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Biodiesel Production from Crude Jatropha Oil (CJO) in Pilot Plant

Conference Paper · April 2013

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 Biodiesel Production from Crude Jatropha Oil
(CJO) in Pilot Plant
1 2
Hazir Farouk Abdelraheem Mohammad Nazri Mohd Jaafar
School of Mechanical Engineering, Faculty of Engineering Department of Aeronautical, Automotive & Ocean Engineering
Sudan University of Science and Technology Faculty of Mechanical Engineering
Khartoum, Sudan Universiti Teknologi Malaysia
hfae76@yahoo.com nazri@fkm.utm.my
3 4
Tirto Prakoso Sabir Mohammad Salih
Department of Chemical Engineering School of Mechanical Engineering
Faculty of Industrial Engineering Technology Faculty of Engineering
Institute of Technology Bandung Sudan University of Science and Technology
Bandung, Indonesia Khartoum, Sudan

Abstract— In this work, a two step-transesterification process This paper discusses in details the use of an acid-catalyst
was adopted to produce biodiesel from different samples of esterification stage to successfully reduce even relatively high
jatropha oil with different acid numbers (8.99 and 15.99 FFA percentages to below 1%, before entry into a second
mgKOH/g). The first sample was subjected to esterification stage of base-catalyst transesterification to produce a
process at lab scale without preheating, and the final acid biodiesel that complies with international standards.
number found to be 0.36 mgKOH/g, with process parameters of
0.225 v/v sulfuric acid (H2SO4), 6:1 w/w methanol (MeOH) to oil A. Transesterification process
mole ratio, reaction temperature of 65°C, and 180 min of Transesterification is regarded as the best method among
reaction time. Using a pilot plant, the final acid number found to the alternative biodiesel production methods, due to its low
be 0.23 mgKOH/g for the second jatropha oil sample, with cost and simplicity. Transesterification is the normal name
preheating and decreasing the methanol to oil mole ratio to 4.5:1
given to the chemical reaction between triglycerides and
w/w. Meanwhile the other parameters remained the same from
the lab scale. The final biodiesel yield obtained was 82% from alcohol to form an ester and glycerol with or without the
the first jatropha oil sample, and 90% from the second one by presence of catalyst. This process is also called alcoholysis of
using base-catalyst process parameters of 1.2 w/w potassium ester. Generally, the reaction time and yield of
hydroxide (KOH), 4.5:1 w/w methanol to oil mole ratio, reaction transesterification can be enhanced by adding catalyst. The
temperature of 60°C at 120 min of reaction time. The basic reaction can be represented as in “Fig. 1”, where the
physiochemical properties of the produced biodiesel from the mechanism of transesterification consists of three reversible
two jatropha oil samples were both found to be within the reactions, in which the triglycerides are converted into
ASTM D6751 specified limits. diglycerides followed by conversion to monoglycerides, and
then lastly converted into glycerol, producing one ester at
I. INTRODUCTION each conversion stage [1-3].
Development of a large-scale biodiesel production Transesterification can be categorized into two main types,
industry in a country interested in reducing dependency on which are the catalytic and non-catalytic methods. Catalytic
petroleum-sourced diesel fuel will require management or transesterification includes alkaline-catalyzed reaction, acid-
solution of many critical issues. One significant problem in catalyzed reaction and enzyme-catalyzed reaction.
production of biodiesel is how to deal with feedstock with a
high free fatty acid (FFA) content, which has a significant
affect in the final yield of methyl ester.
In large scale production of biodiesel from crude jatropha
oil (CJO), while the CJO is the largest input cost, the costs of
the other chemicals used are also significant. Optimizing the
amounts of these chemicals along with other parameters of
reaction temperature and time indicate that real savings can
be made in time and chemical cost, which significantly
improve operating economics. Figure 1. Stoichiometric transesterification of triglycerides [1-3]

This research is sponsored by Aeronautical Research Center (ARC_Sudan)

 Non-catalytic transesterification commonly refers to The acid catalysts will utilize the free fatty acids in the oil
supercritical methanol (SCM) transesterification. At present, and convert them into biodiesel [2]. The successful pretreatment
conversion of vegetable oils into biodiesel is commonly of the high FFA of Jatropha oil to less than 1% has been reported
executed by using alkaline-catalyzed transesterification. This by many researchers. Berchmaus and Hirata
is due to its high effectiveness and because the process is less [8] reported reduction of the FFA of Jatropha curcas oil from
corrosive to the equipment compared to the use of acid and 15% to less than 1%, in combination of 1%w/w of H 2SO4,
enzyme-based catalysts [3]. 60%w/w methanol to oil ratio and reaction time of 1 h at 50 oC.
The transesterification reaction is affected by various Azhari [13] found that using of 1%w/w H 2SO4, 60%w/w of
parameters depending on the reaction conditions. If the methanol to oil ratio, reaction temperature of 60 oC and 180 min
parameters are not optimized either the reaction is incomplete of reaction time can decrease the FFA of jatropha oil from 25.3%
or the yield is reduced to a significant extent. Each parameter to 0.5%. Patil and Deng [14] have achieved a high yield of
biodiesel from Jatropha curcas oil by decreasing the FFA from
is equally important in order to achieve a high quality 14% to less than 1%. They used pretreatment conditions of 6:1
biodiesel which meets the regulatory standards [4]. The
methanol to oil ratio, 0.5% (v/v) of H 2SO4 at 40oC and 120 min.
maximum yield of biodiesel should be reached when values The FFA content of crude Jatropha oil was also reduced
of these variables are optimized. Some of the critical successfully from 21.5% to less than 1% by Siddharth Jain and
variables are molar ratio of alcohol to oil, concentration of M.P. Sharma [11]. They used optimum parameter values of 1%
catalyst, reaction time and reaction temperature. w/w H2SO4, 3:7 w/w of methanol to oil ratio, reaction
II. RESEARCH BACKGROUND temperature of 65oC and 180 min of reaction time. A summary
Jatropha oil is a triglyceride type of non-edible vegetable oil of these approaches is reported in Table 2.
and in its pure form is a potential alternative to fossil diesel fuel. B. Alkaline-base catalyst
This is due to the fact that its methyl ester properties are similar
The primary parameters relevant to biodiesel production
to diesel fuel and also of its plant origin has the ability of absorb
by transesterification of vegetable oils by alcohol using a base
CO2 from the atmosphere when it is utilized in diesel engines catalyst are the FFA content and moisture content. A high
[2]. However, direct burning of Jatropha oil in diesel engine percentage of free fatty acid will result in incomplete reaction
faces many problems related to viscosity. This is due to the oil’s and low yield of biodiesel due to soap formation. However,
high molecular weight as well as its chemical structure is around the main alkaline base catalysts used are sodium hydroxide
ten times higher than the diesel ones. Therefore, the reduction in (NaOH) and potassium hydroxide (KOH). High yields of
viscosity is very important to make Jatropha oil a suitable jatropha methyl ester were reported by many researchers.
alternative fuel far from diesel and this can be achieved by the Chitra et al [16] produced jatropha methyl ester at a high
transesterfication process [1, 2]. yield of 98% by using NaOH in concentration of 1.0 w/w,
Crude Jatropha curcas oil has a wide range of FFA content 5.6:1 methanol to oil ratio, reaction temperature of 60oC and
as shown in Table 1, and are usually beyond the optimum level 90 min of reaction time. Berchmaus et al [17] achieved a 97%
biodiesel yield by using KOH catalyst at concentration of
for alkaline transesterification to occur [5,6]. Alkaline-catalyzed
1.1w/w, 6:1 methanol to oil ratio, reaction temperature of
transesterification of high-FFA CJO will lead to soap formation
that makes separation of the products become difficult. Despite 500C and 120 min of reaction time. A 98% yield was reported
acid catalyst not having this issue; it is not practical due to its by Lu et al. [18]. In combination of of 1.3% w/w KOH, 6:1
long reaction time. Thus, a two-step transesterification is methanol to oil ratio, reaction temperature of 64 0C at 20 min
introduced where the CJO is pretreated with acid-catalyzed of reaction . A summary of these findings is listed in Table 3.
esterification to reduce the FFA content to less than 1%, III. MATERIALS AND METHODS
followed by base-catalyzed transesterification of the CJO to fatty
acid methyl ester (FAME) [7,8]. In this work, two different types of CJO were used. For
the lab scale the Jatropha curcas seeds were provided from a
A. Acid-base catalyst jatropha plantation located at Kosti in the centre of the
Improper handling and storage of CJO leads to increase in Republic of Sudan.
FFA as a result of chemical reactions such as hydrolysis and
polymerization. It has been reported that transesterification TABLE 2: OPTIMIZED CONDITIONS FOR ESTERIFICATION OF CJO
will not occur if the oil contains a high percentage of FFA Optimum esterification process parameters Final
[2]. Among the many proposed pretreatment methods, the Catalyst
Alcohol Reaction Reaction
FFA Ref
esterification of FFA with methanol in the presence of acidic ratio Temp. Time
ratio
catalysts is the most commonly applied method. (MeOH) (oC) (min)
H2SO4 60% wt 50 60 ˂ 1% [8]
TABLE 1: FREE FATTY ACID CONTENT OF CRUDE JATROPHA OIL 1% w/w
H2SO4 60% wt 60 180 0.5% [13]
Free Fatty Acid content (FFA %) Reference
1% w/w
3.4 [9] H2SO4 6:1 40 120 ˂ 1% [14]
7.3 [10] 0.5% v/v w/w
14.9 [8] H2SO4 3:7 65±5 180 ˂ 1% [11]
1% w/w w/w
21.5 [11]
H2SO4 12 wt% 70 120 ˂ 1% [15]
22.6 [12] 1% w/w
 After extraction using a mechanical expeller, the oil was TABLE 4. PHYSIOCHEMICAL PROPERTIES OF CRUDE JATROPHA OIL (CJO)
processed for experimentation in the Laboratory of Oils and Properties CJO CJO
Fats, Department of Chemical Engineering, Institute of (Sudan) (Bionas)
Technology Bandung. For the pilot plant jatropha crude oil Acid number (mgKOH/g) 8.99 15.99
was purchased from Bionas SDN Bhd Company in Kuala Density @ 15oC (g/ml) 0.918 0.92
Lumpur. All chemicals used in the two processes and analysis viscosity@40oC (mm2/s) 41 52
methods were obtained in their analytical grade. Sulfuric acid Saponification (mgKOH/g) 193.6 181
Water content % 0.14 0.07
(H2SO4) was used as catalyst with methanol for the Flash point (oC) 248 240
esterification process, while potassium hydroxide (KOH) was Calorific value (MJ/Kg) - 37.8
the base catalyst selected over sodium hydroxide (NaOH) to Iodine value (mg I2/g) 103.87 -
enhance the reaction for the second step of the Diglycerides (% m/m) - 2.7
transesterification process. The main physiochemical Triglycerides (% m/m) - 97.3
properties of the two CJO samples were determined as per
standard methods and reported in Table 4.
After one hour of the reaction (in vigorous mixing), the
IV. EXPERIMENTAL PROCEDURE mixture was allowed to separate and settle in a funnel for
The following experimental procedure was adopted for 30min to remove the glycerol layer which was formed in the
the production of biodiesel at lab scale and in the pilot plant. bottom of the funnel as shown in “Fig. 2 (c)”. After that the
Due to the high fatty acid number of the selected crude remainder of the mixture was poured again into the round-
jatropha oil samples, the transesterification process was bottomed flask, and the reaction was conducted for one hour
conducted in two steps which are described as follows: by adding the other 20% of the prepared methoxide. The final
product in the funnel after 30min settling was a clear, golden
A. Acid pretreatment step liquid biodiesel without glycerol layer as shown in “Fig. 2
At the lab scale, experiments were performed using the (d)”.
crude jatropha oil without preheating. A three-necked round-
bottomed flask was filled with a mixture of 200 g of crude C. Sample treatment
jatropha oil and methanol in a concentration of (6:1 w/w). A In this step, the produced methyl ester washed three times
water-cooled condenser and a thermometer with cork were with warm water in 50°C till the pH of the water was less
connected to the side openings on either side of the round- than 8 as shown in “Fig. 2(e)”. To remove the moisture, the
bottomed flask. The mixture was warmed up to 50oC by final product was heated up to 70°C for 30 min under vacuum
placing the round-bottomed flask in a heater and stirred using condition. This resulted in a clear light liquid with a viscosity
a magnetic stirrer fixed into the flask as shown in “Fig. 2 (a)”. close to petro-diesel as shown in “Fig. 2(f)”. The final yield
At that point, H2SO4 at ratio of 0.225% (v/v) was added to the was found to be 82%. The sequences of this production steps
mixture and the reaction conducted for three hours at are shown in “Fig. 2’’.
maintained temperature of 65oC. After the reaction was V. PRODUCTION OF BIODIESEL FROM JATROPHA OIL
completed, the reacted mixture was poured into the separating IN PILOT PLANT
funnel and allowed to separate and settle the methanol phase
for 30 minutes as shown in “Fig. 2 (b)”. Before starting the The pilot biodiesel plant is located in Universiti Malaysia
second process step, the acid value was analysed using Pahang. In this pilot plant, 35 liter of jatropha oil was pretreated
titration method and found to be within the desired range for by heating in the reactor of capacity of 75 liter. The
the next step. This esterified oil was subjected to base- transesterification process took place in two steps. The first
catalyzed reaction. esterification step was performed in parameter conditions of
0.225% v/v H2SO 4, 4.5:1 methanol to oil mole ratio, reaction
B. Base-catalyzed step temperature of 65°C and 180 min of reaction time. The required
The esterified oil from the first step was poured into the amount of H2SO4 was added to the mixture of methanol and oil
round-bottomed flask. The required amount of catalyst KOH after the mixture was warmed up to 50°C in vigorously stirring
(1.2% w/w) was weighed and dissolved completely in mode. The reaction was conducted for three hours at maintained
methanol (6:1 w/w) to form potassium methoxide. temperature of 65°C. After that, the reaction was stopped and the
Meanwhile, the esterified oil was warmed up, and then 80% mixture was allowed to settle overnight. After this settling time,
from the prepared methoxide was added into the oil at 60oC. the mixture was separated into two layers. The upper layer was
TABLE 3. OPTIMIZED CONDITIONS FOR TRANSESTERIFICATION OF CJO
removed and a sample of the esterified oil was analyzed for acid
value, which was found to be less than 1%. Then the esterified
Optimum Transesterification process parameters Yield oil was subjected to the second step of transesterification process
Catalyst Alcohol ratio Reaction Reaction Ref
(%) with base catalyst. In this step, the optimum parameter values
ratio (MeOH) Temp. (oC) Time (min)
NaOH
were selected to be 1.2 w/w KOH, methanol to oil mole ratio
6.7:1 65 120 90 [8]
1.4%w/w 4.5:1, reaction temperature of 60°C, and 2 hr of reaction time.
NaOH 5.6:1 60 90 98 [16] The esterified oil was heated in the reaction tank up to 50°C,
1.0%w/w meanwhile the required amount of KOH and methanol were
KOH 6:1 50 120 97 [17] mixed up to form potassium methoxide. In mode of stirring, 80%
1.0%w/w from this mixture was added to the esterified oil and allowed to
KOH 6:1 64 20 98 [18] react for
1.3%w/w
1 hr at maintained temperature of 60±2°C. After the reaction was
completed, it was left to settle for 1 hr, After 1 hr it was
separated into two layers. The lower glycerol layer was drawn
off from the bottom of the settling tank. Then, the rest of the
mixture was warmed again and the 20% of the potassium
methoxide was added, and the reaction conducted for 1 hr. The
settling of the mixture for 30 min resulted in a crude biodiesel
without glycerol. The reactor tank was used as a washing tank
and warm water of 50°C was introduced to the crude biodiesel
and the process of washing was started. During the washing
process, gentle agitation is required to avoid the formation of
emulsion. After 30 minutes, the washing water layer was drained
off from the bottom of the washing tank. The washing process
Figure 3: Biodiesel pilot plant
was repeated four times to ensure that pH of the drained water
from washing process has reached 7, then, the crude biodiesel
was cleared of residual water by being heated to 70°C under VI. RESULTS AND DISCUSSION
vacuum condition, and the transparent final product was ready While the esterification of FFA with methanol in the
for storing after 30 min. The photograph of the biodiesel pilot presence of acidic catalysts is the most commonly applied
plant is in “Fig. 3’’. method, the percentage of acid catalyst used and the molar
ratio of alcohol should be in their optimum value to enhance
the process and decrease the total production cost. Base on
the experimental procedure used in this work, a two-step
transesterification process has been conducted to produce
biodiesel from two samples of crude jatropha oil with
different levels of FFA (8.99 and 15.99 mgKOH/g). This high
level of FFA is going to decrease the final yield due to soap
formation during base-catalyst transesterification. Thus,
esterification process was adopted as a necessary first step to
decrease these values to less than 1%.
The first jatropha oil sample (8.89 mgKOH/g) was
subjected to esterfication process in lab scale without
preheating. The final FFA was found to be 0.36 mgKOH/g, in
the presence of 0.225 v/v H2SO4, 6:1 of methanol to oil mole
ratio, and the reaction completed in temperature of 65°C and
(a) (b) (c) 180 min time.
For the second jatropha sample (15.99 mgKOH/g),
preheating was done first and methanol to oil mole ratio
decreased to 4.5:1. Meanwhile, the other process parameters
remain the same from the lab scale. The final FFA was found
to be 0.23 mgKOH/g. The summary of the first esterification
step process parameters for the two crude jatropha oil
samples used in this work is reported in Table 5.
Some of the work done in transesterification of jatropha oil is
reported in Table 2 and Table 3. From the first table it’s clear
that to reduce the FFA, acid catalyst such as H 2SO4 must be used
for better performance in varying quantities (1%w/w and
0.5%v/v), depending on the feedstock properties. Though the
two samples used in this work were with high FFA, better results
were achieved with 0.225%v/v H2SO4.
(d) (e) (f)
TABLE 5. OPTIMUM E STERIFICATION PROCESS PARAMETERS
PARAMETERS CJO CJO
(SUDAN) (BIONAS)
Catalyst H2SO4 H2SO4
% v/v 0.225 0.225
Figure 2. Transesterification process steps of jatropha methyl ester in lab Alcohol molar ratio MeOH MeOH
scale w/w 6:1 4.5:1
Reaction Time (min) 180 180
Reaction Temp.(oC) 65 65
 The ratio of alcohol to oil used was found to be 6:1 for VII. CONCLUSIONS
most of pervious research work. In this work it found that Cost-effective large-scale production of biodiesel from
decreasing the MeOH ratio to 4.5:1 with preheating is going non-edible oil feedstock requires that free fatty acids be
to bring the FFA to less than 1% and so reduce the biodiesel below 1%, failing this, a highly effective system should be
production cost. The reaction temperature in all the previous developed to deal with higher FFA levels. In practice while
research work didn’t exceed the methanol boiling temperature properly extracted jatropha oil should have FFAs below 1%,
but it went down to 50°C and 40°C in some cases. The it is not unusual for levels to rise due to a number of factors
maximum time used previously was 180 min while some during storage and transport.
used 60 minutes and 120 minutes. This paper identified how well a preliminary acid-catalyst
In the second transesterification process, the process esterification step reduces higher FFA level in jatropha oil
parameters remain the same for the two samples. KOH base feedstock from different two sources. On addition, it also
catalyst was used for better conversion, with 1.2%w/w, the identified some potential optimization (a reduced molar ratio)
optimum ratio of alcohol to oil found to be 4.5:1. Meanwhile, of necessary chemical inputs that will improve the economics
when the reaction continued under maintained temperature of of large scale production. The maximum final biodiesel yield
65°C, it’s found that it’s better to add the methoxide in two of 82% and 90% was achieved from jatropha oil samples
different batches, by conducting the reaction for one hour sourced from Sudan and Malaysia, respectively. The basic
with 80% from methoxide, and one hour with the remain physiochemical properties of the produced biodiesel from the
20%. The results obtained from this technique, were biodiesel two jatropha oil samples were both found to be within the
free from glycerol which accelerated the washing process. A ASTM D6751 specified limits.
summary of these parameters are reported in Table 6.
ACKNOWLEDGMENT
From Table 3 it is obvious that up to 98% biodiesel yield The Author would like to acknowledge Dr. Mohammed
can be achieved by either using NaOH or KOH in the Elhadi Ahmed Elsayed, the general manager of Aeronautical
presence of 6:1 alcohol to oil ratio, reaction time of 90 min Research Centre (ARC_Sudan) for his kindness and
for NaOH and 120 min for KOH, in maximum reaction inspiration through the roadmap development initiated by the
temperature of 65ºC. In this work, the yield percent of Center’s ‘Sudan Biofuel Roadmap’ project. Thanks also are
produced biodiesel in lab scale is found to be 82%, expressed to Gas Turbine Combustion Research Group
meanwhile it was 90% in the pilot plant. Some of the (GTCRG) from the Mechanical Faculty, Universiti Teknologi
properties are reported in Table 7. It’s obvious from Table 7 Malaysia. Thanks also expressed to Assoc. Prof. Dr.
that the main properties of biodiesel produced from the two Abdurahman H. Nour, from Universiti Malaysia Pahang for
crude jatropha oil used in this work were found to be within his guidance in utilization of the pilot plant, and for Dr.
the limits of American Society for Testing and Materials Khalid Silik from Universiti Kebangsaan Malaysia, for his
(ASTM) specifications for biodiesel and diesel fuel. continues assistant and guidance. Special thanks go to Dr.
Tirto Prakoso from the Institute of Technology, Bandung,
TABLE 6. OPTIMUM T RANSESTERIFICATION PROCESS Department of Chemical Engineering, Faculty of Industrial
PARAMETERS Technology for his invaluable guidance, the help provided by
Parameters CJO CJO his assistants Yanti and Meiti, and for the use of laboratory
(Sudan) (Bionas) facilities in performing the experiments and doing the
Catalys KOH KOH physiochemical analysis. The author is also grateful to
% v/v 1.2 1.2
Alcohol molar ratio MeOH MeOH
Andrew Lang from the World Bioenergy Association for
w/w 4.5:1 4.5:1 giving helpful guidance and support throughout this work.
Reaction Time (min) 120 120
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