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CHAPTER 3: SOLID LIQUID

EXTRACTION / LEACHING
CHAPTER / CONTENT
Introduction to Leaching Process
Principles of Leaching

Single Stage Calculation
Multi Stage Countercurrent system
Leaching equipment
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 is also known as solid liquid exraction

In leaching, to separate the desired solute constituent or remove the
undesirable solute component from the solid phase, the solid is contacted with
a liquid phase.

The two phases are in intimate contact and the solute or solutes can diffuse
from the solid to the liquid phase, which causes a separation of the
components originally in the solid.

This process is called liquid solid leaching or simply leaching
Introduction to Leaching Process

Leaching process for biological substances
Introduction to Leaching Process
An important such process is to leach sugar from sugar beets with hot water.

In production of vegetable oils, organic solvents such as hexane, acetone and
ether are used to extract the oil from peanuts, soybeans, flax seeds, castor beans,
sunflower seeds, etc.

In pharmaceutical industry, many different pharmaceutical products are
obtained by leaching plan roots, leaves and stems.

For instant coffee, ground roasted coffee is leached with water and soluble tea
is produced by water leaching of tea leaves.

Tannin is removed from tea barks by leaching with water.
Leaching process for inorganic and organic materials
Introduction to Leaching Process
Used in metal processing industries

In metal ores, the desired metal components usually occur with a large amount
of undesirable constituents and leaching is used to obtain these metal
components in the form of metal salts.

E.g.: Copper salts are leached by dissolving raw copper ores by using sulfuric
acid or ammoniacal solutions.

E.g.: Nickel salts are leached using sulfuric acid ammonia oxygen mixures.

Gold is leached using an aqueous sodium cyanide solution.

The solvent must be transferred from the bulk solvent solution to the
surface of the solids.

Next, the solvent must penetrate or diffuse into the solids.

The solute then diffuses through the solid solvent mixture to the surface
of the particle.

Finally, the solute is transferred to the bulk solution.

The rate of the solvent transfer from the bulk solution to the solid surface
is quite rapid.

However, the rate of transfer of the solvent into the solid can be rather
slow or rapid.

This solvent transfer usually occurs initially when the particle are first
contacted with the solvent.
Principles of Leaching

The rate of diffusion of the solute through the solid and solvent to the
surface of the solid is often the controlling resistance in the overall leaching
process and can depend on a number of different factors.

If the solid is made of porous the diffusion through the porous solid can
be described by an effective diffusivity.

The resistance to mass transfer to the solute from the solid surface to the
bulk solvent is generally quite small compared to the resistance to the
diffusion within the solid itself.
Principles of Leaching
SINGLE STAGE LEACHING
COUNTER CURRENT MULTISTAGE LEACHING
Calculation in Leaching
Single stage Leaching
Process flow
Feed Slurry
L
0
,

N
0
, y
0
, B
Overflow solution
V
1
,

x
1

Underflow solution
L
1
,

N
1
, y
1
, B
V
2
,

x
2

Solvent Feed
V Mass of overflow solution x
A
Composition of A at overflow solution
L Mass of liquid in slurry solution y
A
Composition of A at slurry solution
B Mass of dry, solute free solid.
N Mass of dry,solute (B)/Mass of solution retained (L)
Material balance is divided into 3 parts:
( )
( )
( ) balance Solid
balance A Comp.
balance solution Total
M N L N L N B
Mx x V y L x V y L
M V L V L
M
AM A A A A
= + = + =
= + = +
= + = +
0 0
1 1 0 0
1 1 1 1 2 2 0 0
1 1 2 0
Example 1
Single stage calculations
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 V
1
and the underflow
slurry L
1
leaving the stage.
Single stage calculations
Solution 1
Information given:
Entering solvent, V
2
= 100 kg

Feed Slurry
L
0
,

N
0
, y
0
, B
Overflow solution
V
1
,

x
1

Underflow solution
L
1
,

N
1
, y
1
, B
V
2
,

x
2

Solvent Feed
Feed slurry = 100 kg containing 20 wt% oil

N = 1.5 kg B/kg (A+C)

Single stage calculations
Solution 1
Find coordinate at L
0
.
Coordinate for L
0


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
0 . 4
0 2
80
0 . 1
0 2
20
0
0
0
0
=
+
=
+
= =
=
+
=
+
= =
0
0
C A
B
L
B
N
C A
A
L
A
y
A
(y
A0
, N
0
) = (1.0

, 4.0)
Single stage calculations
Solution 1
Find coordinate at V
2
.
Coordinate for V
2


Mass of A = 0 A = 0 kg

Mass of B = 0 B = 0 kg

Mass of C = 100 kg C = 100 kg
0
1
0
0
0 0
0
2
2
2
2
=
+
=
+
= =
=
+
=
+
= =
00 0
10
C A
B
V
B
N
C A
A
V
A
x
(x
2
, N
2
) = (0

, 0)
Single stage calculations
Solution 1
From material balance calculations:
Total solution balance:

( )( ) ( )( ) ( )
167 . 0
120 0 100 0 . 1 20
2 2 0 0
=
= +
= +
AM
AM
AM A A
x
x
Mx x V y L
kg 120 100 20
1 1 2 0
= = +
= + = +
M M
M V L V L
Component A balance:

Single stage calculations
Solution 1
( )( ) ( ) 667 . 0 120 20 4
0 0
1 1 0 0
= =
=
= = =
M M
M
M
N N
M N L N
M N L N L N B


Solid balance:

Coordinate for M

(x
M
, N
M
) = (0.167

, 0.667)
Plot coordinate M in the graph.

Construct straight vertical line through point M in order to find value V
1
and
L
1

Single stage calculations
Solution 1
From figure,
0
0.5
1
1.5
2
2.5
3
3.5
4
0 0.2 0.4 0.6 0.8 1
x
A
, y
A
N
1
L
1
V
A
x N versus
A
y N versus
Coordinate for V
1


(x
1
, N
1
) = (0.167

, 0)
Coordinate for L
1


(y
1
, N
1
) = (0.167

, 1.5)
0
L
2
V
M
Single stage calculations
Solution 1
From material balance calculations:
Total solution balance:

( ) 1 Eq.

=
= +
= +
1 1
1 1
1 1
120
120
L V
V L
M V L
( )( ) ( )( ) kg 53.36

= =
=
= = =
1 1
1 1
1 1 0 0
120 667 . 0 5 . 1 L L
M N L N
M N L N L N B
M
M
Solid balance:

Single stage calculations
Solution 1
From material balance calculations:
From Eq. (1)

( )
kg
1 Eq.
64 . 66 36 . 53 120
120
1 1
1 1
= =
=
V V
L V



5 min break
Tutorial:
12.9-2-Textbook, page 835

A slurry of flakes soybeans weighing a total of
100kg contains 75kg of inert solids and 25kg
of solution with 10wt% oil and 90wt% solvent
hexane. This slurry contacted with 100kg of
pure hexane in a single stage so that the
value of N for the outlet underflow is 1.5kg
insoluble solid/kg solution retained. Determine
the amount and compositions of the overflow
V1 and the underflow L1 leaving the stage.
Answer:
Coordinate L
o
(0.1, 3.0)
Coordinate V
2
(0,0)
Coordinate M (0.02, 0.6)
Coordinate V1 (0.02,0)
Coordinate L1 (0.02,1.5)
L1= 50 kg
V1=75 kg
Solution balance;
L1 + V1 = M
V1= 125-L1
Solid balance;
N1.L1=B
1.5 (L1)=75
L1=50 kg
Therefore
V1=125-50
= 75kg
Example 12.9-1
In a single stage leaching of soybean oil from flaked
soybeans with hexane, 100 kg of soybean containing 22
wt% oil is leached with hexane. The solvent feed is 80 kg
of solvent containing 3 wt% of soybean oil. 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 V
1

and the underflow slurry L
1
leaving the stage.
Multi stage counter current Leaching
Process flow
Feed Slurry
L
0
,

N
0
, y
0
, B
Overflow solution
V
1
,

x
1

Underflow solution
L
N
,

N
N
, y
N
, B
V
N+1
,

x
N+1

Solvent Feed
V Mass of overflow solution x
A
Composition of A at overflow solution
L Mass of liquid in slurry solution y
A
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
( )
( )
( ) balance Solid
balance A Comp.
balance solution Total
M N L N L N B
Mx x V y L x V y L
M V L V L
M N N
AM A AN N AN N A
N N
= = =
= + = +
= + = +
+ +
+
0 0
1 1 1 1 0 0
1 1 0
Example 2
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 y
A
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
Information given:
Entering solvent (V
N+1
)


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

Feed Slurry
L
0
,

N
0
, y
0
, B
Overflow solution
V
1
,

x
1

Underflow solution
L
N
,

N
N
, y
N
, B
V
N+1
,

x
N+1
Solvent Feed
Feed slurry (L
0
):

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

Multi stage counter current Leaching
Solution 2
Information given:
Feed Slurry
L
0
,

N
0
, y
0
, B
Overflow solution
V
1
,

x
1

Underflow solution
L
N
,

N
N
, y
N
, B
V
N+1
,

x
N+1
Solvent Feed
Underflow solution (L
N
):

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

Multi stage counter current Leaching
Solution 2
Find coordinate at L
0
.
Coordinate for L
0


Mass of A = 800 kg/h

Mass of B = 2000 kg/h

Mass of C = 50 kg/h
35 . 2
850
2000
0 8
2000
94 . 0
850
800
0 8
800
0
0
0
0
= =
+
=
+
= =
= =
+
=
+
= =
5 00
5 00
C A
B
L
B
N
C A
A
L
A
y
A
(y
A0
, N
0
) = (0.94

, 2.35)
Multi stage counter current Leaching
Solution 2
Find coordinate at V
N+1
.
Coordinate for V
N+1

Mass of A = 20 kg/h

Mass of B = 0 kg/h

Mass of C = 1310 kg/h
0
1310 20
0
015 . 0
1330
20
1310 20
20
1
1
1
1
=
+
=
+
= =
= =
+
=
+
= =
+
+
+
+
C A
B
V
B
N
C A
A
V
A
x
N
N
N
N


(x
N+1
, N
N+1
) = (0.015

, 0)
Multi stage counter current Leaching
Solution 2
Find coordinate at L
N
.
Mass of A = 120 kg/h

Mass of B = 2000 kg/h

Mass of C = ?? kg/h
y . N
A
B
L
A
L
B
y
N
y
N
N
N
N
N
N
N
67 16 67 . 16
120
2000
= = = = =
graph, of Slope
Multi stage counter current Leaching
If x = 0.1, N = 16.67 x 0.1 = 1.67
Plot New Coordinate (x

, N) = (0.1

, 1.67)
Solution 2
Multi stage counter current Leaching
-7
-6
-5
-4
-3
-2
-1
0
1
2
3
-0.4 -0.2 0 0.2 0.4 0.6 0.8 1
x
A
, y
A
N
1 + N
V
0
L
N
L
Solution 2
From material balance calculations:
Total solution balance:

( )( ) ( )( ) ( )
376 . 0
2180 015 . 0 1330 94 . 0 850
1 1 0 0
=
= +
= +
+ +
AM
AM
AM N N A
x
x
Mx x V y L
kg 2180 1330 850
1 0
1 1 0
= = +
= +
= + = +
+
+
M M
M V L
M V L V L
N
N N
Component A balance:

Multi stage counter current Leaching
Solution 2
From material balance calculations:
Multi stage counter current Leaching
( )( ) ( ) 916 . 0 2180 850 35 . 2
0 0
0 0
= =
=
= = =
M M
M
M N N
N N
M N L N
M N L N L N B


Solid balance:

Coordinate for M

(x
M
, N
M
) = (0.376

, 0.916)
Plot coordinate M in the graph.

Construct line from point L
N
to point M until it cross at x axis. Point at x
axis = V
1

-7
-6
-5
-4
-3
-2
-1
0
1
2
3
-0.4 -0.2 0 0.2 0.4 0.6 0.8 1
x
A
, y
A
N
Multi stage counter current Leaching
1 + N
V
0
L
N
L
M
1
V
From figure,
Coordinate for V
1


(x
1
, N
1
) = (0.592

, 0)
Coordinate for L
N


(y
1
, N
1
) = (0.12

, 2.0)
Solution 2
From material balance calculations:
Total solution balance:

( ) 1 Eq. =
N
L V 2180
1
Multi stage counter current Leaching
( ) ( ) ( )( )
( )
( ) ( )( ) ( )( )
kg 997.62
above equation into 1 Eq. Insert

= =
= +
= +
= +
= +
N N
N N
N N
N
AM N N
L L
L L
L L
V L
Mx x V y L
88 . 470 472 . 0
68 . 819 592 . 0 56 . 1290 12 . 0
376 . 0 2180 592 . 0 2180 12 . 0
376 . 0 2180 592 . 0 12 . 0
1
1 1
Component A balance:

Solution 2
From material balance calculations:
Total solution balance:

( )
kg
1 Eq.
38 . 1182
62 . 997 2180
2180
1
1
1
=
=
=
V
V
L V
N
Multi stage counter current Leaching
Connect L
0
with V
1
& L
N
with V
N+1
. The cross line operating point.



Total stages: 4 stages
Construct operating point:
-7
-6
-5
-4
-3
-2
-1
0
1
2
3
-0.4 -0.2 0 0.2 0.4 0.6 0.8 1
x
A
, y
A
N
Solution 2
Multi stage counter current Leaching
1 + N
V
0
L
N
L
M
1
V
Construct the stages:
P A
1
L
2
L
3
L


5 min break.
Tutorial
12.10-4 Textbook, page 835
Fresh halibut livers containing 25.7 wt% oil
are to be extracted with pure ethyl ether to
remove 95 % of the oil in a countercurrent
multistage leaching process. The feed rate is
1000 kg of fresh livers per hour. The final exit
overflow solution is to contain 70 wt% oil. The
retention of solution by inert solids (oil free
liver) of the liver varies as follow, where N is
kg inert solid/kg solution retained and y
A
is kg
oil/kg solution
Tutorial
12.10-3 Textbook, page 835

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.
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.
* This means the solution in the liquid phase leaving a stage is the same as the
solution that remains with the solid matrix in the settled slurry leaving the stage.
Equilibrium Relations in Leaching
The settled solid leaving a stage always contains some liquid in which dissolved
solids is present.

The solid liquid stream is called underflow or slurry stream.
Consequently, the concentration of oil or solute in the liquid or overflow stream is
equal to the concentration of solute in the liquid solution accompanying the slurry
or underflow stream.

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 diagrams for leaching:
Equilibrium Relations in Leaching
The concentration of inert or insoluble solid B in the solution mixture or the
slurry mixture can be expressed in kg (lb
m
) units:
solution lb
solid lb
solution kg
solid kg
kg kg
kg
= =
+
=
C A
B
N
For overflow, N = 0

For underflow, N value depending on the solute concentration in the liquid.
Equilibrium Relations in Leaching
The composition of solute A in liquid will be expressed as wt fractions:
( )
|
|
.
|

\
|
=
+
=
=
+
=
liquid underflow
or slurry in liquid

solution kg
solute kg
kg kg
kg
liquid overflow
solution kg
solute kg
kg kg
kg
C A
A
y
C A
A
x
A
A
QUIZ 2
45 minutes

QUIZ 2 (45 minutes)

A continuous countercurrent multistage system is to be used
to leach oil from meal by benzene solvent. The process is to
treat 2000 kg/h of inert solid meal containing 800 kg oil and
also 50kg benzene. The inlet flow per hour of fresh solvent
mixture contains 1310 kg benzene and 20kg oil. The
leached solids are to contain 120 kg oil. If the value of N for
the outlet underflow is constant at 1.85kg solid/kg solution,
determine

a) The exit flows compositions (x
A1
, y
AN
, overflow V
1
and the
underflow L
N
leaving the stage.

b) Number of stages required