DISTILLATION

Distillation is a widely used method for separating the component substances from a liquid
mixture by selective evaporation and condensation. To separate a mixture of liquids, the
liquid can be heated to force components, which have different boiling points, into the
gaseous state.
In industrial chemistry, distillation is a unit operation of practically universal importance,
but it is a physical separation process and not a chemical reaction. Distillation is used for
many commercial processes, such as the production of gasoline, distilled water, xylene,
alcohol, paraffin, kerosene, and many other liquids.

Laboratory Scale Distillation

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.
If water is placed in a sealed container and allowed to evaporate, it will eventually reach
an equilibrium such that the water vapor is condensing just as fast as the water is
evaporating. The pressure of the vapor at this equilibrium is called the vapor pressure.
Vapor pressure is different for different substances and varies with temperature. In a
mixture of two liquids with different boiling points, the vapor will have more of the liquid
that is more volatile, i.e., evaporates more readily. In simple distillation, the liquid mixture
is heated, and the vapor rises through a tube and is collected and recondensed. The
recondensed liquid will have a higher concentration of the more volatile component than
the original mix. If the two liquids in the original mix have widely different boiling points, a
one-step evaporation and recondensation process is all that is necessary. This process
is called simple distillation.
Fractional distillation - It is used in order to separate the components by repeated
vaporization-condensation cycles within a packed fractionating column. This separation,
by successive distillations, is also referred to as rectification.
Fractional distillation is similar to simple distillation, except the same process is repeated
in successive cycles. Each cycle produces a mixture richer in the more volatile compound
than the mixture before it. Fractional distillation is necessary when the boiling points of
the liquids in the original mix are close enough to each other that simple distillation is not
enough to purify either compound.
Vacuum distillation - Some compounds have very high boiling points. Sometimes it’s
easier to lower the pressure than to reach its high boiling point. This technique is referred
to as vacuum distillation and it is commonly found in the laboratory in the form of the
rotary evaporator.
Some liquids boil at such high temperatures that simple or fractional distillation using the
process described above would be impractical or dangerous. Vacuum distillation,
however, offers another alternative. The boiling point of a liquid falls when the pressure
is reduced. The boiling point of water, for example, is lower at high altitude than at sea
level. By reducing the pressure in the container, the boiling point of the liquids in the
mixture can be reduced and the mixture distilled at a lower temperature. This technique
is called vacuum distillation.
Steam distillation - Steam Distillation is a method of distilling compounds which are heat-
sensitive. The temperature of the steam is easier to control than the surface of a heating
element. This allows a high rate of heat transfer without heating at a very high
temperature.
Air-sensitive vacuum distillation - Some compounds have high boiling points as well
as being air sensitive. For these compounds, a simple vacuum distillation system can be
used. Wherein the vacuum is replaced with an inert gas after the distillation is complete.
Short path distillation - It is a distillation technique that involves the distillate traveling a
short distance, often only a few centimeters. This technique is normally done at reduced
pressure allowing a lower operating temperature range.
Zone distillation - It is a distillation process in a long container with a special
arrangement. With the partial melting of refined matter in moving liquid zone and
condensation of vapor in the solid phase at condensate pulling in cold area.
Catalytic distillation - The process by which the reactants are catalyzed while being
distilled to continuously separate the products from the reactants. This method is used to
assist equilibrium reactions reach completion.
Thin film evaporator – It is highly suitable for liquids that are sensitive to heat, viscous
or having high molecular weight. Thin film evaporators quickly separate more volatile from
less volatile components using indirect heat transfer and mechanical agitation of a flowing
product film under controlled conditions. Either the vaporized component (distillate) or the
concentrated component may be the product depending on the application.
Fig A Schematic diagram of thin film evaporator
Azeotropic Distillation
Owing to the intermolecular attractions between molecules in the mixture, mixtures may
have a higher or lower boiling point than either of their components. A mixture of this kind
is called an azeotrope. When the liquids in the azeotrope evaporate, the vapor has the
same composition as the mixture, so azeotropes cannot be distilled using the techniques
described above. They can still be distilled, however, but only through one of several
other methods.
In extractive distillation, a solvent that will mix freely with one component but not the
other is added to the mixture. The new mixture can then be separated by distillation. In
reactive distillation, by contrast, a chemical that will react with one agent but not the
other is added, creating a new mixture that can be separated by distillation. Finally, adding
ionic salts may alter the volatilities of the compounds in the mix in such a way that they
can be distilled. In pressure-swing distillation, the distillation breaks the azeotropic
mixtures by employing both positive and negative pressures. This improves the selectivity
of the distillation.
Industrial Distillation
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 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.
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 efficiency 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.
In modern industrial uses, a packing material is used in the column instead of trays when
low pressure drops across the column are required. Factors that favor packing are
vacuum systems, smaller diameter columns, corrosive systems, systems prone to
foaming, systems requiring low liquid holdup, and batch distillation. Conversely, factors
that favor plate columns are: presence of solids in feed, high liquid rates, large column
diameters, complex columns, columns with wide feed composition variation, columns with
a chemical reaction, absorption columns, columns limited by foundation weight tolerance,
low liquid rate, large turn-down ratio and those processes subject to process surges.
Multi-Effect Distillation - The goal of multi-effect distillation is to increase the energy
efficiency of the process, for use in desalination, or in some cases one stage in the
production of ultrapure water. It is a distillation process often used for sea
water desalination. It consists of multiple stages or "effects". In each stage the feed water
is heated by steam in tubes, usually by spraying saline water onto them. Some of the
water evaporates, and this steam flows into the tubes of the next stage (effect), heating
and evaporating more water. Each stage essentially reuses the energy from the previous
stage, with successively lower temperatures and pressures after each one. Additionally,
between stages this steam uses some heat to preheat incoming saline water.
The plant can be seen as a sequence of closed spaces separated by tube walls, with a
heat source in one end and a heat sink in the other end. Each space consists of two
communicating subspaces, the exterior of the tubes of stage n and the interior of the
tubes in stage n+1. Each space has a lower temperature and pressure than the previous
space, and the tube walls have intermediate temperatures between the temperatures of
the fluids on each side. The pressure in a space cannot be in equilibrium with the
temperatures of the walls of both subspaces. It has an intermediate pressure. Then the
pressure is too low or the temperature too high in the first subspace, and the water
evaporates. In the second subspace, the pressure is too high or the temperature too low,
and the vapor condenses. This carries evaporation energy from the warmer first subspace
to the colder second subspace. At the second subspace the energy flows by conduction
through the tube walls to the colder next space.

Fig B Schematic of a multiple effect desalination plant. The first stage is at the top. Pink
areas are vapor, lighter blue areas are liquid feed water. Stronger turquoise is
condensate. It is not shown how feed water enters other stages than the first. F - feed
water in. S - heating steam in. C - heating steam out. W - Fresh water (condensate) out.
R - brine out. O - coolant in. P - coolant out. VC is the last-stage cooler.
Source
https://byjus.com/chemistry/distillation/
https://sciencing.com/types-distillation-6924000.html
https://en.wikipedia.org/wiki/Distillation
https://en.wikipedia.org/wiki/Multiple-effect_distillation
https://lcicorp.com/thin_film_evaporation/thin_film_wiped_film_evaporator