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Sodium grease formulation from waste engine oil

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2019 9th International Conference on Future Environment and Energy IOP Publishing
IOP Conf. Series: Earth and Environmental Science 257 (2019) 012018 doi:10.1088/1755-1315/257/1/012018

Sodium grease formulation from waste engine oil

N W Abdu Rahman1, N S A Japar1,2, M A A Aziz1, A H A Razik1 and M Y M

Yunus3

1 Faculty of Chemical and Natural Resources Engineering, Universiti Malaysia

Pahang, Kuantan, Pahang, Malaysia
2 Institute of Postgraduate Studies, Universiti Malaysia Pahang, Kuantan, Pahang,
Malaysia
3 Earth Resources Sustainability Centre (ERAS), Universiti Malaysia Pahang, Kuantan,
Pahang, Malaysia

E-mail: maizudin@ump.edu.my

Abstract. The present study was conducted to formulate sodium soap grease using waste
engine oil (WEO). Greases were formulated by homogenizing sodium soap thickener in WEO
for 2 hours at 150°C Different grease composition of oil-to-thickener ratio was designed which
are 90/10, 80/20, 70/30 and 60/40. The formulated greases were analysed by conducting the
consistency, oil bleeding, oil separation and FTIR characterization tests. The present study
found that grease can be formulated using WEO and the thickener percentage have significant
effect on formulated greases properties. Grease formulated with 70 – 80% of base oil and 20 –
30% of thickener was the best grease formulated as it shows desirable grease properties.

1. Introduction
Lubricating grease is a semi-solid material representing a dispersion of a thickener in a liquid lubricant
[1]. It consist of three component which are oil, thickener and additives. Additives and base oil play
the major roles in the grease formulation while the thickener is referred to as a sponge that hold the
lubricant together. Mineral oil are often used in grease production as their fluid component. However,
a better stability can be find in synthetic base oil during extreme temperature (high or low) [2]. To set
the grease apart from the fluid lubricants, the thickener is used. Thickeners are molecules, polymers or
particles that are partially soluble in lubricating fluid.
Earliest production of grease is from the early Egyptian or Roman eras by combining lime with oil.
The product of this saponification produce calcium grease when the lime saponified the triglyceride
that comprises oil. Starting from that, the development of thickeners have a big impact in grease
technology. Lithium thickener has dominated approximately 70% of the grease today [3]. They
searched for additives that are used to extend the capabilities of the basic product. However, this
concept which is over 60 years old invented by Clarence Earle in the 1940’s are the base of a current
grease production. The formulator in the 1970’s and 1980’s target was one single grease which would
be capable of a superior performance in a wide range application, temperature and environment.
Unfortunately, it was too expensive to used multi-purposed grease for a basic application.
In modern days, the impact of grease production has increase environmentally and economically. As
the production and consumption of oil is high every day, the disposal of the waste can give negative
impact to the environment. This also bad for the environment as all the waste oil are categorized as the
scheduled waste [4]. As the raw material for the grease production is a base oil, using waste oil can

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2019 9th International Conference on Future Environment and Energy IOP Publishing
IOP Conf. Series: Earth and Environmental Science 257 (2019) 012018 doi:10.1088/1755-1315/257/1/012018

reduce the numbers of waste oil that are being disposed to the landfill. It also can help to save the
production cost of the grease as the composition of grease consist of 70%-90% of base oil.
Recycling waste oil to replace the base oil can reduce the production cost as the waste oil is much
cheaper in price [5]. The main purpose of this study is to design formulation of soap base grease and
the production of grease by utilizing waste engine oil.

2. Methodology

2.1. Materials
In this study, waste engine oil is used as base oil. The thickener used in this experiment will be sodium
soap thickener. The sodium hydroxide will undergoes saponification process with stearic acid to
produces sodium soap thickener. Stearic acid is one of the material needed for saponification process
that have a long-chain fatty acid consisting of 18 carbon atoms without double bonds. In nature stearic
acid occurs primarily as a mixed triglyceride, or fat, with other long-chain acids and as an ester of a
fatty alcohol.

2.2. Pre-treatment of waste oil

Waste oil will undergoes pre-treatment in order to remove any impurities and water in the oil. Two
step involves in the treatment which are filtering process and heating process. For filtering process, the
oil will be filtered by using filter paper to remove any small impurities in the oil. Then the oil will
undergoes second process which is heating the oil until the temperature higher than 90˚C with
continuous stirring to remove water in the oil. This process will take about 1 hour with a temperature
higher than 150˚C.

2.3. Formulation of soap base grease

In this formulation waste oil was utilized around 60 to 90 wt% and 10 to 40% of sodium soap
thickener was dispersed in the waste engine oil (WEO). The WEO was heated to > 90˚C and stearic
acid was melted at 60˚C. 70% of the heated oil was transferred into the melted stearic acid and
homogenized for about 15 minutes. 6M NaOH solution was then added into the mixture drop by drop
to control excessive foaming at low speed. After the addition of NaOH, the temperature was increased
to 150°C and homogenized for 30minutes. The oil balances were then added completely to the mixture
and homogenized for 2 hours at high speed of 8000rpm and constant temperature. Finally, heat was
removed from the sample and homogenization was continued for another 30 minutes. Grease sample
was stored in an enclosed container and allowed to cool to room temperature for 2 days.

2.4. Analysis of grease

2.4.1. Consistency. Consistency test was carried out to evaluate the level of softness and firmness of
the grease ranging from NLGI number 000 to 6 using SKF grease testing kit.

2.4.2. Oil bleeding. Oil bleeding test was conducted to study the oil bleeding area if the grease for
fresh and used grease. In this test, greases were heated on filter paper for 2 hours at 60°C [6]. Oil
stained created after the test was measured, calculated and compared between fresh and used grease. It
is desirable for the grease to bleed oil within the range of +15% to -15% of oil bleed different between
fresh and used grease [7]. This range shows that in an operation, the grease can still be used without
changing the re-lubrication intervals. Positive values shows that bleeding is increased due to the
broken of grease’s thickener structure. Negative values represent the reduction of oil bled at which
during the grease was used in an operation, the grease dried out before the re-lubrication interval and
the surface is ‘hungry’ for lubrication. In this analysis, used grease is the grease that was aged in an
oven for 10 days at 70°C.

2.4.3. Oil separation. Oil separation test is a test to determine the grease tendency to separate oil
during storage which correlate directly with the oil separation occurs in 35-lb pails of grease during

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2019 9th International Conference on Future Environment and Energy IOP Publishing
IOP Conf. Series: Earth and Environmental Science 257 (2019) 012018 doi:10.1088/1755-1315/257/1/012018

storage. This test was carried out at 25°C after the grease being stored for 2 months where oil
separated on top of the grease were collected and measured. It was desired for the oil separated from
the grease to be < 4% by weight [8].

2.4.4. FTIR Characterization. The base oil and the greases were characterized using Fourier-transform
infrared (FTIR) spectroscopy to study the compound existed in the oil and grease.

3. Results and discussion

3.1. Consistency
Table 1 shows the consistency of each formulated greases in accordance to NLGI number ranging
from 000 to 6. It was found that as the thickener percentage in grease formulation increases, the
consistency of the grease becomes more firm. Commonly, the grease available in the market possess
grease consistency of NLGI no. 1 to no. 3 [9]. From this test, grease of 20 – 30% of thickener content
shows the most desired consistency of NLGI no. 1 to no. 3.
10% of thickener content possessed softer consistency compared to the other grease. This is due to the
insufficient amount of thickener to hold the oil in its thickener system which finally led to softer
consistency. This also applies towards grease with consistency more firm than NLGI no. 3 at which
the amount of thickener were too excessive which cause the lack of oil content in grease. As the matter
of fact, grease consistency can be altered by adjusting the oil-to-thickener ratio [10].

Table 1. Consistency number for grease formulation based on NLGI number.

Base oil (%) Stearic acid (%) Sodium hydroxide (%) NLGI number
90 5 5 0
80 10 10 1 to 2
70 15 15 2 to 3
60 20 20 3 to 4
50 25 25 3 to 4

3.2. Oil separation

Oil separation usually occur when grease are being kept for a long period of times. The grease can be
considered as good grease if the oil separation is under 4%. From this study, it can be seen that all
formulated greases separated oil < 4% (Table 2). There are no oil puddle observed for grease with
thickener more than 30% where it can be concluded that the oil were fully hold by the thickener. Oil
puddle is formed on top of grease formulated with less than 30% of thickener due to their soft
consistency. But, oil contamination such as dust, dirt can also be the factor of oil being drew out from
thickener system over time. The oil separation could be influenced by many factors such as the
percentage of the base oil, the ability of the thickener to hold the oil, and the homogenize level of the
finished grease.

Table 2. Oil separation of the formulated grease.

Base oil (%) Stearic acid (%) Sodium hydroxide (%) Oil separation (%)
90 5 5 1.4
80 10 10 0.6
70 15 15 0.0
60 20 20 0.0
50 25 25 0.0

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2019 9th International Conference on Future Environment and Energy IOP Publishing
IOP Conf. Series: Earth and Environmental Science 257 (2019) 012018 doi:10.1088/1755-1315/257/1/012018

3.3. Oil bleeding

9
Oil bleeding diameter (cm) 8 Oil bleeding (70˚C)
7 Oil bleeding (25˚C)
6
5
4
3
2
1
0
10 20 30 40 50
Thickener (%)

Figure 1. Graph of oil bleeding versus thickener percentage.

Figure 1 shows that as the amount of thickener had significant effects on the formulated grease’s oil
bleeding. In this analysis, oil bleeding was tested in two different condition which are at room
condition of 25°C and at 70°C. The graph above shows that the oil bleeding are relatively linear to
thickener percentage regardless of grease ageing condition. Oil bleeding happened when there is stress
occur to the grease. Although this stress are extremely weak when be compared to the mechanical
stress acted upon grease during usage, but it still can result in the release of a small amount of oil from
the grease [11].

3.4. FTIR analysis

a)

b)

c)

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2019 9th International Conference on Future Environment and Energy IOP Publishing
IOP Conf. Series: Earth and Environmental Science 257 (2019) 012018 doi:10.1088/1755-1315/257/1/012018

d)

Figure 2. FTIR analysis of (a) unfiltered waste oil, (b) new oil, (c) filtered waste oil, (d) comparison
between oil.

a)

b)

c)

d)
Figure 3. FTIR analysis of grease formulation: (a)
60:40, (b) 70:30, (c) 80:20, (d) 90:10

Figure 2 shows the FTIR analysis results for base oil and their comparison against each other. It was
observed that there are no significant difference between new engine oil and waste engine oil (WEO)
either it was filtered or unfiltered. It was also observe that there are no known contaminants presence
in WEO.

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2019 9th International Conference on Future Environment and Energy IOP Publishing
IOP Conf. Series: Earth and Environmental Science 257 (2019) 012018 doi:10.1088/1755-1315/257/1/012018

Figure 3 shows the formulated greases FTIR analysis results. The FTIR spectrum for each greases are
almost similar due to the same type chemicals were used in the formulation. However, the spectrum
shows some variation on peaks as the thickener percentage were increased. Absorption peaks at 2973
cm-1 indicates the asymmetric stretching vibration of CH3 group from the base oil. It was observed that
there were visible peaks at 3400 cm-1 as the thickener percentage increases for which it indicates the
presences of water or glycol compound in grease. This peaks was belongs to the thickener itself for
which there are some traces of water produced when the soap was first formed during the reaction of
NaOH and stearic acid [12,13].

4. Conclusion
Grease can be formulated from waste engine oil. FTIR spectroscopy has found that there were no
significant differences between new oil, waste oil, and all formulated greases. Results of grease
analysis shows that the thickener percentage have significant effect on formulated greases properties
including consistency, oil bleeding and oil separation. Out of all formulation, grease formulated with
70 – 80% of base oil and 20 – 30% of thickener was the best grease formulation as it shows desirable
grease properties of consistency within NLGI no.1 to no. 3, < 4% oil separation, and acceptable oil
bleeding. This, it was proven that grease could be formulated using waste engine oil.

5. References
[1] Donahue C J 2006 Lubricating grease: A chemical primer J. Chem. Educ. 83 862–9
[2] Wright J 2008 Grease Basics Noria
[3] Laurentis N De, Kadiric A, Lugt P and Cann P 2016 Tribology International The in fl uence of
bearing grease composition on friction in rolling / sliding concentrated contacts Tribiology Int.
94 624–32
[4] EPA 2017 Managing, Reusing, and Recycling Used Oil United States Environ. Prot. Agency
[5] Srivastava S P 2014 Rerefining and recycling of used lubricating oil Development in Lubricant
Technology (Hoboken: John Wiley & Sons, Inc.) pp 299–307
[6] SKF 2009 SKF Grease Test Kit TKGT 1: Instruction Manual 1–40
[7] Ludwig L G 2012 Storing Grease to Avoid Bleed and Separation Mach. Lubr.
[8] Lugt P M 2013 Grease Lubrication in Rolling Bearings (Chichester: John Wiley & Sons, Inc.)
[9] Rizvi S Q A 2008 A Comprehensive Review of Lubricant Chemistry, Technology, Selection,
and Design (ASTM International)
[10] Doyle D 2015 General Grease Overview and Bearing Lubrication ALS Tribol.
[11] ExxonMobil 2012 Grease Static Oil Bleed 1
[12] Kholijah A M S, Yeung S L C, Sazwani S and Yunus R M 2012 Production of High
Temperature Grease from Waste Lubricant Sludge and Silicone Oil J. Appl. Sci. 12 1171–5
[13] Núñez N, Martí n-Alfonso J E, Valencia C, Sánchez M C and Franco J M 2012 Rheology of
new green lubricating grease formulations containing cellulose pulp and its methylated
derivative as thickener agents Ind. Crops Prod. 37 500–7