Distillation

Jaya indave
Bhumi Bhatt
• Distillation is defined as the separation of the
components of a liquid mixture by a process
involving vaporization and subsequent
condensation at another place.
 EVAPORATION DISTILLATION

Evaporation is from the surface of the Distillation is from the bulk of the
liquid. liquid.

In evaporation the solvent is generally In distillation the solvent vapours are

water which is not recovered. condensed and are collected in a
receiver.

It is a slow process. It is a fast process.

Evaporation being the operation Distillation being the operation when

when the concentrated liquid residue the condensed vapour is required.
needed
 CLASSIFICATION OF DISTILLATION
METHODS
• Simple distillation
• Flash distillation
• Fractional distillation
• Distillation under reduced pressure
• Steam distillation
• Molecular distillation
• Azeotropic and extractive distillation
• Destructive distillation
• Compression distillation
SIMPLE DISTILLATION / DIFFERENTIAL
DISTILLATION
• This process is known differential distillation,
as distillation is based on the differences in
volatilities and vapour pressures of the
components in the mixture.
• This method requires simple apparatus.
SIMPLE DISTILLATION
Principle:
• Liquid boils when its vapour pressure is equal to
atmospheric pressure.
• Simple distillation is conducted at its boiling
point.
• The higher the relative volatility of a liquid, the
better is the separation by simple distillation.
• Heat is supplied to the liquid so that it boils.
• The resulting vapour is transferred to a different
place and condensed.
• If the liquid of interest is volatile and remaining
components are nonvolatile, then simple
distillation is a useful means of purification and
separation of liquids.
Construction
• The construction of a simple distillation
apparatus is shown in Figure .
• It consists of a distillation flask with a side arm
sloping downwards.
• Condenser is fitted into the side arm by means of
a cork.
• The condenser is usually water condenser, i.e.,
jacketed for circulation of water.
• The condenser is connected to a receiver flask
using an adapter.
• On a laboratory scale, the whole apparatus is
made of glass.
Procedure:
• In the laboratory scale, the liquid to be distilled is
filled into the flask to one-half to two-third of its
volume.
• Bumping is avoided by adding small pieces of
porcelain before distillation.
• A thermometer is inserted into the cork and fixed
to the flask.
• The thermometer bulb must be just below the
level of the side arm.
• Water is circulated through the jacket of the
condenser as shown in Figure.
• The contents are heated gradually.
• The liquid begins to boil after some time.
• The vapour begins to rise up and passes down
the side arm into the condenser.
• The temperature rises rapidly and reaches a
constant value.
• The vapour is condensed and collected into
the receiver.
Applications:
(1) Simple distillation is used for the preparation
of distilled water and water for injection.
(2) Volatile and aromatic waters are prepared.
(3) Organic solvents are purified.
(4) A few official compounds are prepared by
distillation. Examples are spirit of nitrous ether
and aromatic spirit of ammonia.
(5) Non-volatile solids are separated from
volatile liquids.
DISTILLATION UNDER REDUCED
PRESSURE
Principle:
• Liquid boils when vapour pressure is equal to the
atmospheric pressure.
• If the external pressure is reduced by applying vacuum,
the boiling point of liquid decreases.
• Therefore, the liquid boils at a lower temperature.
• This principle is illustrated using an example of water.
• Water boils at 100 °C at an atmospheric pressure of
101.31 kPa (760 mm Hg).
• At 40 °C, the vapour pressure of water is approximately
9.33 kPa (70 mm Hg).
• Hence, the external pressure is reduced to 9.33 kPa
(70 mm Hg) where water boils at 40 °C.
Construction:
• It consists of a double-neck distillation flask
known as Claisen flask (Figure).
• In one of the necks of the Claisen flask, a
thermometer is fitted.
• Bumping occurs readily during vacuum
distillation.
• Placing a fine capillary tube in the second neck
of the flask can prevent bumping.
• Water bath or oil bath is used for heating.
• The Claisen flask is connected to a receiver
through a condenser.
• Vacuum pump is attached through an adapter
to the receiver.
• A small vacuum gauge (manometer) should
be inserted between the pump and the
receiver.
Working:
• The liquid to be distilled is filled one-half to
two-third volume of the flask.
• Small pieces of porcelain are added to the
liquid for facilitating distillation and prevent
bumping.
• The capillary tube and thermometer are kept
in place in the flask (Figure 7-17).
• The required vacuum is applied.
• The contents are heated gradually.
• The temperature rises and liquid gets
vaporised rapidly due to vacuum.
• The vapour passes through the condenser.
• The condensate is collected in the receiver.
Applications:
• Preventing degradation of active constituents:
as at higher temperatures, the active
constituents may undergo decomposition.
• Purification of vitamins.
• For thermolabile material.
• Disadvantages:
• In vacuum distillation, persistent foaming
occurs.
• This may be overcome by adding capryl
alcohol to the liquid or by inserting a fine air
capillary tube in the second neck of the
Claisen flask.
• The above method is not suitable for the
preparation of semisolid or solid extracts.
FLASH DISTILLATION / EQUILIBRIUM
DISTILLATION
Principle:
• When a hot liquid mixture is allowed to enter
from a high-pressure zone into a low-pressure
zone, the entire liquid mixture is suddenly
vaporised.
• This process is known as flash vaporisation.
• The individual vapour phase molecules of high
boiling fraction get condensed, while low
boiling fraction remains as vapour.
Construction:
• The construction of a flash distillation apparatus
is shown in Figure .
• It consists of a pump, which is connected to a
feed reservoir.
• Pump helps in pumping the feed into the heating
chamber which contains a suitable heating
mechanism.
• The other end of the pipe is directly introduced
into the vapour-liquid separator through a
reducing valve.
• The vapour outlet is provided at the top of the
separator and liquid outlet is provided at the
bottom.
Working:
• The feed is pumped through a heater at a
certain pressure.
• The liquid gets heated, which enters the
vapour-liquid separator through a pressure-
reducing valve.
• The individual vapour phase molecules of high
boiling fraction get condensed, while low
boiling fraction remains as vapour.
• The mixture is allowed for a sufficient time, so
that vapour and liquid portions separate and
achieve equilibrium.
• The vapour is separated through a pipe from
above and liquid is collected from the bottom of
the separator.
• By continuously feeding into the still, it is
possible to obtain continuous flash distillation.
• The operating conditions can be adjusted in such
a way that the amount of feed exactly equals the
amount of material removed.
• Therefore, vapour and liquid concentrations at
any point remain constant in the unit.
Uses:
• Flash distillation is used for separating
components, which boil at widely different
temperatures.
• It is widely used in petroleum industry for
refining crude oil.
Advantages:
• Flash distillation is a continuous process.
• It is used for obtaining multi-component
systems, especially in oil refinery.
Disadvantages:
• It is not an efficient distillation when nearly
pure components are required.
FRACTIONAL DISTILLATION
Principle:
• When a liquid mixture is distilled, the partial
condensation of the vapour is allowed to
occur in a fractionating column.
• In the column, ascending vapour from the
distillation flask is allowed to come in contact
with the condensing vapour returning to the
distillation flask .
• Equilibrium between liquid and vapour is set
up, which results in the separation of a more
volatile component.
Construction:
• The assembly of apparatus for fractional
distillation on a laboratory scale is shown in
Figure .
• The fractionating column is inserted between
the distillation flask and the condenser.
• A provision is made for the supply of heat at
the bottom of the column.
• At the top of column, a condenser is provided.
• The column has a large area for providing
sufficient flow conditions.
Working:
• The mixture to be distilled is fed to the boiler and
heated usually by steam.
• The sequence of events occurring in the fractionating
column can be illustrated using the following general
example (Figure ).
• Consider a mixture of two miscible liquids A and B
containing 20% A and 80% B.
• Liquid A (More Volatile Component, MVC) is having a
lower boiling point than B (Less Volatile Component,
LVC).
• These liquids do not produce constant boiling point
mixture.
• The boiling point composition curves of this mixture
are shown in Figure as to represent the steps (ie., in
fractions) in fractional distillation.
• (1) When the boiling point of the mixture is reached, the
vapour composition curves are drawn as shown by lowest
pair of curves. These curves indicate that the vapour
contains 60% of A.
• (2) When this vapour is condensed, the resulting liquid is
again heated to boiling point, this vapour gives the
composition containing 90% of A (second pair of curves
from the bottom).
• (3) This vapour impinging on a cool surface and gets
condensed. This fraction is revaporised by heating to its
boiling point. This boiling point curve of this indicates 98%
of A (Third pair of curves from the bottom).
• (4) This fraction of vapour impinges on a cooling surface.
This gives fourth pair of curves. Now this vapour contains
higher(more than 98%) proportion of A. i.e., vapour of pure
component.
• (5) The vapour moves to a condenser at the top of the
column and gets condensed.
• The liquid B trickles downward to the
distillation flask
• Once the low boiling point fraction has passed
over, distillation should be stopped.
• The liquid available in the distillation flask is
pure B. It can be collected as such or purified
further by simple distillation.
• Distillation is continued until all the MVC has
been distilled off from the top as the product
and the LVC is left in the distillation flask as a
separate product.
Application:
• Fractional distillation is used for the
separation of miscible liquids such as acetone
and water, chloroform and benzene.

Disadvantage :
Fractional distillation cannot be used to separate
miscible liquids, which form azeotropic
mixtures.
STEAM DISTILLATION
Principle:
• A mixture of immiscible liquids begins to boil when the sum of
their vapour pressures is equal to the atmospheric pressure.
• In case of a mixture of water and turpentine, mixture boils
below the boiling point of pure water, though the turpentine
boils at a much higher temperature than that of water.

Turpentine Turpentine + water (B.P = 95.6°C)

160°C. Vapour pressure of Vapour pressure Sum of vapour
water of Turpentine pressure

86.245 kpa 15.06 kpa 101.31 kpa(which

is normal
atmospheric
pressure)

• Thus, high boiling substances may be distilled at a

temperature much below its boiling point, when water
(steam) is used.
Construction:
• The assembly of apparatus for steam distillation on
laboratory scale is shown in Figure.
• It consists of a metallic steam can fitted with a cork
having two holes.
• Through one of the holes, a long tube is passed so as to
reach almost the bottom of the steam generator.
• This tube acts as a safety tube, which maintains the
pressure inside the steam generator.
• Through another hole, a bent tube is passed.
• The other end of the bent tube is connected to the
flask containing non-aqueous liquid through a rubber
cork.
• This tube should reach almost the bottom of the flask.
• Through the other hole of the rubber cork, a
delivery tube is inserted which connects the
flask and the condenser.
• The condenser is connected to a receiver flask
using an adaptor.
Working:
• The non-aqueous liquid is placed in the flask.
• A small quantity of water is added to it.
• Steam can is filled with water.
• The steam generator and the flask are heated
simultaneously, so that a uniform flow of steam
passes through the boiling mixture.
• The mixture gets heated.
• The steam carries the volatile oil and passes into
the condenser, which is cooled by cold water.
• The condensed immiscible liquid is collected into
the receiver.
• Distillation is continued until all the non-
aqueous liquid has been distilled.
• In the receiver, water and organic liquid form
two separate layers, which can be easily
separated using a separating flask.
• For volatile substances, which are miscible
with water, distillation with steam would
involve the same principle of fractional
distillation.
Applications:
(1) Steam distillation is used for the separation
of immiscible liquids. Example 1) toluene and
water 2)turpentine and water.
(2)It is useful in purification of liquid with high
boiling point, for example essential oil of almond
(3) Camphor is distilled by this method.
(4) Aromatic waters are prepared by this
method.
Advantage:
• Volatile oils can be separated at a lower
temperature in steam distillation, without any
decomposition and loss of aroma.
Disadvantage:
• Steam distillation is not suitable when
immiscible liquid and water react with each
other
 MOLECULAR DISTILLATION/
EVAPORATIVE DISTILLATION /SHORT
PATH DISTILLATION.
• Molecular distillation is defined as a
distillation process in which each molecule in
the vapour phase travels mean free path and
gets condensed individually without
intermolecular collisions on application of
vacuum.
Principle:
• The substances to be distilled have very low vapour
pressures.
• Examples are viscous liquids, oils, greases, waxy materials
and high molecular weight substances.
• These boil at very high temperatures.
• In order to decrease the boiling point of the liquids, high
vacuum must be applied.
• At very low pressure, the distance between the evaporating
surface and the condenser is approximately equal to the
mean free path of the vapour molecules.
• Molecules leaving the surface of the liquid are more likely
hit the condenser surface than to collide with other
molecules.
• Little or no re-condensation takes place at the surface of
the liquid.
Applications:
Molecular distillation is used for the purification
and separation of chemicals of low vapour
pressure.
(1) Purification of chemicals such as tricresyl
phosphate, phthalate and dimethyl phthalate.
(2) More frequently used in the refining of fixed
oils.
(3) Vitamin A is separated from fish liver oil.
Vitamin E is concentrated by this method from
fish liver oils and other vegetable oils.
 Falling Film Molecular Still or Wiped
Film Molecular Still
Principle:
• In this method, vaporisation occurs from a
film of liquid flowing down a heated surface
under high vacuum.
• The vapour (molecules) travels a short
distance and strikes the condenser nearby.
• Each molecule is condensed individually.
• The distillate is subsequently collected.
Construction:
• The construction of a wiped film molecular still is
shown in Figure.
• The vessel has a diameter of one metre.
• The walls of the vessel are provided with suitable
means of heating (jacket).
• Wipers are provided adjacent to the vessel wall.
• Wipers are connected to a rotating head through a
rotor.
• The condensers are arranged very close to the wall
(evaporating surface) as shown in Figure .
• Vacuum pump is connected to a large diameter pipe at
the centre of the vessel.
• Provisions are made for collecting the distillate and the
undistilled liquid residue at the bottom
Working:
• The vessel is heated by suitable means.
• Vacuum is applied at the centre of the vessel and wipers are
allowed to rotate.
• The feed is entered through the inlet of the vessel.
• As the liquid flows down the walls, it is spread to form a film by
PTFE (polytetrafluoroethylene) wipers, which are moving at a rate
of 3 metre per second.
• The velocity of the film is 1.5 metres per second.
• Since the surface is already heated, the liquid film evaporates
directly.
• The vapour (molecules) travels its mean free path and strikes the
condenser.
• The condensate is collected into a vessel.
• The residue (undistilled or mean free path not travelled) is collected
from the bottom of the vessel and re-circulated through the feed
port for further distillation.
• Capacity is about 1000 litre per hour.
Centrifugal Molecular Still
Principle:
• In this method, liquid feed is introduced into a
vessel, which is rotated at very high speed
(centrifugal action).
• On account of heating, vaporisation occurs from a
film of liquid on the sides of the vessel.
• The vapour (molecules) travels a short distance
and gets condensed on the adjacent condenser.
• Each molecule is condensed individually.
• The distillate is subsequently collected.
.
Construction:
• The construction of a centrifugal molecular still is
shown in Figure.
• It consists of a bucket-shaped vessel having a diameter
of about 1 to 1.5 metre.
• It is rotated at high speed using a motor.
• Radiant heaters are provided externally to heat the
fluid in the bucket.
• Condensers are arranged very close to the evaporating
surface.
• Vacuum pump is connected to the entire vessel at the
top.
• Provisions are made for introducing the feed into the
centre of the bucket, for receiving the product and
residue for re-circulation.
Working:
• Vacuum is applied at the centre of the vessel.
• The bucket shaped vessel is allowed to rotate at high
speed.
• The feed is introduced from the centre of the vessel.
• Due to centrifugal action of the rotating bucket, liquid
moves outward over the surface of the vessel and forms a
film.
• Since, the radiant heaters heat the surface, the liquid
evaporates directly from the film.
• The vapour (molecules) travels its mean free path and
strikes the condenser.
• The condensate is collected into another vessel.
• The residue is collected from the bottom of the vessel and
is re circulated through the feed port for further distillation.
Disadvantage:
• Construction and operation are more
complicated compared to falling film
molecular still.