International Journal of Petroleum Science and Technology

ISSN 0973-6328 Volume 11, Number 1(2017), pp. 9-21

© Research India Publications
http://www.ripublication.com

Conversion of Waste Cooking Oil to Biodiesel

Rummi Devi Saini

Chemistry Department,
SMDRSD College Pathankot, 145001, India.

Abstract
Recycled waste cooking oil is harmful to health, but it is not environment
friendly to dispose off used cooking oil. The best solution is to use it for
industrial purposes, namely to convert it into biodiesel. Due to the awareness
of adverse effects of conventional fuels to environment and the frequent rise in
crude oil’s price, the need for sustainable and environment friendly alternate
source of energy has gained importance in recent years. Biodiesel is proved to
be the best replacement for diesel because of its unique properties like
significant reduction in greenhouse gas emissions, non-sulphur emissions,
non-particulate matter pollutants, low toxicity and biodegradability. Cost of
biodiesel produced from virgin vegetable oil through transesterification is
higher than that of fossil fuel, because of high raw material cost. To minimize
the biofuel cost, these days, waste cooking oil is used as feedstock. Catalysts
used in this process are usually acids, base, and lipase. Since lipase catalysts
are much expensive, the usage of lipase in biodiesel production is limited. In
most cases, NaOH is used as alkaline catalyst, because of its low cost and
higher reaction rate.
In the case of waste cooking oil containing high percentage of free fatty acid,
alkaline catalyst reacts with free fatty acid and forms soap by saponification
reaction. Also, it reduces the biodiesel conversions. In order to reduce the
level of fatty acid content, waste cooking oil is pre-treated with acid catalyst to
undergo esterification reaction, which also requires high operating conditions.
In this paper, the pre-treatment step, the physical and chemical properties of
waste cooking oil, Esterification, Transesterification and production of
Biodiesel from waste cooking oil by various methods and catalysts reported so
10 Rummi Devi Saini

far and the factors affecting the process parameters reported have been
summarized.

INTRODUCTION
Biodiesel is an alternative diesel fuel derived from vegetable oils or animal fats. The
main components of vegetable oils and animal fats are triglycerides known as ester of
fatty acid attached to glycerol. One of the main driving force for biodiesel widespread
is the limited greenhouse gas emission (CO2 being the major one). The term waste
cooking oil (WCO) refers to vegetable oil that has been used in the cooking of food
and which is no longer viable for its further use in food production. WCO arises from
many different sources, including domestic, commercial and industrial. WCO is a
potentially problematic waste stream which requires proper management. The
disposal of WCO can be problematic when disposed irresponsibly[1,2].
Any fatty acid sources may be used to produce biodiesel. Therefore, any animal or
plant lipid should be ready substrate for the production of biodiesel. The use of edible
vegetable oils and animal fats for biodiesel production has recently been of great
concern because they compete with food material- the food versus fuel dispute. There
are concerns that biodiesel feedstock may compete with food supply in the long term.
From an economic point of view; the production of biodiesel is very feedstock
sensitive. The cost of feedstock accounted for 88% of total estimated cost of
production. Reusing of these waste oils and fats not only reduce the burden of the
government in disposing the waste, maintaining public sewers, and treating the oily
waste water, but also lower the production cost of biodiesel significantly. Biodiesel
can be produced from any material that contains fatty acids, be they linked to other
molecules or present as free fatty acids. Thus various vegetable fats and oils, animal
fats, waste greases, and edible oil processing wastes can be used as feed stocks for
biodiesel production. The choice of feedstock is based on variables such as local
availability, cost, government support and performance as a fuel. The primary
feedstock is a vegetable oil or animal fat. Biodiesel is generally considered to be
renewable[1-4].
Since the carbon in the oil or fat originated mostly from carbon dioxide in the air,
biodiesel is considered to contribute much less to global warming than fossil fuels.
Diesel engines operating on biodiesel have lower emissions of carbon monoxide,
unburned hydrocarbons, particulate matter, and air toxics than when operated on
petroleum-based diesel fuel[23]. Neat (unprocessed) vegetable oil can not be used in
the compression ignition engines as it is reported to cause several problems due to its
high viscosity. Biodiesel which is accepted as an attractive alternative fuel[4,6], is
prepared by transesterification of vegetable oils and animal fats with an alcohol in
presence of a catalyst[3,21,22]. However, the land use for production of edible oil for
Conversion of Waste Cooking Oil to Biodiesel 11

biodiesel feedstock competes with the use of land for food production. Moreover, the
price of edible plant and vegetable oils is usually higher than petro diesel. The use of
waste cooking oil as biodiesel feedstock reduces the cost of biodiesel production .
Hence, the use of waste cooking oils and non-edible oils should be given higher
priority over the edible oils as biodiesel feedstock[9].
Biodiesel is superior to fossil diesel fuel in terms of exhaust emissions, cetane
number, flash point and lubricity characteristics, without any significant difference in
heat of combustion of these fuels[17]. Moreover, biodiesel returns about 90% more
energy than the energy that is utilized to produce it. Biodiesel mixed with
conventional diesel in some proportions can be used to run any existing conventional
compression ignition engine and does not require any amendments to be done to the
engine[20]. Due to benefits like renewable in nature, low cost and green house gas
reduction potential, biodiesel is nowadays incorporated all over the world especially
in developed countries like USA, France, Brazil in different proportions with
diese[4,9]l. It is also estimated that India can supplement 41.14% of its total diesel
fuel consumption, if resources like waste cooking oil and other bio wastes were used
as raw material for biodiesel production.

3. Transesterification of waste cooking oil : In transesterification reaction, the

triglyceride component of oil reacts with the alcohol in the presence of NaOH or any
other catalyst to give ester and glycerol as shown in the reaction-1. In general, there
are three systems of transesterification with vegetable oil or an animal fat as a starting
material, they are homogeneous, heterogeneous systems and enzymatic, based on the
catalyst employed in the process[3,16,21,22]. Used vegetable oil is reacted with
alcohol. In most of the cases methanol is used because of better efficiency[19].
However ethanol and isopropyl alcohol can also be used, Ethanol is used for animal
fats. It has been reported that, transesterification process depends upon many
parameters which are reaction temperature and pressure, reaction time, rate of
agitation, type of alcohol used and molar ratio of alcohol to oil, type and
concentration of catalyst used and concentration of moisture and free fatty acid in the
feed stock waste oil[10,27,41]. The optimal values of these parameters largely depend
on the physical and chemical properties of the feedstock oil for attaining higher
conversion[17].
12 Rummi Devi Saini

Trans esterification reaction

Side reaction ( Saponification Reaction )

Side reaction ( Hydrolysis reaction)

Esterification: A schematic representation of the transesterification reaction.

The production of majority of biodiesel today is done through homogeneous alkali-
catalysed transesterification of edible vegetable oils[22]. Homogeneous catalysts are
soluble during the reaction, they may be liquid or gaseous. They are of two types:
Acidic and Alkaline. Acidic catalysts like H2SO4 are used usually for Esterification
while Alkaline catalysts like NaOH and KOH are used for transesterification. The
benefits of homogenous catalysts are (i) they can catalyse reaction at lower reaction
temperature and atmospheric pressure; (ii) high conversion can be achieved in less
time, (iii) easy availability and its low cost . This process permits a good product
quality in a relatively shorter reaction time .The effective use of Alkaline homogenous
Conversion of Waste Cooking Oil to Biodiesel 13

catalyst is limited only for refined vegetable oil with less than 0.5 wt.% FFA or acid
value less than 1 mg KOH/g. Moreover, the removal of these catalysts after the
reaction is complete needs the washing of biodiesel with water which might result in
loss of Fatty acid alkyl esters, energy consumption and generates large amount of
waste water[11]. This also increases the overall cost of biodiesel production as it is
difficult to recover the catalyst which may cause reactor corrosion. The triglyceride
and alcohol should be anhydrous and a Low free fatty acid (FFA) content of raw
material is necessary to avoid the soap production ( by alkaline catalyst consumption)
and low product yields.
Heterogeneous catalysts are the solids and are insoluble during the reaction .Most of
them are m etal oxides like KBr/CaO, chitosan,SrFe2O4/SiO2-SO3H and catalyst
derived from chicken bones. Heterogeneous (solid) catalysts are preferred over
homogenous as they can be reused, allow a better separation, better quality of the final
products and are economical[3,12]. Solid base catalysts are considered to be
promising catalysts for transesterification as they have advantages such as easy
removal of catalyst from reaction mixture, can tolerate high FFA, no washing is
required, easy regeneration, less corrosive character, low in cost and it is a more
environment friendly. However, there are also few disadvantages of the
heterogeneous catalysts such as they require extreme reaction conditions (higher
temperature and reaction times) for preparation compared to homogeneous
process[22]. The calcinations temperature for catalyst obtained from chicken bones is
9000 ᵒ C. Homogeneous catalysts might be required to be characterized by
sophisticated equipment’s techniques like Fourier Transform Infrared spectrometry
(FTIR), X-ray Diffraction (XRD) and Scanning Electron Microscopy(SEM)
techniques . Moreover, techniques like Response Surface Methodology (RSM) using
Central Composite Design (CCD) need to be employed to study the effects of process
variables on the reaction yield.
Solid acid catalysts like zeolites, mixed oxides, sulphates, zirconia and ion exchange
resins might be very exciting for the production of biodiesel from feedstocks with
high FFA contents, but still their activity is low because it depends upon the reaction
conditions and higher amount of catalyst consumption related to homogeneous
catalysts[3]. Moreover in some of the cases, soap formation is also seen using
heterogeneous catalyst and purification is required in most of the cases to ensure the
needed quality of fuel. Enzymatic catalysts are becoming one of the most promising
catalysts for the biodiesel production. They can stand high FFA and simultaneous
Esterification and Transesterification take place in these reactions. Enzymatic
catalysts[3] are recognised for being cost effective catalysts, smaller reaction time and
lower reaction temperature. However reactions using enzymatic catalysts require
more amount of catalyst and production yield is less compared to homogeneous and
heterogeneous. Generally, heterogeneous base catalysts are made in different ways,
14 Rummi Devi Saini

such as impregnation of amounts of base metals, precipitation, conversion to oxides

by calcination, and co-precipitation. Borges and Díaz used potassium-loaded pumice
material (K-Pumice) as the heterogeneous catalyst in the sunflower oil and waste oil
transesterification reaction for biodiesel production, using a packed-bed catalytic
reactor in a recirculation system[13]. Pumice particles (1.40–3.0 mm) were introduced
into a potassium hydroxide time, 20:1 methanol/oil molar ratio, and an 8.2 cm
catalytic packed-bed length, the value of the content of the biodiesel required by
Standard UNE-EN 14124 (96.5 %) was achieved, reaching a 99.5 % value.
Roschat et al. undertook transesterification aqueous solution in order to attain
potassium interchange, generating some basic sites on the natural material. The
reaction rate increased slightly when the temperature was increased from 50 to
60°C[14]. However, using a 55°C reaction temperature, a 2 hr reaction, mixing WCO,
palm oil, soybean oil and rice bran with methanol to make a biodiesel and glycerol
by-product, using calcined waste coral fragments in solid form as the catalyst. Under
optimum reaction conditions, coral fragments calcined at 700°C for 1 hr, a catalyst/oil
ratio of 100 wt.%, a methanol/oil molar ratio of 15:1, and a reaction temperature of 65
ᵒ C with constant stirring, biodiesel with a yield of over 98 % in 2 hr can be formed.
The synthesized mixed oxide catalysts comprising CaO and ZrO2 mixed oxides with
various Ca-to-Zr molar ratios were employed for the transesterification of WCO as
the feedstock with methanol to produce biodiesel at 65 °C and 1 atm. The
experimental results showed that the activity of synthesized catalysts increases with
increase in molar ratio of Ca-to-Zr but at the same time results in decreased stability
of the catalysts[15]. Under the appropriate transesterification conditions at 65 °C,
catalyst loading 10 wt.%, methanol-to-oil molar ratio 30:1, and reaction time 2 hr, a
biodiesel yield of 92.1 % could be attained over the CaO-ZrO2 catalyst with a Ca-to-
Zr molar ratio of 0.5. If the acid value of waste cooking oil exceeds 1-2 mg KOH/mg
of feed stock, then pre-treatment of waste cooking oil is required before it gets reacted
with alkaline base catalyst[16-19].

FACTORS AFFECTING BIODIESEL PRODUCTION

The viscosity of the vegetable oil changes drastically due to process of
transesterification. The removal of high viscosity component, glycerol, gives the
product which has low viscosity like the fossil fuels. The biodiesel produced is
completely miscible with mineral diesel in all proportions. After transesterification
flash point of the biodiesel is dropped and the cetane number is improved. The yield
of biodiesel in the process of transesterification is dependent on many factors such as
reaction temperature, reaction time, catalyst, presence of moisture and free fatty acids
(FFA), and molar ratio of alcohol and oil [41 and 27] .
Conversion of Waste Cooking Oil to Biodiesel 15

Temperature
Yield of biodiesel is largely affected by the Reaction temperature. For example,
higher temperature increases the reaction rate and reduces the reaction time as the
viscosity of oils is decreased. However, if the reaction temperature is increased
beyond the optimal level, it leads to decrease of biodiesel yield, as higher reaction
temperature speeds up the saponification of triglycerides [28] and facilitates the
vaporisation of methanol resulting in reduced yield [29]. So the transesterification
reaction temperature should be kept below the boiling point of alcohol to prevent the
evaporation of alcohol. The optimal reaction temperature may vary from 50°c to 60°c
depending upon the nature of oils or fats used [28] which should be near the boiling
point of the alcohol for faster conversion. Methyl esterification of the FFAs could be
carried out appreciably at room temperature up to 78% conversion after 60 minutes
but it might require a longer reaction time [30].
Reaction time: An increase in reaction time has been found to increase fatty acid
esters conversion. In the beginning the reaction is slow due to mixing and dispersal of
alcohol and oil, then after some time the reaction proceeds very fast and the maximum
ester conversion has been found to be attained within 90 min. Further increase in
reaction time does not cause any increase in the yield of biodiesel. Moreover, longer
reaction time than this leads to the decrease in the yield of biodiesel due to the
reversible nature of the transesterification reaction causing loss of esters as well as
soap formation [28] and 31].
Methanol to Oil Molar ratio: Esterification reaction is reversible so in order to shift
the reaction to the right i.e to increase the yield of biodiesel, either the use of excess
alcohol or the removal of one of the products from the reaction mixture is
recommended. The removal of one of the products is generally preferred for the
reaction to proceed to completion. The reaction rate has been found to be highest
when 100% excess methanol is used [32 and 29]. Amongst methanol, ethanol,
propanol, butanol and amyl alcohol which can be used in the transesterification
reaction, the methanol is used more frequently due to its low cost. Moreover, it is
physically and chemically advantageous as it is polar and shortest chain alcohol.
Whereas, in the transesterification process ethanol is preferred alcohol compared to
methanol as it is renewable and biologically less invasive to the environment and
could be derived from agricultural products. The effect of volumetric ratio of
methanol/ ethanol to oil has been studied and it was observed that highest biodiesel
yield was nearly 99.5% at 1:6 oil/methanol. But biodiesel yield using methanol has
been found to continuously increase with increase of methanol molar ratio [33].
Type and Amount of Catalyst
Biodiesel formation is also depends on the concentration of catalyst. In the
transesterification process, the type and amount of catalyst needed generally depend
16 Rummi Devi Saini

on the quality of the oil or fat, alcohol and the method applied for the process. Sodium
hydroxide (NaOH) or Potassium hydroxide (KOH) are the most commonly used
catalyst for biodiesel production [28]. For pure starting materials, any type of catalyst
could be used for the transesterification process. However, homogenous
transesterification process is unsuitable for starting materials having high moisture
and free fatty acids contents, as there is a great probability of occurrence of
saponification process instead of transesterification process.
The yield esters usually increase with increasing amount of catalyst as there is
availability of more active sites by additions of larger amount of catalyst in the
transesterification process, but it is not profitable due to cost of the catalyst itself. So
it is necessary to determine the optimum amount of catalyst essential in the
transesterification process [33 and 31].
Mixing Intensity
Mixing is very important in the transesterification process, as oils and alcohols are
not completely miscible and reaction can take place only in the interfacial region
between the liquids hence transesterification reaction becomes a slow process.
Therefore, sufficient mixing between these two types of reactants is essential to
stimulate contact between these two reacting materials in order to promote the
transesterification reactions to take place [31] and [33]. Most of the studies show that
the reactants initially form a two-phase liquid system during the transesterification
reaction and the mixing has been found to play an important role in the slow rate of
the reaction but as phase separation ends, effect of mixing becomes insignificant
[35].The intensity of the mixing may be changed depending on its requirement in the
transesterification process. For sufficient and uniform mixing of the feedstock the
mixing intensity is usually increased, especially if the vegetable oils with high
viscosity are used as the feedstock, intensive mechanical mixing is required [31] and
[33].
Free fatty acid and water content
The free fatty acid and water content have substantial effect on the transesterification
of glycerides with alcohol using catalyst. The high free fatty acid (FFA) content more
than 1% w/w, will cause the soap formation and the separation of products extremely
difficult, and leads to low yield of biodiesel product [36]. In addition to this formation
of gels and foams also hampers the separation of glycerol from biodiesel [28]. For
example, water content in waste cooking oil speeds up the hydrolysis reaction and
simultaneously reduces the amount of ester formation [37]. To overcome this
difficulty, supercritical methanol method was suggested as water has been found to
have less influence in supercritical methanol method [28]. So, water content should
not exceed 0.5% in order to obtain 90% yield of biodiesel and it is more dangerous for
an acid-catalysed reaction than base catalysed reaction [38]. The reaction of FFAs
Conversion of Waste Cooking Oil to Biodiesel 17

with alcohol produces ester along with water which hinders the transesterification of
the glycerides. Thus water formation is the primary mechanism limiting the
completion of the acid catalysed esterification reaction with FFAs.
Process I.
Waste cooking oil may contain particulate matter and other impurities. Such
impurities are removed by filtering the waste cooking oil. Feed stock oils are usually
preheated to 60°C by heat exchangers. Alcohol and acid catalysts are properly mixed
in mixer before they were allowed into the esterification reactor. The mixing
temperature is usually maintained at 60°C. Catalyst mixture and preheated feedstock
are allowed into the esterification reactor. Esterification reaction was carried out
between 80 and 90°C and at 1 atmospheric pressure[39,40]. Products from
esterification reactor were cooled to 45°C, and catalysts are removed or neutralized
before moving into the settling tank to remove the methanol and water
mixture[21,22]. From the top of the settling tank, methanol and water mixture is
removed and taken to distillation column to separate methanol from methanol water
mixture and methanol is reused. The bottom product of separating vessel is taken to
process II for transesterification reaction .
Process II
Catalyst and alcohol are mixed in the mixer and products formed from process are
taken into the transesterification reaction column along with catalyst and alcohol
mixture. Reactor temperature is usually maintained at 65°C, 1 atmospheric pressure,
and 1 : 6 molar ratio of oil to alcohol. Products of transesterification reactor are
moved into separator 2. From the separation tank, biodiesel and alcohol mixture is
distilled to separate methanol and biodiesel. Methanol from distillation column is
recycled and reused. Biodiesel obtained is then washed with hot water and moved to
separator to separate water and biodiesel. From the third separator tank, biodiesel is
moved to storage tank. Bottoms of second separator section are moved to the alcohol
and glycerol distillation column [41,42]. From the top of distillation column methanol
is recycled. Bottom product of distillation column is a by-product.
Purification of Biodiesel: Once the reaction is complete, the mixture of product is
shifted to a separating funnel in which the mixture is allowed to settle down at room
temperature or by centrifuging. The mixture gets separated into two layers in most of
the cases. When ionic liquid is used as catalyst, the product formed separates into
three layers based on the catalyst used [9,10]. The top layer is always biodiesel and
the lower layer is glycerol. This separation is based on the difference in densities.
Biodiesel is collected and washed with distilled water or ethyl acetate for removing
minor impurities. The washed biodiesel is heated to remove any moisture present. It
may also be treated with anhydrous sodium sulphate to remove water and yield the
biodiesel which is a yellow liquid[43, 44].
18 Rummi Devi Saini

CONCLUSION:
Biodiesel has attracted extensive attention in the world as it is a renewable,
biodegradable, nontoxic and environmentally friendly new alternative transportation
fuel. It can be made from different feedstock containing fatty acids such as animal
fats, nonedible oils, waste cooking oils, by products of the refining vegetables oils and
algae etc. Transesterification process is a commonly employed for its formation.
Heterogeneous catalysts are recommended the best catalysts in biodiesel production.
Cost of biodiesel can be reduced by using waste cooking oil as feed stock. High fatty
acid content in waste cooking oil can be reduced by pre-treating waste cooking oil
with acid catalyst. Water produced during the esterification process may inhibit acid
catalyst. It can be removed by stepwise reaction mechanism. Methanol is the most
suitable alcohol because of its low cost and easy separation from biofuel. But still
there is need to improve the biodiesel process economically using environmentally
friendly catalysts and selecting the best process technology.

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