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Chapter Four

Extraction
Dr. Mohammed H. Al-Saleh
Department of Chemical Engineering
Jordan University of Science and Technology

General Introduction
2

In distillation:
The vapor and liquid phases are chemically similar
The separation is based on the relative volatility, which is a
physical property
In Extraction:
The 2 phases are chemically quite different
The separation is based on the physical and chemical properties

Why Extraction?
3

1. Close boiling point compounds vs. cost

Example: Acetic acid/water

2. Complex mixtures/heat sensitive

Pharmaceutical industry (Example: penicillin is extracted from a complex


mixture using butyl acetate)

3. Overlapping in boiling points

Example: mixtures of naphthenes, aromatics, and paraffins

4. Separation of Azeotropic mixtures

5. Separation of compounds present in small quantities

Effectiveness of Extraction
5

The effectiveness of any extraction process is mainly


based on the proper selection of solvent
The Solvent is typically:

Stable
Nontoxic
Noncorrosive
Inexpensive
Easily recoverable
The solute has strong affinity to it
Relatively immiscible with the carrier (better to be completely immiscible)
Have different density from the feed/carrier to facilitate phase
separation

L-L Equilibrium
6

Phase Rule
Assume a typical extraction unit where there is 2 phases and 3
components:



Variables we have
Temperature
Pressure
4 concentrations (2 in each phase)

Triangular Coordinates
C
xA=0.3 ; xB= 0.2

A
A
7

Equilibrium Data
Plate point
C

One phase region

Tie line

Two phase region

P
Phase a:
xA = 0.61
xB = 0.08
xC = 0.31

Phase b:
xA = 0.05
xB = 0.79
xC = 0.16

M
b

A
8

Two Immiscible Pairs

Example
A 100 kg mixture contains 10 kg Acetic acid (A), 60 kg water
(B) and 30 kg isopropyl ether (C); what are the raffinate and
extract layers Composition?
yc= 0.94
yA= 0.04

xA= 0.12 , xC=0.02 xB=

Extract layer
yC vs yA

0.9
0.8

yA= 0.04 , yC=0.94 yB=

0.7

xc, yc

0.6
0.5
0.4
0.3
0.2
0.1
0
0

10

xA=0.12
xc=0.02

0.1

0.2

0.3

xA , yA

0.4

0.5

Raffinate layer
xC vs xA

Extraction Equipment
11

Objective: to bring 2 liquids into intimate contact to get


the highest possible mass transfer rate (High turbulence
and high surface area are required)
Classes of Extraction equipments

Mixing by mechanical agitation

Mixing by liquids flow

Mixer Settler Unit

Must generate high interfacial area


Must provide high mass transfer coefficient
Low entrainment of air bubbles

Low aspect ratio, i.e. of flat geometry


Must allow coalescence and phase separation
Must allow easy collection of phases
12

Mixer Settler- Multistage

Extract

Solvent

1
Raf
ffina
Raffinate

Feed

Feed

Extracting
solvent

Extract
Raffinate

13

Differential Extractors
q

Continuous process
Feed and extracting solvent flow
past one another
One phase is dispersed in the
other

Contacting and phase separation


takes place within one unit
Phases are not in equilibrium
except locally i.e at the interface

14

Spay columns without packing

Random packing materials

Structured Packing

Spay columns with packing


15

Mechanical mixing is used for systems with:


High interfacial tension
Low difference in density
High viscosity
Extract
Feed

Extracting
solvent

Raffinate

16

Scheibel Column

Karr Column

Single Stage Extraction


17

Lever-Arm Rule
V +L=M

V, yA,yC

(I)

Vy A + LxA = MxAM

(II)

VyC + LxC = MxCM

(III)

Combining (I) and (II):

L y A - x AM
=
V x AM - x A

Combining (I) and (III):

L yC - xCM
=
V xCM - xC

xC - xCM xCM - yC
=
x A - x AM x AM - y A

M, xAM,xCM

L, xA,xC

L
xC xC
yC xCM M
yC V
yA xAM xA
xA,, yA

This means that points L, V and M must lie on a straight line.


Using the properties of similar triangles:

L VM
=
V LM

Similarly:

Operating Equation

And the equilibrium

18

L VM
=
M LV

Example
A single-stage extraction is performed in which 400 kg of a
solution containing 35 wt% acetic acid in water is contacted with

400 kg of isopropyl ether. Calculate:


1. The amount and composition of the extract and raffinate
2. The acetic acid percent of removal.

19

Solution

Acetic acid (A) -water (B)-isopropyl ether (C)


1.0
0.9

yc

0.8

xc, yc

0.7
0.6
0.5
0.4
0.3
0.2
0.1

M point
xc

0.0
0.0

0.1

yA

20

0.2

0.3

xA

0.4

0.5

xA , yA

0.6

0.7

0.8

0.9

1.0

Counter-current Multistage Extraction


M point
Vn
yAn

V1
yA1

21

Ln-1
xAn-1

Overall balance

N
LN
xAN

Ln
xAn

VN +1 + Lo = V1 + LN = M

..(1)

y AN +1VN +1 + xAo Lo = y A1V1 + xAN LN = xAM M

x AM =
Component
balance for
component C

VN+1
yAN+1

1
Lo
xAo

Component
balance for
component A

Vn+1
yAn+1

y AN +1VN +1 + x Ao Lo y A1V1 + x AN LN
=
VN +1 + Lo
V1 + LN

yCN +1VN +1 + xCo Lo = yC1V1 + xCN LN = xCM M


xCM =

M point

yCN +1VN +1 + xCo Lo yC1V1 + xCN LN


=
VN +1 + Lo
V1 + LN

Example
Pure solvent of isopropyl ether at a rate of VN+1= 600 kg/h is being
used to extract an aqueous solution of Lo=200 kg/h containing 30 wt%
Acetic acid by countercurrent multistage extraction. The desired exit

acetic acid concentration in the aqueous phase is 4%. Calculate the


compositions and amounts of the ether extract (V1) and aqueous
raffinate (LN). The equilibrium data from appendix A3.

22

Solution
VN+1=600 kg/h
yAN+1=0

V1 = ?
yA1 = ?

N
LN = ?
xAN = 0.04

Lo=200 kg/h
xAo=0.3

Mixture point

23

Acetic acid (A) -water (B)-isopropyl ether (C)

VN+1
1

xcM M=yc1V1+xCNLN

0.9

yA vs. yC

0.8

V1
yA1=0.08
yc1=0.88

0.75 (800)=0.88V1+0.02LN
M=V1+LN

0.7

M point

xc, yc

0.6

800=V1+LN

0.5

V1=680 kg/h
0.4

LN= 120 kg/h


0.3
0.2
0.1

LN

xA vs. xC

0
0

0.1

0.2

0.3

0.4

Lo
24

0.5
xA , yA

0.6

0.7

0.8

0.9

Counter-current Multistage Extraction


Stage to stage
25

V1
yA1

1
Lo
xAo
Balance of stage n

Rearrange

Ln-1
xAn-1

Ln-1 + Vn+1 = Ln + Vn

VN+1
yAN+1

Vn+1
yAn+1

Vn
yAn

Ln
xAn

LN
xAN

. (1)

Ln-1 - Vn = Ln - Vn+1 = D

Difference in flow is constant

This also holds for the component balance

DxD = xn-1Ln-1 - ynVn = xn Ln - yn+1Vn+1

. (2)
What does this equation imply?

Combine equations 1 and 2

xD =

xn-1 Ln-1 - ynVn xn Ln - yn+1Vn +1


=
Ln-1 - Vn
Ln - Vn+1

This gives the coordinates of G

Example

A feed of one thousand kilogram aqueous solution of pyridine per


hour (50% by mass) is to be extracted with pure benzene to
reduce the solute content in the raffinate to 2%. Determine the
number of ideal stages required if the solvent rate is 1.3 times
the minimum.

26

Solution
V1 = ?
yA1 = ?

VN+1=? kg/h
yAN+1=0
1

N
LN = ?
xAN = 0.02

Lo=1000 kg/h
xAo=0.5
VN+1=1.3 VN+1min

First of all we have to find the minimum solvent


flowrate (VN+1)min

27

Dmin

=0.295

OR

1.0 VN+1

xc, yc

0.8
V1min

0.6
0.4

Mmin

0.2
0
-0.2
28

0.0

LN

0.2

0.4

xA, yA

Lo

0.6

0.8

1.0

V1 = ?
yA1 = ?

VN+1=904 kg/h
yAN+1=0
1

N
LN = ?
xAN = 0.02

Lo=1000 kg/h
xAo=0.5
VN+1=1.3 VN+1min

M point

29

VN+1

1.0

V3
V2

xc, yc

0.8

V1

0.6
0.4

0.2
0
-0.2
30

0.0LN

L2

0.2

L1 0.4

xA, yA

Lo

0.6

0.8

1.0

Example
Pure isopropyl ether of 450 kg/h is being used to extract an
aqueous solution of 150 kg/h with 30wt% acetic acid by
countercurrent multistage extraction. The exit acid concentration
in the aqueous phase is 10 wt% calculate the number of stages:

31

Solution
VN+1=450 kg/h
yAN+1=0

V1 = ?
yA1 = ?
1
Lo=150 kg/h
xAo=0.3

N
LN = ?
xAN = 0.1

Mixture point

32

Acetic acid (A) -water (B)-isopropyl ether (C)


1
0.9
0.8
0.7

xc, yc

0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

xA , yA

33

1.4

1.0

xc, yc

0.8
0.6
0.4

0.2
0
-0.1

0.1

0.2

xA , yA
34

0.3

0.4

0.5

Counter-current Multistage Extraction


Immiscible System
35

Example

Pure trichloroethane is being used to extract acetone from an


acetone/water mixture containing 10 wt% acetone and flows at a rate
of 500 kg/h in a counter-current process at 25 oC. It is desired to
decrease the concentration of acetone in the raffinate stream to 0.5

wt%. If water and trichloroethane can be assumed immiscible liquids,


find:
A) Minimum Solvent flowrate?
B) Number of stages required if the solvent flowrate is 1.5 times
the minimum flowrate

36

Solution

a) Minimum Solvent Flowrate?


0.25

0.2

yA1 (max)

0.15

0.1

0.05

0
0.000

0.020

0.040

0.060

0.080

0.100

0.120

0.140

37

xAN

xAo

0.25

0.2

0.15

0.1

0.05

0
0.000

0.020

0.040

0.060

0.080

38

0.100

0.120

0.140

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