Separation Process I

CDB2013

Dr. Lam Man Kee

Department of Chemical Engineering

1
Solid-liquid Extraction
(Leaching)
 Lesson outline

• Single stage leaching process

• Multiple stage leaching processes
 Lesson outcome
At the end of the session, the students are able to:
 Able to determine the exit stream amounts and compositions of
single stage and counter current multiple stage leaching processes.
 Able to estimate the number of theoretical trays needed to achieve
the desired leaching of solutes from solid feed.
 Recap of pervious lesson

• Working principles of solid-liquid processes

• Mode of leaching operations and equipment for leaching

• solid-liquid equilibrium
 Single Stage Equilibrium
• Similar to the previous single stage equilibrium separation processes
(example-liquid-liquid extraction), a single stage leaching process is
shown in the Figure below.
In this process, an overflow solution (solvent +
solute), V(kg/h) with composition xA and
underflow slurry, L (kg/h) with composition yA
based on a given flow rate B (kg/h) of dry,
solute free solid are considered.

The material balance equation are almost

identical to Eq. (5.2) and (5.3) for a single
stage liquid-liquid extraction.

A total solution balance (solute A and solvent

C), a component balance on A and a solid
balance on B, respectively are made as
presented below
 Solution mass balance:
L0  V2  L1  V1  M 6.8

Component balance on A:
L0 yA0  V2 x A2  L1yA1  V1x A1  MxAM
6.9
Component balance on B:
B  N0 L0  0  N1L1  0  NM M 6.10
yA  yC  1.0 and x A  x C  1.0 6.11
Where: M is the total flow rate in kg (A+ C)/h
xAM and NM are coordinates of this points M.
 • As shown in the Figure L0MV2 must
lie on straight line and L1MV1 must
also lie on a straight line

• The point M is the intersection point of

the two lines.

• If L0 entering is the fresh solid feed to

be leached with no solvent C present in
it, it will be located above the N versus
y line as presented in the Figure.
 Example 6.1
Soybean oil is leached from flaked soybean with hexane. 100 kg
soybean with 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.
Solution
Known:

V2 = 100kg, xA2 = 0, xC2 =1.0,

B+L0 = 100kg and

L0 = 0.2 (B+L0)

=0.2(100) = 20kg of A (solute)

B = 100(1-0.2)=80kg insoluble solid,

N0 = B/(A+C)

= 80/(20+0)

= 4 kg solid/kg solution,

yA0 = 1.0
• First calculate the amount of the mixture M
using balance Eqns:
L0 + V2 = L1 + V1 = M
20 + 100 = 120kg
• Using Component balance on A
L0yA0 + V2xA2 = L1yA1 + V1xA1 = MxAM
20(1)+100(0) = 120xAM
so, xAM= 0.167
Using Component balance on B
B = N0 L0 + 0 = N1L1 + 0 =NM M
4(20)+0 = NM 120
so, NM = 0.667
 L0
The vertical tie line is drawn
locating L1 and V1 in
equilibrium with each other.
Then N1 = 1.5, yA1,= 0.167, XA1
= 0.167. Substituting into a
material balance Eqs. (6.8) and
(6.10) and solving :
L1 L1 = 53.3kg and
1.5
V1 =66.7 kg

0.667 M (xAM, NM)

V2 V1

0.167
 Countercurrent multistage leaching
• A process flow diagram for multistage countercurrent leaching process is
similar to that of multistage countercurrent liquid-liquid extraction processes.
• The solvent (c)-solute (A) phase or V-phase is the liquid phase that over
flows counter currently from stage to stage to that of the solid (slurry) while
dissolving solutes from the solid as it moves along.

Process flow for countercurrent multistage

• The slurry phase (L) composed of

inert solid (B) and a liquid of A and C
is a continuous underflow from each
stage.
Note: the composition of the V-phase (liquid phase) is denoted by X;
 The composition of the L-phase (slurry phase) is denoted by y.

Process flow for countercurrent multistage

• It is assumed that B is insoluble and is not lost in the liquid V phase.

• The flow rate of the solids is constant throughout the cascade of stages.
• V is given in kg/h of overflow solution
• L is given in kg/h of underflow liquid retained by the solid in the underflow

Process flow for countercurrent multistage

• Making an overall total solution (solute A + solvent C) balance,

L0  VN 1  L N  V1  M 6.12
Where: M is the total mixture flow rate in kg (A+C)/h
• Next making component balance on A,
L0 yA0  VN 1x AN 1  LN yAN  V1x A1  MxAM
6.13
• Making a total solid balance on B,
B  N 0 L0  N N L N  0  N M M 6.14
• Where NM and xAM are the coordinates of point M as shown in the figure
below which is the operating diagram for the process.

• Similar to liquid-liquid process,

 L0MVN+1 must lie on a straight line
(input condition)
 V1MLN must also lie on the straight
line (exit condition)

• Usually the flows and compositions of

L0 and VN+1 are known and the desired
exit concentration yAN is set.

• The coordinates NM and xAM can be

calculated from Eqn. (6.12)-(6.14)
and mid point M plotted.
 • The point LN, M, and V1 must lie on one
line as shown in the Figure.

• In order to go stage by stage on the

figure so as to determine the flow rate,
compositions and number of stages
required for the desired leaching
process, we must drive the operating
point equation.

• Making a total balance on stage one

and then on stage n

L0  V2  L1  V1 6.15
L n -1  Vn 1  Ln  Vn

Process flow for countercurrent multistage

 • Rearranging Eq.(6.15) for the difference
flows Δ in kg/h

  L0  V1  L1  V2 6.16

• This value Δ is constant and also holds for

Eq.(6.16) rearranged and also for all stages:
  L0  V1  Ln  Vn 1  LN - VN 1  ... 6.17

• This can also be rewritten for the balance on

component A gives:
L0 yA0  V1x A1 L N y N - VN 1xN 1
xA   6.18
L0  V1 L N - VN 1
Where xA Δ is the x coordinate of the operating
point Δ.
 A balance made on solid gives:
B N 0 L0
N  
L0  V1 L N - V1 6.19
Where NΔ is the xAΔ coordinate of the
operating point Δ.
• This point Δ is shown graphically in the figure
as the intersection of lines L0V1 and LNVN+1.

• From Eq.(6.17) we can see that

 V1 is on a line between L0 and Δ,
 VN+1 is a line between LN and Δ , and
so on.
• To graphically determine the number of stages, we start at L0 and draw a line
L0 Δ to locate V1. A tie line through V1 locates L1. Line L1 Δ is drawn given V2. A
tie line gives L2. This is continued until the desired LN is reached. In the Figure
shown about 3.5 stages are required.
 Example 2
• A continuous countercurrent multistage system is to be used to leach oil
from meal by benzene solvent. The process is to treat 2000kg/h of inert
solid meal (B) containing 800kg oil (A) and also 50kg 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. Setting
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/kg solution:

Calculate the amount and composition of the streams leaving the

process and the number of stages required.
Solution • The underflow data from the table
are plotted as shown in the figure
as N versus yA.

• For the inlet condition, in the

untreated solid,
Process flow for countercurrent multistage

L0 = A+C
=800+50
=850kg/h,
yA0= A/(A+C)
=800/(800+50)
=0.941,
B=2000kg/h,
N0=B/(A+C)
=2000/(800+50)
=2.36
 • For the inlet leaching solvent,
VN+1=(C+A)
=1310+20
L0 =1330kg/h a
xAN+1=A/(C+A)
=20/1330
=0.015.

VN+1 • The point VN+1 and L0 are plotted.

• The point LN lies on the N-versus-yA

line in the Figure.
• Also for this point, the ratio
NN/yAN= (kg solid/kg solution)/(kg
oil/kg solution)
=kg solid/kg oil
=2000/120
=16.67.
 LN • Hence, a dashed line through the origin
L0
at
 yA=0 and N=0 is plotted with a
slope of 16.67 and intersects the N-
versus-yA line at LN.
VN+1 • the coordinates of LN at this intersection
are
 NN =1.95kg solid/kg solution and
 yAN=0.118 kg oil/kg solution

• Making an overall balance by substituting

into Eq.(6.12) to determine point M,
L0  VN 1  850  1330  2180 kg/h  M
• substituting into Eq.(6.13) and solving
L 0 y A0  VN 1x AN 1  M xAM
850(0.941)  1330(0.015)  2180x AM
 x AM  0.376
 • substituting into Eq.(6.14) and
LN L0
solving
B  2000  N M M  N M (2180)
M N M  0.918
VN+1 v1 • The point M is plotted with the
coordinate xAM=0.376 and NM=0.918
in the Figure.
• The line VN+1ML0 is drawn, as is line
LNM, which intersects the abscissa at
point V1 where xA1 = 0.600

• The amount of streams V1 and LN are calculated

by substituting into Eq.(6.12) and (6.13), and
solving simultaneously
L0  VN 1  M  2180

L N y AN  V1x1  MLN
L N (0.118)  V1 (0.600)  2180(0.376)
 LN L4 L L L0 • Hence, LN=1016 kg solution/h in the
3 2 L1 outlet underflow stream and
V1=1164 kg solution/h in the exit
M overflow stream.
VvN+1
4 v3 v2 v1 • Alternatively, the amounts could
have been calculated using the lever
arm rule.

• The operating point Δ is obtained as the

intersection of lines L0V1 and LNVN+1 in the figure.
• Its coordinates can also be calculated from
Eq.(6.18)and (6.19).
• The stages are stepped off as shown.
• The fourth stage L4 is slightly past the desired LN.
Δ  Hence, about 3.9 stages are required.