CHAPTER 3: SOLID – LIQUID

EXTRACTION / LEACHING
 CHAPTER / CONTENT

Introduction to Leaching Process

Rates of Leaching

Types of Equipments for Leaching

Equilibrium Relations in Leaching

Calculation in Leaching
 Introduction to Leaching Process

Widely used in the metallurgical, natural product and food industries

under batch, semi – continuous or continuous condition.

The major difference between Leaching and LLE centers about the difficulty
to transport the solid or the solid slurry from stage to stage.

Leaching or also known as solid – liquid exraction involves dissolving

soluble material from its mixture with an insoluble solid.

Many biological inorganic or biological organic substances occur in a

different mixture of different components in a solid.

In order to separate the desired solute constituent or remove the

undesirable solute component from the solid phase, the solid is contacted with
a liquid phase.
 Introduction to Leaching Process

The solutes are diffuse from the solid to the liquid phase, which causes a
separation of the components in the solid by a contact with liquid solvent.

Leaching process applications:

Separation of sugar from sugar beets with hot water.

Extraction of oil from peanuts, soybeans, sunflower seeds, etc. using organic
solvent such as hexane.

Removing metals from their ores. For example, gold is leached from its ore
using an aqueous sodium cyanide solution.
 Introduction to Leaching Process

Simple leaching process: making of green tea

 Rates of Leaching

PRINCIPLES OF LEACHING

RATE OF LEACHING WHEN DISSOLVING A SOLID

METHODS OF OPERATING IN LEACHING

 Principles of Leaching

Generally there are five rate steps in the leaching process:

1) The solvent is transferred from the bulk solution to the surface of the
solid.
2) The solvent penetrates or diffuses into the solid (intraparticle diffusion).
3) The solute dissolves from the solid into the solvent.
4) The solute diffuses through the mixture to the surface of the solid
(intraparticle diffusion).
5) The solute is transferred to the bulk solution.
 Batch leaching

The rate of mass transfer of the solute A being dissolved to the solution of
volume V in m3 is:
where
 NA  kg mol of A dissolving to the solution per second
 k L c AS  c A   Eq.1
NA
A  the surface area of particles in m 2
A
kL  mass tansfer coefficient in m/s
 c AS  saturation solubility of the solid solute A in the
 N A  Ak L c AS  c A 
dcA
V solution in kg mol/m 3
dt
c A  concentration of A in the solution at time t sec in
kg mol/m 3
Integrating from time t = 0 and
cA = cA0 to t = t and cA = cA:

cA t
dcA Ak L
c c AS  c A V
  dt
t 0
A0

c AS  c A
 e k L A V  t
c AS  c A0
 Types of Equipments for Leaching

FIXED – BED LEACHING

MOVING BED LEACHING

AGITATED SOLID LEACHING

 Fixed – Bed Leaching

Used in beet sugar industry and is also used for extraction of tanning
extracts from the tanbark, extraction of pharmaceuticals from barks and
seeds and other processes.

Figure 12.8-1 shows a typical sugar beet diffuser or extractor.

The cover is removable so that

sugar beet slices called cossettes can
be dumped into the bed.

Heated water at 344 K to 350 K

flows into the bed to leach out the
sugar.

The leached sugar solution flows

out the bottom onto the next tank in
series.

About 95% of the sugar in beets is

leached to yield an outlet solution
from the system of about 12 wt%.
 Moving – Bed Leaching

There are number of devices for stagewise countercurrent leaching where

the bed or stages moves.

Used widely in extracting oil from vegetable seeds such as cottonseeds,

peanuts and soybeans.

The seeds are usually dehulled first, sometimes precooked, often partially
dried and rolled or flaked.

The solvents used are

particularly hydrocarbons such
as hexane and the final solvent
– vegetable solution called
miscella may contain some
finely divided solids.
 Agitated Solid Leaching

When the solid can be ground fine abou 200 mesh (0.074 mm), it can kept
in suspension by small amounts of agitation.

Continuous countercurrent leaching can be accomplished by placing the

number of agitator in series, with setttling tanks or thickeners between each
agitator.

Sometimes thickeners are used as combination contactor – agitators and

settlers – shown in Figure 12.8-3.
 Equilibrium Relations in Leaching

To analyze single – stage and countercurrent – stage leaching, an operating line

equation, or material balance relation and the equilibrium relations between the
two streams are needed as in LLE.

Assumptions made by achieving the equilibrium relations:

Sufficient solvent is present so that all the solute in the entering solid dissolved
in the solvent.
The solute in the entering solid dissolved completely in the first stage.
No adsorption of the solute by the solid.

The settled solid leaving a stage always contains some liquid in which dissolved
solids is present.

Consequently, the concentration of oil or solute in the liquid or overflow stream

(xA) is equal to the concentration of solute in the liquid solution accompanying the
slurry or underflow stream (yA).

The amount of solution retained with the solids in the settling portion of each
stage may depend the density and viscosity of liquid in which the solid is
suspended.
 Equilibrium Relations in Leaching

The solid – liquid stream is called underflow or slurry stream.

The solute – liquid stream is called overflow or liquid solution stream.

Concentration of solute in the liquid or overflow stream (xA) is equal to the

concentration of solute in the liquid solution accompanying the slurry or
underflow stream (yA).

Equilibrium diagrams for leaching:

 Equilibrium Relations in Leaching

The three components in leaching process:

solute (A) Inert/leached solid (B) Solvent (C)

The concentration of inert or insoluble solid B in the solution mixture or the

slurry mixture can be expressed as:

kg B (inert/leached solid) kg solid

N  solid concentration in slurry  
kg A (solute)  kg C (solvent) kg solution
For overflow, N = 0

For underflow, N value depending on the solute concentration in the liquid.

The composition of solute A in liquid will be expressed as wt fractions:

xA 
kg A

kg solute
solute concentration in overflow 
kg A  kg C kg solution

yA 
kg A

kg solute
solute concentration in underflow 
kg A  kg C kg solution
 Calculation in Leaching

SINGLE – STAGE LEACHING

COUNTER – CURRENT MULTISTAGE LEACHING

 Single – stage Leaching

Process flow

Overflow solution Solvent Feed

V1, xA1 V2, xA2

Feed Slurry Underflow solution

L0, N0, yA0, B L1, N1, yA1, B

V Mass of overflow solution xA Composition of A at overflow solution

L Mass of liquid in slurry solution yA Composition of A at slurry solution
B Mass of dry, solute – free solid.

Material balance is divided into 3 parts:

L0  V2  L1  V1  M Total solution balance

L0 y A0  V2 x A2  L1 y A1  V1 x A1  Mx AM Comp. A balance
B  N 0 L0  0  N1 L1  0  N M M Solid balance
 Single – stage Leaching

Plot equilibrium diagram. N vs yA and N vs xA.

Plot points V2 (xA2, N) and Lo (yAO, NO).

Plot point M (xAM, NM).

The line V2LoM is drawn.

The vertical tie line is drawn through point M locating

L1 (yA1, N1) at N vs yA line and V1 (xA1, N) at N vs xA
line.

Find the composition of solute in overflow (xA1) and

underflow (yA1).

Find the amount of V1 in overflow and L1 in

underflow using balance equation.
 Single – stage calculations

Example 12.9-1

In a single – stage leaching of soybean oil from flaked soybeans with hexane, 100
kg of soybean containing 20 wt% oil is leached with 100 kg of fresh hexane solvent.

The value of N for the slurry underflow is essentially constant at 1.5 kg insoluble
solid/kg solution retained.

Calculate the amounts and compositions of the overflow V1 and the underflow
slurry L1 leaving the stage.
 Single – stage calculations

Solution 1

Overflow solution Solvent Feed

V1, xA1 V2, xA2

Feed Slurry Underflow solution

L0, N0, yA0, B L1, N1, yA1, B

Information given:

Feed slurry = 100 kg containing 20 wt% oil

Entering solvent, V2 = 100 kg N = 1.5 kg B/kg (A+C)

 Single – stage calculations

Solution 1

Find coordinate at L0.

Mass of A = 0.20 x 100 A = 20 kg

Mass of B = 0.80 x 100 B = 80 kg

Mass of C = 0 kg C = 0 kg

A A 20
y A0     1.0
L0 A  C 20  0
B B 80
N0     4 .0
L0 A  C 20  0

Coordinate for L0 (yA0 , N0) = (1.0 , 4.0)

 Single – stage calculations

Solution 1

Find coordinate at V2.

Mass of A = 0 A = 0 kg

Mass of B = 0 B = 0 kg

Mass of C = 100 kg C = 100 kg

A A 0
x2    0
V2 A  C 0  100
B B 0
N2    0
V2 A  C 0  100

Coordinate for V2 (x2 , N2) = (0 , 0)

 Single – stage calculations

Solution 1

From material balance calculations:

Total solution balance:

L0  V2  L1  V1  M
20  100  M M  120 kg

Component A balance:

L0 y A0  V2 x A2  Mx AM
201.0  1000  120x AM
x AM  0.167
 Single – stage calculations

Solution 1

Solid balance:

B  N 0 L0  N1 L1  N M M
N 0 L0  N M M
420  N M 120 N M  0.667

Coordinate for M (xM , NM) = (0.167 , 0.667)

Plot coordinate M in the graph.

Construct straight vertical line through point M in order to find value V1 and
L1
 Single – stage calculations

Solution 1

From figure,

Coordinate for V1 (x1 , N1) = (0.167 , 0)

Coordinate for L1 (y1 , N1) = (0.167 , 1.5)

 Single – stage calculations

Solution 1

From material balance calculations:

Total solution balance:

L1  V1  M
L1  V1  120
V1  120  L1  Eq.1

Solid balance:

B  N 0 L0  N1 L1  N M M
N1 L1  N M M
1.5L1   0.667120 L1  53.36 kg
 Single – stage calculations

Solution 1

From material balance calculations:

From Eq. (1)

V1  120  L1  Eq.1
V1  120  53.36 V1  66.64 kg
 Multi – stage counter current Leaching

Process flow

Overflow solution Solvent Feed

V1, x1 VN+1, xN+1

Feed Slurry Underflow solution

L0, N0, y0, B LN, NN, yN, B

V Mass of overflow solution xA Composition of A at overflow solution

L Mass of liquid in slurry solution yA Composition of A at slurry solution
B Mass of dry, solute – free solid.
 Multi – stage counter current Leaching

The ideal stages are numbered in the direction of the solids or underflow stream.

The solvent (C) – solute (A) phase or V phase is the liquid phase that overflows
continuously from stage to stage countercurrently to the solid phase, and it
dissolves solute as it moves along.

The slurry phase L composed of inert solid (B) and liquid phase of A and C is the
continuous underflow from each stage.

Composition of V – denoted by x

Composition of L – denoted by y

Assumption: The solid B is insoluble and is not lost in the liquid V phase.

The flow rate of solid is constant throughout the process

Multi – stage counter current Leaching

Total solution balance :

L0  VN 1  LN  V1  M

Component A balance :
L0 y A 0  VN 1 x AN 1  LN y AN  V1 x A1  Mx AM

Solid balance :
B  N 0 L0  N N LN  N M M
 Multi – stage counter current Leaching

Plot equilibrium diagram. N vs yA and N vs xA.

Plot points VN+1 (xAN+1, N) and Lo (yAO, NO).
Plot point LN (yAN, NN). The point LN lies on the N vs
yA line. For this point, find the ratio (slope) of NN/yAN.
N N  kg solid/kg solution   kg solid 
     
y AN  kg solute/kg solution   kg solute (underflow) 
A dashed line is plotted through the origin at yA = 0
and N = 0 with a slope of NN/yAN, which intersects the
N vs yA line at LN. The coordinates of LN are read from
the graph as (yAN , NN).
Plot point M (xAM, NM).
The line VN+1LoM is drawn as is line LNM. Extend the
line LNM to intersect N = 0 at V1(xA1, 0), Value of xA1 is
read from the graph.
Find the amount of V1 and LN using balance equation.
To determine number of stages, the operating point Δ
is obtained as the intersection of lines Lo V1 and
LNVN+1.
A vertical tie line through V1 locates L1. Line L1Δ is
drawn and give V2. Continue until the desired LN is
reached.
 Multi – stage counter current Leaching

Example 12.10-1
A continuous countercurrent multistage system is to be used to leach oil from meal
by benzene solvent (B3).

The process is to treat 2000 kg/h of inert solid meal (B) containing 800 kg oil (A)
and also 50 kg benzene (C).

The inlet flow per hour of fresh solvent mixture contains 1310 kg benzene and 20
kg oil. The leached solids are to contain 120 kg oil.

Data (B3) are tabulated below as N kg inert solid B/kg solution and yA kg oil A/kg
solution

Calculate the amounts and concentrations of the stream leaving the process and the
number of stages required.
 Multi – stage counter current Leaching

Solution 2

Overflow solution Solvent Feed

V1, x1 VN+1, xN+1

Feed Slurry Underflow solution

L0, N0, y0, B LN, NN, yN, B

Information given:

Feed slurry (L0):

A = 800 kg/h B = 2000 kg/h C = 50 kg/h

Entering solvent (VN+1 )

A = 20 kg/h B = 0 kg/h C = 1310 kg/h

 Multi – stage counter current Leaching

Solution 2

Overflow solution Solvent Feed

V1, x1 VN+1, xN+1

Feed Slurry Underflow solution

L0, N0, y0, B LN, NN, yN, B

Information given:

Underflow solution (LN):

A =120 kg/h B = 2000 kg/h C = ?? kg/h

 Multi – stage counter current Leaching

Solution 2

Find coordinate at L0.

Mass of A = 800 kg/h

Mass of B = 2000 kg/h

Mass of C = 50 kg/h

A A 800 800
y A0      0.94
L0 A  C 800  50 850
B B 2000 2000
N0      2.35
L0 A  C 800  50 850

Coordinate for L0 (yA0 , N0) = (0.94 , 2.35)

 Multi – stage counter current Leaching

Solution 2

Find coordinate at VN+1.

Mass of A = 20 kg/h

Mass of B = 0 kg/h

Mass of C = 1310 kg/h

A A 20 20
x N 1      0.015
VN 1 A  C 20  1310 1330
B B 0
N N 1    0
VN 1 A  C 20  1310

Coordinate for VN+1 (xN+1 , NN+1) = (0.015 , 0)

 Multi – stage counter current Leaching

Solution 2

Find coordinate at LN.

Mass of A = 120 kg/h

Mass of B = 2000 kg/h

Mass of C = ?? kg/h
NN
Slope of graph,
yN
B
N N LN B 2000
    16.67  N  16.67 y
yN A A 120
LN

If y = 0.1, N = 16.67 x 0.1 = 1.67

Plot New Coordinate (y , N) = (0.1 , 1.67)

 Multi – stage counter current Leaching

Solution 2

3
LN
2 L0
1
0
VN 1
-0.4 -0.2 -1 0 0.2 0.4 0.6 0.8 1
N

-2
-3
-4
-5
-6
-7
x A, y A
 Multi – stage counter current Leaching

Solution 2

From material balance calculations:

Total solution balance:

L0  VN 1  LN  V1  M
L0  VN 1  M
850  1330  M M  2180 kg

Component A balance:

L0 y A0  VN 1 xN 1  Mx AM
8500.94  13300.015  2180x AM
x AM  0.376
 Multi – stage counter current Leaching

Solution 2

From material balance calculations:

Solid balance:

B  N 0 L0  N N LN  N M M
N 0 L0  N M M
2.35850  N M 2180 N M  0.916

Coordinate for M (xM , NM) = (0.376 , 0.916)

Plot coordinate M in the graph.

Construct line from point LN to point M until it cross at x – axis. Point at x –

axis = V1
 Multi – stage counter current Leaching

3
LN
2 L0
M
1
V1
0 VN 1
-0.4 -0.2 0 0.2 0.4 0.6 0.8 1
-1
N

-2
-3
-4

-5
-6
-7
x A, y A
From figure,

Coordinate for V1 (x1 , N1) = (0.592 , 0)

Coordinate for LN (y1 , N1) = (0.12 , 2.0)

 Multi – stage counter current Leaching

Solution 2

From material balance calculations:

Total solution balance:

V1  2180  LN  Eq.1

Component A balance:
LN y N  V1 x1  Mx AM
LN 0.12  V1 0.592  21800.376

Insert Eq. 1 into equation above

LN 0.12  2180  LN 0.592  21800.376
0.12LN  1290.56  0.592LN  819.68
0.472LN  470.88  LN  997.62 kg
 Multi – stage counter current Leaching

Solution 2

From material balance calculations:

Total solution balance:

V1  2180  LN  Eq.1
V1  2180  997.62

V1  1182.38 kg

Construct operating point:

Connect L0 with V1 & LN with VN+1. The cross line – operating point.

Total stages: 4 stages

 Multi – stage counter current Leaching

Solution 2
Construct the stages:

3
LN L3 L2
2 L1 L0
M
1
V1
0 VN 1
-0.4 -0.2 0 0.2 0.4 0.6 0.8 1
-1
N

-2
-3
-4

-5
P -6
-7
x A, y A