UNIT III

EXTRACTION (Liquid –Liquid Extraction)

Equilibrium in ternary systems; equilibrium stage wise contact calculations for batch and
continuous extractors, differential contact extraction equipment - spray, packed and
mechanically agitated contactors and their design calculations; pulsed extractors, centrifugal
extractors
University Repeated Question

1. Solvent requirement for a single batch operation and for a five. Cross current
stage with equal amount solvent in each stage.

2. Explain the working principle and operation of anyone differential contact

extraction equipment with a diagram.

3. Draw the neat stretch and explain the working of centrifugal extractors.

4. With neat sketches, explain the working principle of Rotating disk contactor and
schebile type extractor.
5. Describe the principle and constructional features of various extraction
equipments with neat sketches.

6. Explain with schematic diagram Multistage Cross-current Extraction

7. Explain the factors to be considered in the choice of solvent for extraction.

8. Explain briefly:
(l) LLE. (or) Explain the effect of temperature on LLE.
(2) Selectivity
(3) Distribution coefficient
(4) Solutropic system.

9. Describe the design methodology to evaluate the number of theoretical stages

in a multi stage counter-current extractor for extracting partial miscible
systems. State the importance of design parameters.

10. Explain with a neat sketch .the working of a mechanically agitated

contactor for Extraction operation.

11. Nicotine in water solution containing 1% nicotine is to be extracted with

kerosene at 20°C. Water and kerosene are essentially immiscible. The
equilibrium data are as follows:
X 0 0.001011 0.00246 0.00502 0.00998
Y 0 0.000807 0.001961 0.00456 0.00913
Where X = kg Nicotine I kg water, Y = kg Nicotine /kg kerosene.
(a)Determine the percentage extraction of nicotine if 100 kg of feed solution is
extracted once with 150 kg of solvent.
(b)What is the percentage extraction of 3 cross current stages if 50 kg of
solvent is used every time?

Liquid Extraction Unit-3 Mass Transfer-II

 12. A solution of nicotine in water containing 1 % nicotine is to be extracted with
kerosene at 293 K. Water and kerosene are essentially insoluble.' Assume the
equilibrium relationship to be: Y= 0.9X
Where, Y = Kg nicotine/Kg kerosene X = Kg nicotine/kg water
(1) Determine the percentage extraction of nicotine if 100 Kg of feed solution
is extracted with 150 Kg of solvent.
(ii) Repeat for 3 theoretical extractions using 50 Kg solvent each time.
(11 question same problem)
.
13. A solution of 5% acetaldehyde (A.A) and 95% toluene is to be extracted with water in
a five-stage cross current extraction to extract acetaldehyde. Toluene and water arte
essentially insoluble. If 25 kg of water l00 kg feed is used, find the amount of
acetaldehyde extracted and the final concentration. The equilibrium relation is given
by : Y= 2.20 X Y(kg acetaldehyde /kg water) X(kg acetaldehyde/kg
toluene) (Both by theoretical arid graphical method)

14. How many kg of minimum solvent required for 1000 kg per hour of dioxane
water solution extracted continuously in counter current fashion and how many
theoretical stages required if 900' kg per hour of solvent is required.
Eqn. data Weight % dioxane in water: 5.1 18.9 25.2
Weight % dioxane in water: 5.2 22.5 32
At these concentrations water and benzene are sustainably insoluble. 1000 kg of a
25% dioxane water solution is to be extracted to remove 95% of dioxane. The benzene
is dioxane free.
1. Calculate minimum solvent required in kg/h if the extraction
2. Calculate the benzene required for five stage cross current operation with
600kg of solvent used in each stage

15. Water-dioxane solution forming an azeotrope, hence it is treated with benzene.

Equilibrium distribution of dioxane between water and benzene at.25°C·
be1ow: Wt% dioxane in water: 5.1 18.9 25.2
Wt% dioxane in benzene: 5.2 22.5 32
At these concentrations water and benzene are sustainably insoluble. 1000 kg
of a 25% dioxane water solution is to be extracted to remove 95% of dioxane.
The benzene is dioxane free.
a)Calculate minimum solvent required in kg/h if the extraction is done in
counter current fashion.
b) Estimate the number of stages needed if 1.5 times the minimum amount
of solvent is used

16 A solution containing 18% (by weight) acetone in water is to be extracted with pure
Mono-chlorobenzene by countercurrent extraction process. Mono-chlorobenzene and
water are immiscible in the operating condition.
x' kg acetone/kg water 0.025 0.073 0.160 0.267
y' kg acetone/kg mono-chlorobenzene 0.028 0.070 0.156 0.237
In order to obtain a raffinate with 1% acetone concentration estimate
(1) Minimum amount solvent needed per kg of feed and

Liquid Extraction Unit-3 Mass Transfer-II

 (2) The theoretical number stages needed if the solvent used is 1.2 times the
minimum.
UNIT- 3

Liquid –Liquid Extraction or Liquid Extraction

Liquid Extraction
1. Liquid- liquid operation is also known as “Solvent Extraction”.The separation of the
constituents of a liquid solution by contact with another insoluble liquid
Extract (E)
The layer which is rich in solvent is known as “Extract” (solvent-rich product)
Raffinate (R)
The (Residual liquid from solute) other layer is known as Raffinate
Solute
The constituents distribute themselves differently between the two layers. The
constituents of the liquid solution which is extracted by the solvent is known as solute
Liquid Equilibria
Extraction involves the use of systems composed of at least three substances and
although most part the insoluble phase are chemically very different, generally all three
components appear at least to some extent in both phase
The following notation scheme used in extraction
In these process to describe the concentration and amount of these ternary mixtures, for
purpose of discussing both equilibria and material balance
1. A and B are pure, substantially insoluble liquids and C is the distributed solute.
Mixture to be separated by extraction are compound A and C and B is extracting
solvent
2. The quantities are measured by mass for batch operation, Mass /time for continuous
operation
• E = Mass/ Time of solution E, an Extraction, Shown on a phase diagram by point E ‘’
• R= Mass/ Time of solution R, an Raffinate, Shown on a phase diagram by point R ‘’
• B = Mass / time of solvent B
Solvent= free (B-Free) quantities are indicates by primed letter, Thus
E’ =Mass B – Free solution / Time

E = E’ (1+ NE)

x = weight fraction ‘c’ in the solvent –lean (A-Rich) or “Raffinate liquid”

y = Weight fraction ‘c’ in the solvent –rich (B-rich) or ‘Extract liquid’

Liquid Extraction Unit-3 Mass Transfer-II

 X’ = x / 1-x = Mass C

Mass non-C in the raffinate liquid

Y’ = y / 1-y = Mass C

Mass non-C in the Extract liquid

X=Weight fraction ‘C’ in the raffinate liquid on a (B-Free) basis (Mass C /Mass A + Mass C)

Y = Weight fraction ‘C’ in the Extract liquid on a (B- Free) basis (Mass C /Mass A + Mass C)

N = Weight fraction ‘B’ on a (B- Free) basis (Mass B /Mass A + Mass C)

Equilateral Triangular Co-ordinates

In a Binary mixture containing 80% A and 20% B. Mixture containing same ratio of A to B

R = line ME = xE – xM ----------1
E line RM x E - xM

System Encountered in Extraction

1. One Pair Partially soluble

2. Two Pair Partially soluble

3. Two partially soluble liquids and one solid

Liquid Extraction Unit-3 Mass Transfer-II

 One Pair Partially soluble
Example
Water (A) - Chloroform (B) – Acetone (C)
Benzene(A) - Water(B) – Acetic acid (C)

• B& C ---- Completely soluble

• A& B, A& C --- Soluble only to limited extent

• A – C ---Feed solvent

Tie line parallel to Base line -----Solutropic system

Liquid ‘C’ dissolves completely in A and B and A and B dissolves only to a limited extent in
each other to give a saturated solution

L- Indicates saturated liquid ‘B’ in ‘A’ (A-Rich)

K- Indicates saturated liquid ‘A’ in ‘B’ (B-Rich)

L- is a binary mixture that separates in 2 soluble liquid phase like ‘L’ in ‘K’

Tie –line

1. LRPEK- indicate the binodal solubility line RE indicates the equilibrium

composition (tie line)

2. Usually the tie line are not parallel, changes their slope in one direction. In some
system , one of the tie line may be Horizontal with base is known as Solutropic
System
Plait point

Liquid Extraction Unit-3 Mass Transfer-II

 Plait point is located near the top of the two-phase envelope, at the inflection point. It
represents a condition where the 3-component mixture separates into two phases, but the
phases have identical compositions

Choice of Solvent for Extraction

Selectivity
The ratio of concentration ratio of solute to the feed solvent in extract phase to that in the
raffinate phase is called as ‘Selectivity’ or ‘Separation factor’

β >1 less solvent requirements & Good Separation occur

β = 1 No separation
1. Recoverability
As solvent should be recovered for reuse frequently by distillation, it should not form an
azeotropes with extracted solute and for low cost recovery, relative volatility is high
2. Distributed co-efficient (y*/ x)
Higher values (>1) of it are generally desirable as less solvent will be required for given
extraction duty
(y*/ x) > 1
3. Density
The difference in density of saturated liquid phases should be larger for physical separation
of phases
4) Interfacial Tension
Interfacial tension should high
5. Insolubility of solvent
The solvent insoluble in original liquid solvent should be preferred and it should have high
solubility for solute to be extracted, Then small amount of solvent of solvent are required
7. The solvent should be stable chemically
8. Chemically inert
9. Non- corrosive
10. Non- toxic
11. Cheap
12. Low cost
13. Low freezing point

Liquid Extraction Unit-3 Mass Transfer-II

 14. Low vapour pressure ,became easy to handling and storage
15. Non-flammable

MIXTURE RULE

ET – MO = EP
MO -RL = PS

Where
R – Raffinate E - Extract M - Mixture
xR, xE , Xm - Mass fraction of solute in raffinate, Extract, Mixture
Overall material balance
R+E = M--------------1
Individual material balance
R xR + E xE = M xM -------------2
Sub M = R + E in equation 2
R xR + E x E = M x M
R xR + E xE = (R+ E) xM
R xR + E xE = R xM + ExM
R xR - R x M = E x M - E x E
R (xR - xM ) = E (xM - xE )
R/E = (xM - xE ) / (xR - xM )
R/E = (xE - xM ) / ( xM - xR) ------3
Component balance from graph
R (line RL) + E (line ET) = M ( line MO)----4
Using equation (1) eliminate ‘M’ from eq 2
Sub eq (1) in eq (4) R+E=M
R (line RL) + E (line ET) = (R + E)( line MO)

Liquid Extraction Unit-3 Mass Transfer-II

R (line RL) + E (line ET) = R( line MO) +E( line MO)
R (line RL) - R (line MO) = E( line MO) - E (line ET)
R (line RL - line MO) = E ( line MO - line ET)
R / E = (line MO - line ET) / (line RL - line MO)
R / E = (line ET - line MO) / (line MO - line RL)
R / E = line EP / Line PS
R / E = line ME / Line RM
R / E = XE - xM / XM –XR

-------------------&---------

Methods of Extraction
I. Single stage contact extraction
II. Multi –stage Extraction
a. Co-Current ( )
b. Counter –Current ( )
c. Cross – current ( ) ( )

Single Stage contact Extraction (co-current)

a. One Pair partially miscible : stage-1

1. Let F be mass of feed solution (in kg) containing solute C and feed solvent A with xf
mole fraction of C is feed to single stage
2. The feed solution is contacted with nass S , of a solvent containing principally B with
ys weight fraction of C
3. If the solvent id pure B, ys = 0 and S1 = B
4. After contacting and phase separation we get equlibrium Raffinate R1 and Extract E1
5. Let x1 be the weight fractoin C in Raffinate
6. Let y1 be the weight fractoin C in Extract
7. Let xf - Mass fraction of C in Feed
8. Let Ys –mass fraction of C in solvent
If the solvent is pure (B) ,Ys =0 the S1 = B
Liquid Extraction Unit-3 Mass Transfer-II
Overall material balance:
F + S1 = M1 = E1 + R1 ------1
The point M1 can be located on the line FS1 by mixture rule , equation 1 becomes
F / S1 F = line length M1 S1 /line length FM1 --------2
Let xM1 is the weight fraction of C in Mixture M1
Individual material balance :
F xf + S1 ys = M1 xM = E1 y1 + R1 x1 ------3
Sub F + S1 = M1 in eq 3
F xF + S1 ys = (F+ S1)xM = E1 y1 + R1 x1
F xF + S1 ys = F xM + S1 xM -----4
F xf - F xM = S1 xM - S1 ys
F( xF - xM ) = S1 ( xM - ys)
S1 / F = ( xF - xM ) / ( xM - ys)-----5
Consider the equation:
M1 xM = E1 y1 + R1 x1 (M1 - E1=R1 )
Eliminate R1 from the equation
E1 y1 + (M1 -E1)x1 =M1 xM
E1 y1 + M1x1 -E1x1 =M1 xM
E1 y1 -E1x1 = M1 xM - M1x1
E1 (y1 -x1 ) = M1 ( xM - x1 )
E1 / M1 = ( xM - x1 ) / (y1 -x1 ) -----6
Note: Expression can be used to find out the amount of solvent required for the
particular separation. Quantity of Extract can be obtained from equation 6

Material balance for solvent free -basis

Liquid Extraction Unit-3 Mass Transfer-II

Single stage extraction solvent free co-ordinates
1. Where E’ indicates mass of the extract in solvent free basis
2. F’,S’,R’ indicates mass of feed , solvent ,and raffinate in solvent free basis
3. xf ,ys ‘ , y1 ‘ ,x1 - weight fraction of C in feed ,solvent , extract and raffinate in
solvent free basis
4. N- Weight of solvent in solvent free basis
5. Nf ,Ns, NE ‘,NR – Weight of solvent in feed ,solvent , extract and raffinate in solvent
free basis
Total material balance : (solvent free basis)
F’,S’,R’, y1 ‘
F’ + S’ = M1’= E1’+R1‘----------7
Component balance (C)
F’ xf + S’ ys = M1’ xm = E1’ y1 +R1‘x1 ----------8
Component balance (B)
F’ Nf + S’ Ns = M1’ N1 = E1’ NE +R1‘NR ----------9
let M1 ‘- E1‘=R1 ‘
M1‘ xm - E1‘y1 =R1‘x1
M1‘ xm = E1‘y1 + (M1‘- E1‘) x1
M1‘ xm = E1‘y1 + M1 ‘ x1 - E1‘ x1
M1‘xm - M1 ‘x1 = E1 ‘y1 - E1 ‘x1
M1 ‘ (‘xm - ‘x1 ) = E1 ‘ (‘y1 - ‘x1 )
(‘xm - ‘x1 )/ (‘y1 - ‘x1 ) = E1 ‘ / M1 ‘ -------- 10
-----------------------------------------------&---------------------------------------------------------
Multi-Stage Cross –Current Extraction
Partially miscible solvent

Liquid Extraction Unit-3 Mass Transfer-II

 Fig shows a three stage cross current extraction operation . Here the raffinate from
any stage acts as a feed for the next stage and as raffinate moves from stage to stage,Finally
from all stages can be combined to get the composited extract (E)
Stage 1:
Overall material balance: M1 = F+ S1
F + S1 = M1 = E1 + R1 -------1
Material balance of individual at solute‘c’
F xF + S1ys = M1xM1 = E1 y1 + Rx1 ------------------2
F xF + S1ys = M1xM1 ------------2.a
F xF + S1ys = (F + S1) xM1
F xF + S1ys = F xM1 + S1xM1
F xF - F xM1 = S1xM1 - S1ys
F (xF - xM1 ) = S1 (xM1 – ys )
S1 / F = (xF - xM1 )/ (xM1 – ys ) ---------3
From eq 2.a becomes
F xF + S1ys = M1xM1
Liquid Extraction Unit-3 Mass Transfer-II
 xM1 = F xF + S1ys / M1 -----------4
From eq 2
M1xM1 = E1 y1 + Rx1
M1xM1 = E1 y1 + (M1- E1)x1
M1xM1 = E1 y1 + M1x1 - E1x1
M1 xM1 - M1x1 = E1 y1 - E1x1
M1 (xM1 - x1 ) = E1 (y1 - x1 )
E1 /M1 = (xM1 - x1 )/ (y1 - x1 ) -------------5
E1 = M1 (xM1 - x1 )/ (y1 - x1 ) -------------6
For stage :2
Overall material balance: M2 = R1+ S2
R1 + S2 = M2 = E2 + R2 -------7
Material balance of individual at solute‘c’
R1 x1 + S2ys = M2xM 2 = E2 y2 + Rx2 -------7.A
R1 x1 + S2ys = M2xM2 ------------2.a
R1 x1 + S2ys = (R1 + S2) xM2
R1 x1 + S2ys = R1 xM2 + S2xM2
R1 x1 - R1 xM2 = S2xM2 – S2ys
R1(x1 – xM2) = S2 (xM2 – ys )
S2 / R1 = (x1 – xM2)/ (xM2 – ys) ------8
From eq 7.a becomes
R1 x1 + S2ys = M2xM2 -----9
xM2 = R1 x1 + S2ys / M1 (R1+ S2 ) -----------10
From eq 7
M2xM2 = E2 y2 + R2x2 R2 = M2 –E2
M2xM2 = E2 y2 + M2 –E2 x2
M2xM2 = E2 y2 + M2x2 - E2x2
M2xM2 - M2x2 = E2 y2 – E2x2
M2 (xM2 - x2 ) = E2 (y2 – x2 )
E2 /M2 = (xM2 - x2 )/ (y2 – x2 )
E2 = M2 (xM2 - x2 )/ (y2 – x2 )-------------11
Liquid Extraction Unit-3 Mass Transfer-II
For stage : nth stage
Overall material balance: Mn = Rn-1+ Sn
Rn-1 + Sn = Mn = En + Rn -------12
Material balance of individual at solute‘c’
Rn-1 xn-1 + Snys = Mn xM n = En yn + Rnxn-------12.A
Rn-1 xn-1 + Snys = MnxMn
Rn-1 xn-1 + Snys = (Rn-1 + S2) xMn
Rn-1 xn-1 + Snys = Rn-1 xMn + SnxMn
Rn-1 xn-1 - Rn-1 xMn = SnxMn– Snys-------13
Rn-1 ( xn-1 – xMn ) = Sn (xMn – ys )
S2 / Rn-1 = (xn-1 – xMn)/ (xMn – ys )------14
From eq 12.a becomes
Rn-1 xn-1 + Snys = MnxMn -----15
xMn = Rn-1 xn-1 + Snys / M1 (Rn-1 + Sn ) -----------16
From eq 12.a

MnxMn = En yn + Rnxn Rn = Mn –En

MnxMn = En yn + Mn –En xn

MnxMn = En yn + Mnxn - Enxn

MnxMn - Mnxn = En yn – Enxn

Mn (xMn - xn ) = En (yn – xn )

En /Mn = (xMn - xn )/ (yn – xn )

En = Mn (xMn - xn )/ (yn – xn )-------------17

Graphically represent of multistage cross current extraction on triangular co-ordinates shown

in fig. The solvent amount used for extraction S 1, S2, and S3 as are have same composition
they are represented by points

------------------------------------------&--------------------------------------------------------------------

MULTI-STAGE CROSS –CURRENT EXTRACTION

(Immiscible solvents)
• In this case ,feed solvent and extraction solvent are completely immiscible .
• In case Raffinate from all stage will contain only ‘A’ and ‘C’ and extract from each
stages contain only B and C

Liquid Extraction Unit-3 Mass Transfer-II

 • Further all ‘A’ in the feed solution will be there in all raffinate and the extract from
each stages contain all the solvent ‘B’ feed to that stage

Case (i)
Consider the equal amount of solvent is used in each stage and the solvent is pure B (ys =0)
xf = (Mass C /Mass A ) in the feed solution
x1, x2, x3 ….= (Mass C /Mass A ) in the Raffinate solution from stage 1,2,3
y1, y2, y3 ….= (Mass C /Mass B ) in the Extract solution from stage 1,2,3
B = Amount of pure solvent added in each stage
From stage 1
Axf = Ax1 + By1 ---------------1
-By1 = Ax1 – Axf
-By1 = A (x1 – xf )
y1 / (x1 – xf ) = - A / B -------------2
Equation 2 is the operating line equation for stage1 of slope (-A/B) and passing through
points (xf , 0) and (x1 ,y1 )
For stage :2
Ax1 = Ax2 + By2
-By2 = Ax2 – Ax1
-By1 = A (x2 – x1 )
y2 / (x2 – x1 ) = - A / B -------------3
Equation 2 is the operating line equation for stage1 of slope (-A/B) and passing through
points (x1 , 0) and (x2 ,y2 )
For stage :n
{ yn / (xn – xn-1 ) } = - A / B -------------4
As the equal amount of solvent are used for each stage , the slope of operating line equation
for all stage is same (-A/B) so the operating line in this case are the parallel to each other on
Y vs X plot

Liquid Extraction Unit-3 Mass Transfer-II

Derivation for obtaining the composition of the final raffinate and the number of stages
required
Material balance of solute over stage 1
Axf = Ax1 + By1 ---------------1
Let y = mx
y1 = mx1 -----------------2
sub eq 2 in eq 1 ,we get

Axf = Ax1 + B mx1

Axf = ( A+ B m) x1

x1 = A / ( A+ B m) xf -------3

Material balance stage 2

Ax1 = Ax2 + By2 ---------------4

Let y = mx

y2 = mx2 -----------------5

sub eq 5 in eq 4 ,we get

Ax1 = Ax2 + B mx2

Ax1 = ( A+ B m) x2

x2= A / ( A+ B m) x1 -----------6

For stage n:

xn = { A / ( A+ B m)}n xf -----------7

xn / xf = { A / ( A+ B m)}n ----------------8

Taking ln on both side 8 we get

Liquid Extraction Unit-3 Mass Transfer-II

 n.ln {A / (A+ B m)}n = ln( xn / xf ) ---------------9

n =ln {A / (A+ B m)}n / ln( xn / xf ) -------10

If A,B, xf and n are known , then calculate the composition of the final Raffinate x n leaving
stage n by using equation 9
If A,B, xf and xn are known ,then calculate the number of stage by using equation 10
Case;II Insoluble liquid –unequal amount of solvent solvent contains some amount of
solute (B is not equal to constant through ys is not equal to zero)

Material balance (stage -n)

Axn-1 +Bnys = Axn + Bnyn ------------------11

Axn-1 - Axn = Bnyn – Bnys
A (xn-1 - xn ) = Bn (yn – ys )
A/ Bn = (yn – ys )/ (xn-1 - xn )
- A/ Bn = (yn – ys )/ (xn - xn-1 ) -----12
from 12 is the operating ilne eq for the stage –n (slope = - A/ Bn )

-------------------------&------------------------------------
Continuous Multistage counter –current Extraction
System of three liquid (one pair partially miscible)

Liquid Extraction Unit-3 Mass Transfer-II

Feed solution is feed to the first stage which leaves it as raffinate R1 which then passes
through further stages and leaves from nth stages as final raffinate Rn.
The fresh solvent enters the nth stages and passes through the stages in the opposite direction
and finally leaves the first stage as the final Extract E1.
Material Balance: (stage 1)
F + E2 = E1 + R1 -------1
F – E1 = R1 -E2 = ∆R ----------2
∆R - Difference point ,the represent the net flow outward at the stage

Overall material balance (entire unit)

F + En+1 = M = En + Rn ---------3
Let En+1 = s
F + S = M = E1 + Rn ---------4
Material balance for solute C:
F xF + S ys = M xm = E1y1 + Rnxn -----------4.A
xm = F xF + S ys / M-------------5 M = F+S
xm = F xF + S ys / F+S-----------6
From eq4
F – E1 = Rn - S = ∆R ----------7
∆R - Difference point ,the represent the net flow outward at the stage
Material balance for stage n:
Rn-1 + S = E + Rn
Rn-1 + S = Rn - S = ∆R ----------8
Graphical construction of number of stages

Multistage Counter current Extraction

(Immiscible solvents)

Liquid Extraction Unit-3 Mass Transfer-II

Consider that A and B are completely Ys = Yn+1 Immiscible so that the solvent content of all
Extract and A content of all raffinate are constant .Concentration of solute C is expressed as
mass ratio.
X = (Mass C /Mass A) in the raffinate liquid
Y = (Mass C /Mass B) in the Extract liquid
Ys = (Mass C /Mass B) in the Solvent used
Material balance of solute ‘C’ -stage 1
Axf + By2= Ax1 + By1 ---------------1
Material balance of solute ‘C’ –( Entire unit)
Axf + Byn+1 = Axn - By1 ---------------2
Axf - Axn = By1 - Byn+1
A (xf - xn )= B (y1 - yn+1 )
A / B = (y1 - yn+1 ) / (xf - xn ) --------------3
(A/B ). (xf - xn ) = y1 - yn+1
(A/B ). (xf - xn ) - y1 = - yn+1
yn+1 =(A/B ). (xn - xf ) + y1 -----------4
Note
yn+1, = ys = mass ratio of solute in solvent used
Eq 3 is the equation of straight line of slope (A/B) on X-Y Diagram.
This is the operating line which passes through points (xf,y1 ) and (xn,yn+1)
Graphical construction for minimum solvent requirement is shown in fig

Liquid Extraction Unit-3 Mass Transfer-II

 University Problem
1. A solution containing 5% acetaldehyde and 95% toluene is to extracted with water in 5 stages
cross current extraction unit to extract acetaldehyde. Toluene and water are essentially
insoluble. If 25 Kg of water each time are used per 100kg of feed, calculate the amount of
acetaldehyde extracted and final concentration of exit solution.
The equilibrium relationship is given as
y = 2.2 x
Where y = kg of acetaldehyde/kg H2O
x = kg of acetaldehyde/kg Toluene
Solution
Basis: 100 kg of feed solution (containing 5% acetaldehyde)
Acetaldehyde present in feed (C) = 5 kg
Toluene present in feed (A) = 95 kg
XF = mass C / mass A = kg C / kg A = 5 / 95
XF = 0.05263
Number of cross current stage n=5
B = 25 Kg
y = 2.2 x
m = 2.2
Insoluble solvent
Multistage cross –current extraction:
immiscible solvent
Xn = [ A/ A+ Bm]n . XF
Xn = [ 95 / 25+ 25* 2.2]5 . 0.05263
Liquid Extraction Unit-3 Mass Transfer-II
 = 0.10189 * 0.05263
Xn = 0.00536
Final raffinate solution contain 0.00536 kg of Acetaldehyde per 1 kg of toluene
Final raffinate solution = 1+ 0.00536
= 1.00536 kg
Wt % of Acetaldehyde in raffinate solution = 0.00536 / 1.00536 * 100
= 0.533% by wt
Amount of Acetaldehyde in final exit solution = 0.00536 / 1 * 95
= 0.509 kg
Amount of Acetaldehyde removed from feed solution = 5 –0.509 = 4.491 kg

2. Nicotine in water solution containing 1% nicotine is to be extracted with kerosene at 20°C.(293K)

Water and kerosene are essentially immiscible. The equilibrium data are as

X= Kg nicotine/ kg water 0 0.001 0.0024 0.0050 0.0075 0.0099 0.204

y = kg nicotine/kg Kerosene 0 0.0008 0.0019 0.0045 0.0068 0.0091 0.0187

Where X = kg Nicotine / kg water, Y = kg Nicotine / kg kerosene.
(i)Determine the percentage extraction of nicotine if 100 kg of feed solution is extracted once
with 150 kg of solvent.
(ii)What is the percentage extraction of 3 cross current stages if 50 kg of solvent is used
every time?
Basis: 100kg of feed solution
Given
Amt of nicotine in feed = 1%
Wt fraction of nicotine = 1/100 = 0.01
Wt fraction of water in feed = 1 - 0.01 = 0.99
Case (i)
Amt of nicotine in feed soln C = 1kg
Amt of water in feed soln A = 99kg
xf = mass C / mass A = Kg C / Kg A = 1/ 99
xf = 0.01010
Amount of solvent (B) = 150KG
Nicotine in feed + Nicotine in solvent = Nicotine in Extract + Nicotine in Raffinate
AxF + Bys = Ax1 + By1 ys = 0 (pure solvent)

Liquid Extraction Unit-3 Mass Transfer-II

 AxF = Ax1 + By1
(y1 / x1 - xF ) = -A/B
= -99/150
(y1 / x1 - xF) = -0.66
Slope = - 0.66
From graph
x1 = 0.0042 kg C /kg A
y1 = 0.0038 kg C /kg B
Nicotine removed from water = A(xF -x1)
= 99(0.0101 – 0.0042)
= 0.5841 Kg
Percentage extraction of nicotine = 0.5841/ 1 * 100
= 58.41%
Case (ii)
Three stage cross –current extraction
(50kg of solvent each time)
A/ B = 99 / 50 = 1.98
Slope = -A/B = -1.98
From graph: x3 = 0.0034
Nicotine removed from water = A (xF –x3)
= 99(0.0101 – 0.0034)
= 0.6633 Kg
Percentage extraction of nicotine = 0.6633/ 1 * 100
= 66.33 %
3.Water-dioxane solution forming an azeotrope, hence it is treated with benzene.
Equilibrium distribution of dioxane between water and benzene at.25°C· be1ow:
Wt% dioxane in water: 5.1 18.9 25.2
Wt% dioxane in benzene: 5.2 22.5 32
At these concentrations water and benzene are sustainably insoluble. 1000 kg of a
25% dioxane water solution is to be extracted to remove 95% of dioxane. The benzene
is dioxane free. Calculate minimum solvent required in kg/h if the extraction is done
in counter current fashion. Estimate the number of stages needed if 1.5 times the
minimum amount of solvent is used
Solution A: Water =75% = 0.75
B : Benzene
Liquid Extraction Unit-3 Mass Transfer-II
 C : Dioxane = 25% =0.25
F= 1000kg/hr = A (Water flow rate)= 1000*0.75 A = 750Kg/hr

Wt fraction dioxane in water X=x/1-x : 0.054 0.233 0.337

Wt fraction dioxane in benzene Y=y/1-y : 0.0548 0.29 0.471

Operating Line Equation for Minimum counter current extraction

Bmin = 650 Kg/hr

Bact = Bmin*1.5
= 650Kg/hr *1.5
Bact = 975 Kg/hr
Operating Line Equation for Actual counter current extraction

Y1act = 0.243
Plot the value of Y1act in y-axis
By stepwise construction the number of stages can be determine as =6
No/ of theoretical plate =6
Types Of Extraction Equipment

Rotating Disc Contactor (RDC) Columns

Process description:
1. The two rotating disc contactors are the main units in this process.
2. As shown in the screenshot of the flow diagram, there are two streams entering the
columns, and two outlets.
3. The rotation of the discs enhances the mass transfer of the component(s) from one
phase to the other.
4. Besides the rotating discs columns, the pilot plant consists of vessels, pumps, valves,
pipeline and controllers.
5. The model of this separation process unit created by Mobatec fulfills all the specified
requirements and it is successfully up and running.
Liquid Extraction Unit-3 Mass Transfer-II
 6. One of the main challenges was not only to model the mass transfer of one component
from one liquid phase to the other defined as a function of the rotational speed,
7. To take into account the role played by the density difference when modeling the
relative movement of the phases inside the columns.

Characteristics
1. Limited efficiency due to axial back mixing
2. Suitable for viscous materials
3. Suitable for fouling materials
4. Sensitive to emulsions due to high shear mixing

Centrifugal Extractor
A centrifugal extractor—also known as a centrifugal contactor or annular centrifugal
contactor—uses the rotation of the rotor inside a centrifuge to mix two immiscible liquids
outside the rotor and to separate the liquids in the field of gravity inside the rotor. This way, a
centrifugal extractor generates a continuous extraction from one liquid phase (fermentation
broth) into another liquid phase (organic solvent).
WORKING OF CENTRIFUGE
Two immiscible liquids of different densities are fed to the separate inlets and are
rapidly mixed in the annular space between the spinning rotor and stationary housing. The
mixed phases are directed toward the center of the rotor by radial vanes in the housing base.
As the liquids enter the central opening of the rotor, they are accelerated toward the wall. The
mixed phases are rapidly accelerated to rotor speed and separation begins as the liquids are
displaced upward. A system of weirs at the top of the rotor allow each phase to exit the rotor
where it lands in a collector ring and exits the stage. Flow from between stages is by gravity
with no need for inter-stage pumps. The centrifugal contactor thus acts as a mixer, centrifuge
and pump.

Liquid Extraction Unit-3 Mass Transfer-II

Configuration Of Centrifuge
1. Mix and separation.
2. Separation by direct feed.
3. Multi-stage processing.
Mix and separation.
The mix & separation configuration is the standard operation for centrifugal
contactors used for liquid-liquid extraction processes. The two liquids (typically an aqueous
phase (heavy) and an organic phase (light)) enter the annular mixing zone where a liquid-
liquid dispersion is formed and extraction occurs as solutes (e.g. dissolved metal ions) are
transferred from one phase into the other. Inside the rotor, the liquids will be separated into a
heavy (blue) and a light (yellow) phase by their respective densities. This proportion of each
phase (phase ratio), total flow rate, rotor speed, and weir sizes are varied to optimize
separation efficiency. The separated liquids are discharged without pressure and flow by
gravity to exit the stage
Separation by direct feed.
For applications requiring only separation of a pre-mixed dispersion (e.g. oil/water
separation in environmental cleanup), the direct feed offers the option to feed the mixed
liquid stream at a low sheer force directly into the rotor. Inside the rotor, the liquids will be
separated into a heavy (blue) and a light (yellow) phase. This principle is used to optimize the
separation efficiency. The separated liquids will be discharged without pressure
Multi-stage processing.
Typically for solvent extraction processes in stage-wise equipment such as the
centrifugal contactor, we would have multiple contactors in series for extraction, scrubbing,
and stripping (and perhaps others). The number of stages needed in each section of the
process would depend on process design requirements (necessary extraction factor). In this
case, four interconnected stages provide a continuous process in which the first stage is a
decanting stage. The next two stages show a counter current extraction. The last stage is
neutralization as a cross stream interconnection.
Mixed settlers equipment

Liquid Extraction Unit-3 Mass Transfer-II

Liquid Extraction Unit-3 Mass Transfer-II
 Pulse Column

Liquid Extraction Unit-3 Mass Transfer-II

Liquid Extraction Unit-3 Mass Transfer-II