SEPARATION PROCESSES 1

Leaching
 introduction
 Leaching is concerned with the extraction of a soluble
constituent from a solid by means of a solvent.
 The process may be used either for the production of a
concentrated solution of a valuable solid material, or in
order to remove an insoluble solid, such as a pigment,
from a soluble material with which it is contaminated.
 The method used for the extraction is determined by
the proportion of soluble constituent present, its
distribution throughout the solid, the nature of the
solid and the particle size
 definition
Leaching is the process of extracting minerals
from a solid by dissolving them in a liquid,
either in nature or through an industrial
process.
 uses

 In metals industry for removing mineral from ores (acid

solvents)
 In sugar industry for removing sugar from beets (water is
solvent)
 In oilseeds industry for removing oil from soybeans, etc.
(hexane or similar organic solvents)
The basic concepts of leaching also apply in the environment,
where materials can be leached out by rainwater and carried
into the groundwater supply. A simple, everyday example of a
leaching process is making your morning coffee.
 Leaching process
 If the solute is uniformly dispersed in the solid, the
material near the surface will be dissolved first, leaving a
porous structure in the solid residue.
 The solvent will then have to penetrate this outer layer
before it can reach further solute, and the process will
become progressively more difficult and the extraction
rate will fall.
 If the solute forms a very high proportion of the solid,
the porous structure may break down almost
immediately to give a fine deposit of insoluble residue,
and access of solvent to the solute will not be impeded.
 Principle of leaching
 Liquid-solid phase equilibrium is important in understanding

leaching, crystallization, and adsorption. Diffusion through

solids is slow, even through pores in the substance, and so

equilibrium is harder to achieve

 Leaching can be batch, semi batch, or continuous.

 It usually operates at an elevated temperature to increase the

solubility of the solute in the solvent. Calculations involve

three component (solid, solvent, solute) systems.

 Principle of leaching
 Feed to a leaching system typically is solid, consisting of basically

insoluble carrier material and a (usually desirable) soluble compound.

The feed usually must be prepared by grinding or chopping. It is then

mixed with a liquid solvent. The desired material dissolves (to some

extent) and so leaves when the liquid is drawn off as overflow. The

solids are then removed as underflow. The underflow is wet, and so

some of the solvent/solute mixture is carried out here as well.

 Flow through a leaching system may be crosscurrent or countercurrent.

 Leaching process stages
Generally, the process can be considered in three parts:
 The change of phase of the solute as it dissolves in the
solvent
 Its diffusion through the solvent in the pores of the solid to
the outside of the particle,
 The transfer of the solute from the solution in contact with
the particles to the main bulk of the solution.
 Any one of these three processes may be responsible for
limiting the extraction rate, though the first process usually
occurs so rapidly that it has a negligible effect on the
overall rate.
Factors influencing the rate of leaching

 The selection of the equipment for an extraction process

is influenced by the factors which are responsible for
limiting the extraction rate.
 Thus, if the diffusion of the solute through the porous
structure of the residual solids is the controlling factor,
the material should be of small size so that the distance
the solute has to travel is small.
 On the other hand, if diffusion of the solute from the
surface of the particles to the bulk of the solution is the
controlling factor, a high degree of agitation of the fluid
is required.
 Factors influencing the rate of leaching

 There are four important factors to be

considered:

1. Particle size
2. Solvent
3. Temperature
4. Agitation of fluid
 Particle size
Particle size influences the extraction rate in a number of
ways.
 Smaller the size, the greater is the interfacial area
between the solid and liquid, and therefore the higher is
the rate of transfer of material and the smaller is the
distance the solute must diffuse within the solid as
already indicated.
 On the other hand, the surface may not be so effectively
used with a very fine material if circulation of the liquid is
impeded, and separation of the particles from the liquid
and drainage of the solid residue are made more difficult.
 solvent
 The liquid chosen should be a good selective
solvent and its viscosity should be sufficiently low
for it to circulate freely.
Generally, a relatively pure solvent will be used
initially, although as the extraction proceeds the
concentration of solute will increase and the rate of
extraction will progressively decrease, first because
the concentration gradient will be reduced, and
secondly because the solution will generally
become more viscous.
 temperature
 In most cases, the solubility of the material which is
being extracted will increase with temperature to
give a higher rate of extraction.
 Further, the diffusion coefficient will be expected to
increase with rise in temperature and this will also
improve the rate of extraction. In some cases, the
upper limit of temperature is determined by
secondary considerations, such as, for example, the
necessity to avoid enzyme action during the
extraction of sugar.
 Agitation of fluid
 Agitation of the solvent is important because
this increases the eddy diffusion and therefore
the transfer of material from the surface of
the particles to the bulk of the solution
happens. Agitation of suspensions of fine
particles prevents sedimentation and more
effective use is made of the interfacial surface.
 Mass transfer in leaching process
 Mass transfer rates within the porous residue are difficult to assess
because it is impossible to define the shape of the channels through
which transfer must take place.
However approximated calculations are based upon following assumptions
 Thin film provide the resistance to transfer,
 batch process in which V , the total volume of solution
 pure solvent is used initially, Co = 0,
 Interfacial area will tend to increase during the extraction and, when
the soluble material forms a very high proportion of the total solid,
complete disintegration of the particles may occur.
 Although this results in an increase in the interfacial area, the rate of
extraction will probably be reduced because the free flow of the solvent
will be impeded by the increase in the effective thickness of film.
 At high degrees of agitation the ratio of the heat and mass transfer
coefficients is almost independent of the speed of the agitator
 Mass transfer in leaching process

 A is the area of solid liquid interface,

 c is the conc. of solute in the bulk of solution at time t
 Cs is the concentration of saturated solution
 M is the mass of solute transferred in time ‘t’
 K’ is the diffusion coefficient (Approximately equal to
the liquid phase diffusivity)
 b is the effective thickness of the liquid film
surrounding the particles,
 Mass transfer in leaching process

 h is the heat transfer coefficient,

 k is the thermal conductivity of the liquid, and
 Cp is the specific heat of the liquid
 Liquid phase diffusivity DL
 KL is the mass transfer coefficient equal to k/b
Where
 k is the diffusion coefficient
 b is the effective thickness of the liquid film surrounding
the particles,
 Equipment for leaching
 Three distinct processes are usually involved in
leaching operations
 Dissolving the soluble constituent.
 Separating the solution, so formed, from the
insoluble solid residue.
 Washing the solid residue in order to free it of
unwanted soluble matter or to obtain as much
of the soluble material as possible as the
product.
 Equipment for leaching
 The type of equipment employed depends on
the nature of the solid—whether it is granular
or cellular and whether it is coarse or fine.
 Coarse solids have sufficiently large settling
velocities for them to be readily separable
from the liquid
 Fine solids can be maintained in suspension
with the aid of only a small amount of
agitation.
 Extraction from cellular materials
 Consists of a vertical cylindrical vessel
divided into two sections by a slanting
partition.
 The upper section is filled with the charge of
seeds which is sprayed with fresh solvent via
a distributor.
 The solvent percolates through the bed of
solids and drains into the lower
compartment where, together with any
water extracted from the seeds, it is
continuously boiled off by means of a steam
coil.
 The vapours are passed to an external
condenser, and the mixed liquid is passed to
a separating box from which the solvent is
continuously fed back to the plant and the
water is run to waste.
 By this means a concentrated solution of the
oil is produced by the continued application
of pure solvent to the seeds.
 Bollmann continuous moving bed extractor

 Consists of a series of perforated baskets,

arranged as in a bucket elevator and contained
in a vapour-tight vessel, is widely used with
seeds which do not disintegrate on extraction
 Solid is fed into the top basket on the
downward side and is discharged from the top
basket on the upward side
 The solvent is sprayed on to the solid which is
about to be discarded, and passes downwards
through the baskets so that countercurrent
flow is achieved.
 The solvent is finally allowed to flow down
through the remaining baskets in co-current
flow.
 A typical extractor moves at about 0.3 mHz (1
revolution per hour), each basket containing
some 350 kg of seeds.
 Generally, about equal masses of seeds and
solvent are used and the final solution, known
as miscella, contains about 25 per cent of oil by
mass
 Leaching of coarse solids
 A simple batch plant used for coarse solids consists of a cylindrical vessel in
which the solids rest on a perforated support. The solvent is sprayed over
the solids and, after extraction is complete, the residue is allowed to drain.
If the solid contains a high proportion of solute such that it disintegrates, it
is treated with solvent in a tank and the solution is decanted.
 In a simple countercurrent system, the solid is contained in a number of
tanks and the solvent flows through each in turn. The first vessel contains
solid which is almost completely extracted and the last contains fresh solid.
 Leaching of coarse solids
 After some time, the first tank is disconnected and
a fresh charge is introduced at the far end of the
battery.
 The solvent may flow by gravity or be fed by
positive pressure, and is generally heated before it
enters each tank.
 The system is unsatisfactory in that it involves
frequent interruption while the tanks are
recharged, and countercurrent flow is not obtained
within the units themselves.
 Flow diagram for continuous leaching plant

A plant has been successfully developed

for the extraction of potassium sulphate
from alums containing about 25 per cent
soluble constituents.
After roasting, the material which is
then soft and porous with a size range
from 12 mm to very fine particles, with 95
per cent greater than 100-mesh (0.15
mm), is leached at 373 K with a solution
that is saturated at 303 K, the flow being .

The make-up water, which is used for washing the extracted solid, is
required to replace that removed in the residue of spent solid, in association
with the crystals, and by evaporation in the leaching tank and the crystalliser.
 Continuous leaching tank
 Consists of an open tank, 3 m in diameter, into the outer portion of which
the solid is continuously introduced from an annular hopper. Inside the
tank a 1.8 m diameter vertical pipe rotates very slowly at the rate of about
one revolution every 2400 s (0.0042 Hz).
 Continuous leaching tank
 It carries three ploughs stretching to the circumference of the tank, and these
gradually take the solid through holes into the inside of the pipe.
 A hollow shaft, about 1 m in diameter, rotates in the centre of the tank at
about one revolution in 200 s (0.005 Hz) and carries a screw conveyor which
lifts the solid and finally discharges it through an opening, so that it falls down
the shaft and is deflected into a waste pipe passing through the bottom of the
tank.
 Leaching takes place in the outer portion of the tank where the reheated
mother liquor rises through the descending solid.
 The make-up water is introduced under the flutes of the screw elevator flows
down over the solid and then joins the reheated mother liquor.
 Thus countercurrent extraction takes place in the outer part of the tank and
countercurrent washing in the central portion.
The plant described achieves between 85 and 90 per cent extraction, as
compared with only 50 per cent in the batch plant which it replaced.
 Leaching of fine solids
 Fine solids offer too high a resistance to flow.
Particles of less than about 200-mesh (0.075 mm)
may be maintained in suspension with only a small
amount of agitation, and as the total surface area is
large, an adequate extraction can be effected in a
reasonable time.
 Because of the low settling velocity of the particles
and their large surface, the subsequent separation
and washing operations are more difficult for fine
materials than with coarse solids.
 Simple stirred tank
 Agitation may be achieved either
by the use of a mechanical stirrer
or by means of compressed air
 The stirrer is often placed inside a
central tube and the shape of the
blades arranged so that the liquid
is lifted upwards through the tube.
 The liquid then discharges at the
top and flows downwards outside
the tube, thus giving continuous
circulation.
 Pachuca tank
 Agitated vessel in which
compressed air is used
 Cylindrical tank with a conical
bottom, fitted with a central pipe
connected to an air supply.
 Continuous circulation is obtained
with the central pipe acting as an
air lift.
 Additional air jets are provided in
the conical portion of the base and
are used for dislodging any
material which settles out.
 Dorr agitator
 Use compressed air for stirring
 Consists of a cylindrical flat-bottomed tank fitted with a central
air lift inside a hollow shaft which slowly rotates.
 To the bottom of the shaft are fitted rakes which drag the solid
material to the centre as it settles, so that it is picked up by the
air lift.
 At the upper end of the shaft the air lift discharges into a
perforated launder which distributes the suspension evenly
over the surface of the liquid in the vessel.
 When the shaft is not rotating the rakes automatically fold up
so as to prevent the plant from seizing up if it is shut down full
of slurry
 Dorr agitator
 This type of agitator can be used for
batch or continuous operation. In the
latter case the entry and delivery
points are situated at opposite sides
of the tank. The discharge pipe often
takes the form of a flexible
connection which can be arranged to
take off the product from any desired
depth.

 Many of these agitators are heated by

steam coils. If the soluble material
dissolves very rapidly, extraction can
be carried out in a thickener,
extensively used for separating the
discharge from an agitator.
COUNTERCURRENT WASHING OF SOLIDS

• Where the residual solid after separation is

still mixed with an appreciable amount of
solution, it is generally desirable to pass it
through a battery of washers, arranged to give
countercurrent flow of the solids and the
solvent.
• In order to define such a system completely,
the following six quantities must be specified
 COUNTERCURRENT WASHING OF SOLIDS
a) The composition of the solvent fed to the system—in particular, the
concentration of soluble material already present.
b) The quantity of solvent used; alternatively the concentration of the solution
to be produced may be specified, and the corresponding amount of solvent
calculated from a material balance.
c) The composition of the solid to be leached.
d) The amount of solid fed to the system; alternatively, the amount of soluble
or insoluble material required as product may be specified, and the
necessary amount of solid feed then calculated from a material balance.
e) The amount of liquid discharged with the solid in the underflow from each
of the thickeners.
f) The number and arrangement of the units; the purity of the product from
the plant can then be calculated. Alternatively, the required purity of the
washed solid may be stated, and the number of units can then be
calculated.
 Agitator and washing system
 The first four relate to the quantities and compositions of the materials used.
Quantity (e) specifies the manner in which each unit operates, and quantity (f)
involves either the number of units or a specification of the duty required of the
plant.
 Assignment
• Example 10.1 and 10.2