Distillation Principle, Types and Properties

1. Distillation:
A process in which a liquid mixture of two or more substances are separated into its
components fraction of desired purity by application and removal of heat.
Distillation refers to the selective boiling and subsequent condensation of a component in a
liquid mixture. Distillation is the most basic method used for the purification of liquids and for
the separation of liquid mixtures. Distillation involves the heating of a liquid to boiling and then
collecting their vapours to condense them in liquid state. It is separation method old but still use
for separation purposes. This method is used for separation of miscible liquids mixture because
immiscible liquids mixture easily separated by separating funnel.
Examples: Benzene (B.p. 80) and Aniline (B.p.184) mixture.
2. Principle:
Distillation depends on:
 Difference in boiling point of individual component
 Vapour pressure
 Volatile nature of liquids
If a liquid has high boiling point its mean it has less vapour pressure and lower
volatility. If a liquid has low boiling point its mean it has high vapour pressure and
higher volatility. It is important to note that distillation is not a chemical reaction but it
can be considered as a physical separation process. The distillation performed on a
laboratory scale often uses batches of the liquid mixture whereas industrial distillation
processes are generally continuous, requiring a constant composition of the mixture to be
maintained.
3. Types of Distillation:
Some important types of distillation include:
 Simple distillation
 Fractional distillation
 Steam distillation
 Vacuum distillation
 Air-sensitive vacuum distillation
 Short path distillation
 Zone distillation
 3.1 Simple Distillation:
Simple distillation involves heating the liquid mixture to the boiling point and
immediately condensing the resulting vapors.
 This method is only effective for mixtures which have the boiling points difference of
25oC
Examples:
 Ether (35oC) toluene (111oC)
 Methanol (65oC) water ( 100oC)
Diagram:

Figure no.1: Simple Distillation

3.2 Fractional Distillation:
If liquids boiling points are closer to each other it carried out by using fractionating
columns. This method is for mixtures which have the boiling points difference of lesser than
25oC.Fractionating columns: There are many types of fractioning columns which are used
during this distillation.

Figure no.2 Types of Fractionating Columns

Examples: Mixture of Acetone (56oC) and methanol (69oC)
 Petroleum products also separated by this method because its components have close
boiling points. At industrial level Air components also separated e.g.., Nitrogen (196oC)
Argon (186oC) Oxygen (183oC)

Figure no.3 Fractional Distillation

3.3 Vacuum Distillation:

Vacuum distillation also known as lower pressure distillation or distillation under reduce
pressure is used for separating mixtures of liquids with very high boiling points. When
these liquids are boiled at low temperature they decomposed. In order to boil these
compounds; heating to high temperatures is an inefficient method. Therefore, the pressure of
the surroundings is lowered. The lowering of the pressure enables the component to boil at
lower temperature. We know that Temperature is directly proportional to pressure.

Once the vapor pressure of the component is equal to the surrounding pressure, it is
converted into a vapor. These vapors are then condensed and collected as the distillate. The
vacuum distillation method is also used to obtain high-purity samples of compounds that
decompose at high temperatures. For creating Vacuum: Steam ejector or vacuum pump is
used.

Example: Glycerol (290oC)

Figure no. 4 Vacuum Distillations

 3.4 Steam Distillation:

Steam distillation is often used to separate heat-sensitive components in a mixture. This is

done by passing steam through the mixture (which is slightly heated) to vaporize some of it.
The process establishes a high heat-transfer rate without the need for high temperatures.

The resulting vapor is condensed to afford the required distillate. The process of steam
distillation is used to obtain essential oils and herbal distillates from several aromatic
flowers/herbs.

Figure no. 5 steam Distillation

3.5 Air-Sensitive Vacuum Distillation

For compounds that are sensitive to air and readily react with it, the vacuum distillation process is carried out
but the vacuum must be replaced with an inert gas once the process is complete. Such a process is often
referred to as air-sensitive vacuum distillation.

3.6 Short Path Distillation

Short path distillation is used to purify a small quantity of a compound that is unstable at high temperatures.
This is done under lowered pressure levels and generally involves the distillate traveling a very small distance
before being collected (hence the name ‘short path’). The reduced distance travelled by the distillate in this
method also reduces the wastage along the walls of the apparatus.

3.7 Zone Distillation

The process of zone distillation involves the partial melting of a substance and the condensation of the
resulting vapour’s to obtain a pure distillate. This is carried out in a long container with the help of a zone
heater.
4.Distillation process at industrial level:

4.1. Working:
The liquid mixture that is to be processed is known as the feed and this is introduced
usually somewhere near the middle of the column to a tray known as the feed tray. The feed tray
divides the column into a top (enriching or rectification) section and a bottom (stripping)
section. The feed flows down the column where it is collected at the bottom in the reboiler.Heat
is supplied to the reboiler to generate vapour. The source of heat input can be any suitable fluid,
although in most chemical plants this is normally steam. In refineries, the heating source may be
the output streams of other columns. The vapour raised in thereboiler is re-introduced into the
unit at the bottom of the column.The liquid removed from the reboiler is known as the bottoms
product or simply, bottoms.Thevapour moves up the column, and as it exits the top of the unit,
it is cooled by a condenser. The condensed liquid is stored in a holding vessel known as the
reflux drum.

The condensed liquid that is removed from the system is known as the distillate or top
product. Thus, there are internal flows of vapour and liquid within the column as well as
external flows of feeds and product streams, into and out of the column.

5. Reflux Ratio:
5.1. Reflux:
Reflux is that portion of a tower’s condensed overhead liquid product that is cycled back to the
top of the tower where it flows downward to provide cooling and condensation of the upflowing
vapors.

 Large-scale distillation towers use a reflux system to achieve a complete product

separation.
 Increased the purity of product.

5.2. Reflux Ratio:

The reflux ratio is defined as the ratio of the liquid returned to the column divided by the
liquid removed as product,
R = Lc/D
5.2.1. For example:
 If five parts of top product is goes back to distillation column then one part into distillate
then reflux ratio will be 5:1
 If no distillate is removed or refluxed then ratio will be 1:0
 If all collected as distillate and not refluxed any liquid back then ratio will be 0:1.

5.3. Principle:
The higher the reflux ratio, the more vapor/liquid contact can occur in the distillation
column.the reflux ratio is inversely related to the number of trays required for a required
separation.
For a given reflux ratio and using McCabe-Thiele method we can determine the number of
theoretical trays required for a given separation
1. Minimum Reflux:
Maximum liquid is taken as distillate and much lesser is refluxed back into the tower
 As reflux is decrease,more and more trays are required. This is easy to verify using
theMcCabe-Thiele method.
 Purity of the product is decreased
2. Maximum Reflux:
Maximum liquid is refluxed back into the tower and minimum is collected as distillate.
 As reflux is increased lesser number of trays are required
 Purity of the product is increased
3. Optimum Reflux:
The Optimum Reflux Ratio (R0) is that at which the total cost of the distillation is a
minimum, taking into account the capital cost of the column (which depends on the
number of theoretical plates) and running cost, which depends on the reflux ratio.
 For designing a distillation plant for new industry Reflux ratio and number of
theoretical trays can be varied
 For existing column number of trays fixed so increases in reflux ratio and hence
increased the purity of the product.