Process report on

Production of Biodiesel from Vegetable Oils

In Partial Fulfillment of the requirement for the degree
Of
Bachelor of Science (Chemical Engineering)
Session 2011-2015

Submitted by:
M. Arslan

(E11-15CE37)

Azhar Abbas

(E11-15CE38)

Kazim Hussain

(E11-15CE39)

Sadain Zafar

(E11-15CE40)

Supervised by:
Dr. Rashid Usman

Institute Of Chemical Engineering And Technology,

University Of The Punjab, Lahore.

Dedications
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We dedicate our work and utmost efforts to ALLAH almighty the creator of this universe and
most merciful and bounteous, you have always been by my side guiding me all the way to this
destiny & Holy Prophet (PBUH) the cause of the creation of this universe. Our parents, who
taught us how to be persevere and be patient in the midst of trials. Our most respected Teachers
who built our knowledge foundations, Our Friends who encouraged and strengthened us, and our
siblings who are our supporters and well-wishers.

Acknowledgement

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All praises to Almighty ALLAH who gave us light in the darkness and gave us ability and
strength to complete our research project and all respects are for His Prophet Muhammad
(PBUH, on whom be ALLAHS blessings and salutations)
We take immense pleasure in thanking our worthy teachers for their valuable help
regarding our process report. We all owe special thanks to our supervisor Dr. Rashid Usman,
who helped us throughout our research work. His motivation, guidance and kind words always
encouraged us to work with commitment. Whenever we found ourselves in any sort of trouble,
we always found him available to cater the issue. This sort of generosity and favors are highly
commendable. We also thank our beloved director Dr. Amir Ijaz to provide us a learning
environment.

Contents
Chapter 1....................................................................................................................... 7
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1.1

What is Biodiesel.................................................................................................. 8

1.2

History of Biodiesel............................................................................................... 9

1.3

Biodiesel Blends.................................................................................................. 10

1.3.1 Low-Level Blends............................................................................................... 10

1.3.2 B20.................................................................................................................. 10
1.3.3 B100 and High Level Blends................................................................................. 10
1.4

Advantages of Biodiesel........................................................................................ 11

1.5 Disadvantages of Biodiesel......................................................................................... 12

1.6 Raw Materials for Biodiesel Production.......................................................................12
1.7 Properties of Biodiesel.............................................................................................. 13
Chapter 2.................................................................................................................... 14
2.1 Biofuel Sources........................................................................................................ 15
2.1.1 Algae............................................................................................................... 15
2.1.2 Carbohydrate rich biomaterial............................................................................. 15
2.1.3 Oil rich biomaterial............................................................................................ 16
2.1.4Agriculture wastes (organic and inorganic sources)...................................................16
2.2 Biodiesel as a fuel..................................................................................................... 16
2.3 Fuel properties........................................................................................................ 17
2.4 Different methods of biodiesel production.....................................................................18
2.4.1 Supercritical process........................................................................................... 18
2.4.2 Ultra- and high-shear in-line and batch reactors.......................................................18
2.4.3 Ultrasonic reactor method.................................................................................... 18
2.4.4 Lipase-catalyzed method..................................................................................... 18
2.4.5 Volatile Fatty Acids from Anaerobic Digestion of Waste Streams.................................19
2.5 Biodiesel Production................................................................................................. 19
2.5.1 Production Process............................................................................................. 21
2.6 Environmental Effects of Biodiesel Fuel.......................................................................23
2.7 Energy security....................................................................................................... 25
2.8 Economic benefits.................................................................................................... 25
Chapter 3.................................................................................................................... 26
3.1 Procedure of Manufacturing the Biodiesel....................................................................27
3.1.1 Filtration.......................................................................................................... 27
3.1.2 Water Removing................................................................................................ 27
3.1.3 Calculation for Cottonseed oil, methanol and catalyst................................................28

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3.1.4 Calculation for Mustard oil, methanol and catalyst...................................................29

3.1.3 Calculation for Sunflower oil, methanol and catalyst.................................................29
3.1.4 Preparation of Sodium Methoxide.........................................................................30
3.1.5 Heating and Mixing............................................................................................ 31
3.1.5 Settling............................................................................................................. 32
3.1.6 Separation........................................................................................................ 33
3.1.6 Washing........................................................................................................... 33
3.1.6 Heating............................................................................................................ 34
3.1.7 Glycerin........................................................................................................... 35
Chapter 4.................................................................................................................... 36
4.1 Flash Point............................................................................................................. 37
4.2 Aniline point........................................................................................................... 38
4.3 Cloud Point............................................................................................................ 39
4.4 Pour Point.............................................................................................................. 41
4.5 Calorific Value........................................................................................................ 42
4.5 Specific Gravity....................................................................................................... 44
References.................................................................................................................. 45

List of Figures
Figure 1: Trans-esterification Reaction............................................................................. 20
Figure 2: Flow chart of Biodiesel Production.....................................................................21
Figure 3: Removal of Water from Vegetable oil...................................................................28
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Figure 4: Preparation of Sodium methoxide.......................................................................31

Figure 5: Transesterification Reaction Figure 6: Preparation of Biodiesel............................32
Figure 7: Prepared Biodiesel
Figure 8: Separation of Biodiesel.........................................32
Figure 9: Removal of Glycerin
Figure 10: Separated Biodiesel..........................................33
Figure 11: Washing of Biodiesel....................................................................................... 33
Figure 12: Biodiesel from Sunflower oil Figure 13: Biodiesel from Cottonseed Oil..................34
Figure 14: Different samples of biodiesel...........................................................................34
Figure 15: Flash Point Tester.......................................................................................... 37
Figure 16: Graph of Flash points..................................................................................... 38
Figure 17: Aniline point Apparatus.................................................................................. 39
Figure 18: Graph of Aniline point.................................................................................... 39
Figure 19: Graph of Cloud Points.................................................................................... 40
Figure 20: Graph of Pour points...................................................................................... 42
Figure 21: Bomb Calorimeter......................................................................................... 43
Figure 22: Graph of GCV.............................................................................................. 43
Figure 23 : Graph of specific gravity................................................................................ 44

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Chapter 1

Introduction

1.1 What is Biodiesel

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Biodiesel is a clean burning alternative fuel produced from domestic, renewable resources. The
fuel is a mixture of fatty acid alkyl esters made from vegetable oils, animal fats or recycled
greases. Where available, biodiesel can be used in compression-ignition (diesel) engines in its
pure form with little or no modifications. Biodiesel is a liquid biofuel obtained by chemical
processes from vegetable oils or animal fats and an alcohol that can be used in diesel engines,
alone or blended with diesel oil. ASTM International (originally known as the American Society
for Testing and Materials) defines biodiesel as a mixture of long-chain mono-alkylic esters from
fatty acids obtained from renewable resources, to be used in diesel engines. Blends with diesel
fuel are indicated as Bx, where x is the percentage of biodiesel in the blend. For instance,
B5 indicates a blend with 5% biodiesel and 95% diesel fuel; in consequence, B100 indicates
pure biodiesel.
Biodiesel is not the same as straight vegetable oil or animal fat. A normal diesel engine will
eventually be damaged through the use of straight vegetable oil or straight animal fat fuel.
Vegetable oils or animal fats must be converted into biodiesel by reacting the oil or fat with an
alcohol and a catalyst. This process is referred to as "trans-esterification."

1.2 History of Biodiesel

Developed in the 1890s by inventor Rudolph Diesel, the diesel engine has become the engine of
choice for power, reliability, and high fuel economy, worldwide. Early experimenters on
vegetable oil fuels included the French government and Dr. Diesel himself, who envisioned that
pure vegetable oils could power early diesel engines for agriculture in remote areas of the world,
where petroleum was not available at the time. Modern biodiesel fuel, which is made by
converting vegetable oils into compounds called fatty acid methyl esters, has its roots in research
conducted in the 1930s in Belgium, but todays biodiesel industry was not established in Europe
until the late 1980s.
The diesel engine was developed out of a desire to improve upon inefficient, cumbersome and
sometimes dangerous steam engines of the late 1800s. The diesel engine works on the principal
of compression ignition, in which fuel is injected into the engines cylinder after air has been
compressed to a high pressure and temperature. As the fuel enters the cylinder it self-ignites and
burns rapidly, forcing the piston back down and converting the chemical energy in the fuel into
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mechanical energy. Dr. Rudolph Diesel, for which the engine is named, holds the first patent for
the compression ignition engine, issued in 1893. Diesel became known worldwide for his
innovative engine which could use a variety of fuels.
The Future of Biodiesel Fuel
Due to its clean emissions profile, ease of use, and many other benefits, biodiesel are quickly
becoming one of the fastest growing alternative fuels in the world. With minimal subsidy
biodiesel is cost competitive with petroleum diesel, and millions of users have found and enjoyed
the benefits of the fuel. The future of biodiesel lies in the worlds ability to produce renewable
feedstocks such as vegetable oils and fats to keep the cost of biodiesel competitive with
petroleum, without supplanting land necessary for food production, or destroying natural
ecosystems in the process. Creating biodiesel in a sustainable manner will allow this clean,
renewable, and cost effective fuel to help ease the world through increasing shortages of
petroleum, while providing economic and environmental benefits well into the 21st century.

1.3Biodiesel Blends
Biodiesel can be blended and used in many different concentrations. The most common are:
B100 (pure biodiesel), B20 (20% biodiesel, 80% petroleum diesel), B5 (5% biodiesel, 95%
petroleum diesel) and B2 (2% biodiesel, 98% petroleum diesel).
1.3.1 Low-level Blends
ASTM International is developing specifications for a wide variety of products, including
conventional diesel fuel (ASTM D975). This specification allows for biodiesel concentrations of
up to 5% (B5) to be called diesel fuel, with no separate labeling required at the pump. Low-level
biodiesel blends, such as B5 are ASTM approved for safe operation in any compression-ignition
engine designed to be operated on petroleum diesel. This can include light-duty and heavyduty diesel cars and trucks, tractors, boats, and electrical generators.
1.3.2 B20
B20 (20% biodiesel, 80% petroleum diesel) is the most common biodiesel blend in the United
States. B20 is popular because it represents a good balance of cost, emissions, cold-weather
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performance, materials compatibility, and ability to act as a solvent.B20 and lower-level blends
generally do not require engine modifications. Engines operating on B20 have similar fuel
consumption, horsepower, and torque to engines running on petroleum diesel. Pure biodiesel
(B100) contains about 8% less energy per gallon than petroleum diesel. For B20, this translates
to a 1% to 2% difference, but most B20 users report no noticeable difference in performance or
fuel economy. Biodiesel has some emissions benefits, especially for engines manufactured
before 2010. For engines equipped with selective catalytic reduction (SCR) systems, the air
quality benefits are the same whether running on biodiesel or petroleum diesel. However,
biodiesel still offers better greenhouse gas (GHG) benefits compared to conventional diesel fuel.
The emissions benefit is roughly commensurate with the blend level; that is, B20 would have
20% of the GHG reduction benefit of B100.
1.3.3 B100 and High Level Blends
B100 and other high-level biodiesel blends are less common than B20 and lower blends due to a
lack of regulatory incentives and pricing. B100 can be used in some engines built since 1994
with biodiesel-compatible material for certain parts, such as hoses and gaskets. B100 has a
solvent effect, and it can clean a vehicle's fuel system and release deposits accumulated from
petroleum diesel use. The release of these deposits may initially clog filters and require frequent
filter replacement in the first few tanks of high-level blends.
When using high-level blends, a number of issues should be considered. The higher the
percentage of biodiesel above 20%, the lower the energy content per gallon. High-level biodiesel
blends can also impact engine warranties, gel in cold temperatures, and may present unique
storage issues. B100 use could also increase nitrogen oxides emissions, although it greatly
reduces other toxic emissions. B100 requires special handling and may require equipment
modifications.

1.4 Advantages of Biodiesel

Some of the advantages of using biodiesel as a replacement for diesel fuel are:
1. Renewable fuel, obtained from vegetable oils or animal fats.
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2. Low toxicity, in comparison with diesel fuel.

3. Degrades more rapidly than diesel fuel, minimizing the environmental consequences of
biofuel spills.
4. Lower emissions of contaminants: carbon monoxide, particulate matter, polycyclic
5.
6.
7.
8.

aromatic hydrocarbons, aldehydes.

Lower health risk, due to reduced emissions of carcinogenic substances.
No sulfur dioxide (SO2) emissions.
Higher ash point (100C minimum).
May be blended with diesel fuel at any proportion; both fuels may be mixed during the

fuel supply to vehicles.

9. Excellent properties as a lubricant.
10. It is the only alternative fuel that can be used in a conventional diesel engine, without
modications.
11. Used cooking oils and fat residues from meat processing may be used as raw materials.

1.5 Disadvantages of Biodiesel

There are certain disadvantages of using biodiesel as a replacement for diesel fuel that must be
taken into consideration:
1.
2.
3.
4.

Slightly higher fuel consumption due to the lower caloric value of biodiesel.
Slightly higher nitrous oxide (NOx) emissions than diesel fuel.
Higher freezing point than diesel fuel. This may be inconvenient in cold climates.
It is less stable than diesel fuel, and therefore long-term storage (more than six months) of

biodiesel is not recommended.

5. May degrade plastic and natural rubber gaskets and hoses when used in pure form, in
which case replacement with Teon components is recommended.
6. It dissolves the deposits of sediments and other contaminants from diesel fuel in storage
tanks and fuel lines, which then are ushed away by the biofuel into the engine, where
they can cause problems in the valves and injection systems. In consequence, the
cleaning of tanks prior to lling with biodiesel is recommended.
It must be noted that these disadvantages are signicantly reduced when biodiesel is used in
blends with diesel fuel.

1.6Raw Materials for Biodiesel Production

The raw materials for biodiesel production are vegetable oils, animal fats and short chain
alcohols. The oils most used for worldwide biodiesel production are replaced (mainly in the
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European Union countries), soybean (Argentina and the United States of America), palm (Asian
and Central American countries) and sunower, although other oils are also used, including
peanut, linseed, safower, used vegetable oils, and also animal fats. Methanol is the most
frequently used alcohol, although ethanol can also be used. Since cost is the main concern in
biodiesel production and trading (mainly due to oil prices), the use of non-edible vegetable oils
has been studied for several years with good results.
Besides its lower cost, another undeniable advantage of non-edible oils for biodiesel production
lies in the fact that no foodstuffs are spent to produce fuel. These and other reasons have led to
medium- and large-scale biodiesel production trials in several countries, using non-edible oils
such as castor oil, Tung, cotton, jojoba and jatropha. Animal fats are also an interesting option,
especially in countries with plenty of livestock resources, although it is necessary to carry out
preliminary treatment since they are solid; furthermore, highly acidic grease from cattle, pork,
poultry, and sh can be used. Microalgae appear to be a very important alternative for future
biodiesel production due to their very high oil yield; however, it must be taken into account that
only some species are useful for biofuel production. Although the properties of oils and fats used
as raw materials may differ, the properties of biodiesel must be the same, complying with the
requirements set by international standards.

1.7 Properties of Biodiesel

What makes a fuel different from others are its cetane number and heat of combustion. The
viscosity of a fuel is important because it influences the atomization of the fuel being inserted
into the engine combustion chamber. For complete combustion to happen, a small fuel drop is
required. The biodiesel fuel property of having the viscosity much closer to diesel fuel than
vegetable oil helps create a much lower drop, which burns cleaner.
The other main property of biodiesel fuel that we will discuss is its lubricating properties. It has
much better lubricating and a higher cetane ratings than today's lower sulfur diesel fuels. Adding
Biodiesel also helps in reducing fuel system wear. The fuel injection equipment depends on the
fuel for its lubrication. The biodiesel fuel properties increase the life of the fuel injection
equipment. Giving better lubricity and a more complete combustion increases the engine energy
output, thus partially balancing for the higher energy density of petro diesel. Older diesel
Mercedes is well known for running on biodiesel.
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Observing the physical properties of biodiesel fuel, it is a liquid which can be different in color,
from golden and dark brown, all depending on the production feedstock. It is immiscible with
water, has a high boiling point and low vapor pressure. The flash point of biodiesel is
considerably higher than that of petroleum diesel. Biodiesel fuel has a density of ~ 0.88 g/cm,
which is less than that of water.
Studying the chemical properties of biodiesel fuel, its calorific value is about 37.27 MJ/L, which
is 9% lower than regular petrol diesel. It has practically no sulfur content, and is frequently used
as an additive to Ultra-Low Sulfur Diesel (ULSD) fuel. Biodiesel fuel has an effect on copperbased materials and as well as zinc, tin, lead, and cast iron. However, the stainless steels and
aluminum are not affected by biofuel.

Chapter 2

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Literature Review

2.1 Biofuel Sources

Here are 4 biofuel sources, with some of their applications in developmental stages, some
actually
Implemented:

2.1.1 Algae
Algae come from stagnant ponds in the natural world, and more recently from algae farms,
which produce the plant for the specific purpose of creating biofuel. Advantage of algae focused
on the followings: No CO2 back into the air, self-generating biomass, Algae can produce up to
300 times more oil per acre than conventional crops. Among other uses, algae have been used
experimentally as a new form of green jet fuel designed for commercial travel. At the moment,
the upfront costs of producing biofuel from algae on a mass scale are in process, but are not yet
commercially viable.

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2.1.2 Carbohydrate rich biomaterial

It comes from the fermentation of starches derived from agricultural products like corn, sugar
cane, wheat, beets, and other existing food crops, or from inedible cellulose from the same.
Produced from existing crops, can be used in an existing gasoline engine, making it a logical
transition from petroleum. It used in the Auto industry, heating buildings (flue less fireplaces).
At present, the transportation costs required to transport grains from harvesting to processing,
and then out to vendors results in a very small net gain in the sustainability stakes.

2.1.3 Oil rich biomaterial

It comes from existing food crops like rapeseed (aka Canola), sunflower, corn, and others, after
it has been used for other purposes, i.e. food preparation (waste vegetable oil, or WVO), or
even in the first usage form (straight vegetable oil, or SVO). Not susceptible to microbial
degradation, high availability, re-used material. It is used in the creation of biodiesel fuel for
automobiles, home heating, and experimentally as a pure fuel itself. At present, WVO or SVO is
not recognized as a mainstream fuel for automobiles. Also, WVO and SVO are susceptible to
low temperatures, making them unusable in colder climates.

2.1.4 Agriculture wastes (organic and inorganic sources)

It comes from agricultural waste which is concentrated into charcoal-like biomass by heating it.
Very little processing required, low-tech, naturally, holds CO2 rather than releasing it into the air.
Primarily, bio char has been used as a means to enrich soil by keeping CO2 in it, and not into the
air. As fuel, the off-gasses have been used in home heating. There is controversy surrounding the
amount of acreage it would take to make fuel production based on bio char viable on a
meaningful scale. Furthermore, use of agriculture wastes which rich with inorganic elements
(NPK----) as compost (fertilizer) in agriculture.

2.2 Biodiesel as a fuel

Biodiesel (B100) is defined as a fuel comprised of mono-alkyl esters of long-chain fatty acids
derived from vegetable oils or animal fats. Biodiesel Fuel can be produced from a variety of
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natural crops, including rapeseed, soybean, mustard, flax, sunflower, canola, palm oil, hemp,
jatropha and waste vegetable oils. In addition, it must meet all of the parameters as defined
within the ASTM specification D6751,
Standard Specification for Biodiesel Fuel Blend Stock (B100) for Middle Distillate Fuels.
Biodiesel has been registered with the U.S. EPA as a fuel and a fuel additive under Section
211(b) of the Clean Air Act. Biodiesel is a fuel designed as a blendstock for use in blending with
petroleum diesel fuel. It is not intended for use with gasoline. Biodiesel has been proven to
reduce the emissions of hydrocarbons, carbon monoxide and particulates when used alone or
with blends that include petroleum diesel. Biodiesel has excellent lubricity properties and is
typically low in sulfur content, thus meeting the needs of the EPA and new generation fuels.
This fuel source is said to reduce engine wear and produce less harmful emissions. Biodiesel is
used as an alternative fuel source, but requires engine modifications.
Biodiesel's physical properties are similar to those of petroleum diesel, but it is a cleaner-burning
alternative. Using biodiesel in place of petroleum diesel, especially in older vehicles, can
reduce emissions.

2.3 Fuel properties

The properties of biodiesel can be grouped by multiple criteria. The most important arethose that
influence the processes taking place in the engine (ignition qualities, ease ofstarting, formation
and burning of the fuel-air mixture, exhaust gas formation and quality and the heating value,
etc.), cold weather properties (cloud point, pour point and cold filter plugging point), transport
and depositing (oxidative and hydrolytic stability, flash point, induction period, microbial
contamination, filterability limit temperature, etc.), wear of engine parts (lubricity, cleaning
effect, viscosity, compatibility with materials used to manufacture the fuel system, etc.).
Others properties:Sulfated ash is a measure of ash formed from inorganic metallic compounds.
After the burning of biodiesel, in addition to CO2 and H2O a quantity of ash is formed consisting
of unburned hydrocarbons and inorganic impurities (e.g. metal impurities). Metallic ash is very
abrasive and may cause excessive wear of the cylinder walls and the piston ring.

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Carbon residue indicates the presence of impurities and deposits in the engine combustion
chamber, and is also an indicator of the quantity of glycerides, free fatty acids, soaps and
Trans-esterification reaction catalyst residues.
Copper-strip corrosion is an indicator of the corrosiveness of biodiesel, of the presence of fatty
Acids derived from materials which did not enter into reaction during the production process.
Content of metals (Ca, Na, Mg, K and P) can lead to combustion chamber deposits, filter and
fuel injection pump clogging, and can harm the catalyst.

2.4 Different methods of biodiesel production

2.4.1 Supercritical process
An alternative, catalyst-free method for trans-esterification uses supercritical methanol at high
temperatures and pressures in a continuous process. In the supercritical state, the oil and
methanol are in a single phase, and reaction occurs spontaneously and rapidly. The process can
tolerate water in the feed-stock, free fatty acids are converted to methyl esters instead of soap, so
a wide variety of feed stocks can be used. Also the catalyst removal step is eliminated. High
temperatures and pressures are required, but energy costs of production are similar or less than
catalytic production routes.

2.4.2 Ultra- and high-shear in-line and batch reactors

Ultra- and High Shear in-line or batch reactors allow production of biodiesel continuously, semicontinuously, and in batch-mode. This drastically reduces production time and increases
production volume.
The reaction takes place in the high-energetic shear zone of the Ultra- and High Shear mixer by
reducing the droplet size of the immiscible liquids such as oil or fats and methanol. Therefore,
the smaller the droplet size the larger the surface area the faster the catalyst can react.

2.4.3 Ultrasonic reactor method

In the ultrasonic reactor method, the ultrasonic waves cause the reaction mixture to produce and
collapse bubbles constantly. This cavitation simultaneously provides the mixing and heating
required to carry out the trans-esterification process. Thus using an ultrasonic reactor for
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biodiesel production drastically reduces the reaction time, reaction temperatures, and energy
input. Hence the process of trans-esterification can run inline rather than using the time
consuming batch processing. Industrial scale ultrasonic devices allow for the industrial scale
processing of several thousand barrels per day.

2.4.4 Lipase-catalyzed method

Large amounts of research have focused recently on the use of enzymes as a catalyst for the
trans-esterification. Researchers have found that very good yields could be obtained from crude
and used oils using lipases. The use of lipases makes the reaction less sensitive to high free fattyacid content, which is a problem with the standard biodiesel process. One problem with the
lipase reaction is that methanol cannot be used because it inactivates the lipase catalyst after one
batch. However, if methyl acetate is used instead of methanol, the lipase is not in-activated and
can be used for several batches, making the lipase system much more cost effective.

2.4.5 Volatile Fatty Acids from Anaerobic Digestion of Waste Streams

Lipids have drawn considerable attention as a substrate for biodiesel production owing to its
sustainability, non-toxic and energy efficient properties. However, due to cost reasons, attention
must be focused on the non-edible sources of lipids, in particular oleaginous microorganisms.
Such microbes have the ability to assimilate the carbon sources from a medium and convert the
carbon into lipid storage materials. The lipids accumulated by these oleaginous cells can then be
trans-esterified to form biodiesel.

2.5 Biodiesel Production

Biodiesel can be produced from straight vegetable oil, animal oil/fats, tallow and waste oils.
There are three basic routes to biodiesel production from oils and fats:

Base catalyzed trans-esterification of the oil.

Direct acid catalyzed trans-esterification of the oil.

Conversion of the oil to its fatty acids and then to biodiesel.

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Almost all biodiesel is produced using base catalyzed trans-esterification as it is the most
economical process requiring only low temperatures and pressures and producing a 98%
conversion yield. For this reason only this process will be described in this report.
The Trans-esterification process is the reaction of a triglyceride (fat/oil) with an alcohol to form
esters and glycerol. A triglyceride has a glycerin molecule as its base with three long chain fatty
acids attached. The characteristics of the fat are determined by the nature of the fatty acids
attached to the glycerin. The nature of the fatty acids can in turn affect the characteristics of the
biodiesel. During the esterification process, the triglyceride is reacted with alcohol in the
presence of a catalyst, usually a strong alkaline like sodium hydroxide. The alcohol reacts with
the fatty acids to form the mono-alkyl ester, or biodiesel and crude glycerol. In most production
methanol or ethanol is the alcohol used (methanol produces methyl esters, ethanol produces ethyl
esters) and is base catalyzed by either potassium or sodium hydroxide. Potassium hydroxide has
been found to be more suitable for the ethyl ester biodiesel production, either base can be used
for the methyl ester. A common product of the trans-esterification process is Rape Methyl Ester
(RME) produced from raw rapeseed oil reacted with methanol.
The Figure 1 shows the chemical process for methyl ester biodiesel. The reaction between the
fat or oil and the alcohol is a reversible reaction and so the alcohol must be added in excess to
drive the reaction towards the right and ensure complete conversion.

Figure 1: Trans-esterification Reaction

The products of the reaction are the biodiesel itself and glycerol.
A successful trans-esterification reaction is signified by the separation of the ester and glycerol
layers after the reaction time. The heavier, co-product, glycerol settles out and may be sold as it
is or it may be purified for use in other industries, e.g. the pharmaceutical, cosmetics etc.

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Straight vegetable oil (SVO) can be used directly as a fossil diesel substitute however using this
fuel can lead to some fairly serious engine problems. Due to its relatively high viscosity SVO
leads to poor atomization of the fuel, incomplete combustion, coking of the fuel injectors, ring
carbonization, and accumulation of fuel in the lubricating oil. The best method for solving these
problems is the trans-esterification of the oil.
The engine combustion benefits of the trans-esterification of the oil are:

Lowered viscosity

Complete removal of the glycerides

Lowered boiling point

High flash point

Lowered pour point

2.5.1 Production Process

An example of a simple production flow chart is proved below with a brief explanation of each
step.

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Figure 2: Flow chart of Biodiesel Production

Mixing of alcohol and catalyst

The catalyst is typically sodium hydroxide (caustic soda) or potassium hydroxide (potash). It is
dissolved in the alcohol using a standard agitator or mixer. The alcohol/catalyst mix is then
charged into a closed reaction vessel and the oil or fat is added. The system from here on is
totally closed to the atmosphere to prevent the loss of alcohol. The reaction mix is kept just
above the boiling point of the alcohol (around 160 F) to speed up the reaction and the reaction
takes place. Recommended reaction time varies from 1 to 8 hours, and some systems recommend
the reaction take place at room temperature. Excess alcohol is normally used to ensure total
conversion of the fat or oil to its esters. Care must be taken to monitor the amount of water and
free fatty acids in the incoming oil or fat. If the free fatty acid level or water level is too high it
may cause problems with soap formation and the separation of the glycerin by-product
downstream.

Separation
Once the reaction is complete, two major products exist: glycerin and biodiesel. Each has a
substantial amount of the excess methanol that was used in the reaction. The reacted mixture is
sometimes neutralized at this step if needed. The glycerin phase is much denser than biodiesel
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phase and the two can be gravity separated with glycerin simply drawn off the bottom of the
settling vessel. In some cases, a centrifuge is used to separate the two materials faster.

Alcohol Removal
Once the glycerin and biodiesel phases have been separated, the excess alcohol in each phase is
removed with a flash evaporation process or by distillation. In others systems, the alcohol is
removed and the mixture neutralized before the glycerin and esters have been separated. In either
case, the alcohol is recovered using distillation equipment and is re-used. Care must be taken to
ensure no water accumulates in the recovered alcohol stream.

Glycerin Neutralization
The glycerin by-product contains unused catalyst and soaps that are neutralized with an acid and
sent to storage as crude glycerin. In some cases the salt formed during this phase is recovered for
use as fertilizer. In most cases the salt is left in the glycerin. Water and alcohol are removed to
produce 80-88% pure glycerin that is ready to be sold as crude glycerin. In more sophisticated
operations, the glycerin is distilled to 99% or higher purity and sold into the cosmetic and
pharmaceutical markets.

Methyl Ester Wash

Once separated from the glycerin, the biodiesel is sometimes purified by washing gently with
warm water to remove residual catalyst or soaps, dried, and sent to storage. In some processes
this step is unnecessary. This is normally the end of the production process resulting in a clear
amber-yellow liquid with a viscosity similar to petro-diesel. In some systems the biodiesel is
distilled in an additional step to remove small amounts of color bodies to produce a colorless
biodiesel.

Product Quality
Prior to use as a commercial fuel, the finished biodiesel must be analyzed using sophisticated
analytical equipment to ensure it meets any required specifications. The most important aspects
of biodiesel production to ensure trouble free operation in diesel engines are:

Complete Reaction

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Removal of Glycerin

Removal of Catalyst

Removal of Alcohol

Absence of Free Fatty Acids

2.6 Environmental Effects of Biodiesel Fuel

Although biodiesel fuel is fast emerging as the oil of the future, a number of environmental
effects of biodiesel fuel are also surfacing associated with its use. These biodiesel fuel
environmental effects potentially include decrease in greenhouse gas emissions, deforestation,
pollution and the rate of biodegradation.

Greenhouse gas emissions

Whether using biodiesel is able to lower greenhouse gas emissions as compared to the fossil
fuels may depend on many factors. Carbon dioxide is known to be one of the major greenhouse
gases. The plant feedstock used in the making biofuels absorbs carbon dioxide from the
atmosphere when it grows and once the biomass is converted into biodiesel and burnt as fuel, the
energy released is used to power an engine while the carbon dioxide is released back into the
atmosphere. When considering environmental effects of biodiesel fuel due to the total amount of
greenhouse gas emissions, it is important to consider the whole production process. Several
factors like production methods, type of feedstock play their role. Assuming today's production
methods, with no land use change, biodiesel from rapeseed and sunflower oil produce 45%-65%
lower greenhouse gas emissions than petro-diesel But calculating the carbon intensity of
biodiesel fuels is a complex and inexact process. However, there is continuing research for
improving the efficiency of the production process of the biodiesel fuels.

Deforestation
There can be grave effects of biodiesel fuel on environment if deforestation and monoculture
farming techniques are used to grow biofuel crops. It may damage the ecosystems and
biodiversity and increase the emission of climate change gases rather than helping controlling
them. To meet the demand for cheap oil from the tropical region, the amount of arable land is
being extended in order to increase production at the cost of tropical rainforest. As feedstock oils
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in Europe and North America are much more expansive than Asia, South America and Africa,
imports to these more affluent nations are likely to increase in the future. Tropics forests are
being cleared to make room for oil palm plantations. These can lead to serious biodiesel fuel
environmental effects as deforestation can be threatening many species of unique plants and
animals.

Pollution
Biodiesel fuel is the only alternative fuel to have effectively completed the Health Effects testing
requirements of the Clean Air Act (1990). The particulate emissions as the consequence of
production are lowered by around 50 percent compared with fossil-sourced diesel. Having a
higher cetane rating than petro-diesel, some positive effects of biodiesel fuel on environment can
be seen as it can improve performance and clean up emissions. Biodiesel also consists of fewer
aromatic hydrocarbons.

Biodegradation
Another of the environmental effects of biodiesel fuels can be sees in its biodegradation rates,
which are 5 times faster than petroleum diesel over a period of 28 days. Biodiesel fuel blends can
also accelerate the rate of petroleum diesel degradation through co-metabolism. Toxicity studies
have revealed no mortalities and any toxic effects of biodiesel fuel on environment.

2.7 Energy security

The US uses roughly 20 million barrels of oil a day. More than half of this number is imported
and the number of these barrel imported are slated for a fast rise in the near future. U.S.
somehow continues its dependence on foreign sources of oil, which can be dangerous. Its time it
looked into ways to lower its dangerous dependence on foreign oil and seek energy security in
biodiesel fuel, which is gaining momentum in the U.S. Today, for US, biodiesel is the fastest
growing alternative fuel. Let us study energy security due to biodiesel fuel on this page.
All across the world, the countries are adopting biodiesel fuel for energy security as it protects
the environment, besides boosting the economy. Today, biodiesel is fast turning as the growing
alternative fuel not only in America, but other parts of the world as well. Beyond the

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environmental and health benefits, biodiesel fuel can also help free the countries from the hold of
imported oil, thus giving them more energy security due to biodiesel fuel.
One of the main reasons behind transition to biodiesel fuel is energy security. As the nation's
reliance on foreign oil gets reduced, use of locally available sources is substituted. Thus a
country finds energy security in biodiesel fuel without a decrease in greenhouse gas emissions.
Although the total energy balance is still a debatable issue, but clearly the energy security due to
biodiesel fuel is enhanced.
Today, US have made it amply clear using biodiesel fuel for energy security is the main driving
force and the main reason behind the US biofuels programme. Clearly changing to biodiesel fuel
for energy security is a major reason for promoting biofuel. It has been stressed properly
managed biodiesel fuels have the prospective for strengthening the security of supply through
branching out of energy sources.

2.8 Economic benefits

Multiple economic studies have been performed regarding the economic impact of biodiesel
production. One study, commissioned by the National Biodiesel Board, reported the 2011
production of biodiesel supported 39,027 jobs and more than $2.1 billion in household
income.The growth in biodiesel also helps significantly increase GDP. In 2011, biodiesel created
more than $3 billion in GDP. Judging by the continued growth in the Renewable Fuel Standard
and the extension of the biodiesel tax incentive, the number of jobs can increase to 50,725, $2.7
billion in income, and reaching $5 billion in GDP by 2012 and 2013.

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Chapter 3

Experimental Work

3.1 Procedure of Manufacturing the Biodiesel

There are some steps which are used to manufacture the Biodiesel, which are given below

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3.1.1 Filtration
Filtration process is carried out for removing the particles from vegetable oil. This process is
carried out by using the double layer of cheesecloth. Cheesecloth helps to remove the solid
particles from oil.

3.1.2 Water Removing

Oil will probably contain water content. After filtration the oil is heated at 100 CC because the
boiling point of water is 100 C. Water in the oil can slow down the reaction and also causes the
soap formation. So for avoiding the specification and slow down the reaction the water is
removed from oil by heating.

Figure 3: Removal of Water from Vegetable oil

3.1.3 Calculation for Cottonseed oil, methanol and catalyst

Weight of Cottonseed oil taken, W

= 300 g

Molecular weight of Cottonseed oil, M

= 879 g/gmole

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Moles of Cottonseed oil, m

= W/M = 0.3412 gmoles

From literature oil to methanol ratio

= 1: 5

Moles of Methanol, N

= 5* 0.312
= 1.7064 gmole

Methanol required

= N*32 = 1.7064*32
= 54.60 grams

Total no.of moles

=0.3412 + 1.7064
= 2.0476 gmoles

1% NaOH is taken as Catalyst.

Moles of NaOH required for this reaction = 0.01*2.0476
= 0.0204 gmole
NaOH required for this reaction

= 0.0204 * 40
= 0.8190 gram

3.1.4 Calculation for Mustard oil, methanol and catalyst

Weight of Mustard oil taken, W

= 300 g

Molecular weight of Mustard oil, M

= 308.5489 g/gmole

Moles of Mustard oil, m

= W/M = 0.9722 gmoles

From literature oil to methanol ratio

= 1:5

Moles of Methanol N

= 5* 0.9722
= 4.8610 gmole

Methanol required

= N*32 = 4.8610 *32

= 154.52 grams

Total no.of moles

=0.9722 + 4.8610
= 5.8332 gmoles

1% NaOH is taken as Catalyst.

Moles of NaOH required for this reaction = 0.01*5.8332
= 0.0583 gmole
NaOH required for this reaction

= 0.0583 * 40

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= 2.3332 gram

3.1.3 Calculation for Sunflower oil, methanol and catalyst

Weight of Sunflower oil taken, W

= 400 g

Molecular weight of Sunflower oil, M

= 278.8148 g/mole

Moles of Sunflower oil, m

= W/M = 1.4346gmoles

From literature oil to methanol ratio

= 1:5

Moles of Methanol, N

= 5* 1.4346
= 7.173gmole

Methanol required

= N*32 = 7.173 *32

= 229.53 grams

Total No.of moles

=1. 4346 + 7.173

= 9.1476gmoles

1% NaOH is taken as Catalyst.

Moles of NaOH required for this reaction = 0.01*9.1476
= 0.0914gmole
NaOH required for this reaction

= 0.0583 * 40
= 3.6590 gram

3.1.4 Preparation of Sodium Methoxide

Calculated amount of Sodium hydroxide and Methanol are mixed together by heating and
stirring. It is stirred and heated at temperature less than that of methanol boiling point till
Sodium hydroxide completely dissolved in methanol. Water is removed by heating. The chemical
reaction is given below:

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CH3OH+NaOH CH3ONa + H2O Equation 1

Figure 4: Preparation of Sodium methoxide

3.1.5 Heating and Mixing

After manufacturing the Sodium meth-oxide, it is mixed with required amount of vegetable oil.
Now the mixture of Vegetable oil and Sodium meth-oxide is stirred for 1 to 2 hours by magnetic
stirrer and heated at 60 CC. The temperature should not rise than 77 CC otherwise methanol will
be evaporating so; the temperature should be maintained below the 77 CC. The transesterification
process separates the methyl-ester and glycerin. There should be a vortex just on the surface. A
vortex can be avoided by the optimum speed of magnetic stirrer. The temperature is maintained
at 60 CC throughout the process by using ta thermostat

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Figure 5: Transesterification Reaction

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Figure 6: Preparation of Biodiesel

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3.1.5 Settling

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After a well mixed mixture of Biodiesel and glycerin is put into the separating flask and giving

them till glycerin is settled down.

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Figure 7: Prepared Biodiesel

Figure 8: Separation of Biodiesel

3.1.6 Separation
After completely settling it will show two liquids which is based on density differences. After
completely settling the glycerin from the Biodiesel is separated from separating flask. If glycerin
is filed in titration flask, then it reheated for easily removing from separating flask.

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Figure 9: Removal of Glycerin

Figure 10: Separated Biodiesel

3.1.6 Washing
After separating the glycerin the biodiesel is washed by water. Water is sprinkled above the
surface of biodiesel. Water soluble with methanol so it will dissolve with methanol and finally
two liquids will be appeared by density differences. Avoid shaking the mixture while washing
otherwise the milky mixture will be appeared and its separation will take several weeks.

Figure 11: Washing of Biodiesel

3.1.6 Heating
Washing the Biodiesel till waters color appears. Most probably methanol removes with water,
but due to better result the biodiesel is heated at 100 CC. The heated temperature should not

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greater than the boiling point of Biodiesel from any vegetable oil. At this temperature methanol
and water will be vaporized and finally the Biodiesel is free from all impurities.

Figure 12: Biodiesel from Sunflower oil

Figure 13: Biodiesel from Cottonseed Oil

Figure 14: Different samples of biodiesel

3.1.7 Glycerin
The Glycerin from vegetable oils is brown which turns to a solid below 100 CC. After sometime
it turns into gelled formed.
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ICET, Pu, Lhr

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Chapter 4

Results

4.1 Flash Point

The flash point is the lowest temperature at which oil gives out sufficient vapors to form an
ignitable mixture in air and catches fire momentarily when flame is applied. Measuring a flash
point requires an ignition source. At the flash point, the vapor may cease to burn when the source
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of ignition is removed. The value of the flash point is helpful for the storage purpose of the
biodiesel.

Figure 15: Flash Point Tester

Procedure

Oil cup is cleaned and dried.

Sample oil is then passes into the cup up to the level indicated by the filling mark.
Place the lid over cup in its position and insert a thermometer in the holder.
Apparatus is heated and stirred is rotated at the rate from 1-2 revolution per second.
Apply the test flame at temperature intervals of 5 in such a manner that the flame is

lowered in one half second, left in its lowered position for one second and quickly raised.
The temperature at which a distinct flash is visible in the observation this reading of
temperature is recorded as flash point.

Flash point of mustard bio-diesel = 61o C

Flash point of cotton seed bio-diesel oil = 54o C
Flash point of sunflower bio-diesel oil = 67o C.

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Flash point

Temperature in celsius

80
70
60
50
40
30
20
10
0

Flash point

Figure 16: Graph of Flash points

4.2 Aniline point

The aniline point of oil is defined as the minimum temperature at which oil is completely
miscible with an equal volume of aniline (C6H5NH2). It is the aromatic content of the oil.
Aniline is used in this method because aniline is miscible by most of the aromatics. Higher the
aniline point lowers the aromatics and higher the paraffin content with very high cetane number
making the oil suitable for use in diesel engine.

Aniline point of mustard bio-diesel = 21o C

Aniline point of cotton seed bio-diesel oil = 24o C
Aniline point of sunflower bio-diesel oil = 26o C.
Figure 17: Aniline point Apparatus

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Aniline Point
30
25
20
Temperature in celsius

Aniline Point

15
10
5
0
Sunflower Biodiesel

Figure 18: Graph of Aniline point

4.3 Cloud Point

When oil is cooled then the temperature at which it becomes cloudy or hazy is called the cloud
point of oil. The haziness is due to the separation of crystals of wax or increase of viscosity at
low temperature.
In the petroleum industry, cloud point refers to the temperature below which wax in diesel or bio
wax in biodiesels form a cloudy appearance. The presence of solidified waxes thickens the oil
and clogs fuel filters and injectors in engines. The wax also accumulates on cold surfaces (e.g.
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pipeline or heat exchanger fouling) and forms an emulsion with water. Therefore, cloud point
indicates the tendency of the oil to plug filters or small orifices at cold operating temperature.

Procedure

Oil is poured into the test jar.

It is important that the inside of jacket shall be clean and dry. The next important factor is

the cooling.
First the assembly is inserted into a cooling medium. So that only about one inch of the

jacket projects above the liquid medium.

As the cooling precede the test jar is withdrawn quickly, but without disturbing the oil at

every 2 degree celsius fall and examined for cloud.

If cloud point doesnt appear, it is cooled again and examined.
The first distinct cloudiness or haze in the oil at the bottom of the test jar is regarded as
the cloud point

Cloud point of mustard bio-diesel oil = -12.7o C

Cloud point of sunflower bio-diesel oil = -1.6o C
Cloud point of cotton seed bio-diesel oil =7o C

Cloud points
10
5
Temperature celsius

0
Mustard Biodiesel
-5
-10
-15

Figure 19: Graph of Cloud Points

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Cloud points

4.4 Pour Point

The temperature at which the oil just ceases to flow (or pure) is called the pour point. It
determines the temperature at which oil cannot be used as a lubricant.
In crudeoil a high pour point is generally associated with high paraffin content, typically found in
crude deriving from a larger proportion of plant material.
Cloud and pour points indicate the suitability of bio-diesel in cold conditions.

Procedure

Oil is poured into the test jar.

It is important that the inside of the jacket shall be clean and dry. The next important

factor is the cooling

First the assembly is inserted into a cooling medium.
As the cooling precede the test jar is withdrawn without disturbing the oil at every 3

fall and examined for pour point.

If oil shows any movement under these conditions the test jar is immediately replaced in

the jacket and a test for flow repeated at the next temperature 3 lower.
As soon as the oil ceases to flow the jar is held in a horizontal position for exactly 5
seconds and then note the temperature.

Pour point of mustard bio-diesel oil = -14.7o C

Pour point of sunflower bio-diesel oil = -3.6 o C
Pour point of cotton seed bio-diesel oil = 5o C

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Pour Points
10
5

Temperature in Celsius

0
Mustard Biodiesel
-5

Pour Points

-10
-15
-20

Figure 20: Graph of Pour points

4.5 Calorific Value

The calorific value, or heat of combustion or heating value of a sample of fuel is defined as the
amount of heat evolved when the unit quantity of fuel is completely burnt and the products of
combustion cooled to a standard temperature of 298 degree K. The calorific value is measured by
bomb calorimeter.

Procedure

Take 1-2 gram of sample and place it into the crucible of the calorimeter.
A piece of firing wire, copper is stretched across the inner terminus of the bomb and a

piece of sewing cotton is attached to it with the other end in contact with the sample.
The bomb is charged with oxygen to a pressure of 25 atmospheres through the needle

valve without displacing the original air

The calorimeter vessel is then with almost 2.5 liters of water to submerge the bomb up till

cover completely.
Place the bomb in the calorimeter after complete assurance of its tightness.
The thermometer is adjusted along with the cover of calorimeter, start the stirrer and

allow it to run for 5 minutes before observations to begin.

The temperature of water is noted after every 5 minutes.
As the temperature rate of change is constant, close the electrical circuit and note the
temperature reading.

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Figure 21: Bomb Calorimeter

Gross Calorific value of mustard bio-diesel oil = 44459.03 KJ/kg
Gross Calorific value of sunflower bio-diesel oil = 34022.18 KJ/kg
Gross Calorific value of cotton seed bio-diesel oil = 37153.61 KJ/kg

Gross Calorific Value

50000
45000
40000
35000
30000
GCV in KJ/Kg 25000
20000
15000
10000
5000
0
Sunflower Biodiesel

Gross Calorific Value

Figure 22: Graph of GCV

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4.5 Specific Gravity

Specific gravity is the ratio of the density of a substance to the density (mass of the same unit
volume) of a reference substance. Apparent specific gravity is the ratio of the weight of a volume
of the substance to the weight of an equal volume of the reference substance.

Take the gravity bottle and measure the weight of bottle by measuring balance.
Gravity bottle is filled with vegetable oil up to the mark.
Again measure the weight of gravity bottle.
Now calculate the difference of weight, which gives us the weight of vegetable oil.
For measuring the density of oil we divided measured weight of the oil by volume of oil

carrying a gravity bottle.

Specific gravity is measured by dividing the calculated density of oil by the density of
water.

Specific gravity of Sunflower biodiesel = 0.8469

Specific gravity of Mustard biodiesel = 0.8475
Specific gravity of Cottonseed biodiesel = 0.8444

Specific Gravity

Specific gravity

0.85
0.85
0.85
0.85
0.84
0.84
0.84

Specific Gravity

Figure 23 : Graph of specific gravity

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References
http://www.extension.org/pages/26602/introduction-to-biodiesel#.VdVzqrKqqko
http://www.make-biodiesel.org/Introduction
http://energy.about.com/od/renewables/a/Introduction-To-Biodiesel.htm
https://en.wikipedia.org/wiki/Biodiesel
https://www.dieselnet.com/tech/fuel_biodiesel_std.php
http://www.sciencedirect.com/science/article/pii/S136403211100390X
http://www.berkeleybiodiesel.org/overview-blends-biodiesel.html
http://www.afdc.energy.gov/fuels/biodiesel_blends.html
http://www.sciencedirect.com/science/article/pii/S136403211300141X
http://www.sciencedirect.com/science/article/pii/S0196890406002378
http://www.sunflowernsa.com/oil/biodiesel/
https://www.google.com.pk/url?
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hXJXBQKHTk7AGI&url=http%3A%2F%2Fwww.diva-portal.org%2Fsmash%2Fget
%2Fdiva2%3A443295%2Ffulltext01.pdf&ei=HnXVVbPlJsm5Ubn2gJAG&usg=AFQjCNF
SwocnQHQrv32iZGnNdADDLSHymw&bvm=bv.99804247,d.d24&cad=rja
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sa=t&rct=j&q=&esrc=s&source=web&cd=3&ved=0CDEQFjACahUKEwiC6NaChrfHA
hXDOBQKHcQMAas&url=http%3A%2F%2Fwww.omicsonline.org%2Foptimization-ofbiodiesel-production-from-sunflower-oil-using-response-surface-methodology-21577048.1000141.pdf&ei=gnXVVYKfO8PxUMSZhNgK&usg=AFQjCNEE4PIYYdNSjOhkyVCKThXDga3ng&bvm=bv.99804247,d.d24&cad=rja
http://www.answers-to-your-biodiesel-questions.com/biodiesel-flashpoint.html
https://en.wikipedia.org/wiki/Vegetable_oil_(disambiguation)
http://www.scientificpsychic.com/fitness/fattyacids1.html
http://www.extension.org/pages/26611/biodiesel-cloud-point-and-cold-weatherissues#.VdV3CLKqqko
http://web.cals.uidaho.edu/biodiesel/biodiesel-shortcourse-cold-flow/
http://www.make-biodiesel.org/Quality-Testing/cloud-point-and-gel-point-tests.html
http://thepaleodiet.com/vegetable-oil-fatty-acid-composition/
https://en.wikipedia.org/wiki/Template:Vegetable_oils,_composition

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http://www.fediol.eu/web/chemical+composition/1011306087/list1187970121/f1.ht
ml
http://thepaleodiet.com/vegetable-oil-fatty-acid-composition/
http://www.sciencedirect.com/science/article/pii/S0308814609006402
http://www.sciencedirect.com/science/article/pii/S0003267097005746
http://www.scientificpsychic.com/fitness/fattyacids1.html
http://www.biofuelnet.ca/2013/07/31/a-brief-history-of-biofuels-from-ancient-historyto-today/
http://www.triplepundit.com/2012/10/history-of-biofuels/
http://humantouchofchemistry.com/the-future-of-biofuels.htm
http://www.mybiodiesel.com/biodiesel-history.php

Book: Introduction to Biofuels by David M. Mousdale

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