tugas#3 - liquid-liquid extraction (tayangan#)
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TUGAS KELOMPOK:
MEMBUAT TAYANGAN
(PPT)
Kalian diminta untuk membuat TAYANGAN yang berbasis dari contoh tayangan berikut ini.
Untuk keperluan kalian, diharapkan kalian dapat menambahkan bahan-bahan lain yang
terdapat pada referensi-referensi lainnya, termasuk yang dimiliki oleh kelompok-kelompok
lainnya (PAGI atau pun SIANG).
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11 Liquid-liquid Extraction
A liquid mixture (e. g. A+B) is treated
with a solvent S (extractant) in which
one or more of the desired components is
preferentially soluble.
The separation of compounds is based on
differences in solubilities
[distribution of components between
(partially) immiscible liquid phases].
11.1 Introduction
11.1.1 Extraction processes
physical operation
depends on the solubilities
in two (partially) immiscible liquids
chemical operation
chemical reaction occurs,
with higher selectivity
Requirement for the solvent in physical
extractions:
(1) the solvent S and liquid-mixture are at
least partially if not completely
immiscible;
(2) its solubilities for components aredifferent.
A+B S
A
A single stage batch extraction:
Subsequent separation process:
distillation, crystallization, reextraction,
solvent S extract E
(S+A+B)
yA, yB
feed F
(solute A +
diluent B )
raffinate R
(B+A+S)xA, xB
B
A
B
A
x
x
y
y>
Extraction is preferable in the following
cases:
(1) when the relative volatility is near unity,
or when the azeotrope is formed;
(2) when the concentration of less volatile
components is low;
(3) when heating must be avoided; and
(4) when the components to be separated
are quite different in nature.
Factors to be considered for selecting
solvent:
(1) solubility
(2) selectivity
(3) subsequent separations
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11.1.2 Contact between two phases
differential contacting equipment
e. g., packed columns, pulsed columns,
spray towers.
stagewise equipment
e. g., mixer-settler units
11.2 Equilibrium of Ternary Systems and
Principle of Extraction
xS = 0.3
xA+xB +xS = 1
x mass fraction S0.2 0.4 0.6 0.8
xS
xA
xB
M
A
0.8
0.6
0.4
0.2
B
11.2.1 Triangular diagram
1. Triangular diagram
0.2
0.4
0.8
0.6
xA = 0.4
xB = 0.3
2. Lever rule
Two liquid mixtures
R kg (xA
,xB
,xS
) and
E kg (yA
,yB
,yS
) are
mixed to form a
mixture
Mkg (zA
,zB
,zS
). S
A
B xS
RxA
yA E
yS
M
zS
zA
Lever rule:
(1) M, E, and R are along the same line;
(2) the mass ratio of mixtures equals to the
length ratio of
line segments.
ME
MR
R
E
=
,RE
MR
M
E=
RE
ME
M
R=
S
A
B xS
RxA
yA E
yS
M
zS
zA
When the solvent S is mixed with the
binary mixture F (A+B) , point M must be
on line SF, and its position is determined by
the lever rule.
S
A
B
MS
MF
F
S=
(11-26)
On the line SF, the mass
ratio of A and B is the same.
FM
11.2.2 Equilibrium of partially misciblesystems
Liquid mixture: solute A + solvent B
New solvent S
Types of ternary mixture:
(1) S may be completely immiscible with
the original solvent B.
(2) S may be partially miscible with B.
(3) S and B, S and A form two partially
miscible liquids.
I
II
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1. Solubility curve, tie line, and plait point
plait point P
conjugate phasesE and R areconnected by thetie line.
P
A
SB
solubility curve
homogeneous
phase
tie line
R0 E0
R1E1
M1
two-phase region
Solubility curve:
Extract on the RHS of pint P
ys = (yA ) (11-9)
Raffinate on the LHS of pint P
xs = (xA ) (11-10)
P
A
SB R0 E0
2. Distribution coefficient and
distribution curve
Distribution curve
yA =f (xA ) (11-8)
Distribution coefficient
A
A
x
y=
(11-6)
kA =mass fraction of A in extract .
mass fraction of A in raffinate
yA
xA0
y = x
P
11.2.3 Phase equilibrium and extraction
operation
1. Single-stage extraction process
solventrecovery
purified extract
E,yA
purified raffinate
R,xA
feed F
solvent S
SB
A
ERR
E
F
extract E
raffinate R
M
2. Selectivity ratio of solvent
Binary systems:
B
A
BA
BA
k
k
xx
yy=
/
/
(11-11)
oo
oo
BA
BA
xx
yy
/
/=
or (11-12)
o
o
o
A
AA
x
xy
)1(1 (11-13)
, = 1, separation by
extraction is impossible.
Note:
distribution coefficientk
phase equilibrium
selectivity ratio
separability by extraction
o
o
o
A
AA
x
xy
)1(1
(11-13)
SB
A
R
E
FM
oo
AA xy=When
E
R
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3. Effect of miscibility of original solvent Band extractant S
small miscibility
larger two-phase region
, better result of separation
lower temperature
miscibility
, surface tension .
11.3 Calculation for an Extraction Process
11.3.1 Mathematical description
1. Material balance
Stage m:
Rm1,xm1, A,xm1, S Rm ,xm, A,xm, S
mEm ,ym, A,ym, S Em+1,ym+1, A,ym+1, S
Total material balance:
Rm1 +Em+1 =Rm +Em
Material balance for solute A:
Rm1xm1, A +Em+1ym+1, A =Rmxm, A +Emym, A
Material balance for solvent S:
Rm1xm1, S +Em+1ym+1, S =Rmxm, S +Emym, S
Rm1,xm1, A,xm1, S Rm ,xm, A,xm, S
mEm ,ym, A,ym, S Em+1,ym+1, A,ym+1, S
2. Equilibrium stage and stage efficiency
Equilibrium stage:
The compositions of the two streams
leaving the stage are in equilibrium,
no mater what composition they have
when they enter the stage.Rm1,xm1, A,xm1, S Rm ,xm, A,xm, S
mEm ,ym, A,ym, S Em+1,ym+1, A,ym+1, S
A problem of extraction may beconsidered from two aspects:
equilibrium stage
it is independent of equipment and
may be calculated first.
stage efficiency
it depends on the equipment, determined
experimentally.
actual number of stages
= equilibrium stage/efficiency
11.3.2 Single-stage extraction
For design:
given:F,xFA
specify:xA
select:zA,zS
calculate: S,E,yA,yS,
R,xS.
For operation:
given:F,xFA
S,zA,zS
calculate:E,yA,yS,
R,xA,xS.
F, xFA
S, zA, zS
R, xA, xS
E, yA, yS
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1. Analytical method
Six unknowns are solved from 6
equations.
Phase equilibrium relationship:
yA =f (xA ) (11-8)
ys = (yA ) (11-9)
xs = (xA ) (11-10)
Total material balance:
F + S =R +E =M (11-20)
Material balance for solute A:
xFA+SzA =RxA+EyA =MxMA (11-21)
Material balance for solvent S:
SzS =RxS+EyS (11-22)
2. Graphical method
(1) Draw the solubility
curve.
(2) Locate points F and
S, and the mixture
M is on the line FS.(3) Locate point R byxA,
find the tie line RE by interpolation,
M is the intersection of lines RE and FS.
R
A
SB
E
M
F
xA
?
A
P E3R3
R2R1
SB
E2
E1
Find the tie line RE:
(a) By estimation;
(b) By auxiliary
curve.
E
R
?
(4) Determine the flowrates of streamsby material balance and lever rule
Total material balance:
M=F + S
R
A
SB
E
M
F
xA
MS
MF
F
S=
R =ME
RE
MRME
=
(5) Find the composition in the extractyAandyS , and the concentration of solvent
in the raffinatexS.
R =F E
are the amount of
purified extract and
raffinate, respectively. xS
E
R
yS
yA
=
ER
FRFE
R
A
SB
E
M
F
xA
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Or: the flowrates of streams may be
obtained by material balance only,
in whichxFA is given,xA is specified,zA is
selected, andxMA andyA are found from the
phase diagram.
AMA
MAFA
zx
xxFS
=
AA
AMA
xy
xxME
=
3. Range of separation in a single-stage
extraction and the limit in the amount of
extractant
Point c:
the maximum amount
of solvent Smax .
Correspondingly,
in raffinate:xA, min
in purified raffinate:xA,min
A
SB
E
M
FxF,A
R co
min,Axo
min,Ax
Point d:
the minimum amount of solvent Smin .
The amount of
solvent used for
operation:
Smin < S < Smax
In general,
S = (1.1 2.0)Smin xA,min
A
SB
E
M
FxF,A
R co
min,Ax
d
Draw a line tangent
to the solubility curve
through point S, we
obtain the maximum
concentration in the
purified extract,o
max,Ay
o
max,Ay
xA,min
A
SB
E
M
FxF,A
R co
min,Ax
d
11.3.3 Multi-stage crosscurrent extraction
for single-stage extraction,
but the amount of liquid
mixture in each stage is
usually different.
Features:
the concentration of solute
is low in the raffinate, and
the amount of solvent is
large.
1
2
3
S E1
S E3
S E2
F
R1
R3
R2
The calculation is the repeat of that 11.3.4 Multistage countercurrent extraction
Higher extract rate may be obtained with
less extractant.
Calculation:
amount of solvent, number of equilibrium
stages, amount and concentration of
streams leaving each stage.
Method of stage-to-stage:
analytical or graphical
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11.3.5 Calculation for extraction with
completely immiscible solvents
1. Representation of composition and phase
equilibrium
X mass ratio in raffinate
(kg solute/kg diluent )
Y mass ratio in extract
(kg solute/kg solvent )
Equilibrium relationship:
Y=KX (11-35)
K distribution coefficient, generally
dependent upon concentration.
2. Single-stage extraction
B amount of original solvent
S amount of pure solvent
Z
mass ratio of A in extractant
Material balance for solute A:
S(YZ) =B(XF X) (11-36)
feed B, XF
solvent S, Z
extract S, Y
raffinate B, X
Equilibrium relationship:
Y=KX (11-35)
Material balance for solute A:
S(YZ) =B(XF X) (11-36)
For givenB,XF andZ, specify one variable
among S, YandX, other two may be
calculated.
3. Multistage crosscurrent extraction and
countercurrent extraction
11.3.6 Extraction with reflux
High purity may be achieved.
11.3.7 Differential contacting
countercurrent extraction
The diameter of column depends on the
flowrates and velocities of two phases.
The height of column may be obtained by
calculating the number of transfer unit or
HETS.
Exercises: 11 1, 3, 5
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11.4 Extraction Equipment
Requirement:
bringing the feed mixture and the solvent
into intimate contact
separation of the resulting two phases
11.4.1 Types of extraction equipment
stagewise contactors
differential contactors
Both may be with or without the addition
of external energy.
Stagewise contactors:
mixer-settler unit
sieve-plate column
Differential contactors:
1. spray tower
2. packed column
3. pulsed packed column
pulsed sieve column
4. vibrational sieve plate column
5. rotary disc column
6. centrifugal extractor
11.4.2 Flooding in extraction equipment
and limit of velocity
The performance of equipment is mainly
determined by:
allowable flowrates of two phases (D)
rate of mass transfer (H)
The superficial velocities of two phases at
which the flooding occurs are the limit for
the velocities.
11.4.3 Rate of mass transfer in extraction
equipment
Factors affecting mass transfer:
(1) drop size and size distribution of
dispersed phase
(2) circulation inside drops and interfacial
disturbance
(3) axial mixing in the equipment
11.4.4 Selection of extraction equipment
Following factors are to be considered:
the number of stages required
production capacity
properties of the materials
residence time
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11.5 Supercritical Fluid Extraction and
Liquid Membrane Extraction
11.5.1 Supercritical fluid extraction
1. Principle
It is an extraction process in which a
supercritical fluid is used as the solvent.
Supercritical fluid:
viscosity that of gas
density and solubility
those of liquid
diffusivity >> that in liquid
S
criticalpoint
t
pSFL
G
2. A process of supercritical extraction
CO2 is compressed as a supercritical
fluid, and used as an extractant.
reducing valveextractfeed
extraction
productraffinate SF
compressor
11.5.2 Liquid membrane extraction
(
separation )
The extraction and reverse extraction
are carried out simultaneously.
(a) make an emulsion by dispersingaqueous drops (in m) into an organic
phase (W/O);
(b) disperse the
emulsion into the
aqueous phase
(in 0.11 mm)
(W/O/W).
liquid
membrane
external
phase
internal
phase
A
B
Or: with O/W/O system.
Extraction with supported membrane:
The liquid
membrane phase
is retained in a
porous medium.liquid
membrane
lyophilic
porous
membrane
recovery
phase
original
liquid
A