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EXTRACTIONS

Solid liquid extractions – Leaching Process (SLE)


Learning Outcomes

Explain principles of SLE systems

Analyse mass transfer in leaching (SLE)

Use equilibrium and operating line data to calculate stages

Describe and explain multi stage extraction process

Describe continuous and batch systems

Describe and classify SL extraction equipment


Solid-Liquid Extraction – Definition
 to extract desired solute constituent
or remove an undesirable solute
component form the solid matrix
using liquid
 solid is contacted with liquid phase
for mass transfer to occur
 referred as solid liquid extraction or
leaching
 In leaching when an undesirable
component is removed from a solid
with water, the process is called
washing
 Example : Making Tea/Coffee,
Gaharu extraction, Ginger extraction
Principles of SLE
 Leaching can be batch, semibatch, or continuous.
 usually operates at an elevated temperature to
increase the solubility of the solute in the solvent.
 Calculations involve three component (solid matrix,
solvent, solute) systems.
 Flow through a leaching system may be crosscurrent
or countercurrent.
Principles of SLE
 Solid Feed consist of insoluble carrier material and a desirable
soluble compound.
 Prior to SLE extraction, solid feed is prepared by grinding or
chopping. It is then mixed with a liquid solvent.
 The desired material or solute dissolves (to some extent) and so
leaves when the liquid is drawn off as overflow.
 The solids are removed as underflow. The underflow is wet, and
so some of the solvent/solute mixture is carried out here as well.
Rates of Leaching
5 Stages in leaching
1. solvent transfer to surface of solid from bulk solvent
2. Solvent diffuse or penetrate into solid
3. Solute dissolves in solvent
4. Solute diffuse through solid solvent mixture to surface or particle
5. Solute is transferred to bulk solution

 Rate of transfer of solvent from bulk to solid surface –rapid


 Rate of transfer of solvent into solid – maybe rapid or slow
 Rate of diffusion of solute through solid and solvent to surface solid
is often the controlling resistance in leaching process
 Resistance to mass transfer of solute from solid surface to bulk
solvent is quite small compared to resistance to diffusion within solid
Rates of Leaching
Rate of mass transfer from solid surface to liquid is controlling factor
 Rate of mass transfer of solute A being dissolved to solution of volume V m3 is
NA NA= kg mole of A dissolving
k L (c AS  c A )
A in solution
 By material balance, rate of accumulation of A in solution is

integrating from t=0; cA = cAo to t=t ; cA = cA;


c AS  c A

 Solution approach a saturated condition exponentially.  e ( K L A / V ) t


c AS  c Ao

 CA = concentration of A in solution at time t sec, kgmol/m3


 CAS = saturation solubility of solid solute A in solution, kgmol/m3
 A = surface area of particles, m2
 kL = mass transfer coefficient, m/s
Rates of Leaching
 kL , mass transfer coefficient can be calculated
 Small particles <0.6 mm (600 µm) - in agitated system

 Larger particles >2.5 mm


 – independent on size

DAB = diffusivity of solute A in solution, m2/s


Dp = diameter of solid particle or bubble, m
µ = viscosity of solution, kg/m.s
g = 9.80665 m/s2
∆ = positive difference between density particle (bubble) and solution, kg/m3
NSc = Schmidt number =
Rates of Leaching

Unsteady state diffusion in


solid is controlling
resistance in leaching
 If average diffusivity DAeff of

solute A approximately
constant, use unsteady state
mass transfer equation
 for
diffusion in x direction
 If particle approximately
spherical, use figure (p. 377,
Fig. 5.3-13, Geankoplis)
Equilibrium Relations in Leaching
 Leaching system consists of the solid mixture to be separated consists
of particles inert insoluble carrier B, solute A and solvent C.
 C, solvent is added to the mixture to selectively dissolve A.
 The overflow from the stage is free of solids and consists of only
solvent C and dissolved A.
 The underflow consists of slurry of liquid of similar composition in the
liquid overflow and solid carrier B.
 In an ideal leaching equilibrium stage, all the solute is dissolved by
the solvent; none of the carrier is dissolved.
 The mass ratio of the solid to liquid in the underflow is dependent on
the type of equipment used and properties of the two phases.
Equilibrium Diagrams
 Diagram for A-solute, B-leached solid, C-solvent
 Two phases : overflow and underflow
 Concentration of inert solid B in solution mixture or slurry mixture is
kgB kg solid
N 
kgA  kgC kg solution

 N=0 for overflow, N = changing for underflow (depend on solute


concentration in liquid)
 Composition of A in liquid kgA kg solute
xA    overflow liquid
kgA  kgC kg solution
xA =weight fraction solute A in overflow liquid
yA=weight fraction of A on a solid-B-free basis
in liquid associated with slurry or underflow kgA kg solute
yA    liquid slurry (underflow)
kgA  kgC kg solution
•Entering solid feed to be leached, N is kg inert
solid/kg solute A and yA =1
•Pure entering solvent, N=0, xA =0
Case 1: 12.9.1a
• Typical equilibrium diagram
• Solute A is infinitely soluble in
solvent C
• Eg. soybean oil (A)-soybean inert
solid meal (B)-hexane solvent (C)
• N vs yA = separated solids under
experimental conditions
• N vs xA = overflow liquid
composition where all solid has
been removed
• Tie line vertical
• x=y on 45o line when draw on y-x
diagram
Case 2: 12.9.1b
Case: 3 • Tie line not vertical due to
• If underflow line N vs y is straight and insufficient contact time
horizontal, amount of liquid associated with solid • Not all solute dissolved (adsorption
in slurry is constant for all concentrations of solute A on solid or solute
• Underflow liquid rate is constant soluble in solid B)
• Hence overflow also constant throughout stages
Single Stage Leaching
 V = kg/h overflow solution with composition xA
 L = kg/h of liquid in slurry solution with composition yA based on flowrate B kg/h of
dry solute-free solid
V1, x1 V2, x2
B, LO Leaching B, L1
No, yo N1, y1

M = total flow rate kg A +C /hr


xAM , Nm = coordinates of M
• A balance of C is not required as xA+xc =1; yA + yc =1
•L1 MV1 must lie on straight line
•Lo MV2 must lie on straight line
•L1 and V1 must lie on vertical tie line
•M is intersection of the above two lines
•If Lo enters as fresh solid feed to be leached with no solvent C, then it will be located above
N vs y line
Single Stage Leaching

V + L = M ( total mass kg)


Lo + V2 = L1 + V1 = M (general) --- [1]

For component A
LoyAO + V2xA2 = L1yA1 + V1xA1 = MxAM ---- [2]

For component B (Solid)


B = NoLO + 0 = N1L1 + 0 =NMM ---- [3]
Single Stage SLE - Example 12.9.1 (Geankoplis)
In a single stage leaching of soybean oil from flaked soybean A – Solute; B – Solid carrier
with hexane, 100 kg of soybeans containing 20 wt% oil is C- Solvent
leached with 100 kg of fresh solvent. The value of N for the
slurry underflow is essentially constant at 1.5 kg insoluble V1= ? kg V2 = 100 kg
xA1 = ? xA2 = 0
solid/kg solution retained. Calculate the amounts and xC1 = ? xC2 = 1.0
1
compositions of the overflow V1 and the underflow slurry L1
leaving the stage Lo= 20 kg L1 = ? kg
Solution : yAo = 1 yA1 =?
yCo = 0 N1
xA2=0, V2 = 100 kg, N is constant=1.5 kg insoluble solid/kg B = 100 (1-0.2)=80 kg
solution, yAo=1, B = 100 (1-0.2) =80 kg insoluble solid, Lo = No
100 (1-0.8)= 20 kg A. No=80/20= 4.0 kg solid/kg solution
1. Calculate M kgB kg solid
Plot M, V2 and Lo N 
2. kgA  kgC kg solution
3. Tie line  Locate L1, V1
4. Get N1, YA1, XA1 substitute into equation balance and
solve. Or use lever arm rule
B = inert insoluble solid carrier

kgA kg solute kgA kg solute


xA    overflow liquid yA    liquid slurry (underflow)
kgA  kgC kg solution kgA  kgC kg solution
V1= ? kg V2 = 100 kg
xA1 = ? xA2 = 0
xC1 = ? 1 xC2 = 1.0

Lo= 20 kg L1 = ? kg
yAo = 1 yA1 =?
yCo = 0 N1
B = 100 (1-0.2)=80 kg
No

By overall balance and solute balance,


(Equation 1, 2, 3) solve for M.

Overall balance  Lo + V2 = L1 + V1 = M=20+100= 120 kg


Solute balance  LoyAO + V2xA2 = 20(1.0)+100(0)= 120xAM
Solve both balance equation to get xAM = 0.167.

Next B = NoLO = 4.0(20) = 80 = NM (120)


Solve  NM = 0.667
 Plot XAM, NM to get point M at Fig 12.9.3. Plot V2 and Lo.
 Draw tie line to get V1 and L1 (in equilibrium)
 Draw N=1.5 (horizontal line)
 Get yA1=0.167, xA1=0.167
 Substitute into balance equation 1 & 3 to get L1=53.3 kg, V1=66.7 kg
 OR can also use lever arm rule
Exercise 1: Single Stage Leaching
 Acetone is used as solvent to leach oil from seed flake. The inlet flow
per hour of fresh solvent mixture contains 1400 kg/h acetone. The
amount of inert solid meal to be treated is 3000 kg/h which
contains 30 wt% of oil. N is essentially constant at 2 kg solid/kg
solution. Calculate the amounts and concentration of the stream
leaving the process.
Exercise 2: Single Stage Leaching
 A slurry of flaked soybeans weighing a total of 100 kg contains 75
kg of inert solids and 25 kg of solution with 10 wt% of oil and 90
wt% of solvent hexane. This slurry is contacted with 100 kg of pure
hexane in a single stage so that the value of N for the outlet
underflow is 1.5 kg insoluble solid/kg solution retained. Calculate
the amounts and compositions of the overflow V1 and the underflow
L1 leaving the stage.

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