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KKEK3171: Lab & Communication II

Semester 1, 2013/2014
Lab Oral Presentation

Experiment 6:
Extraction: Liquid-liquid Equilibrium
By Yew Zhen Xuan KEK110064

Outline
Introduction
Methodology
Results

and Discussion
Conclusion

Objectives
To

study the ternary liquid


system of water-acetone-toluene.

To

find the plait point and tie


lines.

To

verify the tie lines using


Othmer-Tobias and Hands
correlations.
3

Introduction
What is liquid-liquid extraction?
A

liquid feed of two or more components is


contacted with another liquid phase which is
immiscible or partially miscible with one or more
components in the feed and completely or
partially miscible with one or more key
component of the feed. [1]

[1] Seader, J., Henley, E. and Roper, D. 2011. Separation process principles. Hoboken,
NJ: Wiley.

Introduction
Why is liquid-liquid extraction
important?
Close

boiling points of components.

Low

concentration of solute
component.

Heat

sensitive components.
5

Methodology
Method
of
Titratio
n
Method
of
Analysi
s

The binodal curve is


established using
the cloud point
method.

Let a ternary
mixture separate
into two liquid
phases and analyze
the compositions.
6

Methodology

Methodology
Determination of Raffinate Phase
Table 1: Composition of distilled water-acetone
Curve
mixture
Sample

Distilled Water
(ml)

Acetone
(ml)

45

40

10

35

15

30

20

25

25

20

30

Methodology
Determination of Extract Phase
Table 2: Composition of toluene-acetone
Curve
mixture
Sample

Toluene
(ml)

Acetone
(ml)

45

40

10

35

15

30

20

25

25

20

30

Methodology
Determination of Tie Lines
Table 3: Composition of distilled water-acetonetoluene mixture
Sample
Distilled Water
Toluene
(ml)

(ml)

Acetone
(ml)

100

25

50

100

30

45

100

35

40

100

40

35

100

45

30

100

50

25

Methodology (Job Safety


Analysis)
Basic Job Step

Preparation
of
chemical mixture
using
acetone,
toluene
and
distilled water

Potential Hazard
-Liquid
toluene
and
acetone
has
high
volatility. Toluene is
hazardous because of
its
carcinogenic
properties.

Disposing
the Acetone and toluene
waste chemical
are organic chemicals
which will pollute the
drainage
system
if
disposed in improper
manner.

Recommended Action or
Procedure
-Preparation and titration of
liquid chemical must be carried
out in the fume chamber with
opening height not exceeding 6
inches.

-Safety mask has to be put on


to
prevent
inhalation
of
hazardous vapour.

All chemical waste should be


placed
in
the
designated
container
prepared
by
laboratory technician.

Results and Discussion


Table 4: Data to Determine Raffinate Phase (Aqueous-Rich
Phase Curve)
Distilled Water
(ml)

Acetone

Toluene (Titrated)

(ml)

(ml)

45.0

5.0

0.7

40.0

10.0

0.4

35.0

15.0

0.3

30.0

20.0

0.5

25.0

25.0

0.7

20.0

30.0

1.1

Results and Discussion


Why does the refractive index increase with
the increase of mass fraction of acetone?
1.38

1.37
Refractive Index, nD

f(x) = 0.08x + 1.33


R = 0.94

1.36

1.35

1.34

1.33
0.000

0.100

0.200

0.300

0.400

0.500

0.600

Mass Fraction of Acetone

Figure 1: Graph of refractive index against mass


fraction of acetone for aqueous-rich phase.

Results and Discussion


Table 5: Data to Determine Extract Phase (Organic-Rich
Phase Curve)
Toluene, ml

Acetone, ml

Distilled Water
(Titrated), ml

45

2.5

40

10

2.2

35

15

2.1

30

20

1.3

25

25

1.2

20

30

1.2

Results and Discussion


1.5200
1.5000
1.4800

f(x) = 0.24x + 1.36


R = 0.86

1.4600
1.4400
Refractive Index, nD

1.4200
1.4000
1.3800
1.3600
1.3400
0.000 0.100 0.200 0.300 0.400 0.500 0.600
Mass Fraction of Acetone

Figure 2: Graph of refractive index against mass fraction of acetone for


organic-rich phase.
Table 6: Refractive index of pure component
Chemical Used

Refractive Index

Acetone

1.3561

Distilled Water

1.3333

Toluene

1.4969

Data retrieved from: Perry, R. and Green, D. 2008.Perry's chemical engineers'


handbook. [New York]: McGraw-Hill.

Results and Discussion

Figure 3: Phase diagram for acetone-water-toluene ternary system.

Results and Discussion


Verifying
tie lines using Othmer-Tobias

correlation
(1)
Where:
W33 = mass fraction of toluene in the toluene-rich phase
W11 = mass fraction of water in the water-rich phase
0.50

-2.50

f(x) = 0.86x + 0.14


R = 1
-2.00 -1.50 -1.00

0.00
-0.50
0.00

0.50

-0.50

ln ((1-w33)/w33)
-1.00
-1.50
-2.00

ln ((1-w11)/w11)
Figure 4: Graph of ln ((1-w33)/w33) against ln ((1-w11)/w11) for Othmer-Tobias
Correlation.

Results and Discussion


Verifying
tie lines using Hands correlation

(2)

Where:
W21 = mass fraction of acetone in the water-rich phase
W23= mass fraction of acetone in the toluene-rich phase
0.40
0.20

f(x) = 4.74x + 6.14


R = 0.88
-1.50

-1.45

-1.40

-1.35

-1.30

ln (w13/w33)

0.00
-1.25
-1.20
-0.20
-0.40
-0.60
-0.80
-1.00

ln (w21/w23)

Figure 5: Graph of ln (w13/w33) against ln (w23/w23) for Hands Correlation.

Conclusions
More

toluene is needed to extract


acetone from the water-rich phase
mixture.
More water is needed to extract
acetone from the toluene-rich phase
mixture.
The plait point can be plotted by using
conjugate curve extrapolated from tie
lines.
The experimental tie-line data fits
Othmer-Tobias and Hands
1
correlations.

Q & A Session

2
0

Thank You