What is distillation?

• Distillation is a separation technique used in pharmaceutical sector to purify and

separate mixtures of liquids based on their boiling points, , volatility, vapour pressure
exerted and Rate of evaporation.
• Inclusive of :-
1. Vaporisation of liquid mixture.
2. Condensation of vapour
(In which the condensed liquid is termed as distillate).
3. Separation based on volatility.

• Examples :
1. Water Purification.
2. Alcohol Distillation.
 Application

• Separation of Volatile Oils (By Steam Distillation)

• Refining of Petroleum Products (Using Flash Distillation)
• Quality control Method
• Recovery of Solvents.
• Manufacture of Official Preparation. ( By Simple Distillation)
 Types of
Distillation
Method

Simple Flash Steam Fractional Molecular

Distillatio Distillatio Distillatio Distillatio Distillatio
n n n n n
 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.
 Working

Condensation
• The liquid • The condensed
mixture is liquid, called the
heated in a flask. • The vapor is distillate, is
The most volatile collected in a
component in then passed separate
the mixture will through a container.
vaporize first. condenser,
where it cools
Heating Collection
and condenses
back into a
liquid.
 Constructions

• Heat Source : Provides heat to the liquid mixture.

• Distillation Flask (Boiling Flask) : Holds the liquid mixture to
be distilled.
• Thermometer : Measures the temperature of the vapor.
• Distillation Head : Connects the flask to the condenser, with
an outlet for the thermometer.
• Condenser : Cools and condenses the vapor back into liquid.
• Receiving Flask : Collects the condensed liquid (distillate).
• Clamp and Stand : Holds the apparatus components in place
securely.
 Advantages & Disadvantages

Limited
Separatio
Simplicity n
Capabilit
y

Cost-
Speed
Effective

Disadvantag Risk of
Advantages Accuracy Decompos
es ition

Efficiency
Purity for Simple
Mixtures
Scalabilit
y
 Flash Distillation

• It is a process in which the entire liquid mixture is suddenly vaporized (flash)

by passing the feed from a high pressure zone to low pressure zone.
• This method is frequently carried out as a continuos process and does not
involve rectification.

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 vaporized. This
process is known as flash vaporization.
• The Individual vapour phase molecules of high boiling fraction get
condensed, while low boiling fraction remains as vapour.
 Procedure & Working

Flash Vaporization • The vapor and

• The liquid liquid phases are
then separated,
mixture is heated • The mixture is with the vapor
to a high then suddenly containing the
temperature and released into a more volatile
pressure. lower pressure components.
zone, causing a
Heating portion of the Separation
liquid to flash
vaporize.
Construction

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.
 Applications

• It is used for separation components, which boil at widely diff temperature. It

is widely used in petroleum industry for refining crude oil.

Advantages

• It is continuous process.
• Used for obtaining a multi – component systems of narrow boiling range,
especially in oil refinery.

Disadvantages

• Not effective in separating comparable volatility.

• Not effective to achieve pure components.
 FRACTIONAL DISTILLATION
Not for Azeotropic disadvantages
mixture

Separation of miscible
liquid such as acetone
and water, chloroform
Principle works on counter current
and benzene
diffusion

Advanta
ges
FRACTIONAL DISTILLATION TYPES
CONSTRUCTION
DISTILLATION UNDER REDUCED
PRESSURE
 Not used in semi
FACTOR IN EVAPORATION solid Preparation or
Solid extract
Mass of vapour formed ∝ Vapour pressure of evaporating liquid
External pressure Because of
1.Viscosity
2.Teperature sensitivity
Disadvantages : Persistent foaming occurs this
3.Instability/emulsification
may be overcome by adding capryl alcohol to
4.Volatility
the liquid or by inserting a fine air capillary tube
5.Equipment limitation
in the second neck of Claisen flash the stream
of air is drawn in and breaks the rising foam

By reducing surface
tension and increasing
viscosity
Increases liquid flow and
turbulence (Fine air
capillary)
DISTILLATION UNDER REDUCED
PRESSURE
Vacuum distillation is a process used to separate components of
a mixture that have high boiling points under normal
atmospheric pressure. By lowering the pressure inside the
apparatus using a vacuum pump, the boiling points of these
components are reduced, allowing them to vaporize and be
collected as distillate. This method is crucial for separating
substances that are sensitive to heat or decompose at high
temperatures, such as certain oils, fats, and pharmaceutical
compounds. It is widely applied in industries like petroleum
refining to separate different fractions from crude oil and in
laboratories for purifying chemicals and pharmaceuticals
efficiently.
Steam Distillation
Working and procedure
Principle
 USES

• Used to separate immiscible liquids(Water + Toulene)

• TO extract volatile oils like clove,arise and eucalyptus oils
• Purification of essential oils like almond also for some organic liquid
• Prepation of aromatic water
 MOLECULAR DISTILLATION

• Heat apply through jacket vessels is heated then apply

is vacuum and wipers are rotated
• Now introduced the feed through feed inlet and it flow
down the wall spready by polytetrafluoroethylene(PTFE)
• Wiper starts rotating by speed (3m/s) so velocity of film
is 1.5m/s
• Condensate collected into vessels and residue is
collected from bottom
• Product is collected from product outlet and residue is
collected from outlet residue and it recirculated through
feed inlet
 CONSTRUCTION OF FAILING FILM

• The vessel has a diameter of one meter,

provided with suitable means of heating
• Wiper provided adjacent to vessel walls,
connected to a rotating head through rotator
• Condenser are attached close to the wall
• Vacuum pump is connect to large diameter
of pipe at centre of vessel
• Provisions are made for collecting the
distillate
 MOLECULAR DISTILLATION

• It is also called as short path distillation

Used for substance which have
• High have high boiling point
• Are heat sensitive
• Easily oxidized substance using High vaccum(10mm hg)
Application
• Preparation of some chemicals dimethyl phthalate,dibutyl phthalate
• Separation of vitamins(eg vit A from Fish liver oil)
• Refining of fixed oils
• Removal of undesirable compound eg cholesterol from butter
• Purification of butter
 MOLECULAR DISTILLATION

• Principle
• Decrease Boiling point by providing Higher Vacuum
• There is very low difference between evaporator and condenser
• Heavier molecules have shorter mean free path than Lighter
• They both strike condenser at different levels and get distilled
MOLECULAR DISTILLATION
 CENTRIFUGAL MOLECULAR STILL

• Vacuum is applied at the centre of vessels (bucket),then

rotate it at high speed
• Now feed is introduced into centre of
vessels(bucket),through feed inlet
• Due to high speed rotation, centrifugal force create, due to
centrifugal force liquid move outward over the surface of
bucket and form a film

• The vapour molecules its mean free path then it strikes the
condenser then product is collected through product inlet
• Residue is collected through residue outlet and re-
circulated through feed for further distillation