Distillation Still

Distillation
• Distillation is a method of separating mixtures based on differences
in their volatilities in a boiling liquid mixture. Distillation is a
physical separation process, and not a chemical reaction.
• Uses:-
1. Crude oil
2. Water is distilled to remove impurities
3. Air is distilled to separate its components
4. Distillation of fermented solutions to produce distilled beverages
with a higher alcohol content.

The premises where distillation is carried out, especially distillation

of alcohol, are known as a distillery.
Distillation (cont)
VARIOUS TYPES OF
DISTILLATION
 Simple Distillation
 Molecular Distillation
 Vacuum Distillation
 Batch Distillation
 Continuous Distillation
 Flash Distillation
 Fractional Distillation
 Azeotropic Distillation
Simple Distillation

 Single Vaporization/Condensation cycle of a mixture that produces a

distillate that is always impure
 Therefore, it is impossible to completely separate the components in a
mixture with Simple Distillation
 Relatively pure substances can be obtained from a
mixture with Simple Distillation if the boiling points of the components
differ by a large amount (>100oC)
 If a small increment of the initial distillate is separated and redistilled
and this process is repeated many times, effectively producing multiple
sequential Vaporization/ Condensation Cycles, an increasingly pure
solution can be attained.
Fractional Distillation

 Accomplishes the same thing as Multiple Simple Sequential

Vaporization / Condensation Cycles, by inserting a Fractionating
Column (a Vigreux Column) between the Distillation Flask and the
Distillation Head.
 The Fractionating Column, of which there are many types containing a
variety of packing materials, subjects the mixture to many
Vaporization/Condensation Cycles as the material moves up the column
toward the Distillation Head, which is attached to the Condenser.
 With each cycle within the column, the composition of the vapor is
progressively enriched in the lower boiling liquid.
 This process continues until most of the lower boiling compound is
removed from the original mixture and condensed in the receiving flask
Schematic of Distillation
Fractional Distillation (Cont.)

 When the lower boiling liquid is effectively removed from the original
mixture, the temperature rises and a second fraction containing some of
both compounds is produced.
 As the temperature approaches the boiling point of the higher boiling
point compound, the distillate condensing into the third receiving flask
is increasingly pure in the higher boiling point compound.
 Column Efficiency:- A common measure of the efficiency of a
Fractionation Column is given by its number of Theoretical Plates
One Theoretical Plate is equivalent to a Simple Distillation, i.e., one
Vaporization / Condensation Cycle. The smaller the boiling point
difference, the greater the number of theoretical plates a fractionating
column must have to achieve separation of mixtures
 Volume Increments

0.0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
0-65 oC

65-70 oC

70-75 oC

75-80 oC

80-85 oC

85-90 oC

90-95 oC

95-100 oC

100-105 oC

o
105-110 oC

Temperature Increments ( C)
110-115 oC
Simple & Fractional Distillation

115-120 oC

120-125 oC

125-130 oC
Simple & Fractional Distillation

Simple
Fractional
Azeotropic Distillation
 An azeotrope is a mixture of two or more liquids (chemicals) in such a ratio
that its composition cannot be changed by simple distillation. This occurs
because, when an azeotrope is boiled, the resulting vapor has the same ratio
of constituents as the original mixture.
 Because their composition is unchanged by distillation, azeotropes are also
called constant boiling mixtures.
 positive azeotrope is 95.63% ethanol and 4.37% water (by weight).
Ethanol boils at 78.4°C, water boils at 100°C, but the azeotrope boils at
78.2°C.
 negative azeotrope is hydrochloric acid at a concentration of 20.2% and
79.8% water (by weight). Hydrogen chloride boils at −84°C and water at
100°C, but the azeotrope boils at 110°C.
Azeotropic distillation
 Azeotropic distillation usually refers to the specific technique of adding another
component to generate a new, lower-boiling azeotrope that is heterogeneous
(e.g. producing two, immiscible liquid phases), such as the example below with
the addition of benzene to water and ethanol. In actual fact, this practice of
adding an entrainer which forms a separate phase is a specific sub-set of
(industrial) azeotropic distillation methods, or combination thereof. In some
senses, adding an entrainer is similar to extractive distillation.
• Example - distillation of ethanol/water, using normal distillation techniques,
ethanol can only be purified to approximately 96% . Some uses require a higher
percentage of alcohol, eg. when used as a gasoline additive.
• Material separation agent- The addition of a Material Separation Agent, such as
benzene.
• Molecular sieves- For the distillation of ethanol for gasoline addition, the most
common means of breaking the azeotrope is the use of molecular sieves.
Vacuum Distillation
 Vacuum distillation is a method of distillation whereby the pressure
above the liquid mixture to be distilled is reduced to less than its
vapor pressure (usually less than atmospheric pressure) causing
evaporation of the most volatile liquid(s) (those with the lowest
boiling points). This distillation method works on the principle that
boiling occurs when the vapor pressure of a liquid exceeds the
ambient pressure. Vacuum distillation is used with or without
heating the solution.
 Temperature sensitive materials (such as beta carotene) require
vacuum distillation to remove solvents from the mixture without
damaging the product. Vacuum distillation is sometimes referred to
as low temperature distillation. This type of distillation is in use in
the oil industry.
Advantages of Vacuum Distillation
 Industrial-scale vacuum distillation has several advantages.
 One tool to reduce the number of stages needed is to utilize vacuum distillation.
Vacuum distillation columns typically used in oil refineries have diameters ranging
up to about 14 meters (46 feet), heights ranging up to about 50 meters (164 feet), and
feed rates ranging up to about 25,400 cubic meters per day (160,000 barrels per day).
• Vacuum distillation increases the relative volatility of the key components in many
applications. Lower pressures increase relative volatilities in most systems.
• A second advantage of vacuum distillation is the reduced temperature requirement at
lower pressures. For many systems, the products degrade or polymerize at elevated
temperatures.
 Vacuum distillation can improve a separation by:
• Prevention of product degradation or polymer formation because of reduced pressure
leading to lower tower bottoms temperatures.
• Increasing capacity, yield, and purity.
• Another advantage of vacuum distillation is the reduced capital cost, at the expense of
slightly more operating cost. Utilizing vacuum distillation can reduce the height and
diameter, and thus the capital cost of a distillation column.
Molecular Distillation
 A special application of the simple distillation is molecular distillation,
known also as evaporative distillation or short path distillation.

 Theory of molecular distillation:-

The mean free path of a molecule is defined as the average distance
through which a molecule can move without coming into collision with
another. For material that are regarded as non volatile under ordinary
conditions of temperature and pressure are generally removed by this by
increasing the mean free path.

 Characteristics of the molecular distillation process:-

 Very high vacuum
 Evaporating surface must be close to the condensing surface
 The liquid area is large to avoid boiling and evolution of the vapors is from
surface only.
Molecular Distillation (cont.)
• Application of molecular distillation:-
 Purification of oils
 Separating of vitamins
Batch Distillation

 Batch distillation refers to the use of distillation in batches, meaning that a

mixture is distilled to separate it into its component fractions before the
distillation still is again charged with more mixture and the process is
repeated. This is in contrast with continuous distillation where the feedstock
is added and the distillate drawn off without interruption.
 Batch distillation has always been an important part of the production of
seasonal, or low capacity and high-purity chemicals. It is a very frequent
separation process in the pharmaceutical industry and in wastewater
treatment units.
 Because each of the distillate fractions are taken out at different times, only
one distillate exit point (location) is needed for a batch distillation and the
distillate can just be switched to a different receiver, a fraction-collecting
container. Batch distillation is often used when smaller quantities are
distilled.
Continuous Distillation
 Continuous distillation,
1. a form of distillation, is an ongoing separation in which a mixture is continuously (without
interruption) fed into the process and separated fractions are removed continuously as output
streams as time passes during the operation.
2. A distillation produces at least two output fractions. These fractions include at least one
volatile distillate fraction, which has boiled and been separately captured as a vapor
condensed to a liquid, and practically always a bottoms (or residuum) fraction, which is the
least volatile residue that has not been separately captured as a condensed vapor.
3. In a continuous distillation, each of the fraction streams is taken simultaneously throughout
operation; therefore, a separate exit point is needed for each fraction. In practice when there
are multiple distillate fractions, each of the distillate exit points are located at different
heights on a fractionating column.
4. The bottoms fraction can be taken from the bottom of the distillation column or unit, but is
often taken from a reboiler connected to the bottom of the column.
Continuous Distillation (cont.)
 In a continuous distillation, the system is kept in a steady state or
approximate steady state. Steady state means that quantities related to the
process do not change as time passes during operation. Such constant
quantities include feed input rate, output stream rates, heating and cooling
rates, reflux ratio, and temperatures, pressures, and compositions at every
point (location). Unless the process is disturbed due to changes in feed,
heating, ambient temperature, or condensing, steady state is normally
maintained.
 Since a continuous distillation unit is fed constantly with a feed mixture and
not filled all at once like a batch distillation, a continuous distillation unit
does not need a sizable distillation pot, vessel, or reservoir for a batch fill.
Instead, the mixture can be fed directly into the column, where the actual
separation occurs. The height of the feed point along the column can vary
on the situation and is designed so as to provide optimal result.
Flash Distillation
 Flash evaporation is the partial vaporization that occurs when a saturated
liquid stream undergoes a reduction in pressure by passing through a valve
or other device. If the valve or device is located at the entry into a pressure
vessel so that the flash evaporation occurs within the vessel, then the vessel
is often referred to as a flash drum.
 If the saturated liquid is a single-component liquid (for example, liquid
propane or liquid ammonia), a part of the liquid immediately "flashes" into
vapor. Both the vapor and the residual liquid are cooled to the saturation
temperature of the liquid at the reduced pressure. This is often referred to as
"auto-refrigeration" and is the basis of most conventional vapor
compression refrigeration systems.
 If the saturated liquid is a multi-component liquid (for example, a mixture
of propane, isobutane and normal butane), the flashed vapor is richer in the
more volatile components than is the remaining liquid.
Flash Distillation (cont.)
 Flash distillation (sometimes called "equilibrium distillation") is a single
stage separation technique. A liquid mixture feed is pumped through a
heater to raise the temperature and enthalpy of the mixture. It then flows
through a valve and the pressure is reduced, causing the liquid to partially
vaporize. Once the mixture enters a big enough volume (the "flash drum"),
the liquid and vapor separate. Because the vapor and liquid are in such
close contact up until the "flash" occurs, the product liquid and vapor
phases approach equilibrium.
 Simple flash separations are very common in industry, particularly
petroleum refining. Even when some other method of separation is to be
used, it is not uncommon to use a "pre-flash" to reduce the load on the
separation itself.
Extractive Distillation
 Extractive distillation is defined as distillation in the presence of a
miscible, high boiling, relatively non-volatile component, the solvent, that
forms no azeotrope with the other components in the mixture.
 The method of extractive distillation uses a separation solvent, which is
generally nonvolatile, has a high boiling point and is miscible with the
mixture, but doesn't form an azeotropic mixture. The solvent interacts
differently with the components of the mixture thereby causing their
relative volatilities to change.
 The solvent must alter the relative volatility by a wide enough margin for a
successful result. The quantity, cost and availability of the solvent should
be considered. The solvent should be easily separable from the bottom
product, and should not react chemically with the components or the
mixture, or cause corrosion in the equipment. A classic example is of
aniline as suitable solvent.
THANK U
Typical Distillation Setup
• Raoult’s Law
– In a solution of two miscible liquids (A & B) the partial pressure of
component “A” (PA) in the solution equals
the partial pressure of pure “A” (PAo) times its mole fraction (NA)
Partial Pressure of A in solution = PA = (PAo) x (NA)
Partial Pressure of B in solution = PB = (PBo) x (NB)
– When the total pressure (sum of the partial pressures) is equal to
or greater than the applied pressure, normally Atmospheric
Pressure (760 mm Hg), the solution boils
Ptotal = PA + PB = PAo NA + PBo NB
– If the sum of the two partial pressures of the two compounds in a
mixture is less than the applied pressure, the mixture will not boil.
The solution must be heated until the combined vapor pressure
equals the applied pressure
Simple Distillation
• Vapor Pressure / Boiling Point
– According to Kinetic Theory, the molecules in a liquid are in a constant
state of Thermal Motion and some of these molecules are moving fast
enough to escape from the liquid forming a vapor above the liquid. This
vapor exerts a pressure on the surface of the liquid, i.e., Vapor Pressure
– Vapor Pressure – The pressure of the vapor coexisting with a confined
liquid or solid, i.e., the pressure in an evacuated container containing a
liquid at constant temperature after the liquid and escaping molecules
near the surface of the liquid – the vapor - reach equilibrium
– The Vapor Pressure of a liquid increases, generally exponentially, with
temperature
– Boiling Point – As a liquid is heated, the vapor pressure of the liquid
increases to the point at which it just equals the applied pressure -
usually atmospheric pressure. The liquid now begins to bubble (boil)
• Vapor Pressure / Boiling Point (Con’t)
– Different liquid compounds or mixtures of liquids have
different vapor pressures at a given temperature.
– Liquids with high vapor pressures (Volatile compounds)
require relatively little energy (heat) to increase the vapor
pressure to match the applied (atmospheric) pressure, and
thus, boil, i.e. they have low boiling points.
– Liquids with low vapor pressures require considerably more
energy to increase the vapor pressure to the point where it
matches the applied pressure, thus, they have relatively high
boiling points.
– The individual compounds in a mixture each exert its own
pressure – partial pressure.
– The sum of the partial pressures equals to the total vapor
pressure of the solution
• As the distillation proceeds, the composition of the liquid and the
vapor are continuously changing
• The Horizontal and Vertical Lines represent the processes that occur
during a fractional distillation.
• Each Horizontal Line (L3V3, L2,V2), etc., represents both the
vaporization step of a given vaporization/condensation step and the
composition of the vapor in equilibrium with the liquid at a given
temperature.
• Examples:
• At 53oC with a liquid composition of 80% A and 20% B (L4V4 on the
diagram), the vapor would have 95% A and 5% B when equilibrium
has been established between the liquid and the vapor.
• At 63oC with a 50/50 liquid mixture of A&B (L3V3 on the diagram),
the vapor would have a composition of 80% A & 20% B at equilibrium.