LLE

Extraction
Group 5
Xavi Gasulla &
Meritxell Sitjà

1
Objectives
Draw the triangular diagram of a water-THF-cyclohexane mixture at room
temperature and determine the composition of a binary mixture to be extracted.

Liquid-liquid extraction
Separation process consisting of Polar Solvent: Extract
Water
the transfer of a solute from one
solvent to another, the two
solvents being immiscible or
partially miscible with each other.

Solute: THF
Raffinate
Non-polar Solvent:
Cyclohexane 2
Objectives

3
Experimental setup: Equipment

100 mL Erlenmeyers
Analytical scale Refractometer Separatory funnel
Burette

4
Experimental setup: Reagents
Components THF Cyclohexane Water
Chemical Formula C₄H₈O C₆H₁₂ H₂O
Solubility with THF - Miscible Partially miscible
Solubility with Cyclohexane Miscible - Insoluble
Solubility with Water Partially miscible Insoluble -

Hazards and Precautions

5
Experimental setup: Methodology
Prepare binary solutions Slowly add the third
• Solute + Carrier component Calculate the added Measure the refractive
• Solute + Rafinate • using a burette amount of solvent/inert index for the solutions of
• (4 of each) by weighing the sample known concentrations
after addition (for calibration)

Prepare three ternary

mixtures of known Observe phase Collect samples from Measure refractive index
composition under the separation and decant both phase of collected samples
binodal curve (tie lines)

Determine the content of

THF in each fraction

6
 Results and discussion: Triangular diagram
THF
Water-Tetrahydrofuran-
Cyclohexane mixture at room
0 1 THF

temperature and atmospheric 0,1 0,9

Experimental Data

pressure. 0,2 0,8

0,3 0,7
y = -4,1367x2 + 4,1312x - 0,2468
0,4 0,6

0,5 0,5

0,6 0,4

0,7 0,3

0,8 0,2

0,9 0,1

1 0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1
Water Water
Cyclohexane
Cyclohexane

7
 Results and discussion: Calibration curves
1.4 1.418
f(x) = 0.0822109214159358 x + 1.33088828868016
R² = 0.985721257258042 f(x) = − 0.0195363445504901 x + 1.42375124483232
1.39 1.416 R² = 0.997855685151232

1.38 1.414

Refractive index
Refractive index

1.37 1.412

1.36 1.41

1.35 1.408

1.34 1.406

1.33 1.404

1.32 1.402
20% 30% 40% 50% 60% 70% 80% 90% 30% 40% 50% 60% 70% 80% 90%

% weight THF in raffinate % weight THF in extract

8
 Results and discussion: Tie lines
THF
0 1 THF
Experimental Data
RI upper, extract RI lower, raffinate 0,1 0,9 tie line (1)

tie line (2)

1,420 1,336 0,2 0,8
Tie line (3)
0,3 0,7
1,413 1,3455 y = -4,1367x2 + 4,1312x - 0,2468

0,4 0,6

1,405 1,355 0,5 0,5

0,6 0,4

0,7 0,3

0,8 0,2

0,9 0,1

1 0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1

Water Water Cyclohexane Cyclohexane

9
 Results and discussion: Chosen Point
1
0.9
THF: 30%, Water: 20%, Cyclohexane: 50%

Ye, THF in Extract

0.8
f(x) = − 4.74097352589903 x² + 4.2422915905549 x − 0.0500860196071351
0.7
0.6
THF 0.5
0 1 0.4
0.3
0,1 0.9
0.2
0,2 0.8 Choose 0.1
f(x) = − 4.13671573539043 x² + 4.13118386888347 x − 0.246816055469556 n Point
0
0,3 0.7 0.00 0.05 0.10 0.15 0.20 0.25 0.30 0.35

0,4 0.6 Xr, THF in Raffinate

0,5 0.5

0,6 0.4
X Y
0,7 0.3
Raffinate, visiual
0,8 0.2 aproximation 0,11 0,14
0,9 0.1 Extract, visiual
1 0
aproximation 0,83 0,35
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Water Cyclohexane Regression analysis 0,12 0,39

10
Results and discussion: Simulated Data
with Hysys & Bibliographic Data
Water-THF-Cyclohexane mixture at room Water-THF-Cyclohexane/Methylcyclohexane
temperature and atmospheric pressure. mixture at room temperature and atmospheric
pressure.
f(x) = 0
THF Experiment 0 1 THF
Data
Polynomial 0,1 0.9 Exper-
(Experiment iment
Data) Data
NRTL 0,2 0.8
Extended
NRTL 0,3 0.7
Antoine

0,4 0.6

0,5 0.5

0,6 0.4

0,7 0.3

0,8 0.2

0,9 0.1

1 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Water Cyclohexane Water Cyclohexane/methylcyclohexane

11
Conclusions
• Binodal curve of a water-THF-cyclohexane mixture similar to ternary
diagram of methylcyclohexane. Subtle error in calibration .
• Three tie lines below the curve
• Determine the composition of the two phases formed from a chosen
point of a mixture.
• Hysys approximation failed because of fluid package shortcomings.

12
Bibliography
https://www.sciencedirect.com/topics/agricultural-and-biologi
cal-sciences/liquid-liquid-extraction#:~:text=Liquid%2Dliquid%
20extraction%2C%20also%20known,partially%20miscible%20
with%20each%20other
.
https://www.sciencedirect.com/topics/engineering/ternary-di
agram#:~:text=Ternary%20diagrams%20represent%20three%2
Dcomponent,as%20in%20the%20binary%20system
.

13
 LLE Extraction

Thank you
for your
attention!
Group 5
Xavi Gasulla &
Meritxell Sitjà
14