Proposal

Defence
Purification of Biodiesel by Solvent-Aided Crystallization

Name : Farah Wahida Binti Jusoh

ID : 20237
Date : 1st November 2017
Supervisors name : Dr. Shafirah Binti Samsuri
Internal Examiners name : AP. Dr. Suriati Sufian
 Presentation Outline

Background of Study
Problem Statement
Objectives
Scope of study
Literature Review
Research Methodology
Gantt-chart
Project Activities & Key Milestones
Conclusion
 Background of Study
Malaysia has 4.49 million
hectares of palm oil
cultivation and producing
17.73 million tones of palm oil
and 2.13 tones of palm oil
kernel per year. Malaysia
gazette a total of 6 million
tonnes of palm oil to be used
as biofuel.
(Malaysian Palm Oil Council, 2017)
Figure : Palm Oil Fruit
Palm oil biodiesel production
per hectare is 27 times higher
compared to other oil seeds
such as rapeseed and
soybean
(Rahyla, Firdaus &
Purwamningrum,2017)
* Renewable, biodegradable,
non-toxic and safe
* Free of sulphur.
* Reducing sulphur dioxide,
hydrocarbons, carbon
monoxide and carbon
dioxide emissions, and
particulate matters.
* Has higher cetane number
(El-Araby et. al., 2017).
 Background of Study

2. Purification of crude
1. Can be produced by
biodiesel mandatory to
transesterification process,
comply with strict international
somehow it will produced by-
standards and follow ASTM
products as contaminants
standard specification.

Biodiesel

3. Conventional technologies
4. Research stated that via
used in biodiesel purification :
solvent-aided crystallization
Water washing, acid wash,
method, 99.9% of purity can
and washing with ether and Figure : Biodiesel comparison
be obtained.
adsorbents
 Problem Statement

High viscosity and low volatility in crude

biodiesel can cause problem to the forming of
deposition in the fuel engine fuel injector.

It is suggested that the addition of 1-butanol

as a solvent in solvent-aided crystallization
purification method can reduce the viscosity

Current research is focussing only on the

separation of glycerol and water. None this
kind of method has been implemented for
crude biodiesel purification.
 Objectives

To investigate purifications effectiveness of crude biodiesel via

solvent-aided crystallization method. Specific objectives are as follows:

To study the effect of 1-butanol on the efficiency of crude

biodiesel purification via solvent-aided crystallization
method.

To study the effect of operating parameters such as

coolant temperature and stirring rate on the efficiency of
crude biodiesel purification via solvent-aided crystallization
method.
 Scope of Study

The purifications effectiveness of crude biodiesel is evaluated by

1. comparing on the presence of 1-butanol and without the
presence of 1-butanol in the mixture.

2.
The purifications effectiveness of crude biodiesel is evaluated by
varying the coolant temperature in the refrigerated water bath

The purifications effectiveness of crude biodiesel is evaluated by

3. varying stirring rate of biodiesel with speed of 150, 250 and 350
rpm.
 Literature Review
El-Araby et al. (2017) mentioned that palm oil can be converted into biodiesel via
transesterification process whereby it a reaction between oil and alcohol in the
presence of catalyst to form ester and glycerol which has high cetane number.

Marx (2016) base-catalysed transesterification is used because the high conversions

obtained with a short reaction time at a relatively low cost.

Eisenbart, Angermeier, & Ulrich (2017), biodiesel and glycerol has high viscosity thus very
difficult to separate by other means which might cause few problems to the usage in
the diesel engine.

Okawa, Ito & Saito (2008) mentioned that freeze crystallization is a method to
concentrate the solution by making pure ice in solution and eliminating solute or
impurities.

Kim & Ulrich (2001) mentioned that factors such as temperature gradient and cooling
rate influencing crystals attribute.

Eisenbart Angermeier, & Ulrich (2017) solvent-aided layer crystallization is the use of an
additional assisting agent that is added to the melt insufficiently high amounts to
 Literature Review

According to Eisenbart & Ulrich (2015) and Eisenbart et. Al (2017), the two most
important quantities to evaluate the purification experiments are crystal growth,
G and distribution coefficient, k as shown in equation below :

G = r / t (1)
k= Xw,C / Xw,R (2)

r : Radius of equipment
t : Duration of experiment
Xw,C : Mass fraction of water in the growth crystal layer
Xw,R : The mass fraction of water in the residual melt.

Eistenbart and Ulrich (2015) mentioned that by adding 1-butanol, distribution

coefficient, k will be improved by a factor of 24 times meanwhile growth rates,
G could be increased by a factor 5 without harming the separation quality.
 Research Methodology

Methodology

1. Transesterification 2. Solvent-aided crystallization

* Melting point of biodiesel and glycerol different according to the method

used.
* Solvent-aided crystallization method will be proceed if the melting point of
glycerol and biodiesel shows a big different.
 Transesterification

I. 1000ml of palm oil will be heated in the

round bottom flask which equipped with
reflux condenser up to 65C.

II. 12.75g of potassium hydroxide (KOH) is

dissolved in 225ml of methanol (CH3OH).

III. The solution of KOH and CH3OH is then

added to the heated palm oil.

IV. The mixture will be stirred homogenously for

10 minutes.

V. Melting point of both biodiesel and glycerol

will be measured before proceeding with
solvent-aided crystallization method
Figure 1 : Transesterification apparatus arrangement
 Solvent-aided crystallization
I. 1-butanol will be added to the crude
biodiesel.
II. The vessel will be immersed inside
water bath which contain ethylene
glycol solution and water.
III. Stainless steel vessel will be immersed
three quarter (3/4) inside the water
bath.
IV. The temperature of water bath will be
changed and set at the cooling water
control panel.
V. Digital stirrer will be used in order to stir
the crude oil mixture.
VI. The mixture will be cooled until the ice
crystals stop growing.
VII. A stopwatch is used to record the time
of experiment.
Figure 2: Solvent-aided crystallization apparatus arrangement. VIII. The purity of crude biodiesel obtained
will be evaluated by using gas
chromatographymass spectrometry
(GC-MS) machines to evaluate the
data.
 Gantt-Chart
No. Detail/week 1 2 3 4 5 6 7 8 9 10 11 12 13 14

Selection of project
1
topic

2 Preliminary research work

Submission of chemical
3
requisition form

Submission of extended
3
proposal

4 Proposal defence

5 Project work continues

Submission of interim draft

6
report

7
Submission of interim report
Project Activities & Key Project Milestones
Week Process Action
1-2 Selection of project topic Discuss the feasibility and importance of the project
topic for both parties (Individual and Supervisor)
Topic selected :
Purification of biodiesel by solvent-aided crystallization
2-5 Preliminary research work Gather sufficient information from journal, book,
articles and website regarding the topic selected.
A medium such as Science Direct, Open Athens, Royal
Society of Engineering are being used
6 Submission of extended Evaluated by Supervisor FYP Coordinator/Committee
proposal
8 Proposal defence Preparation of presentation slides
Evaluated by Supervisor Internal Examiner, FYP
Coordinator
14 Submission of interim report Evaluated by Supervisor, Internal Examiner, FYP
Coordinator/Committee
 Conclusion
The addition of 1-butanol
in solvent-aided
crystallization increase the
purity and can reduce the
viscosity of biodiesel.
The main objectives of this project
is to determine the effectiveness of
1. crude biodiesel purification by
using solvent-aided crystallization
method.
2.
Previous research towards the
purification of glycerol and water
3. showed positive result on this
method. However, an
improvement from previous study is
expected from this research
Q&A
 References

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doi:https://doi.org/10.1016/j.renene.2013.02.035

Atadashi, I. M. (2015). Purification of crude biodiesel using dry washing and membrane technologies.
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Atadashi, I. M., Aroua, M. K., & Aziz, A. A. (2011). Biodiesel separation and purification: A review.
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Beierling, T., Micovic, J., Lutze, P., & Sadowski, G. (2014). Using complex layer melt crystallization models for
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Eisenbart, F., & Ulrich, J. (2015). Solvent-aided layer crystallizationCase study glycerolwater. Chemical
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Eisenbart, F. J., Angermeier, N., & Ulrich, J. (2017). Production of highly dry glycerol by solvent-aided melt
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 References

El-Araby, R., Amin, A., El Morsi, A. K., El-Ibiari, N. N., & El-Diwani, G. I. (2017). Study on the characteristics of
palm oilbiodieseldiesel fuel blend. Egyptian Journal of Petroleum.
doi:https://doi.org/10.1016/j.ejpe.2017.03.002

He, Q., McNutt, J., & Yang, J. (2017). Utilization of the residual glycerol from biodiesel production for
renewable energy generation. Renewable and Sustainable Energy Reviews, 71(Supplement C), 63-76.
doi:https://doi.org/10.1016/j.rser.2016.12.110

James, C. S. (April 3, 2017). Biodiesel production becoming a zero-sum game. Latin American Energy
Review: Intelligent debate on energy issues.

Kim, K.-J., & Ulrich, J. (2001). Purification of crystalline layers by controlling the temperature gradient.
Powder Technology, 121(1), 81-87. doi:https://doi.org/10.1016/S0032-5910 (01)00383-7

Knothe, G., & Razon, L. F. (2017). Biodiesel fuels. Progress in Energy and Combustion Science,
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Leoneti, A. B., Arago-Leoneti, V., & de Oliveira, S. V. W. B. (2012). Glycerol as a by-product of biodiesel
production in Brazil: Alternatives for the use of unrefined glycerol. Renewable Energy, 45(Supplement
C), 138-145. doi:https://doi.org/10.1016/j.renene.2012.02.032
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