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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

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 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


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.

Introduction to Leaching Process


Leaching process for inorganic and organic materials
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.

Principles of Leaching
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.

Calculation in Leaching

SINGLE STAGE LEACHING

COUNTER CURRENT MULTISTAGE LEACHING

Single stage Leaching


Process flow
Overflow solution
V1, x1
Feed Slurry
L0, N0, y0, B

V
L
B
N

Solvent Feed
V2, x2
Underflow solution
L1, N1, y1, B

Mass of overflow solution


xA
Composition of A at overflow solution
Mass of liquid in slurry solution yA
Composition of A at slurry solution
Mass of dry, solute free solid.
Mass of dry,solute (B)/Mass of solution retained (L)

Material balance is divided into 3 parts:

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

Single stage calculations


Example 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, x1
Feed Slurry
L0, N0, y0, B

Solvent Feed
V2, x2
Underflow solution
L1, N1, y1, 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 MxAM

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
L0

4
3.5
3

2.5
2

N versus y A

L1

1.5
1

0.5

N versus x A

V1

0
0

V2

0.2

0.4

0.6
x A, y A

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

Coordinate for L1

(y1 , N1) = (0.167 , 1.5)

0.8

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

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 Lo (0.1, 3.0)
Coordinate V2 (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 V1
and the underflow slurry L1 leaving the stage.

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


L0 VN 1 LN V1 M

Totalsolution balance

L0 y A0 VN 1 x AN 1 LN y AN V1 x A1 MxAM
B N 0 L0 N N LN N M M

Comp. A balance

Solid balance

Multi stage counter current Leaching


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 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
xN 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 x = 0.1, N = 16.67 x 0.1 = 1.67


Plot New Coordinate (x , 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 MxAM

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 MxAM

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

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 yA 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.

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.
* 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.
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.

Equilibrium Relations in Leaching


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:
The concentration of inert or insoluble solid B in the solution mixture or the
slurry mixture can be expressed in kg (lbm) units:
N

kg B
kg solid
lb solid

kg A kg C kg solution lb solution

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:
xA

kg A
kg solute
overflow liquid

kg A kg C kg solution

yA

kg A
kg solute

kg A kg C kg solution

liquid in slurryor

underflow
liquid

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 (xA1, yAN, overflow V1 and the
underflow LN leaving the stage.
b) Number of stages required