Journal of Engineering and Applied Sciences 11 (6): 1396-1401,2016

ISSN: 1816-949X
© Medwell Journals, 2016

Recycling Used Lubricating Oil Using Untreated,

Activated and Calcined Clay Methods
1
JD. Udonne, 2 V.E. Efeovbokhan, 2AA Ayoola, 2D.E. Babatunde, 1Ajalo Ifeoluwa and 1l.J Ajalo
1
Department of Chemical and Polymer Engineering, Lagos State University, Lagos, Nigeria
'Department of Chemical Engineering, Covenant University, Otta, Ogun State, Nigeria

Abstract: This study addresses recycling of used lubricating oils treated using different methods involving
rmtreated clay as the control sample, clay activation and calcined clay methods. A recycling process of the used
lube oil was carried out which eventually led to comparison of results of the recycled oil with the fresh lube oil
using ASTM standards. Tests carried out on the used, fresh and recycled lube oils include: flash point,
kinematic viscosity at 40 and 100°C, respectively, specific gravity/density, appearance and total base oil. The
results show that recycled lubricating oil had the following properties: flash point was 227°C for the calcined
clay, 229°C or activated clay and 224°C for nntreated clay, compared with 204°C for nntreated waste oil. Also
Ttal Bse Number IBN) gave the followiug: 6.25mg KOHg-' for calcined clay method, 6.24 mg KOH g-' for
activated clay and 5.56 mg KOH g-' for uutreated clay method, compared with 4.41 mg KOH g-' for uutreated
waste lubricating oil. This gives the recycled lube oil the potential to be reused in car engines after adding the
required additives.

Key words: Used lubricating oil, refined lube oil, activated clay, calcined clay, environmental pollution

INTRODUCTION the environmental threats posed and preserves crude

oilreserves (Dwrani et al., 2011 ). Several techniques are
Lubricating oils are viscous liquids of petrolelllll available for the regeneration of used lubricating oil,
origin, used for the protection of moving parts of engines amoug which are chemical treatment (Ogbeide, 2010), acid
and machines (Boyde, 2002). Typical lubricating oil activated process that is similar to acid-clay process with
contains 90% base oil, most often petrolelllll fractions little modification, physical treatment by distillation and
calledmineral oils and <1 0% additives. The chemical thin fihn evaporation (Brinkman et al., 1981) and solvent
breakdown of these additives during use resulted to build extraction (Katiyar and Husain, 2010).
up of halogemted hydrocarbons in the oil. Polycyclic The pwpose of this research is to obtain a high
Aromatic Hydrocarbons (PAHs) as well as other quality production of lubricating oil from used lubricating
polycyclic componnds are generated and acclllllulate oil by there-refining of it, thereby reducing environmental
inthe oil (Wong and Wang, 2001) together with metals pollution caused by used lube oil. This process makes, it
from wear and tear of the engine being lubricated essential for the used lube oil to be re-used to perform
(Chuug et al., 2007). These compouuds gradually reduced different fnnctions such as for lubricating moving part of
its quality leading tochange in its physical and chemical engines and machine, reduce friction, transfer heat, carry
properties and thereby deteriorated (Kamal and Khan, away contaminants and debris and transmit power.
2009). These components are highly toxic upon released The conventional steps in lubricating oil manufacture
to the environment posing harmful effects toaquatic lives are pretreatment of the crude oil charge, followed by
and human beiugs (Kanokkautapoug et al., 2009). The distillation of the crude in two steps (an atmospheric
improper disposal of used lubricating oil pollutes tower and vaculllll tower), de-asphalting (as required by
environment to a great extent as each volllllle of it can the nature of the crude oil charge), de-waxing, solvent
pollute not lesstlian two huudred and fifty thousand extraction, filtering and blending including mixing various
volllllles of water (Udonne, 2011 ). Proper management of additives with the final lubricating oil. Recycling of used
this hazardous material is therefore important in order to lubricating oil is the process of regenerating its used
make it a valuable product bygreatly reducing the substance so that it can be used again. It is the process
quantity being disposed improperly (Dang, 1997). involving the removal of the impurities in the used oil and
Therefore, re-refining of used lubricating oil will eliminate bringing it back to the initial state The conventional

Corresponding Author: J.D. Udolllle, Department of Chemical and Polymer Engineering, Lagos State University, Lagos, Nigeria
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methods of recycling of waste engine oil either requires a temperature of II 0°C and allowed to dry up. The dried
high cost technology such as vacuwn distillation or the clay was again ground into very fine particles and sieved
use of toxic materials such as sulfuric acid. These to a mesh of 0.5 mm using test sieve on a mechanical sieve
methods also produce contaminating by products which shaker. The clay soil was then sub-divided into three
have high sulfurlevels. The adsorption treatment of waste portions to be used for untreated clay, activated clay and
lube oil is based on the ability of adsorbent to selectively calcined clay preparations.
extract resinous and sulfur containing compmmds,
rmsaturated and polycyclic material and also organic Untreated clay: This is the portion of clay without
residues of sulfuric acid and solvents from oils. Natural chemical activation after the clay sample was ground,
clay, activated and calcinedare used as adsorbent in the washed and dried in the oven at 11 0°C.
treatment of oils. There are basically two treatment
methods and they include contact treatment and Clay activation: The 200 g of clay (after dirt. sand and
percolation or filtration through a bed of granulated stone have been removed) was made into sltmy with
adsorbent. 80 ern' of distilled water and followed by the addition
of 60 mL of 0.35 M solution of sulfuric acid. The slurry
MATERIALS AND METHODS
was then poured into allllllinlllll pan and left for 1 h at
temperature 1 00°C. The sltmy was then washed several
Clay soil, filter paper, fresh premilllll motor engine oil,
times with distilled water in order to remove any excess
used premilllll motor engine oil and distilled water which
acid, until it was neutral. The washed clay mixture was
was used throughout the experiment for sample
dried in an oven for 1 h and grounded into powdery form
preparation and dilution.
(ObohandAworh, 1991).
Collection of test samples: Clay soil was collected from
Iraye-Epe area of Lagos state, Nigeria. The test sample of Calcined clay: The third portion of the clay sample from
fresh lube oils (premilllll motor oil SAE-40) was collected section 2.3.2 above was then calcined by heating the clay
from 1.1RS oil service station. The used lubrication oil was soil in a fwnace at about 600°C for 5 h.
collected from a car mechanic's used oil dlllllp in Iba-Ojo
area of Lagos, Nigeria. Purification process of the used oil: The used engine oil
was purified using the various clay samples. Beginning
Apparatus/equipment: Apparatus and equipments used with the activated clay, it was ground and mixed with the
include conical flask, beaker (Pyrex), hydrometer, used engine oil that had been pre-heated for 5 min. The
plasticbowls, allllllinlllll pan, BW1Sen bwner, weighing mixture was then thoroughly blended together with the
balance, oven, mechanical shaker, Thermostatbath aid of a stirrer. The mixture was kept 24 h to allow for
(FALC WB-MF Model). prolonged contact and chemical reaction between the
spent oil and the activated clay. The impurities in the used
Experimental procedure: The methods used in the engine oil and the clay particles were allowed to settle and
re-refining of the used lubricating oils include methods
with the aid of sieve cloth, the oil was sieved to obtain the
such as, filtration process to remove impurities, clay
purified lube oil sample. The purification of the used lube
preparation before clay activation and calcined clay
oil was repeated using other clay types.
soil.

RESULTS AND DISCUSSION

Filtration process: The used lubricating oil was filtered to
remove impurities such as metal chips, sand, dust,
particles, micro impurities that are contained in the lube The results of the research research which
base oil. This was done using a fUllllel with a filter paper investigates the recycling of used lubricating oil and
placed in it. compared with the fresh lubricating oil sample using three
different clay methods have been carefully detailed in
Clay preparation: The clay sample was first grmmd and Table I and Fig. 1-7. The Table I also includes the results
then made into sltmy with distilled water. Impurities such of the various quality tests (appearance, viscosities at
as sand and stones were first allowed to settle at the 40 and 100°C, flash point, specific gravity, density and
bottom in plastic bowls and were then removed by total base nlllllber) performed using ASTM methods on
decantation. The sltmy was kept in an oven at the lubricating oil products.

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Table 1: Sumrmny of analysis of result

Untreated clay Clay activation Calcined clay
Tests Unit Test method S2ecification Fresh oil Used oil method method method
Appearance Visual Bright and Clear Dark Dark Dark Dark
Flash point (oC) ASTM:-D0092 Min. 225 230.0 204.0 208.0 229.0 227.0
Viscosity kin, 40° C (CST mm sec-1) ASTM:-D0445 130-150 146.50 135.52 139.83 145.77 144.41
Viscosity kin, 1oooc (CST mm sec' ) ASTM:-D0445 12.5-16.3 14.70 12.87 13.44 14.32 14.11
Viscosity index (CST mm sec-1) Calculated 99.1 7 85.38 89.59 95.62 94.11
Total base number (MgKOHg-1) ISO 3771 7.00-10.00 8.50 4.41 5.56 6.26 6.20
Density (Kgm-' ) ASTM:-Dl298 896.5 892.0 894.6 896.0 895.9
S2ecific B!:avity (g cm- 32 ASTM:-D1298 0.8965 0.8920 0.8946 0.896 0.8959

150

145

;:
~ 135

~ 130

125

120
Minim um Fresh Oil Used Oil Untreated Clay Clay Activa t ion Calcined Clay
Specification Method Met hod Met hod

Fig. 1: Effects of the recycling of used lube oil on its flash point

155

15 0

145

~ 140
E
E • Lu b Oil
..... 135 Sam p les
Q
?:
·;;; • Min5pec
13 0
8
5 1 25 • Max Spec

12 0
Sp eci ficat•on Fresh Oil Used OOntrea ted Cla~~a tlon ~lm:d! Clay Method

Fig. 2: Effects of the recycling of used lube oil on its viscosity at 40°C
18

16

14

12
~
..,~
10

~ 8

i'
8
6

:S 4

0
spccificaton fresh oil used oil un treated clay act ivation c.alcfncd clay
clay method method method

Fig. 3: Effects of the recycling of used lube oil on its viscosity at 100°C

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 J. Eng. Applied Sci., 11 (6): 1396-1401,2016
105 T

100

-;;;
:e,_
E
95

Q 90
?:
'8
!:( 85
5
80

75
f resh oil u sed oi l unt rea ted clay clay activa t ion calcined clay
m e t hod met hod met hod

Fig. 4: Effect of recycling of waste used lube oil on its viscosity index

6
~

..
::r::
~ 5

..,~ 4
.... 3

0
Fresh Oil Used Oil U n trea ted Clay Clay Activat ion Calcined Clay
Method Method Met hod

Fig. 5: Effect of recycling of used lube oil on its Total base oil

0 .896

0 .895
-E
"3 0 .894
?:
-~ 0 .893
.:5
:E 0 .892
i 0 .891

0 .89

0.889
Fresh 011 Used Oil Untreated Clay Clay Act•va t 1on Calcined Clay
Method Method Method

Fig. 6: Effect of recycling of waste used lube oil on its specific gravity

Appearance: This indicates the brightness and clarity of the treated lube oil have a dark appearance. The dark
petroleum products. The results of the appearance appearance of the used lube oil and those from the
(Table 1) of the fresh lube oil, used lube oil treated methods were due to their combustion and
and the treated lube oil show that the fresh oil oxidation at high temperature by the combustion engine
have a clear and bright color while the used and for a very long time.

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897

896

895

I:::
-s
~ 892
891

890

889
u sed ou Unt,.c~ tcd Clav Cl.:-v Act•vi.ltion CiJiclncd Cli.lv
Mc·t hod Met hod Me·thod

Fig. 7 : Effect of recycling of used lube oil on its density

Flash Point: The flash point indicates how easy shown in Table 1. The plot of kinematic viscosities
lubricating oil may ignite and burn. The flash point of of each of the lube oils (Fig. 3) reveals that they all fell
lubricating oil is the lowest temperature where it will within the required mmnnum and maxnnum
evaporate enough fluid or vapor to form a combustible specification limits of lube oils.
concentration of gas with air that can be ignited
spontaneously by a specified flame. Viscosity index: The viscosity index is obtained by
The result of the flash point of the fresh lube oil, used electronic software which depends on the kinematic
lube oil and the treated lube oil above shows that, there viscosity of the samples at 40 and 1OOOC, respectively and
was a decrease in the used lubricating oil which is below shows a linear relationship. The result also indicates that,
the minimum specification of SAE-40 lube oils. The the used lube oil have the least viscosity index which
decrease in the used lube oil was due to contamination of indicate the dilution of light oil or very volatile component
very volatile component. On treating, the volatile but after treatment, the volatile components were
components were extracted from the used lube oil. There extracted to an extent which then increased the
by increasing the flash point above the minimum viscosity index of the lube oil. Figure 4 shows the various
specification of SAE-40 except the untreated clay method. viscosity indexes of four lube oil samples compared
to the fresh oil sample.
Viscosity at 40°C: The results (Table 1) of the Kinematic
Viscosities (KV) at 40°Cusing the ASTM-D 0092 Method Total base number: Total Base Number (TBN) 1s a
shows that the waste used oil sample with Kinematic measure of reserved alkaline additives put into lubricants
Viscosity (KV) of 135.52 CST mm sec-2 and those of the to neutralize acids, retard oxidation and corrosion,
recycled lube oil are as follows from the untreated clay enhance lubricity, improve viscosity characteristic and
method, KV is 139.83 CSTmm sec-2, from Clay Activation reduce the tendency of sludge buildup. It is a test to
Method, KV is 137 .41 CSTmm sec-2 and from calcined measure the ability to neutralize corrosive acids that may
method, KV is 139. 77 CST mm sec-2 The plot of be formed during normal operation.
kinematic viscosities of each of the lube oils (Fig. 2) Internal combustion engine oils are formulated with
reveals thatthey all fell within the required specification a highly alkaline base additives package to neutralize the
range (Brinkman et al., 1981 ). This shows that at 40°C, the acidic products composition. The TBN is a measure of
waste used oil and the recycled methods still retained the this package and it may be used as an indication for the
viscosity specification range (130-150 CST mm sec-2). engine oil's replacement time. This is because TBN
depletes with time in service. Higher oil TBN values are
Viscosity at 100°C: The result of the kinematicviscosity more effective at neutralizing acids for longer periods of
at 1 00°C shows that there is a decrease in the viscosity of time (Dong et al., 2001 ). The results of the analysis of the
lube oil as the temperature is increasing. The result also total base number show that, there is a decrease of the
indicates that, the used lube oil have the least viscosity TBN of used oil and those from the recycled methods
compared to the recycled and fresh lube oils. This may be compared to that of the fresh oil. This is because some
due to contamination of a very volatile component amount of base has been used up to neutralize the acid
(light oil) present in the oil. After treatment, the volatile formed during usage of the oil. After treatment there was
components were extracted from the used oil and an increase of the total base number from 5.56 (used lube
consequently increased the viscosity of the lube oils as oil) to 6.20 for oil from the untreated clay method, 6.26 for

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 J. Eng. Applied Sci.• 11 (6): 1396-1401. 2016

oil from the calcined clay method except for the clay ACKNOWLEDGEMENTS
activation method where a decrease in IBN ( 4.41) was
noticed. But in comparison with the IBN (8.20) of the Researchers gratefully acknowledge the financial
fresh lube oil, there is a decrease IBN of lube oil in all the support from the Management of Covenant University to
methods used. This may be due to the presence of the publish this study.
metallic and acidic elements present in the clay sample.
The decrease is however, more pronmmced in the clay REFERENCES
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