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* Corresponding author:  K Kundu  TERI University, New Delhi; 2 MERADO, Ludhiana ISSN: 0976-3031 RESEARCH ARTICLE ETHANOLYSIS OF JATROPHA OIL AND PROCESS OPTIMIZATION O P Chaturvedi 1 , Sanjay Mande 1 , Y P Abbi 1, K Kundu* 2  1 TERI University, New Delhi; 2 MERADO, Ludhian a ARTICLE INFO ABSTRACT Ethanol is renewable in nature and it is preferable to prepare biodiesel; a renewable fuel with the use of all renewable ingred ients. However, production of biodiesel with bio-ethano l is relatively little more complex than compared to using chemical methanol. Here an attempt has been made for the transesterification of jatropha oil with anhydro us and aqueous ethanol through optimization of various process parameters such as catalyst concentration, reaction time and temperature. With anhydrous ethanol, the separation of glycerol layer from the biodiesel phase was found somewhat difficult with selected process variables. Entire mixture was looked like homogeneous liquid for the selected settling time of 12 hrs and even till 72 hrs with anhydrous ethanol. No separation could be found with catalyst concentration level upto 1.0%. It was also clearly observed that, with increased catalyst amount the yield of Jatropha ethyl ester (JEE) also increased and the highest yield 82.3% was observed with 3.0% catalyst concentration. . However the corresponding viscosity of  jatropha ethyl ester was observed 7.6 cSt, which is not in accepta ble r ange as per the BIS standards. It is seen that in respect of viscosity and yield of ester, the results are very much symmetrical for the all the process chains and increasing yield of jatropha ethyl ester was observed with increasing purity of ethanol. This extensive experimental process optimization study for the production of jatropha ethyl recommends reaction time of 75 minutes, reaction temperature of 60ºC, molar ration of 6:1, and catalyst concentration of 3.0% with ethanol purity 85%. INTRODUCTION Biodiesel is renewable in nature and can be blended at any level with petroleum diesel to create a biodiesel blend or can also be used in its pure form. Just like petroleum derived diesel (petro-diesel), biodiesel operates in compression ignition (CI) engine; which essentially requires very little or no engine modifications, because quite similar properties. Technical advantages of biodiesel include biodegradability, excellent lubricity and high flash point, which make the fuel safe to handle and transport (Knothe, 2002). Besides biodegradable, it is nontoxic and has low emission  profiles making it environmentally beneficial (Michael et al, 1998). Both edible oils such as Soybean, Rapeseeds, Canola, Sunflower, Cottonseeds, etc. and non-edible oils like Jatropha (  Jatropha curcas ), Karanja (Pongamia pinnata), Jojoba (Simmondsia chinensis), Mahua (  Madh uca latifolia ) etc. have  been tried to supplement diesel fuel in various countries. In US, biodiesel program is based on their surplus edible oils like soybean and in Europe from rapeseed and sunflower oils. However in India emphasis has always been on exploring the  possibility of using non-edible oils for biodiesel production and a program has been undertaken for large-scale cultivation of jatropha on wastelands thoughout the country (Planning Commission Report, 2003). There are a number of ways to make the vegetable oil equivalent to diesel fuel. These methods include; Transesterification, Pyrolysis, Micro Emulsion, blending and thermal depolymerization (Srivastava and Prasad, 2000). The most common method to prepare  biodiesel is transesterif ication of vegetable oil with a mono- hydric alcohol (Figure 1) or esterification of fatt y acids (Figure 2). Transesterification is one of the reactions that are used to prepare esters (Otera, 1993). This is not a new process and by all accounts it was conducted as early as 1853, by the two chemists E. Duffy and J. Partrick. One of the first uses of transestrified vegetable oil was powering heavy-duty vehicles isSouthAfricab eforeWorldWa r II(www.dfwbiodiese l.com/tech nology.html). Transesterificatio n of vegetable oil is the process of reacting triglycerides with methanol in order to obtain fatty acid methyl esters and glycerol and the process is important for  preparation Figure 1 Transesterification of triglycerides Figure 2 Esterification of free fatty acids CH 2 CH CH 2 HO HO HO Triglyceride Alcohol Alkyl esters Glycerol + 3ROH Catalyst + R 1 COOR R 2 COOR R 3 COOR CH 2 CH CH 2 R 1 COO R 2 COO R 3 COO Fat ty ac id Alc oho l Al kyl este rs + ROH R  1 COOR R 1 COOH + H 2 O Catalyst Acid  Available Onlin e at http:/ /www.rece ntscient ific.com  International Journal  of Recent Scientific  Research  International Journ al of Recent Scientifi c Research  Vol. 4, Issue, 6, pp.1005– 1010, July, 2013   Article History: Received 14 th , June, 2013 Received in revised form 26 th , June, 2013 Accepted 16 th , July, 2013 Published online 30 th July, 2013  Key words: Jatropha, Ethyl ester, esterification, transesterificat ion, Biodiesel , biodiesel plant © Copy Right, IJRSR, 2013, Academic Journals. All rights reserved.

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* Corresponding author: K Kundu TERI University, New Delhi; 2MERADO, Ludhiana

ISSN: 0976-3031

RESEARCH ARTICLEETHANOLYSIS OF JATROPHA OIL AND PROCESS OPTIMIZATION

O P Chaturvedi1, Sanjay Mande1, Y P Abbi1, K Kundu*2 

1TERI University, New Delhi; 2MERADO, Ludhiana

ARTICLE INFO ABSTRACT

Ethanol is renewable in nature and it is preferable to prepare biodiesel; a renewable fuel

with the use of all renewable ingredients. However, production of biodiesel with bio-ethanolis relatively little more complex than compared to using chemical methanol. Here an

attempt has been made for the transesterification of jatropha oil with anhydrous and aqueousethanol through optimization of various process parameters such as catalyst concentration,reaction time and temperature. With anhydrous ethanol, the separation of glycerol layer 

from the biodiesel phase was found somewhat difficult with selected process variables.Entire mixture was looked like homogeneous liquid for the selected settling time of 12 hrsand even till 72 hrs with anhydrous ethanol. No separation could be found with catalystconcentration level upto 1.0%. It was also clearly observed that, with increased catalystamount the yield of Jatropha ethyl ester (JEE) also increased and the highest yield 82.3%

was observed with 3.0% catalyst concentration. . However the corresponding viscosity of  jatropha ethyl ester was observed 7.6 cSt, which is not in acceptable range as per the BISstandards. It is seen that in respect of viscosity and yield of ester, the results are very muchsymmetrical for the all the process chains and increasing yield of jatropha ethyl ester wasobserved with increasing purity of ethanol. This extensive experimental process

optimization study for the production of jatropha ethyl recommends reaction time of 75minutes, reaction temperature of 60ºC, molar ration of 6:1, and catalyst concentration of 3.0% with ethanol purity 85%.

INTRODUCTION 

Biodiesel is renewable in nature and can be blended at anylevel with petroleum diesel to create a biodiesel blend or canalso be used in its pure form. Just like petroleum derived diesel

(petro-diesel), biodiesel operates in compression ignition (CI)engine; which essentially requires very little or no enginemodifications, because quite similar properties. Technical

advantages of biodiesel include biodegradability, excellentlubricity and high flash point, which make the fuel safe tohandle and transport (Knothe, 2002).

Besides biodegradable, it is nontoxic and has low emission

 profiles making it environmentally beneficial (Michael et al,1998). Both edible oils such as Soybean, Rapeseeds, Canola,Sunflower, Cottonseeds, etc. and non-edible oils like Jatropha

( Jatropha curcas), Karanja (Pongamia pinnata), Jojoba(Simmondsia chinensis), Mahua ( Madhuca latifolia) etc. have been tried to supplement diesel fuel in various countries. In

US, biodiesel program is based on their surplus edible oils likesoybean and in Europe from rapeseed and sunflower oils.However in India emphasis has always been on exploring the

 possibility of using non-edible oils for biodiesel productionand a program has been undertaken for large-scale cultivation

of jatropha on wastelands thoughout the country (PlanningCommission Report, 2003). There are a number of ways tomake the vegetable oil equivalent to diesel fuel. Thesemethods include; Transesterification, Pyrolysis, Micro

Emulsion, blending and thermal depolymerization (Srivastavaand Prasad, 2000). The most common method to prepare

 biodiesel is transesterification of vegetable oil with a mono-hydric alcohol (Figure 1) or esterification of fatty acids(Figure 2). Transesterification is one of the reactions that are

used to prepare esters (Otera, 1993). This is not a new processand by all accounts it was conducted as early as 1853, by thetwo chemists E. Duffy and J. Partrick. One of the first uses of 

transestrified vegetable oil was powering heavy-duty vehiclesisSouthAfricabeforeWorldWar II(www.dfwbiodiesel.com/tech

nology.html). Transesterification of vegetable oil is the processof reacting triglycerides with methanol in order to obtain fattyacid methyl esters and glycerol and the process is important for  preparation

Figure 1 Transesterification of triglycerides

Figure 2 Esterification of free fatty acids 

CH2

CH

CH2

HO

HO

HO

Triglyceride Alcohol Alkyl esters Glycerol

+ 3ROH

Catalyst

+

R 1COOR 

R 2COOR 

R 3COOR 

CH2

CH

CH2

R 1COO

R 2COO

R 3COO

Fatty acid Alcohol Alkyl esters

+ROH R  

1

COOR R 1

COOH + H2O

Catalyst

Acid 

 Available Online at http://www.recentscientific.com

 International Journal 

 of Recent Scientific Research  International Journal of Recent Scientific Research 

Vol. 4, Issue, 6, pp.1005– 1010, July, 2013 

 Article History:

Received 14th, June, 2013

Received in revised form 26th, June, 2013

Accepted 16th, July, 2013

Published online 30th July, 2013

 Key words:

Jatropha, Ethyl ester, esterification,

transesterification, Biodiesel, biodiesel plant 

© Copy Right, IJRSR, 2013, Academic Journals. All rights reserved.

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 International Journal of Recent Scientific Research, Vol. 4, Issue, 7, pp. 1005 - 1010, July, 2013 

1006

Alkali catalysts are commonly used for transesterification of oils since they require short reaction time even at room

temperature (Encinar  et al., 2002). Other types of catalystsused for transesterification includes bronsted acids (sulfuricacid, sulfonic acid, etc.) (Goff  et al., 2004), heterogeneous

catalysts such as basic zeolites, alkaline metal compounds,enzymes such as lipases (Meher  et al., 2006) and also anionexchange resins (Toda et al., 2004). The high free fatty acid 

(FFA) content oil needs acid catalyzed pretreatment to lower the acid value by esterification of FFA (Figure 2), followed byalkali catalyzed transesterification of the glycerides for 

 preparation of fatty acid alkyl esters (Canakci and Gerpen,1999; Canakci and Gerpen, 2001). The transesterification of vegetable oil is also accomplished in supercritical methanol

without catalyst. Saka and Kusdiana (2001) had studied the preparation of biodiesel in supercritical methanol attemperature > 239.4ºC and pressure > 8.09MPa where the

reaction was completed in 4minutes. In addition, the processhas been used for simultaneous esterification of free fatty acidsand transesterification of triglyceride for biodiesel preparation

from high free fatty acid rapeseed oil (Kusdiana and Saka,

2001; Warabi et al., 2003). Non-catalytic alcoholysis of oilsfor biodiesel preparation has also been reported in the literature

(Dasari et al., 2003; Yamazaki et al., 2004).

Ethanolysis is often discussed as the more environmentallyfriendly alternatives, as it allows the production of an entirelynatural fuel, if the alcohol is derived from fermentation of 

harvested residue, i.e. bio-ethanol. As opposed to this,methanol is mainly produced from fossil sources. A very fewreports are available for transesterification of vegetable oil

with higher grade of alcohol and these reports reveal that thereaction is difficult at selected temperature and more problemson separation of glycerol and biodiesel phase. Most of the

researches on esterification of jatropha oil have been done withmethanol, being cheaper. A very few studies have been donewith ethanol despites its distinct advantages over methanol.

Ethanol is renewable in nature and it is preferable to prepare biodiesel, a renewable fuel with the use of all renewableingredients. Thus, here an attempt has been made to optimize

 process variables for the ethanolysis of jatropha oil.

MATERIALS AND METHODS

The jatropha seeds were purchased from M/s Raj & company, Neemuch (MP), India. The solvent extraction oil methods wereused to assess the oil content of seeds. The oil content of 

 jatropha seed was 32.4%. The ethanol and potassium

hydroxide was purchased from Merck. Vegetable oil containsvarious kind of fatty acid. The comparative estimation of fattyacid present in the oil used in the experiment was done using a Nucon make, 5700 series gas chromatograph.

The apparatus used for optimization of process variablesconsists of water bath, reaction flask with condenser and 

digital rpm (revolution per minute) controlled mechanicalstirrer. The volume of the glass reactor was 1-liter capacity and consisted of three necks, one for stirrer, the others for 

condenser and inlet of the reactants. A digital temperatureindicator was used to measure the reaction temperature. The batch reactor had a valve at the bottom for collection of the

final products. The reaction unit is kept inside a water bath inorder to maintain constant temperature. The schematic diagram

of the reactor is shown in Figure 3 The variables influencing

 biodiesel production have been optimized by carrying out thefactorial design of experiment. The responses have been

measured by yields of ester and the viscosity of vegetable oil.As per the literature review and past experience of the variousresearchers, the experimental process variables can be

classified as follows:

Quantitative variables

  Molar ratio of vegetable oil and alcohol  Reaction temperature

  Reaction time

  Amount of catalyst (% wt of vegetable oil)

  Settling time

  Rate of agitation (Mixing intensity, rpm)

Qualitative variables

  Vegetable oil

  Alcohol

  Purity of AlcoholIn this experimental plan, both quantitative and qualitativevariables have been analyzed for maximum biodiesel yield.

Out of above explained variables (Qualitative and Quantitativevariables) the following parameters were kept constant duringthe experiments:

  Molar ratio of vegetable oil and alcohol (6:1)

  Settling time (12 hrs)

  Rate of agitation (500 rpm)

Figure 3 schematic diagram biodiesel reactors

RESULTS AND DISCUSSIONS

 Physico-chemical properties of jatropha oil 

The physico-chemical characteristics of jatropha oil such asfree fatty acid, acid value, saponification value, iodine value,unsaponifiable matters and water content were determined by

using IS:548 test methods (Table 1). The free fatty content of  jatropha oil was observed to be 0.46, which is quite good fromthe view point of transesterification. However, the water 

content of oil was slightly higher, thus the oils required  preheating before processing.

Stirrer

rpm meters

Condenser

Temperature

indicator

Water bath

Thermocouple

Beaker

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 International Journal of Recent Scientific Research, Vol. 4, Issue, 7, pp. 1005 - 1010, July, 2013 

1007

Generally, it is recommended that vegetable should have FFA

level below 1% and water content as low as possible but notexceeding 0.5% the fatty acid profile of jatropha oil are presented in Table 2.

Optimization of qualitative variables for jatropha ethyl ester (JEE)

For the maximizing the yield of jatropha ethyl eater, theexperiment was started with 100 percent pure i.e. anhydrousethanol and by varying the concentrations of catalyst (KOH) at

different levels. The selected concentration levels were 0.5,1.0, 1.5, 2.0, 2.5 and 3.0 weight percentage of oil. The reactiontime (60 minute), reaction temperature (60ºC), molar ratio

(6:1), mixing intensity (500 rpm) and settling time (12 hrs)were kept constant during the entire process. The catalystconcentration and purity of ethanol were optimized for  jatropha ethyl ester (JEE). No separation was found by using

100% ethanol at different level of catalyst concentration from0.5 to 3.0% (Table 3). Entire mixture looked like ahomogeneous liquid for the selected settling time and evenwith increasing the settling time from 12 hrs to 72 hrs. Thus,

further study was conducted with aqueous ethanol.

By keeping aqueous ethanol (85%) constant and catalystconcentration was varied from 0.5 to 3.0% (at 0.5% slab). The

observed results are summarized in Table 4. There were noseparation found with catalyst concentration level upto 1.0%after that it was clearly observed that, the yield of JEE was

increasing with increased catalyst amount and the highest yield of 76.8% was observed at 3.0% catalyst concentration. Further the experiment was set with different aqueous ethanol. For 

these sets of experiments, the catalyst concentration was keptconstant at a previously optimized level 3.0% and the purity of 

ethanol was varied from 97.5% to 85% (at 2.5% slab) and theobserved results are summarized in Table 5. It was observed that, as the aqueousness of ethanol was reduced, the yield of 

 jatropha ethyl ester was increases and clear separation of layer was observed at some level of catalyst. The highest yield of 

JEE was found with 85% aqueous ethanol with 3.0% catalystconcentration. Thus this experimental optimizationinvestigation concluded that, the ethyl ester production

required some degree of aqueous ethanol.

 Influence of reaction time and temperature on the yield 

 and viscosity of JEEKeeping purity of ethanol constant 85%, reaction time and temperature were varied with different process chain like

JEE9, JEE10, JEE11 and JEE12. The temperature was varied from 60 to 40

ºC (at 5

ºC slab) variation and reaction time was

varied from 75 to 30 minutes (at 15 minute slab). Accordingly,

the yield and viscosity were measured. It was found that theJEE yield varied from 66.1% to 45.9% for JEE9. It was alsoclearly observed that maximum yield of 66.1% was observed 

with 60ºC reaction temperature and 75 minute reaction time.

The correspondence viscosity was observed to be 5.4 cSt. Itwas observed that, for all process chains, at lower temperature

regime of 40ºC and 45

ºC, no ester yield was observed. At 50

ºC

with reaction time of 60, 45 and 30 minutes, the viscosity of JEE was not in the range of standard limits and also the lower 

yield of ester was observed. However, again with 2% catalystconcentration (JEE10), it was found that maximum yield 68.4% was observed with 60ºC and 55ºC reaction temperature

and 60 minutes reaction time and correspondence viscositywas 5.4 and 6.1 cSt. It is clearly seen from the Figure 4 thatapproximately similar yields of ester were observed for the

 process JEE9 and JEE10 at different catalyst concentrations.At catalyst concentration of 2.5% (JEE11), the maximum yield of ester was found 74% at 75 minute reaction time and 55ºC

reaction temperature. It is clearly seen that the yield of JEE

was increased by 10% with catalyst concentration of 2.5%compare to catalyst concentrations of 1.5% and 2.0%.

However, the corresponding viscosity values were not in anacceptable range.

Maximum yield of jatropha ethyl ester was found at 60ºC with

75 minute reaction time irrespective of catalyst concentrationfor JEE12 and corresponding viscosity 7.8 cSt, (Figure 5)which was in the acceptable range. It was thus concluded that,as the catalyst concentration increased the yield of jatrophaethyl ester (JEE) also increases with aqueous ethanol. Also, it

can be concluded that production of jatropha ethyl ester is agood choice as it reduces the input cost of raw materialresulting in reduced production cost of biodiesel apart the fact

that use of bio-ethanol makes it completely renewable fuel. In

order to further maximize the yield of JEE further experimentswere conducted with this by varying other process parameters.

Table 1 Physico-chemical properties of jatropha oil

Property Unit Jatropha oil

Free fatty acid % 0.46

Acid value mg KOH/g 0.94

Saponification value mg KOH/g 179

Unsaponifiable matter w/w percent 3.2

Iodine value g I2/100g  94

Water content ppm 667

Table 3 Effect of catalyst concentration on transesterification of jatropha oil withanhydrous ethanol

Process

Chain

Purity of 

Alcohol

(%)

Catalyst

Concentration

(% wt of oil)

Reaction

Time (min)

Reaction

Temp (deg

C)

Biodiesel Yield

(% wt of oil)

JEE 1 100 0.5 60 60 NS

JEE 2 100 1.0 60 60 NS

JEE 3 100 1.5 60 60 NS

JEE 4 100 2.0 60 60 NS

JEE 5 100 2.5 60 60 NS

JEE 6 100 3.0 60 60 NS

Table 2 Fatty acid composition Jatropha oil

Fatty acid (%w/w) Jatropha oil

Palmitic acid (C16:0) 13.6

Stearic acid (C18:0) 6.2

Oleic acid (C18:1) 47.2

Linoleic acid (C18:2) 31.0

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 International Journal of Recent Scientific Research, Vol. 4, Issue, 7, pp. 1005 - 1010, July, 2013 

1008

Optimization of quantitative variables for jatropha ethyl

ester (JEE)

 Influence of reaction timeand temperature on the yield  and viscosity of JEE

Keeping purity of ethanol constant 85%, reaction time and temperature were varied with different process chain likeJEE9, JEE10, JEE11 and JEE12. The temperature was varied 

from 60 to 40ºC (at 5

ºC slab) variation and reaction time was

varied from 75 to 30 minutes (at 15 minute slab). Accordingly,the yield and viscosity were measured. It was found that theJEE yield varied from 66.1% to 45.9% for JEE9. It was alsoclearly observed that maximum yield of 66.1% was observed 

with 60ºC reaction temperature and 75 minute reaction time.

The correspondence viscosity was observed to be 5.4 cSt. Itwas observed that, for all process chains, at lower temperature

regime of 40ºC and 45

ºC, no ester yield was observed. At 50

ºC

with reaction time of 60, 45 and 30 minutes, the viscosity of JEE was not in the range of standard limits and also the lower yield of ester was observed. However, again with 2% catalyst

concentration (JEE10), it was found that maximum yield 68.4% was observed with 60ºC and 55

ºC reaction temperature

and 60 minutes reaction time and correspondence viscositywas 5.4 and 6.1 cSt.

It is clearly seen from the Figure 4 that approximately similar yields of ester were observed for the process JEE9 and JEE10at different catalyst concentrations. At catalyst concentrationof 2.5% (JEE11), the maximum yield of ester was found 74%at 75 minute reaction time and 55

ºC reaction temperature. It is

clearly seen that the yield of JEE was increased by 10% with

catalyst concentration of 2.5% compare to catalystconcentrations of 1.5% and 2.0%. However, the correspondingviscosity values were not in an acceptable range.

Maximum yield of jatropha ethyl ester was found at 60ºC with

75 minute reaction time irrespective of catalyst concentration

for JEE12 and corresponding viscosity 7.8 cSt, (Figure 5)which was in the acceptable range. It was thus concluded that,as the catalyst concentration increased the yield of jatropha

ethyl ester (JEE) also increases with aqueous ethanol. Also, itcan be concluded that production of jatropha ethyl ester is a

good choice as it reduces the input cost of raw materialresulting in reduced production cost of biodiesel apart the factthat use of bio-ethanol makes it completely renewable fuel. In

order to further maximize the yield of JEE further experimentswere conducted with this by varying other process parameters.

40

45

50

55

60

30

40

50

60

70

80

90

100

30

45

60

75

JEE9

JEE10

JEE11

JEE12

   B   i  o   d   i  e  s  e   l   Y   i  e   l   d   (   %

   )

    R   e  a  c   t   i  o

  n    T   i

  m  e   (   m

   i  n    )

R e a c t i o n  T e m  p e r t u r e  ( d e  g  C  ) 

 Figure 4 Effect of reaction time and temperature on the yield of JEE

 Influence of reaction time and temperature with variation in aqueousness of ethanol on the yield and viscosity of JEE

In order to evaluate the effect of purity of ethanol on the yield 

and viscosity of jatropha ethyl ester (JEE), other important process parameters viz. reaction temperature and reaction time

was varied with process chain JEE16, JEE17 and JEE18.

Five levels of reaction temperatures (60, 55, 50, 45 and 40ºC)and four levels of reaction time (75, 60, 45 and 30 minutes)

was selected as a asymmetric factorial experiments. Theobtained results are summarized in Figure 6 and Figure 7. Itwas observed that, for all process chains, at lower temperature

regime of 45ºC and 40

ºC, no ester formation was found. With

varying temperatures from 60ºC to 50

ºC the JEE yield varied 

from 32.4% to 68.2% for the process chain JEE16 and the

highest yield (68.2%) was observed at 60ºC with 60 minute

reaction time. However, the corresponding viscosity was 6.9cSt. The viscosity ranged from 6.9 cSt to 9.2 cSt for the process chain JEE16 with variation of temperatures from 60

ºC

to 50ºC (with 5ºC slab) and reaction time of 75 minutes to 30

minutes (with 15 minutes slab). The results found weresymmetric but the yield was lower compared to other process

chains for JEE. For the process chain JEE17, the highest yield of ester was found at 60

ºC with 75 minute reaction time and 

corresponding viscosity was observed at 7.6 cSt, which is not

Table 4 Effect of catalyst concentration on transesterification of jatropha oil with aqueous ethanol

Process

Chain

Purity of 

Alcohol (%)

Catalyst Concentration

(% wt of oil))

Reaction

Time (min)

Reaction Temp

(deg C)

Biodiesel Yield

(% wt of oil)

JEE 7 85 0.5 60 60 NS

JEE 8 85 1.0 60 60 NS

JEE 9 85 1.5 60 60 58.2

JEE 10 85 2.0 60 60 68.4

JEE 11 85 2.5 60 60 72.1

JEE 12 85 3.0 60 60 76.8

Table 5 Effect of purity of ethanol on transesterification of jatropha oil

Process

Chain

Purity of 

Alcohol (%)

Catalyst Concentration

(% wt of oil)

Reaction

Time (min)

Reaction Temp

(deg C)

Biodiesel Yield

(% wt of oil)

JEE 13 97.5 3.0 60 60 NSJEE 14 95 3.0 60 60 50.4

JEE 15 92.5 3.0 60 60 53.2

JEE 16 90 3.0 60 60 66.3

JEE 17 87.5 3.0 60 60 71.2

JEE 18 85 3.0 60 60 76.8

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 International Journal of Recent Scientific Research, Vol. 4, Issue, 7, pp. 1005 - 1010, July, 2013 

1009

60

55

50

45

40

3

4

5

6

7

8

9

10

75

60

45

30

JEE9

JEE10

JEE11

JEE12

   V   i  s  c  o  s   i   t  y   (  c   S   t   )

    R   e  a  c   t   i  o

  n    T   i

  m  e    (   m

   i  n    )

R e a c t i o n  T e m  p e r t u r e  ( d e  g  C  ) 

 Figure 5 Effect of reaction time and temperature on the viscosity of JEE  

In the acceptable range. But, for process chain JEE18, the

highest yield of 82.3% was found with 75 minute reaction timeat 60ºC and corresponding viscosity observed was 5.3 cSt,

which is lower than process chain JEE16 and JEE17.

60

55

50

45

40

30

40

50

60

70

80

90

100

75

60

45

30

JEE16

JEE17

JEE18

   B   i  o   d

   i  e  s  e   l   Y   i  e   l   d   (   %   )

    R   e  a  c   t   i  o

  n    T   i

  m  e    ( 

  m   i  n    )

R e a c t i o n  T e m  p e r t u r e  ( d e  g  C  ) 

 Figure 6 Effect of reaction time and temperature on the yield of JEE with

variation in purity of ethanol

60

55

50

45

40

3

4

5

6

7

8

9

10

75

60

45

30

JEE16

JEE17

JEE18

   V   i  s  c  o  s   i   t  y   (  c   S   t   )

    R   e  a  c   t   i  o

  n    T   i

  m  e    ( 

  m   i  n    )

R e a c t i o n  T e m  p e r t u r e  ( d e  g  C  ) 

 Figure 7 Effect of reaction time and temperature on the viscosity of JEE with

variation of catalyst concentration and aqueous ethanol

The highest yield (82.3%) of process chain JEE18 wasapproximately 20% higher than compared to process chain

JEE16 and JEE17. It is seen that in respect of viscosity and yield of ester, the results are very much symmetrical for the allthe process chains. It has also been seen that with increasing

the aqueousness of ethanol the yield of jatropha ethyl ester wasalso increasing. Thus the recommended process parameters for the production of jatropha ethyl ester (JEE) can be summarized 

as reaction time of 75 minute, reaction temperature of 60ºC,molar ration of 6:1, and catalyst concentration of 3.0% with85% ethanol purity. The observed results also indicate that, for 

higher aqueousness ethanol, the biodiesel quality is very good compare to lower aqueousness of ethanol.

CONCLUSIONS

 No ester separation was found by using 100% ethanol atdifferent level of catalyst concentrations from 0.5 to 3.0% and 

similarly at lower temperature regimes of 45ºC and 40

ºC. With

varying temperatures from 60ºC to 50

ºC the yield was varied 

from 32.4% to 68.2%. For the process chain JEE17, thehighest yield of ester was found at 60

ºC with 75 minute

reaction time and corresponding viscosity was observed 7.6cSt, which is not in acceptable range. But, for process chain

JEE18, the highest yield 82.3% was found with 75 minutereaction time at 60

ºC and corresponding viscosity 5.3 cSt,

which is lower than process chain JEE16 and JEE17. The

highest yield (82.3%) of process chain JEE18 wasapproximately 20% higher than compare to process chainJEE16 and JEE17. It is seen that in respect of viscosity and 

yield of ester, the results are very much symmetrical for the allthe process chains. It is also observed that with increasing the purity of ethanol the yield of jatropha ethyl ester was also

increasing. The recommended process parameters for the

 production of jatropha ethyl ester (JEE) are: reaction time75 minute, reaction temperature 60ºC, molar ration 6:1, and 

catalyst concentration 3.0% with ethanol purity 85%. Theobserved results also indicate that, for higher degree of proof of ethanol, the biodiesel quality is very good compare to lower 

 proof of ethanol.

References

Canakci, M. and Van Gerpen, J. 1999. Biodiesel production viaacid catalyst. Transactions of the ASAE , 42 (5) : 1203-1210.

Canakci, M., Gerpen, J.V., 2001. Biodiesel production from oils

and fats with high free fatty acids. Trans. ASAE 44 (6), 1429-1436.

Dasari, M.A., Goff, M.J., Suppes, G.J., 2003. Non-catalyticalcoholysis kinetics of soybean oil. J. Am Oil Chem. Soc. 80(2), 189-192

Encinar, J.M., Gonzalez, J.F., Rodriguez, J.J., Tajedor, A., 2002.Biodiesel fuel from vegetable oils: Transesterification of 

Cynara cardunculuc L. oil with ethanol. Energy Fuel 16 (3),443-450.

Goff, M.J., Bauer, N.S., Lopes, S., Sutterlin, W.R., Suppes, G.J.,2004. Acid catalyzed alcoholysis of soybean oil. J. Am. OilChem. Soc. 81 (1), 415-420.

Knothe, G., 2002b. Structure indices in FA chemistry. Howrelavent is the iodine value? J. Am. Oil Chem. Soc. 79 (9),847-854.

Kusdiana, D., Saka, S., 2001. Methyl esterification of free fattyacids of rapeseed oil as treated in supercritical methanol. J.Chem. Eng. Japan 34 (3), 383-387.

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 International Journal of Recent Scientific Research, Vol. 4, Issue, 7, pp. 1005 - 1010, July, 2013 

1010

Meher, L. C.; Naik, S. N. and Das, L. M.2004. Methanolysis of 

Pongamia pinnata (Karanja) oil for production of biodiesel.  Journal Scientific and Industrial Research, 63, 913-929.

Michael S. G. and Robert, L.M., 1998. Combustion of fat and vegetable oil derived fuels in diesel engines. Prog. Energy

combust. Sci., Vol,24, pp125-164.Otera, J., 1993. Transesterification. Chem. Rev. 93 (4), 1449-

1470.

Planning Commission Report, 2003. National mission on biofuels.Published by Ministry of planning commission, Govt of India.

Saka, S., Kusdiana, D., 2001. Biodiesel fuel from rapeseed oil as

 prepared in supercritical methanol. Fuel 80 (2), 225-231.Srivastava A, Prasad R. 2000. Triglycerides-based diesel fuel.

Renewable and Sustainable Energy Reviews. Vol 4, 111-133.

Toda, T., Honda, H., Fukumura, T., Sibasaki-Kitakawa, N.,Yonemoto, T., 2004. Novel production method of biodiesel

fuel using anion exchange resin as a heterogeneous catalyst.10

thAsian Pacific Confederation of Chemical Eng. Congress

2004, Kitakyushu, Japan.

Warabi, Y., Kusdiana, D., Sakam, S., 2004. Reactivity of triglycerides and fatty acids of rapeseed oil in supercriticalalcohols. Bioresource Technol. 91 (3), 283-287.

Yamazaki, R., Iwamoto, S., Nabetani, H., Osakada, K.,Miyawaki, O., Sagara, Y., 2004. Biodiesel fuel production bynon-catalytic alcoholysis of oils. 10th Asian Pacific

Confederation of Chemical Eng. Congress 2004, Kitakyushu,Japan.

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