Leaching 365

first filtrate is passed again through the filter ak

(polishing) before being discharged as misceu:· ; to r~m?ve finely divided solids
is quite similar to Rotocel extractor. · e pnnciple behind the operation

11.s.4.5 Recovery of oil

. .
The recovery of solvent from both the miscella and leached solids
. 1s an •
feature in these operations. Recovery of oil in misc 11 . essential
. I d .f e a is accomplished bY
evaporation of so vent an i necessary by further strippin •
·1 . . g m a tray column t0
remove the soIvent-free 01 . The 011 m solid is removed b .
· V fr Y steaming and
subsequent coohng. ent gas om condensers can be sent to an b b
· I h. •i a sor er and
scrubbed with petro eum w ite 01 and the resulting mixture can be sm·pped to
recover the solvent.

11.4 DEFINITIONS
Let, B = insoluble solid or inert solid (kg),
C = soluble solute (kg),
A = pure solvent (kg),

x =-C-; Weight fraction of solute in effluent solution (on B fre~ basis)

A+C

y= ~ ; Weight fraction of solute in the solid or slurry or sludge (on B

A+C
free basis)

N = _B_ ; (in each phase)

- A+C
The variation of N, x and y under different conditions are as follows:

(a) For a dry solid (free from solvent) N = B (": A= 0)

C
y = 1.0
(b) Solid free from solvent and solute N = oo (": A= 0; C = 0)
(c) Pure solvent x =0, N =0 (": B = O; C = 0)

11.5 DIFFERENT TYPES OF EQUILIBRIUM

DIAGRAMS
11.5.1 Type 1
A typical trend of N vs x, y and equilibrium relationship is shown in Fig. 11.11 (a)
characteristics of such systems are:
• Preferential adsorption of the solute occurs on solid.
• Solute is soluble in the solid B and distributes unequally between liquid and
solid phases at equilibrium.
• Insufficient contact time between solute and solvent.
• EF is a tie line.
 /'
Mass Transfer-Theory and Practice
366

-----i-- N VS y

N
~-----t--- N VS X

0 x,y 1.0

Fig. [Link](a) Type I equilibrium ..

11.5.2 Type II
A typical trend of N vs x, y and equilibrium relationship is shown in Fig. [Link](b).
The characteristics of such systems are:
• No adsorption of solute occurs.
• Solution withdrawn and the solution associated with the solid have the same
composition.
• Tie lines are vertical.
• The distribution coefficient is unity.
• Solids are drained to the same extent at all solute concentrations and such
a condition is known as constant underflow condition.
• No B is present in solution either dissolved or suspended.

Nvst F

,,---r-- N VS X
0 x, y E: 1.0
1.6r----~--.

QO X 1.6
Fig. [Link](b) Type II rquilibrium.

11.5.3 Type tn
A typical trend of N vs x, Y and equilibrium relationship is shown in Fig. [Link](c).
The characteristics of such systems are:
• Solute C has a limited solubility xs in solvent A and one can never have a
clear (leach) solution stronger than xs.
• T~e lines joining slurry and saturated solution converge as shown.
I
• Till the concentration of xs is re~ched, the solution retained in the solid and
 Leaching 367
tr at io n an d he nc e th e distribution
some concen n of solute occurs.
the clear solution have e lin e FE . N o ad so rp tio
up to the ti
coefficient is unity, i.e. th e sa m e so lu te co ncentration in
right of F E indica te
• The tie lines to th e lu te co nc en tr at io n in slurry as indicated by
cl ea r solu, tio
H .n but a different so
points G
w ill fa ll in an y on e of the above three
ss situations which
In practice we come acro
types.

1.0

I /1
I
1,0 I

0.0 1.0

I equilibrium.
Fig. 11 .l l( c) TYl)e II
 Leac hing -371

l\{ULTISTAGE COU NTE RCU RRE NT OPE RAT ION

11.8
. alance for the system as a whole gives,
soiuuon b
F + RN p +l = R1 + EN p = M
· the total mass of B (inert) free mixture.
where M is

Fig. 11.16 A typical multistage countercurrent operation.

Solute balance gives,

F. YF + RN p +l 'XN p +l. = R1X1 + EN p . YN p = M. YM

where,

YM =
F + RN p
+l

A solution balance for the first two stages gives

F + R2 = R 1 + E 1
1.e. F - R1 = E1 - R2 = !l.R.
Similarly a solution balance for the first two -stages yields
F - R 1 = E2 - R3 = !l.R.
It clearly indicates that the difference in flow betw een streams
at either ends in
each stage remains constant. '·
In a typical operation, the number ·of stages (for a given recovery and
a given
amount of solvent) or concentra,tion of solute in the leaving strea m
(for a given
number of stages and solvent used) or the amount of solvent (for a
given numb er
of stages and percentage recovery) will be needed.
Example 8.2: The senting cbaracteristics of a slurry consisting of CaC~ suspended in a solution c:
NaoH and watcr is given below w-bich indicate that the amount of the solution entrained with the soli:.s
,--ary ~ith solution concentration:
.x, w ei ght fraction NaOH in the [Link] O 0_02 0_04 0.06 0_08 Q_lO
Entrainment.. kg solution /kg CaC~ L496 1553 L640 1_760 L9ll 2_083

Assume that there is no preferential adsorption of NaOH on the sofui A slurry consisting of l CYi
'CaC03~ 5% NaOH and 8590 water is allowed to settle_ (a) Plot the practical equihoriwn curve o:.
inert to solute (weight of B/weight of C). If the solvent used is pure, no H and L 1s preseru auu u1~1 c-1 v 1 ~ ,
y = 0, N = 0. Consider, for example, 100 kg of a seed containing 25 weight% oil being leached with
225 kg of n-hexane. The unsettled slurry M consists of 75 kg inert insoluble cake (B) suspended in
250 kg oil-hexane solution (A+C) containing 25 kg oil (C) dissolved in it For this suspension, N and x are
.
given as
mass of B 75
N - - - - - - - - - 0 30
- mass of (A+C) - 250 - ·

mass of C 25
x=-----=-=0.10
mass of (A+ C) 250
~ A countercurr ent extraction battery is used t~~xtract c~u~ti~ soda adhering to the CaCO3 sludg;
from the reaction
Na 2 CO 3 + CaO + H 2 O ➔ CaCO3 + 2NaOH
The products leaving the reaction vessel contains 0.6 kg of water with every kg of CaCO3, but no
excess reactants are present. It is desired to recover 97 percent of the NaOH. The final overflow
contains 12% by weight NaOH. The underflow from each stage carries solution the weight of
which varies with the concentratio n as
Wt % NaOH in solution 0.0 5.0 10.0 15.0 20.0
N- 1, kg solution/ kg CaCO3 1.50 1.75 2.20 2.70 3.60

Determine for treating 100 kg/h of CaCO3:

(a) The solvent added, kg/h
(b) The quantity and ~omposition of the solution in the final underflow sludge
(c) The number of stages required.
(Answer: (a) 664 kg (b) 157 kg, 1.53% NaOH (c) 2.65)
- - - - - --
 ,- ---- .. -- ..
_, ~

~ Oil is extracted from halibut livers using pure ether as solvent in a countercurrent extraction
to recov er
~ [Link] charg e conta ining 25.0 weig ht% oil is to be extra cted with pure ethyl ether
98% of the oil. The feed is admi tted at a rate 1000 kg fresh livers per hour. The final overflow
solut ion
solution is to conta in 70 weig ht% oil. The unde rflow conc entra tion varie s with
concentration as given in the follow ing table :
x, kg oil/kg soluti~n 0 0.2 0.4 0.6 0.81
N, kg inert solid/ kg soluti on 4.88 3.50 2.47 1.67 1.39

Determine:
(a) The amou nt of solve nt requi red
rt) The amou nt of overf low solut ion
(i,) The quantity and comp ositio n of unde rflow sludg e
(d) The numb er of stage s
(Answer: (a) 260.7 kg (t/) 350 kg (c) 160.7 solut ion and 750 kg exhau sted meal:
0.5% oil, 17.1 % ether , 82.4% exhau sted liver) ~ 8)
1 r
 -- -.. ,1:;1 - \1\1.J
froIIl each washing stage contains two parts by weight of water
the number of stages required. per every part of gangue. Detennine
(Answer: 7.2 stages (Analytical M
A countercurrent extraction battery is used to extract caustic,soctacCabe),_7.8 (Ponchon-Savarit ))
s.31 froOl the reaction adhenng to the CaCO3 sludge
Na 2 CO 3 + CaO + H2O ➔ CaCO 3 + 2NaOH
A feed consisting of 2000 kg/h of Na2CO3 in water is admitted t th .
· vesse1 contain· s 10 kg of water 0
reactton esse1. The
products leaving the reaction with e e v
k
thfOUgh a series of three continuous countercurrent thickeners It is desvired
.ery thg of CaC03 is fed
· nl 1 N OH Th . .
contains o~ drying o y percent a . . e underflow from each stage carries at the final prod
3 Parts b uct
of water with every part of CaCO3. Detemune the rate at which water is admitted t Y~ass
or 1eaching.
S.3l One thousand and five hundred kg/h of dry sea-shore sand containing 1 percent(Answer: 18304 kg/h)
by f
is to be washed with 1500 kg/h of fresh water running countercurrently to the sand :;::s : salt
Classifiers in series. The sand dischar
.
ged from each classifier contains one part by ufg two
for every two of sand. Detemune: mass o water
(a) Toe percentage of salt in the final dried sand
(b) Water rate required in a single classifier in order to wash the sand to the same extent as
in (a).
. . . (Answ~r: (a) 0.247% (b) 3030.3 kg/h)
S.3J One thousand kg/h ofbanum sulphide (MW= 169.4) dissolved m 2500 kg/h water together with
stoichiometric quantities of sodium carbonate (MW= 106) are fed to a reaction vessel where the
following reaction occurs:
BaS + Na 2 CO 3 ➔ BaCO 3 + Na 2 S
Toe products of the reaction are washed with water in a three-stage countercurrent washing
system to free the barium carbonate (MW =197.4) of the adhering sodium sulphide (MW= 78).
Toe concentrated overflow solution is to contain 10% sodium sulphide. The underflow sludge
from all thickeners contains two parts water with every part of barium carbonate by mass.
Determine:
(a) Toe quantity and composition of the dried barium carbonate precipitate
(b) Toe rate at which water is to be supplied to the third thickener
(c) Toe percent recovery of sodium sulphide in the final extract
(Answer: (a) 1221.4 kg, 4.6% Na2S (b) 3482.1 kg (c) 88.12%)
Countercurrent leaching (Variable underflow)
8.34 Seeds containing 20 % by weight oil are extracted in a countercurrent plant and 95% of the oil is
to be recovered in a solution containing 50% of oil. It has been found that the amount of solution
removed in the underflow in association with every kg of insoluble matter is given by

N
+
..!.._ = 0.7 + 0.5y 3y 2
where y is mass fraction of solute in the overflow solution. If the seeds are extracted with fresh
solvent, how many ideal stages are required?
& · (Answer: 10.8 stages)
~ Oil is extracted from meal using benzene as solvent in a countercurrent extractio
n battery. Toe
hourly feed of oil-meal to the unit contains 500 kg oil, 1000 kg insoluble meal and 50 kg benzene.
The solvent is admitted at a rate 800 kg/hand contains 12 kg oil. The solids leaving the last stage
664 ■ Mass Transfer: Theory and Appli cation s
~~~ ~~~ ~~: :.:: .:.~ ~-- --= -_! _-- ---- ---- ---- ---- ---- ...._
as final underflow contain 75 kg/h unextracted oil. The mass of solution retained by the solidi
from a stage varies with the concentration of the solution as:
--- --- --- --- --- --- --- --- --- --- --. ... _
x, kg oil/kg solution 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
N- 1, kg solution/ kg solid 0.500 0.505 0.515 0.530 0.550 0.571 0.595 0.620
--....
Detennine: (a) The concentration of final overflow (b) Concentration of solution retained by the
exhausted meal (c) The mass of solution in the final underflow solids (d) The mass of overflow
(e) The number of stages required.
. . (Answer: (a) 0.521 (b) 0.148 (c} 511.3 kg (d) 838,7 kg (e) 2.7)
8.36 Oil 1s extracted from soyabean flakes containing 20% oil using hexane as solvent which is
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