Unit 5 Leaching Class

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LEACHING PROCESS –

Fundamentals and Applications


Dr.R.BASKAR
Syllabus for Leaching
• Leaching: Solid-liquid equilibrium, single
stage leaching, multi stage cross current and
countercurrent leaching operations.
• Leaching equipments – Bollman extractor,
Rotocel extractor, Kennedy Extractor, Pachuca
tank, Dorr agitator – working principle and
applications.

CO5: Perform leaching calculations and illustrate the


Applying
principle and operation of leaching equipments
What is Leaching
• Mass Transfer Operation in which solid
mixture (Feed )is contacted with a liquid
solvent for Removal of one or more
constituents (Solute) of solid mixture
• Purpose : Production or Purification
Under flow and Overflow : Definition
and Requirements

Feed , B + C
OVERFLOW
LEACHING
Solvent , A

A – Solvent B- InsolubleS C- Solute


Examples for Leaching
Edible oils extracted from seeds ( Soybeans, Organic solvents like
01 sunflower oils, rice bran, cotton seeds palm, hexane, acetone and ether
coconuts etc..)
02 Extraction of sugar from sugar beets Hot water
03 Tannin from tree barks Water
04 Removal of caffeine from coffee Water or Super critical CO2
05 Natural organic products separated from seeds, Suitable solvents
roots, fruits, leaves, stems and tree barks
06 Recovering Useful ingredients from Food Suitable solvents
industry wastes
07 Large scale recovery of metals like copper, gold, Suitable solvents
aluminum, cobalt, manganese, nickel, zinc etc…
08 Copper from its ore Sulphuric acid
09 Gold from its ore Sodium cyanide solution
10 Washing Precipitates Suitable solvents
Different Names for Leaching
Lixiviation Leaching of Alkali from wood Ash
Decoction Leaching using solvents
Elutriation Washing of soluble materials from the surface of
insoluble solids
Expression When the oil content in the seed is relatively
high, it can be recovered by compressing the
solid by a process of Expression

Leaching Process Involves :


I - Contact
II- Separation (Mechanical)
* Taking place in same equipment or Different Piece of Equipment
Rate of Leaching  General steps involving when
solid feed is brought into contact with a liquid solvent
1. The solvent is transferred from the bulk liquid to the solid
surface
2. The solvent diffuses in to solid particles
3. The solute dissolves in the solvent
4. The solute diffuses through the solid- solvent mixture to
the surface of solid particle
5. The solute is transferred from the surface to the bulk
solution
1,2,3  occur quickly
4th step decribed by means of effective diffusivity *
4, 5th steps are rate controlling steps
5th step Agitation increases rate of leaching
* If the solute is present in the solution contained within the pores of the inert solid,
the diffusion through the porous solid can be described by means of effective
diffusivity
Factors affecting Leaching Process
1. if the particle size is small,
Particle Length of diffusion path is small + interfacial area of mass transfer is High
Size Relativity high rate of mass transfer + Rate of Solute transfer from feed to
solvent is high

If too small,
• Separation of solid from the liquid and the drainage of the solid residue are
difficult
• Very fine particles will wedge in the interstices of the solid and block free
passage of liquid and hinder leaching

Uniform particle size of feed solid is preferred in leaching because to have


approximately same time for extraction of all particles

Preparation of feed :
crushing , grinding  Inorganic and organic ( if the soluble constituents are
surrounded by inert insoluble material)
limit the extent of crushing the feed  it is expensive operation
if the soluble fraction is present as a solid solution or is uniformly distributed
throughout the whole solid( feed) then  Grinding may not be required
Slicing, rolling, flaking, drying  Material of vegetable and animal nature
Factors affecting Leaching Process
Selective and high solubility towards solute minimize quantity of solvent
Solvent needed
Less viscous, chemical stability, recoverability, Low vapour pressure, low
density, low surface tension, low toxicity and flammability
Temperature The rate of leaching is increased at increased temperature due to
1. Solubility of the solute is high Driving force for mass transfer is high
2. decreased liquid viscosity and increased diffusivity
Upper limit for temperature may be set by considering :
1. deterioration of the solute
2. sensitivity of materials of construction to corrosion or erosion
Agitation Agitation will be desirable if
1. the rate is controlled by the diffusion of the solute from the surface of
the particle to bulk
2. Preventing sedimentation effective use of interfacial surface
Equilibrium Conditions in Leaching

• Representing Real situations


• JKL Separated solids ( Under flow or wet solids) the
locus of underflow compositions
• MNP  Clear solution with drawn ( Over flow or Leach
solution)  the locus of over flow compositions
• As MNP Lies above N= O axis (i.e x axis) overflow contains
some amount of insoluble solid B.
• Possible reasons : Either an insoluble solid is slightly soluble
in solvent or a partially settled solution is withdrawn so that
some amount of insoluble solid is also carried away.
• KM  Tie line is not vertical
• Possible reasons : (i) If in adequate contact time with
leaching solvent to dissolve all the solute is provided (ii) If
adsorption of the solute occurs (iii) If solute C is soluble in
an insoluble solid B
Equilibrium Conditions in Leaching
Represent Ideal cases where:
• Adsorption of solute does not occur clear
solution is withdrawn (overflow)
• Solution associated with the solid in the underflow
have same composition as the overflow
• Tie lines are vertical
• x vs y curve coincides with 45 degree diagonal and
the distribution co-efficient m =y/x =1
• Overflow contains no insoluble solid B either
dissolved or suspended so that the locus of
overflow composition is represented by x-axis
• Line JK representing the wet solids/ under flow (
Locus of underflow composition) is horizontal 
Amount of solution retained by the insoluble solid
B in the underflow is constant and independent of
solute concentrations.
• (i.e) Solids are settled to the same extent at all
solute concentrations
Classification of Leaching Methods
PERCOLATION vs IMMERSION
Percolation Batch or Continuous
Flow open permeable bed of solids
Bed  stationary or moving
Leaching course particles [settle solids retain less amount of solution
 less quantities of solvent for washing  concentrated extract]
Operation is slow and incomplete

Immersion Batch or continuous [ Multi stage Counter current operation is


common]
Immersion of solid in liquid with agitation
For solids disintegrate on leaching
Leaching fine particles [ Costly, settle solids retain considerable
amount of solution  large quantities of solvent for washing  dilute
extract]
Very rapid and complete leaching
HEAP LEACHING

• Solid in a stationary  solvent percolates


• Heap is constructed on impervious polymeric membrane  small chunks
agglomerates from the fine powder
• Heap may built in to piles on a pattern of perforated drain pipes around on an
impervious clay base
• Heaps  trapezoidal in cross section typically 120 m wide at the base, 6to8 m tall and
800 m long [ Example]
• Widely used for recovery of metals from ores
Insitu leaching

• Also known as solution mining


• Recovering minerals from ores ( example Uranium) & salts such as sodium
chloride
• Used when the deposits are too deep, or beds are too thin for under
ground mining
• Used for removal of toxic materials from under ground
• Disadvantages : Environmental Impact
Counter current Shank system

Also known as Extraction batteries


Number of tanks vary from 6 to 16
Open vessel or closed vessel
If the system using closed tanks operated at high pressures called diffusion batteries
Getting Strong solution
Multi stage counter current leaching without physically moving solids
One tank is always empty will be loaded with a fresh batch of solids
The solution obtained from the tank (just before fresh loading tank) will have
maximum solute concentration because the solution comes after contact with fresh
solids
DIFFUSERS
• Percolation vessels for leaching at
high pressure and temperature
• Application : Sugar from sugar beeds,
tanin from wood barks,
pharmaceuticals from barks and
seeds
• Flow by gravity , pumping
• Closed vessel  less evaporation,
leaching can be carried out above
the boiling point
• Several diffusers can be arranged in
shanks system
• Heaters are placed between the
vessels
• T : 344 K to 350 K
• 95% to 98% of sugar in the beets (
containing 12% sugar)
ESPRESSO MACHINE- For rapid extraction of coffee
• Leaching device based on the percolation method to leach coffee
from ground coffee beans.
• Burr grinder  250- 750 microns
• Portafilter to hold ground coffee
• Pressure vessel which receives water pumped at pressure 10-15
bar
• Solenoid valve
• Temperature of water : 361 to 365 K
• Time of leaching : 20 to 30 s
• Advantages :
– Short time interval between grinding and leaching
– Leaching operation with short residence time
– Water at controlled temperature and pressure
– Very fine powder for leaching
“Extraction of flavour – chemicals keeping the dissolution of unfavourable
chemicals that give bitternesss to the coffee to the minimum”
EQUIPMENTS
Bollmann Extractor
Vertical basket type extractor : Perforated baskets
attached to chain conveyer move in vertical axis

Feed usually in thin fakes first exposes with Half


Miscella at RHS
RHS  Feed and solvent contact co-current
RHS Bottom  Strong solute solution (Full miscella
)

After solute recovery from Full miscella , solvent can


be recycled

LHS  Fresh solvent is introduced in the basket


where exhausted feed is available
LHS  Feed and solvent contact co-current

LHS Bottom  Weak solute solution (Half miscella


) recycled without solute recovery

Equipment Partially counter current  suffers


from the problem of Channelling

Low stage efficiency


Horizontal Extractor

Varient of Bollman’s Extractor – Horizonatl movement of baskets


Kennedy Extractor

• Series of chambers and tubs – solids are transported in succession from chamber to
chamber by slow impellers
• Perforation provided in the impellers facilitates drainage of solution from the bed of solids
emerging from solution when the impeller lifts the solid above the liquid level
• Impellers  scrapped to discharge the solids which are then dumped in to adjacent
chamber
• Perfect counter current operation
• Solids are subjected to mechanical shear  Fragile materials ( like flaked oil seeds ) are
not preferred
• Requires only less Head room
ROTOCEL
• Moving bed percolation type
multistage equipment
• Closely simulating / resembling
Shanks system
• Circular Rotor Divided in to
compartments with perforated
bottom
• When Rotar Revolves each cell
passes successively through solid
feed area, a series of solvent
sprays, a final spray and drainage
area
• Solvent solution from
compartments  pumped to the
cell preceding the cell from which
they are withdrawn
• Perfect counter current operation
• Strong solute solution is drawn
off from the compartment under
the freshest solids
• Can handle flakes and seeds
Hildebrandt Extractor

• Immersion – Type
continuous Extractor
• Three screw conveyers
arranged in U-Shape
• Helix surface is perforated so
that the solvents can pass
through continuously
• Counter current
• Preferred for light
permeable solids
Pachuca Tank

• Immersion type batch extractors


• Air agitated vessels
• Fine feed solids smaller than 0.1
mm
• Air lift mechanism
• Leaching is completed air flow
is cut off  solids are allowed to
settle
• Clear solution withdrawn by
siphoning from the top of the tank
• Settled solid drawn off as
sludge from bottom of the tank
DORR AGITATOR

• Immersion type Continuous


extractor
• Both air lift principle and
mechanical raking of solids
• Central air lift  Hollow shaft
• Rakes  drag the solids to
center
• Perforated launder at top 
distributes the suspension
evenly over the surface of the
liquid in vessel
Dorr Thickener
Units for the Notations

A = solvent B = Insoluble C= Solute


F , E1 ,R 0 ,R1  ?
NF, N1  ? Take 2
minutes
yF, y1, X0, X1  ?
Units/ Formulae for the Notations

Ym1
Nm1

A = Solvent B = Insolubles C= Solute


F , E1 ,R 0 ,R1  A + C
NF, N1  B/( A+C)
yF, y1, X0, X1  C/( A+C)

Ym1 = (FyF+R0X0)/(F+R0)
Nm1= B/(F+R0)
PROBLEM
Solving the problem :

Given Data :
Feed = Solids
Feed contained 100 g insoluble solids and 10 g oil
200 g of organic solvent
Single stage leaching Solvent used is fresh
N= -4y+8

Determine the amount of oil left after leaching


Solving the problem : ( Continued)

• Step 1: Create N-x,y Data


x 0.02 0.04 0.06 0.08 N = -4Y+8
y 0.26 0.28 0.31 0.34
N

• Step 2 : Create four box for input and out put


parameters
INPUT OUTPUT
Solids to be leached Leached Solids

INPUT OUTPUT
Leaching solvent Leach solution
Solving the problem : ( Continued)

• Step 1: Create N-x,y Data


x 0.02 0.04 0.06 0.08 N = -4Y+8
y 0.26 0.28 0.31 0.34
N 6.96 6.88 6.76 6.64
Solving the problem : ( Continued)
• Step 2 : Create four box for input and out put parameters
USE Given
Data for
A,B,C
INPUT: Solids to be leached OUTPUT : Leached Solids

A = A =
B = B =
C = C = TO DETEMINE
F = E1 =
YF = N1 =
NF = Y1 =

INPUT : Leaching solvent OUTPUT: Leach solution


A =
B = A =
C = B =
R0 = C =
X0 = R1 =
X1 =
Solving the problem : ( Continued)

Given Data :
Feed = Solids
Feed contained 100 g insoluble solids and 10 g oil
200 g of organic solvent
Single stage leaching Solvent used is fresh
N= -4y+8
Solving the problem : ( Continued)
• Step 2 : Create four box for input and out put parameters
From
Given Basis : 100 gm of Insolubles
Data

INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A =
B = 100 gm B = 100 gm
C = 10gm C =TO DETEMINE
F = E1 =
YF = N1 =
NF = Y1 =

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm
B = 0 gm A =
C = 0 gm B =0 gm
R0 = C =
X0 = R1 =
X1 =
Solving the problem : ( Continued)
• Step 2 : Create four box for input and out put parameters
From
Given Basis : 100 gm of Insolubles
Data

INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A =
B = 100 gm B = 100 gm
C = 10gm C =TO DETEMINE
F = E1 =
YF = N1 =
NF = Y1 =

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm
B = 0 gm A =
C = 0 gm B =0 gm
R0 = C =
X0 = R1 =
X1 =
Solving the problem : ( Continued)
• Step 2 : Create four box for input and out put parameters

USE
formulae

INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A =
B = 100 gm B = 100 gm
C = 10gm C =TO DETEMINE
F = A+ C = ? E1 =
YF = C / (A+C) = ? N1 =
NF = B / (A+C) = ? Y1 =

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm
B = 0 gm A =
C = 0 gm B =0 gm
R0 = A+C = ? C =
X0 = C/ A+C = ? R1 =
X1 =
Solving the problem : ( Continued)
• Step 2 : Create four box for input and out put parameters

USE
formulae

INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A =
B = 100 gm B = 100 gm
C = 10gm C =TO DETEMINE
F = A+ C = 10g E1 =
YF = C / (A+C) = 1 N1 =
NF = B / (A+C) = 10 Y1 =

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm
B = 0 gm A =
C = 0 gm B =0 gm
R0 = A+C =200 gm C =
X0 = C/ A+C = 0 gm R1 =
X1 =
Solving the problem : ( Continued)

Step 3 : Calculate M1 point (Ym1 , Nm1 )


Ym1 = (FyF+R0X0)/(F+R0)= ?
Nm1= B/(F+R0) =?
Solving the problem : ( Continued)

Step 3 : Calculate M1 point (Ym1 , Nm1 )


Ym1 = (FyF+R0X0)/(F+R0)= 0.0476
Nm1= B/(F+R0) = 0.476
Step 4 : Draw N vs x,y curve
Draw x vs y curve ( Both in same sheet)
Solving the problem : ( Continued)
Solving the problem : ( Continued)

• Locate M1 ( (0.0476,0.476) in the graph


• Tie line is a straight line connecting E1 and R1
and passing through M1
• E1 point corresponds to y1 and R1 point
correspond to x1
• But We don’t know x1 and y1 .
• We can make trail and error way to fix
• Trial 1 : let we take x1= 0.02 and check
whether E1R1 passes through M1
Solving the problem : ( Continued)
• Trial 1 : let we take
x1= 0.02 and check
whether E1R1
passes through M1
• Corresponding y1 is
0.256
• E1 point
corresponds to y1
and R1 point
correspond to x1
• Line joining E1 and
R1 is not passing
through M1
• Trial 2 : let we take
x1= 0.03 and check
whether E1R1
passes through M1
• Corresponding y1 =
0.27
• Line joining E1 and
R1 is passing
through M1
Solving the problem : ( Continued)

x1 = 0.03 and y1 = 0.27


We know N1= -4Y1+8
N1= ?

Also N1= B/(A+C)  B/A+C = ?


B=100 gm
A+C = ?
Solving the problem : ( Continued)

x1 = 0.03 and y1 = 0.27


We know N1= -4Y1+8
N1= 6.92

Also N1= B/(A+C)  B/A+C = 6.92


A+C = 14.45 gm

Y1 = C/ A+C
0.27= C/ 14.5
C= 3.9 gm which is nothing but oil left in the solids (
unextracted)
Oil in seeds = 10 gms
 % oil left in seeds ( as unextracted) = (3.9/10)x100 = 39%
Solving the problem : ( Continued)

INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A =
B = 100 gm B = 100 gm
C = 10gm C = 3.9 gm( DETEMINED)
F = A+ C = 10g E1 = 14.45 gm (A+C)
YF = C / (A+C) = 1 Y1 = 0.27
NF = B / (A+C) = 10 N1 = 6.92

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm A =
B = 0 gm B = 0 gm
C = 0 gm C =
R0 = A+C =200 gm R1 =
X0 = C/ A+C = 0 gm X1 = 0.03
Solving the problem : ( Continued)
INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A = 10.6 gm
B = 100 gm B = 100 gm
C = 10gm C = 3.9 gm
F = A+ C = 10g E1 = 14.45 gm (A+C)
YF = C / (A+C) = 1 Y1 = 0.03
NF = B / (A+C) = 10 N1 = 6.92

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm
B = 0 gm A =
C = 0 gm B =0 gm
R0 = A+C =200 gm C =
X0 = C/ A+C = 0 gm R1 =
X1 = 0.03

For Leached solids:


A+C = 14.45  A +3.9 = 14.5 Therefore A = 10.6 gm
Solving the problem : ( Continued)

INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A = 10.6gm
B = 100 gm B = 100 gm
C = 10gm C =3.9 gm
F = A+ C = 10g E1 = 14.45 gm
YF = C / (A+C) = 1 Y1 = 0.03
NF = B / (A+C) = 10 N1 = 6.92

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm
B = 0 gm A = ?
C = 0 gm B = 0 gm
R0 = A+C =200 gm C = ?
X0 = C/ A+C = 0 gm R1 = A+C = ?
X1 = 0.03

For Leached solids:


A = 200 -10.6 = 189.4 gm
C = 10-3.9 = 6.1 gm R1 = A+C= 195.5 gm
Solving the problem : ( Continued)

INPUT: Solids to be leached OUTPUT : Leached Solids

A = 0 gm A = 10.6gm
B = 100 gm B = 100 gm
C = 10gm C = 3.9 gm
F = A+ C = 10g E1 = 14.45 gm
YF = 1 Y1 = 0.03
NF = 10 N1 = 6.92

INPUT : Leaching solvent OUTPUT: Leach solution


A = 200 gm
B = 0 gm A = 189.4 gm
C = 0 gm B = 0 gm
R0 = A+C =200 gm C = 6.1 gm
X0 = C/ A+C = 0 gm R1 = 195.5 gm
X1 = 0.03
Problem 1
One hundred kg each of a solid feed containing
25% solute (C) and 75 % insolubles (B) is
subjected to single – stage leaching using one
hundred kg of a pure solvent (A). After settling
75 Kg of clear solution is withdrawn as overflow.
What is the inert to solution weight ratio[
B/(A+C)] in the underflow?. No insolubles (B)
present in overflow.
Problem 2
One hundred kg each of a solid feed containing
25% solute (C) and 75 % insolubles (B) is
subjected to single – stage leaching using one
hundred kg of a pure solvent (A). After settling
75 Kg of clear solution is withdrawn as overflow.
No insolubles (B) present in overflow. The value
of Nm1 is
Problem 3
One hundred kg each of a solid feed containing
25% solute (C) and 75 % insolubles (B) is
subjected to single – stage leaching using one
hundred kg of a pure solvent (A). After settling
75 Kg of clear solution is withdrawn as overflow.
No insolubles (B) present in overflow. The value
of ym1 is
Problem 4
The seeds containing 25% oil and the rest
insoluble are mixed with hexane. The
composition of the resulting mixture if the seeds
and solvent are mixed in equal amounts by
weight is

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