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Chapter Five

Leaching
Dr. Mohammed H. Al-Saleh
Department of Chemical Engineering
Jordan University of Science and Technology

Introduction

L-S separation process involves preferential solvation of the


desired component/s (solute/s) from a mixture of different
components in a solid
Diffusion of solutes through the solid phase:

Slow
Complicate the separation process

Difficult to attain equilibrium

If water is used to leach undesired components from a solid


The process is called washing
Wide use in the food and biological industries

Leaching of sugar from sugar beets using hot water


Vegetable oils are leached using organic solvents such as hexane and
acetone.

In pharmaceutical industries, many products are obtained by


leaching plants roots, leaves and stems
In metal industries, Copper salts are extracted from ground ores
by sulfuric acid
Coffee/tea

Solid preparation for leaching


4

In leaching, solvent diffuses inside the solid material to the


active sites where solute is available and dissolution occurs,
thus the solid material should be ready for this mechanism
The method for preparing the solid depends on:

Percent of the solute/s to be leached


The distribution of the solute/s within the solid
The original particle size
The nature of the solid (e.g. material that is completely surrounded by
insoluble material, plant cell)

A
B

A
B

this would increase the rate of leaching where the solid portion
becomes more accessible to the solvent
Preparation techniques:
Crushing and grinding

Slices: like in sugar beet

Drying of roots/leaves/stems: which causes rupture the cell wall


(used in pharmaceutical industry)

Rolling and flaking: used for soybeans and vegetable seeds where
reducing the size to 0.1-0.5 mm cause cell walls rupture

Leaching Equipment
A Fixed Bed Leaching

B Moving Bed Leaching

Used in sugar industry

In such equipment, 95% of


sugar can be leached

Solvent: Hot water

Bed or stage moves instead of


being stationary
Used in extracting oil from
vegetable seeds, soybeans
Solvent: Usually petroleum
products, eg. hexane

C Agitated Solid Leaching

When solids can be ground to 0.074 mm

Why 0.074mm?

Equilibrium Relations
8

A : Solute
B: Solid
C: Solvent

Overflow, contains A and C

Underflow (Slurry),
contains A,C and B

In leaching we typically assume that there is no adsorption for


the solute by the solid.

Thus, Liquid (A,C) in the underflow is the same liquid in the overflow
(A,C), i.e. concentration of solute in the underflow liquid (yA) is the same
as that in the overflow (xA)

Equilibrium Diagram

Concentration of the solute in the overflow liquid:

xA =

Concentration of the solute in the underflow liquid:

yA =

kg A
kg A + kg C

kg A
kg A + kg C

Concentration of the solid (B) in the overflow and underflow

N=

kg solid
kg B
=
kg A + kg C kg solution

Ideal case: Solute A is infinitely soluble in the solvent C.


underflow

N vs. yA

xA=yA

overflow
0

N vs. xA
xA, yA
1

yA

0
10

xA

Non-Ideal Case: This case happens


when:

There is insufficient contact time


the solute will not be completely
dissolved
OR There is adsorption of the solute
on the solid

underflow

N vs. yA
N
overflow

N vs. xA
xA, yA

OR solute being soluble in solid

yA> xA

yA

0
11

xA

Single stage leaching


12

Overflow
V1, x1

Solvent
V2, x2

Slurry
L0, N0, y0, B

Underflow
L1, N1, y1, B

Total Balance:

Total flowrate of
A and C

L0 + V2 = L1 + V1 = M

Component A balance: L0 y A0 + V2 x A2 = L1 y A1 + V1 x A1 = MxAM


Component B balance: B = L0 N 0 + 0 = L1 N1 + 0 = MN M

L : Flowrate of (A+C) in the slurry/underflow


V: flowrate of the Overflow solution (A+C)
B: Flowrate of dry solute free solid

L1

L1MV1 : Should be on straight line (and most likely vertical)


LoMV2 : Should be on straight line

N
NM

V1
V2 xAM

L0

xA, yA

Example

In a single-stage leaching of soybean oil from flaked soybeans with


hexane, 100 kg of soybeans 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
13

Overflow

Slurry

Solvent

V2=100
xA2=0; xC2=1

Underflow

B=100*(1-0.2)= 80 kg
Lo=100*0.2 = 20 kg
yAo=(kgA)/(kgA+kgC)
= 20/(20+0) = 1

Lo

No=80/20 = 4

yAoLo+xA2V2= MxAM
(1)(20)+(0)(100)= 120xAM xAM=0.17

xA1=yA1=0.17
NoLo=N1L1L1=(4*20)/1.5 = 53.3 kg
14

L1+V1=M V1=120 -53.3=66.7 kg

Find M point:
Lo+V2=20+100=120 kg

N vs. yA

L1

2
1

V20

0.2

V1

0.4

0.6

0.8

xA, yA

N vs. xA

Countercurrent Multistage Leaching


15

Leaching solvent

Overflow
V1, x1

V2
1

y0, N0
L0, B

L1

Vn+1

V3 Vn
2

L1 Ln-1

VN-1
LN-2

VN

VN+1, xN+1
N

N1
LN-1

Ln

Feed solid

yN, NN
LN, B
Leached solid

V = Solvent (C) + Solute (A)


L (slurry) = Liquid phase (A and C)
B = amount of solid
Assumption: Solid B is insoluble and is not lost in the liquid
Overall balance for the first n stages:

Vn+1 + L0 = V1 + Ln

Component A balance for the first n stages:

Vn+1 xn+1 + L0 y0 = V1 x1 + Ln yn

If we plot the above operating line-equation on xy diagram, it


will passes through the terminal points (x1, yo) and (xN+1,yN)

Solve for xn+1

xn+1 =

1
Vx -L y
yn + 1 1 0 0
1 + (V1 - L0 ) / Ln
Ln + V1 - L0

If the viscosity and density of the solution change remarkably


with the solute concentration

Solid from the lower-numbered leaching stages may retain more


liquid solvent because A concentration decreases from stage 1 to N

Ln and the slope of operating line will vary from stage to stage
16

A Variable underflow (Case 1)


The approach is similar to liquid-liquid extraction with partially miscible liquids
Overall total solution balance (A+C):

VN +1 + L0 = V1 + LN = M

VN +1 x AN +1 + L0 y A0 = V1 x A1 + LN y AN = MxAM

Component A balance :

B = N0 L0 = N N LN = N M M

Total solid balance on B:

Terminal and M points

L0

L0 and VN+1 are usually known & yAN is set

LN

The coordinates of point M (xM,NM) can be calculated


L0 M VN+1 must lie on a straight line

V1 M LN must also lie on a straight line

NM

V 1 can be found

V1

VN+1 xAM
xA, yA

17

Stage to stage calculations

For stage 1:

V2 + L0 = V1 + L1

For stage n:

Vn+1 + Ln-1 = Vn + Ln

Rearrange for the difference D:


This holds for all stages:

L0 - V1 = Ln - Vn+1 = LN - VN +1 = = D

The coordinates for the point D can be determined by applying


component A balance and balance on solid B:
x AD =

L0 y A0 - V1 x A1
L0 - V1

B
B
=
D L0 - V1

ND =

18

L0 - V1 = L1 - V2 = D

LN y AN - VN +1 x AN +1
LN - VN +1

N 0 L0
L0 - V1

Operating point
D

Graphical determination of the point D:

1) Locate the terminal points


2) Draw the line L0V1
3) Draw the line LNVN+1
4) The intersection of the two lines is D

LN L
2 L1

Number of Stages

L0

1) Draw a tie line from V1 to locate L1


2) Draw the line L1D to locate V2

3) Draw A tie line from V2 gives L2


4) Continue until you reach the desired LN

According to the drawing on the right, 3 stages


are required for the separation

VN+1 V2 V1
xA, yA

D
19

Example
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 (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. Settling experiments similar to those in the
actual extractor show that the solution retained depends upon the
concentration of oil in the solution. The data 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

20

VN+1=1310+20= 1330 kg/h


V1 , x1

xAN+1=20/1330= 0.015

Overflow

Leaching solvent
Leached solid

Feed solid

y N , NN
LN, B

B= 2000 kg/h
Lo= 800+50=850 kg/h

yAo= 800/850= 0.94


No=2000/850 = 2.36
NN=kg B/LN

yAN=kg A/LN

NN/yAN=kg B/kg A = 2000/120 = 16.67

Go to the figure and plot a straight line from the yA=0 and N=0
with a slope of 16.67
21

Overall balance

Lo+VN+1= M= 850+1330 = 2180 kg/h

Component balance yAoLo+xN+1VN+1= xAMM


(0.941)(850)+(0.015)(1330) = xAM 2180
xAM = 0.38
Solid balance

B=NmM 2000=Nm 2140


Nm=0.92
LN+V1= M = 2140 kg/h
yANLN+xA1V1= xAMM
(0.12)LN+(0.6)V1 = (0.38)(2180)
LN= 1016 kg/h

22

V1= 1164 kg/h

LN
2

L4

Lo
L3

L2

V3 0.3

V2

L1

0
-0.5

-0.3

-0.1

VN+1

0.1
V4

0.5

0.7

V1

0.9

1.1

-1

-2

-3

-4

-5

-6

-7

Number of stages = 4

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B Constant underflow (Case 2)


In this case, Ln in the underflow solid is constant from stage to stage

The slope of the operating line:


Vx -L x
1
xn+1 =
yn + 1 1 0 0
1 + (V1 - L0 ) / Ln
Ln + V1 - L0
is also constant and on x,y line this corresponds to a
straight line

yA=xA
Also in many cases, equilibrium is given by yA
= xA; thus the two lines can be plotted
together and McCabe-Thiele method can be
used

x1

2
N

xN+1
24

yN

y0

The procedure for variable underflow can be used.

The N versus yA will be horizontal

LN

L0

VN+1

V1
xA, yA

25

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