DISTILLATION

TYPES AND APPLICATIONS

Distillation is method of separation of mixtures on the basis of difference in
the Boiling Point of components.
Separation is done by selective boiling and then condensation of
vapours.
It is a physical separation technique.
 History of Distillation goes to back to 1200 BC.
 Distilled water has been in use since 200 A.D.
 Distillation of alcohol was done by the Arab chemist Al Kindi in 9th-century.
 Fractional distillation was developed by Tadeo Alderotti in the 13th
century.
 In 1500, German chemist Hieronymus Braunschweig published Liber de
Arte Aestillandi (The Book of the Art of Distillation), the first book solely
dedicated to the subject of distillation.
The distillation process is dependent on the following two laws.

Raoult’s Law:
The vapour pressure of a single liquid component in an ideal liquid
mixture equals the product of the vapor pressure of the pure component
and its mole fraction.

P = Po x1
Dalton’s Law:
The total pressure exerted by a mixture of gases is equal to the sum
of the partial pressures of all the constituent gases.

Ptotal = P1 + P2 + P3
Distillation is one of the most widely used separation techniques. Some of
its general uses are mentioned below:
 Desalination of Saline Water
 Separation of volatile oils
 Purification of organic compounds
 Refining of petroleum products
 Recovery of solvents
 Cryogenic distillation of Air
Distillation is very important in the field of Pharmacy as given:
 Separation of drugs obtained from plant and animal sources
 Purification of drugs obtained from chemical process
 Manufacture of official preparations
 Quality control methods
There are various types of Distillation which are given below:
 Simple Distillation
 Vacuum Distillation
 Fractional Distillation
 Steam Distillation
 Destructive Distillation
Simple distillation is the process which involves heating the liquid mixture
to the boiling point and immediately condensing the resulting vapors.
→ Also named as differential distillation.
→ The purity of the distillate (the purified liquid) is governed by Raoult’s
law
o This method is only effective for mixtures wherein the boiling points of
the liquids are considerably different (a minimum difference of 25oC).
Simple distillation involves a single vaporization and subsequent
condensation.
Apparatus for Simple distillation at laboratory scale includes:
◙ Distillation Flask
◙ Condenser
◙ Collecting Flask
The apparatus is usually made of glass.
Fig. 1.2: A Simple Distillation
Apparatus
General applications of simple distillation include:
 Desalination of Saline Water
 Purifying drinking water on both a large and small scale.
 Purification of ethanol into fuel grade alcohol
 Non-volatile solids are separated from volatile liquids.
Pharmaceutical applications include:
 Preparation of distilled water and water for injection
 Preparation of volatile oils and aromatic waters
 Preparation of pharmaceutically important compounds e.g. Sprit
The distillation process in which the liquid is distilled at a temperature lower
than its boiling point by reducing the external pressure.
→ As boiling point depends upon the atmospheric pressure, we can lower
the boiling point by lowering external pressure.
→ It is the distillation under reduced pressure or low-temperature distillation.
◙ It consists of a double-neck Claisen flask.
◙ A thermometer is fitted in one neck of the Claisen flask.
◙ A fine capillary tube, through second neck, is dipped in the boiling liquid,
so that a stream of air bubbles is drawn out.
◙ The Claisen flask is connected to a receiver through a condenser.
◙ Vacuum pump is attached through an adapter to the receiver.
◙ Water bath or oil bath is used for heating.
Fig. 1.3: Vacuum Distillation
at laboratory Scale
Two further variants Vacuum Distillation are:
Molecular Distillation: Molecular distillation is a type of vacuum
distillation, performed at an extremely low vacuum pressure, 0.01 torr or
below.
Air Sensitive Vacuum Distillation: For the compounds having high
boiling points as well as being air sensitive, the vacuum over the sample is
then replaced with an inert gas (such as Nitrogen or Argon).
General applications of Vacuum distillation include:
 For the purification of heat sensitive compounds e.g. Glycerol
 In Desalination process to increase the efficiency
 To prevent thermal cracking in Crude oil
 Saves energy and time
 Increases the overall capacity, yield and efficiency of the system
Pharmaceutical applications include:
 Preventing degradation of active constituents. For example,
• Enzymes (malt extract, pancreatin)
• Vitamins (B1 and C)
• Glycosides (Anthraquinone i.e. Cascara sagrada extract)
• Alkaloids (Atropine)
 Evaporation of the manstrum in the preparation of extract
 Separation of Glycerol from Soap after Saponification
Fractional distillation involves several vaporization-condensation steps
(which takes place in a fractioning column).
→ It is often used to separate mixtures of liquids that have similar boiling
points.
→ This process is also known as rectification.
In fractional distillation, vapours of mixture are allowed to pass through the
fractionating column, where a part of the vapour is condensed.
The liquid with higher boiling point is condensed first and vapour becomes
richer with the liquid having the lower boiling point which gets condensed in
a condenser.
Fig. 1.4: Fractional Distillation
in Laboratory
General applications of Fractional distillation are:
 In oil refineries for separation of Petroleum products from crude oil.
 In Chemical plants for purification and separation of organic compounds.
 For the separation of liquefied air into liquid nitrogen, oxygen, argon etc.
 In the production of high-purity silicon from Chlorosilanes.
Pharmaceutical applications include:
 Alcohol is purified from the mixture of alcohol and water obtained from
fermentation tank.
 It is used for the separation of miscible liquids, such as, alcohol and
water, acetone and water, chloroform and benzene.
Steam distillation is done by passing steam through the mixture to vaporize
some of it. Then vapours are condensed to get the required distillate.
→ Steam Distillation is used to separate immiscible and heat sensitive
compounds.
Steam distillation requires the following apparatus:
◙ Steam Generator
◙ Distillation Flask
◙ Condenser
◙ Receiving Flask
Steam Generator is heated to get steam which moves to distillation flask
and vapourizes the mixture. Vapours get condensed in condenser and
distillate is received in receiving flask.
Fig. 1.6: Steam Distillation
Apparatus
General applications of Steam distillation are:
 Used to separate immiscible liquids.
 Extraction at much lower temperature to protect from decomposition.
 Aromatic water are prepared.
 Steam distillation is also sometimes used to separate intermediate or
final products during the synthesis of complex organic compounds.
 Steam distillation is also widely used in petroleum refineries and
petrochemical plants.
Pharmaceutical applications include:
 To extract volatile oils like clove, anise, orange and eucalyptus oils.
 Purification of essential oils like almond oil.
 Camphor is distilled by this method.
 It is used to determine the percentage of volatile oil in the drug.
Strong heating of organic matter in absence of air is called Destructive
distillation.
→ It is also named as Dry Distillation
→ Breakdown of Organic Matter (Pyrolysis) occurs.
The dried organic matter is heated in a suitable apparatus, until all the
volatile substances are driven off and the residue is left behind. The residue
is subjected to carbonization.
◙ Distillate is decomposition product of constituents of the organic matter
burnet in absence of air.
Fig. 1.6: Destructive Distillation
of Coal
General applications of Destructive distillation are:
 Destructive distillation of wood gives many compounds including
tar, terpenes, turpentine, methanol with a solid residue of charcoal.
 Destructive distillation of 1 tonne of coal produces 700 kg of coke, 100
liters of liquor ammonia, 50 liters of coal tar and 400 m3 of coal gas.
 Destructive distillation is used for recycling monomers derived from
waste polymers.
 Destructive distillation of natural rubber resulted in the discovery
of Isoprene which led to the creation of synthetic rubbers such
as neoprene.
Pharmaceutical applications include:
 Destructive distillation of wood gives acetone, menthol, cresol, wood tar
etc. while charcoal remains in the still.
 Ichthammol is prepared by the destructive distillation of fish fossils.
 Pyridine is often obtained from the distillation of the oil obtained, in turn,
from the destructive distillation of bones.
 Juniper-tar oil is obtained by the destructive distillation of the wood of
Juniperus.