UNIT-IV

solid-liquid extraction
(leaching)
 OVER VIEW
 Introduction to leaching.
 principles of leaching
 Leaching equipments.
 Principles of Continuous Countercurrent
Leaching.
 CALCULATE material balance and number of
ideal stages for multistage leaching.
 LEACHING
• Leaching” is a unit operation in which a solid mixture
is contacted with a liquid solvent for removal of one
or more soluble constituents of the solid mixture
• It is generally necessary to recover or separate either
by evaporation or any other means the component
of new system i.e., solute and solvent which was
extracted.
• It is important because it is generally necessary for
product the most economical scheme for leaching
process.
 LEACHING
Leaching differs very little from the washing of filtered
solids and leaching equipment strongly resembles the
washing section of various filters.
In leaching the amount of solute material removed is
often greater than in ordinary filtration washing and the
properties of the solids may change considerably during
the leaching operation.
Coarse, hard or granular feed solids may disintegrate into
pulp when their content of soluble material is removed.
 Examples of leaching operation

• Extraction of gold from its ores by using

sodium cyanide solution.
• Extraction of sugar from sugar beats using hot
water.
• Extraction of tannin from tree bark using H2O
• Extraction of perfumes from flowers
• Preparation of tea and coffee
Factors affecting the rate of leaching
1. Particle size
Smaller size particles provide greater interfacial
area between the solid and liquid which in turns
results in higher rate of transfer of materials
2. Solvent;
The solvent used should be a selective solvent and
should have low viscosity
Temperature
Generally, the solubility of soluble solute material
increases with temperature , so high temperature
favour the leaving operation
Agitation
Agitation increase the eddy diffusion and thus
increase the rate of transfer of material from the
soild surface to the bulk of the solution
Example: Agitation favours the leaching process
Involved in leaching operation
1. Contacting the solid with the selective solvent in
order to dissolve soluble solute in the solvent
2. Separation of insoluble phases ,separation of
liquid phase from the solid phases physically by
settling , filtration, etc.,
In the component leaching operation, the
components are:
• pure solvent (A)
• Insoluble solid (B)
•Soluble solute (C)
 LEACHING EQUIPMENTS
• Different types of equipment used for leaching. 
Major two categories are
• Percolation....."Liquid Added to Solids“.
• The solvent is contacted with the solid in a
continuous or batch method. 
• This method is popular for in-place ore leaching or
large scale "heap" leaching. 
• Popular for extreme amounts of solids.
 Dispersed Solids

Dispersed Solids....."Solids Added to Liquid" The

solids are usually crushed into small pieces before
being contacted with solvents. 
This is a popular leaching method when an especially
high recovery rate can economically justify the
typically higher operating cost.
(Ex/ gold extraction)
Leaching EquipmentS
Two types on the basis of nature of solids:
• When the solid form an open permeable mass
throughout the leaching operation. Solvent
may be percolated through an unagitated bed
of solids.
• With impermeable solids or materials that
disintegrate during leaching, the solids are
dispersed into the solvent and later separated
from it.
Leaching by percolation

Two types
• Through stationary solid
beds
• Through Moving bed
leaching
Through stationary solid beds

• 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
1 passage of solvent is
sufficient otherwise
battery of tanks is used.
 Solid bed leaching
Shanks Process
• The tanks in the battery are kept in countercurrent operation by
advancing the inlet and drawoff tanks one at a time as the
material is charged and removed.
• Such a process is called as Shanks Process.

Diffusion Battery
• If the solvent used is volatile, then closed vessels should be
operated under pressure.
• Pressure is also needed to force solvent through beds of some
less permeable solids.
• A Series of such pressure tanks operated with counter current
solvent flow is known as a diffusion battery.
Heap Leaching
 Heap Leaching

• Then as these partially extracted solids rise through the left hand side
of the machine a stream of pure solvent is sprayed on them to obtain
a dilute solution of the oil (half miscella) at the bottom of the
chamber.
• This pure solvent percolates counter-currently through them and
collects in the left hand sump which is then passed to the Half
Miscella storage tank.
• The fully extracted solids are then dumped from the baskets at the
top of the elevator to the hoppers from which they are removed by
Screw Conveyors.
• Usually the conveyor speed is one revolution per hour.
 Heap Leaching
• Heap Leaching is a technique where run-of-mine or crushed
(generally >5 mm) and/or
• Agglomerated ores are stacked over an engineered
impermable pad, wetted with lixiviant (solvent) chemicals
under atmospheric conditions and leachate (metal loaded
solutions) are collected for metal reovery processes.
• Because percolation of the lixiviant solution through the ore
is acheived under gravity
• Atmosperic conditions, completion of metal recovery
requires longer time periods (weeks to months, even several
years in bio-processes) for each pad loading sequence
compared to tank leaching (hours to days).
• Upon completion of heap leaching, the processed ore stack is
generally decommissioned in place
 Heap Leaching

• This technique does not require use of a tailings

disposal (spent ore repository) facility.
• In some operations processing is done on a lined
surface that is covered with stabilized surface
(on/off pad) to allow removal of the processed
ore usually by loaders or mechanised equipment.
• The processed ore is moved to a lined facility
(spent ore repository) for final closure and
reclamation, with the stabilized/lined leach pad
area is being reused.
Dispersed Solid Leaching

Dispersed Solid Leaching

Solids that form impermeable beds, either before or during leaching, are
treated by dispersing them in the solvent by mechanical agitation in a tank
or flow mixer.

The leached residue is then separated from the strong solution by settling
or filtration.

Small quantities can be leached batch wise in this way in an agitated vessel
with a bottom draw off for settled residue. Continuous counter current
leaching is obtained with several gravity thickeners connected in series.

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Moving Bed Leaching

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 Bollman Extractor (or) Basket Extractor

• One of the very oldest continuous extractor and still listed among
the best is the Bollman Extractor.
• The Bollman Extractor was invented by H. Bollman in Germany in
1920.
• Bollman Extractor is mainly used for the recovery of additional oil
from the residues obtained after mechanical pressing of solids.
• The Bollman Extractor essentially consists of a vapour tight vertical
chamber in which a series of perforated baskets are attached to a
chain conveyor.
• The baskets are provided with perforations at the bottom.
• At the top right hand corner of the extractor solids are conveyed in
to the perforated baskets.
• The baskets are loaded with flaky solids.
 Bollman Extractor (or) Basket Extractor

• These fully loaded baskets are then sprayed with Half

Miscella as they travel downward through the right
hand side.
• Half Miscella is the intermediate solvent containing
some extracted oil and some small solid particles.
• As the solids and solvent flow co-currently down the
right hand side of the machine, the solvent extracts
more oil.
• Simultaneously the fine solids are filtered out of the
solvent, so that the clean full miscella can be pumped
from the outlet provided at the right hand bottom.
 ROTOCEL EXTRACTOR
• A horizontal basket is divided into walled
compartments with a floor that is permeable to the
liquid.
• The basket rotates slowly about a vertical axis.
• Solid are admitted to each compartment at feed
point.
• The compartments then pass a number of solvent
sprays, a drainage section and a discharge point.
• To give countercurrent extraction, the fresh solvent
is fed only to the last compartment before the
discharge point.
 AGITATED VESSEL

• Tube coils afford one of the cheapest means of obtaining heat transfer
surface.
• They are usually made by rolling lengths of copper, steel or alloy tubing
into helixes or doublehelix coils in which inlet and outlets are
conveniently located side by side.
• Helical coils of either type are frequently installed in vertical cylindrical
vessels with or without an agitator, although free space is provided
between the coil and the vessel wall for circulation.
• When such coils are used with mechanical agitation, the vertical axis of
the agitator usually corresponds to the vertical axis of the cylinder.
• However very limited data are available for predicting heat transfer
coefficient from submerged coil to the surrounding fluid in natural
• convection although the coefficients are undoubtedly lower.
• A mechanical agitation can improve the heat transfer coefficient
between fluid in the agitated vessel and the coil.
AGITATED VESSEL
Methods of Leaching
1. Single- stage leaching
2. Multistage leaching
Single- stage leaching

Solid to be Leached, B,F,NF,yF B,E1,N1,y1, Leached solid

Leaching solvent, Ro,xo R1,x1, Leach solution

Let
B - Mass insoluble in solids to be leached
F - Mass (A and C ) in solids to be leached
NF - (Mass B/Mass A+C) in solids to be leached
yF - (Mass C /Mass A+C) in solids to be leached
Ro - Mass solution (A+C) in leaching solvent
xo – Mass C/ mass (A+C) in leaching solvent
E1 - Mass (A+C) in leached solid
N1 - Mass B/ mass (A+C) in the leached solid
y1 - (Mass C /Mass A+C) in the leached solid
x1 - (Mass C /Mass A+C) in the leach solution
R1 - Mass solution (A+C) in the leach solution
Consider a single stage leaching operation in which the
solids to be leached are contacted with the leaching
solvent and then insoluble phases are physically
separated and effluent streams are withdrawn as
leached solid and leach solution
For no solid in the overflow and insolublity of B in A
Mass of insoluble (B) Mass of insoluble in the
In leached solid = solid to be leached
Material balance of B;
B = NF .F = E1 N1 ---------------1

Material balance of C
C in solids to be leached + C in leaching solvent =
C in leached solids + C in leach solution
F .yF + Ro xo = E1 y1 + R1 x1 -------------------2
Material balance of a solvent (A)
F .(1-yF ) + Ro (1-xo)= E1 (1-y1)+ R1 (1-x1 ) ----------3
Material balance of (A + C)
F + Ro = E1 + R1 = M1------------------4
Nm1 - Mass insolubles / Mass A+C) totally
Nm1 = B / F + Ro
= B / M1
From eq2
F .yF + Ro xo = E1 y1 + R1 x1 = M1 ym
F .yF + Ro xo = M1 ym
ym = F .yF + Ro xo / M1 M1 = F + Ro
ym = F .yF + Ro xo / F + Ro
Multi –stage cross current leaching
R1,x1 R2, x2 R3,x3 (Composited leach
Solution

Solid to be Leached solids Es,Ns, ys

leached F,Nf,yF

R0,x0 R0,x0 R0,x0

This simply an extraction of single stage leaching in which the

leached solids are successively contacted with fresh leach
solvents .This may be performed in batch or continously
here leached solids from any stage act as feed solids to that
next , so more and more amount of solute is removed from
the soilds
The figure shows three –stage cross current
leaching operation in which unequal amounts of
the leaching solvent of same composition are
used in all the 3 stages
Material balance of insoluble (B) for any stage n;
B = En-1 Nn-1 = En Nn ---------------1
Stage n
B = NF .F = E1 N1 ---------------2
Solution (A+C) balance for any stage –n is
En-1 + Ron = En + Rn = Mn ---------------3
For Stage ; 1
En-1 = F
E1 + Ro1 = E1 + R1 = M1 --------------- 4

For Stage ; 2
E1 + Ro2 = E2 + R2 = M2 --------------- 5

Balance of solute (C) for any stage –n:

En-1 yn-1+ Ron + xo = En yn + Rn xn = Mnymn ---------6
ymn = En-1 yn-1+ Ron + xo / Mn
ymn = En-1 yn-1+ Ron + xo / En-1 + Ron -----------7
But for stage 1
En-1 = F and yn-1 = yF
ym1 = F .yF + Ro1 + xo / F+ Ro1 -----------8
Concentration of insolubles:
Balance of B for any stage –n is
B = En-1 Nn-1 = En Nn = Mn Nmn
Nmn = B/ En-1 + Ron = B / Mn -------------9 En-1 =F
For stage :1
Nmn1 = B/ F+ Ro1 -------------------10
Fig shows the graphical representation of various
streams for 3-stage cross current leaching operation
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Ideal Stages In Counter Current Extraction:

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 Steps for identifying no. of ideal stages
• Equilibrium
• Operating Line:
• Constant and Variable underflow:
• Number of Ideal stages for constant underflow:

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Multi –stage counter current leaching

Consider multistage counter current leaching system

containing n- stage as shown in fig stage -1 represents
one end of the system at which the solids to be
leached are fed and from which strong leach solution
(overflow) of highest solute concentration
Stage –n represents another end of the system at which
fresh leaching solvent is introduced and from which the
leached solid (underflow)
with the lowest solute concentration leaves
Assume
Solid B is insoluble and clear strong leach solution is
obtained and steady state condition present
F – Mass (A+C)/ time in solids to be leached
B – Mass / time insoluble in solids to be leached
Material balance of solution (A+C) over the entire unit
F + Rn+1 = R1 + En = M-----------------------1
Material balance of solute (C) over the entire unit
F .yF + Rn+1 xn+1 = R1 x1 + En y0 = M ym ---------2
B = F .NF = En yn ---------------------3
Nm = B/ M = = B / F + Rn+1 ----------4
From equation (2)
F .yF + Rn+1 xn+1 = M ym
ym = F .yF + Rn+1 xn+1 / M
ym = F .yF + R+1 xn+1 / F + Rn+1 -------5
Equation 1 can be rearranged as
F - R1 = En - Rn+1 =∆R -----------------------6
Material balance of solution (A+C) over first 2 stages
F + R3 = R1 + E2 ---------------------- 7
465
=4.65/0.01
 EQUILIBRIUM
• Equilibrium is attained when the solute is
completely dissolved and the concentration of the
solution so formed is uniform.
• The concentration of the liquid retained by the
solid leaving any stage is the same as that of the
liquid overflow from the same stage.
• The equilibrium relationship is simply xe = y.
 OPERATING LINE
Total solution:

Solute:

Operating line equation:

 As usual, the operating line passes through the points (xa, ya) and
(xb, yb), and if the flow rates are constant, the slope is L/V.
 CONSTANT AND VARIABLE
UNDERFLOW
• Two cases are to be considered.
• If the density and viscosity of the solution change
considerably with solute concentration, the solids from the
lower-numbered stages may retain more liquid than those
from the higher-numbered stages.
• The slope of the operating line varies from unit to unit.
• If the mass of solution retained by the solid is independent
of concentration, then Ln is constant and the operating line
is straight. – called as constant solution underflow.
• If the underflow is constant, so is the overflow.
• Constant underflow and variable underflow are given
separate consideration.
 NUMBER OF IDEAL STAGES FOR
CONSTANT UNDERFLOW

• Use McCabe Thiele Method if the operating

line is straight
• In leaching, the operating line is always
straight
• The equilibrium line is on 450 line.
 NUMBER OF IDEAL STAGES FOR
VARIABLE UNDERFLOW

• When the underflow and overflow vary from stage to

stage, a modification of the McCabe Thiele graphical
method may be used for calculation.
• The terminal point on the operating line are
determined using material balances.
• Will be discussed later….
 QUESTION 1
EXAMPLE 23.1.
Oil is to be extracted from meal by means of benzene using a
continuous countercurrent extractor. The unit is to treat 1,000
kg of meal (based on completely exhausted solid) per hour. The
untreated meal contains 400 kg of oil and is contaminated with
25kg of benzene. The fresh solvent mixture contains 10kg of oil
and 655 kg of benzene. The exhausted solids are to contain
60kg of unextracted oil. Experiments carried out under
conditions identical with those of the projected battery show
that the solution retained depends on the concentration of the
solution, as shown in Table 23.1.
Find:
(a) the concentration of the strong solution, or extract;
(b) the concentration of the solution adhering to the extracted
solids;
(c) the mass of solution leaving with the extracted meal;
(d) the mass of extract;
(e) the number of stages required.
All quantities are given on an hourly basis.
1/N 2 1.98 1.94 1.87 1.818 1.75 1.68 1.61

x, y 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7

Basis: 1000 Kg of Meal

B= 1000 Kg
C (Oil) = 400 Kg
A (Solvent) = 25 Kg

NF = 1000/(A + C) = 2.35

yF = 400/425 = 0.94

Feed Point F is given by (NF, yF) = (2.35, 0.94)

 F

0 0.7 1.0
 Oil in the final extract ?

R Np+1 is given by (NNp+1, x Np + 1)

N Np+1 = 0/A+C = 0

xNp+1 = 10 / 665 = 0.015

R Np+1 = (0, 0.015)

= 67.5/(500 +67.5) = 0.118 Oil in the Feed = 400 Kg

Oil in the solid Feed after leaching = 60 Kg

= 1000/(500 +67.5) = 1.762
Assuming the solvent inlet and solid are in
equilibrium
Solution retained by the solid = 0.5 per kg of solid
Solution retained by the solid = 500 Kg
C in the solution retained by the solid - = 0.015 *
500 = 7.5 Kg
Oil (c) in the extrac t = 400 + 10 – 67.5 = 342.5
Solvent in the extract = 25 + 645 – 492.5 = 187.5
B=0

R1 (0, 342.5/(342.5+187.5) ) = (0, 0.65)

Oil in the final extract ?

R Np+1 is given by (NNp+1, x Np + 1)

N Np+1 = 0/A+C = 0

xNp+1 = 10 / 665 = 0.015

R Np+1 = (0, 0.015)

Oil in the Feed = 400 Kg

Oil in the solid Feed after leaching = 60 Kg

Assuming the solvent inlet and solid are in

equilibrium
Solution retained by the solid = 0.5 per kg of solid
Solution retained by the solid = 500 Kg
C in the solution retained by the solid - = 0.015 *
500 = 7.5 Kg
Solution
Let x and y be the mass fractions of oil in the underflow and
overflow solutions. At the solvent inlet,

Determine the amount and composition of the solution in the spent

solids by trial. If Xb = 0.1, the solution retained, from Table 23.1, is
0.505 kg/kg. Then;
From Table 23.1, the solution retained is 0.507 kg/kg:

Benzene in the underflow at Lb is 507 - 60 = 447 kg/h.

At the solid inlet,
e) Determine the inlet and exit concentrations for the first stage and
locate the operating line for the remaining stages.
Since x1 = ya = 0.60, solution retained is 0.595 kg/kg solid.

Overall material balance:

Oil balance:
• The point x1 = 0.60, y2 = 0.408 is at one end of the operating line
for the remaining stages.
• To determine an intermediate point on the operating line, choose
xn = 0.30.

• By an overall balance,

• An oil balance gives

• The points xn , xn+1 , xa , ya and xb , yb define a slightly curved
operating line, as shown in Fig. 23.3.
• Four ideal stages are required.
 QUESTION 2

EXCERCISE1 (LEACHING)
We wish to treat 1000 kg/hr (wet basis) of meal (D) that
contains 0.20 wt frac oil (A) and no benzene (S). The
inlet solvent is pure benzene and flows at 662
kg/hr. We desire an underflow product that is 0.04 wt
frac oil. Temperature and pressure are constant, and
the equilibrium data are given in Table 1. Find the
outlet extract concentration and the number of
equilibrium stages needed in a countercurrent
leaching system.
Test Data For Extraction Of Oil From Meal With Benzene

Mass Fraction Oil Mass Fraction Underflow (Rafffinate)

(Solute) in Solution
yA xA xD xS
0 0 0.67 0.333
0.1 0.0336 0.664 0.304
0.2 0.0682 0.66 0.272
0.3 0.1039 0.6541 0.242
0.4 0.1419 0.6541 0.213
0.5 0.1817 0.6366 0.1817
0.6 0.224 0.6268 0.1492
0.7 0.268 0.6172 0.1148
 QUESTION 2

The calculation procedure for countercurrent

leaching operations is exactly the same as for LLE.
1. Plot the equilibrium data.
2. Plot the locations of known points.
3. Find mixing point, M.
4. Locate EN.
5. Find the ∆ point.
6. Step off stages.