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)
2)
3)
4)
5)

The solvent is transferred from the bulk solution to the surface of the
solid.
The solvent penetrates or diffuses into the solid (intraparticle diffusion).
The solute dissolves from the solid into the solvent.
The solute diffuses through the mixture to the surface of the solid
(intraparticle diffusion).
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
k L c AS c A
A

Eq.1

dcA
V
N A Ak L c AS c A
dt

Integrating from time t = 0 and

cA = cA0 to t = t and cA = cA:
cA

dcA
Ak L

c c AS c A V
A0

dt

t 0

c AS c A
e k L A V t
c AS c A0

NA

kg mol of A dissolving to the solution per second

the surface area of particles in m 2

kL

mass tansfer coefficient in m/s

c AS saturation solubility of the solid solute A in the

solution in kg mol/m 3
c A concentration of A in the solution at time t sec in
kg mol/m 3

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:
N solid concentration in slurry

kg B (inert/leached solid)
kg solid

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

kg A kg C kg solution

solute concentration in overflow

yA

kg A
kg solute

kg A kg C kg solution

solute concentration in underflow

Calculation in Leaching

SINGLE STAGE LEACHING

COUNTER CURRENT MULTISTAGE LEACHING

Single stage Leaching

Process flow
Overflow solution

Solvent Feed

V2, xA2

V1, xA1

Underflow solution

Feed Slurry
L0, N0, yA0, B

V
L
B

Mass of overflow solution

Mass of liquid in slurry solution
Mass of dry, solute free solid.

L1, N1, yA1, B

xA
yA

Composition of A at overflow solution

Composition of A at slurry solution

Material balance is divided into 3 parts:

Total solution balance

L0 y A0 V2 x A2 L1 y A1 V1 x A1 Mx AM Comp. A balance
Solid balance
B N 0 L0 0 N1 L1 0 N M M
L0 V2 L1 V1 M

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
V1, xA1
Feed Slurry

L0, N0, yA0, B

Solvent Feed

V2, xA2
Underflow solution
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

y A0

A
A
20

1.0
L0 A C 20 0

N0

B
B
80

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

x2

A
A
0

0
V2 A C 0 100

N2

B
B
0

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

201.0 1000 120x 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

420 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

1.5L1 0.667120

L1 53.36 kg

Single stage calculations

Solution 1
From material balance calculations:

From Eq. (1)

V1 120 L1
V1 120 53.36

Eq.1
V1 66.64 kg

Multi stage counter current Leaching

Process flow
Overflow solution

Solvent Feed
VN+1, xN+1

V1, x1

Underflow solution

Feed Slurry

LN, NN, yN, B

L0, N0, y0, B

V
L
B

Mass of overflow solution

Mass of liquid in slurry solution
Mass of dry, solute free solid.

xA
yA

Composition of A at overflow solution

Composition of A at slurry solution

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
is obtained as the intersection of lines Lo V1 and
LNVN+1.
A vertical tie line through V1 locates L1. Line L1 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

VN+1, xN+1

V1, x1

Underflow solution

Feed Slurry

LN, NN, yN, B

L0, N0, y0, 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

VN+1, xN+1

V1, x1

Underflow solution

Feed Slurry

LN, NN, yN, B

L0, N0, y0, 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
y A0

A
A
800
800

0.94
L0 A C 800 50 850

N0

B
B
2000
2000

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
x N 1

A
VN 1

N N 1

B
VN 1

A
20
20

0.015
A C 20 1310 1330

B
0

0
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
Slope of graph,

NN
yN

B
N N LN B 2000

16.67
A
yN
A 120
LN

N 16.67 y

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
2

LN

L0

1
0

-0.4

-0.2

-1 0

VN 1

0.2

-2
-3
-4
-5
-6
-7
x A, y A

0.4

0.6

0.8

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

8500.94 13300.015 2180x 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

2.35850 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

V1

0
-0.2

-0.4

-1

VN 1

0.2

0.4

-2
-3
-4
-5
-6
-7

From figure,

L0

x A, y A

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

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

0.6

0.8

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 21800.376

Insert Eq. 1 into equation above

LN 0.12 2180 LN 0.592 21800.376

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

-1

VN 1

0.2

-2
-3
-4
-5

L0

V1

0
-0.2

L1

-0.4

L2

-6
-7
x A, y A

0.4

0.6

0.8