SPE-189183-MS

Production of Biolubricant From Castor Oil

Ibrahim N. Dibal and Paul C. Okonkwo, Department of Chemical Engineering, Ahmadu Bello University Zaria;
Ibrahim Haruna, National Research Institute for Chemical Technology Zaria

Copyright 2017, Society of Petroleum Engineers

This paper was prepared for presentation at the Nigeria Annual International Conference and Exhibition held in Lagos, Nigeria, 31 July – 2 August 2017.

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Abstract
In this research, bio-lubricant was produced from castor oil in two stage processes where methyl ester of the
oil was produced by esterification and then transesterified using homogenous catalyst (NaOH). It was then
blended with 15w/w% of Sodium Lauryl Sulphate (SLS) to produce bio-lubricant. By varying the amount
of homogenous catalyst (1.0-1.2 w/w %), three (3) different grades of bio-lubricant samples were produced
and subjected to physical and chemical test to determine their characteristics. The three grades of the bio-
lubricant samples weighs 88.76g, 125.23g and 162.61g respectively with varying degrees of kinematic
viscosity of 89.68, 67.24 and 58.01cst respectively at 40°C, and 8.14, 7.92 and 7.59cst respectively at 100°C.
The viscosity indexes of the three samples are; 32, 78 and 91, pour points are −21, −18 and −18°C, and the
flash points are 215, 211 and 223°C respectively for each of the samples. The properties of the biolubricant
samples indicates that they can be used under wide range temperatures. Our results are comparable with
mineral based lubricant standards of Motorlube (SAE 20W40).
Keywords: Castor oil, Sodium Lauryl Sulphate, Motorlube, Bio-lubricant, Transesterified, Esterification

Introduction
The quest for sustainable development due to increasing environmental challenges have increased the
interest in the search of renewable, biodegradable and, environmentally friendly products and processes’
development (Sahoo et al., 2007; Basha et al., 2009; Demirbas, 2009; Refaat, 2010; Yang et al., 2012).
The increasing demands depleting fossil fuel energy reserves, cost of production and the overall damage to
the environment fuelled the search for renewable sources of energy and other products which has resulted
in significant discoveries. Solar, hydro and vegetables have contributed significantly in meeting the global
demands for renewable energy. The bio-degradable fuel and lubricants made from vegetables and cereals
based oils usually comprise of 60–99% base oil, and the remaining are additives which varies depending
on the desired level of performance (Wagner et al., 2001, Jacques et al., 1997). The use of biodegradable
and environmentally accepted lubricants from vegetable oil has increased over the past 25 years (Willing,
2001), however, dependence on consumable vegetables and cereals for biodegradable fuel and lubricants has
far reaching implications on sustainable development. The greatest challenge of fossil fuels and lubricants
is that millions of tons are dumped into the environment annually through leakages and careless disposal
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methods, and some of these wastes are not degradable thereby contaminating the environment. The major
issues researchers are faced with in the lubricant industry are; the search for renewable raw materials that
can be used for lubricant production and the development of products that are biodegradable (Silva, 2011).
The usage of vegetables and cereals oils (mainly triglycerides), which contains three hydroxyl groups
and long chain unsaturated free fatty acids attached at the hydroxyl group by ester linkages (Fox and
Stachowiak, 2007; Waleska et al., 2005), have to be balanced between the needs for human and animal
consumption, and the derive for energy generation. Although vegetable and cereal oils are commonly used
as bio-fuel, currently they are not widely used as lubricant base oils largely due to their undesirable physical
properties which include; high melting point and insufficient thermal oxidative stability (Uosukainen et
al., 1998). The chemical properties of bio-oils can be modified to improve their thermal, oxidative and
hydrolytic stabilities, however the effects of such modified lubricants on the environment has not been
fully studied and documented. The most important modifications occur on the carboxyl groups of the fatty
acids which is approximately 90%, while oleo chemical reactions on the fatty acid chain are approximately
10% (Fox, and Stachowiak, 2007). Various studies have been carried out using different vegetables and
cereal oils (Bilal, et al., 2013; Wan, 2012; Srivastava and Sahai, 2013; Yusuf, et al., 2015; Jieyu, 2012).
The vegetable and cereals oils are classified into two; those edible by human being and animals and those
that are not edible. In our quest for sustainable development, the non-edible (castor seed) seed oil having
homogeneous catalyst was used to develop biolubricant balancing the needs for human consumption and
sustainanable energy demands. This research is focused on the development of biodegradable lubricants
from renewable sources using non-edible plant seed (castor seed), this is aimed at reducing pressure on
the increasing demands for consumable oils and guarantee sustainability. The overall target of this research
work is the reduction of the over dependence on fossil fuel thereby encouraging sustainable and environment
friendly development. Processing castor seed oil into lubricant will save foreign exchange and create job
opportunities. The multiplier effect of the gains could be replicated using other non-edible seed.

Materials and Method

Castor oil extracted from castor seed using traditional method of extraction was obtained, 500 ml was used
for the research using facilities at the Department of Chemical Engineering, Ahmadu Bello University,
Zaria and National Research Institute for Chemical Technology (NARICT), Zaria. Methanol and Sodium
hydroxide (NaOH) was used as homogeneous catalyst, and the test study chemicals were: Potassium
hydroxide (KOH), Phenolphthalein, Propan-2-ol, and Distilled water for acid value test. The carboxyl group
of the castor oil was modified by transesterification using methanol in the presence of sodium hydroxide as
a catalyst to break the molecule of the raw vegetable oil into methyl esters with glycerol as a by-product.
Few transesterification reactions are reported with higher alcohols C8 to C14, for use as lubricants (Whitby,
2005), transesterification may be affected by the mode of reaction, molar ratio of alcohol to oil, type of
alcohol, nature and amount of catalysts, reaction time, and temperature (Knothe, 2005).
The chemical and physical properties of the crude castor oil was determined to confirm its suitability
for the production of lubricant, this enable us apply the requisite standards in the conversion of the oil to
lubricant. Using small sample of the crude castor oil, the acidic value of the crude castor oil, percentage
free fatty acid (% FFA), and the density of the oil were determined by sample/sample volume in SI units.
The oil sample was put in viscometer tube and allowed in bath for 30 minutes at 40°C and 100 ºC so that it
attains the bath temperature. The above procedure was replicated four times so as to reduce variation. The
specimen is then cooled to allow for the formation of paraffin wax crystals to enable us determine the pour
point temperature, readings were taken at 3°C intervals to determine the pour oint temperature.
Details of the procedure involved in the conversion of castor oil to biolubricant is outlined as follows;
methyl ester was prepared using purified castor oil (esterified castor oil) and methanol with a homogeneous
catalyst of sodium hydroxide (NaOH). Having esterified the castor oil, the % free fatty acid was reduced to
SPE-189183-MS 3

a value less than 0.5% and further transesterification was carried out by pouring about 300g of castor seed
oil into a conical flask. The reactor assembly was then heated to temperature of 60°C, (10.8% mass of oil
(g)) of methanol and (1-1.2% of the mass of oil (g)) of homogeneous catalyst i.e. NaOH was added to the
reactor. Finally, after transesterification was carried out, the catalyst and glycerol parts were separated from
the methyl Easter mixture, then the methyl ester mixture was washed using hot distilled water. Thereafter,
the unreacted methanol and trace moisture was removed by heating to a temperature above 100°C. The
methyl ester was obtained as a clear amber-yellow liquid. Sodium lauryl sulphate (SLS) was used in order
to improve its characteristic. For this process 15% SLS were mixed with fatty acid methyl ester. This
mixture was blended until foam formation stabilizes and the additives completely solubilize in the ester by
continuous heating.

Results and Discussion

The crude crude castor oil was analysed to determine its chemical and physical properties using three
samples and the initial % FFA was found to be 67.32, 24.12 and 93.97 for sample A, B and C respectively.
The crude castor samples were esterified within at an interval of 1 hour using methanol (30w/w%) and
H2SO4 (1w/w%) as the catalyst to reduce the % FFA to a value of about 0.5. The esterification of the crude
castor samples were done iteratively for five times as shown in Table 1 where the titre values were obtained
for the determination of % FFA of sample A, B,and C. The five iterations consist of 3 turns using the drastic
esterification method and mild esterification methods for the last 2 times. The process was repeated twice
in the determination of % FFA values to reduce variation. The results in Table 1 shows the drastic reduction
of the Free Fatty Acid of each of the three samples, and Table 2 gives the summary of esterification results
for samples A, B and C showing the % FFA respectively.

Table 1—Esterification Results for Samples A, B and C

4 SPE-189183-MS

Table 2—Sumarry of Esterification Results

Figures 1-3 shows the graphs of the % FFA versus Number of Esterification times for samples A, B and
C, where the values were drastically reduced to 0.56, 0.28 and 0.56 for the three samples respectively.

Figure 1—Graph of %FFA versus Number of Esterification Times (hours) for sample A

Figure 2—Graph of % FFA versus Number of Esterification Times (hours) for sample B
SPE-189183-MS 5

Figure 3—Graph of % FFA versus Number of Esterification Times (hours) for sample C

Samples A, B and C were transesterified after esterification using methanol and sodium hydroxide
(NaOH) as homogenous catalyst. The amount of catalyst used was varied from (1.0-1.2% of the mass of
oil) and that of methanol (10.8 % of the mass of oil) as shown in Table 3 above.

Table 3—Amount of Regents Used for Transestrification

The amount of biodiesel produced from samples A, B and C were 91.7g, 129.8g and 142.3g respectively.
Table 4 also shows the titre values obtained for the determination of the % FFA of the biodiesel. The biodiesel
samples produced (samples A, B and C) were blended with Sodium Lauryl Sulphate (SLS) to improve the
properties of the biolubricant. The process yields 88.76g, 125.23g and 162.61g amount of biolubricant from
sample A, B and C respectively as shown in Table 5.

Table 4—Biodiesel %FFA

6 SPE-189183-MS

Table 5—Quantity of Biolubricant Samples Produced

Table 6 shows the summary of the physical and chemical properties of the biolubricants produced for
samples A, B and C where the best sample (C) was compared with the mineral based lubricant (Motorlube
SAE 40). The biolubricant properties; viscosity, density, flashpoint and pour point were determined using
ASTM standards. The kinematic viscosities of the three samples at 40°C are 89.68, 67.24 and 58.01cst
respectively, and at 100°C the values are 8.14, 7.92 and 7.59cst respectively resulting in the following
viscosity index as 32, 78 and 91 respectively. The pour point and the flash point for the three samples also
varies as presented in Table 6. The properties of the best biolubricant produced (sample C) compares very
well to the mineral based lubricant (Motorlube SAE 40) thereby conforming to the SAE standard.

Table 6—Physical and Chemical Properties of Biolubricant Samples A, B and C

Figures 4, 5, 6 and 7 shows the graphical variation of the kinematic viscosities at 40°C and 100°C
respectively, viscosity index, pour point and flash point of the three (3) biolubricant samples.

Figure 4—Kinematic Viscosity of Samples at 40°C and 100°C

SPE-189183-MS 7

Figure 5—Viscosity Index of Samples

Figure 6—Pour Point of Samples

Figure 7—Flash Point of Samples

Conclusion
The biodiesel produced from castor oil was blended with Sodium Lauryl Sulphate (SLS) to improve the
properties of the biolubricant. With varying quantities of the catalyst used, the biolubricant samples A, B
and C showed varying degrees of the kinematic viscosities, flash point, pour point and viscosity index. The
8 SPE-189183-MS

biolubricant sample C produced was the best among the three variants of the biolubricants produced, its
chemical and physical properties compares very well to the SAE standards for mineral based lubricants
(Motorlube SAE 20W40). The findings of this research indicate that better results could be obtained when
additional secondary additive known as Cocamidopropylbetaine butadiene is used, however due to its
scarcity commercially, this leaves an opening for further research, and enzymatic synthesis of biolubricants
will also be an interesting area for future biolubricant production.

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