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The Pyrolizing of Waste Lubricating Oil

(WLO) Into Diesel Fuel Over a Supported
Calcium Oxide Additive
a a a
H. Aburas , A. Bafail & A. Demirbas
a
King Abdulaziz University, College of Engineering, Department of
Industrial Engineering, Jeddah, Saudi Arabia
Published online: 20 Dec 2014.

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To cite this article: H. Aburas, A. Bafail & A. Demirbas (2015) The Pyrolizing of Waste Lubricating Oil
(WLO) Into Diesel Fuel Over a Supported Calcium Oxide Additive, Petroleum Science and Technology,
33:2, 226-236, DOI: 10.1080/10916466.2014.973604

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 Petroleum Science and Technology, 33:226–236, 2015
Copyright 
C Taylor & Francis Group, LLC
ISSN: 1091-6466 print / 1532-2459 online
DOI: 10.1080/10916466.2014.973604

The Pyrolizing of Waste Lubricating Oil (WLO) Into Diesel

Fuel Over a Supported Calcium Oxide Additive

H. Aburas,1 A. Bafail,1 and A. Demirbas1

Downloaded by [Australian National University] at 02:57 13 January 2015

1
King Abdulaziz University, College of Engineering, Department of Industrial Engineering,
Jeddah, Saudi Arabia

Most the lubricant oils are generally obtained from petroleum resources. Waste lubricating oil can be
converted into valuable fuel products by refining and treating processes. Recycling is the applicable
process for upgrading of petroleum-based wastes by converting them into reusable products such as
gasoline, diesel fuel, and heavy oil. Possible acceptable processes are cracking and pyrolysis. A pyrolytic
distillation process is often employed in oil refinery operations to produce lower molecular weight
hydrocarbon fuels from waste feedstocks. If the purpose is to maximize the yield of distillate products
resulting from lubricant oil pyrolysis, a low temperature, high heating rate, and short gas residence time
process would be required. The effect of calcium oxide (CaO) as additive on density, viscosity, flash
point, sulfur content, higher heating value, and pyrolytic distillation yields was investigated. The purified
oil samples are blended separately with additives having mass bases of 2%, 4%, 6%, 8%, and 10%.
Keywords: waste lubricating oil, recycling waste, pyrolysis, CaO additive, catalytic effect

INTRODUCTION

In recent years, diminishing fossil fuel sources, growing demand and cost of petroleum-based fuels,
and environmental hazards as a result of burning of them have encouraged researchers to investigate
possibility of using alternative fuels instead of the fossil fuels. Therefore, we have focused on finding
alternative new energy resources and utilizing them (Demirbas, 2009).
Petroleum is the largest single source of energy consumed by the world’s population, exceeding
coal, natural gas, nuclear, hydro, and renewables. In fact today, over 80% of the energy we use comes
from three fossil fuels: petroleum, coal, and natural gas.
While fossil fuels are still being created today by underground heat and pressure, they are being
consumed more rapidly than they are created. Unfortunately the petroleum oil is in danger of
becoming short in supply. Petroleum-based fuels are limited reserves concentrated in certain regions
of the world and are shortening day by day (Demirbas, 2007a, 2007b, 2008). Therefore, most of the
research works presented in literature on renewable energy sources have focused on different waste
energy sources (Demirbas, 2002, 2005). These wastes are commonly known as waste lubricating oil
(WLO), trees, plastics, and tires. There is a large amount of waste energy sources discharged to the
environment in the world. Waste lubricant engine oil is one of the most important types of the energy
sources. It gradually loses its lubricant properties, and the oil absorbs many dust and metal particles
from the engine block, due to the extreme conditions encountered. About 40 million metric tons per

Address correspondence to A. Demirbas, King Abdulaziz University, College of Engineering, Department of Industrial
Engineering, P.O. Box 80204, Jeddah 21589, Saudi Arabia. E-mail: [email protected]

226
 PYROLIZING OF WASTE LUBRICATING OIL 227

annum are produced worldwide, and around 60% of the production becomes waste (Gómez-Rico
et al., 2003). Most of them are petroleum-based oils, and the utilization rate is about 97% of the total
lubricant oil production (Bhaskar et al., 2004).
Most of the lubricant oils are generally obtained from petroleum resources. Waste lubricating
oil can be converted into valuable fuel products by refining and treating processes (Bhaskar et al.,
2004). Recycling is the applicable proces for upgrading of petroleum-based wastes by converting
them into reusable products such as gasoline, diesel fuel and heavy oil. Possible acceptable processes
are cracking and pyrolysis (Brinkman and Sickson, 1995; Nerı́n et al., 2000; Song et al., 2010).
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CRACKING AND PYROLYSIS PROCESSES

Cracking and pyrolysis are thermochemical processes occurring in the absence of oxygen or when
significantly less oxygen is present than required for complete combustion.

Cracking

Catalytic cracking employs catalysts using hydrogen-driven reducing reactions to accelerate the
breakdown of high molecular weight compounds into smaller products. This cracking process is
often employed in oil refinery operations to produce lower molecular weight hydrocarbon fuels from
waste feedstocks. These include gasoline from heavier oils, distillation residuals, and waste plastic.
Various technologies exist for cracking waste oils for use as automotive or gaseous fuels. The
process can rarely compete directly with the direct use of waste oil as a fuel. The most common type
of cracking is catalytic cracking (Redwan and Ali, 1992). The most common process is fluid catalytic
cracking, in which the oil is cracked in the presence of a finely divided catalyst, which is maintained
in an aerated or fluidized state by the oil vapors. The cracking process yields a highly unstable
low-grade fuel oil, which can be acid-corrosive, tarry, and discolored along with a characteristically
foul odor.

Pyrolysis

Pyrolysis is the thermal decomposition of organic matter occurring in the absence of oxygen or when
significantly less oxygen is present than required for complete combustion.
Fast pyrolysis (more accurately defined as thermolysis) is a process in which a material is
rapidly heated to high temperatures in the absence of oxygen. Rapid heating and rapid quenching
produced the intermediate pyrolysis liquid products, which condense before further reactions break
down higher-molecular-weight species into gaseous products. High reaction rates minimize heavy
oil formation. At higher fast pyrolysis temperatures, the major product is gas (Bridgwater and
Peacocke, 2000; Babu and Chraurasia, 2003; Mohan et al., 2006; Nasim et al., 2014). If the purpose
is to maximize the yield of distillate products resulting from crude oil pyrolysis, a low temperature,
high heating rate, short gas residence time process would be required. For a high heavy oil production,
a low temperature, low heating rate process would be chosen.
Flash pyrolysis describes the rapid, moderate temperature (450–650◦ C) pyrolysis that produces
liquids. Crude oil is heated at rates of 100–10,000◦ C/sec and the vapor residence time is normally
less than 2 sec.
Pyrolysis appears to be a technique that is able to reduce a bulky, high polluting industrial waste,
while producing energy or valuable chemical compounds. The pyrolysis of WLO has been claimed
as an alternative to incineration because valuable products are obtained (Nerı́n et al., 2000). The
 228 H. ABURAS ET AL.

composition of waste oils changes with the use, since some contaminants are present in the virgin
oil but most of them are a consequence of the processes in which the oil is involved. Sulfur contents,
hydrocarbons, and metals such as chromium or lead make it a toxic waste.
Four different waste oils (machine waste oil, automotive waste oil, hydraulic waste oil, and cutting
waste oil) have been pyrolyzed using an experimental bench scale pyrolysis unit at 873 K under
atmospheric pressure and the polyaromatic hydrocarbons have been analyzed in the valuable liquid
fraction (Domeño and Nerı́n, 2003).
Liquid and gas fractions have been analyzed for organic products and metals. High yields of
valuable light olefins such as ethylene and propylene and light aromatics as benzene, toluene, xylene,
and naphthalene derivatives have been obtained. Pyrolysis of industrial waste oils is considered as
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an alternative use to direct combustion. In the pyrolysis approach the target is to obtain valuable
liquids what means that liquids must be free of metals (Lázaro et al., 2001; Lázaro et al., 2002).
Various samples of used car and truck tires were pyrolyzed in a batch mode under vacuum and
in a continuous feed reactor (Pakdel et al., 2001). The pyrolysis temperature varied in the range of
715–845 K. The scrap tires were pyrolyzed in a fixed bed reactor and the evolved pyrolysis gases
were passed through a secondary catalytic reactor. The composition of oils derived from the batch
pyrolysis of tires was determined (Williams and Brindle, 2003). The results showed that the derived
tire oils had fuel properties similar to those of a light petroleum fuel oil. The influence of pyrolysis
temperature showed an increase in the aromatic content of the oils with increasing temperature, with
a consequent decrease in aliphatic content. Pyrolysis has the potential of transforming used tires into
useful recyclable products. Pyrolytic char is one of the most important products of tire pyrolysis
(Helleur et al., 2003).
Process variables for crude oil pyrolysis are heat flux, temperatures, partial pressure, feedstock,
API gravity, heating rates, residence time, heat and mass transfer, and catalytic mineral matter
content.
It is known that the WLO is highly viscous andcontains plenty of sulfur, carbon soots, small metal
particles and some gum-like materials (Demirbas, 1998). The contaminants exist originally in the
lubricating oils. In order to understand the production processes of the waste oil, procedures of the
processes should be explained briefly. The production processes can be described in three sections,
which are purification, thermal treatment, and distillation processes.
A recycling process was developed that eventually led to comparable results with some of the
conventional methods (Nerı́n et al., 2000). This gives the recycled oil the potential to be reused in car
engines after adding the required additives. The advantage of using the acetic acid is that it does not
react or only reacts slightly with base oils. The recycling process takes place at room temperature. It
has been shown that base oils and oil additives are slightly affected by the acetic acid. Upon adding
0.8% by volume of acetic acid to the waste engine oil, two layers were separated, transparent dark
red colored oil and a black dark sludge at the bottom of the container. The base oils resulting from
other recycling methods were compared to the results of obtained from acetic acid treatment method.
The comparison showed that the recycled oil produced by acetic acid treatment is comparable to
those recycled by the other conventional methods (Hamawand et al., 2013).
Optimum conditions for recycling used lubricating oil using this method are room temperature
and atmospheric pressure. The process for recycling is simple, as it only requires mixing at room
temperature, settling, centrifugation, and finally mixing with kaolinate. The base oil produced by
the glacial acetic acid method is of comparable quality to that produced by the acid-clay method.
Also, it has a potential to be reused in car engines after adding the required additives (Hamawand
et al., 2013).
Waste lubricating oil is a high pollutant material that requires responsible management. Waste
lubricating oil may cause damage to the environment when dumped into the ground or into water
streams including sewers. This may result in groundwater and soil contamination (Hopmans, 1974;
Hamawand et al., 2013). The oxidized and polymerized products dissolved and suspended in the oil
 PYROLIZING OF WASTE LUBRICATING OIL 229

may cause an increase of the oil viscosity, while decreases in the viscosity of engine oils indicate
fuel contamination. Oxidation of base oils during use in an engine environment produces corrosive
oxidized products, deposits, and varnishes, which lead to an increase in the viscosity (Diaz et al.,
1996).

EXPERIMENTAL

Samples of WLOs were supplied from the Trabzon (Turkey) auto repair industry. Before experiments
the air-dried WLO samples were filtered to pass 250-mesh sieve to separate metal particles and other
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particular materials. While the WLO was flowed through the filters, it was purified from the oil from
small dust, carbon soot, small metal particles, and some gum-type materials.
The pyrolysis experiments were carried out in a laboratory scale apparatus at Sila Science
laboratories. The main element of the pyrolysis device was a vertical reactor of stainless steel.
Figure 1 shows pyrolysis reactor. The reactor was inserted vertically into an electrically heated
furnace and provided with an electrical heating system power source. The nominal heating time was
35 min. For each run, the heater was started at 25◦ C and terminated when the desired temperature.
The most important part of the system is the reactor in which thermal treatment of the WLO was
carried out. It has a cylindrical shape with dimensions of 6 cm in diameter and 10 cm in height
and with cylindrical shape neck with dimensions of 2 cm in diameter and 20 cm in height. It has a
capacity that will be able to produce 90 mL of fuel.
The reactor was isolated with glass wool having a thickness of 5 cm to minimize heat loss from
the reactor. Electrical heaters with a total heating capacity of 3.5 kW were used to heat the oil and
were placed around the reactor container. The electrical heaters have special resistance heaters which
can heat the waste oil sample up to 600◦ C. The heating rate can be controlled by the control unit
adjusting voltage to keep temperature of the oil at desired levels. Temperature measurement was
performed by means of thermocouple. It was placed in locations where temperature measurement
was needed, namely in the middle of the reactor. The other important component of the system is
the condenser, which is employed to condense the oil exposed to pyrolytic distillation process. The
fuel in the condenser is cooled and condensed by cooling water.
The pyrolysis products were condensable liquids, noncondensable gaseous products, and solid
residue. The yield of liquid products was defined as
Condensed liquids from pyrolysis
Yield of liquid products × 100 (1)
Mass of sample loaded into reactor
The additive known as calcium oxide (CaO) was added to the clean oil in the reactor and blended
with mass basis of 2%, 4%, 6%, 8%, and 10%, separately. The new sample was mixed continuously
and kept for 30 min at a room temperature of 25◦ C. Then, it was exposed to thermal and pyrolytic
treatments. The thermal and pyrolytic treatments of the samples were performed in the presence of
additives. Each sample mixed continuously was distillated and collected in an Erlenmeyer flask.

RESULTS AND DISCUSSION

This study was carried about purification and conversion of the WLO into diesel-like fuel by
blending purified oil and additive amount of CaO with mass basis of 2%, 4%, 6%, 8%, and 10%.
Fuels were produced from the WLO by applying pyrolytic distillation method. Thermal and physical
characteristics of the produced fuel samples such as flash point, density, viscosity, and sulfur contents,
as well as distillation tests, were examined by using measurement devices. The results obtained from
the measurements are given in Table 1.
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230
H. ABURAS ET AL.

FIGURE 1
The pyrolysis reactor.
 PYROLIZING OF WASTE LUBRICATING OIL 231

TABLE 1
Physical Properties of Diesel Fuel, Heavy Fuel Oil and DLF Obtained

Diesel Fuel Heavy Fuel

Physical Property TS3082-EN 590 Oil DLF

Density at 15◦ C, kg/m3 820–845 940 820

Viscosity at 40◦ C, mm2/sec 2–4.5 — 3.6
Flash point, ◦ C >55 — 58
Sulfur, ppm 50 60 3400
Water, mg/kg <200 110 130
Higher heating value, kJ/kg 42,700 42,675 42,525
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Temperature at 250◦ C, max. volume, % v/v 65 — 20

Temperature at 250◦ C, min. volume, % v/v 85 — 90
Volume at 95%, max. temperature, ◦ C 360 — 360

Characteristics of the Produced Fuel

The physical properties of the produced diesel-like fuel (DLF) from waste lubricating oil are
measured. These characteristics are shown in Table 1, together with standard values of a diesel fuel
and heavy fuel oil. Table 1 shows that some of the parameters of density, boiling point, viscosity,
flash point, and lower heating value are in the standard values of the diesel oil or reasonably close to
the standard values. But, sulfur amount is considerably higher than that value. It should be decreased
below the value of 50 ppm. Density is another important property of diesel fuel. It is the weight of a
unit volume of fluid. The density of diesel fuel ranges between 820 and 845 kg/m3. Density of DLF
is measured as 820 kg/m3, which is close to the lowest limit. Viscosity is one of the most important
properties of diesel fuels, as it affects the operation of the fuel injection equipments particularly at
low temperatures when the increase in viscosity affects the fluidity of the fuel. High viscosity leads
to poorer atomization of the fuel spray and less accurate operation of the fuel injectors (Demirbas,
2006). Higher heating value (HHV) of the DLF is obtained as 42,525 kJ/kg by using adiabatic bomb
calorimeter. It is close to HHV of typical diesel fuel, which is 42,700 kJ/kg. A diesel fuel having of
the heating value gives good engine performance during combustion in a diesel engine.

Effects of the Additives and Distillation Temperature on Distillation Yield

The distillation test results of the DLF, together with the diesel fuel are shown in Table 2.
It is clear that the distillation temperature of the DLF resembles to the distillation temperature
of the diesel fuel. Its distillation temperature is smooth and increases gradually, like the diesel’s
temperature, and its boiling point is closer to that of the diesel. But its distillation temperature
for each droplet is higher than that of the diesel sample used in the study. The higher distillation
temperature will give the higher combustion efficiency, which will increase engine performance.
The effects of additive (CaO) on distillation temperatures are shown in Table 3.
As seen from Table 3, it is clear that 2% of CaO, which is blended with the WLO, decreases the
distillation temperature, and increases the volatility of the sample. Under the same conditions, when
6% and 10% of CaO are mixed with the oil, the distillation temperatures increase and volatility
decreases due to additives. It is not useful to add the additives to the oil because of the increase
in volatility. But, it is very useful to add more additives to the oil in order to decrease the amount
of sulfur. It is necessary that distillation curve of any DLF should be parallel with the distillation
curve of diesel fuel, and also it is necessary that its thermophysical properties are suitable to the
same values of the diesel fuel. Under these conditions, utilization of a fuel in a diesel engine will be
 232 H. ABURAS ET AL.

TABLE 2
Distillation Values of Standard Diesel Fuel and Diesel-like Fuel From Waste Lubricating Oil

Distillation Volume of Distillation Volume of

Temperature, ◦ C Diesel Fuel, cm3 Diesel-like Fuel, cm3

145 0 0
183 10 —
188 20 —
198 30 —
224 40 10
246 — 20
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253 50 —
265 — 30
278 60 40
286 — 50
294 — 60
304 70 —
310 — 70
335 80 80
350 — 90
360 90 95

suitable. It will be useful to compare the distillation test results obtained with the distillation results
of a diesel fuel.
Table 4 shows the distillation test results of the two samples comprised of oil and additives of
CaO with ratios of 2% and 10%, respectively.
Distillation test result of diesel fuel is also shown in these tables in order to compare the effects
of the additives on distillation temperatures.
When the WLO is blended with 2% of CaO, distillation results of the samples indicate parallel
behavior with the temperatures of the present diesel fuel in a volume of 30%. This is a very important
criterion due to the gradual increment of distillation temperature at a finite value. This gradual
increment is important because the starting ability and warm-up property of the fuel is evaluated
with the evaporation temperatures of 20–70% vaporization region of the distillation temperatures
(Yumrutas et al., 2008). Vaporization at a very narrow band of temperature is not desirable since
it will result in an immediate burning and high rate of pressure rise. The burning of all the fuel
increases temperature and the pressure of gas in the combustion chamber. Such a condition can give
rise to dangerous effects on engine components (Yumrutas et al., 2008). It is necessary that a fuel
sample burn gradually in a combustion chamber of an engine. When the sample is used as a fuel in
a diesel engine, there will be no damage to engine components. Also, 30% amount of the samples
is lighter than the diesel fuel. This is useful for the initial starting operation of the engine, but it
is detrimental for the engine when the temperature of the engine increases. When 10% amount of
the additive is blended with the oil sample, distillation temperatures increase, but they continue to
show a behavior parallel to the diesel fuel sample. That is, it is far away from the diesel fuel sample.
According to these data, it gives the best results by utilizing 2% of CaO as an additive after 30% of
total volume of the blend. The best result of the decrease in sulfur amount in the waste oil and the
effect of the CaO on the distillation temperatures.
Light and heavy fuels need to be separated from each other in order to eliminate the light portion
of the fuel or the detrimental effects of the light portion on an engine. Therefore, purified WLO
was blended with 2% CaO, and the blended oil sample was distilled. Light amount of the sample
comprising approximately first 25% of the purified sample or 20% of total oil sample was collected in
 PYROLIZING OF WASTE LUBRICATING OIL 233

TABLE 3
Effect of Temperature on Distillation Volume With CaO Additive Runs

Distillation Volume Distillation Volume Distillation Volume Distillation Volume Distillation Volume
Temperature (◦ C) for 0% CaO for 2% CaO for 4% CaO for 6% CaO for 10% CaO

46 — — — 0 —
49 — 0 — — —
50 — — — — 0
52 0 — — — —
54 — — 0 — —
73 — — — — 0
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109 — — — 10 —
118 — 10 — — 10
121 10 — 10 — —
125 — — — — —
158 — — 10 20 —
165 — 20 — — 20
171 20 — — — —
176 — — 20 — —
203 — — — 30 —
206 — 30 — — —
211 — — — — 30
218 30 — — — —
229 — — 30 — —
242 — 40 — 40 —
248 — — — — 40
256 40 — — — —
268 — — 40 — —
271 — — — 50 —
273 — 50 — — —
275 — — — — 50
285 50 — — — —
298 — 60 — 60 60
308 60 — — — —
312 — — 60 — —
315 — — — 70 —
320 — 70 — — —
327 70 — — — —
335 — — 70 — 70
337 — — — 80 —
346 — 80 — 90 —
351 80 — — — —
354 — 90 — — —
356 — — 80 — 80
360 — 95 — — —
364 90 — 90 — —
369 — — — — 90
383 — — 95 — —

a flask, and the remaining 75% part of the purified sample or 60% of total oil sample was collected in
another flask. The first and second distilled portions were distilled again. The distillation test results
of the heavy fuel, together with the diesel fuel, are shown in Table 2. It is clear that the distillation
temperature of the heavy fuel resembles to the distillation temperature of the diesel fuel. Hence, the
 234 H. ABURAS ET AL.

TABLE 4
Effect of additives (2% and 10%) on Distillation Temperature

Distillation Temperature (◦ C) Temperature (◦ C) Temperature (◦ C)

Volume, cm3 for Diesel Fuel for 2% CaO for 10% CaO

0 151 49 50
10 182 118 118
20 203 165 165
30 225 206 211
40 239 242 248
50 260 273 275
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60 277 296 297

70 298 320 334
80 329 346 357
90 360 354 368
95 — 360 —

produced heavy fuel from the purified waste oil is DLF. The higher distillation temperature will give
the higher combustion efficiency, which will increase engine performance.

Effects of the Additives on Flash Point and Density

The flash point of a flammable fuel is the lowest temperature at which it can form an ignitable mixture
in air. At this temperature the vapor may cease to burn when the source of ignition is removed. The
flash point is often used as one descriptive characteristic of liquid fuel, but it is also used to describe
liquids that are not used intentionally as fuels. Density is also important property of a fuel, as air–fuel
mixture and flame can propagate uniformly in combustion chamber of an engine. Therefore, effects
of the additives on the flash point and density are studied in this work. The results show that flash
points and densities increase with increasing the additive content. Densities of the samples increase
as a dependence of densities of the additives.

Effects of the Additives on Sulfur Removal

One very important consideration in the selection of a diesel fuel is its sulfur content. While sulfur
is one of the combustible elements in the fuel and generates energy, the primary product of that
combustion is sulfur dioxide (SO2 ), which is a major environmental pollutant. The sulfur dioxide
reacts with atmospheric water vapor to produce sulfurous and sulfuric acids, both of which contribute
to acid rains (Archie, 1991). That is why sulfur amount present in any fuel should be decreased
below the standard values if it is possible.
The additives decrease the sulfur amounts present in the waste engine oil. It is known that there
are several catalysis mechanisms to absorb sulfur present in the waste oil. One of them is given by
Guchhait et al. (2005).
In this study, CaO is used as additive to investigate effects of them on density, viscosity, flash
point, sulfur content, heating value, and distillation temperature. The effects of additive amounts
used in the present study on sulfur content of the purified oil samples. Sulfur content in the WLO
decreases when the amount of the additive increases. The highest decrease (65%) in sulfur present
in the waste lubricating oil takes place when the CaO with the ratio of 10% is blended with the oil.
CaO is the best additive for removal of sulfur in WLO, due to its strong basic character.
 PYROLIZING OF WASTE LUBRICATING OIL 235

CONCLUSIONS

In this study, the feasibility of using WLOs as a DLF was investigated experimentally. In this context,
a DLF was produced by applying pyrolytic distillation method. In the production process, WLO was
purified by filtration operation.
The additive known as CaO with ratios of 2%, 4%, 6%, 8%, and 10% were blended with the
purified waste lubricating oil. After the pyrolytic distillation of the mixed samples was performed.
Fuel characteristics of the DLF, such as density, flash point, viscosity, sulfur content, and heating
value were tested and found to be close to the values of the diesel fuel used in the present study.
Flash point and density increase but sulfur amount decreases with the increasing of additive
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amounts. The lowest flash point, density, and sulfur of the fuel samples were obtained by using CaO.
The most suitable distillation product was obtained when CaO was used as an additive with a
ratio of 2% after 10% amount of the sample.

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