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Mass Transfer (ChE - 392)

4-Leaching (Solid-Liquid Extraction)

Saeed GUL, Dr.Techn, M.Sc. Engg.


Professor

Department of Chemical Engineering,


University of Engineering & Technology Peshawar, PAKISTAN
Introduction
Leaching is concerned with the extraction of a soluble
constituent from a solid by means of a solvent
The desired component diffuses into the solvent from its natural
solid form
Typical users include:
 the metals industry for removing mineral from ores
(acid solvents)
 the sugar industry for removing sugar from beets
(water is solvent)
 the oilseeds industry for removing oil from soybeans, etc.
(hexane or similar organic solvents)

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
General Principles
Generally, the process can be considered in three parts:
1. The change of phase of the solute as it dissolves in the
solvent
2. Solute diffusion through the solvent in the pores of the solid
to the outside of the particle
3. The transfer of the solute from the solution in contact with
the particles to the main bulk of the solution

Any one of these three processes may


be responsible for limiting the
extraction rate, though the first process
usually occurs so rapidly that it has a
negligible effect on the overall rate

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
General Principles
If the solute is uniformly dispersed in the solid:
The material near the surface will be dissolved first, leaving a
porous structure in the solid residue. The solvent will then have
to penetrate this outer layer before it can reach further solute,
and the process will become progressively more difficult and the
extraction rate will fall.
If the solute forms a very high proportion of the solid:
The porous structure may break down almost immediately to
give a fine deposit of insoluble residue, and access of solvent to
the solute will not be impeded.

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
General Principles

If the soluble material is distributed in small isolated pockets in a


material which is impermeable to the solvent:
Such as gold dispersed in rock, for example. In such cases the
material is crushed so that all the soluble material is exposed to
the solvent.
If the solid has a cellular structure:
The extraction rate will generally be comparatively low because
the cell walls provide an additional resistance

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Factors influencing the rate of extraction
There are four important factors to be considered:
1. Particle Size
I. Surface area
II. Should not very small to be difficult to separate
2. Solvent
I. Selective
II. Viscosity
3. Temperature
I. Solubility
II. Diffusion Coefficient
4. Agitation of the Fluid
I. Increases eddy diffusion
II. Prevent Sedimentation

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Mass Transfer in Leaching Operations
Mass transfer rates within the porous residue are difficult to
assess because it is impossible to define the shape of the
channels through which transfer must take place.
It is possible, however, to obtain an approximate indication of
the rate of transfer from the particles to the bulk of the liquid.
Using the concept of a thin film as providing the resistance to
transfer, the equation for mass transfer may be written as:

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Mass Transfer in Leaching Operations
For a batch process in which V, the total volume of solution, is
assumed to remain constant, then:

The time t taken for the concentration of the solution to rise from
its initial value c0 to a value c is found by integration, on the
assumption that both b and A remain constant.
Rearranging:

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Mass Transfer in Leaching Operations
If pure solvent is used initially, c0 = 0, and:

which shows that the solution approaches a saturated condition


exponentially.
In most cases the interfacial area will tend to increase during the
extraction and, when the soluble material forms a very high
proportion of the total solid, complete disintegration of the
particles may occur.
Although this results in an increase in the interfacial area, the
rate of extraction will probably be reduced because the free flow
of the solvent will be impeded and the effective value of b will
be increased.
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Example 10.1

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Example 10.1

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Equipment for Leaching
The selection of the equipment for an extraction process is
influenced by the factors which are responsible for limiting the
extraction rate.

Thus, if the diffusion of the solute through the porous structure


of the residual solids is the controlling factor, the material
should be of small size so that the distance the solute has to
travel is small.

On the other hand, if diffusion of the solute from the surface of


the particles to the bulk of the solution is the controlling factor,
a high degree of agitation of the fluid is required.

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Equipment for Leaching
Processes involved
Three distinct processes are usually involved in leaching
operations:
1. Dissolving the soluble constituent.
2. Separating the solution, so formed, from the insoluble solid
residue.
3. Washing the solid residue in order to free it of unwanted soluble
matter or to obtain as much of the soluble material as possible as
the product.
The type of equipment employed depends on the nature of the solid —
whether it is granular or cellular and whether it is coarse or fine.
The normal distinction between coarse and fine solids is that the
former have sufficiently large settling velocities for them to be readily
separable from the liquid, whereas the latter can be maintained in
suspension with the aid of only a small amount of agitation
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Equipment for Leaching
Extraction from cellular materials
With seeds such as soya beans, containing only about 15 per cent of oil,
solvent extraction is often used because mechanical methods are not
very efficient.
 Light petroleum
fractions are generally
used as solvents.
 Trichlorethylene has
been used where fire
risks are serious, and
acetone or ether where
the material is very wet

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Extraction from cellular materials

 The upper section is filled with the


charge of seeds which is sprayed
with fresh solvent via a distributor
 The solvent percolates through the
bed of solids and drains into the
lower compartment where,
together with any water extracted
from the seeds, it is continuously
boiled off by means of a steam coil
 The vapors are passed to an external condenser, and the mixed
liquid is passed to a separating box from which the solvent is
continuously fed back to the plant and the water is run to waste
 By this means a concentrated solution of the oil is produced by the
continued application of pure solvent to the seeds
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Extraction from cellular materials
Bollmann Extractor
 Continuous moving bed extractor
Series of perforated baskets
 widely used with seeds which do not
disintegrate on extraction
 A typical extractor moves at about 1
revolution per hour
 Each basket containing some 350 kg of
seeds.
 Generally, about equal masses of seeds
and solvent are used.
 The final solution, known as miscella,
contains about 25 per cent of oil by
mass
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Leaching of coarse solids

 In continuous unit in which


countercurrent flow is
obtained: Solid is introduced
near the bottom of a sloping
tank and is gradually moved
up by means of a rake.
 The solvent enters at the top
and flows in the opposite
direction to the solid, and
passes under a baffle before
finally being discharged over a
weir Tray classifier / the Dorr classifier

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Leaching of coarse solids

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Leaching of fine solids

Coarse solids may be leached by causing the


solvent to pass through a bed of the material,
fine solids offer too high a resistance to flow.
Particles of less than about 200-mesh (0.075
mm) may be maintained in suspension with only
a small amount of agitation, and as the total
surface area is large, an adequate extraction can
be effected in a reasonable time.
Because of the low settling velocity of the
particles and their large surface, the subsequent
separation and washing operations are more
difficult for fine materials than with coarse
solids.
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Leaching Operations

Figure 1: Single-stage leaching unit

Figure 2: Multistage cross-flow leaching unit

Figure 3: Multistage countercurrent leaching unit


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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Material Balance-Countercurrent Process

 The stages are numbered in the direction of flow of the solid.


 The light phase is the liquid that overflows from stage to stage in a
direction opposite to that of the flow of the solid, dissolving solute
as it moves from stage N to stage 1.
 The heavy phase is the solid flowing from stage 1 to stage N.
 Exhausted solids leave stage N, while concentrated solution
overflows leave from stage 1.
 For purposes of analysis, it is customary to assume that the solute
free solid is insoluble in the solvent so that the flow rate of this solid
is constant throughout the process unit
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Design and Predictive Equations

The solute /solvent equilibrium and process throughput determine the


cross-sectional area and the number of theoretical and /or actual
stages required to achieve the desired separation.
The equation for the operating line is obtained by writing a material
balance.
From Figure above

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Design and Predictive Equations

If the density and viscosity of the solution change considerably with


solute concentration, the solids from the lower stages might retain
more liquid than those in the higher stages. The slope of the operating
line then varies from stage to stage.
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Design and Predictive Equations

If, however, the mass of the solution retained by the solid is


independent of concentration, LN is constant, and the operating line
is straight. These two mentioned conditions describe variable and
constant overflow, respectively.
It is usually assumed that the inerts are constant from stage to stage
and insoluble in the solvent. Since no inerts are usually present in
the extract (overflow) solution and the solution retained by the
inerts is approximately constant, both the underflow LN and overflow
VN are constant, and the equation for the operating line approaches
a straight line.
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Design and Predictive Equations
Since the equilibrium line is also straight, the number of stages can be
shown to be (with reference to Fig. 12.12)

The above equation should not be used for the entire extraction
cascade if Lo differs from L1, L2, . . . , LN (i.e., the underflows vary
within the system). For this case, the compositions of all the streams
entering and leaving the first stage should first be calculated before
applying this equation to the remaining cascade.

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Single stage problems
EXAMPLE
Calculate the grams of water that need to be added to 40 g of sand
containing 9.1 g salt to obtain a 17 % salt solution. If the salt
solution is to be reduced to 15 %, calculate the amount of salt that
must be removed (“leached”) from the solution.
SOLUTION:
Set V to be the grams of water required. The describing equation is:

Let Z be equal to the final amount of salt in the sand–water–salt


solution. The describing equation is

The amount of salt removed is therefore 9.1 - 0.61 = 8.49 g.


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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Single stage problems
A sand–salt mixture containing 20.4% salt enters a solid–liquid
extraction at a rate of 2500 lb /h. Calculate the hourly rate of fresh
water that must be added for 99% of the salt to be “leached” from the
sand–salt mixture if the discharge salt–water solution contains 0.153
(mass) fraction salt.
SOLUTION:
Let W equal to the hourly rate of water. The describing equation from
a mass balance is

Also note that the feed consists of 510 lb salt and 1990 lb sand. On
discharge, the sand contains only 5.1 lb salt. The discharge water
solution consists of the 2820 lb water plus 504.9 lb salt.
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Number of Stages for Countercurrent
Washing by Graphical Methods

The separation of Soluble constituents from a solid by extraction


with a solvent may be considered to consist of two steps:
1. Contacting the solid with liquid phase and
2. Separation of the liquid phase from the solid

In actual operation it is impossible to completely separate the


liquid phase from the solid. Consequently, the streams resulting
from the 2nd step will consist of:
 A liquid phase stream (solution) which during normal operation
does not contain any solid. This stream will be called overflow
 A slurry consisting of the solid plus adhering solution

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Number of Stages for Countercurrent
Washing by Graphical Methods
It is convenient to use the concept of a stage in performing the
calculations. A stage consist of two steps:
Contacting solid with liquid and
Separation of the overflow from the underflow
In Solid-Liquid extraction , an ideal stage is defend as :
A stage in which the solution leaving in the overflow is of the same
composition as the solution retained by the solid in the underflow
For the purpose of calculations, the solid-liquid extraction system may
be considered to consist of three components:
1. The solute component (A)
2. The inert solid component (B)
3. The solvent component (S)

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Number of Stages for Countercurrent
Washing by Graphical Methods

 The calculations for leaching system may be based on the material


balance and the ideal stage concept.

 Both mathematical and graphical methods of solution may be used.

 The graphical solution possesses advantage in presenting a


generalized treatment of the more complex cases and in permitting
a better visualization of what is occurring in the process.

 Although it may be inconvenient to use if a large number of stages


are involved but typically in most of the cases the number of stages
used is not large

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Rectangular triangular Diagram
S 100 % S

0.8 1
Mole fraction of Component S, xs

0.6

0.4
0.2
0.4
0.2
0.8 0.6

B A
0.2 0.4 0.6 0.8 100 % A
100 % B
Mole fraction of Component A, xA
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Single Stage Extraction system
Overflow Product Solvent Feed
V1, y1 Single Stage V2, y2

Feed
Extraction System Underflow Product
L0, x0 L1, x1

Overall Material Balance


L0 + V2 = L1 + V1
The Material Balance for components A, B and S:
L0(xA)0 + V2(yA)2 = L1(xA)1 + V1(yA)1

L0(xB)0 + V2(yB)2 = L1(xB)1 + V1(yB)1

L0(xS)0 + V2(yS)2 = L1(xS)1 + V1(yS)1


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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Counter Current Multistage Extraction
System
V1 V2 V3 Vj Vj+1 Vn Vn+1

Stage Stage Stage Stage


L0 1 L1 2 L2 Lj -1 j Lj Ln-1 n Ln

Overall Material Balance


L0 + Vn+1 = Ln + V1
The Material Balance for components A, B and S:

L0(xA)0 + Vn+1(yA)n+1 = Ln(xA)n + V1(yA)1

L0(xB)0 + Vn+1(yB)n+1 = Ln(xB)n + V1(yB)1

L0(xS)0 + Vn+1(yS)n+1 = Ln(xS)n + V1(yS)1


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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
PROBLEM 10.5
Seeds, containing 20 per cent by mass of oil, are extracted in a counter
current plant and 90 per cent of the oil is recovered in a solution
containing 50 per cent by mass of oil. If the seeds are extracted with
fresh solvent and 1 kg of solution is removed in the underflow in
association with every 2 kg of insoluble matter, how many ideal stages
are required?
GIVEN:
Underflow feed: Underflow product:
Seeds contain 20% by mass 1 kg solution is associated with 2 kg of
of oil insoluble matter.

Overflow feed: Overflow product:


Fresh Solvent 90% of oil is recovered in solution containing
50% by mass of oil
REQUIRED:
Number of ideal stages=?

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow Line:
The initial step is to obtain the underflow lone for which we proceeds as follows
E-Intercept:
E-intercept=intercept of absissa and ordinate
𝑘𝑘
E=
𝑘𝑘 + 1
K term is used where underflow is constant and K is given by
𝑀𝑀𝑀𝑀𝑀𝑀𝑀𝑀 𝑜𝑜𝑜𝑜 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟𝑟 𝑖𝑖𝑖𝑖 𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢
𝐾𝐾 =
𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖𝑖 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠
1
𝐾𝐾 = = 0.5
2
0.5
𝐸𝐸 = = 0.33
0.5 + 1
E= 0.333
Note: The composition of the underflow is therefore represented on the graph by a
straight line parallel to the hypotenuse of the triangle with an intercept of 0.333 on
the main two axis.
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow feed composition:
Underflow feed contain solute and inert, so:
XAO = 0.2 XB0=0.8 XSO=0
This point is marked as X1 on graph i.e. X1 = 0.2
Overflow feed composition:
Since overflow feed is pure solvent, so:
YAn+1 = 0 YBn+1= 0 YSn+1= 1
This point is marked as Yn+1 on graph i.e. Yn+1=1
Overflow Product composition:
Overflow product contains solute and solvent and no inert, so:
YA1= 0.5 YB1=0 YS1=0.5
This point is marked as Y1 on the graph , i.e. Y1= (0.5,0.5)

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow Product composition:
2kg of inert relates to 1kg of solution so 1 kg of inert relates to 0.5 kg of solution.
Oil recovery is 90% in overflow showing that 10% is left which is being taken up with
the under flow product,
XAn=10%*XA0
XAn= 0.1*0.2 = 0.02
The mass fraction of inert is same in both underflow feed and product i.e. XBn = XBo
XBn=0.8
To find out point a:
Calculation on solvent free basis :
𝑋𝑋𝑋𝑋𝑋𝑋 0.02
a(A) = =
𝑋𝑋𝑋𝑋𝑋𝑋+𝑋𝑋𝑋𝑋𝑋𝑋 0.02+0.8

a(A) = 0.024
Difference Point:
The difference point is now find by drawing in the two lines connecting X1 with Y1
and point a with Yn+1
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Yn+1
Y5 1. Locate underflow line
Y4 (0.333,0.333) and join it through
Y3 line.
Y2 2. Locate points, X1, Y1, Yn+1 and a
and joint Y1 to X1 and point Yn+1
Y1 to ‘a’

0.333
3. Join Y1 to B and locate X2, join X2
Xn X5 and Z and extend the line to fine
X4
X3 Y2 and repeat the procedure.
X2
4. From graph, Xn lies in between
X5 and X6. so number of stages
a X1 0.333
are 5.

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Problem 10.11
Seeds containing 25 percent by mass of oil are extracted in a
countercurrent plant and 90 percent of the oil is to be recovered in a
solution containing 50 per cent of oil. It has been found that the
amount of solution removed in the underflow in association with
every kilogram of insoluble matter is given by:

k = 0.7 + 0.5ys + 3𝑦𝑦𝑦𝑦 2

where ys is the concentration of the overflow solution in terms of


mass fraction of solute. If the seeds are extracted with fresh solvent,
how many ideal stages are required?

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
GIVEN:

Underflow feed: Overflow product:


Seeds contain 25% by mass 90% of oil is recovered in solution containing
of oil 50% by mass of oil

Overflow feed: Underflow product:


Fresh Solvent solution removed in the underflow in association
with every kilogram of insoluble matter is given by:
k = 0.7 + 0.5ys + 3𝑦𝑦𝑦𝑦 2
REQUIRED:
Number of ideal stages=?

SOLUTION:
Basis = 100 kg underflow feed to 1st stage

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow Line
The first step is to obtain the underflow line, that is a plot of xs against xA. The
calculations are made as follows:
Ratio (kg/kg inert) Mass fraction
Ys K oil solvent underflow line oil solvent
K*ys K(1-ys) K+1 XA = K*ys/(K+1) Xs = K*(1-ys)/(K+1)
0 0.7 0 0.700 1.7 0 0.412
0.1 0.78 0.078 0.702 1.78 0.044 0.394
0.2 0.92 0.184 0.736 1.92 0.096 0.383
0.3 1.12 0.336 0.784 2.12 0.158 0.370
0.4 1.38 0.552 0.828 2.38 0.232 0.348
0.5 1.70 0.850 0.850 2.70 0.315 0.315
0.6 2.08 1.248 0.832 3.08 0.405 0.270
0.7 2.52 1.764 0.756 3.52 0.501 0.215
0.8 3.02 2.416 0.604 4.02 0.601 0.150
0.9 3.58 3.222 0.358 4.58 0.703 0.078
1 4.2 4.2 0 5.2 0.808 0

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow feed composition:
Underflow feed contain solute and inert, so:
XAO = 0.25 XB0=0.75 XSO=0
This point is marked as X1 on graph i.e. X1 = 0.25
Overflow feed composition:
Since overflow feed is pure solvent, so:
YAn+1 = 0 YBn+1= 0 YSn+1= 1
This point is marked as Yn+1 on graph i.e. Yn+1=1
Overflow Product composition:
Overflow product contains solute and solvent and no inert, so:
YA1= 0.5 YB1=0 YS1=0.5
This point is marked as Y1 on the graph , i.e. Y1= (0.5,0.5)

17 April 2019 42
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow Product composition:
Oil recovery is 90% in overflow showing that 10% is left which is being taken up with
the under flow product,
XAn=10%*XA0
XAn= 0.1*0.25 = 0.025
The mass fraction of inert is same in both underflow feed and product i.e. XBn = XBo
XBn=0.75
To find out point a:
Calculation on solvent free basis :
𝑋𝑋𝑋𝑋𝑋𝑋 0.025
a(A) = =
𝑋𝑋𝑋𝑋𝑋𝑋+𝑋𝑋𝑋𝑋𝑋𝑋 0.025+0.75

a(A) = 0.0322
Since there is no solvent so; a(s) = 0
Point “a” is therefore; a = ( 0.0322 , 0 )
Difference Point:
The difference point is now find by drawing in the two lines connecting X1 with Y1 and
point “a” with Yn+1
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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
1. Locate underflow points and
join it through line.

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Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Yn+1
Y6
Y5
1. Locate underflow points and
Y4
join it through line.
Y3

Y2
2. Locate points, X1, Y1, Yn+1 and a
and joint Y1 to X1 and point Yn+1
Y1
to ‘a’ and locate point Z.
X7
X6
X5
X4
X3
3. Join Y1 to B and locate X2, join X2
X2
and Z and extend the line to fine
Y2 and repeat the procedure.
4. From graph, Xn and X7 are
almost at same point so
X1
a number of stages are 7.

Z
17 April 2019 45
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Problem 10.12
Halibut oil is extracted from granulated halibut livers in a
countercurrent multibatch arrangement using ether as the solvent.
The solids charge contains 0.35 kg oil/kg of exhausted livers and it is
desired to obtain a 90 per cent oil recovery. How many theoretical
stages are required if 50 kg of ether are used/100 kg of untreated
solids. The entrainment data are:

17 April 2019 46
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
GIVEN:
Underflow feed:
The solid charge contains 0.35 kg oil per kg of exhausted livers
Overflow product:
90% of oil is recovered
Overflow feed:
Fresh Solvent

REQUIRED:
Number of theoretical stages=?

SOLUTION:
Basis = 100 kg unreacted solids

17 April 2019 47
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow Line
The first step is to obtain the underflow line, that is a plot of xs against xA. The
calculations are made as follows:
Entrainment Ratio (kg/kg inerts) Mass fraction
overflow conc.
kg soln/kg
Kg oil/kg soln
livers oil solvent underflow line oil solvent
ys K K*ys K(1-ys) K+1 XA= K*ys/(K+1) Xs=K*(1-ys)/(K+1)
0 0.28 0 0.28 1.28 0 0.219
0.1 0.34 0.034 0.306 1.34 0.025 0.228
0.2 0.4 0.080 0.32 1.4 0.057 0.229
0.3 0.47 0.141 0.329 1.47 0.096 0.224
0.4 0.55 0.220 0.33 1.55 0.142 0.213
0.5 0.66 0.330 0.33 1.66 0.199 0.199
0.6 0.8 0.480 0.32 1.8 0.267 0.178
0.67 0.96 0.643 0.3168 1.96 0.328 0.162

Plot the XA against XS so that we get the underflow line

17 April 2019 48
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow feed composition:
Solid charge= 0.35 kg / kg exhausted livers
Total feed = 0.35+1 = 1.35 kg
XAo = 0.35/1.35 = 0.26 XB0 = 1-0.26 = 0.74
XAO = 0.25 XB0=0.75 XSO=0
This point is marked as X1 on graph i.e. X1 = 0.26
Overflow feed composition:
Since overflow feed is pure solvent, so:
YAn+1 = 0 YBn+1= 0 YSn+1= 1
This point is marked as Yn+1 on graph i.e. Yn+1=1
Underflow Product composition:
Oil recovery is 90% in overflow showing that 10% is left which is being taken up with the
under flow product,
XAn=10%*XA0
XAn= 0.1*0.26 = 0.026
17 April 2019 49
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
The mass fraction of inert is same in both underflow feed and product i.e. XBn = XBo
XBn=0.74
To find out point a:
Calculation on solvent free basis :
𝑋𝑋𝑋𝑋𝑋𝑋 0.026
a(A) = 𝑋𝑋𝑋𝑋𝑋𝑋+𝑋𝑋𝑋𝑋𝑋𝑋= 0.026+0.74

a(A) = 0.034
Since there is no solvent so; a(s) = 0
Point “a” is therefore; a = ( 0, 0.034 )
To find Y1:
Since the recovery of oil is 90% so overall mass balance becomes:

17 April 2019 50
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
To find e:
To find “e” i.e. ether in underflow product
In the underflow product:
oil 2.6
the ratio i.e. exhausted livers = = 0.035 kg/kg
74
which, from the entrainment data, is equivalent to xA = 0.025, xs = 0.228

ether
The ratio exhausted livers = 0.306 kg/kg (through interpolation)

Or e = 0.306 × 74 = 22.6 kg

Overflow product composition:


The mass of ether = (50 − 22.6) = 27.4 kg

23.4
YA = = 0.46,
23.4+27.4
from which Ys = 0.54 which is marked in as Y1.
This point is marked as Y1 on the graph , i.e. Y1= ( 0.46 , 0.54 )
17 April 2019 51
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
1. Locate underflow points and
join it through line.

17 April 2019 52
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Yn+1

Y3
1. Locate underflow points and join
it through line.
Y2
2. Locate points, X1, Y1, Yn+1 and a
Y1
and joint Y1 to X1 and point Yn+1
to ‘a’ and locate point Z.

3. Join Y1 to B and locate X2, join X2


and Z and extend the line to fine
X4
X2
Y2 and repeat the procedure.
X3
4. From graph, Xn lies between X3
and X4 so number of stages are
a X1 3.

17 April 2019 53
Z Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Assignment / Do yourself
Oil is extracted from meal by means of benzene in a
continuous counter current extractor. The unit is to treat
1000 lb of meal based on completely exhausted solids per
hour. The untreated meal contains 400 lb of oil and no
benzene. The final product obtained from the operation is to
contain 60% oil and 90% of oil from the underflow is
recovered. Assume no carry over of inert in overflow. Test
data results that constant under flow solution is not possible.
Ys 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
K 0.5 0.505 0.515 0.53 0.55 0.571 0.595 0.62
17 April 2019 54
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Problem
It is desired to extract the oil from halibut liver by continuous counter
current multiple contact extraction with ethyl ether. The quality of solution
retained by granulated liver has been determined experimentally as a
function of composition of:

lb of oil/lb of soln 0 0.1 0.2 0.3 0.4 0.5 0.6 0.65 0.70 0.72
Lb of soln/lb of
extracted liver 0.205 0.242 0.286 0.339 0.405 0.489 0.600 0.676 0.765 0.810

The fresh halibut liver contains 25.7 mass % oil. If 95% of oil is to be extracted
and the final solution obtained from the operation is to contain 70 mass % oil.
Compute;
i. The lb of oil free ether per 1000 lb charge of fresh liver
ii. The no. of ideal stages required
iii. The no. actual stages required if overall efficiency is 70%
iv. The quantity of discharge solid.
17 April 2019 55
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
GIVEN:
Underflow feed: Overflow product:
Seeds contain 25.7% by The final product contains 70 mass % oil
mass of oil

Overflow feed: Underflow product:


Fresh Solvent 95% oil is recovered. So 5% is left in the
underflow product
REQUIRED:
i. The lb of oil free ether per 1000 lb charge of fresh livers = ?
ii. Number of ideal stages=?
iii. If Ƞ = 70%, number of actual stages = ?
iv. The quantity of discharged solids = ?
SOLUTION:
Basis = 1000 lb of fresh halibut livers as underflow feed to 1st stage
Part 1:
Lbs of free oil ether per 1000 lb charge of fresh livers = ?
First of all we find the underflow line and compositions, for which we proceed as
follows
17 April 2019 56
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow line
1st step is to draw underflow line i.e. XA vs Xs
From the given data of K and Ys, we find XA and Xs as follows.

oil/kg Lb soln/lb Ratio (kg/kg inerts) Mass fraction


soln inert oil solvent underflow line Oil solvent
ys K K*ys K(1-ys) K+1 XA= K*ys/(K+1) Xs=K*(1-ys)/(K+1)
0 0.205 0 0.2050 1.205 0 0.1701
0.1 0.242 0.0242 0.2178 1.242 0.0195 0.1754
0.2 0.286 0.0572 0.2288 1.286 0.0445 0.1779
0.3 0.339 0.1017 0.2373 1.339 0.0759 0.1772
0.4 0.405 0.1620 0.2430 1.405 0.1153 0.1729
0.5 0.489 0.2445 0.2445 1.489 0.1642 0.1642
0.6 0.600 0.3600 0.2400 1.600 0.2250 0.1500
0.65 0.676 0.4394 0.2366 1.676 0.2621 0.1412
0.7 0.765 0.5355 0.2295 1.765 0.3034 0.1300
0.72 0.810 0.5832 0.2268 1.810 0.3221 0.1253

17 April 2019 57
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow feed composition:
Underflow feed contain solute and inert, so:
XAO = 0.257 XB0=0.743 XSO=0
This point is marked as X1 on graph i.e. X1 = 0.257
Overflow feed composition:
Since overflow feed is pure solvent, so:
YAn+1 = 0 YBn+1= 0 YSn+1= 1
This point is marked as Yn+1 on graph i.e. Yn+1=1
Overflow Product composition:
Overflow product contains solute and solvent and no inert, so:
YA1= 0.57 YB1=0 YS1=0.3
This point is marked as Y1 on the graph , i.e. Y1= (0.7,0.3)

17 April 2019 58
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Underflow Product composition:
Oil recovery is 95% in overflow showing that 5% is left which is being taken up with
the under flow product,
XAn=5%*XA0
XAn= 0.05*0.257 = 0.01285
The mass fraction of inert is same in both underflow feed and product i.e. XBn = XBo
XBn=0.743
To find out point a:
Calculation on solvent free basis :
𝑋𝑋𝑋𝑋𝑋𝑋 0.01285
a(A) = =
𝑋𝑋𝑋𝑋𝑋𝑋+𝑋𝑋𝑋𝑋𝑋𝑋 0.01285+0.743

a(A) = 0.02
Since there is no solvent so; a(s) = 0
Point “a” is therefore; a = ( 0.02 , 0 )
Difference Point:
The difference point is now find by drawing in the two lines connecting X1 with Y1 and
point “a” with Yn+1
17 April 2019 59
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Yn+1 1. Locate underflow points and
join it through line.

2. Locate points, X1, Y1, Yn+1 and a


and joint Y1 to X1 and point Yn+1
to ‘a’ and locate point Z.

Y1

a X1

17 April 2019 60
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Yn+1 1. Locate underflow points and
join it through line.
Y5
2. Locate points, X1, Y1, Yn+1 and a
Y4 and joint Y1 to X1 and point Yn+1
to ‘a’ and locate point Z.
Y3
3. Join Y1 to B and locate X2, join X2
Y2 and Z and extend the line to fine
Y2 and repeat the procedure.
Y1
Xm 4. Join Yn+1 with X1 and Xn with Y1 so
that we get point Xm.
Xn X5 X4
X3
X2
5. From graph, Xn lies
a X1
between X5 and X6 so
number of stages are 5.
Z

17 April 2019 61
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Now by lever rule
Yn+1*(Yn+1*Xm) = X1* (X1*Xm)
Yn+1 X1∗Xm
X1 = Yn+1∗Xm
Where, Yn+1/X1 = lbs of oil free ether removed per 1000 lb of fresh liver
From graph; Yn+1.Xm = 10.4 X1.Xm = 2.7
Putting these values in equation
Yn+1 X1∗Xm
=
X1 Yn+1∗Xm
Yn+1 2.7
X1 = 10.4 = 0.259 lb
Here; X1 = 1000 lb
So; Yn+1 = 0.259 * X1
Yn+1 = 0.259*1000
Yn+1 = 259 lb
Thus the charge of ether per 1000 lb of fresh liver is 259 lbs
17 April 2019 62
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
Part 2:
From graph, it is seen that Xn lies between X5 and X6 so number of stages are 5.
Part 3:
No. of actual stages = ?
Ƞ = 0.7
Actual number of stages = 5/0.7 = 7.2
i.e. 8 number of stages are required
Part 4:
The quantity of discharge solids = ?
𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 𝑖𝑖𝑖𝑖 𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢 𝑓𝑓𝑓𝑓𝑓𝑓𝑓𝑓
Quantity of discharge solids = ∗ 𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡𝑡 𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑𝑑
𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠𝑠 𝑖𝑖𝑖𝑖 𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢𝑢 𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝𝑝
0.743
Quantity of discharge solids = ∗ 1000
0.82

Quantity of discharge solids =906.9 lb


17 April 2019 63
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
17 April 2019 64
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan
17 April 2019 65
Dr. Saeed GUL, Department of Chemical Engineering, UET Peshawar, Pakistan

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