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AZEOTROPIC

DISTILLATION OF
TOLUENE WITH
METHANOL

INTRODUCTION
AZEOTROPIC DISTILLATION
a mixture form an azeotrope or close boiling mixture

because the molecular interactions between them


a mixture of liquids that distil at isothermal condition but

without change in composition are called azeotrope


azeotropic distillation method use to saparate the

complex mixture (two azeotropic solvents) by entrainer.


(eg : toluene and methanol by using water or xylene as
entrainer

INTRODUCTION
AZEOTROPIC DISTILLATION
Benefits of water as entrainer :

i)very cheap
ii) environment friendly
iii) easily available
iv) can be easily disposed
low positive concentration of entrainer used to

remove solvent which is azeotrope


Can be done continously or batch- wise

INTRODUCTION
TYPES OF AZEOTROPIC
DISTILLATION
Homogenous
azeotropic
distillation
alter relative
volatility of two
azeotropic
constituents without
inducing liquid-liquid
phase saparation

Heterogenous
azeotropic distillation
alter relative
volatility and
inducing liquidliquid phase
saparation

INTRODUCTION

INTRODUCTION
BASED ON FIGURE 1.1
saparation sequence cointains two column

the first column called extractive columnbreaks the azeotrope and yield the azeotropic
constituents as the pure product
the second column called entrainer recovery
column-saparate the second azeotropic
constituent from the entrainer which is
recycled extractive column

OBJECTIVE
to determine the
displacement of
methanol and toluene
azeotrope by using
pervapouration or
extractive distillation

to investigate the
various waste
stream that
difficult
recovered with
traditional
saparation and
purification
process

to study the vapor


liquid equillibrium
(VLE) of methanol and
toluene

Objective
of the
experime
nt

to extablish
industrial
operating
conditions for the
extractive
distillation process
of methanol and
toluene by using
water as entrainer

PROBLEM STATEMENT
the complex mixture are not
easy to saparate rather than
using the azeotropic
distillation method

the relative volatility, of


the mixture are too low at
whatever pressureentrainer is introduce to
increase the relative
volatility
recovering solvent which are
expensive and large volume
needed for economic and
enviromental benefits

THEORY
Not all liquid mixtures follow Raoults Law
Binary mixtures, which form azeotropes or close-boiling mixtures
are characterized as behaving like a pure component when
submitted to a distillation process. Diagram 2.1 shows the vaporPOINT
F
liquid equillibrium (VLE) graph where the azeotrope
occur

Diagram
2.1 : Point F
is the point
where the
azeotrope of
mixture
occurs

THEORY

Function of
entrainer: To

METHODOLOGY
GENERAL START-UP PROCEDURE
Clean the 4 neck round bottom glass flask
Put into the heating mental
Connect the vertical packed column in on the
glass flask
Put thermometer in the thermo well and this
thermo- well insert in one ef the neck of the
glass
Connect top vapour outlet in glass coiled type
condensor, connect second condensor in series,
connect the coolling water in primary and chilliing
water in the secondary condensor connect flask to
condensate collection oulet

METHODOLOGY
PROCEDURE FOR DISTILLATION
Charge 3500ml to 4000ml of spent solvent mixture
into the 5000ml into the four necks round bottom
glass flask
Send the sample for analyzing content, moisture and
specific gravity
Apply the cooling water in primary condensor and
chill water in secondary condensor
Start heating and keep the solvent under reflux for
30-60 minutes
Start collection of first fraction (toluene) from the top
column, at the same time feed the water (entrainer)
from the top of the column

METHODOLOGY
PROCEDURE FOR DISTILLATION
After collecting toluene fraction send the sample for
complete analysis by GC
Stop feeding water from the top fractionation
column
Start collection of second fraction (methanol) from
the top column
Keep the reflux ratio 1:3
Check the water content of methanol ( in process
analysis), after collecting and saparating methanol
fraction completely, stop heating and cool the
remaining residue, unload residue and measure it.

METHODOLOGY
EXPERIMENTAL SET-UP

METHODOLOGY

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