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Welcome

MICROWAVE ASSISTED
TRANSESTERFICATION OF
VEGETABLE OIL (BIO-DIESEL)

Dr.K.Ramakrishnan
Professor
Chemical Engineering
Siva Subramaniya College of
Engineering, Chennai - 603 110.
Biodiesel
Bio diesel-Mono alkyl esters of fatty acids derived from
vegetable oils
Produced from the chemical reaction of vegetable oil and
alcohol with an alkali as catalyst.
Biodiesel-non-toxic,Oxygenated, Biodegradable, High
Flash Point, High Cetane Number ,Eco friendly Fuel
Alternative Fuel - order of the day.

Transesterified vegetable oil (Bio-Diesel) - can be used


directly without engine (Diesel) modification.

Production cost - comparable if mass plantation of non-


edible oil sources - Jatropha, Pungam - etc.

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Advantages of Biodiesel

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Esterification and Transesterification
Example:
H2SO4
Ethanol + Acetic Acid D
Ethyl Acetate
H2SO4 +Water
Propanol + Acetic Acid Propyl acetate + water
D

Transesterification :

Example:
Triglyceride + methanol catalyst Glycerol+Methylester
Acid / alkali
Ethyl acetate + methanol catalyst Methyl Acetate+Ethanol
Acid / alkali
Various Vegetable oils for Bio Diesel making

1) Jatropha
2)Pungam
3)Used vegetable oil
4)Ground nut oil
5)Sunflower oil
6)Soya bean oil
7)Mustard oil
8)Coconut oil
9) Other Non edible oils
GAS CHROMATOGRAPHIC
ANALYSIS OF VEGATABLE OIL
(General)

Triglycerides of Composition (%)


Myristic Acid 0.28
Palmitic Acid 20.42
Oliec + Stearic Acid 41.29
Linoliec Acid 35.80
Linolenic Acid 1.18
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COMPOSITION OF TRIGLYCERIDES OF
VARIOUS FATTY ACID IN VEGETABLE OIL

LINOLEIC ACID

PALMITC ACID OLEIC +


STEARIC ACID

LINOLENIC
ACID
MYRISTIC ACID

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Transesterification Process
Transesterification- Conversion of vegetable oil to Biodiesel
Process of reacting a triglyceride molecule with an excess of alcohol in
the presence of strong base catalyst such as KOH, NAOH to produce
fatty esters and glycerine or glycerol as by-product
Due to ester interchange the process is called transesterification.
Chemical Reaction:

CH2OCOR1 CH3COOR1 CH2OH


| Catalyst | |
CH2OCOR2 + 3CH3OH---------- CH3COOR2 +CHOH
| KOH/ | |
CH2OCOR3 NaOH CH3COOR3 CH2OH
Triglyceride Methanol Methyl Ester Glycerine
(BioDiesel)
R1,R2,R3-> Long fatty acid chains

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Transesterification Process
(Contd..)
The most important issue during biodiesel production is the
completeness of the transesterification reaction. The basic
chemical process that occurs during the reaction is indicated by
the following sequence of events

Triglyceride Diglyceride Monoglyceride Glycerol

Methyl Ester Methyl Ester Methyl Ester

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Transesterification Process
(contd..)
Where R1, R2 and R3 are long chains of carbon and hydrogen atom
sometimes called fatty acid chains. There are generally four types of
chains that are common are in Jatropha and Pungamia (Others are
present in small amounts).

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Transesterification (Reaction
Mechanism
Estergroup

O H O H
R C O C H + H O CH R C O CH H O C H
1 3 1 3
O O
Na+
R C O C H + H O CH R C O CH + H O C H
2 3 2 3
O O
R C O C H + H O CH R C O CH H O C H
3 3 3 3
H H
Catalyst
1 Oil or Fat + 3 Methanol 3 Methylester + 1 Glycerin
1 Triglycerid + 3 Alcohol
1 Tri-Ester H H H
H H H H H H H
H H H
H H H H
Example for R: C C C C C C C C C C C
H C C C C C C
H H H H H H H H H
H H H H H H
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Transesterification (Industrial Process)

Reactor 1 Reactor 2

Oil Biodiesel

Wash
Column
Methanol
Methanol
Recovery
Glycerin
Catalyst
Catalyst Water
Closed WASH-
Evaporation
Glycerin WATER loop
Water

Crude Glycerin

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SCHEMATIC DIAGRAM
Side Reactions
In the Biodiesel Process

O O
R C O CH + H O H R C O H + H O CH
1 3 1 3

Methylester Water Fatty Acid Methanol

O O
R C O H + Na O CH R C O Na + H O CH
1 3 1 3

Fatty Acid Sodium Methylate Soap Methanol

Catalyst !!!

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Key Process Variables Influencing
Transesterification Reaction
Free fatty acid content in the raw oil

Operational Temperature

Quantity of Alkali added

Speed of stirring

Washing of Biodiesel

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CHOICE OF METHODS
a) Conventional
b) Non-conventional
i) Microwave Assisted
ii) Ultrasound techniques (Sonicator)
iii) Supercritical Method
iv) Centrifugation
v) And etc.,
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MICROWAVE OVEN
It operates at 12.2 cm wavelength and 2450MHZ to avoid
interference with other systems like Radar & Radio frequencies.
At 2.45 GHZ, the microwaves from the magnetron penetrate
into the depth of 1 to 2 makes the water molecules to vibrate
at the rate of 2 billion times per second and the food is heated
up.
The material is heat up because of vibration and polarization of
particles.

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MICROWAVE OVEN COOKING
ADVANTAGES

I) Domestic Microwave oven The cooking


rate is fast.
II) Amount of fruit juice yield is more.
III) Peeling of garlic pearls skin is easier.
IV) Only content gets heated not the
container.
V) Drying operation - is effective.
VI) Some specific chemical reaction are faster.

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EXPERIMENTAL SETUP

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The following procedure for
transesterification was carried out with
microwave assistance
Known quantity of oil was taken in the reactor which is kept inside the
microwave oven. Suitable temperature was maintained.
A mixture of premixed KOH and methanol was added to the oil and it
war allowed to react for the required time. Suitable speed of stirrer was
maintained.
After the reaction, the mixture was settled in a separating funnel over
night. Glycerin was separated at the bottom. Top layer consists of the
Methyl Ester (Bio-Diesel) with little amount of Methanol.
The Glycerol was removed and excess methanol was recovered from
the Methyl Ester layer. Washing with water was done to remove the
catalyst.
Washed layer was dried and filtered to get pure Methyl Ester.
The yield of Bio Diesel was calculated on weight basis.
Similarly experiments were carried out for other powers i.e. 160W,
320W, 480W, 640W, 800W.

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EXPERIMENTAL RESULTS

SL.NO Microwave Power Yield (% w/w)


(watts)
1 160 93.8
2 320 91.9
3 480 88.1
4 640 80.4
5 800 76.6
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GAS CHROMATOGRAPHIC
ANALYSIS OF VEGETABLE OIL
BIO DIESEL
Table : 3
Methyl Esters of Composition (%)
Myristic Acid 0.28
Palmitic Acid 20.05
Oliec + Stearic Acid 42.7
Linoliec Acid 34.46
Linolenic Acid 1.07
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COMPOSITION OF METHYL ESTERS OF
VARIOUS FATTY ACIDS IN VEGETABLE OIL
BIO DIESEL

OLEIC +
STEARIC ACID
PALMITIC ACID LINOLEIC ACID

LINOLENIC
ACID

MYRISTIC ACID

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CONCLUSION
The Bio Diesel from Sunflower oil was produced using
microwave assistance by operating the microwave at various
powers.
The analysis of the composition of oil and the respective methyl
ester of oil was done using Gas Chromatography.
Also the properties of Oil, Diesel and Bio Diesel for Vegetable
Oil such as Acid Value, Flash and Fire Point etc., were
determined and compared.
The properties of the bio diesel produced met all the required
specifications.
The most important observation was the reaction completed
within ten minutes duration. (The conventional method takes 60
minutes).

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Villagers can set up the plant either in
their house or in the society forms
Example : Hosur Forest area using
Pungam oil

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REFERENCES
http://en.wikipedia.org/wiki/Esterificat
ion
http://en.wikipedia.org/wiki/Transester
ification

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WISHING THE NATION A
GREENER FUTURE

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