Studies on biodiesel produced from Jatropha oil in Cambodia by a non-catalytic using C 2 H 5 OH •

Different technologies are currently available for biodiesel production from various kinds of lipid containing feedstock. Among them, the alkaline-catalyzed methods are the most widely studied. However, here are several disadvantages related to biodiesel production using alkaline catalysts such as generation of wastewater, catalyst deactivation, difficulty in the separation of biodiesel from catalyst and glycerin, etc. To limit the problems mentioned above, in this study, biodiesel is produced by a noncatalytic using C2H5OH. The effect of experimental variables (the molar ratio ethanol/oil of 41.18:1 – 46.82:1, reaction times of 50 90 minutes and reaction temperatures of 2750C 2950C) on the yield of biodiesel was studied. The 96% yield of Cambodia biodiesel of reaction between C2H5OH and Jatropha Oil at 46:1 at temperature 2900C at 60 minutes no using catalysts. Obtained biodiesel fuel was up to the International Standard ASTM D6751 for biodiesel fuel blend stock (B100).

Studies on biodiesel produced from Jatropha oil in Cambodia by a noncatalytic using C 2 H 5 OH

• Nguyen Van Phuoc
Institute for Environment and Resources • Chhoun Vi Thun

• Pham Thanh Quan
Hochiminh City University of Technology (Manuscript Received on 07.08. 2014, Manuscript Revised 14.10, 2014) ABSTRACT: Different technologies are currently available for biodiesel production from various kinds of lipid containing feedstock.Among them, the alkaline-catalyzed methods are the most widely studied.However, here are several disadvantages related to biodiesel production using alkaline catalysts such as generation of wastewater, catalyst deactivation, difficulty in the separation of biodiesel from catalyst and glycerin, etc.To limit the problems mentioned above, in this study, biodiesel is produced by a non-catalytic using C2H5OH.The effect of experimental variables (the molar ratio ethanol/oil of 41.18:1 -46.82:1, reaction times of 50 -90 minutes and reaction temperatures of 275 0 C -295 0 C) on the yield of biodiesel was studied.The 96% yield of INTRODUCTION Jatropha curcas L. is a small shrub with gray bark, white sap flows when cut.Normally plants grow 4m high and can reach a height of up to 5 meters in favorable conditions [2].In Cambodia, they grow mainly and abundantly in a mountainous region of the north and central part, the littoral region from Banteaymeanchey province to Kampongthom province as traditional medicine and hedge such as: Battambong, Pursat, Kampongspeu, Sihanouk city, Kandal, Preyveng, Kampot, Kampongcham.
The oil content in seeds is 30 -50% depending on varieties, soil, cultivation technique, providing sample supply of raw materials which derived from vegetation and animals.
Biodiesel is a mixture of fatty acid alkyl esters that can be produced by different techniques such as microemulsion, direct use or blending, thermal cracking (or pyrolysis), and transesterification (Boro et al., 2012).Among them, transesterification (or alcoholysis) is the most common method to produce biodiesel from

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various lipid containing feedstocks such as vegetable oils and animal fats.Recently, supercritical transesterification has been proposed as an attractive method to produce biodiesel in the absence of catalyst, which is more efficient and environmentally friendly than catalytic transesterification process.This paper focuses on optimizing the reaction condition for molar ratio of ethanol to oil, duration of reaction with 1 process and operation temperature in one step procedure to produce biodiesel fuel (BDF) from Jatropha oil.

Materials and Equipment
Jatropha Curcas L., seeds are provided by Sodeco Company, Banteaymeanchey province, Cambodia.The Jatropha seeds were pressed by the Germany press machine -GTZ Organization, the power of 10W to extract oil.The oil was then stored in the tank, let stand for 24 hrs and carefully decanted.
The fatty acid profile of the crude oil was determined by gas chromatography, using GC -MS according

Experiments setup and reactor operation
To achieve purpose of this study, the experiment was conducted as follows: The molar ratios of ethanol/oil in the reaction processes was 41.18:1, 42:1, 44:1, 46:1 and 46,82:1, the reaction times ranged of 50 -90 minutes and reaction temperatures was 275 0 C, 280 0 C, 285 0 C, 290 0 C and 295 0 C. The analysis method have a high accurate and repeated 3 times for each of experimental.
Operation of transesterification process: Small scale production of biodiesel was carried out using 87 gram of oil.Transesterification result of jatropha oil was investigated by changing ethanol to oil molar ratios, residence time and temperature, respectively.
After the reaction ends, product was poured into the separator and settled for 3 hours.The mixture was separated into two phases: EE pale yellow liquid above, the glycerol was the darker colored liquid on the bottom.The light phase was extracted, neutralized acetic acid and settle for 1 hour.The product after settling was cleaned in warm water and settle for 30 minutes, then dried by stirring with heat at 120 0 C.

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The conversion of oil to BDF was monitored by thin layer chromatography (TLC) using silicagel 60 F254 (Merk) plates.
The solvents consisting of chloroform to petroleum ether varied continuously from 1:10 to 10:10 with the total amount of the eluent at 20 ml.The optimal ratio of 1:2 was used as preliminary analysis of oil composition.

BDF from jatropha oil in Cambodia
Composition of methyl esters were identified by high pressure liquid chromatography (HPLC) according to the following analysis process: Aliquots (1ml) were taken from the outlet at each two volumes replacement and left to stand for 2 hrs for products separation.An accurate amount of 100 mg from the upper layer was diluted in the mobile phase to a concentration of 3% (w/w) and analyzed for the concentration of triglycerides, diglycerides, monoglycerides, and FAEEs by reversed phase chromatography.The composition of the transesterification reaction products was determined by HPLC using a Shimadzu chromatograph, consisting of a Model LC -10A HPLC pump and a Model RID 10A refractive index detector.
The LC column was a Cadenza CD -C18 polymerbased column, 25 cm x 3.0 mm with 4 µm diameter particle size silica.
In all cases, the mobile phase was an acetone/acetonitrile mixture, 70:30, with a flow rate of 0.4 ml/min and a loop of 20 µl.By using standard grade reagent calibration curves were generated using as internal standard nhexadecane.
The molar concentrations of triglycerides and ethyl esters (EE) were evaluated from the areas of relevant peaks, according to the The Biodiesel performance H (%) according to the following formula: Where C is concentrations of ethyl esters, mbiodiesel is weight of biodiesel, m is weight of Jatropha oil, M and MFAEE is the average molecular weight of Jatropha oil and FAEE.

Effect of reaction conditions on the ethyl esters yield
Small scale production of biodiesel was carried out using 87 gram of oil.Transesterification result of jatropha oil was investigated by changing ethanol to oil molar ratio, residence time and temperature, respectively.
From the experimental results, after building the regression equation and eliminating the inconsistent regression coefficient -the coefficient f <f (0,05;3) = 2.35, and checking the fit of the model by Fisher standard (F model = 1.86 <F table (0,05;5;3) = 9.01).

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The real equation: Y = 223.63-8.24 Z1 + 0.15 Z2 + 0.098 Z1 2 The regression equation shows the performance of biodiesel is affected by the proportion level 1 of reaction temperature, level 1 and level 2 of ethanol/oil.With the molar ratio ethanol/oil from 42:1 to 46:1, the higher performance of biodiesel catalysis when higher concentrations.In the same molar ratio ethanol/oil, biodiesel performance is directly proportional to the reaction temperature.From the regression equation above, optimal conditions to achieve the highest performance biodiesel (96%) as follows: the ratios of ethanol/oil 46:01, reaction time of 60 min and reaction temperature of 290 o C.  The properties of jatropha biodiesel (B100) from Jatropha oil.
The properties of jatropha biodiesel (B100) is presented in Table 4. From this table, it can be seen that, all properties of biodiesel fuel from Jatropha oil (i.e.flash point, Catani number, acid number, cloud point, and kinematic viscosity at 40 0 C) are in conformance with ASTM D6751 standard.
following formula: CTG = (a * ATG/AIS + b) * CIS + b) * C * IS 100/M.Where a is the slope of calibration function, b is the intercept of calibration function, CTG is the weight percentage of triglycerides in the sample, ATG is the sum of peak area of individual triglycerides, AIS is the peak area of internal sample, weight; and M is weight of sample.The data presented are averages of three replicates of determination [5].

Figure 2 .
Figure 2. Actual biodiesel performance compared with the model

Table 1 .
Chemical composition of jatropha seed oil in Cambodia

Table 2 .
Effect of reaction yield

Table 3 .
The results of analysis of factors affecting coding for regression models