Fractional distillation - Wikipedia Page 1 of 6

Fractional distillation
From Wikipedia, the free encyclopedia

Fractional distillation is the separation of a mixture into its component parts, or fractions, separating
chemical compounds by their boiling point by heating them to a temperature at which one or more
fractions of the compound will vaporize. It uses distillation to fractionate. Generally the component parts
have boiling points that differ by less than 25 °C from each other under a pressure of one atmosphere. If
the difference in boiling points is greater than 25 °C, a simple distillation is typically used.

Contents
◾ 1 Laboratory setup
◾ 1.1 Apparatus
◾ 1.2 Discussion
◾ 2 Industrial distillation
◾ 2.1 Design of industrial distillation columns
◾ 3 See also
◾ 4 References

Laboratory setup
Fractional distillation in a laboratory makes use of common laboratory glassware and apparatuses,
typically including a Bunsen burner, a round-bottomed flask and a condenser, as well as the single-
purpose fractionating column.

Apparatus

◾ heat source, such as a hot plate with a bath, and ideally with a magnetic stirrer.
◾ distilling flask, typically a round-bottom flask
◾ receiving flask, often also a round-bottom flask
◾ fractionating column
◾ distillation head
◾ thermometer and adapter if needed
◾ condenser, such as a Liebig condenser or Allihn condenser
◾ vacuum adapter (not used in image to the right)
◾ boiling chips, also known as anti-bumping granules
◾ Standard laboratory glassware with ground glass joints, e.g. quickfit apparatus.

Discussion

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As an example consider the distillation of a mixture

of water and ethanol. Ethanol boils at 78.4 °C while
water boils at 100 °C. So, by heating the mixture,
the most volatile component (ethanol) will
concentrate to a greater degree in the vapor leaving
the liquid. Some mixtures form azeotropes, where
the mixture boils at a lower temperature than either
component. In this example, a mixture of 96%
ethanol and 4% water boils at 78.2 °C; the mixture
is more volatile than pure ethanol. For this reason,
ethanol cannot be completely purified by direct
fractional distillation of ethanol-water mixtures.

The apparatus is assembled as in the diagram. (The

diagram represents a batch apparatus as opposed to a
continuous apparatus.) The mixture is put into the
round bottomed flask along with a few anti-bumping
granules (or a Teflon coated magnetic stirrer bar if
using magnetic stirring), and the fractionating
column is fitted into the top. The fractional
distillation column is set up with the heat source at Fractional distillation
the bottom on the still pot. As the distance from the An Erlenmeyer flask is used as a receiving flask.
stillpot increases, a temperature gradient is formed Here the distillation head and fractionating column
in the column; it is coolest at the top and hottest at are combined in one piece.[1]
the bottom. As the mixed vapor ascends the
temperature gradient, some of the vapor condenses
and revaporizes along the temperature gradient. Each time the vapor condenses and vaporizes, the
composition of the more volatile component in the vapor increases. This distills the vapor along the
length of the column, and eventually the vapor is composed solely of the more volatile component (or an
azeotrope). The vapor condenses on the glass platforms, known as trays, inside the column, and runs
back down into the liquid below, refluxing distillate. The efficiency in terms of the amount of heating
and time required to get fractionation can be improved by insulating the outside of the column in an
insulator such as wool, aluminium foil or preferably a vacuum jacket. The hottest tray is at the bottom
and the coolest is at the top. At steady state conditions, the vapor and liquid on each tray are at
equilibrium. The most volatile component of the mixture exits as a gas at the top of the column. The
vapor at the top of the column then passes into the condenser, which cools it down until it liquefies. The
separation is more pure with the addition of more trays (to a practical limitation of heat, flow, etc.)
Initially, the condensate will be close to the azeotropic composition, but when much of the ethanol has
been drawn off, the condensate becomes gradually richer in water. The process continues until all the
ethanol boils out of the mixture. This point can be recognized by the sharp rise in temperature shown on
the thermometer.

The above explanation reflects the theoretical way fractionation works. Normal laboratory fractionation
columns will be simple glass tubes (often vacuum-jacketed, and sometimes internally silvered) filled
with a packing, often small glass helices of 4 to 7 mm diameter. Such a column can be calibrated by the
distillation of a known mixture system to quantify the column in terms of number of theoretical trays. To

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improve fractionation the apparatus is set up to return condensate to the column by the use of some sort
of reflux splitter (reflux wire, gago, Magnetic swinging bucket, etc.) - a typical careful fractionation
would employ a reflux ratio of around 4:1 (4 parts returned condensate to 1 part condensate take off).

In laboratory distillation, several types of condensers are commonly found. The Liebig condenser is
simply a straight tube within a water jacket, and is the simplest (and relatively least expensive) form of
condenser. The Graham condenser is a spiral tube within a water jacket, and the Allihn condenser has a
series of large and small constrictions on the inside tube, each increasing the surface area upon which
the vapor constituents may condense.

Alternate set-ups may use a multi–outlet distillation receiver flask (referred to as a "cow" or "pig") to
connect three or four receiving flasks to the condenser. By turning the cow or pig, the distillates can be
channeled into any chosen receiver. Because the receiver does not have to be removed and replaced
during the distillation process, this type of apparatus is useful when distilling under an inert atmosphere
for air-sensitive chemicals or at reduced pressure. A Perkin triangle is an alternative apparatus often
used in these situations because it allows isolation of the receiver from the rest of the system, but does
require removing and reattaching a single receiver for each fraction.

Vacuum distillation systems operate at reduced pressure, thereby lowering the boiling points of the
materials. Anti-bumping granules, however, become ineffective at reduced pressures.

Industrial distillation
Fractional distillation is the most common form of
separation technology used in petroleum refineries,
petrochemical and chemical plants, natural gas processing
and cryogenic air separation plants.[2][3] In most cases, the
distillation is operated at a continuous steady state. New
feed is always being added to the distillation column and
products are always being removed. Unless the process is
disturbed due to changes in feed, heat, ambient temperature,
or condensing, the amount of feed being added and the
amount of product being removed are normally equal. This
is known as continuous, steady-state fractional distillation.

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 centimeters to 6 meters and heights ranging
from about 6 meters to 60 meters or more. The distillation
towers have liquid outlets at intervals up the column which
allow for the withdrawal of different fractions or products Typical industrial fractional distillation
having different boiling points or boiling ranges. By columns
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.

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For example, fractional distillation is used in oil refineries to separate crude oil into useful substances
(or fractions) having different hydrocarbons of different boiling points. The crude oil fractions with
higher boiling points:

◾ have more carbon atoms

◾ have higher molecular weights
◾ are less branched chain alkanes
◾ are darker in color
◾ are more viscous
◾ are more difficult to ignite and to burn

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 reflux liquid
flowing downwards provides the cooling needed to condense the
vapors flowing upwards, thereby increasing the effectiveness of
the distillation tower. The more reflux 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 provided for a given desired
separation, the fewer theoretical plates are required.

Fractional distillation is
also used in air
separation, producing
liquid oxygen, liquid
nitrogen, and highly Diagram of a typical industrial
concentrated argon. distillation tower
Distillation of
chlorosilanes also enable the production of high-purity silicon
for use as a semiconductor.

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
Crude oil is separated into fractions by vacuum. This packing material can either be random dumped
fractional distillation. The fractions at packing (1-3" wide) such as Raschig rings or structured sheet
the top of the fractionating column metal. Typical manufacturers are Koch, Sulzer and other
have lower boiling points than the companies. Liquids tend to wet the surface of the packing and
fractions at the bottom. All of the the vapors pass across this wetted surface, where mass transfer
fractions are processed further in other takes place. Unlike conventional tray distillation in which every
refining units. 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

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useful to compute a number of "theoretical plates" 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.

Design of industrial distillation columns

Design and operation of a distillation column depends on the

feed and desired products. Given a simple, binary component
feed, analytical methods such as the McCabe–Thiele method
[3][4][5]
or the Fenske equation[3] 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 columns are
typically lower than that of a theoretical 100% efficient
equilibrium stage. Hence, a distillation column needs more
plates than the number of theoretical vapor–liquid equilibrium
stages.

Reflux refers to the portion of the condensed overhead

product that is returned to the tower. The reflux flowing
downwards provides the cooling required for condensing the
vapours flowing upwards. The reflux ratio, which is the ratio
of the (internal) reflux to the overhead product, is conversely
related to the theoretical number of stages required for
efficient separation of the distillation products. Fractional
distillation towers or columns are designed to achieve the
required separation efficiently. The design of fractionation
columns is normally made in two steps; a process design,
followed by a mechanical design. The purpose of the process
design is to calculate the number of required theoretical Chemical engineering schematic of
stages and stream flows including the reflux ratio, heat reflux typical bubble-cap trays in a distillation
and other heat duties. The purpose of the mechanical design, tower
on the other hand, is to select the tower internals, column
diameter and height. In most cases, the mechanical design of
fractionation towers is not straightforward. For the efficient selection of tower internals and the accurate
calculation of column height and diameter, many factors must be taken into account. Some of the factors
involved in design calculations include feed load size and properties and the type of distillation column
used.

The two major types of distillation columns used are tray and packing columns. Packing columns are
normally used for smaller towers and loads that are corrosive or temperature sensitive or for vacuum
service where pressure drop is important. Tray columns, on the other hand, are used for larger columns
with high liquid loads. They first appeared on the scene in the 1820s. In most oil refinery operations,
tray columns are mainly used for the separation of petroleum fractions at different stages of oil refining.

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In the oil refining industry, the design and operation of fractionation towers is still largely accomplished
on an empirical basis. The calculations involved in the design of petroleum fractionation columns
require in the usual practice the use of numerable charts, tables and complex empirical equations. In
recent years, however, a considerable amount of work has been done to develop efficient and reliable
computer-aided design procedures for fractional distillation.[6]

See also
◾ Azeotropic distillation
◾ Batch distillation
◾ Extractive distillation
◾ Freeze distillation
◾ Steam distillation

References
1. Laurence M. Harwood; Christopher J. Moody (13 June 1989). Experimental organic chemistry: Principles
and Practice (Illustrated ed.). pp. 145–147. ISBN 978-0-632-02017-1.
2. Kister, Henry Z. (1992). Distillation Design (1st ed.). McGraw-Hill. ISBN 0-07-034909-6.
3. Perry, Robert H.; Green, Don W. (1984). Perry's Chemical Engineers' Handbook (6th ed.). McGraw-Hill.
ISBN 0-07-049479-7.
4. Beychok, Milton (May 1951). "Algebraic Solution of McCabe-Thiele Diagram". Chemical Engineering
Progress.
5. Seader, J. D.; Henley, Ernest J. (1998). Separation Process Principles. New York: Wiley. ISBN 0-471-
58626-9.
6. Ibrahim, Hassan Al-Haj (2014). "Chapter 5". In Bennett, Kelly. Matlab: Applications for the Practical
Engineer. Sciyo. pp. 139–171. ISBN 978-953-51-1719-3.

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Categories: Distillation Fractionation Industrial processes Laboratory techniques

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