Distillation Principles
PEOP1012 – Industrial Processes II
Is a separation process based on the fact that a mixture would contain
substances that differ in boiling points.
This means that, on the application of heat, different substances will
vaporize at different temperatures.
Simple Distillation
Is used for purifying salt water.
The liquid is collected from the solution while the solid stays in the flask.
Steam would be generated and thus condensed to yield the pure water.
It is also referred to as single-stage distillation. Often, when a high level of
purity in the resulting condensate is desired, it may be necessary to subject
the condensate to multiple processes of distillation to remove additional
impurities – a process called rectification.
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Simple
Distillation
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Fractional Distillation
Is used to separate two miscible liquids which have different boiling points
eg. separating ethanol (b.p. 78°C) and water (b.p. 100°C). Miscible liquids
are liquids which mix completely (one homogeneous phase observed).
A fractionating column is used, through which the vapours from the boiling
solution is passed.
The temperature of the column gradually decreases along its length.
Components with higher boiling points condense in the column and flow to
the base of the column; components with lower boiling points vaporize
and pass upwards through the column to be condensed and collected.
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Industrial distillation is typically performed in large, vertical cylindrical
columns known as "distillation or fractionation towers" or "distillation
columns" with diameters ranging from about 65 cm - 6 m and heights
ranging from about 6 m - 60 m or more.
The distillation towers have liquid outlets at intervals up the column which
allow for the withdrawal of different fractions or products having
different boiling points or boiling ranges.
By increasing the temperature of the product inside the columns, the
different hydrocarbons are separated. 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.
This type of distillation can occur under pressure or vacuum conditions.
Laboratory
Fractional
Distillation
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Industrial
Fractional
Distillation
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Vacuum Distillation
The pressure above the liquid mixture to be distilled is reduced to less than its vapour
pressure (usually less than atmospheric pressure) thereby causing evaporation of the
most volatile liquid(s).
This distillation method works on the principle that boiling occurs when the vapour
pressure of a liquid exceeds the ambient pressure. Vacuum distillation is used with or
without heating the mixture.
Vacuum distillation increases the relative volatility (the vapour pressure of a more
volatile component at a given temperature divided by the vapour pressure of a heavier
component at the same temperature) of the key components in many applications. The
higher the relative volatility, the more separable are the two components; this connotes
fewer stages in a distillation column in order to effect the same separation between the
overhead and bottoms products. Lower pressures increase relative volatilities in most
systems.
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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,
Reduction of product degradation or polymer formation because of reduced mean
residence time especially in columns using packing rather than trays.
Increasing capacity, yield, and purity.
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.
Reduced energy consumption.
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Steam Distillation
Steam distillation is used to purify or isolate temperature sensitive materials,
like natural aromatic compounds. Many organic compounds tend
to decompose at high sustained temperatures.
Separation by normal distillation would then not be an option, so water
or steam is introduced into the distillation apparatus. By adding water or
steam, the boiling points of the compounds are lowered, allowing them to
evaporate at lower temperatures, preferably below the temperatures at
which the deterioration of the material becomes appreciable.
The goal is to heat and separate the components at temperatures below their
decomposition point. Steam distillation is used in the manufacture of
perfumes and in the petrochemical industry/oil refineries (referred to as
steam stripping). 10
Steam
distillation
Apparatus
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Principles
For separation of components to occur, there must be a point of contact
between the fluids in the distillation column, namely liquid streams and gas
streams.
Thus trays, or packed columns are used. These provide surfaces for the liquid
(which is richer in the less volatile components) to intimately contact the
vapour (richer in the more volatile components).
Liquid flows down the column while vapour flows up the column.
Each time the liquid comes into contact with the vapour, simultaneous
vaporization and condensation takes place. The vapour strips (vaporizes) the
liquid of the more volatile component which moves upwards with the
vapour, while the less volatile component condenses out of the vapour,
which moves downward with the liquid flow.
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Typical distillation
setup
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Terms used in distillation operations
Reflux
This is the portion of condensed overhead product that is returned to the upper part of the
column to aid in maintaining the temperature profile of the column for good separation
efficiency.
The reflux flows across each tray, over a weir and down the downcomer to the tray below.
Simultaneously, the vapour rising from the top tray goes to a condenser and then through an
accumulating drum, also called a reflux drum, where part is returned to the column as reflux
and the rest is removed as overhead product to be further cooled.
The temperature profile is maintained through the column, because while the above is
occurring, simultaneously vapour is generated in the reboiler which is returned to the
column and enters the bottom tray where it is partially condensed and re-vaporises to give a
vapour of a new composition. This operation of partial condensation of the rising vapour and
partial vaporisation of the reflux liquid is repeated on each tray.
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Reflux ratio
Denoted by R, is the ratio of the top overflow to the quantity of top product. The number
of plates/trays required depends on this ratio. Any change in the reflux ratio will change
the number of plates needed for a particular separation. If no product is withdrawn from
the column, it is said to be operating under total reflux.
As the reflux ratio is increased, what this means is that more and more liquid that is rich in
the more volatile components are being recycled back into the column. Separation then
becomes better and thus less trays are needed to achieve the same degree of separation.
However, an increased reflux ratio means that the steam requirements for the reboiler and
cooling water requirements for the condenser are increased, and a column of larger
diameter is needed, thus greater operating costs are involved.
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Condensate
The use of a condenser at the top of the column is necessary for the condensation of overhead
vapours. The condensate is therefore the purified top overhead product. In batch distillation,
the condensate is usually further distilled for more purity. The condensate is rich in the most
volatile components of the mixture that was distilled.
Residue
The bottoms fraction obtained from a distillation column. It is obtained as a liquid, and is rich
in the heaviest components of the mixture that was distilled. Usually, a portion is recycled
through a re-boiler, to be vaporized and returned to the column as the heat source of the
column.
Fraction
The various side-draw products obtained from distillation of a multi-component mixture. For
example, in the fractionation of crude oil, the respective fractions are shown previously.
Fractions are further processed downstream to yield more valuable/usable products.
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Ancillary equipment
Besides distillation towers, equipment such as centrifugal pumps, shell and tube heat
exchangers (reboilers, condensers, pre-heaters and coolers), steam jet ejectors (for creating
vacuum), and product storage tanks are needed. Process piping systems as well as
instrumentation and controls are also required.
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References
“Working Guide to Process Equipment” – Norman Lieberman
AIChE E-learning Course – “Distillation in Practice”
Distillation: Process and Application | Method of Separation
[Link]
Crude Oil and Fractional Distillation
[Link]
Vacuum Distillation
[Link]
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