Separation

Processes II

Engr. Ajibola T. Ogunbiyi

Lecturer’s details:

Name: Engr. Ajibola T. Ogunbiyi

Office: Room F02, Petro-Chemical Building
Email: ajibola.ogunbiyi@cu.edu.ng

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SOLID-LIQUID EXTRACTION

LEACHING

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Recommended Texts:
1. Treybal, R. E. (1980). Mass-Transfer Operations. Singapore: McGraw-Hill.
2. McCabe, W. L., Smith, J. C., and Harriot, P. (1993). Unit Operations of
Chemical Engineering. Singapore: McGraw-Hill
3. Geankoplis, C. J. (1993). Transport Processes and Unit Operations (3rd
Edition). New Jersey, USA: Prentice-Hall International Inc.
4, Coulson, J.M. and Richardson, J.F. CHEMICAL ENGINEERING, Volume 1;
Butterworth-Heinemann
5. Coulson, J.M. and Richardson, J.F. (2002). CHEMICAL ENGINEERING,
Volume II. Fifth Edition. Particle Technology and Separation Processes.
Published by Butterworth-Heinemann
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Module Content
Introduction
Principles of leaching
Examples of leaching in the industry
Rate of Leaching
Methods of Operation and Equipment types
Unsteady-state Operation
Steady-state (Continuous) Operation
Methods of Calculation
Stage efficiency
Practical equilibrium
Single-stage leaching
Multistage Crosscurrent leaching
Multistage Countercurrent leaching
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INTRODUCTION TO LEACHING

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 General principles
Leaching, one of the oldest unit operation in the
chemical industries, has been given many names,
depending to some extent upon the technique used for
carrying it out.

Leaching, originally referred to percolation of the liquid

through a fixed bed of the solid, but is not used to
describe the operation generally, by whatever means it
may be done. Engr. A. T. Ogunbiyi CHE320
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Leaching has to do with the extraction of a soluble
component of a solid mixture by means of a solvent.
The process may be used either for the production of a
concentrated solution of a valuable solid material, or to
remove an insoluble solid, such as a pigment, from a
soluble material with which it is contaminated.

Leaching is the selective solution of a component from a

solid mixture by a liquid solvent. The diffusion in this
case is from the solid to the liquid phase.
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Examples of leaching operations
1. Leaching processes for biological substances
a. Biological and food processing industry
- Extraction of vegetable oil from seeds like soybean, cottonseed,etc by
leaching with organic solvents
- Extraction of sugar from sugar beets using hot water
- Production of soluble instant coffee, ground roasted coffee is leached
with fresh water.
- Making of soluble tea
b. Pharmaceutical industry – leaching plant roots, leaves, and
stem. Tannin is produced from tree bark via leaching with water
(in agriculture).
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2. Leaching processes for inorganic and organic materials
Large uses of leaching processes take place in the metallurgy
industry – processing of metals.
• Extraction of metal like:
- Copper: leaching with sulphuric acid or ammoniacal solutions
- Cobalt:
- Nickel:
- Gold: leaching of gold ores with sodium cyanide solution
Other metals are aluminium, manganese, zinc, etc
3. Washing: chemical precipitates are frequently washed of their
adhering mother liquors
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Solid preparation for leaching:

1. For inorganic and organic materials:

- proportion of the soluble constituents present
- its distribution throughout the original solid
- the nature of the solid - plant cells or whether the solute is
surrounded by a mass of insoluble matter.
- the original particle size

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Case (a): If the soluble material is surrounded by a matrix of insoluble
(impervious) matter, the solvent must then diffuse into the mass, and the
resulting solution must diffuse out, before a separation can result.
Crushing and grinding will be needed in this case to increase the leaching
rate, since this will aid the accessibility of the soluble portions by the
solvent. This is the case with many metallurgical materials.

Case (b):When the soluble material is more or less uniformly distributed

throughout the solid or even in solid solution, the grinding action may
not be necessary. The passage of additional solvent is then made easier,
and grinding to very small sizes may not be necessary. Grinding of the
particle is not necessary if the soluble material is dissolved in the solution
adhering to the solid. In this case, simple washing can then be used.
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2. Vegetable and animal bodies:
- biological materials are cellular in structure and the soluble components are
generally found inside the cells
- rate of leaching may be slow due to the resistance to diffusion from the cell
- sugar beets are cut into thin wedge-shaped slice for faster leaching action
- the cells of sugar beets are kept intact to make it semi-permeable

• Leaching of pharmaceuticals from leaves, stem and roots

- drying of the material before extraction helps rupture the cell wall, making
the solute easily dissolvable
- Cellwalls of soybean and vegetable seeds are significantly ruptured when the
original sizes are reduced to about 0.1 to 0.5 mm, making the vegetable oil easily
accessible to the solvent

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RATE OF LEACHING

Three general steps of a leaching process:

(1) the change of phase of the solute as it dissolves in the solvent,
(2) its diffusion through the solvent in the pores of the solid to the
outside of the particle (picture this), and
(3) the transfer of the solute from the solution in contact with the
particles to the main bulk of the solution.

Any one of the above 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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Factors affecting the rate of leaching
• The selection of the equipment for an extraction process is influenced
by factors which are responsible for limiting the extraction rate
(controlling factor).

• 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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1. Particle size: Particle size influences the extraction rate in a
number of ways. The 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.

2. Solvent: a liquid with a selective dissolvability with sufficiently

low viscosity should be chosen.

3. Temperature: generally, higher temperature leads to increases

the solubility of the solute in the solvent, lower the viscosity of the
liquid and increases the diffusivities, thereby causing increased
rates of leaching. There are exceptions though – sugar beets - (read
up). Engr. A. T. Ogunbiyi CHE320
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4. Agitation: 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, as discussed in the following section. Further,
agitation of suspensions of fine particles prevents
sedimentation and more effective use is made of the
interfacial surface.

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Mass transfer in leaching operation/rate of leaching
when dissolving a solid
When a material is being dissolved from the solid to the solvent
solution, the rate of mass transfer from the solid surface to the liquid is
the controlling factor. There is essentially no resistance if it is a pure
material.
The rate of mass transfer of the solute A being dissolved to the solution
of volume V (m3) is

ഥ𝐴
𝑁
= 𝑘𝐿 (𝑐𝐴𝑠 − 𝑐𝐴 ) (1)
𝐴

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Where
ഥ𝐴 is kgmol of A dissolving to the solution/s,
𝑁
A is surface area of particles in m2,
𝑘𝐿 is a mass-transfer coefficient in m/s,
𝑐𝐴𝑠 is the saturation solubility of the solid solute A in the solution in
kgmol/m3,
and 𝑐𝐴 is the concentration of A in the solution at time t sec in kg
mol/m3.

By a material balance, the rate of accumulation of A in the solution is

equal to:

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 𝑑𝑐𝐴
𝑉 ഥ𝐴 = 𝐴𝑘𝐿 (𝑐𝐴𝑠 − 𝑐𝐴 )
=𝑁 (2)
𝑑𝑡

(3)

(4)

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Interpretation:
• The solution approaches the saturated condition exponentially.

• Usually, the interfacial area A will increase during the extraction if the
external surface becomes irregular.

• If the soluble material forms a high proportion of the total solid,

disintegration of the particles may occur.

• If the solid is completely dissolving, the interfacial area changes

markedly. In that case, the mass-transfer may then change.
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Special cases:
• For very small particles, mass-transfer coefficient can be predicted
using the following equations: (section 7.4 - Geankoplis)

Read up: Equations of mass

transfer to small particles/mass
transfer to suspension of small
particles.

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• For larger particles, the case usually experienced in leaching, the
equations used to predict the mass-transfer coefficient, kL in agitated
mixing vessels are: (section 7.4; Reference B1) - Geankoplis

• Read up: Principle of unsteady-state diffusion and convective mass

transfer (for more information.

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Example

To be solved later.

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 Day 2, Week 4

LEACHING EQUIPMENT

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LEACHING EQUIPMENT
Processes involved in leaching:
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.
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Different classifications of leaching equipment
1. Classification based on nature of solid – granular or cellular and
coarse or fine. (Richardson & Coulson, Vol. 2)
(a) Extraction from cellular materials
- Bollman continuous moving bed extractor
(b) Leaching of coarse solids
- Dorr classifier
(c) Leaching of fine solids
- Dorr agitator
- Thickeners
(d) Batch leaching in stirred tanks

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2. Classification based on the position/motion of leaching bed
(Gean Koplis &McCabe & Smith)
(a) Fixed-bed leaching (by percolation through stationary solid beds)
- extraction battery (shanks process)
- diffusion battery
(b) Moving-bed leaching
- Bollman extractor
- Hildebradt extractor
(c) Agitated solid leaching
- thickeners
(d) Dispersed solid leaching
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3. Classification based on solid type
Two (2) major techniques are used here:

1. Spraying or trickling the liquid over the solid

(percolation) – coarse solids

2. Immersing the solid completely in the liquid – fine solids

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4. Classification based on mode of operation
Treybal

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Methods of operation of leaching equipment
• Batch and semi-batch operations – unsteady state conditions

• Continuous operation – steady state conditions

- stage-wise and continuous-contact equipment

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.
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Unsteady-state operation
This can be divided into two:

1. Batch operation: This includes those operations where the solid

and liquid are contacted in a purely batchwise fashion

2. Semi-batch: where a batch of solid is contacted with a continually

flowing stream of liquid.

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2. Classification based on the position/motion of leaching bed
(Gean Koplis &McCabe & Smith)
(a) Fixed-bed leaching (by percolation through stationary solid beds)
- extraction battery (shanks process)
- diffusion battery
(b) Moving-bed leaching
- Bollman extractor
- Hildebradt extractor
(c) Agitated solid leaching
- thickeners
(d) Dispersed solid leaching
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Typical fixed-bed apparatus

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Moving-bed leaching

Bollman extractor

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Bollman bucket-type extractor
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Bollmann extractor – filling and emptying of baskets

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Hildebrandt screw-conveyor extractor
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Thickeners

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4. Classification based on mode of operation
Treybal

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In-place (in situ) leaching (Solution Mining)

Source: Liu X, Xing X, Wen D, Chen L, Yuan Z, Liu B, Tan J. Mining-Induced Time-Series Deformation Investigation
Based on SBAS-InSAR Technique: A Case Study Engr.of
A. T.Drilling
Ogunbiyi Water Solution Rock Salt Mine. Sensors. 2019;
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19(24):5511. https://doi.org/10.3390/s19245511
The reagent must be injected continuously through one set of pipes
drilled down while the resulting liquor are pumped out through a
different set. Alternatively, the reagent may be pumped down
intermittently and withdrawn through the same well.

Applications:
• Removal of salt from deposit from below the earth’s surface by
dissolution of the salt in water which is pumped down the earth
• Leaching of low-grade copper ores containing as little as 0.2% copper
and to ores as deep as 1100 ft below the earth’s surface.
• Used in the solution mining of uranium

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Reading Assignment

Read up “leaching equipment”

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Assignment 8 marks
Choose an industrial process of your choice that employs leaching as one of
the unit operations, for example, production of soybean oil from soybean
seeds, the production of sugar from sugar-beets, extraction of a specified
metal from its ores, etc (you can refer to the examples of leaching operations
in the slide). Describe the entire process briefly from A to Z. Then, zero in on
the leaching aspect of the process with a detailed description - type of solids
to be leached, rationale behind choice of leaching equipment type, name and
category of extractor used, solid preparation method, method of operation
(steady or unsteady), continuous-contact or stagewise, schematic of
equipment and the description of the process including the process
conditions.
Both soft copy and hard copies are to be submitted. The writeup must be in font 12, Arial,
1.5 spacing, not more than 7 pages in all and is to submitted via the “turnitin” plagiarism
checker platform. Check the Moodle today, Friday 18th June, 2021 for the complete
information including the date of submission.

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Next Class

Methods of Calculation

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