the
column valve can be closed to start the distillation. Then reflux ratio is set to certain
value and heater is turned on. When vapor condenses sample is taken for measurment
of density. After tepmperature is above 82 degrees C, heating pover is reduced. The
data is shown in the section 4.1.2.

Figure 4: Continuous distillation block diagram

In this case feed stream is present and mixture is fed to the column at the centre plate
and the vapour and top product is extracted and given to condenser and reboiler
respectively. Somne amount of liquid after condenser returns to the column and this
process overall is continuous nonstop distillation. Flow should be controlled by valve to
keep the desired level.

Results
Batch process
Reflux set to 35%

15:52

Sample from top product

21,8

Density of
top
product
Kg/m3
822,8

15:57

Sample from top product

21,2

823

79,5

0,6

0,735

16:02

Sample from top product

20,8

824,8

79,8

0,53

0,725

16:07

Sample from top product

21,2

827,4

79,8

0,53

0,705

16:12

Sample from top product

21,5

823,6

79,8

0,53

0,730

16:17

Sample from top product

21,8

823,4

79,8

0,53

0,711

Time

T 13
C

T 12
C

x mole fraction
experim.

79,2

x mole
fractio
n
theory
0,65

0,733

Table 1: 0.35 Reflux Ratio

Batch process Refl ux ratio 35%

0.800
0.700
0.600
0.500
Mole fraction of Ethanol

Experimental values

0.400

Theoretical values

0.300
0.200
0.100
0.000
15:50

15:57

16:04

16:12

16:19

Time

Figure 5: Experimental vs theoretical at reflux ratio 35%

Reflux set to 45%
Time

11:1
5
11:2
1
11:2
8

Sample from top

product
Sample from top
product
Sample from top
product

Densit
y of
top
produc
t
Kg/m3
827

T 12
C

T 13
C

x mole
fractio
n
theory

x mole
fraction
experim.

79,8

0,53

0,693

828

80,4

0,42

0,682

830

80,7

23,
7
24,
5
23,
7

0,39

0,658

11:3
4
11:3
8
11:4
6

Sample from top

product
Sample from top
product
Sample from top
product

830

80,8

23,
2
830
80,8
23,
4
831
80,7
24,
1
Table 2: 0.45 Reflux Ratio

0,38

0,660

0,38

0,659

0,39

0,665

Batch process Refl ux ratio 45%

0.800
0.700
0.600
0.500
Mole fraction of Ethanol

Experimental values

0.400

Theoretical values

0.300
0.200
0.100
0.000
11:09 11:16 11:24 11:31 11:38 11:45 11:52
Time

Figure 6: Experimental vs theoretical at reflux ratio 35%

Refl ux 35% vs Refl ux 45%

0.7
0.6
0.5
mole fraction of ethanol

0.4

Reflux 35%

0.3

Reflux 45%

0.2
0.1
0

Time

Figure 7: Illustration of effect of reflux ratio on the top product composition

Continuous process
8

Temperatur
eC
Density
kg/m3
Mole
fraction of
ethanol

Feed

Distillate

Bottom product
(after cooling)

14.4

23

24.2

968

818,8

971,6

9,93 %

7,31 %

75,36%

Table 3: Stream properties for continuous distillation

Figure 8: Determination of theoretical number of stages

According to the figure above, the theoretical number of trays are equal to 7.

Discussion of results
Batch process

For batch process two different reflux ratio values was used to see the effect of
them on the distillate composition. 35% and 45% was chosen to be set reflux ratios.
Using T-x-y diagram with McCabe method theoretical values for distillation column was
calculated. Then experimental values was determined using Density-Temperature-Mass
fraction tables. Tables were provided by GUNT (experiment apparatus manufacturer).
Plotting distillate composition over the time it is seen that ethanol fraction is decreasing
over the time which is quite feasible. Experimental values for refluxe ratios in both cases
are larger than theoretical ones which also normal.

Continuous process
In continuous distillation column as mentioned before main factor is the number of
plates and it has been found theoretically. In data set 2 there is nothing about flow rates
of the feed which makes calculations even harder. In this case we used Aspen Hysys to
evaluate the number of plates using q line. After constructing McCabe diagram it was
found that theoretical number of trays is 7. In fact distillation column used in the
experiment has 8 plates. Generally when designing a distillation column in practice
there should be more plates than in theory as there can be some loses preventing to
achieve desired distillation.

Conclusion
Overall, all aims of this report has been achieved. Effect of changing conditions has
been discussed. All theoretical values was checked to be feasible against the
experimental ones. Experiment was carried out successfully while not considering some
data incompatibilities.

References
Separation processes A B49CA Heriot Watt University,
Batch and Continuous Rectification experiment demonstrators notes

10

Appendix A
Selected data: Data set 2/ Batch Log A
Firstly mole composition of the distillate is determined. Composition is found using T-x-y
diagram. This method is shown below.
Step1
Reflux set to 35%
T 12 (C )
15:52 Sample from top product
79,2
15:57 Sample from top product
79,5
16:02 Sample from top product
79,8
16:07 Sample from top product
79,8
16:12 Sample from top product
79,8
16:17 Sample from top product
79,8

11

Figure: T-x-y diagram

For all different temperatures shown below this estimation has been done and then experimental
composition is found.
Reflux set to 35%
density
T 12 (C )
x mole
fraction
15:52 Sample from top product
822,8
79,2
0,65
15:57 Sample from top product
823
79,5
0,6
16:02 Sample from top product
824,8
79,8
0,53
16:07 Sample from top product
827,4
79,8
0,53
16:12 Sample from top product
823,6
79,8
0,53
16:17 Sample from top product
823,4
79,8
0,53
Step 2
Reflux set to 35%
15:52
15:57
16:02
16:07
16:12
16:17

Sample from top product

Sample from top product
Sample from top product
Sample from top product
Sample from top product
Sample from top product

T 13 (C)
21,8
21,2
20,8
21,2
21,5
21,8

density
kg/m3
822,8
823
824,8
827,4
823,6
823,4

T 12
C
79,2
79,5
79,8
79,8
79,8
79,8

x mole fr

x mass fr

0,65
0,6
0,53
0,53
0,53
0,53

In the table there is only integers shown and for this reason values found has been
approximated to the nearest integer. A = (82%m, 21C) = 824.88 kg/m
B = (82%m, 22C) = 824.01 kg/m
C = (83%m, 21C) = 822.28 kg/m
D = (83%m, 22C) = 821.41 kg/m
As a result, 23 = (82%m, 21, 8 C) is produced by linear interpolation as:

23=B +

22T m
2221.8
( A B ) =824.01+
( 824.88824.01 )=824.18
2221
2221

Correspondingly, for 24 = (83%m, 21,8 C) the value 821.58 kg/m is obtained.

The value wE being sought is obtained by linear interpolation with the aid of 23 and 24 as per:

w E =82+

23M
824.18822.8
( 8382 ) =82+
( 8382 )=82.6
23 24
824.18821.58

wE = 82.6%m is found after rounding.

12

0,826
0,793
0,742
0,742
0,742
0,742