Академический Документы
Профессиональный Документы
Культура Документы
LIQUID EXTRACTION
CHAPTER / CONTENT
Solvent selection
Original Extracting
solvent (B) solvent (C)
containing A
A A A portion of A will
A
A cross to form a
A new solution in C.
A
A = solute B B
B = original solvent B
B B
C = extracting solvent
B B
Definition & Application of LLE (cont.)
The simplest LLE involves only a ternary (i.e 3 component system)
Application:
Presence of azeotropes or low relative volatilities are involved (α value near unity
and distillation cannot be used)
Density
• must be different so that phases can be separated by settling
Chemical Reactivity
• solvent should be inert and stable
Safety
• toxicity, flammability
Cost
Solvent selection (detailed)
The solvent is the key to a successful separation by LLE. The several criteria:
• Distribution Coefficient.
A distribution coefficient other than unity implies that the solute must
have different affinity in the two phases. If only one solute is involved
(such as in the recovery of an impurity from an effluent stream), only the
distribution coefficient need to be considered, and it is desirable for this to
be as large as possible.
Solvent selection (detailed)
If there are more than one solutes (sat two solutes A and B), then
consideration should be given to the selectivity of the solvent for solutes A
against B.
Insolubility of Solvent.
The solvent should have low solubility in the feed solution, otherwise
the separation is not ‚clean‛. For example, if there is significant solubility
of solvent in the raffinate stream, an additional separation step is required
to recover the solvent.
Solvent selection (detailed)
Recoverability.
It is always necessary to recover the solvent for re-use, and this must
ordinarily be done by other means, e.g distillation. If distillation is to be
used, the solvent should form no azeotrope with the extracted solute and
mixtures should show high relative volatility. The solvent should also be
thermally – stable under the distillation temperature.
Density.
Interfacial tension.
Chemical Reactivity.
The solvent should be stable chemically and inert toward the other
components of the system and toward the common materials of
construction.
Solvent selection (detailed)
These should be low for ease in handling and storage, for example, a
high viscosity leads to difficulties with pumping, dispersion and mass
transfer rate.
Other Criteria.
Plait Point
P
Extract F Feed
E
Mixing point
R Raffinate
Tie-lines
Solvent S
Carrier
Right-angle triangular diagram
(rectangular coordinate)
LLE for Partially Miscible Solvent
Solvent and the solution are in contact with each other only once and thus
the raffinate and extract are in equilibrium only once.
Liquid-Liquid Extraction
Extracting Solvent, S
Extract phase, E
ys (A) Intermediate, M y* (A)
Note: Intermediate shown just for purpose of demonstration. Don’t have to draw it when
answering the question
Single – stage calculations
xF F y S S xM M Eq. (2)
Using the calculated value of xM, locate point M (xM) on the FS line. Note that
point M must be on FS line.
Draw a new tie line that pass through point M. This new tie line must take shape
of the nearest given tie lines.
From the new tie line, you can locate point E and R and hence you can
determine the composition of raffinate, R and extract, E that are in equilibrium.
Single – stage calculations
Once you have determine composition of R and E, you can determine the
masses of E and R using the material balance as follows:
x F F y S S x * R y * E Eq. (4)
Example 1
100 kg of a solution containing 0.4 mass fraction of ethylene glycol (EG) in water is
to be extracted with equal mass of furfural 250C and 101 kPa. Using the ternary
phase equilibrium diagram method, determine the followings:
Solution 1
Locate point F & S, draw line FS. Locate point xM on FS line. Draw new tie
line that pass through point xM. From that tie line, locate point E and R hence
you can determine the composition of R (x*) and E (y*) which is in equilibrium.
From the graph, y* = 0.26, x* = 0.075 (Solution for point 1)
Single – stage calculations
M E
R
S
Single – stage calculations
Equilateral method
E M
R
S
Single – stage calculations
Solution 1 (cont’)
Normally numbering of the stages begin at the top down to the bottom.
Thus the top most stage is named as stage 1, stage directly below stage 1 is
stage 2 and so on.
N-1
xF F y S S xM M Eq. (2)
Using the calculated value of xM, locate point M (xM) on the FS line. Note that
point M must be on FS line.
Solute
Plait Point
E1
Feed
M Operating Point
P
RN
Carrier
Multi – stage counter current system
Draw a line from the operating point P through R1 to the extract side of
the equilibrium curve. The intersection locates E2
Solute
Plait Point
E1
E2
Feed
E3 Operating Point
E4 R1
M P
E5
E6 RN
Carrier
Solvent C
Multi – stage counter current system
Minimum solvent flow rate is the lowest rate / amount at which solvent could be
theoretically used for a specified extraction.
Occurs when operating line touches the equilibrium curve at which the
separation requires infinite number of ideal stages.
Point M is dependent upon the solvent flow rate / amount. The larger the rate /
amount, the closer is point M to point S on the FS line.
Multi – stage counter current system
Draw a best tie line that originate from F. The intersection of this line with
extract half – dome is point Emin (minimum extract flow rate / amount).
Draw a straight line from Emin to point R. The intersection of this line with
FS gives point Mmin. From point Mmin you can read the value of xmin.
Use the value of xmin and material balance to calculate the Smin .
Example 2
5300 kg/h of a solution containing 30% by weight of ethylene glycol (EG) in water
is to be reduced to 4.5% (solvent free) by a continuous extraction in a
countercurrent column using recycled furfural that contains 1.5% EG as the
extracting solvent:
Determine the minimum solvent flow rate for the extraction above
If the solvent enters at 1.25 times the minimum solvent rate, how many ideal
stages are required?
Determine the number of real stages if the overall efficiency of the column
is 60%
Multi – stage counter current system
Solution 2
Emin
F
Mmin
RSF
S
Multi – stage counter current system
E5 P
RSF
S
M N y' S x' B
Example 3
If 100 kg of isopropyl ether is added to the solution, what weight of acetic acid
will be extracted by isopropyl ether if equilibrium is attained?
x’ (kg acid/kg water) 0.030 0.046 0.063 0.070 0.078 0.086 0.106
y’ (kg acid/kg isopropyl ether) 0.10 0.15 0.20 0.22 0.24 0.26 0.30
Single – stage calculations
Solution 3
The equilibrium data and equation above is plotted in figure next page.
Solution 3
0.35
0.3
0.25
0.2
y'
0.15
0.1
0.05
0
0 0.02 0.04 0.06 0.08 0.1 0.12 0.14
x'
Multi – stage counter current system
The principle is quite same with the partially miscible solvent, but in this case
the extraction process involved the immiscible solvent.
B kg/h pure diluent B in feed solution S kg/h pure solvent in extract phase
N-1
For immiscible solvents, analysis of the extraction process become much simpler
since the flow rate of pure solvents (extracting solvent and feed solvent (diluent) )
are constants).
The operating line equation for multi stage liquid –liquid extraction:
B y' S x' 2 B
y' x' 2 Form of y = mx + c
S S
The operating line can be plotted by locating points (x’1,y’1) and (x’2,y’2) and
draw a straight line through these points.
Using the method similar to Mc Cabe – Thiele diagram, the number of ideal
stages can be determined by drawing the triangular steps connecting equilibrium
line and the operating line.
Multi – stage counter current system
Example 4
x’ (kg acid/kg
0.000 0.025 0.050 0.100 0.150 0.200 0.220 0.240 0.260 0.300
water)
y’ (kg acid/kg
0.000 0.005 0.013 0.030 0.046 0.063 0.070 0.078 0.086 0.106
isopropyl ether)
Multi – stage counter current system
Solution 4
0.8(8000) kg/h of water in 20,000 kg/h isopropyl ether (C) in extract phase
x’2 y’2
TOP (2)
BOTTOM (1)
0.8(8000) kg/h of water (B) in raffinate
0.02 kg A/kg (solvent free) 20,000 kg/h isopropyl ether (C) in
x’1 y’1
Multi – stage counter current system
Solution 4
For location 1,
Solution 4
For location 2,
Feed
Extract
Solution 4
For location 2,
Extract
The points for operating line are (0.0204, 0) and (0.250, 0.0735).
Solution 4
Multi – stage counter current system
Minimum solvent flow rate, Smin is defined as the flow rate of solvent at which
the number of stages approaches infinity.
B B
m min S min
S min m min
Example 5
Determine the minimum flow rate of isopropyl ether for the problem in
Example 4.
Multi – stage counter current system
Solution 5
The line tangential to the equilibrium curve and originates from (x’1,y’1)
which is (0.0204, 0) is drawn in figure below:
B 0.8 8000
The slope of the tangential line = 0.343 S min = 18 658.89 kg/h.
m min 0.343
Liquid – liquid extraction equipment
2) Vessels in which the mixing is done by the flow of the fluid themselves.
One phase is usually dispersed into the other in the form of small droplet.
In figure 12.6 – 1(a) for typical mixer settler, mixer or agitator is entirely
separate from the settler. The feed of aqueous phase and organic phase are
mixed in the mixer, and then the mixed phases are separated in the settler.
In figure 12.6 – 1(b) for combined mixer settler, sometimes used in extraction
of uranium salts or copper salts from aqueous solution.
Liquid – liquid extraction equipment