LIQUID EXTRACTION

CHE 411
 What is extraction and methods of extraction?
Extraction is the process of separating a
component substance (the solute) from a solid or
liquid mixture by dissolving it in a liquid solvent.

Extraction methods include solvent extraction,

distillation method, pressing and sublimation
according to the extraction principle. Solvent
extraction is the most widely used method.
Main purpose of extraction:
There are several reasons to use extraction in the
chemistry lab. It is a principal method for isolating
compounds. Extraction moves compounds from one
liquid to another, so that they can be more easily
manipulated or concentrated. It also enables the
selective removal of components in a mixture
 Concept of Extraction
Extraction is a common technique used to isolate a
target compound. In the extraction process, a solute
is transferred from one phase to another to separate
it from unreacted starting materials or impurities
The three most common types of extractions are:
liquid/liquid, solid/liquid, and acid/base (also
known as a chemically active extraction). The coffee
and tea examples are both of the liquid/solid type in
which a compound (caffeine) is isolated from a solid
mixture by using a liquid extraction solvent (water)
 The separation of the components of a liquid mixture by treatment
with a solvent in which one or more of the desired components is
preferentially soluble is known as liquid– liquid extraction — an
operation which is used, for example, in the processing of coal tar
liquids and in the production of fuels in the nuclear industry, and
which has been applied extensively to the separation of
hydrocarbons in the petroleum industry. In this operation, it is
essential that the liquid-mixture feed and solvent are at least
partially if not completely immiscible and, in essence, three stages
are involved:
1.Bringing the feed mixture and the solvent into intimate contact,
2.Separation of the resulting two phases, and
3. Removal and recovery of the solvent from each phase.

It is possible to combine stages (1) and (2) into a single piece of

equipment such as a column which is then operated continuously. Such
an operation is known as differential contacting.
Extraction is in many ways complementary to distillation and is
preferable in the following cases:

Where distillation would require excessive amounts of heat, such as,

for example, when the relative volatility is near unity.
When the formation of azeotropes limits the degree of separation
obtainable in distillation.
When heating must be avoided.
When the components to be separated are quite different in nature.

Important applications of liquid– liquid extraction include the separation of

aromatics from kerosene-based fuel oils to improve their burning qualities and the
separation of aromatics from paraffin and naphthenic compounds to improve the
temperature-viscosity characteristics of lubricating oils. It may also be used to
obtain, for example, relatively pure compounds such as benzene, toluene and
xylene from catalytically produced reformates in the oil industry, in metallurgical
and biotechnology industries
Solid-liquid extraction: Solid-liquid extraction is a type of extraction
process of extraction which is performed between the solid and liquid
phases.
•In this type of extraction solute particle(dispersed phase) is in a solid
state and the solvent(dispersed medium) is in the liquid state.
•Solid-liquid extraction is a method that is used mainly to remove
soluble components from solids using a solvent.
•Example: Separation of tea leaves from tea, leaching of metal salts from
ores, or obtaining oil from oilseeds; coffee brewing: which involves the
mixing of solid coffee grounds with water.

It offers a range of benefits over liquid-liquid extraction such as the

removal of possible emulsion formation and the ability for quantitative
recovery. It is available in three main types: normal phase, reversed
phase, and ion exchange – that are typically useful for polar, non-polar,
and charged compounds, respectively.
Solvent extraction is the process in which a compound transfers from
one solvent to another owing to the difference in solubility or
distribution coefficient between these two immiscible (or slightly
soluble) solvents.
• It is a method of quantitative separation of compounds.
• When extracting solvent is stirred with solution containing solute
then solute from original solvent gets transferred into an extracting
solvent.
• When stirring is stopped extracting solvent form separate layer and
now it contains solute of interest.

• Compared with other separation methods, it gives a better

separation effect than chemical precipitation, and a higher degree of
selectivity and faster mass transfer than the ion exchange method.
• Compared with distillation, solvent extraction has advantages such
as low energy consumption, large production capacity, fast action,
easy continuous operation and ease of automation.
 EXTRACTION PROCESSES
In the single-stage batch
process illustrated in Figure
.1, the solvent and solution
are mixed together and then
allowed to separate into the
two phases: the extract E
containing the required
solute in the added solvent
and the raffinate R, the
weaker solution with some
associated solvent. With this
simple arrangement mixing
and separation occur in the
same vessel.
A continuous two-stage operation is shown in Figure 2, where the mixers and separators are
shown as separate vessels. There are three main forms of equipment. First there is the mixer-
settler as shown in Figure 1, secondly, there is the column type of design with trays or packing
as in distillation and, thirdly, there are a variety of units incorporating rotating devices such as
the Scheibel and the Podbielniak extractors. In all cases, the extraction units are followed by
distillation or a similar operation in order to recover the solvent and the solute.
 LIQUID EXTRACTION
• Liquid (or solvent) extraction is the separation of the constituents of a
liquid solution by contact with another insoluble liquid. If the substances
constituting the original solution distribute themselves differently between
the two liquid phases a certain degree of separation results, which can be
enhanced by use of multiple contact.

• In distillation, the liquid is partially vaporized to create the vapour phase.

The separation of the components depend on the relative vapour press of
the substances. The vapour & liquid phases are similar chemically. In liquid
extraction, the two phases are chemically widely different which leads to
the separation of the component according to physical and chemical
properties.

• Solvent extraction can sometimes be used as an alternative to separation

by distillation or evaporation. For example, acetic acid can be removed
from water by distillation or by solvent extract using an organic solvent.
The resulting organic solvent – acetic acid solution is then distilled. Choice
of distillation or solvent extraction depends on relative cost.
 Equilibrium Data
The equilibrium condition for the distribution of one
solute between two liquid phases is conveniently
considered in terms of the distribution law. Thus, at
equilibrium, the ratio of the concentrations of the
solute in the two phases is given by
CE/CR,= K×,

where K× is the distribution constant.

the relation will apply accurately only if both solvents are
immiscible and if there is no association or dissociation of
the solute. are immiscible, and if there is no association or
dissociation of the solute.
If the solute forms molecules of different molecular weights,
then the distribution law holds for each molecular species.
Where the concentrations are small, the distribution law usually
holds provided no chemical reaction occurs.
The addition of a new solvent to a binary mixture of a solute in
a solvent may lead to the formation of several types of mixture:
(a)A homogeneous solution may be formed and the selected
solvent is then unsuitable.
(b)The solvent may be completely immiscible with the initial
solvent.
(c)The solvent may be partially miscible with the original
solvent resulting in the formation of one pair of partially
miscible liquids.
(d)The new solvent may lead to the formation of two or three
partially miscible liquids.
• If a solution of acetic acid in water is agitated with a liquid
such as ethyl but a water (ester), some of the acid or
relatively little water with enter the ester phase. Since at
equilibrium, the densities of the aqueous and ester layers
differ, they will settle when agitation starts and can be
decanted from each other. Since the ratio of acid in water in
the ester layer is different from that in the original solution
and also different from that in the residual water solution, a
certain degree of separation has been achieved. The acid
content can still been achieved. The acid content can still be
further noticed with more ester. The use to reflux also
enhances the ultimate separation still further.

• Mixer, settler (decanter) are needed in solvent extraction

when the two liquid are mixed, an emulsion is formed.
Commonly used solvents
• ethyl acetate (8.1 %),
• diethyl ether (6.9 %),
• dichloromethane (1.3 %) and
• chloroform (0.8 %) dissolved up to 10 % in water.
Water also dissolves in organic solvents:
• ethyl acetate (3 %),
• diethyl ether (1.4 %),
• dichloromethane (0.25 %)
• chloroform (0.056 %).

Uses of solvent extraction process

• Solvent extraction is used in the processing of perfumes,
vegetable oil, or biodiesel.
• It is also used to recover plutonium from irradiated nuclear fuel,
a process which is usually called nuclear reprocessing.
• The recovered plutonium can then be re-used as nuclear fuel.
Properties of solvent used for solvent extraction
1. The solvent should be well miscible with the liquid
to be extracted.
2. The solvent should not be miscible with the other
components of the mixture or react with the solute.
3. The boiling point of the solvent should be low
enough ( well below the melting point of the solute)
such that it can be evaporated easily after collection.
4. It should have a favourable temperature coefficient
Points to be considered
1 The solvent should be able to dissolve at least one component to a
large extent than the rest of the components in the
mixture.
2 The reaction taking place should be stable and irreversible.
Reversible reactions can bring back the dissolved components in their
previous form and the extraction will not be completed successfully.
3 The compound formed after the reaction should be easily separated
from the extracted compound so that it can be reused.
4 The density of the compound should be different from the required
component to help the separation readily.
5 It should be inexpensive and cost-effective.
6 The solvent should not be toxic or corrosive as it can harm the
extraction instruments.
7 Other factors important during solvent selection are viscosity,
boiling point, flammability, etc.
 When is Liquid Extraction Desirable?

1 In competition with other mass transfer operations.

• The product of distillation and evaporation are
composed of essentially pure substances while liquid
extraction produces new solution which must in turn
be separated often by distillation or evaporation. For
example acetic acid can be separated from dilute
solution with water, with difficulty by distillation or
with relative ease by extraction into ethyl ethanoate
followed by distillation of the ester. For the more dilute
solutions, particularly where water must be vaporized,
extraction is more economical.
• Extraction may also be attractive as an
alternative to distillation under high vacuum at
very low temperature to avoid thermal
decomposition. For example, long-chain fatty
acids can be separated from vegetable oil by high
vacuum distillation but more economically by
extraction with liquid propane. Tantalium and
nobium can be separated by tedious fractional
crystallization of the double fluoride or potassium
but with relative ease by liquid extraction of the
HF acid solutions with methyl isobutyl ketone
(MIK).
2 As a substitute for chemical methods
• Chemical methods consume reagents and also
lead to expensive disposal problems for chemical
by products. Liquid extraction incurs no chemical
consumption or by-product formation and is less
costly. Metal separations such as uranium-
vandadium, tungsten-molybdenum and the
fission products of atomic energy processes are
more economical by liquid extraction. Even lower
cost metals such as copper, and inorganic
chemicals such as phosphoric acid e.t.c are
economically purified by liquid extraction.
3. for separations not possible by other methods.
• Separation according to chemical and physical
types are possible in liquid extraction. For
example, aromatic and paraffinic hydrocarbon of
nearly the same molecular weight are
impossible to separate by distillation because
their vapour pressures are nearly the same but
they can readily be separated by extraction with
any of a number of solvents such as liquid SO2,
diethyleme glycol. Many pharmaceutical
products e.g. penicillin are produces in complex
fermentation mixtures and only liquid extraction
is a feasible separation device.
 Distribution ratio
Many substances undergo dissociation in aqueous phase like
weak carboxylic acid such as benzoic acid, phenol, etc.
• Now consider the weak acid HA which will dissociate in
aqueous phase as follows –
HA A- + H+

• The distribution coefficient in modified form can be

defined as distribution ratio (D)

• D = [HA ] org
[A-]aq + [HA] aq
• The solution which is to be extracted is called the feed,
and the liquid with which the feed is contacted is called
the solvent. The solvent-rich product of the operation
is called the extract and the residual liquid from which
solute has been removed is the raffinate or the solvent-
leant phase.

• More complicated processes may use two solvents to

separate the feed component. For example, a mixture
of p- and o- nitrobenzoic acids can be separated by
distributing them between the insoluble liquids
chloroform and water. The chloroform and water
preferentially dissolve the para and the ortho isomer
respectively. This is called double-solvent (or fractional)
extraction.
phases of extract and raffinate?
Liquid extraction is the separation
of the constituents of a liquid by
contact with another insoluble
liquid called solvent. The
constituents get distributed
between the two phases. The
solvent rich phase is called
extract and the residual liquid
from which the solute has been
removed is called raffinate.
 Equipment for Liquid Extractions
• There are two main classes of solvent extraction
namely single-stage and multi-stage.
• The extraction equipment can be operated
batchwise or continuously.
• In the single stage, two phases are contacted with
a high degree of turbulence in order to obtain high
mass transfer rate. It generally consists of a mixer-
settler unit. There are two types of mixers
generally used
(i) agitated and
(ii) flow
 References
• Lecture note on Extraction
• Datis Energy Company (2021)Manual on Solid-
Liquid Extraction.
• Coulson And Richardson’s Chemical Engineering.
Vol. 2, 5th Ed.
• Warren L. McCabe, Julian C. Smit& Peter Harriot
(2005) Unit operations of Chemical Engineering,
7th Ed. Chap 23, PP: 764-792
• Perry’s Chemical Engineers’ Handbook. 8th Ed