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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

Copyright, sharing, and attribution notice

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Unported License. To view a copy of this license, please visit

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This license allows you:

to adapt - but you must distribute the new result under the

same or similar license to this one

commercial purposes

(when used without modication)

2

We appreciate:

All of the above can be done by writing to

kevin.dunn@mcmaster.ca

or anonymous messages can be sent to Kevin Dunn at

http://learnche.mcmaster.ca/feedback-questions

If reporting errors/updates, please quote the current revision number: 256

3

Liquid-liquid extraction (LLE)

[Flickr# 3453475667]

4

References

Chemical Engineers, chapter 1.9

3rd edition, chapter 8

5th edition, chapter 13

Principles, 4th edition, chapter 12.5 and 12.6

DOI:10.1002/14356007.b03 06.pub2

5

Denitions

y

E,A

= concentration of A, the solute, in extract.

We aim for the solute (A) to be mostly in the extract stream.

R,A

A

=

y

E,A

x

R,A

D

A

=

0

R

0

E

RT

=

chemical potential dierence

(R)(temperature)

6

Where/why LLE is used

Where?

Bioseparations

Why?

volatility)

Azeotrope-forming mixtures

7

Extractor types: 3 major steps required

1. Mixing/contacting:

2. Phase separation:

3. Collection of phases leaving the unit

8

What are we aiming for?

Main aims

R

and high y

E

)

E

)

How to achieve this?

Cocurrent mixer-settlers

solvent in extract stream

9

Co-, cross-, counter-current operations

[Hanson article, Chemical Engineering, posted to course website]

10

Some photos of equipment

[http://www.ickr.com/photos/51009184@N06/5062827346/]

11

Some photos of equipment

[http://www.rousselet-robatel.com/images/products/Mixer-settler-pic-2lg.jpg]

12

Equipment for LLE

1. Mixer-settlers (integrated unit)

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

layers of packing

(coalescence)

pulsate

[Seader, 3ed, p302]

19

Rotating devices

[Seader, 3ed, p 306]

Used when foams and emulsions would easily form: i.e. gentle

mass transfer.

Look up in your own time: centrifuge mixer-settlers

20

Linking up units (more on this later)

[Richardson and Harker, p 723]

21

Integration with downstream units

[Schweitzer, p 1-257]

22

Selecting a solvent

Schweitzer: The choice of solvent for a LLE process can often

have a more signicant impact on the process economics than any

other design decision that has to be made.

Which properties of a solvent inuence our aims with LLE?

23

Calculating the distribution coecient (in the lab only)

Mass balance:

Fx

F

+Sy

S

= Ey

E

+Rx

R

D =

y

E

x

R

If F = S = E = R and y

s

= 0, then

only measure x

R

:

D =

x

F

x

R

1 only in this special case

Once D is determined, we can obtain phase diagrams to

understand how the process will operate.

Also: see Perrys for many values of D

24

Triangular phase diagrams: from laboratory studies

[Flickr# 3453475667]

25

Using a triangular phase diagrams

[http://www.youtube.com/watch?v=gGYHXhcKM5s]

26

Lever rule

[Richardson and Harker, p 726]

Mix P and Q

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)?

F

)

Answer: range of feed concentrations (x

F

) is wider, i.e. more

desirable, for (a). Dierence between (a) and (b):

28

Q2: Using the lever rule

Mix a feed stream, F, containing C and A (i.e. x

F

) with a pure

solvent stream S (i.e. y

S

= 0). Composition of the mixture?

29

Q2 solution: Using the lever rule

Composition of the mixture? we need more information (e.g.

amount of F and S must be given to nd point M)

30

Q3: Going to equilibrium

Let that mixture M achieve equilibrium. What is the composition

of the ranate and extract?

31

Q3 solution: Going to equilibrium

What is the composition of the ranate and extract? Use the tie

lines [solid lines]; or interpolate between existing ones.

32

Q4: Altering ows

Recovery =

fraction of

solute

recovered

For 1 stage

1

(x

R

)(R)

(x

F

)(F)

Specically

1

(x

R,A

)(R)

(x

F,A

)(F)

Same system, but now lower solvent ow rate (to try save money!). What

happens to (a) extract concentration and (b) solute recovery?

33

Q4 solution: Altering ows

Recovery =

fraction of

solute

recovered

For 1 stage

1

(x

R

)(R)

(x

F

)(F)

Specically

1

(x

R,A

)(R)

(x

F,A

)(F)

(a) extract concentration increases: (A at E*) > (A at E): y

E

> y

E

(b) solute recovery drops: (A at R*) > (A at R): x

R

> x

R

34

Q5: Composition of the mixture, M?

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

Answer: M = x

M,A

= x

M,C

= x

M,S

=

35

Q5 solution: Composition of the mixture, M?

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

M = F +S

Answer: M = 350kg; x

M,A

= 0.17; x

M,C

= 0.54; x

M,S

= 0.29

36

Q6: Composition of the 2 phases leaving in equilibrium?

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

R

1

= x

R

1

,A

= x

R

1

,C

= x

R

1

,S

=

E

1

= y

E

1

,A

= y

E

1

,C

= y

E

1

,S

=

37

Q6 solution: Composition of the 2 phases in equilibrium?

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

M = E

1

+R

1

R

1

= 222kg; x

R

1

,A

= 0.10; x

R

1

,C

= 0.82; x

R

1

,S

= 0.08

E

1

= 128kg; y

E

1

,A

= 0.33; y

E

1

,C

= 0.06; y

E

1

,S

= 0.61

38

Link units in series

[Richardson and Harker, p 723]

Introduce fresh solvent each time

39

Q7: send ranate from Q6 to second mixer-settler

Question: how much solvent should we use in the second stage?

40

Q7 solution: send ranate from Q6 to second mixer-settler

Compare extract:

Compare volumes:

Answer: equilibrium from point B (most solvent), C, D (least solvent) will each be

dierent. Trade-o: higher extraction vs lower recovery

41

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)

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]

recovered

1

(x

R

N

)(R

N

)

(x

F

)(F)

solute leaving in each extract

stream, divided by total extract

ow rate

N

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)

streams

(Only 2 in illustration)

In general: y

E

1

> y

E

2

> . . .

stage

Recovery = 1

(x

R

N

)(R

N

)

(x

F

)(F)

Concentration = y

E

1

solvent ow?

You will have an assignment question to compare and contrast

these two congurations

49

What we are aiming for

General approach:

1. Use ternary diagrams to determine operating lines

2. Estimate number of theoretical plates or theoretical

stages

3. Convert theoretical stages to actual equipment size. E.g.

assume we calculate that we need N 6 theoretical stages.

do that, but costly)

6 counter-current mixer-settlers that fully reach equilibrium

stage

HETS number of theoretical stages

stage eciency

50

For example

[WINTRAY (Japanese company; newly patented design)]

51

Two counter-current units

Reference for this section: Seader textbook, 3rd ed, p 312 to 324.

Consider N = 2 stages for now. Steady state mass balance:

F +E

2

= R

1

+E

1

R

1

+S = R

2

+E

2

Rearrange:

F E

1

= R

1

E

2

R

1

E

2

= R

2

S

(F E

1

) = (R

1

E

2

) = (R

2

S) = P

Note: each dierence is equal to P (look on the ow sheet above

where those dierences are).

52

Counter-current graphical solution: 2 units

Rearranging again:

F = E

1

+P

R

1

= E

2

+P

R

2

= S +P

Interpretation: P is a ctitious operating point on the ternary

diagram (from lever rule)

1

and P

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:

2. For the overall 2-stage cross-current system, nd the:

3. The objective now is to have a counter-current system so the ranate

leaving in the N

th

stage, R

N

has y

R

N

= 0.025

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

neighbourhood

accumulate, when spills occur

[Courtesy of ALTA Solvent Extraction Short Course, Alan Taylor]

74

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