World University of Bangladesh

An Assignment
On
Process and Significance of Distillation

Course Code: PHR-301

Course Title: Physical Pharmacy-II
Program: Bachelor of Pharmacy (Hons.)
Department of Pharmacy
World University of Bangladesh

Submitted By
Name: Md. Nure Alamin Siddik
Id: Wub14/19/25/729
Batch: 25th
Department of Pharmacy
World University of Bangladesh

Submitted To
Taqiayah Akhtar
Lecturer
Department of Pharmacy
World University of Bangladesh

Date of Submission: 16 June 2020

 PROCESS AND SIGNIFICANCE OF DISTILLATION

Distillation

Distillation refers to the selective boiling and subsequent condensation of a component in a

liquid mixture. It is a separation technique that can be used to either increase the
concentration of a particular component in the mixture or to obtain (almost) pure components
from the mixture. The process of distillation exploits the difference in the boiling points of
the components in the liquid mixture by forcing one of them into a gaseous state.

Figure- Distillation process

Process of Distillation

The distillation process can be carried out in various mode such as –

 Continuous distillation
 Batch distillation

 Continuous distillation
Continuous distillation is an ongoing distillation in which a liquid mixture is continuously
(without interruption) fed into the process and separated fractions are removed continuously
as output streams occur over time during the operation. Continuous distillation produces a
minimum of two output fractions, including at least one volatile distillate fraction, which has
boiled and been separately captured as a vapor and then condensed to a liquid. There is
always a bottoms (or residue) fraction, which is the least volatile residue that has not been
separately captured as a condensed vapor.
 Figure- Continuous distillation process

Continuous distillation differs from batch distillation in the respect that concentrations should
not change over time. Continuous distillation can be run at a steady state for an arbitrary
amount of time. For any source material of specific composition, the main variables that
affect the purity of products in continuous distillation are the reflux ratio and the number of
theoretical equilibrium stages, in practice determined by the number of trays or the height of
packing. Reflux is a flow from the condenser back to the column, which generates a recycle
that allows a better separation with a given number of trays. Equilibrium stages are ideal
steps where compositions achieve vapor–liquid equilibrium, repeating the separation process
and allowing better separation given a reflux ratio. A column with a high reflux ratio may
have fewer stages, but it refluxes a large amount of liquid, giving a wide column with a large
holdup. Conversely, a column with a low reflux ratio must have a large number of stages,
thus requiring a taller column.
 Batch distillation
Heating an ideal mixture of two volatile substances, A and B, with A having the higher
volatility, or lower boiling point, in a batch distillation setup (such as in an apparatus depicted
in the opening figure) until the mixture is boiling results in a vapor above the liquid that
contains a mixture of A and B. The ratio between A and B in the vapor will be different from
the ratio in the liquid. The ratio in the liquid will be determined by how the original mixture
was prepared, while the ratio in the vapor will be enriched in the more volatile compound, a
(due to Raoult's Law, see above). The vapor goes through the condenser and is removed from
the system. This, in turn, means that the ratio of compounds in the remaining liquid is now
different from the initial ratio (i.e., more enriched in B than in the starting liquid).

Figure- Batch distillation process

The result is that the ratio in the liquid mixture is changing, becoming richer in component B.
This causes the boiling point of the mixture to rise, which results in a rise in the temperature
in the vapor, which results in a changing ratio of A : B in the gas phase (as distillation
continues, there is an increasing proportion of B in the gas phase). This results in a slowly
changing ratio of A : B in the distillate.

If the difference in vapor pressure between the two components A and B is large – generally
expressed as the difference in boiling points – the mixture in the beginning of the distillation
is highly enriched in component A, and when component A has distilled off, the boiling
liquid is enriched in component B.
There are various type of process of Distillation are following as below-

1. Simple distillation

Figure- Simple distillation procedure

In simple distillation, the vapor is immediately channeled into a condenser. Consequently, the
distillate is not pure but rather its composition is identical to the composition of the vapors at
the given temperature and pressure. That concentration follows Raoult's law.

As a result, simple distillation is effective only when the liquid boiling points differ greatly
(rule of thumb is 25 °C) or when separating liquids from non-volatile solids or oils. For these
cases, the vapor pressures of the components are usually different enough that the distillate
may be sufficiently pure for its intended purpose.

A cutaway schematic of a simple distillation operation is shown at left. The starting liquid 15
in the boiling flask 2 is heated by a combined hotplate and magnetic stirrer 13 via a silicone
oil bath (orange, 14). The vapor flows through a short Vigreux column 3, then through a
Liebig condenser 5, is cooled by water (blue) that circulates through ports 6 and 7. The
condensed liquid drips into the receiving flask 8, sitting in a cooling bath (blue, 16). The
adapter 10 has a connection 9 that may be fitted to a vacuum pump. The components are
connected by ground glass joints (gray).
2. Fractional distillation

The process begins by drilling into the reservoir rocks the ground and extracting the crude
oil; once extracted it is sent to one of the many refineries around the world. In these refineries
the crude oil is pumped through pipes into the fractional distillation tower. The tower
separates the crude oil by heating it through a boiler, and changing its state to a gas. This gas
is passed through a distillation column that becomes cooler with height. When certain gases
reach the temperature that is the distinct temperature below the compounds boiling point,
they condense into a liquid. These liquids are then separated into their own distilling column
at the various heights.

Crude oil can be separated into seven different main distilling columns; Residue (at 1050°F
or higher), Fuel Oil (at 650°F to 1050°F), Diesel Oil (at 450°F to 650°F), Kerosene (at 350°F
to 450°F), Naphtha (at 185°F to 350°F), Gasoline (at 85°F to 185°F), Butane, propane and
lighter products (at 85° F or lower).

Figure- Fractional distillation procedure

3. Stem Distillation

Like vacuum distillation, steam distillation is a method for distilling compounds which are
heat-sensitive. The temperature of the steam is easier to control than the surface of a heating
element, and allows a high rate of heat transfer without heating at a very high temperature.
This process involves bubbling steam through a heated mixture of the raw material. By
Raoult's law, some of the target compound will vaporize (in accordance with its partial
pressure). The vapor mixture is cooled and condensed, usually yielding a layer of oil and a
layer of water.

Figure- Stem distillation

Steam distillation of various aromatic herbs and flowers can result in two products; an
essential oil as well as a watery herbal distillate. The essential oils are often used in
perfumery and aromatherapy while the watery distillates have many applications in
aromatherapy, food processing and skin care.

4. Vacuum distillation

Some compounds have very high boiling points. To boil such compounds, it is often better to
lower the pressure at which such compounds are boiled instead of increasing the temperature.
Once the pressure is lowered to the vapor pressure of the compound (at the given
temperature), boiling and the rest of the distillation process can commence. This technique is
referred to as vacuum distillation and it is commonly found in the laboratory in the form of
the rotary evaporator.

This technique is also very useful for compounds which boil beyond their decomposition
temperature at atmospheric pressure and which would therefore be decomposed by any
attempt to boil them under atmospheric pressure.
 Figure- Vacuum distillation

Molecular distillation is vacuum distillation below the pressure of 0.01 torr. 0.01 torr is one
order of magnitude above high vacuum, where fluids are in the free molecular flow regime,
i.e. the mean free path of molecules is comparable to the size of the equipment. The gaseous
phase no longer exerts significant pressure on the substance to be evaporated, and
consequently, rate of evaporation no longer depends on pressure. That is, because the
continuum assumptions of fluid dynamics no longer apply, mass transport is governed by
molecular dynamics rather than fluid dynamics. Thus, a short path between the hot surface
and the cold surface is necessary, typically by suspending a hot plate covered with a film of
feed next to a cold plate with a line of sight in between. Molecular distillation is used
industrially for purification of oils.

5. Air sensitive distillation

Some compounds have high boiling points as well as being air sensitive. A simple vacuum
distillation system as exemplified above can be used, whereby the vacuum is replaced with an
inert gas after the distillation is complete. However, this is a less satisfactory system if one
desires to collect fractions under a reduced pressure. To do this a "cow" or "pig" adaptor can
be added to the end of the condenser, or for better results or for very air sensitive compounds
a Perkin triangle apparatus can be used.
 Figure- Air sensitive distillation process

The Perkin triangle, has means via a series of glass or Teflon taps to allows fractions to be
isolated from the rest of the still, without the main body of the distillation being removed
from either the vacuum or heat source, and thus can remain in a state of reflux. To do this, the
sample is first isolated from the vacuum by means of the taps, the vacuum over the sample is
then replaced with an inert gas (such as nitrogen or argon) and can then be stoppered and
removed. A fresh collection vessel can then be added to the system, evacuated and linked
back into the distillation system via the taps to collect a second fraction, and so on, until all
fractions have been collected.

6. Short path distillation

Short path distillation is a distillation technique that

involves the distillate travelling a short distance, often
only a few centimeters, and is normally done at reduced
pressure. A classic example would be a distillation
involving the distillate travelling from one glass bulb to
another, without the need for a condenser separating the
two chambers. Figure- Short path distillation process
This technique is often used for compounds which are unstable at high temperatures or to
purify small amounts of compound. The advantage is that the heating temperature can be
considerably lower (at reduced pressure) than the boiling point of the liquid at standard
pressure, and the distillate only has to travel a short distance before condensing. A short path
ensures that little compound is lost on the sides of the apparatus. The Kugelrohr is a kind of a
short path distillation apparatus which often contain multiple chambers to collect distillate
fractions.

Significance of Distillation

Many of the products we use every day are the result of distillation, from the gasoline that
powers our cars to the water we drink. Distillation is a physical process that uses heat to
purify or separate mixtures containing one or more liquids. As a mixture is heated, the liquid
with the lowest boiling point will boil and turn into vapor, leaving behind any solid material
or other liquids. The vapor is captured and cooled until it condenses, resulting in a purified
version of the liquid.

 Scientific Uses

One practical use of distillation is in the laboratory. While the results of this type of
distillation may not find their way directly into our homes, the process is used regularly in
chemical and pharmaceutical research, quality assurance testing for many consumer products
and law enforcement forensics.

 Water Purification

Water from natural sources contains a variety of minerals and other impurities, many of
which can be removed by distillation. Distilled water is commonly used in situations where
the presence of minerals might reduce the effectiveness of certain equipment, such as in
steam irons or cigar humidors. Some people drink distilled water because they like the taste
or want to avoid the minerals found in tap water. Parents will often use distilled water when
preparing baby formula for their infants. Desalination plants also use distillation to turn
seawater into drinking water
 Alcoholic Beverages

Distillation is used to produce a variety of alcoholic beverages, such as whiskey, rum and
brandy. When fruit and plant materials ferment, a dilute version of ethyl alcohol is produced.
Distilling the fermented material purifies and concentrates the ethanol. A variety of other
components, such as water, esters and other types of alcohol, are also collected during the
distillation process, which accounts for the unique flavor of each alcoholic spirit.

 Petroleum Products

A number of products can be produced from crude oil. Because each of these products has a
unique boiling point, a process known as fractional distillation is used to refine oil into
separate materials. These include:

 gasoline
 diesel fuel
 lubricating oil
 fuel oil
 paraffin wax
 petrochemicals

 Perfume

One of the earliest uses of distilling was to make perfume, which began around 3500 B.C.
The aroma from various plants and herbs is contained in what are known as essential oils,
which can be extracted through distillation. However, many aromatic plants tend to
decompose at high temperatures so separation by normal distillation isn’t practical. In those
instances, steam is passed through the plant material to draw out the essential oils without
burning the mixture. The steam is then captured and condensed just as in normal distillation.