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Liquid-liquid extraction
ChE 4M3
Kevin Dunn, 2013
kevin.dunn@mcmaster.ca
http://learnche.mcmaster.ca/4M3
Overall revision number: 256 (November 2013)
1
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D
A
=
0
R
0
E
RT
=
chemical potential dierence
(R)(temperature)
6
Where/why LLE is used
Where?
Bioseparations
Azeotrope-forming mixtures
7
Extractor types: 3 major steps required
1. Mixing/contacting:
Cocurrent mixer-settlers
mix: impellers
mix: nozzles
settle: ultrasound
settle: centrifuges
2. Column-type units contain:
(a) nothing or
(e) agitation
3. Rotating devices
Important point: LLE is an equilibrium-limited separation (as
opposed to rate-limited separations seen up to now).
13
Mixer-settlers
[Richardson and Harker, p 745] Common in mining industry: requirements
40000 L/min ows
14
Mixer-settlers
KnitMesh coalescer: consistency of steel wool
[Richardson and Harker, p 747]
15
Horizontal gravity settling vessel
[Seader, 3ed, p302]
16
Spray columns: separation principle is gravity
[Richardson and Harker, p 751]
17
Tray columns
[Richardson and Harker, p 749]
coalescence on each
tray
breaks gradient
formation (axial
dispersion)
18
Tray columns with mechanical agitation
shearing to create
dispersion
mixture = K
PK
KQ
=
mass Q
mass P
The converse
applies also:
when a settled
mixture
separates into
P and Q
Applies
anywhere:
even in the
miscible region
27
Q1: Using the lever rule
Which is a more exible system: (a) or (b)?
C = water (carrier)
S = furfural (solvent)
AIM: to remove ethylene glycol (solute) from water (carrier) into
solvent (furfural)
1. Calculate the mixture composition, M
2. Calculate the equilibrium compositions in E
1
and R
1
Note: extract is dened as the solvent-rich stream leaving the system
42
43
Solution: Phase diagram: furfural, water, ethylene glycol
Feed Solvent
F = 100 kg S = 200 kg
x
F,A
= 0.45 x
S,A
= 0.0
x
F,C
= 0.55 x
S,C
= 0.0
x
F,S
= 0.00 x
S,S
= 1.0
C = water (carrier)
S = furfural solvent
M = 300kg; x
M,A
= 0.15; x
M,C
= 0.18; x
M,S
= 0.67
R
1
= 82kg; x
R
1
,A
= 0.33; x
R
1
,C
= 0.57; x
R
1
,S
= 0.10
E
1
= 218kg; y
E
1
,A
= 0.09; y
E
1
,C
= 0.04; y
E
1
,S
= 0.87
44
Recap: Cross-ow arrangements
N = 3 in this illustration
[Schweitzer, p 1-263]
n
(y
E
n
)(E
n
)
N
n
E
n
45
Review from last time
46
Review from last time
47
Review from last time
48
Cross-current vs counter-current
Cross-current (N = 2 stages) Counter-current (N = 2 stages)
(Only 2 in illustration)
In general: y
E
1
> y
E
2
> . . .
Recovery = 1
(x
R
N
)(R
N
)
(x
F
)(F)
Concentration = y
E
1
R
1
is on the line that connects E
2
and P
R
2
is on the line that connects S and P
53
Counter-current graphical solution: 2 units
Step 1
Feed Solvent
F = 250 kg S = 100 kg
x
F,A
= 0.24 x
S,A
= 0.0
x
F,C
= 0.76 x
S,C
= 0.0
x
F,S
= 0.00 x
S,S
= 1.0
Overall balance gives:
M = S +F = E
1
+R
2
For example, lets require x
R
2
,A
= 0.05 (solute concentration in ranate).
Given an S ow rate, what is y
E
1
,A
? (concentration of solute in extract) 54
Counter-current graphical solution: 2 units
Step 2
Note: the line connecting
E
1
to R
2
is not a tie line.
We use the lever rule and
an overall mass balance
(F +S = E
1
+R
2
) to
solve for all ows and
compositions of F, S, E
1
,
and R
2
.
y
E
1
,A
0.38 is found from an overall mass balance, through M.
Simply connect R
2
and M and project out to E
1
. 55
Counter-current graphical solution: 2 units
Step 3
Recall:
F = E
1
+P
F is on the line that connects E
1
and P
R
2
= S +P
R
2
is on the line that connects S and P
Extrapolate through these lines until intersection at point P.
56
Counter-current graphical solution: 2 units
Step 4
Once we have E
1
, we can start: note that in stage 1 the R
1
and E
1
streams leave in equilibrium and can be connected with a tie line. 57
Counter-current graphical solution: 2 units
Step 5
Again recall:
R
1
= E
2
+P
R
1
is on the line that connects E
2
and P
Since we have point P and R
1
we can bring the operating line back
and locate point E
2
58
Counter-current graphical solution: 2 units
Step 6
The last unit in a cascade is a special case: we already know
R
N=2
, but we could have also calculated it from the tie line with
E
2
. We aim for some overshoot of R
N
. (Good agreement in this example.)
59
In general: Counter-current units
F +E
2
= E
1
+R
1
E
2
+R
2
= E
3
+R
1
E
n
+R
n
= E
n+1
+R
n1
Rearrange:
F E
1
= R
1
E
2
R
1
E
2
= R
2
E
3
R
n1
E
n
= R
n
E
n+1
(F E
1
) = (R
1
E
2
) = . . . = (R
n1
E
n
) = (R
n
E
n+1
) = . . . = (R
N
S) = P
Notes:
1. each dierence is equal to P (the dierence between ows)
2. E
n
and R
n
are in equilibrium, leaving each stage [via tie line]
60
Counter-current graphical solution
1. We know F and S; connect with a
line and locate mixture M
2. Either specify E
1
or R
N
(we will
always know one of them)
3. Connect a straight line through M
passing through the one specied
4. Solve for unspecied one [via tie line]
5. Connect S through R
N
and
extrapolate
6. Connect E
1
through F and
extrapolate; cross lines at P
7. Locate P by intersection of 2 lines
8. In general: connect E
n
and R
n
via
equilibrium tie lines
61
Tutorial-style question
Consider a system for which you have been given the ternary
diagram (see next slides). A = solute, S = solvent (100% pure),
C = carrier. The feed, F enters at 112 kg/hr with composition of
25 wt% solute and 75 wt% carrier.
1. Calculate the ow and composition of the extract and ranate from:
Show the construction on the ternary diagram for the number of equili-
brium stages to achieve x
R
N
= 0.025, given a solvent ow of 28 kg/hr.
Plot on the same axes the concentrations in the extract and ranate
streams.
62
Tutorial solution: step 1
63
Tutorial solution: step 2
64
Tutorial solution: step 3
65
Tutorial solution: step 4
66
Tutorial solution: step 5
67
Tutorial solution: step 6
68
Tutorial solution: concentration prole
69
For practice (A)
70
For practice (B)
71
Counter-current graphical solution: 2 units
Step 3(b)
Recall:
F +P = E
1
R
2
+P = S
Thought experiment: What is the minimal achievable E
1
concentration? mentally move point M towards S. What happens
to P as solvent ow S is increased? Alternative explanation next.
72
Counter-current graphical solution: maximum solvent ow
Step 3(b)
Recall:
F +P = E
1
R
2
+P = S
Subtle point: minimal achievable E
min
1
concentration:
note that R
2
is xed (specied) in this example
73
Safety concerns
Liquid-liquid (solvent) extraction units safety concerns can be
reduced by:
feed organic phase from the bottom of tank, not the side, to
avoid splashing