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Production of Biolubricant from Castor Oil

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

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
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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

1 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 methods, and some of these wastes are not degradable thereby contaminating the
2

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.

2 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.
 3

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 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.

3 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.

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

Esterification Times
Crude Castor 1st 2nd 3rd 4th 5th
Mass of Oil Sample A (g) 04.00 500.00 450.00 447.70 301.60 254.10
Titre Value (cm3) 1st 22.20 06.20 01.90 00.50 00.80 00.30
2nd 24.00 04.90 01.80 00.50 00.90 00.20
FFA% 1st 62.27 17.39 05.05 01.40 02.24 00.84
2nd 67.32 13.74 05.33 01.40 02.52 00.56
Mass of Oil Sample B (g) 04.00 360.60 375.90 384.20
Titre Value (cm3) 1st 08.30 05.30 02.40 00.20
2nd 08.60 05.40 02.40 00.10
FFA% 1st 23.28 14.87 06.73 00.56
2nd 24.12 15.15 06.73 00.28
Mass of Oil Sample C (g) 04.00 250.00 304.00 325.40
Titre Value (cm3) 1st 35.30 03.00 01.60 00.20
2nd 33.50 03.00 01.60 00.20
FFA% 1st 98.74 08.42 04.49 00.56
2nd 93.97 07.42 03.37 00.56

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.
4

Table 2: Sumarry of Esterification Results

Sample A (FFA%) Sample B (FFA%) Sample C (FFA%)
1 2 1 2 1 2
Crude Castor 62.27 67.32 23.28 24.12 98.74 93.97
Esterification Times 1st 17.39 13.74 14.87 15.15 08.42 08.42
2nd 05.05 05.33 06.73 06.73 04.49 03.37
3rd 01.40 01.40 00.56 00.28 00.56 00.56
4th 02.24 02.52
5th 00.84 00.56

SAMPLE A
Series1 Series2 Series3

80
PERCENTAGE FFA (%)

60

40

20

0
CC 1ST 2ND 3RD 4TH 5TH
ESTERIFICATION (HOURS)

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

SAMPLE B
Series1 Series2

30
PERCENTAGE FFA (%)

25
20
15
10
5
0
CC 1ST 2ND 3RD 4TH 5TH
ESTERIFICATION (HOURS)

Figure 2: Graph of % FFA versus Number of Esterification Times (hours) for sample B
 5

SAMPLE C
Series1 Series2

120

100
PERCENTAGE FFA(%)

80

60

40

20

0
CC 1ST 2ND 3RD 4TH 5TH
ESTERIFICATION (HOURS)

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

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.

Table 3: Amount of Regents Used for Transestrification

Sample A Sample B Sample C
Mass of Oil (g) 224.10 437.50 302.10
Methanol (w/w 10.8%) 24.20 47.25 32.60
NaOH (w/w 1.2%) 02.24 04.80 00.36

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 4: Biodiesel %FFA

Sample A Sample B Sample C
Mass of Biodiesel (g) 97.10 129.80 142.3
Titre Values (cm3) 00.30 00.30 00.30
% FFA 00.84 00.84 00.84

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
6

biolubricant from sample A, B and C respectively as shown in Table 5.

Table 5: Quantity of Biolubricant Samples Produced

Sample A (g) Sample B (g) Sample C (g)
Biodiesel 77.90 109.20 141.40
Sodium Lauryl Sulphate (15% Biodiesel) 11.69 16.38 21.21
Biolubricant Produced 88.76 125.23 162.61

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

Properties Test Method Crude Castor Sample A Sample B Sample C Motorlube SAE 40
Physical Appearance Dark Bright and Clear Bright and Clear Bright and Clear Bright and Clear
Colour ASTM D2622 L4.0 Dil ASTM L3.5 Dil ASTM L3.5 Dil ASTM L3.5 Dil ASTM L3.5 ASTM
Odour Soupy Odour Soupy Odour Soupy Odour
Solubility in Water Insoluble Insoluble Insoluble Insoluble
Specific Gravity (15oC) ASTM D4052 0.8522 0.8452 0.8323 0.8323 0.8755
Kinematic Viscosity (40oC) cSt ASTM D445 256.17 89.68 67.24 58.01 130.22
Kinematic Viscosity (100oC) cSt ASTM D446 22.78 08.14 07.92 07.59 14.42
Viscosity Index ASTM D2270 109 32 78 91 110
Flash Point (oC) ASTM D93 296 215 211 223 260
Pour point (oC) ASTM D97 -12 -21 -18 -12 -12
Acid Value (mg KOH/mg) ASTM D74 187.94 01.12 00.56 01.12
FFA% 93.97 00.56 00.28 00.56
Reactivity Stable but avoid strong oxidizing agents
Biodegradability All the Biolubricants are more biodegradable than Petroleum Lubricants Not Biodegradable

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.

KV AT 40˚C/100˚C OF SAMPLES
100
KINEMATIC VISCOSITIES (40˚c/100˚c)

80

60

40

20

0
A B C
SAMPLES

Series1 Series2

Figure 4: Kinematic Viscosity of Samples at 40˚C and 100˚C

 7

VISCOSITY INDEX OF SAMPLES

100
90
80
VISCOSITY INDEX

70
60
50
40
30
20
10
0
A B C
SAMPLES

Figure 5: Viscosity Index of Samples

POUR POINT OF SAMPLES

-16.5
-17 A B C
-17.5
POUR POINT (˚C)

-18
-18.5
-19
-19.5
-20
-20.5
-21
-21.5
SAMPLES

Figure 6: Pour Point of Samples

8

FLASH POINT OF SAMPLES

225

FLASH POINT (˚C)

220

215

210

205
A B C
SAMPLES

Figure 7: Flash Point of Samples

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.

4 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 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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