Distillation
Basic principles and methodology of simple distillation, flash distillation, distillation under
reduced pressure, steam distillation and molecular distillation
• Distillation is used to purify a liquid by separating the components of a liquid mixture.
• And separation is occurred, due to difference in boiling point of liquids.
• Mixture (Alcohol + Water) Distillation to Alcohol + Water (Separate)
Simple Distillation
It is used for separating the components of liquid mixtures.
Principle:
• It is used for separating liquid having boiling point difference approx. 25 °C.
• The liquid having the lower boiling point, evaporate first and then collected it an
another beaker through condensation, and other liquid is left behind round bottom flask.
Eg: Distillation of (Acetone + Water)
Distillation of (Alcohol + water)
B.P. of water = 100 °C, B.P. of Acetone-56 °C
Methodology:
Firstly put the mixture in round bottom flask, which we want to separate.
Then fit the thermometer at top for check the temperature in round bottom flask.
Then vapour’s outlet tube is connected with condenser which open in receiver.
And then, start to provide heat to the round bottom flask.
Boiling point of both liquid in mixture is different. So boil mixture till reach lower BP
• On reached on boiling point, liquid (acetone) starts to converting into vapours.
• And then it collect in receiver through condenser, because when vapour passed through
it again convert vapour into liquid.
• There are cold liquid in condenser which condense vapours.
• And other liquid (High boiling point) left in round bottom flask and collected through
it.
• Note: Boiling point difference is approx. 25 °C or more than 25 °C.
• On reached on boiling point, liquid (acetone) starts to converting into vapours.
• And then it collect in receiver through condenser, because when vapour passed through
it again convert vapour into liquid.
• There are cold liquid in condenser which condense vapours.
• And other liquid (High boiling point) left in round bottom flask and collected through
it.
• Note: Boiling point difference is approx. 25 °C or more than 25 °C.
Flash Distillation
• Principle: In which we pass the entire liquid mixture from heater and increase the
temperature up to their boiling point, so mixture is suddenly vapourised (flash), and
when we pass it in high pressure zone to a low pressure zone through pressure reducing
pump. So, vapour become cool and convert into liquid.
• It happened due to difference in boiling point. Low boiling point vapour condensed
first, which we separate from second liquid.
• Methodology:
• Firstly feed is pumped through a heater at a certain pressure (when mixture vapourised).
• Then liquid get heated and converting into vapours which further enters the vapour-
liquid separator, through a pressure-reducing valve.
• Pressure reducing valve reduce the pressure and vapour started to be condensed.
• Now, firstly vapours of high boiling fraction get condensed which we get in vapour-
liquid separator. And low boiling fraction remains as vapour.
• Then after some time second liquid also condense and we collect it.
• In vapour-liquid separator, there are sufficient time to separate out the liquid portion.
• So, liquid is collected from buttom and vapour’s of second liquid separated out from
top.
• It is possible to obtain continuous flash distillation.
It is possible by adjusting operating condition in such a way that the amount of feed exactly
equal the amount of material removed.
So, vapor and liquid concentration at any point remains constant in the unit.
• Uses:
• It is used for separating components which boil at widely different temperature.
• Used in petroleum industry for refining crude oil.
• Advantage:
• It is continuous process.
• Reduce the cost of operation
• Disadvantage:
• Not suitable for those, whose boiling point are not different widely.
• It is not efficient distillation when nearly pure components are required.
Fractional Distillation
• It is used for separate for those whose boiling point are close (miscible volatile liquids).
• And in which we can also separate more 2 liquid components mixtures.
• It is separated by means of a fractionating column.
Introduction: It is a process in which vaporization of liquid mixture gives rise to a mixture of
constituents from which the desired one is separated in pure form. This method is also known
as rectification, because a part of the vapour is condensed and returned as a liquid.
Principle:
When a liquid mixture is distilled partial condensation of vapour is allowed in a fractionating
column. Now that liquids vapour which boiling point is slightly low than other is pass out from
fractionating Column and through condenser it receive in receiver, while other liquid is condensed in
fractionating column and return back in distillation flask.
Now we change the receiver, and by applying same process we also collect second liquid in
pure form in receiver.
Construction:
It is same as simple distillation, one burner, round bottom flask, condenser, receiver, but the
only difference is that in this, fractionating column between round bottom flask (distillation)
and condenser.
Methodology:
Firstly take mixture of miscible liquid mixture in distillation flask.
Liquid mixture has low boiling point difference.
There is a fractionating column (vertical long tube) that affected continuously to condensation
and revapourisation.
• Now after introducing mixture on flask, start providing heating.
• Now, their are some distance in boiling point (may be it little).
• So, on heating all the liquid mixture convert into vapours and start moving upward.
• Now, those boiling point is less move upward first and other liquids vapour is below
from it.
• so, on moving upward from fractionating coloumn, low B.P. liquids vapour passes
easily (because it is upward) in to condenser and collected into receiver.
• And second liquid’s vapour (High B.P.) condensed in fractionating column and return
back into flask.
• After receiving, change the receiver, and we collect it, and other’s liquid is left in flask.
• If we want it in pure form, then repeat this, and heat provide is slightly more than before.
• And also collect if from second receiver.
• Uses:
• Used for those liquids mixture, whose B.P. is not far different.
Eg- [Benzene (80.1 °C) + Alcohol (78 °C)]
[Acetone (56 °C) + Methyl Alcohol (65 °C)]
[Air= O2 (183 °C) + N2 ( 196 °C) + Ar (186 °C)]
So it is used to separate out components from these mixtures.
Distillation Under Reduced Pressure (Vacuum Distillation)
• The process in which a liquid is boil (convert into vapours) at temperature lower than
its normal boiling point by reducing pressure of its surface is called distillation under
reduced pressure.
Principle:
Liquids boils when vapour pressure is equal to the atmospheric pressure.
If the external pressure is reduced by applying vacuum, the boiling point of liquid is lowed,
therefore, the liquid boils at a lower temperature.
So we get vapours and distilled at lower temperature.
Construction
• It consists of a double-neck distillation flask known as Claisen flask.
• In which, one capillary tube in one neck, and thermometer in another neck.
• Capillary tube prevent bumping and also regulate the air.
• Thae Claisen flask is connected to a receiver through a condenser.
• Vacuum pump is attached through an adaptor to the receiver.
• A small pressure (manometer) should be connected through pump for check pressure
different (which we reduced).
• Thick walled glass apparatus with inter-changeable standard glass joints are used for
vacuum distillation.
Methodology:
• Firstly take liquid and filled up to ½ or 2/3 volume of flask.
• For avoid bumping process mix some amount of porcelain in it.
• And placed thermometer and other parts acc. To their construction.
• Apply required vacuum and reduced pressure so liquid’s B.P. decreases and we get
liquid vapourised early.
• Now, vapour pass through condenser and pure liquid is collected in receiver.
Uses:
• It is used for the concentration of extracts containing thermolabile order to prevent their
destruction.
• It is used for separating substances which undergo decomposition when heated under
normal atmospheric pressure (eg. Glycerol) 290 °C.
• Thermolabile- enzymes, vitamins, glycorides etc.
Disadvantage:
In this distillation, foaming occurs due to vacuum, it may be overcome by adding capryl alcohol
to the liquid.
Stem Distillation
• In which, we use steam for distillation.
• It is used to separate high boiling substance from non-volatile impurities (immiscible
liquids).
Principles:
• A mixture of immiscible liquid begins to boil when sum of their vapour pressure is
equal to atmospheric pressure.
• It is happened because steam has also some boiling point and vapour pressure, which
mix the pressure of organic substance and reaches to its atmospheric pressure and liquid
convert into vapours.
Construction:
• Metallic steam can fitted with cork having two holes.
• Safety tube inserted up to bottom through one hole to maintain pressure in side steam
can, more over when steam comes out from safety tube indicates that can is empty.
• Through other hole bant tube is passed and other end of this tube is connected to the
flask containing liquid mixture in which tube is dipped.
• Flask and condenser is connected with delivery tube.
• Condenser is connected to receiver.
• Provision are made to heat both steam can and flask separately.
• Working:
• Firstly fill water in steam can and set all apparatus according to construction.
• Then fill impure organic liquid (organic liquid + non-volatile impurities) in distillation
flask with some water.
• Organic liquid must be insoluble in water. (Aniline, Nitrobenzene, toluene etc)
• Now, after setup start to providing heat, and steam also created on steam can, which
further enter into distillation flask.
•
• Organic liquid mixture has high boiling point, so it get some heat from burner’s heat
and if we provide heat upto their boiling point, it may be decompose, because these are
heat sensitive.
• So, these liquid mixture get vapour pressure from steam and it mix with steam and their
vapor pressure is equal to atmospheric pressure at low temperature.
• Now, there mixture converts into vapours and pass through condenser and receive
(collected) into receiver.
• Non-volatile impurities is left in distillation because it does not convert into vapours.
• Product (water + pure organic substance) which we collect in receiver is separated
through separating funnel (insoluble).
Uses:
• Used to separate immiscible liquids. Eq. (water + toluene, aniline) etc.
• To extract volatile oils like clove, anise and eucalyptus oils.
• Purification of essential oils like almond oil also for some organic liquid.
• Preparation for aromatic water.
Disadvantages:
Not suitable, if two immiscible liquids react with each other.
Molecular Distillation
• It is also called as short path distillation or evaporative distillation.
• It is used for those substance which have high boiling point, heat sensitive and easily
oxidized substances by applying high vacuum (Up to 10-4 mmHg).
Principle:
• By applying high vacuum, decreasing boiling pressure, so substance evaporate very
low temperature.
• And there are very low distance between evaporator surface and condenser, so at very
low pressure mean free path of molecules is equal to it.
• But heavier molecules have shorter mean free path value that lighter molecules, so they
both strikes condenser at different location and get distilled.
Mean free path of molecules
• The average distance through which a molecules can move without coming into
collision with another.
(or move between collision).
• Based on formation of liquid film, apparatus divided into two types:
i) Falling film molecular distillation/ wiped film molecular still
II) Centrifugal molecular still
i) Falling film 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, which spread
by (Polytetrafluroethylene) PTFE wiper to form a thin film.
• Now, wiper rotated by speed approx. 3m/S. So velocity of the film is 1.5 m/s.
• The vapour molecules travel to its mean free path and strikes the condenser.
• Condensate collected into vessels and residue is collected from bottom.
• Product is collected from product outlet and residue collected from outlet residue and
it re-circulated through feed inlet.
Centrifugal Molecular Still
• Vacuum is applied at the centre of vessels (bucket), then rotate it an 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 travel 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.
Applications:
Preparation of some chemicals: dibutyl phthalate, dimethyl phthalate etc.
Separation of vitamins (e.g. Vit. A from fish liver oil)
Refining of fixed oils.
Removal of undesirable compound e.g. cholesterol removal from butter
Purification of oils.