International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882

Volume 3, Issue 6, September 2014

SYNTHESIS OF BIO-DIESEL AND PURIFICATION OF GLYCERIN BY

ELECTROLYSIS
Prashant S. Patil1*, Ghayas A. Usmani2, Kiran E. Suryavanshi3*
1*, 2

Department of Oil Technology, University Institute of Chemical Technology,

North Maharashtra University, Jalgaon, MS, India
3*
Department of Chemistry, R.C.Patel Institute of Technology, Shirpur MS, India

ABSTRACT
In the present research work, synthesis of Bio-Diesel was carried out by trans-esterification reaction of palm
stearin with methanol by using base catalyst KOH. Glycerin is one of the main by-products of this reaction mixture. The
purification of crude glycerin was done by two methods: adsorption and electrolysis. Glycerin with 80-85% purity has
been successfully obtained by Electrolysis Process. The purified glycerol is characterized by using Fourier Transform
Infra-Red (FTIR) and High Performance Liquid Chromatography (HPLC).
Keywords - biodiesel synthesis, glycerin treatment, waste, purification.

I.

INTRODUCTION

Bio-diesel is liquid fuel made from plant materials and animal fats. It is obtained by the trans-esterification process [13]. Bio-diesel is used as substitute for conventional fuel in vehicle engine or industries. According to the World Biodiesel
Production Annual Growth Rate System, rate of bio-diesel production is increasing continuously. For the year 2011, the
growth rate is 26.28 % and the production has reached to 1.3 billion liters [4]. Glycerin is the by-product obtained by
trans-esterification of vegetables oils and animal fats [5-8]. 1 kg of crude glycerol is synthesized during production of 10
kg of biodiesel [9, 10]. Purification of glycerin is very important for economic and environmental reasons [11]. In this
study purification of crude glycerin is done by electrolysis process. In the electrolysis technique decomposition of
chemical species is done by using electrical power. In this process, prepared bio-diesel is reacted with methanol in
presence of base catalyst (KOH, NaOH etc.) to give alkyl esters of fatty acids and glycerol. The obtained crude glycerol is
not in a pure form and it contains large amount of impurities such as fatty acid soap, methanol, and other degraded
glycerin products [12, 13]. The general scheme of purification of crude glycerin includes removal of methanol, free fatty
acid, soap, color, pH neutralization, adsorption, filtration and electrolysis.

II.

EXPERIMENTAL

STEP -1 SYNTHESIS OF BIO-DIESEL FROM PALM STEARIN

Palm stearin was heated to melt it into liquid state and remove moisture. Palm stearin with an appropriate volume
of methanol were taken (i.e. molar ratio of methanol to palm stearin 7:1) with alkaline catalyst (KOH) (0.7 to 2.0g) in a
dry reaction flask equipped with reflux condenser and magnetic stirrer. Reaction mixture was mixed for one hour at a
temperature of 60 0C. The ester layer was then separated from the glycerol layer in a separating funnel. Crude ester layer
consisted of methyl ester, unreacted palm stearin, methanol, glycerol and catalyst. In the separating funnel, this layer was
washed with hot water. This ester was dried and filtered [14].
STEP-2 PURIFICATION OF GLYCERIN (BY PRODUCT FORM BIO-DIESEL PRODUCTION)
USING ELECTROLYSIS PROCESS
Initially the removal of menthol from glycerin is done by evaporation at 69 - 75 0C. Crude glycerin is passed through
evaporator. The pH of 4.1 to 4.9 is maintained with the addition of 85% phosphoric acid at a temperature of 50550C.Two
layers are formed, Glycerin is appeared as bottom layer and fatty acids, salt as upper layer of separating funnel followed
by decantation of glycerin. The separated glycerins so obtained are neutralized by adjusting pH 6.8-7.2 by using 55%
NaOH Solution. Glycerin was heated to a temperature between 61-660C before adsorption process. The color and
contaminates were adsorbed on the surface of activated charcoal (0.070 g) followed by filtration 60 0C. The remaining free
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International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 3, Issue 6, September 2014

fatty acid and trace of other impurity are now removed by electrolysis process. The electrolysis cell is dipped glycerin
under continuous stirring and DC voltage varying between 3.45 V to 9.20V. The water present in glycerin was removed
by evaporation 100-1150C. The purified glycerin is stored in sealed bottles.

III.

PHYSICAL PROPERTIES OF GLYCEROL

Table I Physical properties of purified glycerol
Sr.
No.
1
2

IV.

Parameter
pH

Electrolysis of
Purified Glycerol
7.05-7.30

Chemical treatment of Purified

Glycerol
7.08-7.80

1.2610

1.1701

Density (g/cm3) at 280C

Color

Clear liquid

Light brown

Viscosity (400C)

243.5

167.4

% Water (wt)

1.23

14.01

% FFA (wt)

1.14

8.06

% Glycerin

85.14-95.20

70.1-75.80

CHARACTERIZATION

In this study, the glycerin produced was characterized by Fourier Transform Infrared Spectroscopy (FTIR) and High
Performance Liquid Chromatography techniques. The functional group of produced glycerin was analyzed by using
Fourier Transform Infrared Spectroscopy (FTIR) and purity of produced glycerin was determined by using High
performance Liquid Chromatography techniques. The conclusion from the analysis is compared with the standard
glycerin.

FOURIER TRANSFORM INFRA-RED (FTIR)

The FTIR analyses the changes in the functional group found in crude glycerol after electrolysis process. The result
was then compared with commercial sample.
Table II Functional group of commercial glycerol
Functional group

Wave number (cm-1)

O-H stretching

3310

C-H stretching

2920 to 2800

H20 bending
C-O stretching

1610
1110 to 1450

C-O-H bending

1406 to 1454

The FTIR spectrum for crude glycerol sample is shown in fig.1. The FTIR spectrum for crude glycerol sample
obtained from palm oil based biodiesel waste representing the removal of free fatty acids. This spectrum also represents

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938

International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 3, Issue 6, September 2014

the total number of mineral salts presented in glycerol. This mineral compound is identified as a specific inorganic
compound such Na, K, Ca and etc. Narrow Peak band present at 3300 to 3000 cm-1 indicate removal of moisture.

Fig.1. FTIR spectrum for crude glycerol sample

HIGH PERFORMANCE LIQUID CHROMATOGRPHY (HPLC)
The actual glycerol content in crude glycerol, chemically treated and electrolysis treated glycerol sample was
analyzed using HPLC. The HPLC for synthesized glycerol is shown in fig.2.

Fig.2. HPLC for Electrolysis glycerol

In the HPLC for commercial grade sample, the glycerol shows retention time (Rt) 4.7667. The synthesized glycerol
shows retention time (Rt) 4.4000- 4.8833.

V.

CONCLUSION

The study shows the treatment and quality analysis of crude glycerol purified by using combined approach of
chemical and physical methods. The crude glycerol obtained as a by-product from palm stearin bio-diesel has high content
of water, soap, salts and free fatty acids. Purification of glycerin by-product from biodiesel using electrolysis process is
capable to remove free fatty acids, moisture, salts and soap impurity. All these materials were successfully removed and
high purity level of glycerol was obtained by using absorption and electrolysis process. The FTIR spectra indicated the
appearance of glycerol functional group matching with a standard glycerol. The HPLC analysis of purified glycerol by
electrolysis shows retention time (Rt) 4.4000- 4.8833 and purity 85.14 to 95.20 %.

ACKNOWLEDGEMENT
Authors are thankful to M/S. Panama Petrochem. Ltd. Ankleshwer for donating Crude Glycerin, a by-product derived
from the production of Palm Sterain Biodiesel.

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International Journal of Scientific Research Engineering & Technology (IJSRET), ISSN 2278 0882
Volume 3, Issue 6, September 2014

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