Experiment No,-3(a)

SEPARATION OF TWO MISCIBLE LIQUIDS IN A SIEVE PLATE

DISTILLATION COLUMN
Introduction

When all the components in a solution are volatile to some extent, distillation helps in separating
the components, based on their distribution between the solution and its adjoining vapor phase.
In industrial scale, the separation is conducted in multistage counter-current tower with reboiler
at the bottom and condenser at the top of tower. Distillation under total reflux involves returning
all the distillate to the top tray as reflux, and reboiling the entire residue. The feed to the tower is
fed to the reboiler under this mode.

Objective

1) To study the different parts of a distillation column;

2) To determine the performance of the column
3) To compare the experimental results with those calculated by McCabe-Thiele
method.

Theory

Refer to the text book (Mass Transfer Operations by Treybal) for McCabe- Thiele
method of estimating the number of theoretical stages. Brush up the definitions of Rectification,
Reflux, Total Condenser. Partial Condenser, Reboiler and conditions of feed. For convenience of
calculation, it is assumed that the plates of the column behave as an ideal plate or theoretical
plate where the time of contact between phases is sufficient so that the exit streams are in
equilibrium. However, in reality all the plates do not function to yield equilibrium composition
for exit streams. This has to be verified from experimental data.

Experimental Set-up

The experimental set-up consists of a column containing 16 sieve plates, reboiler,

condenser, cooler, feed tank, distillate tank, etc. and accessories like rotameter, pump, heaters,
digital temperature indicators, etc.

The students should personally observe the different parts of the set-up and present a
brief write-up on this in the report.

Contd---P/2

Mass Transfer Lab IIT Kgp 
 ‘2’

Procedure

A mixture of ethyl alcohol and water of some unknown composition is put in the rebolier
(nearly half of reboiler volume is filled up with this mixture). Its composition is determined by
the refractive index method. The reboiler heaters are then switched on. The distillation column
slowly gets heated up. The cooling water is allowed to pass through the cooler-condenser.
When considerable condensate accumulates in the distillate tank, the distillate is allowed to
enter the top plate by switching on the reflux pump.

Liquid samples are collected from alternate plate, reboiler (before start of the operation and
during the operation). The temperature at various locations is noted.

The analysis of the liquid samples is made using the technique of refractive index. The
column is operated under total reflux condition.

Data Analysis

The specifications of the distillation column are to be mentioned.

Present the calibration data of RI vs composition and determine the liquid composition on
plates, rebolier, residue and distillate.

Compare the liquid compositions obtained from plates with those from McCabe Thiele
diagram. Determine the number of plates required under total reflux condition.

Mass Transfer Lab IIT Kgp 
Mass Transfer Lab IIT Kgp