FACULTY OF CHEMICAL ENGINEERING

UNIVERSITI TEKNOLOGI MALAYSIA

POLLUTION CONTROL & CHEMICAL REACTION

ENGINEERING LABORATORY

BIODIESEL SYNTHESIS (E6)

No of Experiment 6

Group Number 3

Group Members Amiruddin b Mohd Tajudin

(A11KK0036)
Muhamad Fahmi b Che Ani
(A11KK0002)
Khairul Zaid b Jamaludin
(A11KK0005)
Muhamad Khairul Afandi b Ab Aziz
(A11KK0021)
Date of Experiment 25 November 2013

Date of Submission 16 December 2013

Marks obtained

Lecturer’s Name DR. NORAINI BT. JAAFAR

ABSTRACT

Biodiesel, defined as monoalkyl ester is an alternative fuel for diesel engines that is
biodegradable and can contribute to alleviate environmental pollution. This experiment requires
the researching and learning of a method to produce biodiesel from palm oil on a laboratory
scale. In this work, it is prepared by using crude palm oil and methoxide. Palm oil is reacted
with methanol, catalyzed by sodium hydroxide (NaOH) lye through a process called
transesterification. The heating temperature of the palm oil before the addition of methoxide is
60 ºC. The mixture is then to be settled for almost 1 hour. This process involves the breaking
up of the triglyceride chain in palm oil and combination of each chain with methanol, isolating
out glycerine. When mixing and reaction are finally complete, the ester (biodiesel) and
glycerine will isolate themselves away as two separate liquid phases. They are separated by
draining off the bottom layer which is glycerine layer.
The biodiesel layer is collected and weighed after 1 hour. The biodiesel produced in this
experiment for 3:1 ratio and 5:1 ratio were 79.11g and 115.45g respectively. The yield product
of 3:1 ratio and 5:1 ratio were 59.4% and 86.72% respectively.
 Table of Content

No Content

1.0 Introduction

2.0 Literature Review

3.0 Methodology

4.0 Results

5.0 Discussion

6.0 Conclusion

7.0 References
1.0 INTRODUCTION

1.1 Background of The Experiment

For more than two centuries, the world’s energy supply has relied heavily on no-
renewable fossil fuels. 90% of the fossil fuels were consumed for generation of energy and
transportation purposes. It is also known that emissions from the combustion of these fuels such
as carbon dioxide and carbon monoxide will contribute various environmental problem for
example , global warming.
This situation has initiated and sustained interest in identifying and channelling
renewable raw materials especially biomass into manufacture of liquid fuel alternatives.
Besides, development of such product would ensure that new technologies are available to keep
pace with society’s need for new renewable energy alternatives in the future.
Biodiesel (fatty acid alkyl esters) is an alternative fuel for diesel engines. It is an alcohol
ester product from the transesterification of triglycerides in vegetable oils or animal fats. This
can be accomplished by reacting lower alcohols such as methanol or ethanol with triglycerides.
The reaction proceeds well in the presence of some homogeneous catalysts such as sodium
hydroxide. This study is carried out to study the effect of quantities of methanol to the
production of biodiesel from methanol and crude palm oil.

1.2 Objective of The Experiment

 To study the lab-scale production of biodiesel from palm oil, methanol and sodium
hydroxide.

1.3 Scope of Experiment

 Using the most common route of biodiesel production via base catalyzed trans-
esterification
 Using a simple technique in small scale production of biodiesel
 Compare biodiesel production by using different ratio
2.0 LITERATURE REVIEW

The United States is the largest single consumer of fossil fuels in the world. Each year,
the U.S. consumes 125 billion gallons of gasoline and 60 billion gallons of diesel fuel. It is
desired to find alternative feedstock due to high current energy consumption. One such
alternative feedstock is vegetable oil. Vegetable oil offers the benefits of a greener synthetic
route for obtaining diesel fuel. This fuel source is known as biodiesel, and can be synthesized
on an individual level or on an industrial scale.
Biodiesel is a biodegradable fuel and the fact that engines running on biodiesel do not
emit black smoke can help to improve current environmental pollution problems caused by
fossil fuels. In fact, biodiesel possesses fuel properties comparable to those of petroleum diesel.
The biodiesel process turns the oil into ester, separating out the glycerine, which sinks to the
bottom while the biodiesel floats on top. This process is called transesterification.
In the transesterification of different types of oils, triglycerides react with an alcohol,
generally methanol or ethanol, to produce esters and glycerin. To make it possible, a catalyst is
added to the reaction.

The overall process is normally a sequence of three consecutive steps, which are
reversible reactions. In the first step, from triglycerides, diglyceride is obtained, then from
diglyceride, monoglycerides is produced and in the last step, from monoglycerides, glycerin is
obtained. In all these reactions esters are produced. The sequences reactions are shown below:
  Triglycerides (TG) + R’OH ↔ Diglycerides (DG) + R’COOR1
 Diglyceride (DG) + R’OH ↔ Monoglycerides (MG) + R’COOR2
 Monoglycerides (MG) + R’OH ↔ Glycerin (GL) + R’COOR3

In the first step of the reaction, NaOH reacts with methanol in an acid-base reaction.
The product of this reaction is the very strong base sodium methoxide and water. In the second
step, the sodium methoxide acts as a nucleophile and attacks the three carbonyl carbons of the
vegetable oil. This produces a tetrahedral intermediate that is highly unstable which also called
the "cracking" of the triglyceride. The elimination of the glycerol backbone leads to the
formation of the three methyl esters (the biodiesel) and glycerol.
The NaOH is reproduced as a product in the reaction. If the biodiesel is removed from
the mixture, glycerol and unreacted NaOH and methanol remain. The glycerol can be converted
to soap through a saponification reaction if excess NaOH is used. Excessive amount of NaOH
will produce a jelly like mix of glycerol and soap.
For a basic catalyst, sodium hydroxide (NaOH) or potassium hydroxide (KOH) should
be used with methanol or ethanol as well as any kind of oils. Alcoxy is produced before the
reaction to obtain a better efficiency. The alcoxi reaction is

R-CH2OH + NaOH → H2O + R-CH2ONa

The alcohol–oil molar ratio that should be used varies from N =1:1–6:1. However N =
6:1 is the most used ratio conversion for the alkali catalyst without using a great amount of
alcohol. The types of alcohol are usually methanol and ethanol which is less toxic. As raw
materials, the oils used could come from any vegetable, e.g., corn, canola, peanut, sunflower,
soybean, olive, palm, or palm kernel.
The amount of catalyst that should be added is any values between 0.005% and
0.35%w/w. Besides that, one important variable is the reaction temperature. The standard
temperature for the reaction to take place is 60⁰C, but depending on the type of catalyst used
because different temperatures will give different degrees of conversion. Other examples of
catalysts are tabulated in Table 1.
 Table 1: Experimental conversions to methyl ester for different catalysts
CATALYST CATALYST TYPE CONVERSION (%)
NaOH Strongly basic 100.0
Amberlyst A26 Anion-exchange resin 0.1
Amberlyst A27 Anion-exchange resin 0.4
Amberlyst 15 Cation-exchange resin 0.7
MELCat XZO682:01 Sulphate doped zirconium hydroxide 0.0
MELCat XZO645:01 Silica doped zirconium hydroxide 0.0
TIS Titanium silicate 0.6
TILCOM STC Titanium chelate 0.5
SnCl2 Lewis acid 3.0
MgO Metallic oxide 11.0
USY-292 Zeolite 0.2
Novozym 435 Immobilized lipase 0.0
3.0 METHODOLOGY

3.1 Apparatus
Aluminium foils, beaker, electronic balance, hot plate magnetic stirrer, measuring cylinder,
separating funnel, thermometer,

3.2 Materials
Palm oil, methanol, sodium hydroxide powder, distilled water

3.3 Procedure
1. Mass of sodium hydroxide powder needed is weighed in a beaker and the volume of
methanol needed is measured using measuring cylinder.
2. Methanol is added into a beaker and stirred using hot plate magnetic stirrer until sodium
hydroxide powder completely dissolves. The reaction produces sodium methoxide.
3. Volume of palm oil needed is measured using measuring cylinder and transfer to the
beaker to be warm up to 55 ºC using hot plate magnetic stirrer.
4. Maintain temperature at 55 ºC and allow the stirrer continue to run while sodium
methoxide is added to the beaker.
5. The beaker is then covered with aluminium foil and stir rapidly for 30 minutes.
6. Let the compounds cooled for a while.
7. Transfer the contents of the flask into a separating funnel and set aside for 30 minutes
for separation to take place.
8. The lower layer of glycerin is drain off and wash the upper layer of crude biodiesel with
distilled water.
9. The lower layer of water is drains off and the biodiesel is collected in another beaker to
be weighing using electronic balance.
10. The result is recorded in a table.
4.0 RESULTS

4.1 Amount of Reactant Used

Volume of palm oil (mL) = 150 mL

Weight of palm oil = 150mL x ρ
= 150mL x 0.8875g/mL
= 133.13g
Weight of catalyst, NaOH (g) = 2.66g

Samples A B
Molar ratio methanol to palm oil 3:1 5:1
Volume of methanol (mL) 19 32

4.2 Data obtained

Samples A B
Weight of empty beaker (g) 50.85 51.25
Weight of beaker + product (g) 129.96 166.7
Weight of product (g) 79.11 115.45
Percentage yield (%) 59.4 86.72
5.0 DISCUSSION

According to the stoichiometric, 3 moles of methanol for each mole of glycerides (palm
oil) is required to yield 3 moles of fatty acid methyl ester and 1 mole of glycerol. In the
experiment, the ratio of methanol: oil was set at 3: 1 and 5: 1. This is because excess methanol
is required in driving the reaction towards the end product, due to the factor transesterification
process as a reversible reaction. Supported by most literature, the conversion increases as the
mole ratio of methanol oil increases. However, there is a maximum ratio. Further increase in
methanol to FFA molar ratio conversion does not increase (Rakib Uddin et al, 2012).
In this experiment, it was observed that there were two layers formed in the separating
funnel after palm oil mixture is left for about half and hour. The pale yellow upper layer was
biodiesel while the dark color bottom layer was glycerin.
The biodiesel weight for molar ratio methanol to palm oil 3:1 and 5:1 are 79.11g and
115.45g respectively. Based on the value obtained, it shows that 5:1 ratio produce more yield
which is 86.72% compared to 3:1 ratio which produced only 59.4%. Thus, it was proved that
the higher the molar ratio of methanol to palm oil, the higher the yield.
However, in this experiment, it is found that there were some precaution need to be taken
into the account. This is very important to increase the production of biodiesel. One of the errors
was due to the absorption of moisture in NaOH pellets during the measuring and stirring
processes that may affect the reaction. The NaOH pellets were rapidly absorbing moisture from
the atmosphere especially while taken too long time to weight the NaOH pellets.. Besides that,
the pellets were dissolved in a beaker which was exposed to the atmosphere and were hard to
dissolve and left some residues which caused impurities in the biodiesel obtained. Another error
in this experiment was caused by the low temperature of surrounding. During the settling
process, the glycerine layer was hardened and become gel which caused difficulties in draining
off the byproducts. Thus, the weight of biodiesel obtained might not be accurate.
Thus, there were some of suggestion that can be done in order to get more accurate result.
Firstly, NaOH pellets and methanol should be handled quickly during the measuring and stirring
processes to avoid moisture being absorbed to them and can be done in fume cupboard.
Secondly, it is also important to ensure that the methoxide solution and palm oil were well
mixed and reaction was complete. Lastly, while draining off the byproducts, careful handling
the biodiesel to avoid any impurities and wastage

6.0 CONCLUSION
Biodiesel can be produced from palm oil by transesterification with methanol and catalyzed
by sodium hydroxide. Through transesterification, palm oil reacts with methanol to form
biodiesel and glycerine, which are two separable liquids. The pale yellow upper layer is
biodiesel while the dark colour bottom layer is glycerine byproducts. The biodiesel produced
in this experiment for 3:1 ratio and 5:1 ratio were 79.11g and 115.45g respectively. The yield
product of 3:1 ratio and 5:1 ratio were 59.4% and 86.72% respectively.

7.0 REFERENCES

Choo, Y.M., Ma, A. N., Chan, K.W., and Yusof Basiron, 2005, Palm Diesel: An Option For
Greenhouse Gas Mitigation In The Energy Sector: Journal of Oil Palm Research, v. 17, p.
47-52.

Dott, R.H. Jr., and Bourgeois, Joanne, 1982, Hummocky stratification: Significance and its
variable bedding sequences: Bulletin Geological Society of America, v. 93, p. 663-680.

Marchetti, J.M., Miguel, V.U., and Errazu, A.F., 2007, Possible methods for biodiesel
production: Renewable and Sustainable Energy Reviews, v. 11, p. 1300 – 1311.

Crabbe, E., Nolasco-Hipolito, C., Kobayashi, G., Sonomoto, K., and Ishizaki, A., 2001,
Biodiesel production from crude palm oil and evaluation of butanol extraction and fuel
properties: Process Biochemistry, v. 37, p. 65 – 71.

Kim, H.J., Kang, B.S., Kim, M.J., Park, Y.M., Kim, D.K., Lee, J.S., and Lee, K.Y., 2004,
Transesterification of vegetable oil to biodiesel using heterogeneous base catalyst: Catalysis
Today, v. 93–95, p. 315–320