Liquid-liquid extraction

Maria Paula Rincon Torres 1
Maria Paula Bonilla Gonzales 1
 
1.Laboratory of separation operations

Introducción

Liquid-liquid extraction is an operation of a physical nature that aims to separate 2 or more

components in a liquid mixture by adding a solvent in which one of the components is soluble, it
must be taken into account that the solutes present it is distributed in the aqueous phase and the
organic phase (Yaruro, G.2005).The solvent choice is based on its polarity; generally, polar solvents
extract polar analytes more efficiently than do apolar analytes. Consequently, LLE cannot be
specific for a particular analyte, as the solvent can extract all molecules from the matrix with similar
physicochemical properties (Krintz, 2014).
This extraction is an important separation method in research and chemical analysis. As a
commercial process, it is frequently used in the chemical and mining industries and in the
downstream recovery of fermentation products like, antibiotics, amino acids, and steroids. Its
applications to food are restricted to isolated cases, such as the transfer of carotenoid pigments from
organic solvents to edible oils or the production of “terpeneless” essential citrus oil by extracting
the oxygenated compounds of the essential oil with aqueous ethanol (Berk, 2018). There are two
common types of extractions: countercurrent and cross flow. In the countercurrent system, the two
phases flow in opposite directions. Each stage is assumed to be an equilibrium stage, so the two
phases that come out of the stage are in equilibrium. The solute, A, initially dissolves in the diluent,
D, in the feed. The solute is extracted with solvent, S. The incoming solvent stream is often
presaturated with diluent. Streams with high diluent concentrations are called raffinate, while
streams with high solvent concentrations are the extract. The other type that is used occasionally is
the crossflow system. Each stage is supposed to be an equilibrium stage. In this system, fresh
extract streams are added to each stage and extract products are removed. (Wankat, 2006).
Therefore, it seeks to establish how efficient the separation of a mixture of water, acetic acid and oil
is, in addition to determining the number of stages necessary for the process. The S / Fmin must
also be defined in mass form.

Methodology
For the separation, the behavior of the mixture is first determined with a decantation in this case, 50
ml of water and 50 ml of oil were added in addition to this, the amount of acetic acid added to the
mixture was varied in this case 3,6,9 and 12 ml. To achieve separation, the density of the oil was
determined in triplicate, the mixture was added in the decanter and stirred to wait for the phases in
this case to separate. Then it is opened to in this case obtain the extract where the water is present
and the acetic acid is titrated with NaOH at 1 M.

For the operation of the equipment, the tank must be filled with the organic phase in the lower tank
and fill the water feed tank, then the water feed pump is turned on and the column is filled with
water at a high flow rate. As soon as the water is above the top of the packing, reduce the amount of
water and start the organic phase metering pump when the water overflows at the top of the column,
the level should be checked then empty the column and Return the organic solvent and the water to
their own feed tanks, the refined and extract is placed in tanks for subsequent titration.
 Figure 1. Diagram of equipement

Results and análisis

Graph 1. Ternary diagram AA-W-Q

In the laboratory practice, the liquid-liquid extraction equipment of the University of La Sabana was
used. The objective is to separate acetic acid from an oil feed with the use of water as a solvent in
the L-L extraction equipment. In this practice, the two most common systems being countercurrent
flow and cross flow, which will be analyzed to define the best system for extraction.
In the simulation with the Excel program, it’s considered that it is an immiscible system, therefore,
the oil feed will be equal to the refining flow and the solvent, which is water, will be equal to the
extract flow. With this assumption, the concentration of acetic acid (solute) is determined in each of
the flows that are had in the liquid-liquid extraction.
For the countercurrent system, the simulation carried out in the Excel program the results obtained
are: All flows are in grams.

Feed 300 Solvent 219,3 Raffinate 247,8 Extract 203,13

xA,o 0,012 yA,N+1 0 xA,N 0,011 yA,1 0,0132
Table 1. Simulation results in Excel countercurrent system.

The results for the crossflow system are:

Feed 300 Solvent 219,3 Raffinate 247,8 Extract 203,13

xA,o 0,012 yA,N+1 0 xA,N 0,011 yA,1 0,017
Table 2. Simulation results in Excel crossflow system.

For each system, the McCabe-Thiele was carried out in order to establish the number of necessary
stages in the liquid-liquid extraction.

Graph 2. McCabe Thiele for the Countercurrent system.

 Graph 3. McCabe Thiele for the crossflow system.

According to McCabe Thiele, the countercurrent system fails to define a complete stage and
becomes a fraction of a stage whose value is 0.57. Only one stage was found in the crossflow
system.

This gives an idea that the crossflow system would be more economical in terms of the stage count,
however, the acetic acid concentration in the raffinate flow is lower than in the countercurrent
system, so the extraction efficiency liquid-liquid would decrease. Likewise, production costs would
increase. With the crossflow system, there is one stage and the best concentration of the extracted
acetic acid, which, although it increases due to the number of stages, will generate better
production.

For the simulation in the Aspen Plus program, glycerol was used replacing the oil used in the
laboratory. This decision was made considering that the software did not find the oil used along
with its properties and it was decided to replace it with a triglyceride, the main component of the
oil. The results were the following:

Figure 2. Main Flowsheet for Aspen Plus simulation

 Feed Solvent Extract Raffinate
Flow (kg/h) 300.00 219.300 284.147 193.353
Glycerol 98,8% 0% 27,3% 91,8%
Water 0% 100% 72,6% 7,1%
Acetic Acid 1,2% 0% 0,4% 1,1%
Table 3. Simulation results in Aspen Plus.

For this simulation, two stages in the extraction process are considered because the concentration of
acetic acid in the exhaust outlet is lower than that calculated compared to the cross flow, for this
reason more stages are considered than those obtained in the McCabe Thiele diagram, so the
concentration is closer than expected. As well as the program did not allow a stage or a fraction of a
stage. In addition to this for the recovery of the solvent in this case the water can be used distillation
as a technique to evaporate it and that the components of the oil and the acid remain in the mixture
and in you case obtain the water thanks to a condenser.

Conclusions

 According to the results, the process that had the greatest efficiency in the extraction of
acetic acid was crossflow, even when there was only one stage.
 In the Aspen plus simulation the extraction is better compared to the countercurrent.
However, the number of steps in the processes used to obtain a higher concentration of
acetic acid at the outlet with the solvent should be increased.
 A S / F min of 0.7 was determined.
 According to the results, the process that had the greatest efficiency in the
extraction of acetic acid was crossflow, even when there was only one stage.
 Water is a good solvent in this case, since the desired result was reached in terms of what
was to be obtained in the mass fraction of acetic acid in the refining

Bibliografía
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 Zeki Berk, Chapter 11 – Extraction, Editor(s): Zeki Berk, In Food Science and
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0-12-812018-7.00011-7.
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 Wankat, P. C. (2006). Separation process engineering. Pearson Education.