4 Leaching Solid Liquid Extraction

Mass Transfer (ChE - 392)
4-Leaching (Solid-Liquid Extraction)
Saeed GUL, Dr.Techn, M.Sc. Engg.

Associate Professor
Department of Chemical Engineering,

University of Engineering & Technology Peshawar, PAKISTAN
Introduction
Leaching is concerned with the extraction of a soluble
constituent from a solid by means of a solvent
The desired component diffuses into the solvent from its natural
solid form
Typical users include:
 the metals industry for removing mineral from ores
(acid solvents)
 the sugar industry for removing sugar from beets
(water is solvent)
 the oilseeds industry for removing oil from soybeans, etc.
(hexane or similar organic solvents)
6 May 2016 2
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
General Principles
Generally, the process can be considered in three parts:
1. The change of phase of the solute as it dissolves in the
solvent
2. Solute diffusion through the solvent in the pores of the solid
to the outside of the particle
3. 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
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General Principles
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.
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General Principles
If the soluble material is distributed in small isolated pockets in a

material which is impermeable to the solvent:
Such as gold dispersed in rock, for example. In such cases the
material is crushed so that all the soluble material is exposed to
the solvent.
If the solid has a cellular structure:
The extraction rate will generally be comparatively low because
the cell walls provide an additional resistance
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Factors influencing the rate of extraction
There are four important factors to be considered:
1. Particle Size
I. Smaller
II. Larger
III. Same particle size range
2. Solvent
I. Selective
II. Viscosity
3. Temperature
I. Solubility
II. Diffusion Coefficient
4. Agitation of the Fluid
I. Increases eddy diffusion
II. Prevent Sedimentation
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Mass Transfer in Leaching Operations
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.
It is possible, however, to obtain an approximate indication of
the rate of transfer from the particles to the bulk of the liquid.
Using the concept of a thin film as providing the resistance to
transfer, the equation for mass transfer may be written as:
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For a batch process in which V, the total volume of solution, is
assumed to remain constant, then:
The time t taken for the concentration of the solution to rise from
its initial value c0 to a value c is found by integration, on the
assumption that both b and A remain constant.
Rearranging:
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If pure solvent is used initially, c0 = 0, and:
which shows that the solution approaches a saturated condition

exponentially.
In most cases the 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 and the effective value of b will
be increased.
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Example 10.1
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Example 10.1
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Equipment for Leaching
Leaching by percolation through stationary solid beds

Moving-bed leaching
Dispersed-solid 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.
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Processes involved
Three distinct processes are usually involved in leaching
operations:
1. Dissolving the soluble constituent.
2. Separating the solution, so formed, from the insoluble solid
residue.
3. 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.
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.
The normal distinction between coarse and fine solids is that the
former have sufficiently large settling velocities for them to be readily
separable from the liquid, whereas the latter can be maintained in
suspension with the aid of only a small amount of agitation
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Extraction from cellular materials
With seeds such as soya beans, containing only about 15 per cent of oil,
solvent extraction is often used because mechanical methods are not
very efficient.
Light petroleum fractions
are generally used as
solvents. Trichlorethylene
has been used where fire
risks are serious, and
acetone or ether where the
material is very wet
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Extraction from cellular materials
Bollmann Extractor
 Continuous moving bed extractor
Series of perforated baskets
 widely used with seeds which do not
disintegrate on extraction
 A typical extractor moves at about 1
revolution per hour
 Each basket containing some 350 kg of
seeds.
 Generally, about equal masses of seeds
and solvent are used.
 The final solution, known as miscella,
contains about 25 per cent of oil by
mass
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Leaching of coarse solids
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Leaching of fine solids
Whereas coarse solids may be leached by causing the solvent to
pass through a bed of the material, 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.
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Leaching of fine solids
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Leaching Operations
Figure 1: Single-stage leaching unit
Figure 2: Multistage cross-flow leaching unit
Figure 3: Multistage countercurrent leaching unit

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Material Balance-Countercurrent Process
 The stages are numbered in the direction of flow of the solid.

 The light phase is the liquid that overflows from stage to stage in a
direction opposite to that of the flow of the solid, dissolving solute
as it moves from stage N to stage 1.
 The heavy phase is the solid flowing from stage 1 to stage N.
 Exhausted solids leave stage N, while concentrated solution
overflows leave from stage 1.
 For purposes of analysis, it is customary to assume that the solute
free solid is insoluble in the solvent so that the flow rate of this solid
is constant throughout the process unit
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Design and Predictive Equations
The solute /solvent equilibrium and process throughput determine the

cross-sectional area and the number of theoretical and /or actual
stages required to achieve the desired separation.
The equation for the operating line is obtained by writing a material
balance.
From Figure above
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If the density and viscosity of the solution change considerably with

solute concentration, the solids from the lower stages might retain
more liquid than those in the higher stages. The slope of the operating
line then varies from stage to stage.
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If, however, the mass of the solution retained by the solid is

independent of concentration, LN is constant, and the operating line
is straight. These two mentioned conditions describe variable and
constant overflow, respectively.
It is usually assumed that the inerts are constant from stage to stage
and insoluble in the solvent. Since no inerts are usually present in
the extract (overflow) solution and the solution retained by the
inerts is approximately constant, both the underflow LN and
overflow VN are constant, and the equation for the operating line
approaches a straight line.
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Since the equilibrium line is also straight, the number of stages can be
shown to be (with reference to Fig. 12.12)
The above equation should not be used for the entire extraction
cascade if Lo differs from L1, L2, . . . , LN (i.e., the underflows vary
within the system). For this case, the compositions of all the streams
entering and leaving the first stage should first be calculated before
applying this equation to the remaining cascade.
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Single stage problems
EXAMPLE
Calculate the grams of water that need to be added to 40 g of sand
containing 9.1 g salt to obtain a 17 % salt solution. If the salt
solution is to be reduced to 0.015, calculate the amount of salt
that must be removed (“leached”) from the solution.
SOLUTION:
Set V to be the grams of water required. The describing equation is:
Let Z be equal to the final amount of salt in the sand–water–salt

solution. The describing equation is
The amount of salt removed is therefore 9.1 2 0.61 ¼ 8.49 g.

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Single stage problems
A sand–salt mixture containing 20.4% salt enters a solid–liquid
extraction at a rate of 2500 lb /h. Calculate the hourly rate of fresh
water that must be added for 99% of the salt to be “leached” from the
sand–salt mixture if the discharge salt–water solution contains 0.153
(mass) fraction salt.
SOLUTION:
Let W equal to the hourly rate of water. The describing equation from
a mass balance is
Also note that the feed consists of 510 lb salt and 1990 lb sand. On
discharge, the sand contains only 5.1 lb salt. The discharge water
solution consists of the 2820 lb water plus 504.9 lb salt.
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Compositions in Ternary Diagrams
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Triangular Grid Method
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Representation of a three-component system on a
right-angled triangular diagram
Representation of underflow
stream
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Graphical method of solution with a
triangular diagram
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Number of Stages for Countercurrent
Washing by Graphical Methods
The separation of Soluble constituents from a solid by extraction

with a solvent
may be considered to consist of two steps:
1. Contacting the solid with liquid phase and
2. Separation of the liquid phase from the solid
In actual operation it is impossible to completely separate the
liquid phase from the solid. Consequently, the streams resulting
from the 2nd step will consist of:
 A liquid phase stream (solution) which during normal operation
does not contain any solid. This stream will be called overflow
 A slurry consisting of the solid plus adhering solution
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It is convenient to use the concept of a stage in performing the
calculations. A stage consist of two steps:
Contacting solid with liquid and
Separation of the overflow from the underflow
In Solid-Liquid extraction , an ideal stage is defend as :
A stage in which the solution leaving in the overflow is of the same
composition as the solution retained by the solid in the underflow
For the purpose of calculations, the solid-liquid extraction system may
be considered to consist of three components:
1. The solute component (A)
2. The inert solid component (B)
3. The solvent component (S)
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The calculations for leaching system may be based on the material
balance and the ideal stage concept.
Both mathematical and graphical methods of solution may be used.
The graphical solution possesses advantage in presenting a generalized
treatment of the more complex cases and in permitting a better
visualization of what is occurring in the process, although it may be
inconvenient to use if a large number of stages are involved but
typically in most of the cases the number of stages used is not large
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Rectangular Diagram
Mole fraction of Component S, xs S 100 % S
1
0.8
0.6
0.2
0.4
0.4
0.6
0.2
0.8
B A
0.2 0.4 0.6 0.8 100 % A
100 % B
Mole fraction of Component A, xA
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Single Stage Extraction system
Overflow Product Solvent Feed
V1, y1 Single Stage V2, y2
Feed
Extraction System Underflow Product
L0, x0 L1, x1
Overall Material Balance

L0 + V2 = L1 + V1
The Material Balance for components A, B and S:
L0(xA)0 + V2(yA)2 = L1(xA)1 + V1(yA)1
L0(xB)0 + V2(yB)2 = L1(xB)1 + V1(yB)1
L0(xS)0 + V2(yS)2 = L1(xS)1 + V1(yS)1

6 May 2016 36
Counter Current Multistage Extraction
System
V1 V2 V3 Vj Vj+1 Vn Vn+1
Stage Stage Stage Stage

L0 1 L1 2 L2 Lj -1 j Lj Ln-1 n Ln
Overall Material Balance

L0 + Vn+1 = Ln + V1
The Material Balance for components A, B and S:
L0(xA)0 + Vn+1(yA)n+1 = Ln(xA)n + V1(yA)1
L0(xB)0 + Vn+1(yB)n+1 = Ln(xB)n + V1(yB)1
L0(xS)0 + Vn+1(yS)n+1 = Ln(xS)n + V1(yS)1

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4 Leaching Solid Liquid Extraction

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Mass Transfer (ChE - 392)

4-Leaching (Solid-Liquid Extraction)

Saeed GUL, Dr.Techn, M.Sc. Engg.

Department of Chemical Engineering,

Any one of these three processes may

If the soluble material is distributed in small isolated pockets in a

which shows that the solution approaches a saturated condition

Leaching by percolation through stationary solid beds

Figure 1: Single-stage leaching unit

Figure 2: Multistage cross-flow leaching unit

Figure 3: Multistage countercurrent leaching unit

 The stages are numbered in the direction of flow of the solid.

The solute /solvent equilibrium and process throughput determine the

If the density and viscosity of the solution change considerably with

If, however, the mass of the solution retained by the solid is

Let Z be equal to the final amount of salt in the sand–water–salt

The amount of salt removed is therefore 9.1 2 0.61 ¼ 8.49 g.

The separation of Soluble constituents from a solid by extraction

Overall Material Balance

L0(xB)0 + V2(yB)2 = L1(xB)1 + V1(yB)1

L0(xS)0 + V2(yS)2 = L1(xS)1 + V1(yS)1

Stage Stage Stage Stage

Overall Material Balance

L0(xA)0 + Vn+1(yA)n+1 = Ln(xA)n + V1(yA)1

L0(xB)0 + Vn+1(yB)n+1 = Ln(xB)n + V1(yB)1

L0(xS)0 + Vn+1(yS)n+1 = Ln(xS)n + V1(yS)1

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