ADSORPTION AND ION EXCHANGE - Slide 1

SEPARATION PROCESSES (CHE432)
ADSORPTION AND ION

EXCHANGE
Engr. Ajibola T. Ogunbiyi
Introduction
History of the Adsorption Technology
• Bleaching of solutions containing dyes
• Removal of bad odour from airstreams by passing through charcoal
Engr. Ajibola T. Ogunbiyi Nov. 2021 2

• The classical experiments of several scientists including
Brunauer, Emmett and Teller, McBain and Bakr, Langmuir, and
later by Barrer, all in the early part of the twentieth century,
shed light on the manner in which solids removed contaminants
from gases and liquids.
• It soon became clear, for example, that the observed effects

were best achieved with porous solids and that adsorption is
the result of interactive forces of physical attraction between
the surface of porous solids and component molecules being
removed from the bulk phase.

• Thus adsorption is the accumulation of concentration at a surface (as
opposed to absorption which is the accumulation of concentration
within the bulk of a solid or liquid).
• Adsorption, like any other separation process, must capitalize or zero

in on a particular property to achieve its separation purpose.
• The adsorption operations exploit the ability of certain solids

preferentially to concentrate specific substances from solution
(gaseous mixture or liquid solution) onto their surfaces.
• Hence, components of either gaseous or liquid solutions can be

separated from each other, or purified.
Separation vs Purification
What is the difference between these two?

• Industrial applications of adsorbents became common practice following
the widespread use of charcoal for decolourizing liquids and, in
particular, its use in gas masks during the 1914–18 World War for the
protection of military personnel from poisonous gases.
Fig. 1: Gas masks Engr. Ajibola T. Ogunbiyi Nov. 2021 6

• Adsorbents for the drying of gases and vapours included alumina,
bauxite and silica gel;
• Bone char and other carbons were used for sugar refining and the
refining of some oils, fats and waxes;
• Activated charcoal was employed for the recovery of solvents, the

elimination of odours and the purification of air and industrial gases;
• Fuller’s earth and magnesia were found to be active in adsorbing

contaminants of petroleum fractions and oils, fats and waxes;

• Base exchanging silicates were used for water treatment while
some chars were capable of recovering precious metals.
• Some activated carbons were used in medical applications to

eliminate bacteria and other toxins.
• Equipment for such tasks included both batch and continuous

flow configurations, the important consideration for the design
of which was to ensure adequate contact between adsorbent
and fluid containing the component to be removed (the
adsorbate).
Examples of Gaseous Adsorptive Separation
1. Dehumidification of air and other gases
2. Removal of bad odours and impurities from industrial gases
such as CO2
3. Recovery of valuable solvent vapours from dilute mixtures
with air and other gases.
4. Fractionation of mixtures of hydrocarbon gases containing
such substance as methane, ethylene, ethane, propene,
and propane.

Examples of Liquid Adsorptive Separation
1. Removal of mixture dissolved in gasoline
2. Decolorization of petroleum products and aqueous sugar

solutions.
3. Removal of bad taste and odour from water.
4. Fractionation of mixtures of aromatic and paraffinic

hydrocarbons.
• The scale of operations ranges from the use of a few grams of adsorbent in
the laboratory to industrial plants with an adsorbent inventory 135 tons.
• Similarity among all these operations (See Fig. 2).
Mixture to be
Adsorbent solid + separated
Unequal
Insoluble phase distribution
of the
original
constituents
Adsorbed phase + Bulk of the Fluid BETWEEN
Fig. 2: Basic adsorption steps Engr. Ajibola T. Ogunbiyi Nov. 2021 11
• All the techniques previously found valuable in the contact of
insoluble fluids are useful in adsorption.
• Thus, we have: (1) Batchwise single-stage
• Continuous multistage
The rigidity and immobility of a bed of solid adsorbent particles make

possible useful application of semicontinuous methods, which are not
at all practicable when two fluids are contacted.

Introduction to ion exchange
• Another solid-liquid operation of great importance is ion exchange.
• Ion exchange is the reversible exchange of ions between certain solids

and an electrolyte solution which permits the separation and
fractionation of electrolytic solutes.
• Ion exchange, which is chemical in nature, involves the interaction of

the ions with the solid and the diffusion of ions within the solid
phase.

Types of adsorption
1. Physical adsorption
 Readily reversible phenomenon
 Result of intermolecular forces of attraction between of solid and the
substance adsorbed (illustration).
The adsorbed substance does not penetrate within the crystal lattice of the
solid and does not dissolve in it but remains entirely upon the surface.
For highly porous solid containing many fine capillaries, however, the
adsorbate will penetrate these interstices
(Use of the analogy of a concave liquid surface of very small aperture and that of a very
large flat surface)

• At equilibrium, the partial pressure of the adsorbed substance equals
that of the contacting phase.
• By lowering the pressure of the gas phase or by raising the temperature,

the adsorbed gas is readily desorbed in unchanged form.
• The recovery of adsorbent for reuse is based on this reversibility.

Chemisorption
This results from chemical interaction between the solid and the
adsorbed substance.
The adhesive force is generally much greater than that found in

physical adsorption.
The strength of the chemical bond may vary considerably and
identifiable chemical compounds in the usual sense may not actually
form.
The heat liberated during chemisorption is usually large, of the order of
the heat of chemical reaction.

Chemisorption (Contd.)
The process is usually irreversible, and on desorption, the original

substance will often be found to have undergone a chemical
change.
Temperature also influences which of physiosorption or

chemisorption takes place on a surface. Higher temperature
favours chemisorption. Both may occur at the same time.
Chemisorption is of particular importance in catalysis but will not

be considered here.
Nature of adsorbents
Fig. 3: ExamplesEngr.ofAjibola
adsorbents
T. Ogunbiyi Nov. 2021 18
• Adsorbent solids must possess certain engineering properties depending
upon the application to which they are put.
• They are usually in granular form, varying in sizes from approx. 12 mm to
50 μm in diameter.
Adsorbents in a fixed bed through which a liquid or gas is to flow must

not offer too great a pressure drop for flow nor must they easily be carried
away by the flowing stream.
• They must have adequate strength and hardness so as not to be reduced
in size during handling or crushed in supporting their own weight in beds
of the required thickness.
• If they are to be transported frequently in and out of bins, they should
be free-flowing.
Adsorptive ability of solids
• Common solids will adsorb gases and vapours at least to a certain

extent. E.g. dried porcelain crucible on a humid day
• Only solids of sufficient specificity and adsorptive capacity are
considered as useful industrial adsorbents.
• Solids are frequently very specific in their ability to adsorb certain
substances in large amounts; hence, we can say that the chemical
nature of the solid is obviously linked with its adsorption
characteristics.
• The adsorptive capacity/ability of an adsorbent depends on its
method of manufacture and on its prior history adsorption and
desorption. Engr. Ajibola T. Ogunbiyi Nov. 2021 20
• Large surface area per unit weight is essential to all useful
adsorbents.
• Adsorbent surface comprises external or gross surface and
internal surface. The very much large internal surface of the
pores is more important.
• The pores though very small are large n number and as little
as 1 g of an sorbent can have surface of between 100 -1500
m2.
• There are other properties which are not understood, and
for these, we must rely largely on empirical observation for
recognition of adsorptive ability.
Principal adsorbents in general use
1. Fuller’s earth*: These are natural clays containing majorly magnesium
aluminium silicates in the form of the minerals attapulgite and
montmorillonite. The clay is heated and dried, during which operation, it
develops a porous structure, ground, and screened.
Size range: From coarse granules to fine powders.
Applications: The clays are particularly useful in decolorizing, neutralizing,
and drying such petroleum products as lubricating oils, transformer oils,
kerosenes, and gasolines, and vegetable and animal oils.
Regeneration: By washing and burning the adsorbed organic matter
accumulating upon the clay during use, the adsorbent can be reused many
times.
*Fulling is the practice of removing grease from woolen materials via the use of clay minerals.
The mineral name to be known as fuller’s earth.
2. Bauxite: this is a form of naturally occurring hydrated alumina
which must be activated by heating to temperatures varying rom
230 – 815oC to develop its adsorptive ability.
Applications: for decoloring petroleum products and for drying

gases.
Reactivation/regeneration: by heating

3. Molecular sieves: These are porous, synthetic zeolite crystals. On a
molecular level, there are “cages” in the crystals cells that can entrap
adsorbed matter. Molecules are sieved based on molecular size viz-a-viz
diameter of the passage ways. Molecules of mixtures are also separated
by adsorption based on (1) molecular polarity (2) degree of unsaturation.
Application: (1) Dehydration of gases and liquid

(2) Separation of gas and liquid hydrocarbon mixtures
(3) A great variety of processes
Regeneration: Heating or elution

4. CARBONIZED POLYMERS AND RESINS
Resins such as phenol formaldehyde and highly sulphonated styrene/divinyl benzene
macroporous ion exchange resins can be pyrolysed to produce carbonaceous
adsorbents which have macro-, meso- and microporosity.
Surface areas may range up to 1100 m2/g. These adsorbents tend to be more
hydrophobic than granular activated carbon and therefore one important application
is the removal of organic compounds from water.
5. BONE CHARCOALS
Animal bones can be carbonized to produce adsorbent materials which have only
meso- and macropores and surface areas around 100 m2/g. The pore development
activation step used with activated carbons is dispensed with.
The surface is carbon and hydroxyl apatite in roughly equal proportions and this dual
nature means that bone charcoals can be used to adsorb metals as well as organic
chemicals from aqueous systems. Decolourizing sugar syrup is another application.

6. SILICA GEL
Silica gel is a partially dehydrated polymeric form of colloidal silicic acid
with the formula SiO2.nH2O. This amorphous material comprises spherical
particles 2–20 nm in size which aggregate to form the adsorbent with pore
sizes in the range 6–25 nm. Surface areas are in the range 100–850 m2/g,
depending on whether the gel is low density or regular density.
The surface comprises mainly SiOH and SiOSi groups and, being polar, it
can be used to adsorb water, alcohols, phenols, amines, etc. by hydrogen
bonding mechanisms. Other commercial applications include the
separation of aromatics from paraffins and the chromatographic
separation of organic molecules.
7. ACTIVATED ALUMINA
Activated alumina is a porous high area form of aluminium oxide with the
formula Al2O3.nH2O. Its surface is more polar than that of silica gel and,
reflecting the amphoteric nature of aluminium, has both acidic and basic
characteristics. Surface areas are in the range 250–350 m2/g. Because
activated alumina has a higher capacity for water than silica gel at elevated
Temperatures, it is used mainly as a desiccant for warm gases including air
but in many commercial applications, it has now been replaced by zeolitic
materials. Gases for which activated alumina is suitable include argon,
helium, hydrogen, low molecular weight alkanes (C1–C3), chlorine, hydrogen
chloride, sulphur dioxide, ammonia and fluoroalkanes. Other uses for
activated alumina include chromatography and drying of liquids such as
kerosene, aromatics, gasoline fractions and chlorinated hydrocarbons.
Others are:
• Molecular-screening activated carbon
• Gas-adsorbent carbon
• Decolorizing carbons
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SEPARATION PROCESSES (CHE432)

ADSORPTION AND ION

• Bleaching of solutions containing dyes

• Removal of bad odour from airstreams by passing through charcoal

Engr. Ajibola T. Ogunbiyi Nov. 2021 2

• It soon became clear, for example, that the observed effects

Engr. Ajibola T. Ogunbiyi Nov. 2021 3

• Adsorption, like any other separation process, must capitalize or zero

• The adsorption operations exploit the ability of certain solids

• Hence, components of either gaseous or liquid solutions can be

Engr. Ajibola T. Ogunbiyi Nov. 2021 5

Fig. 1: Gas masks Engr. Ajibola T. Ogunbiyi Nov. 2021 6

• Activated charcoal was employed for the recovery of solvents, the

• Fuller’s earth and magnesia were found to be active in adsorbing

Engr. Ajibola T. Ogunbiyi Nov. 2021 7

• Some activated carbons were used in medical applications to

• Equipment for such tasks included both batch and continuous

Engr. Ajibola T. Ogunbiyi Nov. 2021 9

2. Decolorization of petroleum products and aqueous sugar

3. Removal of bad taste and odour from water.

4. Fractionation of mixtures of aromatic and paraffinic

The rigidity and immobility of a bed of solid adsorbent particles make

Engr. Ajibola T. Ogunbiyi Nov. 2021 12

• Ion exchange is the reversible exchange of ions between certain solids

• Ion exchange, which is chemical in nature, involves the interaction of

Engr. Ajibola T. Ogunbiyi Nov. 2021 13

Engr. Ajibola T. Ogunbiyi Nov. 2021 14

• By lowering the pressure of the gas phase or by raising the temperature,

• The recovery of adsorbent for reuse is based on this reversibility.

Engr. Ajibola T. Ogunbiyi Nov. 2021 15

The adhesive force is generally much greater than that found in

Engr. Ajibola T. Ogunbiyi Nov. 2021 16

The process is usually irreversible, and on desorption, the original

Temperature also influences which of physiosorption or

Chemisorption is of particular importance in catalysis but will not

Adsorbents in a fixed bed through which a liquid or gas is to flow must

• Common solids will adsorb gases and vapours at least to a certain

Applications: for decoloring petroleum products and for drying

Engr. Ajibola T. Ogunbiyi Nov. 2021 23

Application: (1) Dehydration of gases and liquid

Regeneration: Heating or elution

Engr. Ajibola T. Ogunbiyi Nov. 2021 24

Engr. Ajibola T. Ogunbiyi Nov. 2021 25

Engr. Ajibola T. Ogunbiyi Nov. 2021 28

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