BATCH DISTILLATION COLUMN

1. OBJECTIVE:
➢ To determine mixture composition by using refractometer.
➢ To determine pressure drop over distillation column for various boil-up rate.
➢ To determine overall column efficiency.
➢ To separate liquid mixtures if different boiling points.

2. ABSTRACT:
In this experiment we have to determine the composition of ethanol and water b using
refractometer. For this purpose, we made six samples of ethanol and water and find their
refractive indexes. First sample has 100% ethanol, second sample has 80% ethanol, third
sample has 60% ethanol, fourth sample has 40% ethanol, fifth sample has 20% ethanol
and last sample has 100% water in it. We also add mixture of ethanol and water in batch
distillation column and collect five samples from the overhead and from the bottom to
determine their refractive indexes. We compared the results of the samples we made and
samples from batch distillation column and found their efficiency.

3. INTRODUCTION:
Distillation​ is the process of ​separating​ the components or substances from a liquid ​mixture​ by
using selective ​boiling ​and ​condensation​. Distillation may result in essentially complete
separation (nearly pure components), or it may be a partial separation that increases the
concentration of selected components in the mixture. In either case, the process exploits
differences in the ​volatility​ of the mixture's components. In ​industrial chemistry​,
distillation is a ​unit operation​ of practically universal importance, but it is a physical
separation process, not a ​chemical reaction​. Distillation can be done by batch distillation
column and continuous distillation column. Distillation process is the most of common
separation used in industry because it is known as 90% efficiency in separation process
and significantly user of energy in the heating process that necessarily involved. (1)​.
 Fig: 1 (Batch Distillation Column)

Batch distillation ​refers to the use of ​distillation​ in batches, meaning that a mixture is distilled to
separate it into its component fractions before the distillation still is again charged with
more mixture and the process is repeated. This is in contrast with ​continuous
distillation​ where the feedstock is added and the distillate drawn off without interruption.
Batch distillation has always been an important part of the production of seasonal, or low
capacity and high-purity ​chemicals​. It is a very frequent ​separation process​ in
the ​pharmaceutical industry (2)​. ​The column of the distillation column has many types of
tray such as
➢ Bubble cap trays
➢ Sieve trays
➢ Valve trays.
➢ Bubble Cap Trays:
A bubble cap tray has riser or chimney fitted over each hole, and a cap that covers the
riser. The cap is mounted so that there is a space between riser and cap to allow
the passage of vapors. Vapors rises through the chimney and is directed
downward by the cap, finally discharging through slots in the cap, and finally
bubbling through the liquid on the tray. The principal of bubble cap tray is not a
counter current flow but cross flow on every stage (3).
 ​Fig: 2 (Bubble Cap Tray)
➢ Sieve Trays:
Sieve trays are simply metal plates with holes in them. Vapour passes straight upward
through the liquid on the plate. The arrangement, number and size of the holes are
design parameters. Sieve trays flow with counter current flow (3).

​Fig: 3 (Sieve Tray)

➢ Valve Trays:
In valve trays, perforations are covered by liftable caps. vapor flows lifts the caps, thus
self-creating a flow area for the passage of vapor. The lifting cap directs the vapor
to flow horizontally into the liquid, thus providing better mixing than is possible
in sieve trays (3).

Fig: 4 (Valve Tray)

4. APPARATUS DESCRIPTION:
The equipment is mounted on a floor standing, welded tubular steel framework with four
adjustable feet. The equipment comprises a 50 mm diameter sieve plate column made up
of two glass sections each contain four sieve plates. The columns are separated by a
central feed section and arranged vertically for counter-current vapor/liquid flow. Also,
installed within the framework are: (4)
 ➢ Reboiler
➢ Condenser
➢ Top product lank
➢ Decanter
➢ Reflux valve
➢ Vacuum
➢ Pump

Fig: 5 (Process Flow Sheet of Batch Distillation Column)

5. PROCEDURE:
➢ First I prepared six samples containing ethanol and water (10 ml). First sample
contain 100% ethanol, second sample has 80% ethanol, third sample has 60%
ethanol, fourth sample has 40% ethanol, fifth sample has 20% ethanol and last
sample has 100% water in it.
➢ Then I found the refractive indexes of these samples with the help of
refractometer.
➢ On the other hand, I set up the batch distillation column at total reflux so the
charge of feed mixture can be loaded directly into the reboiler through the filter
cap provided without first charging the feed tank. At total reflux there will be no
feed or top product or bottom product.
➢ I left the apparatus for at least 30 minutes so that the system can reach an
equilibrium condition after setting the heat controller.
➢ After this I took a small sample of the overheads through the valve V3 and a small
sample from bottom through the valve V2.
➢ I took for more samples after 10 minute interval for each sample from overhead
and bottom and found their refractive indexes through refractometer.
 ➢ Then I draw the graph between refractive index and composition of the sample
from the apparatus and the samples I made to compare the results.
➢ At the end I found the efficiency of the column.
6. RESULTS AND CALCULATIONS:
Refractive index of pure water = 1.33
Refractive index of ethanol = 1.361

Composition of Water % Composition of Ethanol % Refractive index

100 0 1.327

80 20 1.334

60 40 1.346

40 60 1.356

20 80 1.361

0 100 1.363

Table: 1

Fig: 6 (Refractive Index VS % of Ethanol)

I found the refractive index of overhead and bottom samples from batch distillation column. I
found their composition by using two point slope formula and found the value of x.
x−x1 y−y
x −x
= y −y1
2 1 2 1
 x−40 1.354−1.35
60−40
= 1.355−1.35

x = 56%

We can find the composition of remaining samples of ethanol and water by this method.
After this, to find the efficiency of column number of theoretical plates and number of
actual plates must be known. Number of theoretical plates can be found by Fenske’s
Method:
[log( )d×( )b]
xA xB
xB xA
n+1= log(αAB )av

Where;
n = Number of Theoretical plates
x​A​ = Mole Fraction of More Volatile Component
x​b​ = Mole Fraction of Less Volatile Component
α​AB​ = Average Relative Volatility = 10.575 (from literature)

Overhead Bottom Efficiency %

R.I thanol % R.I Water %

1.354 56 1.352 48

1.355 60 1.355 60

1.356 64 1.356 64

1.357 68 1.354 56

1.359 76 1.355 60

7. DISCUSSION:
The main purpose of this experiment is to determine the refractive index of water and ethanol
mixture. Samples with different mole fractions of ethanol and water were prepared and
each of the samples refractive index was measured by using refractometer. From the
result obtained from the experiment, graph of refractive index versus composition of
ethanol as in Figure 6 is plotted. Based on the graph, we can see that the graph gives us
an increasing curve.
8. REFRENCES:
1) ​Harwood & Moody 1989​, pp. 141–143
2) Perry, Robert H. & Green, Don W. (1984). ​Perry's Chemical Engineers'
Handbook​ (7th ed.). McGraw-Hill. ​ISBN​ ​978-0-07-049841-9
3) HENRY Z. KISTER, 1992, Distillation design, McGraw-Hill, New York
4) Lab Manual