Post on 21-Feb-2023
A STUDY ON PRODUCTION OF BIO-DIESEL AND GLYCERIN SOAP
2012-2013
CHAPTER 1
INTRODUCTION
1.1 GENERALBiodiesel is becoming prominent among the alternatives to
conventional petro-diesel due to economic, environmental and
social factors. The quality of biodiesel is influenced by the
nature of feedstock and the production processes employed.
High amounts of free fatty acids (FFA) in the feedstock are
known to be detrimental to the quality of biodiesel. Vegetable
oils are among the various sources of energy fuels being
considered as alternatives to fossil fuels. Rapeseed, soybean,
sunflower, coconut and palm oils have been the main raw
materials for biodiesel production. However, these oils are
required in refined forms to obtain quality biodiesel and in
addition they are food stuffs. This makes production of
biodiesel from these sources uneconomical. Non-edible plant
oils such as found in jatropha and castor beans may provide
better alternatives. Plant-derived oils could be used directly
in diesel engines or blended with petro-diesel however, their
high viscosity lead to problems in the engine .
Biodiesel is the name for a variety of Easter-based
fuels generally defined as the mono alkyl esters made from non
edible oils such as Pongamia or Jatropha or Neem or Simaruoba
oil, or sometimes from animal fats through a simple trans-
esterification process. This renewable source is as efficient
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2012-2013
as petroleum diesel in powering unmodified diesel engine. The
concept of using vegetable oil as an engine fuel by Rudolf
Diesel(1858-1913) when he developed the first engine to run on
peanut oil, as he demonstrated at the World Exhibition in
Paris in 1900. Unfortunately, Rudolf Diesel died in 1913,
before his vision of a vegetable oil powered engine was
realized. After R. Diesel’s findings the petroleum industry
rapidly developed and produced a cheap by-product “diesel
fuel” powering a modified “diesel-engine”. Thus, clean
vegetable oil was forgotten as a renewable source of power.
From 1990-91 to 2010-11, India’s oil imports increased
dramatically from 21 to 120 million tonnes. Biodiesel could
stimulate agricultural development and create employment and
income for many of the rural poor. At the same time, thereby
satisfy a significant part of the country’s fuel demand,
increasing India’s energy security and saving foreign
exchange. Shifting to biodiesel could also reduce greenhouse
gas emissions and urban air pollution.
The Government of India approved a National
policy on Bio fuels in September 2008, setting an indicative
target to raise blending of biodiesel with diesel to 20% by
2017 and scrapping taxes and duties on biodiesel.
A by-product from making bio-diesel is glycerine. In a
process called transesterification, waste vegetable oil (WVO)
is broken down into esters (bio-diesel) and glycerine. This
glycerine can be filtered to remove any food particles or
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2012-2013
impurities, and used as an industrial degreaser in its raw
form, composted and used as a fertilizer, or made into bar
soap. Bar soap made from our glycerine by-product is excellent
for use in the shop because of its degreasing abilities, but
can also be used as a household soap for everyday use. Adding
fragrances and dyes will make household use. Ingredients used
in making bar soap from glycerine are, glycerine, water and
lye. The amounts of water and lye used will affect the
lathering abilities of the soap, and found that the more water
used, the more lather the soap will produce. And using more
lye will produce a soap which is very strong and cuts grease
well, but also dries out the skin.
Glycerol (also known as glycerine) is a major by-
product in the biodiesel manufacturing process. As the
biodiesel industry is rapidly expanding, a glut of crude
glycerol is being created. Because this glycerol is expensive
to purify for use in the food, pharmaceutical, or cosmetics
industries, biodiesel producers must seek alternative methods
for its disposal. The objective of this project is to provide
a general background in terms of waste glycerol utilization.
1.2 Importance of the study
The scarcity of fossil fuels, growing emissions of
combustion-generated pollutants, and their increasing costs,
have made alternative fuel sources more attractive. Biodiesel
(fatty acid methyl esters) produced by the process of trans
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2012-2013
esterification of vegetable oils or animal fats with methanol
are potential substitutes for petroleum-based diesel fuels.
Compared to conventional diesel, biodiesel has the advantages
of being biodegradable, renewable, non-toxic, and has low
pollutant emissions (especially SOx) . In process of biodiesel
production, a heavier separate liquid phase is formed, termed
the glycerol phase. The glycerol portion represents
approximately 16 to 18% of the weight of the input of the oil
and fat, and its composition is not stabilized.
Today`s world is extremely dependent on hydrocarbons for
its energy requirements. Unfortunately, these resources are
exhaustible and are being used up at a rapid rate. Thus, there
is a need for alternative energy sources. Biodiesel provide an
efficient and inexpensive alternative. Biodiesel is a very
good proposition to replace non-renewable energy sources like
petroleum. There are many benefits of using biodiesel, Firstly
it is a clean fuel. By “clean” we mean it is friendly to the
environment. The second major benefit of biodiesel is that it
is highly biodegradable. Because of its very low
degradability, crude oil is often a big problem in cases like
oil spills.
Biodiesel eliminates this problem. Biodiesel is also
immensely helpful in reducing pollution as it significantly
reduces CO2 emissions compared to the conventional diesel. The
world is getting modernized and industrialized day by day. As
a result vehicles and engines are increasing. But energy
sources used in these engines are limited and decreasing
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2012-2013
gradually. This situation leads to seek an alternative fuel
for diesel engine. Biodiesel is an alternative fuel for diesel
engine. The esters of vegetables oil, animal fats are known as
Biodiesel. Compared to diesel fuel, biodiesel emissions are
substantially better for the environment and, in turn, better
for the health of the environment's inhabitants. Specifically,
the emissions of particulate matter, carbon monoxide and total
unburned hydrocarbons from biodiesel are each much less than
those from petroleum diesel.
Commonly sulphur is added to diesel fuel to increase its
lubrication. Once burned, sulphur dioxide is emitted and acid
rain results. Biodiesel, however, is naturally lubricious and
good for engine parts. Biodiesel contains only trace amounts
of sulphur so its exhaust has considerably less sulphur
dioxide. Biodiesel is miscible in petroleum diesel. This means
that the two can be mixed in any proportion and poured into
the fuel tank. Common language for a biodiesel/diesel mix is
"B" followed by the percent of biodiesel; so 20% biodiesel and
80% diesel is called B20. Pure biodiesel is called B100. That
biodiesel is miscible in petroleum diesel is advantageous when
a user has only limited biodiesel supply, is concerned about
the slightly higher cost of biodiesel or needs a greater
amount of petroleum diesel for cold-weather operability. In
very cold conditions, biodiesel begins to crystallize becomes
thicker and may be unusable on the engine. Some take this as
grounds to criticize biodiesel, but there are simple and
effective ways to use biodiesel throughout the winter.
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2012-2013
One may use additives in the fuel, install any of a
number of heating systems or use the biodiesel in a blend with
petroleum diesel (which crystallizes at a lower
temperature).There are many operating benefits for the user.
As mentioned already, biodiesel provides significantly higher
lubrication for the engine. Biodiesel has been shown to reduce
the need for engine maintenance. When any kind of maintenance
is required for the engine, the mechanic needs no specific
training because biodiesel does not require any sort of engine
modification. The mechanic need not even know that the engine
runs on grease. Additionally, the flash point of biodiesel is
more than 300oF and is safer to handle and store than any
petroleum based fuels.
Bio-fuels are derived from renewable bio-mass resources
and, therefore, provide a strategic advantage to promote
sustainable development and to supplement conventional energy
sources in meeting the rapidly increasing requirements for
transportation fuels associated with high economic growth, as
well as in meeting the energy needs of India’s vast rural
population. Bio fuels can increasingly satisfy these energy
needs in an environmentally benign and cost effective manner
while reducing dependence on import of fossil fuels and
thereby providing a higher degree of National Energy Security.
The growth of bio-fuels around the globe is spurred largely by
energy security and environmental concerns and a wide range
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2012-2013
of market mechanisms, incentives and subsidies have been put
in place to facilitate their growth. Developing countries,
apart from these considerations, also view bio-fuels as a
potential means to stimulate rural development and create
employment opportunities. The Indian approach to bio-fuels,
in particular, is somewhat different to the current
international approaches which could lead to conflict with
food security. It is based solely on non-food feed stocks to
be raised on degraded or wastelands that are not suited to
agriculture, thus avoiding a possible conflict of fuel vs.
food security.
Glycerol is generated as a by-product, not only when
biodiesel fuels are produced chemically, but also when they
are manufactured enzymatically and during the production of
bio-ethanol. The dramatic growth of the biodiesel industry has
created a surplus of glycerol that has resulted in a dramatic
10-fold decrease in crude glycerol prices in recent years and
has generated environmental concerns associated with
contaminated glycerol disposal. Anaerobic digestion is an
attractive waste treatment practice in which both pollution
control and energy recovery can be achieved.
1.3 Scope of the present study
Biodiesel production produces three major biodiesel
waste products: glycerine, methanol, and (sometimes) water.
Untreated biodiesel waste product is toxic - mostly because it
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2012-2013
contains methanol. In a lot of smaller plants biodiesel waste
product is not disposed of properly. This is unfortunate as
biodiesel producers are typically very environmentally aware.
The glycerine that comes out of the biodiesel process is laden
with methanol and caustic chemicals. Glycerine is probably the
worst biodiesel waste product. The real problem with glycerine
is that it is hard to process without investing a lot of money
in expensive equipment. For every 100 litres of biodiesel that
we make we will end up with 20-25 litres of glycerine. This
20-25 litres of glycerine can have up to 25% methanol in it
and should be considered hazardous waste. 50ml of methanol is
a lethal dose so there is a lot of methanol in glycerine.
Glycerine soap is gentler on skin than most soaps, making it a
good choice for people who have particularly dry or sensitive
skin. According to Vermont Soap Organics, glycerine soap also
has a lower pH than other soaps, which helps the skin retain
its natural moisture. Since glycerine is hygroscopic, it may
also help moisturize the skin by attracting water from the
air. Hence glycerine should be used as a by-product for
manufacture of soap. The present scope of the study is to
manufacture of soap using glycerine which is hazardous in
nature.
India is one of the fastest growing economies in the
world. The Development Objectives focus on economic growth,
equity and human wellbeing. Energy is a critical input for
socio-economic development. The energy strategy of a country
aims at efficiency and security and to provide access which
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2012-2013
being environment friendly and achievement of an optimum mix
of primary resources for energy generation. Fossil fuels will
continue to play a dominant role in the energy scenario in our
country in the next few decades. However, conventional or
fossil fuel resources are limited, non-renewable, polluting
and, therefore, need to be used prudently. On the other hand,
renewable energy resources are indigenous, non-polluting and
virtually inexhaustible. India is endowed with abundant
renewable energy resources. Therefore, their use should be
encouraged in every possible way. The crude oil price has
been fluctuating in the world market and has increased
significantly in the recent past, reaching a level of more
than $ 140 per barrel. Such unforeseen escalation of crude oil
prices is severely straining various economies in all over the
world, particularly those of the developing countries.
Petro-based oil meets about 95% of the requirement for
transportation fuels, and the demand has been steadily
rising. Provisional estimates have indicated crude oil
consumption in 2007-08 at about 156 million tonnes. The
domestic crude oil is able to meet only about 23% of the
demand, while the rest is met from imported crude. India’s
energy security would remain vulnerable until alternative
fuels to substitute and supplement petro-based fuels are
developed based on indigenously produced renewable feed
stocks. In bio fuels, the country has a ray of hope in
providing energy security. Bio fuels are environment
friendly fuels and their utilization would address
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2012-2013
global concerns about containment of carbon emissions. The
transportation sector has been identified as a major
polluting sector.
CHAPTER-2
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LITERATURE REVIEW
2.1 GeneralIn this chapter, the available literature in the area of
present investigation has been reviewed and an attempt has
been made to bring out gaps in the knowledge relevant to
present host, different studies on manufacturing process of
bio-diesel and production of glycerine soap have been
reviewed. In addition various report techniques to analyse the
bio-diesel and glycerine soap are also been made.
Kazi mostafijur rahman et.al.(4) has carried out investigation
on “Bio-diesel from jatropha oil as an alternative fuel for
diesel engines.” The world is getting modernized and
industrialized day by day. As a result vehicles and engines
are increasing. But energy sources used in these engines are
limited and decreasing gradually. This situation leads to seek
an alternative fuel for diesel engine. Biodiesel is anBabaganagutti, et.al.(2) has carried out investigation on
“Biodiesel kinematics viscosity analysis.” Biodiesel is a
renewable and promising fuel alternatively ear marked for use
in Compression Ignition (CI) engines. For it to be applicable
in CI engines, there are a number of quality tests required
for its certification. Kinematics viscosity is one of the most
significant test properties. The viscosity difference
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2012-2013
experienced between the oil and the biodiesel produced forms
the basis of an analytical method use to determining the
conversion of vegetable oil to methyl ester. This paper
presents the definitions, test procedure specifications, and
experimental results for the kinematics viscosity of
Balaniteaegyptiaca oil to biodiesel. In addition, the
kinematics viscosity results have been used to extrapolate the
Viscosity Index (VI) values of the produced biodiesel
Aldo okullo et.al.(1) has carried out investigation on
“Physico-chemical properties of biodiesel from jatropha and
caster oils”. Biodiesel is becoming prominent among the
alternatives to conventional petro-diesel due to economic,
environmental and social factors. The quality of biodiesel is
influenced by the nature of feedstock and the production
processes employed. High amounts of free fatty acids (FFA) in
the feedstock are known to be detrimental to the quality of
biodiesel. In addition, oils with compounds containing
hydroxyl groups possess high viscosity due to hydrogen
bonding. American Standards and Testing Materials, (ASTM DMedachandrashekar et.al.(6) has carried out investigation on
“Synthesis of biodiesel.”The Petroleum product resources are
limited and their consumption is increasing very fast with
globalization and high technology development since last
decade.. Since the prices of these products are on the rise at
any given time, there is a need to search for an alternate
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2012-2013
source, which would fuel our vehicles without any major
vehicle modification. The solution to these problems will be
obtained by utilizing the vegetable oils. Especially, some
vegetable oils like Jatropha, Mahua, Neem are chosen because
some of their properties resembled diesel. The test has been
carried out in compression ignition engine.
Diesel is a fossil fuel made from crude oil or petroleum.
It is found in pools or reservoirs in ground. More than a
million year is required to form a single drop of diesel and
it cannot be produced in laboratory. Therefore the supply of
diesel is limited. Today India is mainly dependent on Arab
countries for their fuel supplies. Even the Rajasthan Oil
reservoirs are expected to yield only about 2 to 2.5 million
tonnes annually. The country will thus have to continue
importing oil over 70% of its need until some alternative
fuels are used which makes India self sustainable.
2.2 Biodiesel
Biodiesel is a biodegradable and non-toxic alternative
fuel produced from new or used vegetable oil that is produced
from renewable resources. It can be used in any Diesel engine
without modification. Pure biodiesel has the highest BTU
content of any alternative fuel. It also has the highest
energy balance of any fuel. For every unit of fossil energy
needed to produce biodiesel, more than 3 units of energy are
gained. As for gasoline and diesel, every one unit put in
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yields only about one half unit. Because biodiesel is made
from plant oil or animal fat, it is renewable. Moreover, the
carbon dioxide taken up by plants during photosynthesis helps
to mitigate the carbon dioxide emitted from using biodiesel so
there is no net carbon introduced to the atmosphere. Compared
to diesel fuel, biodiesel emissions are substantially better
for the environment and, in turn, better for the health of the
environment's inhabitants. Specifically, the emissions of
particulate matter, carbon monoxide and total unburned
hydrocarbons from biodiesel are each much less than those from
petroleum diesel. Commonly sulphur is added to diesel fuel to
increase its lubrication. Once burned, sulphur dioxide is
emitted and acid rain results. Biodiesel, however, is
naturally lubricious and good for engine parts. Biodiesel
contains only trace amounts of sulphur so its exhaust has
considerably less sulphur dioxide.(Murugesan, et.al.)
Biodiesel has been shown to reduce the need for engine
maintenance. When any kind of maintenance is required for the
engine, the mechanic needs no specific training because
biodiesel does not require any sort of engine modification.
The mechanic need not even know that the engine runs on
grease. Additionally, the flash point of biodiesel is more
than 300F and is safer to handle and store than any petroleum
based fuels. Biodiesel can be produced from different
varieties of feed stocks. These feed stocks include most
common edible vegetable oils(jatropha, Pongamia....)as well as
waste oils. Biodiesel has several distinct advantages compared
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with petro diesel in addition to being fully competitive with
petro diesel in most technical aspects;
1. Derivation from a renewable domestic resource, thus
reducing dependence on and preserving petroleum.
2. Biodegradability.
3. Reduction of most exhaust emissions.
4. Higher flash point, leading to safer handling and storage
5. Excellent lubrication.
2.3 Why are vegetable oils and animal fats
Transesterified to biodiesel
The major reason that vegetable oils and animal fats are
Transesterified to biodiesel is that the kinematic viscosity
of the biodiesel is much closer to that of petro diesel. The
high viscosity of untransesterified oils and fats leads to
operational problems in diesel engine such as deposits on
various engine parts. Although there are engines and burners
that can use untransesterificated oils, the vast majority of
engines require the lower-viscosity fuel.
2.4 Biodiesel Crops Biodiesel crops are harvested and pressed in oil presses
to extract the vegetable oil (SVO). The oil is then mixed with
a catalyst and methanol. It goes through a process
called transesterification to produce this bio fuel. Biodiesel
can also be made from waste vegetable oil (WVO), and animal
fats. Each source of oil has unique benefits.
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Soybeans. Soybeans are America's primary source of biodiesel
feedstock (90% in 2006). They can produce 48 gallons of oil
per acre. Soy plants grow well in America. Soybeans were one
of the largest crops in 2000.
Palm , which can produce an astounding 635 gallons of oil per
acre, has the highest oil yield of plants currently grown for
biodiesel feedstock. It is mainly grown in Malaysia and
Indonesia. It does pose some environmental concerns though.
Jatropha seeds can contain up to 40% oil, producing an average
of 202 gallons of oil per acre. Another benefit is that this
plant can thrive in marginal lands. Also, the seeds are
poisonous; therefore using this as a biodiesel crop would not
compete with food supply.
Canola is a genetically modified type of rapeseed. It will
produce an average of 100 gallons of oil per acre. In
2008/2009, it was the third most produced vegetable oil in the
world.
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2.5 Some of the Less Common Feedstock Crops:-
• Mustard seed is a type of rapeseed. It contains 25-40% oil.
The meal left over after processing can be used as an organic
pesticide.
• Radish - wild radish can contain up to 48% oil, and is
drought tolerant.
• Sunflower produces an average of 102 gallons of oil per
acre.
• Castor bean averages 151 gallons of oil per acre.
• Coconut produces approximately 287 gallons per acre.
2.6 Ingredients of biodiesel
Biodiesel is an alternative, clean-burning fuel that canbe used in any diesel engine. We can make our own homemade
biodiesel using a few basic ingredients: vegetable oil,
methanol and lye. We should use extreme caution when making
our own biodiesel because there is a potential for chemical
burns and inhalation of toxic fumes. Always use safety
equipment to minimize our risk of these dangers.
A) Vegetable Oil
At the heart of any biodiesel recipe is the actual oil,
and vegetable oil is an economical and plentiful choice
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compared to other types of oils. Vegetable oil is about 20
percent glycerine, which is separated from the vegetable oil
in a process called transesterification. When vegetable oil
is mixed with an alcohol, such as methanol, and then combined
with a catalyst, such as lye, the glycerine is separated from
the vegetable oil. With the glycerine taken out of the
mixture, the result is far less viscous, which will help to
increase engine efficiency.
B) Methanol
Methanol, also known as wood alcohol, is a flammable
alcohol. It is produced using a chemical process that combines
natural gas and a catalyst to produce methanol and water
vapour as a by-product. Using methanol that is 25 percent by
volume will produce the highest quality biodiesel with a
complete reaction of approximately 98 percent, according to
the Rensselaer Polytechnic Institute. Methanol is combined
with the catalyst, usually sodium hydroxide or lye, which is
then added to the vegetable oil. When combining methanol and
lye, be cautious because the fumes released are toxic. Mix
these chemicals in a well-ventilated area, such as outdoors,
to protect our self from the fumes.
C) Sodium Hydroxide
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Sodium hydroxide is also known as lye, and it can be
purchased at most plumbing or home improvement stores. Sodium
hydroxide is used as the catalyst in the biodiesel making
process. Lye is a corrosive substance that can cause skin
burns, so it’s important to wear rubber gloves when handling
it. Steve Howell, the technical director for the National
Biodiesel Board, says that sodium hydroxide is the catalyst of
choice when it comes to making homemade biodiesel because it
is effective and cheap. The disadvantage of using lye is that
when mixed with methanol, it can become extremely explosive if
exposed to a spark of flame.
2.7 Quality standards:
Development of test methods, procedures and
protocols would be taken up on priority along with
introduction of standards and certification for different bio
fuels and end use applications. The Bureau of Indian
Standards (BIS) has already evolved a standard (IS-15607) for
Bio-diesel (B 100), which is the Indian adaptation of the
American Standard ASTM D-6751 and European Standard EN-14214.
BIS has also published IS: 2796: 2008 which covers
specification for motor gasoline blended with 5% ethanol and
motor gasoline blended with 10% ethanol.
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2.8Benefits Substitute or extender for petroleum diesel.
No need of any special pumps or high pressure equipment
for fuelling.
No need to buy special vehicles or engines to run on
bio-diesel.
100 percent bio diesel reduces carbon dioxide emissions
by more than 75 percent compared to petroleum diesel.
Using a blend of 20 percent bio-diesel reduces carbon
dioxide emissions by 15 percent.
Biodiesel is an oxygenated fuel, so it contributes to a
more complete fuel burn and a greatly improved emissions
profile. Biodiesel produces fewer particulate, carbon
monoxide, greenhouse gases and sulphur dioxide emissions,
reducing public health risks.
It will reduce the country's dependence on imported oil.
Its flash point is > 150°C, compared to 77°C for
petroleum diesel. Hence, it is safe to handle, store, and
transport.
Has superior lubrication capabilities and increases
engine life.
2.9Waste produces from bio-diesel and its effect onenvironment
Biodiesel production produces three major biodiesel waste
products: glycerin, methanol, and (sometimes) water...
Untreated biodiesel waste product is toxic - mostly because it
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contains methanol. In a lot of smaller plants biodiesel
waste product is not disposed of properly. This is unfortunate
as biodiesel producers are typically very environmentally
aware. The glycerin that comes out of the biodiesel process
is laden with methanol and caustic chemicals. Glycerin is
probably the worst biodiesel waste product. The real problem
with glycerin is that it is hard to process without investing
a lot of money in expensive equipment. For every 100 litres of
biodiesel that we make we will end up with 20-25 litres of
glycerin. This 20-25 litters of glycerin can have up to 25%
methanol in it and should be considered hazardous waste. 50ml
of methanol is a lethal dose so there is a lot of methanol in
glycerin. It should be treated in the same way as pure
methanol,
In small scale production three things typically happen to theglycerin.
1. It is thrown down the drain
2. It is stored somewhere in containers in the hope that
someday a use will be found for it.
3. It is spread on the ground or thrown into a landfill.
we have seen producers with small plants who have thousands of
litres of glycerin stashed away, this is a bad idea!
2.9.1 Wash Water
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The wash water that is used to clean biodiesel will also be
contaminated with methanol. As a biodiesel waste product this
must be disposed of properly. The water from the first wash
will have a lot of methanol in it. This methanol means that
the water is toxic. It will also contain a lot of soaps and
caustic chemicals. We should check with our local water
treatment plant as to whether this is acceptable to them or
not. Some water treatment plants do not mind some methanol as
the bacteria in the plant thrive on it. However it is always a
matter of degree and we must consult them before doing
anything.
The wash water should never be disposed off into ground
water. Doing so can result in methanol contaminating the water
table which could be a major pollution problem.
2.10 BY-PRODUCT UTILIZATION
Glycerin and Seed cake utilisation
Glycerin is a by-product of making biodiesel.
After the glycerin is filtered to remove any food
particles or impurities, we can make it
into lye bar soap.
Seed cake utilisation
Considering the future scenario of non edible
oil seeds utilization for biodiesel production in the
country from Atrophy and panama pinnata, there is need
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for efficient utilization of their cakes. The direct
utilization of cake is also not recommended for use as
organic manure. The present and forthcoming use of non-
edible oil seeds in India for production of biodiesel is
due to massive plantation of Jatropha and pongamia
pinnata on waste lands.
The utilization of generated cakes in an environment
friendly manner cannot be ignored, because its disposal
as waste would create environmental problems. The
presence of non-edible oil seed cakes in the open
atmosphere would generate following gases due to self
decomposition of biomass over the action of various
microorganism.
Gases from waste sources:CH4, N2O, H2S, NH3, CO2.
The best strategy is to manage and utilize non-
edible cakes as ‘biomass’ resources rather than disposing
them as ‘waste’ so that energy and economic benefits, as
well as environmental benefits, can be realized.
Anaerobic digestion of these cakes could significantly
reduce the gaseous emissions from waste disposal.
Therefore, anaerobic digestion of these cakes would be a
better way of cake utilization for energy generation and
further, effluent as enriched organic manure for organic
farming.
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Mechanical/solvent extraction of oil
oil
Non edible seeds
Anaerobic digestion
Transesterification
Deoiled
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FIG-2.1 Schematic diagram of utilization of non-edible
oil seeds for production of renewable liquid (biodiesel)
and gaseous fuels (biogas).
Source: Karnataka state Biodiesel Development board and
KSCST Bangalore,
2.11 GLYCERINE
Glycerine is a neutral, sweet-tasting,Department of Environmental Engineering PESCE, Mandya Page 25
Glycerine
Biodiesel
Methane enrichment and bottling into cylinder(Bio-methane equivalent to CNG)
Application (substitute of CNG)
CNG vehicles for automotive and transport purposes.
Biogas(60-70%CH4
Direct application (cooking,heatin
EnrichedOrganic manure
Slurry
Diesel engine operation (Blending
Industrial applications(soap manufacturin
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2.14 Properties of glycerine
1) Molecular weight = 92.09
2) Specific Gravity (in air) 1.2636 (20°C); 1.2620
(25°C)
3) Melting point =18.17ºC
4) Boiling point(760mm Hg) = 290ºC
5) Density (20ºC) =1.261 g/cm3
6) Vapour pressure = 0.0025 mm Hg at 50ºC
= O.195 mm Hg at 100ºC
= 4.3 mm Hg at 150ºC
= 46 mm Hg at 200ºC
7) Refractive index = 1.474
8) Surface tension = 63.4 dyne/cm at 20ºC(100%
glycerol)
9) Compressibility (28.5ºC) = 2.1×10 MPa
10) Viscosity = 1499 c.p. at 20ºC (100% glycerol)
11) Specific heat = 0.5779 cal/gm at
26ºC(99.94%glycerol)
12) Heat of vaporization = 21060 cal/mole at 55ºC
= 18170 cal/mole at 195ºC
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13) Heat of formation = 159.6 Kcal/gm mole
14) Heat of combustion = 1662 KJ/mole
15) Heat of fusion = 18.3 KJ/mole
16) Thermal conductivity = 0.29 w/ºK
17) Flash point = 177ºC
18) Fire point = 204ºC
Glycerol is completely soluble in water and alcohol. It
is slightly soluble in ether, ethyl acetate, and
dioxane and insoluble in hydrocarbons. Glycerol has
useful solvent properties similar to those of water and
simple aliphatic alcohol's because of its three-
hydroxyl groups. Glycerol is a useful solvent for many
solids, both organic and inorganic which is
particularly important for the preparation of
pharmaceuticals. The solubility of gases in glycerol,
like other liquids is temperature and pressure
dependent.
CHEMICAL PROPERTIES
Glycerol is a reactive molecule that undergoes all the
usual reactions of alcohols. The two terminal primary
hydroxyl groups are more reactive than the internal
secondary hydroxyl group. Under neutral or alkaline
conditions, glycerol can be heated to 250ºC without
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formation of acrolein. Reactions with glycerol are
therefore best carried out under alkaline or neutral
conditions at 180ºC, alkaline glycerol begins to
dehydrate forming ether-linked polyglycerols. At room
temperature glycerol rapidly absorbs water. When dilute
it is attacked by microorganism. On oxidation, glycerol
yields variety of product depending upon the reaction
conditions. By the use of mild oxidizing agent it is
possible to oxidize only one hydroxyl group to yield
Glyceraldehyde. These compounds may be considered very
simple aldose and simplest ketoses respectively and
mixture of two compounds obtained from glycerol as well
as glyceraldehyde has been Called glycerose. Nitric
acid converts glycerol to glyceric acid CH2CHCHOHCOOH
melting at 134-135ºC when pure, but usually obtained as
syrupy. Oily liquid soluble in water and alcohol, but
insoluble in ether.
Some industrially important reaction products of
glycerol include:
1) Mono-,di-,and tri esters of inorganic and organic
acids
2) Mono and diglyceride of fatty acids formed by
transesterification of triglycerides(from fats)
3) Aliphatic and aromatic esters formed by reactions
with alkylating agents respectively
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4) Polyglycerols formed by the intermolecular
alienation of water with alkaline catalyst
5) Cyclic 1,2-or 1,3-acetals or ketals formed by the
reaction with aldehyde or ketons respectively
2.15 Products from glycerine
There are products that can be made out of the glycerine,
most commonly soaps, hand cleaners, floor cleaners etc.
Although it is brown and very unattractive the glycerine makes
a very good soap. It is important that the methanol is removed
before it is converted into another product. Manufacturing
soap out of a biodiesel waste product like glycerine is very
beneficial as it is recycling an already recycled item. The
easiest way to remove the methanol is to distil it out. You do
not need a sophisticated still to remove the methanol, a
relatively simple column still will do just fine.
Once the methanol has been removed the glycerine is a lot
safer to dispose off and this can be done in a number of ways.
It can be composted in a big compost heap. A smaller
compost heap is soon overwhelmed. we should only compost
glycerine made from potassium based catalysts.
It can be neutralized with acid and then disposed of
through regular drains. Check with our water treatment
plant before throwing anything down the drain.
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We can make soaps and cleaning products out of it or use
it as is for a floor cleaner. Feed it into an anaerobic
digester.
Mix it 50% with kerosene, it makes a great engine
cleaner.
Glycerin can be used to produce a hydrogen rich gas for
use in fertilizers, food production and chemical plants.
It can also be taken to a wastewater treatment plant
where it will be added to a methane digester .
2.16 Glycerin Soaps – Benefits and AdvantagesMany of the commercial soaps available today don’t
have glycerine in them. The reason for this is because
glycerine, which is a natural by-product of the soap
production process, has fantastic moisture retention and
softening qualities. These are all the qualities that
manufacturers of lotions and cream are after. Thus,
manufacturers of mass produced commercial soaps extract
the glycerine from the soaps and sell it off to
manufacturers of lotions and creams. There are many
advantages and benefits to using glycerine soap as these
soaps are proven to be more moisturizing. In fact,
glycerine soaps are considered to be some of the most
moisturizing soaps available on the market. Qualities of
these soaps allow the soap to be both moisturizing and
softening and suitable for different type of skins. These
soaps will help our skin to remain moisturized and become
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healthy. There are various other benefits to using
glycerine soap, including the following:
• An all natural soap: One of the main advantages of
using glycerine soap is that if we buy the correct brand, it
can be made from entirely natural ingredients and processes.
These soaps aren’t produced from synthetic ingredients.
However, we will need to keep in mind that
different soap manufacturers make use of different
manufacturing processes. Although most glycerine soaps are
100% natural, certain manufacturers of glycerine soaps might
add some synthetic ingredients to their soaps so it is worth
verifying that the soaps completely natural.
• Sensitive skin: Sensitive skin in particular will
benefit from glycerine soap due to its moisturizing and
softening qualities and natural ingredients. The use of
synthetic ingredients in soap can actually cause severe skin
complications or irritate or exacerbate skin problems. Even
the most sensitive of skin can use glycerine soaps. These
soaps can even be used on skins suffering from problems such
as psoriases and eczema. The skin irritations and negative
reactions produced by regular soap is not a problem for
those who use glycerine soap.
• Skin moisturizing: Glycerin has been proven to act as
humectants, which means that it is able to attract moisture.
Thanks to this inherent quality of glycerine, this soap will
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attract moisture to the skin and also effectively lock it
in. This will provide the skin with a constant source of
hydration, preventing the skin from drying out. This is not
the case with certain other brands of commercial soap with a
low or nonexistent level of glycerine, which dries the skin
out and makes it feel tight and flaky.
• Healthier skin: By using glycerine soap, we will keep
our skin moisturized which will create the great foundation
for a healthy and vibrant, supple skin. This will help us to
even prevent wrinkles, tears in the skin and stretch marks,
among other benefits.
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CHAPTER-3
MATERIALS AND METHODOLOGY
3.1 General
Making biodiesel can be a simple, effective way to
produce liquid transportation fuel that has both financial and
environmental benefits. Another advantage of biodiesel is that
it can be made from waste cooking oil after it has already
been used for cooking foods in the kitchen, cafeteria, or
restaurant. Unfortunately, the chemical process of making
biodiesel, transesterification, results in two products:
biodiesel and glycerine. The biodiesel is the primary product,
but the glycerine is very useful as well. Therefore we refer
to the glycerine produced during the biodiesel reaction as a
“by-product”. By-products retain both financial and
environmental value. Glycerin derived from biodiesel
production is a low quality product because it contains many
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contaminants from the biodiesel reaction. Biodiesel glycerine
is actually a mixture of free fatty acids (FFA) that were
neutralized during transesterification. The only contaminant
that poses a risk is the methanol. The yield of glycerine from
a batch of biodiesel is about 20 percent. When making 100
litres of biodiesel, there will be at least 20 litres of
glycerine as a side product. If you were to turn the whole 20
litres of glycerine into bars of soap you would end up with at
least 100 of them. Seriously though, it does open the
possibility for another source of income, selling hand
cleaners and floor cleaners etc.
3.2 PRODUCTION OF BIODIESEL
3.2.1Materials used
The Materials used for making 100ml of biodiesel are as
follows
100 ml of oil
20 ml of methanol
0.9 grams of KOH.
Erlenmeyer flask
Magnetic stirrer bar
3.2.2 Calculation of Free Fatty Acid (FFA)
Calculation Formula:
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FFA Content= 28.2x(Normality of NaOH) x (Titration value)
(Weight of the oil)
Example: If the weight of oil is 10 grams, the Titration
value is 15 ml (burette reading of ml of NaOH consumed during
titration), and normality of NaOH is 0.1
Then FFA Content = 28.2 X 0.1X 15= 4.23 % FFA
10
3.2.3 Procedure for production of biodiesel
The production of biodiesel is carried out in two methods one
is Single stage method and other is Double stage method,
depending upon the amount of FFA present in the crude oil. If
the percentage of FFA is 5 and above single stage is not
allowed. We should follow the Double stage process.
Single stage process Procedure for making 100 ml of Biodiesel in single stage
process are as follows,
1. Take 100 ml of oil in an Erlenmeyer flask.
2. Place a magnetic stirrer bar into the flask and
start heating upto 55-60oC.
3. In a separate Erlenmeyer flask take 20 ml of
methanol and add 0.9 grams of KOH and stir until
dissolved.
4. Once the methanol and KOH is mixed (called
methoxide), it can be added to the warm oil in three
phases.
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5. In the first phase add 12.0 ml of methoxide and the
oil is stirring.
6. Keep the remaining methoxide covered tightly until
it is needed.
7. Let the oil and methoxide mixture react for 45 to 60
minutes at 55-60oC temperature.
8. After the oil and methoxide mixture reacted, pour
into a seperatoryfunnel and allow the glycerine
waste to settle for about one hour.
9. After settling, drain the glycerine from the bottom
of the funnel and pour the top layer (crude
biodiesel) back into the Erlenmeyer flask.
10. In the second phase add 4 ml of methoxide to
the crude biodiesel and, repeating steps 6-8.
11. In the third phase add the remaining 4 ml of
methoxidean repeat steps 6-8 for a third time.
12. After the third reaction, put the crude
biodiesel into a clean beaker and stir and heat to
about 75oC in order to boil off any remaining
methanol that may present.
Washing of crude biodiesel
The next step is to wash the crude biodiesel that we
produced,
1.Pour the warm methanol-free, crude biodiesel into
a clean separator funnel
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2.Add 75-100 ml of warm tap water to the separator
funnel with the biodiesel and allow to settle for 15
minutes.
3. Let the water settle out of the biodiesel layer
(water is on bottom) and then drain out the water.
4. Repeat the steps 2 and 3 in two times. Check the
pH in between every washing. The desired pH after
washing is completed is 7.
5. Heat the washed biodiesel to 105oC in order to
remove the residual water.
Double stage processProcedure for making one litre of Biodiesel are as follows,
1. Measure the FFA level in the raw oil, take 1
litre of raw oil into
3-Neck flask and put the magnetic pellet and
adjust the RPM to suitable speed.
2. Fix the reflux condenser and keep water
circulation on and maintain temperature at 60oC
3. Add 2.25 grams of methanol and 0.05 grams of
H2SO4 for each percentage of FFA (calculate
properly)
4. Agitate the mixture in the reaction vessel (3-
Neck flask) at 60oC for about 60 to 90 minutes.
5. Transfer the mixture to the separating funnel
and allow settling for at least 2-3 hours.
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6. A dark layer will appear at the top of the oil
is an Acid layer.
7. Drain the bottom layer to 3-Neck flask and
measure the new FFA.
8. If the new FFA is more than 2%, then adjust the
RPM to 200 and set the temperature to 60oC.
Return to step no, 2 and repeat the process
till the FFA level is reduced to less than 2%.
9. In the mean time, take 200ml of methanol per
litre of oil and calculate quantity of NaOH (as
per new FFA) and mix it in a beaker, and add
the same to 3-Neck flask slowly.
10. After the addition of “Methoxide mixture”
into the reaction vessel, agitate the mixture
at a suitable RPM and maintain the temperature
at 63oc for 60 to 90 minutes.
11. Then follow the procedure as per single
stage process.
Note: Methanol should be added first and then H2SO4 should be
added to oil, very slowly and carefully.
3.2.4 Calculation of methanol and H2SO4 in double stage
Density of pongamia oil 0.925
Weight of pongamia 925grams per litre
Methanol standard 2.25/FFA
H2SO4 standard 0.05/FFA
Methanol density 0.794
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Density of H2SO4 1.84
Example:
Qty of raw oil =100 gm
FFA level = 5%
Required Methanol = 2.25 x 5 FFA = 11.25gm/0.794 = 14.168ml
Required H2SO4 = 0.05 x 5 FFA = 0.25gm/1.84 = 0.1356ml
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Plantation ofBio-fuel
Harvesting ofseeds
Drying ofthe seeds
Sorting ofseeds and
Expelling ofoil by
Crude oilSeed cake
Settling of heavy particles in the
Application in pharmaceuticals animalfeed pesticide etc,
Filtering of theMethoxide
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Fig 3.1 Schematic Diagram of Biodiesel Production
Source: Karnataka state Biodiesel Development board and KSCST
Bangalore,
3.3 BIODIESEL TESTING
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Determination ofFFA
Transesterification
GlycerolBiodiesel /methyl
Recovery ofmethan
Soap producti
Washing of Biodiesel
Drying of Biodiesel at
Biodiesel quality analysis DensityFlash pointCopper strip corrosion test
Ready for blending
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Plate 3.1 Flash Point Test By Pensky Marten’s
PROCEDURE:1. Thoroughly clean and dry all parts of the cup and itsaccessories before starting the test.
2. Fill the cup with the sample of biodiesel to be tested tothe level indicated.
3. Place the lid on the cup and set the heating.(Heat at arate of 5-60C per minute with continuous stirring of biodiesel
4. Dip the test flame into oil vapour when temp is within 100Cof the probable temperature.
5. Check after every 10C rise in temperature.
6. When test flame produces distinct flash, note thetemperature.
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PROCEDURE:
1. Pour measured quantity of biodiesel in the copper
strip corrosion test bomb.
2. Immerse the polished copper strip in the oil in the
test bomb apparatus.
3. Keep the copper strip corrosion test bomb apparatus
with biodiesel in a water bath vertically.
4. Heat the water bath for 3 hours.
5. Maintained the temperature at 50oC± 1oC.
6. After 3 hours remove the copper strip from the
apparatus.
7. Compare with ASTM copper strip corrosion standards.
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Plate 3.3 Density Test By Hydrometer Method
PROCEDURE:
1. Take 500ml of the biodiesel in a clean dry measuring
cylinder.
2. Heat it to a temperature of 15oC.
3. Allow the biodiesel to settle.
4. Gently lower the hydrometer into the biodiesel in the
cylinder unit it floats freely. Note, the point at which
the surface of the biodiesel touches the stem of the
hydrometer. Read the hydrometer level.
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5. The hydrometer reading is the density of the
biodiesel.
Plate 3.4 Kinematic Viscosity Test
PROCEDURE:
1. Fill the biodiesel in the cannon-fenske viscometer
tube no,100 (Direct type).
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2. Hold the viscometer tube in the viscometer-water-
bath apparatus.
3. Heat to 40oC and maintain the temperature for a
period of 20-30 minutes.
4. The above procedure is carried out so that oil
attains the prescribed temperature during test.
5. After 30 minutes open the and simultaneously start
the stop watch.
6. Stop the stop watch once flow reaches the bottom of
mark in a bulb.
7. Note the time in seconds on the stopwatch.
Kinematic viscosity= (no, of seconds) x
(standard factor of the bulb of the
viscometer tube using for testing)
3.4 PRODUCTION OF GLYCERIN BAR SOAP
3.4.1 Removing Methanol
The first step in any of these recipes is to remove the
methanol from the glycerine. If we do not do methanol recovery
in our glycerine it will contain a high percentage of
methanol. This will be dangerous to the health of whoever is
using the products as well as being dangerous to you when you
heat the glycerine. All residual methanol must be removed
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before the glycerine can be used for other purposes. Methanol
will boil off at temperatures above 68°C.The glycerine can be
distilled to capture the methanol or simply heated under a
fume hood to remove methanol. Allow 45 minutes of boiling at
temperature to ensure all methanol is driven off. Once the
methanol is removed, the glycerine is safe to handle and is
suitable for making soap.
3.4.2 Materials:-
The Materials used for making Glycerin bar soap are as follows
Glycerine
Strainer
Measuring containers
Lye
Stainless steel pot
Stainless steel spoon
Plastic storage bin
Knife
Zipper plastic bags
Fragrance oils (optional)
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3.4.3 ProcedureProcedure for making glycerine bar soap are as follows,
1.Place the glycerine in a stainless steel pot and heat it to
150oF to remove any traces of methanol.
2.Strain the glycerine to remove any impurities and then
return it to the pot.
3.Take 1/4 litre of water for every litre of glycerine and
heat the water to 100o F. This works out to a 1-to-4 ratio of
water to glycerine.
4.Stir approximately 38.5 grams per litre of lye in to the
heated water until it is completely dissolved.
5.Add the water and lye mixture to the glycerine.
6.Continue to heat for another 10 minutes, stirring
occasionally.
7.Remove the mixture from the heat and stir for another 10
minutes. we may see it start to foam.
8.Pour the mixture into a shallow container. A plastic storage
bin with a lid works well. The size and number of containers
needed depends on the amount of glycerine we are using and the
desired thickness of the soap.
9.Cover the liquid with a piece of plywood or cardboard to
help hold the heat in so the soap cures properly. Let it cool
and solidify for 24 hours.
10.Run a knife around the edge of the soap to loosen it and
then flip the container over to remove the soap.
11.Cut the soap into 45 bars that measure 3-by-2 inches.
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12.Wait at least 4 more days before using the soap. During
this additional drying time, the soap will turn from a dark
brown to a lighter tan colour.
13.Store the soap in zipper plastic bags with wax paper
between the bars so they don’t stick together.
References
[1] Aldo.okullo et,al.”Physico-chemical properties of
biodiesel from jatropha and caster oils" Department of
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chemical and mining engineering university of Dar es Salaam.
Vol.2, no.1, 2012
[2] Babaganagutti,et.al“Biodiesel kinematics viscosity
analysis.” ARPN Journal of engineering and applied science
vol.7 no:4, 2012
[3] Gonzalez-Pajuelo M, (2005) et,al. Metabolic engineering of clostridium acetobutylicum for the industrial production of1,3-propanediol from glycerol. Metabolic Engineering 7: 329-336.
[4] Kazimostafijurahman,et.al. .“Bio-diesel from jatropha oil
as an alternative fuel for diesel engines.” International
journal of IJMME-IJENS vol,10 no:03
[5] Manual by Karnataka state Biodiesel Development board and
Karnataka state council for science and technology, Indian
Institute of science campus, Bangalore
[6]Meda Chandra sekhar et.al.“Synthesis of
biodiesel.”International journal of engineering science and
technology vol,2(8).2010
[7] Murugesan A., Umarani C., et al., “Production and Analysis
of Biodiesel from non-edible oils”. A Review.Renewable and
Sustainable Energy Reviews, vol. 13, pp. 825-834, 2009.
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[8] Mu Y, Teng H, et,al. (2006) Microbial production of 1,3-propanediol by klebsiella pneumoniae using crude glycerol frombiodiesel preparations. Biotechnology Letters 28: 1755-1759.
[9] Pramanik K, “Properties and use of jatropha curcas oil
and diesel fuel blends in compression ignition engine”.
Renewable Energy, vol. 28, pp. 239-248, 2003.
[10] Schievano, A.and D'Imporzano, G.et,al. Substituting
energy crops with organic wastes and agro-industrial residues
for biogas production. Journal of Environmental Management
90:2537-2541. 2009.
[11] Thompson, J.C., and He. B.B. “ Characterization of crude
glycerol from biodiesel production from multiple feedstocks."
Applied Engineering in Agriculture 22:261-265. 2006.
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