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CLB 21204 TRANSPORT PROCESS PRINCIPLE

UNIVERSITI KUALA LUMPUR


MALAYSIAN INSTITUTE OF CHEMICAL
& BIOENGINEERING TECHNOLOGY

LABORATORY REPORT COVER PAGE


Title of experiment: Experiment 3: PULSED COLUMN LIQUID-LIQUID
EXTRACTION UNIT

Group number: Section:

Date of experiment: 8 / 10 / 2019 Date of submission: 22 / 10 / 2019

Name & ID No.: 1. Wan Muhamad Ajmal bin Zainal 55218117247


2. Seri Syuriati Sulyana Binti Abdul Razak 55217117122
3. Nur An Nisaa Binti Tahat 55217117113
4. Hanis Farahana Binti Mohamad Zaki 55218117152
5. Nurul Najwa Binti Mohd Afif 55218117241
*Penalty:
 For any late of submission, the mark will be reduced by 5% per day to a maximum of 3 days, after which it will NOT BE
ACCEPTED.
 Plagiarism will not be tolerated and will be given ZERO.
Unacceptable Poor Satisfactory Good Excellent Marks
Criteria
(1) (2) (3) (4) (5)
Report format (5%)
1.Organization of the report.
Summary (10%) – max 1 page
1.Brief review on the objectives of the experiment, major
findings and significant conclusions
Objectives (5%)
1.State the objectives of the experiment in point form
Introduction & Theory (10%) – max 2 pages
1. State the background to the experiment conducted.
2. Summary of theories including formulations related to
the experimental work.
Data & Results (10%)
1. Data are presented as deemed suitable with
complete labels and units.
Analysis & Discussion (40%)
1. Explanations of the referred table and figure are
presented after the table and figure
2. Discuss on the findings and relations to the theory
and objective of experiment
Conclusion & Recommendation (10%)
1.Summary of the results to relate the findings or results
with the theory applicable to the experimental
2.Suggest improvements in apparatus or measurement
procedure, or experimental procedures for future
References (5%)
1. Cite references in the text.
2. References taken from books, journals and articles.
References from website are not recommended.
Appendices (5%)
1. Put raw data and sample calculation.

TOTAL (100%)

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CLB 21204 TRANSPORT PROCESS PRINCIPLE

SUMMARY
Liquid-liquid extraction, also known as partitioning, is a separation process
consisting of the transfer of a solute from one solvent to another, the two solvents being
immiscible or partially miscible with each other. The Pulsed Column Extractor or
reciprocating columns extractor uses a reciprocating pump to create pulses of short
amplitude that are superimposed on the usual flow of the liquid phases. The objective of
this experiment is to operate a liquid – liquid extraction experiment using a pulsed column
liquid-extraction unit and to determine the height equivalent theoretical plates (HETP) for
column by using equilateral triangular diagram. It is also to investigate the effect of the
pulsation stroke on the HETP. There were two phases in this process, where one or more
elements went through a immiscible liquid solvent (Phase 2) was selectively removed from
a liquid or solid mixture which was the feed (Phase 1). Based on t he calibration curve, it
shows that the raffinate and extract weight of percentage acetone are at 25.4wt% and 83.17wt%
at 0 minutes, 25.4wt% and 89wt% at 5 minutes, 23.4wt% and 84.29wt% at 10 minutes,
25.4wt % and 44.88wt% at 15 minutes and 25.4wt% and 44.88wt % at 20 minutes. From
the result obtained, it shows that the data acetone composition for extract are not uniform
with increase of time. The pulsed column liquid-liquid extraction experiment determined the
required theoretical extraction stage. Four theoretical stages have been achieved in this
experiment

OBJECTIVES
The purpose for conducting this experiment are:

 To operate a liquid – liquid extraction experiment using a pulsed column liquid – extraction
unit.
 To determine the height equivalent theoretical plates (HETP) for column by using
equilateral triangular diagram.
 To investigate the effect of the pulsation stroke on the HETP.

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CLB 21204 TRANSPORT PROCESS PRINCIPLE

INTRODUCTIONS

Liquid liquid extraction, also known as partitioning, is a separation process consisting of the
transfer of a solute from one solvent to another, the two solvents being immiscible or partially
miscible with each other. Frequently, one of the solvents is water or an aqueous mixture and the
other is a non-polar organic liquid. As in all extraction processes, liquid liquid extraction comprises
a step of mixing (contacting) followed by a step of phase separation.

The Pulsed Column Extractor or reciprocating columns extractor uses a reciprocating pump
to create pulses of short amplitude that are superimposed on the usual flow of the liquid phases.
The column itself may contain packing or perforated plates. An increase efficiency of sieve-plate a
packed extraction column is obtained by applying a sinusoidal pulsation to the contents of the
column.

The unique features of pulsed column extractor are low axial mixing and a relatively small
increase in axial mixing with increase in column diameter. The pulsation causes the light liquid to
be dispersed into the heavy phase on the upward stroke and the heavy phase to jet into the light
phase on the downward stroke.

The light and dense liquids passing counter currently through the columns are acted on by
pulsations transmitted hydraulically from a dispersion of drops. The pulsation device is connected
to the side of the column usually at the base though a pulse leg. Pulsed Column Extractor is a
more energy efficient way to obtain a phase dispersion. Reciprocating of plates requires less
energy and has the same effect in terms of mixing patterns and uniform dispersion.

Liquid liquid 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 (antibiotics, amino acids, 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.

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CLB 21204 TRANSPORT PROCESS PRINCIPLE

DATA & RESULTS

Table 1: Result of Pulsed Column Liquid-Liquid Exraction Unit

Raffinate Extract
(water rich phase ) (Toluene rich phase)
Feed Solvent Solvent Pulsation
Time Refractive Solute Refractive Solute
flowrat flowrat to Feed stroke
(min) Index (Acetone) Index (Acetone)
e (L/hr) e (L/hr) ratio (mm)
Composition Composition
(wt %) (wt %)

12 12 1 5 0 1.347 25.4 1.356 83.71


12 12 1 5 5 1.347 25.4 1.347 89.00
12 12 1 5 10 1.346 23.4 1.355 84.29
12 12 1 5 15 1.347 25.4 1.422 44.88
12 12 1 5 20 1.347 25.4 1.422 44.88

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CLB 21204 TRANSPORT PROCESS PRINCIPLE

Figure 1: Calibration Curve for Toluene Rich Phase

Figure 2: Calibration Curve for Water Rich Phase

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CLB 21204 TRANSPORT PROCESS PRINCIPLE

ANALYSIS & DISCUSSION

This experiment is about the extraction unit of pulsed liquid-liquid column. There are three
objectives to execute this test. First, using a pulsed column liquid-liquid extraction system to run a
liquid-liquid extraction experiment. Secondly, by using an equilateral triangular diagram to evaluate
the height equivalent theoretical plates (HETP) for the column and thirdly to investigate the effect
from the HETP pulsation movement. The variables used in this test are the flow rate of feed (L/hr),
the flow rate of solvents (L/hr), the flow rate of feed solvents, the pulsation stroke (mm), the period
(min) and also the refractive index and solution for the composition of acetones (percent) in
distilled (water-rich phase) and extract (toluene-rich phase) .

Extraction is a method in which one or more elements, through an immiscible liquid solvent
(Phase 2), is selectively removed from a liquid or solid mixture, the feed (Phase 1). The transition
of the materials from the feed to the solvent in the following step is regulated by the solubility
activity of each element. The extraction process, one enriched (Extract Phase) and the other
depleted (Raffinate Phase), results in two phases. Liquid-liquid separation defines a way for
extracting solvent components by using an unequal distribution of two immiscible liquid stages. In
most instances, this procedure is done by closely separating the two immiscible liquids, enabling
the liquid to be selectively moved from one phase to the next, and requiring the two phases to be
removed. Usually, one step is an aqueous liquid that usually contains the materials to be extracted
and the other phase is an organic solvent. Which has a high affinity for certain particular solution
ingredients. The method becomes reversible by touching the liquid filled with solvent with another
immiscible layer with a greater tolerance than the organic state for the solvent. The transition of
the liquid from one stage to the other process is called extraction (K. NAJIM, 2007).

Three compounds that are acetone (solute), purified water (diluent) and toluene (solvent)
are used in this test. Mixing acetone and liquid solution in feed vessel B1 started the test.
Appropriate amounts of acetone in distilled water are combined with 20 liters of 50wt percent
acetone solution in liquid. While adding pure toluene solvent in the feed vessel B2. Then, by
following all the procedures in the laboratory manual, the experiment was carried out. The raffinate
and extract refractive index were reported between 0 minutes and 20 minutes. The calibration
curve shows, the raffinate and extract weight of percentage acetone are at 25.4wt% and 83.17wt%
at 0 minutes, 25.4wt% and 89wt% at 5 minutes, 23.4wt% and 84.29wt% at 10 minutes,
25.4wt % and 44.88wt% at 15 minutes and 25.4wt% and 44.88wt % at 20 minutes. From
the result obtained, it shows that the data acetone composition for extract are not uniform
with increase of time.

CLB 21204/TRANSPORT PROCESS PRINCIPLE/JAN 2019


CLB 21204 TRANSPORT PROCESS PRINCIPLE

Based on the results, the pulsed column liquid-liquid extraction experiment determined the
required theoretical extraction stage. Four theoretical stages have been achieved. There are a
couple of factors that would help increase the transfer rate of the solution. First is the selectivity,
where the capacity to extract and isolate the alcohol from the other elements that are likely to be
present in the liquor of the feed. Additionally, is the density gap, which will result in issues of
isolation, reduced efficiency and a too low-density disparity between the stages. Too broad in the
difference in density can render achieving the fall sizes required for the best extraction difficult.
Second, the rational physical properties in which a liquid that is too viscous can hinder both the
transition of mass and energy. Too low interfacial pressure may lead to problems with emulsion. If
the latter is to be extracted by distillation, the boiling point should be sufficiently different from that
of the solution (B.Todd, 2009).

The impact of pulsation speed on time to reach a steady percentage of solute state quality
was analyzed when preserving constant flow rates of feed mixture and solvent. Increasing
pulsation rate resulted in a significant decrease in time to achieve a consistent percentage of
solute content in the extract process. Higher pulsation frequency values resulted in the breakdown
of the dispersed phase drops which increased the transfer of solvent mass. This proves that the
mass transfer coefficient is improved by increasing the frequency and amplitude of the pulse. The
increase in the number of Reynolds in the streamline flow area due to pulsation is substantial
(Akhtar, 2007)

Lastly, there are a few mistakes that could have resulted in this study which cause the not
accurate result obtain. Firstly, it may be incorrect to interpret the refractive index. Secondly, by
adopting the exact measurement, the acetone-water solution was not correctly filled in and the
incorrect result could be reached. Furthermore, the machinery could be unreliable, resulting in low
rates of extraction. Thus, it can be assumed that in this study all the targets are met.

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CLB 21204 TRANSPORT PROCESS PRINCIPLE

CONCLUSION & RECOMMENDATION

As the conclusion, extraction is a method in which one or more elements, through an


immiscible liquid solvent (Phase 2), is selectively removed from a liquid or solid mixture, the feed
(Phase 1). This experiment contain three objectives, there are to operate a liquid – liquid extraction
experiment using a pulsed column liquid – extraction unit, to determine the height equivalent
theoretical plates (HETP) for column by using equilateral triangular diagram, and to investigate the
effect of the pulsation stroke on the HETP. In most instances, this procedure is done by closely
separating the two immiscible liquids, enabling the liquid to be selectively moved from one phase
to the next, and requiring the two phases to be removed. Three compounds were used in this
experiment. There are acetone (solute), purified water (diluent) and toluene (solvent). The result
shows that the data acetone compositions for extract are not uniform with increase of
time. Based on the result, the pulsed column liquid-liquid extraction experiment determined the
required theoretical extraction stage. Four theoretical stages have been achieved. Higher pulsation
frequency values resulted in the breakdown of the dispersed phase drops which increased the
transfer of solvent mass. This proves that the mass transfer coefficient is improved by increasing
the frequency and amplitude of the pulse.

There several recommendations to avoid the errors and to obtain the best result. Firstly,
the refractive index should be calibrated before use. Secondly, use the correct glassware/
equipment to measure the solution to prevent from incorrect result. Furthermore, the equipment
should be services time by time to ensure the quality of result.

CLB 21204/TRANSPORT PROCESS PRINCIPLE/JAN 2019


CLB 21204 TRANSPORT PROCESS PRINCIPLE

REFERENCES

A.Todd, J. D. (2009). Liquid-Liquid Extraction Equipment. 14.

Akhtar (2007). Effect of operating parameters on extraction in sieve plate pulsed extraction

column. 189-196.

Berk, Z. (2013). Extraction. Food Process Engineering and Technology, 287–309. doi:

10.1016/b978-0-12-415923-5.00011-3

K. Najim &M.V. Le Lann. (2007). Control Of A Pulsed Liquid-Liquid Extraction Column Based On A

MultileVEL SYSTEM OF AUTOMATA. Chemical Engineering Communications, 70(1), 109-

112.

Pulsed Column Extractor. (2019). Retrieved October 23, 2019, from

https://www.stscanadainc.com/pulsed-column-extractor.html.

Tarikh Azis Ramadani, Fadilatul Taufany, Siti Nurkhamidah, Ali Altway. (2018). Study of packed

sieve tray column in ethanol purification using. Malaysian Journal of Fundamental and

Applied Sciences, Vol. 15, 69.

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CLB 21204 TRANSPORT PROCESS PRINCIPLE

APPENDICES

CALCULATION:
Weight percent acetone of the extract (toluene rich phase):

Weight percent acetone of the raffinate (water rich phase):

CLB 21204/TRANSPORT PROCESS PRINCIPLE/JAN 2019