Introduction

Distillation is a method of separating mixtures based on differences in their

volatilities in a boiling liquid mixture. Distillation is a unit operation, or a physical
separation process, and not a chemical reaction.

Commercially, distillation has a number of applications. It is used to separate crude

oil into more fractions for specific uses such as transport, power generation and
heating. Water is distilled to remove impurities, such as salt from seawater. Air is
distilled to separate its components—notably oxygen, nitrogen, and argon—for
industrial use. Distillation of fermented solutions has been used since ancient times 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.

Applications of distillation

The application of distillation can roughly be divided in four groups: laboratory scale,
industrial distillation, distillation of herbs for perfumery and medicinals (herbal
distillate), and food processing. The latter two are distinctively different from the
former two in that in the processing of beverages, the distillation is not used as a true
purification method but more to transfer all volatiles from the source materials to the
distillate.

The main difference between laboratory scale distillation and industrial distillation is
that laboratory scale distillation is often performed batch-wise, whereas industrial
distillation often occurs continuously. In batch distillation, the composition of the
source material, the vapors of the distilling compounds and the distillate change
during the distillation. In batch distillation, a still is charged (supplied) with a batch of
feed mixture, which is then separated into its component fractions which are collected
sequentially from most volatile to less volatile, with the bottoms (remaining least or
non-volatile fraction) removed at the end. The still can then be recharged and the
process repeated.

In continuous distillation, the source materials, vapors, and distillate are kept at a
constant composition by carefully replenishing the source material and removing
fractions from both vapor and liquid in the system. This results in a better control of
the separation process.

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Idealized distillation model

The boiling point of a liquid is the temperature at which the vapor pressure of the
liquid equals the pressure in the liquid, enabling bubbles to form without being
crushed. A special case is the normal boiling point, where the vapor pressure of the
liquid equals the ambient atmospheric pressure.

It is a common misconception that in a liquid mixture at a given pressure, each

component boils at the boiling point corresponding to the given pressure and the
vapors of each component will collect separately and purely. This, however, does not
occur even in an idealized system. Idealized models of distillation are essentially
governed by Raoult's law and Dalton's law, and assume that vapor-liquid equilibria
are attained.

Raoult's law assumes that a component contributes to the total vapor pressure of the
mixture in proportion to its percentage of the mixture and its vapor pressure when
pure, or succinctly: partial pressure equals mole fraction multiplied by vapor pressure
when pure. If one component changes another component's vapor pressure, or if the
volatility of a component is dependent on its percentage in the mixture, the law will
fail.

Dalton's law states that the total vapor pressure is the sum of the vapor pressures of
each individual component in the mixture. When a multi-component liquid is heated,
the vapor pressure of each component will rise, thus causing the total vapor pressure
to rise. When the total vapor pressure reaches the pressure surrounding the liquid,
boiling occurs and liquid turns to gas throughout the bulk of the liquid. Note that a
mixture with a given composition has one boiling point at a given pressure, when the
components are mutually soluble.

An implication of one boiling point is that lighter components never cleanly "boil
first". At boiling point, all volatile components boil, but for a component, its
percentage in the vapor is the same as its percentage of the total vapor pressure.
Lighter components have a higher partial pressure and thus are concentrated in the
vapor, but heavier volatile components also have a (smaller) partial pressure and
necessarily evaporate also, albeit being less concentrated in the vapor. Indeed, batch
distillation and fractionation succeed by varying the composition of the mixture. In
batch distillation, the batch evaporates, which changes its composition; in
fractionation, liquid higher in the fractionation column contains more lights and boils
at lower temperatures.

The idealized model is accurate in the case of chemically similar liquids, such as
benzene and toluene. In other cases, severe deviations from Raoult's law and Dalton's
law are observed, most famously in the mixture of ethanol and water. These
compounds, when heated together, form an azeotrope, which is a composition with a
boiling point higher or lower than the boiling point of each separate liquid. Virtually
all liquids, when mixed and heated, will display azeotropic behaviour. Although there
are computational methods that can be used to estimate the behavior of a mixture of
arbitrary components, the only way to obtain accurate vapor-liquid equilibrium data is
by measurement.

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It is not possible to completely purify a mixture of components by distillation, as this
would require each component in the mixture to have a zero partial pressure. If ultra-
pure products are the goal, then further chemical separation must be applied. When a
binary mixture is evaporated and the other component, e.g. a salt, has zero partial
pressure for practical purposes, the process is simpler and is called evaporation in
engineering.

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 which 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 the starting liquid).

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 in turn
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 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

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of the distillation is highly enriched in component A, and when component A has
distilled off, the boiling liquid is enriched in component B.

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 as time passes during the operation.
Continuous distillation produces at least two output fractions, including at least one
volatile distillate fraction, which has boiled and been separately captured as a vapor
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.

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. Given a feed of in a specified composition, the main
variables that affect the purity of products in continuous distillation are the reflux
ratio and the number of theoretical equilibrium stages (practically, 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.

Continuous distillation requires building and configuring dedicated equipment. The

resulting high investment cost restricts its use to the large scale.

General improvements

Both batch and continuous distillations can be improved by making use of a

fractionating column on top of the distillation flask. The column improves separation
by providing a larger surface area for the vapor and condensate to come into contact.
This helps it remain at equilibrium for as long as possible. The column can even
consist of small subsystems ('trays' or 'dishes') which all contain an enriched, boiling
liquid mixture, all with their own vapor-liquid equilibrium.

There are differences between laboratory-scale and industrial-scale fractionating

columns, but the principles are the same. Examples of laboratory-scale fractionating
columns (in increasing efficiency) include:

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Simple distillation

In simple distillation, all the hot vapors produced are immediately channeled into a
condenser which cools and condenses the vapors. Therefore, the distillate will not be
pure - its composition will be identical to the composition of the vapors at the given
temperature and pressure, and can be computed from Raoult's law.

As a result, simple distillation is usually used only to separate liquids whose boiling
points differ greatly (rule of thumb is 25 °C), or to separate liquids from involatile
solids or oils. For these cases, the vapor pressures of the components are usually
sufficiently different that Raoult's law may be neglected due to the insignificant
contribution of the less volatile component. In this case, the distillate may be
sufficiently pure for its intended purpose.

Fractional distillation

For many cases, the boiling points of the components in the mixture will be
sufficiently close that Raoult's law must be taken into consideration. Therefore,
fractional distillation must be used in order to separate the components well by
repeated vaporization-condensation cycles within a packed fractionating column. This
separation, by successive distillations, is also referred to as rectification [27].

As the solution to be purified is heated, its vapors rise to the fractionating column. As
it rises, it cools, condensing on the condenser walls and the surfaces of the packing
material. Here, the condensate continues to be heated by the rising hot vapors; it
vaporizes once more. However, the composition of the fresh vapors are determined
once again by Raoult's law. Each vaporization-condensation cycle (called a
theoretical plate) will yield a purer solution of the more volatile component.[28] In
reality, each cycle at a given temperature does not occur at exactly the same position
in the fractionating column; theoretical plate is thus a concept rather than an accurate
description.

More theoretical plates lead to better separations. A spinning band distillation system
uses a spinning band of Teflon or metal to force the rising vapors into close contact
with the descending condensate, increasing the number of theoretical plates.[29]

Industrial distillation

Large scale industrial distillation applications include both batch and continuous
fractional, vacuum, azeotropic, extractive, and steam distillation. The most widely
used industrial applications of continuous, steady-state fractional distillation are in
petroleum refineries, petrochemical and chemical plants and natural gas processing
plants.

Industrial distillation is typically performed in large, vertical cylindrical columns

known as distillation towers or distillation columns with diameters ranging from
about 65 centimeters to 16 meters and heights ranging from about 6 meters to 90
meters or more. When the process feed has a diverse composition, as in distilling
crude oil, liquid outlets at intervals up the column allow for the withdrawal of

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different fractions or products having different boiling points or boiling ranges. The
"lightest" products (those with the lowest boiling point) exit from the top of the
columns and the "heaviest" products (those with the highest boiling point) exit from
the bottom of the column and are often called the bottoms.

Large-scale industrial towers use reflux to achieve a more complete separation of

products. Reflux refers to the portion of the condensed overhead liquid product from a
distillation or fractionation tower that is returned to the upper part of the tower as
shown in the schematic diagram of a typical, large-scale industrial distillation tower.
Inside the tower, the downflowing reflux liquid provides cooling and condensation of
the upflowing vapors thereby increasing the efficacy of the distillation tower. The
more reflux that is provided for a given number of theoretical plates, the better the
tower's separation of lower boiling materials from higher boiling materials.
Alternatively, the more reflux that is provided for a given desired separation, the
fewer the number of theoretical plates required.

Such industrial fractionating towers are also used in air separation, producing liquid
oxygen, liquid nitrogen, and high purity argon. Distillation of chlorosilanes also
enables the production of high-purity silicon for use as a semiconductor.

Design and operation of a distillation tower depends on the feed and desired products.
Given a simple, binary component feed, analytical methods such as the McCabe-
Thiele method or the Fenske equation[27] can be used. For a multi-component feed,
simulation models are used both for design and operation. Moreover, the efficiencies
of the vapor-liquid contact devices (referred to as "plates" or "trays") used in
distillation towers are typically lower than that of a theoretical 100% efficient
equilibrium stage. Hence, a distillation tower needs more trays than the number of
theoretical vapor-liquid equilibrium stages.

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In industrial uses, sometimes a packing material is used in the column instead of trays,
especially when low pressure drops across the column are required, as when operating
under vacuum.

This packing material can either be random dumped packing (1-3" wide) such as
Raschig rings or structured sheet metal. Liquids tend to wet the surface of the packing
and the vapors pass across this wetted surface, where mass transfer takes place.
Unlike conventional tray distillation in which every tray represents a separate point of
vapor-liquid equilibrium, the vapor-liquid equilibrium curve in a packed column is
continuous. However, when modeling packed columns, it is useful to compute a
number of "theoretical stages" to denote the separation efficiency of the packed
column with respect to more traditional trays. Differently shaped packings have
different surface areas and void space between packings. Both of these factors affect
packing performance.

Another factor in addition to the packing shape and surface area that affects the
performance of random or structured packing is the liquid and vapor distribution
entering the packed bed. The number of theoretical stages required to make a given
separation is calculated using a specific vapor to liquid ratio. If the liquid and vapor
are not evenly distributed across the superficial tower area as it enters the packed bed,
the liquid to vapor ratio will not be correct in the packed bed and the required
separation will not be achieved. The packing will appear to not be working properly.
The height equivalent of a theoretical plate (HETP) will be greater than expected. The
problem is not the packing itself but the mal-distribution of the fluids entering the
packed bed. Liquid mal-distribution is more frequently the problem than vapor. The
design of the liquid distributors used to introduce the feed and reflux to a packed bed
is critical to making the packing perform to it maximum efficiency. Methods of
evaluating the effectiveness of a liquid distributor to evenly distribute the liquid
entering a packed bed can be found in references. Considerable work as been done on
this topic by Fractionation Research, Inc. (commonly known as FRI).

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Conclusion

In conclusion I finished my report about distillation in general. I defined what

distillation is mean. I also wrote application of distillation, idealized distillation
method , batch distillation, continuous distillation, general improvement, simple
.distillation, fractional distillation, and industrial distillation
I wrote general information about these points. I also put some picture that related to
.distillation