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CHE 303: Mass Transfer I

Washing and Leaching


Dr. Md. Iqbal Hossain
Associate Professor
Department of Chemical Engineering, BUET
iqbalhossain@che.buet.ac.bd and +8801927885215

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Chapter Objective:
1. Explain what washing is and apply the
McCabe Thiele and Kremser procedures to
washing problems

2. Explain what leaching is and apply both


McCabe-Thiele and Kremser methods to
leaching problems

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Washing:
 When solid particles are being processed in liquid slurries, the
solids entrain liquid with them. The removal of any solute
contained in this entrained liquid is called washing.

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Washing: Features
 To be specific, consider an operation that mines sand from the ocean. The wet
sand contains salt, and this salt can be removed by washing with pure water.
The entrained liquid is called underflow liquid, because the solids are normally
removed from the bottom of a settler.
 Washing is done by mixing solid (sand) and wash liquor (water) together in a
mixer and sending the mixture to a settler or a thickener
 The solids and entrained underflow liquid exit from the bottom of the settler,
and clear overflow liquid without solids is removed from the top.
 In washing, the solute (salt) is not held up or attached to the inert solid
(sand). The salt is assumed to be at the same concentration in the underflow
liquid as it is in the overflow liquid. Thus, it can be removed by displacing it
with clear water.
 The separation can be done in single-stage, cross-flow, and countercurrent
cascades.
 A variety of different equipment have been developed for washing and
leaching, which use essentially the same equipment

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Washing: Equilibrium
The equilibrium condition for a washer is that solute concentration is
the same in both the underflow and overflow liquid streams. This
statement does not say anything about the solid, which changes the
relative underflow and overflow flow rates but does not affect
concentrations. Thus, the equilibrium equation is-

where y = mass fraction solute in the overflow liquid and x = mass


fraction solute in the underflow liquid.

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Finally the kg/h of underflow liquid

If the solids rate, ε, ρf, and ρs are all constant, then Uj = U =


constant. If U is constant, then an overall mass balance shows that
the overflow rate, Oj, must also be constant. Thus, to have constant
flow rates we assume:
1. No solids in the overflow and solids do not dissolve. This ensures
that the solids flow rate will be constant.
2. ρf and ρs are constant. Constant ρf implies that the solute has little
effect on fluid density or that the solution is dilute.
3. Porosity ε is constant. Thus, the volume of liquid entrained from
stage to stage is constant.

An alternative way of stating the problem would be to specify the volume of


wet solids processed per hour. Then the underflow volume is

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McCabe-Thiele diagram for washing

(xo,y1)

(xN,yN+1)

The Kremser equation can also be applied to countercurrent washing


with no additional assumptions. 7
Example 14-1. Washing
In the production of sodium hydroxide by the lime soda process, a
slurry of calcium carbonate particles in a dilute sodium hydroxide
solution results. A four-stage countercurrent washing system is used.
The underflow entrains approximately 3 kg liquid/kg dry calcium
carbonate solids. The inlet water is pure water. If 8 kg wash water/kg
dry calcium carbonate solids is used, predict the recovery of NaOH in
the wash liquor.
Sol#
Recovery is defined as 1 – xout/xin
Thus, recovery can be determined even though xin is unknown

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Leaching: Features
 Leaching, or solid-liquid extraction, is a process in which a soluble solute is
removed from a solid matrix using a solvent to dissolve the solute.

 The most familiar examples are making coffee from ground coffee beans and
tea from tea leaves. The complex mixture of chemicals that give coffee and tea
their odor, taste, and physiological effects are leached from the solids by the hot
water.

 An espresso machine just does the leaching faster into a smaller volume of
water. Instant coffee and tea can be made by leaching ground coffee beans or
tea leaves with hot water and then drying the liquid to produce a solid.

 There are many other commercial applications of leaching such as leaching


soybeans to recover soybean oil (a source of biodiesel), leaching ores to recover
a variety of minerals, and leaching plant leaves to extract a variety of
pharmaceuticals (Rickles, 1965; Schwartzberg, 1980, 1987).

 The equipment and operation of washing and leaching systems are often very
similar. In both cases a solid and a liquid must be contacted, allowed to
equilibrate, and then separated from each other. Thus, the mixer-settler type of
equipment shown earlier is also commonly used for leaching easy-to-handle
solids.
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How Leaching differs from Washing-

 In leaching, the solute is initially part of the solid and dissolves


into the liquid. In washing, which can be considered as a special
case of leaching, the solute is initially retained in the pores of the
solid and the solid itself does not dissolve.

 In leaching, the equilibrium equation is usually not y = x, and the


total solids flow rate is usually not constant. Since diffusion rates in
a solid are low, mass transfer rates are low. Thus, equilibrium may
take days for large pieces such as pickles, where it is desirable to
leach out excess salt, or even years for in-situ leaching of copper
ores (Lydersen, 1983).

 A rigorous analysis of leaching requires that the changing solid and


liquid flow rates be included. This situation is very similar to partially
miscible extraction. In this section we will look at simple cases
where a modified McCabe-Thiele or Kremser equation can be used.

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A countercurrent cascade for leaching is shown in Figure below. We will
consider the (idealized) case where entrainment of liquid with the solid
underflow can be ignored.

The assumptions are:


1. The system is isothermal.
2. The system is isobaric.
3. No solvent dissolves into solid.
4. No solvent entrained with the solid.
5. There is an insoluble solid backbone or matrix.
6. The heat of mixing of solute in solvent is negligible.
7. The stages are equilibrium stages.
8. No solid is carried with the overflow liquid.

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Countercurrent leaching; (A) cascade, (B) McCabe-Thiele diagram

The equilibrium curve is now the equilibrium of the solute between the solvent
and solid phases. The equilibrium data must be measured experimentally. If the
equilibrium line is straight, the Kremser equation can be applied.
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In the previous analysis, assumptions 4 and 7 are often
faulty.

 There is always entrainment of liquid in the underflow (for the


same reason that there is an underflow liquid in washing).
 Since diffusion in solids is very slow, equilibrium is seldom
attained in real processes.

The combined effects of entrainment and nonequilibrium stages are


often included by determining an “effective equilibrium
constant.” This effective equilibrium depends on flow conditions
and residence times and is valid only for the conditions at which it
was measured. Thus, the effective equilibrium constant is not a
fundamental quantity. However, it is easy to measure and use. The
McCabe-Thiele diagram will look the same as Figure 14-3B.

Further simplification is obtained by assuming that the effective


equilibrium is linear, y = mEx.

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Problem D2.You are working on a new glass factory near the ocean.
The sand is to be mined wet from the beach. However, the wet sand
carries with it seawater entrained between the sand grains. Several
studies have shown that 40% by volume seawater is consistently
carried with the sand. The seawater is 0.035 wt frac salt, which must
be removed by a washing process.

Densities: Water, 1.0 g/cm3 (assume constant); Dry sand, 1.8 g/cm3
(including air in voids); Dry sand without air, 1.8/0.6 = 3.0 g/cm 3.

a. We desire a final wet sand product in which the entrained water


has 0.002 wt frac salt. For each 1000 cm3 of wet sand fed we will
use 0.5 kg of pure wash water. In a countercurrent washing
process, how many stages are required? What is the outlet
concentration of the wash water?

b. In a cross-flow process we wish to use seven stages with 0.2 kg of


pure wash water added to each stage for each 1000 cm3 of wet sand
fed. What is the outlet concentration of the water entrained with the
sand?

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Sol#

XN=0.002
yN+1=0

Xo=0.035

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Problem D7. In the leaching of sugar from sugar cane, water is used
as the solvent. Typically about 11 stages are used in a countercurrent
Rotocel or other leaching system. On a volumetric basis liquid flow
rate/solid flow rate = 0.95. The effective equilibrium constant is
mE=1.18, where mE = (concentration,g/liter, in liquid)/(concentration,
g/liter, in solid) (Schwartzberg, 1980). If pure water is used as the
inlet solvent, predict the recovery of sugar in the solvent.

Sol#

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Problem D10. A countercurrent leaching system is recovering oil
from soybeans. The system has five stages. On a volumetric basis,
liquid flow rate/solids flow rate = 1.36. 97.5% of the oil entering with
the nonsoluble solids is recovered with the solvent. Solvent used is
pure. Determine the effective equlibrium constant, mE, where mE is
(kg/m3 of solute in solvent)/(kg/m3 of solute in solid) and is given by
the equation y = mEx.

Sol#

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Problem D3.We wish to wash an alumina solids to remove NaOH from
the entrained liquid. The underflow from the settler tank is 20 vol %
solid and 80 vol % liquid. The two solid feeds to the system are also 20
vol % solids. In one of these feeds, NaOH concentration in the liquid is 5
wt %. This feed’s solid flow rate (on a dry basis) is 1000 kg/hr. The
second feed has a NaOH concentration in the liquid of 2 wt %, and its
solids flow rate (on a dry basis) is 2000 kg/h. We desire the final NaOH
concentration in the underflow liquid to be 0.6 wt % (0.006 wt frac)
NaOH. A countercurrent operation is used. The inlet washing water is
pure and flows at 4000 kg/h. Find the optimum feed location for the
intermediate feed and the number of equilibrium stages required.
Data: ρw = 1.0 kg/liter (constant), ρalumina = 2.5 kg/liter (dry crushed)
Sol#

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XN=0.006
yN+1=0

Xo=0.035

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