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Signature Date
0ctobert 2023

Synopsis

The aim of the practical which was to investigate and develop an understanding of a multistage
batch distillation column operating under vacuum, to carry out material balances around the
column.

Distillation is a separation process widely used in the chemical and petrochemical industries for the
separation and purification of liquid mixtures. A distillation column operates by exploiting the
differences in the boiling points of the components in the feed mixture. In a batch distillation
process, the separation is conducted over time, and the column is typically operated under vacuum
to lower the boiling points of the components.

Using the data recorded we calculate the concentration first but since the refractive index was not
included in the table in the practical manual, I had to interpolate to determine the percentage by
weight in the first place.

Since ethanol is an alcohol, it functioned as a solute in this situation, while water served as a solvent.
Refractive indices were taken from the refractometer at the conclusion of the experiment and
recorded. Next, weight percentages were determined using the refractive indices, and these
were used to compute mole fractions. In the condenser and column, where the equilibrium phase
exists and has a continuous overflow of moles, there was a holdup of vapour and liquid that was
disregarded on the material balance.

Contents
Synopsis.................................................................................................................................................2
Introduction...........................................................................................................................................4
Theory...................................................................................................................................................5
Experimental Procedure........................................................................................................................6
Results...................................................................................................................................................7
Discussion..............................................................................................................................................8
Conclusion.............................................................................................................................................8
Reference..............................................................................................................................................9
Appendixes..........................................................................................................................................10
Introduction

Distillation is a separation process widely used in the chemical and petrochemical industries for the
separation and purification of liquid mixtures. A distillation column operates by exploiting the
differences in the boiling points of the components in the feed mixture. In a batch distillation
process, the separation is conducted over time, and the column is typically operated under vacuum
to lower the boiling points of the components. Distillation serves as a method for isolating liquids
from substances that do not readily vaporize, such as the extraction of alcoholic beverages from
fermented substances, or for separating two or more liquids with distinct boiling points, as in the
extraction of gasoline, kerosene, and lubricating oil from crude oil.

Distillation columns, which range in size from 0 to 10 m in diameter and 3 to 75 m in height, require
more engineering design flexibility than any other processing equipment. Designers must provide
consistent product purity while maintaining the required level of quality, even in the event that feed
composition varies. A distillation unit should be evaluated in conjunction with the control system
that it is connected to, as it is frequently used in conjunction with multiple independent units.
Theory

A very basic separation principle is used in distillation: to improve an effective mass transfer
between the two phases, close contact is made between the starting mixture and the second phase.
In order for the component to be separated from the feed mixture to enter the second phase, the
thermodynamic conditions are selected in this manner. The phases are then divided into two distinct
phases, each having a unique composition.

Since a fixed energy consumption can be achieved with any degree of separation by increasing the
number of equilibrium stages, it is especially well suited for high purity separations.
 S=
( )
xL
xH
T

( )
xL
xH
B

Using the separation factor—where x represents the mole fraction of a component, subscript L
stands for light component, H for heavy component, T for the top of the section, and B for the
bottom—we can define the degree of separation between two components in a column or in a
column section.

The McCabe- Thiele

The combined mass balance ("operation line") and VLE ("equilibrium line") equations can be
graphically solved with insight using the McCabe-Thiele diagram, which plots y as a function of x
along the column. Binary mixtures are its primary application. When determining the number of
theoretical stages for mixtures with constant molar flows, it is frequently utilized. It's possible that
the equilibrium relationship—y as a function of x at each stage—is not perfect. L and V are constant
within each section and the operating lines (y as a function of x between the stages) are straight in
the case of constant molar flow. The net transport of light components is shown in the upper
section, w=xDD

Reflux

Note that the reflux ratio of the batch column used in this practical is expressed as an outlet
percentage, and that the variation of this ratio with this percentage is linear. The reflux valve will be
operated with the column in the 100% reflux position and maintained there for the duration of this
practical task. All of the condensed vapor will be extracted and distilled at this point.

Experimental Procedure

1. Fill the reboiler with the mixture to be distilled (by using the filling valve with funnel provided)
until the electrical heater is completely plunged.

2. Take a sample of the initial feed mixture charged to the reboiler and measure its refractive index
by using the hand refractometer.

3. Turn the heating control to position 1, turn the potentiometer of the electrical resistor clockwise
to increase the heating power.

4. Take the mixture to its boiling point (85°C) and allow the mixture to boil until plates 1 – 7 are wet.
5. Fix the cooling water flow rate on valve V6.

6. Let the column run at total reflux until vapour appears in the condenser section.

7. Set the solenoid valve for the reflux ratio control at a constant output of 100%.

8. Start a timer, allowing the distillation process to run for 20 minutes.

9. Record the cooling water flow rate and the inlet and outlet cooling water temperatures across the
condenser during the 20-minute run.

10. Once 20 minutes has lapsed, record the volume of distillate collected in the distillate collection
tank.

11. Additionally, take samples from the distillate collection tank and the residue left in the reboiler.

12. Measure the refractive indexes of the samples by using the hand refractometer

Results
Table 1: Data Recorded

Feed 1,2 L
Concentration 1,358
Vacuum Pressure feed -0,4 mmHg
Concentration Distillate -1,3636
Volume Distillate 1,35 ml
Concentration Bottom 1,3546
Temperature Condenser 20

Table 2: refractive indexes and weight % of feed

Feed
 Refractive index Ethanol (%) Water (%)

1.3575 38 62

1.358 39 61

1.3583 40 60

Table 3: refractive indexes and weight % of distillate

Distillate

Refractive index Ethanol (%) Water (%)

1.3634 58 42
1.3636 59 39
1.3638 60 40

Table 4: refractive indexes and weight % of bottom

Bottom

Refractive index Ethanol (%) Water (%)

1.346 32 68

Table 5: Number of moles

Mol for ethanol Mol for water

Feed 0.852 3.371

Distillate 1.281 2.275

Bottom 0.695 3.774

Table 6: Mole fractions

 X ethanol X water

Feed 0.2 0.8

Distillate 0.36 0.64

Bottom 0.156 0.844

Discussion

Along with the mole fraction increasing on the distillate and decreasing at the bottoms, the
concentration of ethanol decreases on the bottoms and increases on the distillate. It has been noted
that ethanol concentration rises with increasing time. The refractive index and weight percentage
have a directly proportional relationship; that is, the higher the refractive index, the higher the
weight percentage. Since the refractive index was not included in the table in the practical manual, I
had to interpolate to determine the percentage by weight in the first place.

Since ethanol is an alcohol, it functioned as a solute in this situation, while water served as a solvent.
Refractive indices were taken from the refractometer at the conclusion of the experiment and
recorded. Next, weight percentages were determined using the refractive indices, and these
were used to compute mole fractions. In the condenser and column, where the equilibrium phase
exists and has a continuous overflow of moles, there was a holdup of vapour and liquid that was
disregarded on the material balance.

Conclusion
The aim of the practical which was to investigate and develop an understanding of a multistage
batch distillation column operating under vacuum, to carry out material balances around the column
was achieved.

Reference

Stichlmair, J.G., Klein, H. and Rehfeldt, S., 2021. Distillation: principles and practice. John Wiley &
Sons.

Górak, A. and Sorensen, E. eds., 2014. Distillation: fundamentals and principles. Academic Press.

Halvorsen, I.J. and Skogestad, S., 2000. Distillation theory. Encyclopedia of Separation Science,
pp.1117-1134.

Petlyuk, F.B., 2004. Distillation theory and its application to optimal design of separation units.
Cambridge University Press.
Appendixes

40−38
Interpolation: Feed=38+(1.358−1.3575)( )
1,3583−1,3575

x=39 , 25 %

60−58
Interpolation: Distillate=58+(1.3636−1.3634)( )
1,3638−1,3634

x=59 %

Number of moles calculation

Ethanol % weight at initial = 28.27%

39 , 25
n et h anol = = 0,852mol
46 , 06

100−39 , 25
n water= = 3,371 mol
18 , 02

Mole fraction calculation

no of moles solute
xf =
no of moles of solute+ no of moles of solvent

0.852
xf = = 0.2
0.852+ 3,371

For water: x w =1−0 ,2=0 , 8

Material Balances

Feed basis of 100 mol/hr

F=W + D

100= W+D

W = 100-D

Component balance (Ethanol)

F x f =D x D avg+ W x wfinal

100(0.2) = 0,36D + (100-D) (0,156)

20 = 0,36D +15.6 -0,156D

4.4=0,204D

∴ D=21,569 mol /hr

W= 100-21,569

= 78,431mol/hr

Q D=V x Y mix

Y mix =Y ethanol X D +Y water (1−X D )

= (38.58) (0.36) + (40.66) (1−¿0.36)

=39.91 kJ /mol

Q D=V × γ mix

= (21,569) (3.91)

= 860,82kJ/hr