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Waste Management 47 (2016) 149154

Contents lists available at ScienceDirect

Waste Management
journal homepage: www.elsevier.com/locate/wasman

Biodiesel production using fatty acids from food industry waste using
corona discharge plasma technology
A.L.V. Cubas a,, M.M. Machado b,c, C.R.S.C. Pinto c, E.H.S. Moecke b,e, A.R.A. Dutra d
a
UNA PCA, Articulation Academic Unit of Production, Construction and Agribusiness, Environmental Engineering, University of Southern Santa Catarina UNISUL, Avenue
Pedra Branca, 25, CEP: 88279900, Palhoa, SC, Brazil
b
Environmental Engineering, University of Southern Santa Catarina (Unisul), CEP 80137270, Palhoa, SC, Brazil
c
Post Graduation in Environmental Engineering, Federal University of Santa Catarina (UFSC), CEP 88040900, Florianpolis, SC, Brazil
d
Production Engineering, University of Southern Santa Catarina (Unisul), CEP 80137270, Palhoa, SC, Brazil
e
Departament of Science and Technology of Food, Federal University of Santa Catarina (UFSC), CEP 88034001, Florianpolis, SC, Brazil

a r t i c l e

i n f o

Article history:
Received 9 March 2015
Revised 26 May 2015
Accepted 26 May 2015
Available online 7 July 2015
Keywords:
Fatty acids
Waste frying oil
Methyl esters
Corona discharge plasma
Biodiesel

a b s t r a c t
This article aims to describe an alternative and innovative methodology to transform waste, frying oil in a
potential energy source, the biodiesel. The biodiesel was produced from fatty acids, using a waste product
of the food industry as the raw material. The methodology to be described is the corona discharge
plasma technology, which offers advantages such as acceleration of the esterication reaction, easy
separation of the biodiesel and the elimination of waste generation. The best conditions were found to
be an oil/methanol molar ratio of 6:1, ambient temperature (25 C) and reaction time of 110 min and
30 mL of sample. The acid value indicates the content of free fatty acids in the biodiesel and the value
obtained in this study was 0.43 mg KOH/g. Peaks corresponding to octadecadienoic acid methyl ester,
octadecanoic acid methyl ester and octadecenoic acid methyl ester, from the biodiesel composition, were
identied using GCMS. A major advantage of this process is that the methyl ester can be obtained in the
absence of chemical catalysts and without the formation of the co-product (glycerin).
2015 Elsevier Ltd. All rights reserved.

1. Introduction
Waste oils and fats should not be discarded in the public
sewage system, because they can cause signicant environmental
impact (Giraol et al., 2011). Oils in rainwater and sanitary sewage
systems emulsify with organic matter, causing blockages in grease
traps and pipes. Due to their immiscibility with water and lower
density, there is a tendency toward the formation of oily lms on
the water surface, inhibiting the exchange of gases with the
atmosphere. This leads to the depletion of oxygen and anaerobic
conditions in water bodies, resulting in the death of sh and other
aerobic organisms (Reis et al., 2007).
In the public sewage system, blockages can cause pressure to
build up, leading to the inltration of sewage into the soil, groundwater pollution and/or surface reux% (Reis et al., 2007).
Furthermore, in areas where sewage treatment is installed, when
waste oil enters the system it interferes with the treatment
processes and increases the cost by up to 45% (Reis et al., 2007).

Corresponding author.
E-mail address: anelisecubas@gmail.com (A.L.V. Cubas).
http://dx.doi.org/10.1016/j.wasman.2015.05.040
0956-053X/ 2015 Elsevier Ltd. All rights reserved.

As a result of impacts and environmental damage caused by the


improper disposal of frying oils, it is necessary to treat these
wastes nal disposal or, in the reuse of this waste. The utilization
of frying oils for biodiesel production is a form of reuse, which is
through the transesterication reactions which can be performed
through homogeneous catalysis with use of a basic catalyst or acid,
enzyme catalysis (biocatalyst) heterogeneous catalyst (zeolites,
clays) or in the absence of catalyst, with the use of an alcohol in
supercritical conditions (Demirbas, 2006; Ranganathan et al.,
2008), or by using corona discharge plasma as a catalyst for
reactions.
Biodiesel is the fuel obtained from vegetables oils or animal fat,
which can substitute petroleum diesel, total or partially in car
engines, trucks, tractors, and also in stationary engines, such as
electricity generators, motor pumps, among others (Silva and
Freitas, 2008).
Rodrigues and Lunkes (2011) point out that the production of
biodiesel does not compete economically with mineral diesel due
to its high cost of production, however, offers advantages in environmental and social aspects. In the environmental scope, it shows
a reduction in the amount of pollutants emitted upon ring, such
as carbon monoxide, sulfur oxides and carbon dioxide. In the social

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A.L.V. Cubas et al. / Waste Management 47 (2016) 149154

scope, it is observed that the production of biodiesel was conceived


as a means of social inclusion of family farming in the production
chain and the economy as a whole, beneting from the creation of
jobs and income.
The use of waste frying oil as a feedstock for biodiesel production can therefore reduce the cost of the nal product, besides
being environmentally friendly. Due to the rapid decline in crude
oil reserves, the use of vegetable oils for the production of diesel
fuels is being promoted in many countries. Depending on the
climatic and soil conditions, different nations are looking into
different vegetable oils for diesel fuel production. For example,
soybean oil in the USA, rapeseed and sunower oils in Europe,
palm oil in Southeast Asia (mainly Malaysia and Indonesia), and
coconut oil in Philippines are being considered as substitutes for
mineral diesel (ElSolh, 2011).
The world production of waste oils and fats in 2008 was around
154 million tons. A variety of raw materials can be used to produce
biodiesel (MPCO, 2008). These include virgin oil feedstock
(U.S Energy Information, 2013), waste vegetable oil (WVO), animal
fats (Leonard, 2007), algae (Kiong, 2006), oil from halophytes such
as Salicornia bigelovii (Glenn et al., 1998) and sewage sludge
(Casey, 2010). Many researchers have suggested that WVO is the
best raw material to produce biodiesel, but since the available
supply is considerably less than the amount of petroleum
based-fuel that is burned for transportation and home heating
globally, this local solution does not scale well.
However, oils and fats undergo several physical and chemical
changes when used repeatedly in the frying process. The physical
changes observed in vegetable oil after frying include: (i) increased
viscosity, (ii) increased specic heat, (iii) a change in the
surface tension, and (iv) a change in the color (Cvengros and
Cvengrosova, 2004).
During the frying process, different types of reactions occur in
the oils, for instance, thermolytic, hydrolytic and oxidative
(Kulkarni and Dalai, 2006; Bensmira et al., 2007; Cvengro and
Cvengroov, 2004). These reactions can lead to the formation of
undesirable compounds which are harmful to human health, such
as free fatty acids (FFA). These polar compounds FFA signicantly
affects the conversion to alkyl esters (biodiesel) in the conventional
transesterication process with basic catalysts. In the transesterication of vegetable oils, a triglyceride reacts with an alcohol in the
presence of a strong acid or base, producing a mixture of fatty
acids, alkyl esters and glycerol (Schuchardt et al., 1998).
Among the most commonly used alkaline catalysts in the biodiesel industry are potassium hydroxide and sodium hydroxide
akes which are inexpensive, easy to handle in transportation
and storage, and are preferred by small producers (Singh et al.,
2006). However, these catalysts are now considered to be outdated, since even when using rened vegetable oils with a low content of free fatty acids and low water content, small amounts of
soap are formed, promoting the entrainment of esters with varying
amounts with glycerin phase, thereby reducing the ester yield in
the light phase containing glycerin and generating more contaminants. In biodiesel production carried out through traditional
processes the amount of glycerol generated is equivalent to 10%
of the biodiesel produced, and this negatively inuences the
national and international market for glycerin (Dasari et al., 2005).
In this article, different biodiesel production processes which
involve the use of a corona plasma reactor are described. For this
purpose, a pilot corona discharge plasma system was built for
the production of biodiesel, appropriate pilot conditions being set
to obtain the best rates for the conversion of waste into biodiesel.
The batch production of biodiesel occurred without the use of acid
or alkaline catalysts, while the biofuel samples were subjected to
chromatography analysis (GCMS) to conrm the presence of
esters (biodiesel). This technology is considered to be more

promising than the conventional catalytic processes due to a


shorter reaction time, no formation of glycerin and ease of
biodiesel separation.
The corona plasma process is also known as corona plasma, as
well as dielectric barrier (Ragazzi et al., 2014), plasma jet, electron
beam, etc. (Fridman, 2008; Fridman et al., 2007; Kim, 2004; Preis
et al., 2013; Pankaj et al., 2014). The corona discharge plasma
comprised of a partially ionized gas, in which the average energy
of the electrons is considerably higher than the energy of the ions
and the gas molecules. Plasma discharges are widely used for
processing and are indispensable in many technological applications (Milosavljevic et al., 2007).
The plasma discharge is formed by applying an intense electric
eld, which causes the formation of an electronic self-propagating
arc within the gas volume. Once the ionized gas is generated, the
electrons collide with molecules, creating chemically-active
species known as radicals. Radicals, once produced, can replace
the conventional chemical form of the catalyst during transesterication reactions, facilitating the separation of the biodiesel
formed (Istadi, 2006; Istadi et al., 2009; Kogelschatz, 2003).
The corona discharge plasma reactor technology offers
advantages related to the production of biodiesel compared to
conventional methods due to faster reaction times and the easy
separation of the nal product (Istadi et al., 2009).

2. Methodology
2.1. Raw material acquisition and preparation
The raw material, waste frying oil originating from the food
frying process, was purchased from local restaurants. The oils
and fats initially underwent a pretreatment step with heating to
50 C and ltering for the removal of impurities.
Before starting the experiments to obtain biodiesel, the raw
material was characterized by determining the acidity number
by titration (AOAC n. 940.28, 2005) and the water content by using
the Karl-Fischer method (ISO 12937, 2000). Saponication and
peroxide values were determined by the AOAC ofcial method
920.160 and 965.33, respectively. The AOAC ofcial method
993.20 (Wijs method) was used to determine the Iodine values.
2.2. Corona discharge reactor
The body of the reactor was comprised of a cylindrical quartz
tube (300  110 mm), wrapped with a spiral of stainless steel
250 mm in length, which served as an electrode. A stainless steel
screw (400  5 mm) in the center of the quartz tube was used to
seal the exits and keep the second electrode (screw) in the center
of the tube (Fig. 1).
The used frying oil with methanol and water was introduced
into the reactor through an access positioned at the right side of
the reactor cap, throughout the process was injected 1 L/min of
argon into the reactor. The nal product, methyl ester (biodiesel),
is pulled across the reactor and a source of alternating current
voltage of 17 kV is used to generate the plasma.
A photo of the system transporting the waste frying oil can be
seen in Fig. 2 (note the violet uorescence emitted by the plasma).
2.3. Pilot optimization
To establish the appropriate conditions for the pilot and obtain
better oil to biodiesel conversion rates using the corona discharge
plasma technology, tests were carried out varying the residence
time of the sample in the reactor (15120 min), and the sample

A.L.V. Cubas et al. / Waste Management 47 (2016) 149154

151

Fig. 1. Plasma reactor with annular cylindrical electrodes. Source: Author.

(RTX-5 MS 30 m  0.25 mm and thickness of 0.25 lm), using


helium as the carrier gas with a ow rate of 1.2 ml/min. The analysis was performed in split mode. The temperature program used
for the GC analysis was: 60 C, held for 5 min, increased at a heating rate of 6 C/min to 300 C, held for 15 min. The total chromatographic analysis time was 60 min. The temperatures of the injector
and the ion source were 280 C and 200 C, respectively. The transfer line was maintained at 250 C.

3. Results and discussion


3.1. Waste frying oil properties

Fig. 2. Non-thermal plasma reactor used in the experiments. Source: Author.

quantity in the reactor (20 and 30 ml), keeping the molar fraction
of methanol:oil equal to 1:6.
2.4. Biodiesel production process
In the production of biodiesel using plasma technology, the
transesterication reaction occurred inside the corona discharge
plasma reactor after mixing the raw material with a short-chain
alcohol (in this case 99.8% methanol, obtained from Audaz
Brasil), gas argon (1 L/min). The corona discharge plasma reactor
promoted the transesterication reaction, where the highly energetic plasma atmosphere promotes the formation of methyl esters
(biodiesel) in the absence of a chemical catalyst, thereby replacing
chemical catalysis.
The transesterication reaction that may occur in the plasma
process can be seen in Fig. 3.

The sample of waste frying oil used in the production of biodiesel through the cold plasma technology contained high concentrations of free fatty acids and high levels of peroxides, as shown in
Table 1.
The peroxide value (19.60 mEq/kg) and the content of free fatty
acids (2.16%) indicate that changes in the waste frying oil occurred
during its use. These changes are expected for this type of oil,
which is generally discarded since it is unt for food preparation.
Frying oil should not be used when the content of free fatty acids
exceeds 0.9% (Brazil, 2004). Yuan et al. (2008) recommends that
the content of free fatty acids for the production of ethyl and
methyl esters (biodiesel) with alkaline chemical catalysis should
be less than 2% and the oil must be pretreated in order to decrease
the amount of acidity.
The saponication number is an indication of the relative
amount of fatty acids of high and low molecular weight present
in the oil composition. The iodine value is a measure of the
amount of fats present and is expressed in terms of the number
of centigrams of iodine absorbed per gram of sample (% of
absorbed iodine). This value indicates the amount of unsaturated
fatty acids, such as linolenic acid (C18H30O2 C18:3), linoleic acid
(C18H32O2 C18:2) and oleic (C18H34O2 C18:1), present in the
oil (Singh and Singh, 2010).

2.5. Methyl esters (biodiesel) characterization


3.2. Methyl ester (biodiesel) production
To characterize the biodiesel the following parameters were
determined: peroxide and acid number according to AOAC
(2005), color, appearance and miscibility in diesel oil, as recommended by the Brazilian Agency of Petroleum (ANP) and
Resolution n. 45/2014 (Brazil, 2014). The composition of the biodiesel products were analyzed using a ThermoFinnigan Gas
Chromatograph, model Trace GC Ultra, Milan, Italy, coupled to a
Finnigan Polaris Q mass spectrometer with a capillary column

The operation variables were oil/methanol molar ratio


(1:31:6), water concentration (0.01.0 wt%), and reaction time
(15120 min), and in all experiments the reactions were carried
out in the absence of catalysts and the alcohol used was methanol
(xed parameters).
The reaction between the waste frying oil and methanol,
assisted by corona discharge plasma, was monitored by

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Fig. 3. Biodiesel transesterication reaction by plasma. Source: Debacher et al. (2015).

Table 1
Properties of the waste frying oil used in the production of biodiesel through an
innovative process of non-thermal plasma corona discharge. Source: Author.
Properties

Value

Acid value (mg KOH/g)


Peroxide value (mEq/kg)
Moisture (%)
Saponication value (mg KOH/g)
Iodine value (g iodine/100 g sample)
Density at 20 C (g/cm3)

2.16
19.60
0.58
174.89
106.03
0.9276

thin-layer chromatography (TLC) and the retention factor (Rf) value


of 0.8 veried the formation of methyl esters.
The best conditions were found to be an oil/methanol molar
ratio of 6:1, ambient temperature (25 C) and reaction time of
110 min and 30 mL of sample and 1 ml of H2O.
Table 2 shows the properties of the biodiesel obtained from the
waste frying oil. The acid value indicates the content of free fatty
acids in the biodiesel and the value obtained in this study was
0.43 mg KOH/g. The presence of free fatty acids can lead to corrosion and may be a symptom of water in the fuel (Gerpen, 2005).
The acid value of 0.48 mg KOH/g complies with the ANP
Resolution n.45 of 25/8/2014 which deals with the biodiesel specications, with regard to marketing, certication and tax documents (Brazil, 2014).

The free fatty acids in the oils were transesteried using the
non-thermal plasma technology. Fig. 4 shows the GCFID
(Fig. 4A) and CGMS chromatograms obtained for the waste frying
oil methyl esters. The GCMS analysis showed the three fatty acid
components of the esters: octadecadienoic acid methyl ester
(C18:2 D9,12) (Fig. 4 E), octadecanoic acid methyl ester (C18:1
D9) (Fig. 4F) and octadecenoic acid methyl ester (C18:0) (Fig. 4G).
The nonexistence of specic papers in the literature on the
application of plasma corona discharge to produce biodiesel hampers the description of the exact mechanism of plasma biodiesel
forming reaction, but studies of possible reactions of the
non-thermal plasma (Debacher et al., 2015) suggest that the
high-energy atmosphere of plasma facilitates the breakage of the
double bonds and hydroxyl groups, which leads to the conclusion
that, besides the formation of the methylated esters, there is the
formation of H2O present in a small percentage of methanol which
does not react with triglyceride and appears with biodiesel formed
in the end of the process (Fig. 3).
The addition of water molecules in biodiesel production processes with discharge leads to generation of H+ and OH via dissociation, ionization and vibrational/rotational excitation of water
molecules. In the reaction with organic compounds is generated
three basic mechanisms of reaction, are hydrogen abstraction,
the unsaturated electrophilic addition reaction and electron transfer (Jiang et al., 2014). In the case of compounds having aliphatic
hydrocarbons such as waste cooking oil, the hydrogen abstraction
is the primary mechanism for producing methylated esters and
water. (Jiang et al., 2014).

3.3. Identication of esters by chromatography (CGFID and CGMS)


The NIST (National Institute of Standards and Technology)
library was used in the GCMS to conrm whether the peaks
matched with known standards (considering both the retention
times and structural details) and, additionally, to identify novel
peaks in our samples using the highest probability methods
(considering the retention times, structural details and isotopic
patterns; Fig. 4BD).

Table 2
Waste frying oil methyl ester biodiesel properties. Source: Author.
Properties

Value

Acid number (mg KOH/g)


Peroxide value (mEq/kg)
Retention factor (Rf)
Aspect

0.48
9.60
0.82
Clear and free of impurities

4. Conclusions
Based on the results of this study, it is possible to produce biodiesel from waste frying oil (saturated) using corona discharge
plasma technology. Gas chromatography (GCFID) was used to
verify the formation of methyl esters of fatty acids. Peaks corresponding to octadecadienoic acid methyl ester, octadecanoic acid
methyl ester and octadecenoic acid methyl ester, from the biodiesel composition, were identied using GCMS. A major advantage
of this process is that the methyl ester can be obtained in the
absence of chemical catalysts and without the formation of the
co-product (glycerin).
This study showed that corona discharge plasma is a promising
technology, since it does not require a catalyst and the formation of
a co-product does not occur. Thus, with the use of waste frying oil
as a raw material and the application of the innovative technology
of cold plasma an environmentally-friendly product.

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4.00

uV(x100,000)
Chrom atogram

3.75

I-Octadecanoic acid methyl ester

(A)

3.50

325.0

II-Octadecenoic, acid methyl ester

300.0

3.25

275.0

III

3.00
2.75

250.0

2.50

225.0

2.25

200.0

II

2.00

175.0

1.75
1.50

150.0

1.25

125.0

1.00

100.0

0.75
0.50

75.0

0.25

50.0

0.00

25.0

-0.25
5.0

(B)

10.0

15.0

20.0

25.0

30.0

35.0

40.0

45.0

50.0

min

0.0

I-Octadecanoic acid methyl ester

(E)

II-Octadecenoic, acid methyl ester


III-Octadecadenoic, acid methylester

(C)

(D)

(F)

(G)

Fig. 4. Comparison of results for the same sample of waste frying oil methyl esters analyzed by GCFID and GCMS; (A) GCFID spectrum; (BD) NIST library ndings for the
unidentied peak of interest using GCMS; (E) GCMS showing unidentied peak of interest now identied as octadecadienoic acid methyl ester; (F) GCMS showing
unidentied peak of interest now identied as octadecanoic acid methyl ester; (G) GCMS showing unidentied peak of interest now identied as octadecenoic acid methyl
ester.

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A.L.V. Cubas et al. / Waste Management 47 (2016) 149154

Acknowledgements
The authors acknowledge UNISUL, UFSC and nancial support
from Foundation for Research and Innovation of Santa Catarina
State FAPESC (Brazil).
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