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Distillation may be defined as the separation of the

constituents of a mixtures including a liquid by partial


vaporization of the mixture and separate collection of
the vapour.
This process include-
* The separation of one liquid from non-volatile
impurities.
* The separation of one liquid from one or more other
liquids, with which it may be miscible, partially
miscible or immiscible.
• Distillation may be of four types:-
a) Simple distillation:- Simple distillation is the process of
converting a liquid into it’s vapor, recovering the liquid by
condensing the vapor, usually leading it into contact with a cold
surface.
b) Fractional distillation:- (Rectification) Fractional distillation is
the process employed to separate miscible volatile liquids
having different boiling points.
c) Steam distillation:- Steam distillation is used for the
distillation of water immiscible liquids of high boiling points. Ex.
turpentine, aniline etc.
d) Destructive distillation:- Destructive distillation is used to
describe the decomposition of a substance, usually a natural
product by heat, followed by the condensation and collection of
the volatile product decomposition.
A condenser is fundamentally a heat exchanger. The
surface of a condenser is kept cold by a stream of water
on one side.

۩ A large volume of cooling water is required on account of


the latent heat of vaporization evolved on condensing
the vapor.

♪ In cooling 1 gm of steam (100˚C), approximately 2.27KJ


heat are evolved.
۩ For liquids boiling point above 150˚C; simple air cooling is
used.
Fig: Steam – jacketed still
♫ The condenser must be constructed as to be easily
cleaned.
♫ The cooling surface must be large.
♫ The condensing surface must be a reasonably good
conduction of heat.
♫ The film of condensed liquid is bad conductor and
must be removed quickly.
♫ The warmer water in contact with the condensing
surface must be quickly carried away and it’s place
taken by fresh cold water.
¶ Recovery of alcohol in the preparation of dry extracts.

¶ Preparation of purified water, BP and water for injections,


BP by simple distillation.

♫ Purification of water by distillation is a special case


because,
☻Gases including CO2 dissolved in the raw water
must be removed.
☻The residue of solids must not be concentrated to a
point where hydrolysis occurs.
Fig: Distillation unit for purified water
The general arrangement of a Fractional distillation unit is
known here:-
۩ The mixture to be distilled is fed to the boiler and
heated, usually by a steam coil.
۩ The vapor is taken to a condenser at the top of the
column.
۩ The condensed liquid is split in a reflux divider, a suitable
quantity being returned to the column as reflux and the
remainder taken off as product.
۩ The ratio of reflux/product is known as reflux ratio.
۩ Distillation will continue until all the MVC (More Volatile
Component) has been distilled off and forms the top
product and the LVC (Less Volatile Component) is left in
the boiler to provide the bottom product.
• Fractional distillation depends upon -----
♠ heating the mixture
♠ repeatedly condensing the vapor
♠ re-heating the liquid
♠ equilibrium between liquid and vapor state

♣ From the operational point of view, Fractional distillation is a


mass transfer process.

Application: Vaccum fractionation is extensively used


for the separation of the mixed fatty acids derived from
oils and fats.
Fig: Fractional distillation column
THEORY
• A mixture of immiscible liquids begins to boil when the sum of their vapor
pressure is equal to the atmospheric pressure.

A. A high boiling point substances (turpentine 160°c) may be distilled


with water at a temperature much below its boiling point under reduced
pressure.

B. Substances of low volatility can be steam distillated when molecular


weight is considerably higher than that of water. Here, the following
equation is followed---

W1 /W2 =ρ1M1 /ρ2M2 Where,


ρ1, ρ2 = Vapor pressure of two molecules
M1, M2 = molecular weight
W1, W2 = proportion by weight
• The safety tube in the steam generator permits the
expulsion of some water if excessive pressure is
developed.
• The distillate separates into two layers (water and
other component) that are separated in a separating
funnel.
• The actual yield is greater than the calculated yield
since minute particles are carried over mechanically
by the steam.
Fig: Steam distillation apparatus
• It has a jacket and contains manholes in the top
and side for charging and discharging.
• Most volatile oils are lighter than water and will
separate from the distillate as an upper layer.
• Some volatile oils are heavier than water, here
the process is reversed.
When specific gravity = 1, separation does not
take place; then it is necessary to collect the
whole of the distillate and extract it with a volatile
solvent and subsequently distilling off the solvent
from the oil.
Fig: Still for steam distillation of volatile oils.
THANKS
GOOD BYE…
• For the determination of volatile oils in drugs.
• Distillation with toluene is used for the determination
of moisture in drugs.
• For extracting volatile oils like clove, aniseed,
eucalyptus.

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