SOLID-LIQUID EXTRACTION

(LEACHING)

Dr. Neetu Singh

 LEACHING
Solid-liquid extraction (Leaching) is the process of removal of a substance from a
solid via a liquid extraction media.
The desired component diffuses into the solvent from its natural solid form.
Soluble material- Target product
Inert solid residue- By-product (solid waste)
Example:
Extraction of oil from oil seed (oil is the product and cake is by-product)
Removal of sugar from sugar beets with hot water.
Removal of soluble components of In the metals processing industry,
the soil. The loss of water soluble leaching is used to remove the metals
plant nutrients. from their ores, which contains many
undesirable constituents, as solute salts.
Example- gold leaching (gold is leached
from its ore using an aqueous sodium
cyanide solution).
Factors
There are four important factors that aid in leaching.
Temperature
Contact time
Solvent selection
Particle size/Area
 Factors
There are four important factors that aid in leaching.
Temperature- Extraction rate increases with the temperature. (Diffusivity of the solute
in solid as well as its miscibility with solvent increases with temperature).
Contact time- Liquid-solid contact is essential for sufficient time to complete the
extraction.
Solvent selection- Plays an important role in separation step. A solvent in which solute
has high solubility is definitely preferred.
Agitation- Nearly all leaching equipment employs some type of agitation to aid in mass
transfer and to ensure proper mixing. Intense agitation increases the solid-liquid mass
transfer coefficient as a result increases rate of extraction but may disintegrate the solid
as well, causing the settling problem.
Particle size/Area- Maximize the contact area per unit volume reduces equipment size.
Leaching Equipments
There are many different types of equipments used for leaching. Most of these
equipments fall in one of these categories.

1. Percolation (Liquid added to solid)- The solvent is contacted with the solid in
continuous or batch method. This method is popular for in-place ore leaching
or large scale “heap” leaching. Popular for extreme amount of solids.

2. Dispersed Solids (Solid added to liquid)- The solids are usually crushed in to
small pieces before being contacted with solvents. This is popular leaching
method when an especially high recovery rate can economically justify the
typically high operating cost (Ex- gold extraction).
 Leaching Equip….
Two types on the basis on nature of solids:
1. When the solid form an open permeable mass throughout the leaching
operation. Solvent may be percolated through an unagitated bed of solids.
2. With impermeable solids or materials that disintegrate during leaching, the
solids are dispersed in to the solvent and later separated from it.
Leaching by percolation
1. Through stationary solid bed
2. Through moving bed leaching
 LEACHING
EQUIPMENTS

Stationary Solid
Beds

Moving-bed
Leaching

Dispersed-
solid Leaching

DESIRED
DESIRED OUTPUT
OUTPUT
 Through stationary solid bed
Is done in a tank with a
perforated false bottom to
support the solids and permit
drainage of the solvent.
In some cases the rate of
solution is so rapid that one
passage of solvent is sufficient
otherwise battery of tank is
used.
Moving bed leaching
Bollman Extractor
1. Widely used for the extraction of vegetable oils
from seeds.
2. Consists of a number of baskets fixed to an endless
chain, having a descending & an ascending leg.
3. Each basket has a wire-mesh bottom.
4. Two chambers at the bottom of the vessel
separated by a partition plate hold the extract
streams.
Bollman Extractor
Advantage-
Because there is no agitation, the rich solvent leaving the extractor
remains reasonably clear.

Disadvantage-
Channelling of the liquid in the baskets may occur.
Hildebrand Extractor
1. This is a vertical total immersion extractor (continuous counter-current extraction
device)
2. Consists of a U-shaped screw conveyer fitted with three screw.
3. The helical profiles of the screws are perforated to allow flow of the solvent.
4. The solid is fed at the top of one of the leg and is propelled through the barrel.
5. Solvent is fed at the top of the other vertical leg and flows counter-current to the solid
through the perforations of the screw.
Major disadvantages of Hildebrand Extractor

1. Excessive disintegration of the solid if feed is in form of flakes.

2. Occasional choking with fines.
The Bonotto extractor
1. It consists of a vertical column divided into a number of compartments by horizontal plates.
2. Each plate has a slot that is oriented in the opposite side of the slot in an adjacent plate.
3. A scrapper is provided on each plate, which is fixed to a shaft running axially.
4. Solvent flows up through the column and the rich extract leaves at the top.
Horizontal Basket Extractor
1. This is widely used in oil extraction from seeds.
2. Consists of a train of horizontal baskets fitted to a drive chain enclosed in a big chamber.
3. Each basket has a wire-mesh or perforated bottom.
4. The liquid percolates through the solid in each basket, leaves through the perforated bottom.
5. Before a basket makes a complete turn, the nearly exhausted solid is sprayed with fresh solvent.
Continuous Belt Extractor
1. It is used for extraction of sugar from sugar beet.
2. Solid is fed at one end of a perforated endless moving belt.
3. Fresh solvent is fed at the solid discharge end.
4. The liquid drains into a catch basin and is pumped to the top of the adjacent section of the bed.
Rotocel Extractor
1. Has a rotating basket construction.
2. Consists of a number of cells (15-18) fixed to a central rotor.
3. Each basket is fitted with a perforated bottom so that solvent can percolate through the flakes.
4. Fresh solid enters the device at one end and the spent solid enters at the other.
5. Miscella from one compartment is pumped and sprayed on the next basket in the counter-
current direction.
Advantages of Rotocel Extractor
1. Solid is not subject to attrition & counter-current extraction is achieved.
2. Beside oil extraction from flaked seeds, these are used for removing solubles from plant materials
(leaves, bark etc.)
Dispersed Solid Leaching
The solid and the extracting solvent are agitated in a vessel of suitable size, shape
and design. Different types of agitators have been in use depending upon the
characteristics of the solid. Separation of the inerts from the solution & recovery
of the product from the solution is done.
ADSORPTION
ADSORPTION
“A mass transfer process which involves the accumulation of substance at the interface
of the two phases, such as, liquid-solid, gas-solid, liquid-liquid or gas-liquid interface.”
ADSORBATE- A substance which is adsorbed on the surface of another substance.
Examples gases, dyes, water vapors etc.
ADSORBENT- the substance which adsorbs
the other substance at its surface.
Examples: activated charcoal, bone
charcoal, alumina, silica gel, kaolin
and filler’s earth.
ADSORPTION is a spontaneous process
It is an exothermic process
(ΔH is negative)
Principle
Driving Force for Adsorption
Adsorption is a surface phenomenon and consequence of surface energy. The surface of a
liquid or solid is in a state of strain or unsaturation which results in unbalanced residual
force at the surface.
These unbalanced residual forces results in higher surface energy. Consequently, the
surface of liquids/solids always have a tendency to attract and retain the molecular species
with which it comes in contact. This tendency is responsible for the phenomenon of
Adsorption
Adsorption in Liquids & Solids
LIQUID: A molecule in the interior of a liquid is, completely surrounded
by other molecules, it is attracted equally in all directions. On a molecule
in the surface, however, there is a resultant attraction inwards, because
the number of molecules per unit volume is greater in bulk of the liquid
than in the vapour, this gives rise to surface tension. Hence, particles at
surface and particles at the bulk are in different environment thus giving
rise to difference in free energy at the surface & in the bulk.

SOLID: The gap between big crystals of solid into smaller units is done
to increase surface area. Due to cleavage of a big crystal into smaller unit,
residual forces or vacancies gets generated on the surface of the solid.
Occupancy of these vacancies by some other molecular species results
into Adsorption.
Classification of adsorption
Classification of adsorption is based on how strong is the interaction between the adsorbent and adsorbate.

Physical adsorption/Physisorption- If Chemical adsorption/Chemisorption-

the force of ineraction is rather weak If the interaction between a solute and
the type of adsorption is called the adsorbent is very strong a chemical
Physisorption. The forces of physical bond may be formed between them.
adsorption is Vadder Waal’s force.
Physical adsorption is reversible but
chemisorption may not be so.
Types of Adsorption Processes
 Physical adsorption
Physisorption (Physical Adsorption)- in which there is a van der Waals
interaction between the adsorbate & the substrate. Examples , A dispersion or
dipolar- dipolar interaction . Van der Waals interactions are long range but are
weak. Energy released when a particle is physisorbed is of the same order of
magnitude as the enthalpy of condensation . Such small energies can be
absorbed as vibrations of the lattice & dissipated as thermal motion, & a
molecule bouncing across the surface will gradually lose all its energy &
finally adsorb to it.
Chemical adsorption

Chemisorption (Chemical Adsorption)- in which the molecules or atoms

stick to the surface of adsorbent by forming a chemical bond (usually
covalent) and tend to find sites that maximize their coordination number with
the substrate. The distance between the surface & the closest adsorbate atom
is also typically shorter for chemisorption . A chemisorbed molecule may be
torn apart at the demand of the unsatisfied vacancies of the surface atoms, &
the existence of molecular fragments on the surface as a result of
chemisorption is one reason why solid surface catalyse reactions 
Physisorption/Chemisorption
Physical Adsorption / Physisorption Chemical Adsorption/Chemisorption
a. Not very Specific a. Highly Specific
b. No electron transfer , although polarization b. Electron transfer leading to bond
of adsorbate may occur formation between adsorbate & adsorbent
c. Rapid, non-activated & reversible c. Activated , may be slow & irreversible
d. No dissociation of adsorbed species d. May involve dissociation
e. Monolayer or Multilayer e. Monolayer only
f. Only significant at relatively low f. Possible over a wide range of
temperatures temperatures
g. Enthalpies are in the region of -20 kJ/mol g. Enthalpies are in the region of -200
h. With the increases in temperature, of kJ/mol
process Physisorption decreases. h. Chemisorption first increases & then
decreases with increase in temperature.
Factors affecting adsorption
1. Temperature
2. Pressure
3. Surface area
Factors affecting adsorption
Temperature- Adsorption is an exothermic
process, therefore the magnitude of
adsorption should increase with decrease in
temperature in physical adsorption. In
chemical adsorption magnitude of
adsorption first increases with rise in
temperature and then starts decreasing.
Factors affecting adsorption
Pressure- with increase in pressure,
adsorption increases up to extent of
saturation level, no more adsorption
takes place no matter how high the
pressure is applied.
Factors affecting adsorption
Surface area- It is a surface phenomena therefore
adsorption capacity of adsorbent increases with
increase in its surface area. Smaller the size of
particles of solid adsorbents more is the extent of
adsorption.
Activation of Solid adsorbent- Activation of adsorbent
surface is done to provide more vacant sites on surface.
This can be done by breaking solid crystals in small
pieces or into powders.
Commercial Adsorbents
Silica Gel Activated Carbon Activated alumina
Commercial Adsorbents
Zeolite Polymers & Resins Clay
Success of adsorption process
Ease of separation-
Solute concentration-
Process Conditions-
Adsorbent criteria-
Adsorption Isotherms
The equilibrium relation between the amount between the amount
adsorbed (mass adsorbed per unit mass of the adsorbent) and the
concentration (or partial pressure) of adsorbate at a constant temperature is
called adsorption isotherm.
Adsorption Isobar: A plot of equilibrium adsorbent loading vs temperature
at a constant pressure is called isobar.
Adsorption Isostere: A plot of logarithm of the concentration (ln C) or the
partial pressure (ln p) of the solute in the fluid vs inverse of absolute
temperature (1/T) is called an isostere.
Types of Adsorption Isotherms
Different types of adsorption isotherms occur for various adsorbent-adsorbate pairs.
Five basic types of adsorption isotherms:

Type I- represents a system in which adsorption

proceeds at Best up to the formation of monolayer of
adsorbate. For solute present in low concentration.

Type II- An indefinite monolayer is forms after

completion of Centre point on the curve indicates the
complete monolayer formation. Such a behaviour is very
common in case of physical adsorption.
 Types of Adsorption Isotherms
Type III- Rare type of isotherm. The amount of gas
adsorbed increases Indefinitely as its relative
saturation approaches unity.

Type IV & V- These isotherms have alternating

convex & concave Regions and reflects the
phenomena of capillary condensation within the
pores.
Mathematical form of Adsorption Isotherms
Few mathematical forms adsorption isotherms are available, which can be fitted with physical
adsorption data. Some of the isotherms have reasonable theoretical basis while the others are
purely empirical.
1. Langmuir Isotherm- based on simple model of physical adsorption, which assumes that –
Molecules are adsorbed at discrete active sites on the surface.
Each active site adsorbs only one molecule.
The adsorbing surface is energetically uniform.
There is no ineraction among the adsorbed molecules.
2. Freundlich Isotherm- This is an empirical isotherm, which assumes that the amount adsorbed at
equilibrium has a power law dependence on the partial pressure (or concentration) of solute.
3. Toth Isotherm
4. Sips Isothem
5. BET (Braunauer-Emmet-Teller) equation for multilayer adsorption.