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Definition & Application
LLE= Separation of constituents (solutes) of a liquid solution by contact with another insoluble liquid. Solutes are separated based on their different solubilities in different liquid. LLE= Separation process of the components of a liquid mixture by treatment with a solvent in which one or more desired components is soluble. There are two requirements for liquid liquid extraction to be feasible: component (s) to be removed from the feed must preferentially distribute in the solvent. the feed and solvent phases must be substantially immiscible
Solvent
Diluent
Extract
Raffinate -
In the inorganic chemical industry, they are used to recover high boiling components such as phosphoric acid, boric acid and sodium hydroxide from aqueous solution.
Extraction of benzylalcohol from a salt solution with toluene. Removing of H2S from LPG with MDEA Extraction of caprolactam from ammonium sulfate solution with benzene Extraction of acrylic acid from wastewater with butanol Removing residual alkalis from dichlorohydrazobenzene with water
The solution normally binary solution containing solute (A) dissolved in a diluent or carrier (B). The extracting solvent can be either pure solvent C or may content little A. Raffinate (R) is the exiting phase rich in carrier (B) while extract is exiting phase rich in solvent (C).
When liquid solution mixed with solvent (C), an intermediate phase M momentarily forms as the light liquid moves through the heavy liquid in the form of bubbles. These bubbles provide a large surface area for contact between the solution and the solvent that speed up mass transfer process.
Liquid-Liquid Extraction
Extracting Solvent, S
ys (A)
Intermediate, M xM (A)
F E M yS x*
Mass of feed solution Mass of extract phase Mass of intermediate Mass fraction of A in S Equilibrium mass fraction of A in R
S R xF xM y*
Mass of extracting solvent Mass of raffinate phase Mass fraction of A in F Mass fraction of A in M Equilibrium mass fraction of A in E
Note: Intermediate shown just for purpose of demonstration. Dont have to draw it when answering the question
FS M
Eq. (1)
Determine mass fraction of solute A in intermediate M using material balance for solute A :
xF F y S S xM M
Eq. (2)
FS RE
Using the material balance for solute A:
x F F y S S x * R y * E
Eq. (3)
Eq. (4)
% EG
0.0 8.5 14.5 21.0 29.0 42.0 50.0 51.0
% water
5.0 4.5 4.5 6.0 7.0 8.5 14.0 33.0
% furfural
95.0 87.0 81.0 73.0 64.0 49.5 36.0 16.0
% EG
0.0 2.0 5.5 7.0 8.0 14.0 31.0 51.0
% water
92.0 89.6 86.0 84.4 83.3 77.2 60.0 33.0
% furfural
8.0 8.4 8.5 8.6 8.7 8.8 9.0 16.0
Use the following equilibrium tie line to construct the ternary phase diagram
FS M
100 100 M
M 200 kg
Determine mass fraction of solute A in intermediate M using material balance for solute A:
xF F y S S xM M 0.4 100 0 100 x M 200 x M 0.2
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)
F M R E
F E M R S
FS RE
100 100 R E
R 200 E
Eq. (i)
% of EG extracted =
y * E 0.26 135.14 100% x100% 87.8% xF F 0.40 100
Tutorial
1. 12.5-2 2. 12.5-4
Tutorial
1. 12.5-2 (Textbook-page 832)
A single stage extraction is performed in which 400kg of a solution containing 35 wt% acetic acid in water is contacted with 400 kg of pure isopropyl ether. By using equilateral diagram, determine the composition of raffinate and extract phases the mass of extract and raffinate the percent acetic acid extracted
Tutorial
2. 12.5-4 (Textbook-page 832)
A mixture weighing 1000kg contains 23.5 wt% acetone and 75.5 wt% water and is to be extracted by 500 kg methyl isobutyl ketone in a single stage extraction. By using equilateral diagram, determine the composition of raffinate and extract phases the mass of extract and raffinate the percent acetone extracted
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.
Feed solution, F xF (A)
1 2
3
n N-1 N
The analysis of multistage extraction can be performed using right angle or equilateral triangular diagram to determine the number of ideal stages required for a specified separation.
FS M
Eq. (1)
Determine mass fraction of solute A in intermediate M using material balance for solute A :
xF F y S S xM M
Eq. (2)
Locate the Operating Point by finding the intersection of operating lines for the left most and right most stage. Draw a line through E1 and F. Draw a line through S and RN. Locate the intersection P. This point is the operating point P.
Solute
RN
S Carrier
Solute
Plait Point
E1 E2 E3 E4 E5 E6
Feed
M
R1 RN
Carrier
Operating Point P
Solvent C
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.
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 . % Overall efficiency of multi stage extraction column: % Overall efficiency = (number of ideal stage / number of real stage) x 100%
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%
Smin=1127.66 kg/h
S = 1409.58 kg/h
FS M
5300 1409.58 M
M 6409 .58 kg
Determine mass fraction of solute A in intermediate M using material balance for solute A: From material balance:
RSF
RSF
Exercise
1. 12.7-3 (Textbook, pages 833)
An aqueous feed solution of 1000 kg/hr containing 23.5 wt% acetone and 76.5 wt% water is being extracted in a countercurrent multistage extraction system using pure methylisobutyl ketone solvent at 298-299 K. The outlet water raffinate will contain 2.5 wt% acetone. By using equilateral method, a) Determine the minimum solvent that can be used (Answer: Xmin = 0.18, Smin = 305.56 kg/hr , Mmin = 1305.56 kg/hr) b) Using a solvent flow rate of 1.5 times the minimum, determine the number of theoretical stages. (Answer: S= 458.34 kg/hr, Xm=0.16 , 5 stages)
Sometimes extraction use a solvent C that is only slightly soluble in B or the solvent C used is in range where the solubility in B is so low that for all practice purpose, it can be assumed to be completely insoluble / immiscible in B and vice versa.
Bancroft weight fractions or mass ratio, x and y are defined as follows: x (in raffinate phase) = mass of solute A / mass of diluent B y (in extract phase) = mass of solute A / mass of solvent C
y'
B MN x' S S
Eq. (3)
B = Water
C = Isopropyl ether
80 kg diluent B in Raffinate x kg A/kg diluent B 100 kg solvent C in Extract y kg A/kg solvent C
The equilibrium data and equation above is plotted in figure next page.
y'
0.15 0.1 0.05 0 0 0.02 0.04 0.06 x' 0.08 0.1 0.12 0.14
Form of y = mx + c
The operating line gives a relationship between mass fraction of A (xn) in raffinate phase coming out of the nth stage, with mass fraction of A (yn) in extract phase entering the nth stage.
The operating line can be plotted by locating points (x1,y1) and (x2,y2) 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.
0.000 0.000
0.025 0.005
0.050 0.013
0.100 0.030
0.150 0.046
0.200 0.063
0.220 0.070
0.240 0.078
0.260 0.086
0.300 0.106
y'1
Coordinates for (x2,y2) = (0.250, 0.0735) The points for operating line are (0.0204, 0) and (0.250, 0.0735). No. of theoretical stages = 14 stages
TOP (0.250,0.0735)
BOTTOM (0.0204,0)
S min
Example 5
Determine the minimum flow rate of isopropyl ether for the problem in Example 4.
TOP (0.250,0.0735)
BOTTOM (0.0204,0)
S min
Tutorial
12.7-6 (Textbook)
A water solution of 1000kg/hr containing 1.5 wt% nicotine in water is stripped with a kerosene stream of 2000kg/hr containing 0.05 wt% nicotine in a countercurrent stage tower. The exit water is to contain only 10% of the original nicotine, that is, 90% is removed. 1.Determine the number of theoretical stages needed. 2. Determine the minimum solvent(kerosene) flow rate
1)
2)
In some cases the heavy liquid is sprayed downward into a rising, light continuous phase.