03 Script Examples Extraction PDF
03 Script Examples Extraction PDF
Solvent
Feed
Mixer
Raffinate
Separator
Extract
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse -2-
Two mixtures R and E, which contain both the three compounds A, B, and C, have to
mixed in the ratio 1:2. This ternary system has no miscibility gap so that all
compounds are completely soluble each other. The mixture R has a composition of
x A , R = 0,7 and x B , R = 0,2 ; the mixture E exists of x A , E = 0,1 and x B , E = 0,5 .
Please determine:
a) The points R and E in the triangle diagram and the concentration of the
active agent C and
b) the mixing point (calculation and graphical determination).
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse -3-
For a partial solubility of substances A and B, which is essential for extraction, all
three compounds have to be taken into account for drawing of the phase equilibrium.
For this reason triangle co-ordinates are used, where each of the vertexes represents
the pure compounds. Points at the triangle side represent the composition of the
binary system and points inside the triangle the composition of the ternary system.
The representation of a ternary point is based on the fact that the sum of the normal
distances in a equal sided triangle is corresponding to the height of the triangle. If the
height of the triangle is set 100% so result the concentrations of the single
compounds from the normal distances (see figure).
xC , R = 0,1 xC , E = 0,4
b) Mixing point
If two mixtures with given composition in the triangle diagram are mixed then the
resulting mixing point lays on the connection line between these two points. The
position of the mixing point can be calculated by a mass balance or graphically by the
use of the law of balance.
Calculating:
Total balance:
R+ E = M
R ⋅ xC , R + E ⋅ xC , E
xC , M =
R+ E
R 1
with = the mass R and E can be eliminated, which results in
E 2
0,5⋅ xC , R + xC , E
xC , M =
1,5
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse -5-
xC , M = 0,3
Graphically:
Law of balance:
RM E
=
ME R
R 1 ME 1
with = follows =
E 2 RM 2
From the diagram the length of the distance RE can be determined with 77 mm.
77 − RM
RE = RM + M E ⇒ 0,5 =
RM
RM = 51,3 mm
Drawing this length in the diagram results the mixing point M and the concentrations
of the compounds can be determined.
x A , M = 0,3
x B , M = 0,4
xC , M = 0,3
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse -6-
Triangle diagram
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse -7-
A waste water from a process is loaded with acetone, which should be extracted with
chlorobenzene.
The equilibrium data for the ternary system water / acetone / chlorobenzene are
given.
a.) the triangle diagram including the phase equilibrium line and connodes.
b.) The water and chlorobenzene content of the aqueous phase (raffinate) with an
acetone concentration of 45 % and of the coexisting phase.
In the for the extraction interesting heterogeneous region a mixture splits in raffinate
and extraction phase along a connode, which connects the two coexisting phases.
The higher the amount of the active agent (extractable substance C) is the shorter
the connodes become until they melt to one point, the critical point K. By this critical
point K the binodal curve is split into two parts. Normally the part on the left side
represents the raffinate phase R, which has a low content of solvent B, and the right
side represents the solvent rich extract phase E.
According to the given table the coexisting phases (connodes) are given which can
now be drawn in the triangle diagram. One line in the table corresponds to one
connode.
Connecting these two points gives the first connode and analogous for the other
given data. The last row corresponds to the critical point K. By connecting all raffinate
and all extract points the result is the binodal curve.
the active agent C and crossing this with the binodal curve at the left side gives the
point of the aqueous phase, so that the concentrations of water and chlorobenzene
can be determined.
w A , R = 0,535 w B , R = 0,015
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse -9-
Possibility 1:
By interpolation between the two connodes next to the point the connode through the
given point can be constructed, but in a very inaccurate way.
Possibility 2:
With the help of the conjugation line the connode can be determined better and with
higher accuracy. For this purpose the right and left triangle side has to be shifted
parallel through the points of the connodes and the crossing of these two lines
represents one point of the conjugation line. All these by this way constructed point
and the critical point have to be connected to the conjugation line.
The searched coexisting phase can be constructed analogous: parallel shifting of the
right triangle side through R, crossing with the conjugation line and crossing of the
parallel shifted left triangle side through the point on the conjugation line with the right
side of the binodal curve.
The by this way determined concentrations are:
w A , E = 0,04 w B , E = 0,41 wC , E = 0,55
This point of the binary mixture has to be connected with the point C, pure acetone,
and somewhere on this line the mixing point must be. The boundary between one
and two phase region is the binodal curve. Therefore the searched mixing point M
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 10 -
can be determined by crossing the line GC with the binodal curve. The necessary
amount of acetone can be determine by the law of balance.
CM = 40 mm M G = 69 mm CG = 109 mm
G CM 200 40
= Æ =
C MG C 69
C = 345 g
w B , M = 0,25 wC , M = 0,75
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 11 -
Triangle diagram
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 12 -
The basic mixture of 100 kg exists of 40 mole% acetone and 60 mole% water and
has to be extracted with trichloroethane, which is preloaded with 15 mole% acetone.
Your have to determine:
a) the phase diagram of the system acetone / water / trichloroethane in the
triangle diagram.
b) the minimum and maximum amount of solvent,
c) the necessary amount of solvent, if the raffinate contains 4,82 mole%
acetone,
d) the amount and composition of the produced raffinate and extract,
e) the extraction process in the triangle diagram
Drawing of the single connode points analogous to example 2 and constructing the
connodes and combining the single point to the binodal curve.
The critical point was not drawn because the composition is not given and therefore
the exact position is not defined.
solvent:
xC , L = 0,15 x B , L = 0,85
The mixing point M has to be on the line between these two points F and L and M
has to be in the two phase region, because for extraction the mixture has to separate
in two phases. The minimal and maximal amount of solvent ( M min and M max ) are
the two crossings of the connection line FL with the binodal curve. By the length,
which can be determined from the diagram, the searched amounts can be calculated.
M min = 4,57 kg
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 14 -
FM max 91,5 − 2
M max = F ⋅ = 100 ⋅
M max L 2
M max = 4.475 kg
FM 91,5 − 45,5
L = F⋅ = 100 ⋅
ML 45,5
L = 1011
, kg
Extract E:
x A , E = 0,0503 x B , E = 0,5901 xC , E = 0,3596
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 15 -
amount of raffinate:
total balance: E + R = F + L = 100 + 1011
, = 2011
, kg
RM E
law of balance: =
ME R
RE = 95 mm ME = 26 mm
2011
,
R=
95 − 26
+1
26
R = 55 kg
amount of extract:
E= F+ L− R
E = 146,1 kg
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 16 -
From 2.000 kg/h of an acetic acid / water mixture with 45 wt% acetic acid the acetic
acid has to be extracted by a multi step cross flow extraction at an operation
temperature of 20°C. The residual concentration of acetic acid has to be 10 wt% and
the used solvent isopropyl ether is free of acetic acid.
b) the necessary number of theoretical steps in the triangle diagram for the case that
a solvent ration L& F& S of 1 is chosen and in every step the same amount of
solvent is added.
In the single steps equilibrium between raffinate and extract is reached so that the
compositions can be determined in the triangle diagram.
First the equilibrium data have to be drawn and the binodal curve with the given
connodes has to be constructed.
Then the point of the feed F and of the solvent L is drawn. The mixing point M1 has to
be on the connection line FL . For the minimum amount of solvent the crossing point
Mmin at the raffinate side of the binodal curve is significant. From the law of balance
results :
The mixing point M1 of the first step can be determined by calculation or graphically.
Calculation:
L& FM 1 wC , F − wC , M 1 0,45 − wC , M 1
& = = = = 0,55 ⇒ wC , M 1 = 0,29
F M 1L wC , M 1 − wC , L wC , M 1 − 0
Graphically:
The length of FL is 173 mm and ha to divided according the ratio L& F& = 0,55 .
FM 1 + M 1 L = 173 mm
0,55⋅ M 1 L + M 1 L = 173 mm
173
M1L = = 111,6 mm
1,55
Amount of the mixing point:
M& 1 = F& + L& = 2.000 + 1100
. = 3100
. kg h
The connode through the mixing point M1 gives the extract E1 and the raffinate R1.
The according compositions can be taken from the diagram.
wC , E1 = 0,21 wC , R1 = 0,355
raffinate flow:
R& 1 wC , M 1 − wC , E1
=
M& 1 wC , R1 − wC , E1
(
M& 1 ⋅ wC , M 1 − wC , E1 ) . ⋅ ( 0,29 − 0,21)
3100
R& 1 = = = 1710
. ,3 kg h
wC , R1 − wC , E1 0,355 − 0,21
extract flow:
E& 1 = M& 1 − R& 1 = 3100
. − 1710
. ,3 = 1389
. ,7 kg h
2. step
For the second step the flow rate of the solvent isopropyl ether is also 1.100 kg/h.
L& R1M 2 .
1100
= = = 0,643
R& 1 M2L . ,3
1710
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 20 -
R1M 2 + M 2 L = 167 mm
0,643⋅ M 2 L + M 2 L = 167 mm
167
M2L = = 101,6 mm
1,643
amount of mixing point:
M& 2 = R& 1 + L& = 1710
. ,3 + 1100
. = 2.810,3 kg h
concentrations:
wC , E2 = 0,14
wC , M 2 = 0,215
wC , R2 = 0,29
raffinate flow:
(
M& 2 ⋅ wC , M 2 − wC , E2 ) 2.810,3⋅ ( 0,215 − 0,14)
R& 2 = = = 1405
. ,15 kg h
wC , R2 − wC , E2 0,29 − 0,14
extract flow:
E& 2 = M& 2 − R& 2 = 2.810,3 − 1405
. ,15 = 1405
. ,15 kg h
3. step
L& R M 1100
.
& = 2 3= = 0,783
R2 M 3L 1405
. ,15
R2 M 3 + M 3 L = 171 mm
0,783⋅ M 3 L + M 3 L = 171 mm
171
M 3L = = 95,9 mm
1,783
amount of mixing point:
M& 3 = R& 2 + L& = 1405
. ,15 + 1100
. = 2.505,15 kg h
concentrations:
wC , E3 = 0,097 wC , M 3 = 0,16 wC , R3 = 0,225
raffinate flow:
(
M& 3 ⋅ wC , M 3 − wC , E3 ) 2.505,15⋅ ( 0,16 − 0,097)
R& 3 = = = 1233 kg h
wC , R3 − wC , E3 0,225 − 0,097
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 21 -
extract flow:
E& 3 = M& 3 − R& 3 = 2.505,15 − 1233
. = 1272,15 kg h
4. step
L& RM 1100
.
& = 3 4= = 0,892
R3 M4L 1233
R3 M 4 + M 4 L = 175 mm
0,892 ⋅ M 4 L + M 4 L = 175 mm
175
M4L = = 92,5 mm
1,892
amount of mixing point:
M& 4 = R& 3 + L& = 1233
. + 1100
. = 2.333 kg h
concentrations:
wC , E4 = 0,07 wC , M 4 = 0,117 wC , R4 = 0,173
raffinate flow:
(
M& 4 ⋅ wC , M 4 − wC , E4 ) 2.333⋅ ( 0,117 − 0,07)
R& 4 = = = 1064
. ,6 kg h
wC , R4 − wC , E4 0,173 − 0,07
extract flow:
E& 4 = M& 4 − R& 4 = 2.333 − 1064
. ,6 = 1268
. ,4 kg h
5. step
L& R4 M 5 1100
.
= = = 1,033
R& 4 M5L 1064
. ,6
R4 M 5 + M 5 L = 180 mm
1,033⋅ M 5 L + M 5 L = 180 mm
180
M5L = = 88,54 mm
2,033
amount of mixing point:
M& 5 = R& 4 + L& = 1064
. ,6 + 1100
. = 2.164,6 kg h
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 22 -
concentrations:
wC , E5 = 0,045 wC , M 5 = 0,084 wC , R5 = 0,128
raffinate flow:
(
M& 5 ⋅ wC , M 5 − wC , E5 ) 2.164,6 ⋅ ( 0,084 − 0,045)
R& 5 = = = 1017,1 kg h
wC , R5 − wC , E5 0,128 − 0,045
extract flow:
E& 5 = M& 5 − R& 5 = 2.164,6 − 1017,1 = 1147,5 kg h
6. step
L& R5 M 6 1100
.
= = = 1,082
R& 5 M6L 1017,1
R5 M 6 + M 6 L = 183 mm
1,082 ⋅ M 6 L + M 6 L = 183 mm
183
M6L = = 87,9 mm
2,082
amount of mixing point:
M& 6 = R& 5 + L& = 1017,1 + 1100
. = 2117,1 kg h
concentrations:
wC , E6 = 0,033 wC , M 6 = 0,06 wC , R6 = 0,094
raffinate flow:
(
M& 6 ⋅ wC , M 6 − wC , E6 ) 2.117,1⋅ ( 0,06 − 0,033)
R& 6 = = = 937,1 kg h
wC , R6 − wC , E6 0,094 − 0,033
extract flow:
E& 6 = M& 6 − R& 6 = 2.117,1− 937,1 = 1180 kg h
The concentration of the raffinate of this 6. step is lower than the necessary
concentration so that the extraction can be stopped.
N th = 6
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 23 -
The acetic acid / water mixture of example 4 has to be extracted in a multi step
countercurrent extraction cascade with isopropyl ether as solvent. The residual acetic
acid concentration is also given with 10 wt%.
construction:
wC , F = 0,45 wC , E1 = 0,227 wC , Emax = 0,291
The mixing point M is given by the ratio of feed F and solvent B and has to be on the
connection line FB . The amount of the mixing point M can be determined by a total
balance:
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 25 -
. . . . .
= + =
M F B R n E1+
The point E1 has to be on the binodal curve and on the connection line R n M .
The points F and E1 are connected by the upper pole line. F represents the feed,
which enters the first extraction step and E1 is the extract which leaves this first step.
The lower pole line is given by the connection of the solvent L and the raffinate Rn
leaving the extraction plant.
For the case that the first extraction step is a theoretical step the leaving phases
have to be in equilibrium. R1 as point of the leaving raffinate phase R& 1 , has to be on
the binodal curve and has to be on a connode through the extract E1.
The raffinate phase R& 1 and the extract phase E& 2 contact in the next extraction step.
The point E2 of the extract phase E& 2 has to be on the binodal curve and further on
Doing the construction for all points R2, R3 … and E3, E4 by this method finally the
necessary number of theoretical steps Nth for the extraction can be determined.
N th = 6,5
For the calculation of the amounts of Ei and Ri the concentrations are determined
from the triangle diagram.
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 26 -
step 1 2 3 4 5 6 7
wC , Ri 0,383 0,335 0,285 0,233 0,171 0,119 0,029
balance:
F& ⋅ wC , F + L& ⋅ wC , L = E& 1 ⋅ wC , E1 + R& n ⋅ wC , Rn
1. step
F& + E& 2 = R& 1 + E& 1
( ) (
F& ⋅ wC , F − wC , R1 + E& 1 ⋅ wC , R1 − wC , E1 )
E& 2 =
wC , R1 − wC , E2
2. step
( ) (
R& 1 ⋅ wC , R1 − wC , R2 + E& 2 ⋅ wC , R2 − wC , E2 )
E& 3 =
wC , R2 − wC , E3
R& 2 = 1788
. + 3114
. − 3.214 = 1688
. kg h
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 27 -
3. step
( ) (
R& 2 ⋅ wC , R2 − wC , R3 + E& 3 ⋅ wC , R3 − wC , E3 )
E& 4 =
wC , R3 − wC , E4
R& 3 = 1688
. + 2998 − 3114
. = 1572
. kg h
4. step
( ) (
R& 3 ⋅ wC , R3 − wC , R4 + E& 4 ⋅ wC , R4 − wC , E4 )
E& 5 =
wC , R4 − wC , E5
R& 4 = 1572
. + 2.930 − 2998 = 1504
. kg h
5. step
( ) (
R& 4 ⋅ wC , R4 − wC , R5 + E& 5 ⋅ wC , R5 − wC , E5 )
E& 6 =
wC , R5 − wC , E6
R& 5 = 1504
. + 2.905 − 2.930 = 1479
. kg h
6. step
( ) (
R& 5 ⋅ wC , R5 − wC , R6 + E& 6 ⋅ wC , R6 − wC , E6 )
E& 7 =
wC , R6 − wC , E7
1479
. ⋅ ( 0,171 − 0,119) + 2.905⋅ ( 0,119 − 0,036)
E& 7 = = 2.865 kg h
0,119 − 0,008
R& 6 = 1479
. + 2.865 − 2.905 = 1439
. kg h
Examples LiquidLiquid Extraction Lecturer: Dr. Gamse - 28 -