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Energy
EnergyProcedia
Procedia143 (2017) 000–000
00 (2017) 742–747
www.elsevier.com/locate/procedia

World Engineers Summit – Applied Energy Symposium & Forum: Low Carbon Cities & Urban
World Engineers
EnergySummit – Applied Energy
Joint Conference, Symposium
WES-CUE & Forum:
2017, 19–21 Low Carbon
July 2017, Cities & Urban
Singapore
Energy Joint Conference, WES-CUE 2017, 19–21 July 2017, Singapore
Biodiesel
Biodiesel production in
in aa reactive
The 15th International
production Symposiumdistillation
reactive column
on District Heating
distillation catalyzed
catalyzed by
and Cooling
column by
heterogeneous
heterogeneous potassium catalyst
Assessing the feasibility ofpotassium
using the heat catalyst
demand-outdoor
temperature
Yano Surya Pradana , Arif Hidayat , Agus Prasetya , Arief Budimana,c,forecast
function
Yano Surya Pradanaa,for
a
ArifaHidayat
long-term
b, Agusdistrict
b
Prasetyaa,heat
a
Ariefdemand
Budimana,c,*
*
a
Chemical Engineering Department, Faculty of Engineering, Universitas Gadjah Mada, Jalan Grafika No. 2, Yogyakarta 55281, Indonesia
a,b,c aof Engineering, Universitas
a b Jalan Grafika No. 2,cYogyakarta 55281, Indonesia
c
a
Chemical
b
I. Andrić
Engineering
Chemical Engineering *, A. Pina , P. Ferrão , J. Fournier ., B. Lacarrière , O. Le Corre
Department, FacultyUniversity
Department, of Islam Indonesia,Gadjah Mada,
Jalan Kaliurang KM. 14,5, Yogyakarta 55584, Indonesia
c bChemical Engineering Department, University of Islam Indonesia, Jalan Kaliurang KM. 14,5, Yogyakarta 55584, Indonesia
Master Program of Systems Engineering, Universitas Gadjah Mada, Jalan Teknika Utara No. 3, Yogyakarta 55281, Indonesia
IN+Master
CenterProgram of Systems Engineering, Universitas Gadjah Mada,Superior
Jalan Teknika Utara No. 3, Yogyakarta 55281, Lisbon,
Indonesia
a c
for Innovation, Technology and Policy Research - Instituto Técnico, Av. Rovisco Pais 1, 1049-001 Portugal
b
Veolia Recherche & Innovation, 291 Avenue Dreyfous Daniel, 78520 Limay, France
c
Département Systèmes Énergétiques et Environnement - IMT Atlantique, 4 rue Alfred Kastler, 44300 Nantes, France
Abstract
Abstract
Biodiesel is a bio-based fuel synthesized from a renewable feedstocks, such as vegetable oils or animal fats. Conventionally, it is
Abstract
Biodiesel
made is a bio-based
through fuel synthesized
transesterificating oils wherefromthe a renewable feedstocks,
process involves suchand
catalyst as vegetable
alcohol tooils be or animal
reacted infats. Conventionally,
batch reactor. The most it is
made through transesterificating oils where the process involves catalyst and alcohol
common catalyst for biodiesel production is homogeneous liquid catalyst. These catalytic systems, however, are difficult onto be reacted in batch reactor. The most
District heating
common
separating the finalnetworks
catalyst for
product are suffer
biodiesel
and commonly
production addressed
is homogeneous
from environmental in the literature
liquid
problems as one
catalyst.
because of are
These
they thecatalytic
most effective
hazardous, systems, solutions
caustic however, foraredecreasing
and hygroscopic. difficult
In order the
on
togreenhouse
separating
eliminatethegasfinal
the emissions
product and
problems, from the
wesuffer building sector. These
from environmental
develop potassium systems
problems
loaded require they
because
on activated high investments
are
carbon (K/AC) which
hazardous, areand
ascaustic returned through
hygroscopic.
heterogeneous Inthe heat
order
solid catalyst.
tosales. Due tothe
eliminate
Heterogeneous theproblems,
solid changed
catalyst isclimate
weeasily conditions
develop potassium
regenerated, and building
leadingloaded
to more renovation
on activated
secure, policies,
lowercarbon
in cost,heat
anddemand
(K/AC) more in the future could
as environmentally
heterogeneous solid decrease,
catalyst.
friendly.
prolonging
Heterogeneous the investment
solid catalyst return
is period.
easily regenerated, leading to more secure, lower in cost, and more
The purpose of this study is to demonstrate a process using catalytic reactive distillation column applied to biodiesel production environmentally friendly.
Thepurpose
The
from main oil.
palm scope of study
ofReactive
this this distillation
paper
is toisdemonstrate
to assess thea feasibility
process using
is the simultaneous of using
process the heat
catalytic demand
reactive
implementing – outdoor
distillation
reaction temperature
andcolumn
separationapplied function
in a for
to biodiesel
process heat demand
production
single column.
forecast.
from
This palm The
method districtseveral
oil.presents
Reactive of Alvalade,
distillation is located
advantages the such in
as Lisbon
simultaneous (Portugal),
process
increasing wasimproving
implementing
conversion, usedreaction
as aselectivity,
case
andstudy. The process
separation
reducing district
catalystis requirement,
in aconsisted ofand
single column. 665
buildings
This method that vary
presents in both
several construction
advantages period
such as and typology.
increasing
avoidance azeotrope mixture. Reaction temperature (varied from 50 to 60 Three
conversion, weather
oC) andscenarios
improving (low,
selectivity, medium,
reducing high)
catalyst and three
requirement,
methanol-palm oil molar ratio (varied from 4:1 district
and
renovation
avoidance
to 8:1) were scenarios
azeotrope
optimized were
mixture. developed
to find Reaction
the highest (shallow,
temperature
conversion intermediate,
(varied
in 4 from
hours.deep).
50The To
to 60 estimate
oC)
higher and
reactionthe temperature
error, obtained
methanol-palm heatratio
oilaccelerated
molar demand
(varied
the values were
fromrate,
reaction 4:1
tocompared
8:1) were
resulting with
higher results
optimized from
to find
conversion a dynamic
of the into heat
oil highest demand
conversion
methyl ester.model,
in previously
4 hours.
Meanwhile, The developed
thehigher
higherreactionand validated
temperature
methanol-palm by the
oil authors.
accelerated
molar ratio the reaction
affected rate,
slightly
The results
resulting
differences inshowed
higher reaction that
conversion when of only
conversion. weather
oil Reaction
into methyl changeester.is Meanwhile,
temperature considered,
should bethe the margin
higher
limited of error could
methanol-palm
to the boiling beoil
point acceptable
of molar
methanol fortosome
ratio avoidapplications
affected theslightly
lower
(the error
differences
reaction rateincausing
annual
reaction demand
by was lower
conversion.
vaporization. Reactionthantemperature
Moreover, 20% for allshould
weather
the methanol-palm scenarios
beoillimited
molarto considered).
thewas
ratio also However,
boiling point after
by theintroducing
of methanol
controlled to avoid the
availability renovation
lower
of active
scenarios,
reaction rate the error
causing value
by increased
vaporization. up to
Moreover,59.5% the (depending
methanol-palm on the
oil weather
molar and
ratio renovation
was also scenarios
controlled
site in the catalyst surface. Thus, the highest conversion of triglyceride, 0.8269, was obtained at temperature of 60 C and methanol- by combination
the availability
o considered).
of active
Theinoil
site
palm value
themolarof slope
catalyst coefficient
surface.
ratio of Thus,
6:1. increased
the
It has highestthat
proven on theaverage
conversion ofwithin the posses
triglyceride,
continuous RD range of
an 3.8%
0.8269, up toperformance
was obtained
enhanced 8% at per decade,
temperature that
on theof 60corresponds
oC and methanol-
biodiesel to the
production,
decrease
palm
compared in
oil molar the
to batch number
ratio of heating hours of 22-139h during the heating season (depending
of 6:1. It has proven that the continuous RD posses an enhanced performance on the biodiesel
reactor. on the combination of production,
weather and
renovation
compared to scenarios
batch reactor.considered). On the other hand, function intercept increased for 7.8-12.7% per decade (depending on the
©coupled
2017 The Authors. The
scenarios). Published
valuesby Elsevier Ltd.
© 2017 The Authors. Published bysuggested
Elsevier Ltd.could be used to modify the function parameters for the scenarios considered, and
Peer-review
©improve
2017 The under
theAuthors. responsibility
accuracyPublished of
of heat demand the estimations.
scientific
by Elsevier Ltd. committee of the World Engineers Summit – Applied Energy Symposium &
Forum: Low Carbon Cities & Urban Energy Joint Conference.
© 2017 The Authors. Published by Elsevier Ltd.
Peer-review under responsibility of the Scientific Committee of The 15th International Symposium on District Heating and
Cooling.
* Corresponding author. Tel.: +62-274-902-171; fax: +62-274-902-170.
* E-mail
Corresponding
address:author. Tel.: +62-274-902-171; fax: +62-274-902-170.
abudiman@ugm.ac.id
Keywords: Heat demand;
E-mail address: Forecast; Climate change
abudiman@ugm.ac.id
1876-6102 © 2017 The Authors. Published by Elsevier Ltd.
1876-6102 © 2017
Peer-review underThe Authors. Published
responsibility of theby Elsevier committee
scientific Ltd. of the World Engineers Summit – Applied Energy Symposium &
Peer-review
Forum: Low under responsibility
Carbon of the
Cities & Urban scientific
Energy Jointcommittee of the World Engineers Summit – Applied Energy Symposium &
Conference.
Forum: Low Carbon Cities & Urban Energy Joint Conference.
1876-6102 © 2017 The Authors. Published by Elsevier Ltd.
Peer-review under responsibility of the Scientific Committee of The 15th International Symposium on District Heating and Cooling.
1876-6102 © 2017 The Authors. Published by Elsevier Ltd.
Peer-review under responsibility of the scientific committee of the World Engineers Summit – Applied Energy Symposium & Forum: Low
Carbon Cities & Urban Energy Joint Conference.
10.1016/j.egypro.2017.12.756
2 Author name / Energy Procedia 00 (2017) 000–000

Peer-review under responsibility of the scientific committee

Yano Surya Pradanaofetthe
al. /World
EnergyEngineers (2017)–742–747
Summit
Procedia 143 Applied Energy Symposium & 743
Forum: Low Carbon Cities & Urban Energy Joint Conference.

Keywords: biodiesel; reactive ditillation column, heterogeneous potassium catalyst, potassium loaded on activated carbon

1. Introduction

Recently, renewable energy has become a major concern. Biodiesel is one of the bio-based energy produced from
renewable feedstocks, such as vegetable oils and animal fats [1] and has been recognized as an attractive fuel to substitute
petroleum diesel fuel [2]. Currently, it can be synthesized from palm oil, soybean oil and jathropa oil [3]. The low-cost
feedstocks, such as palm fatty acid distillate and used cooking oil, are also explored to minimize raw material cost [4]. It
has several advantages compared to petroleum diesel fuel: leading to more secure, non-toxic, bio-degradable, better
lubricant and less sulphur content [5]. Although the chemical content is different, both fuels have similar properties and
performance parameters [6].

Nomenclature

GF free glycerol
GT total glycerol
K/AC potassium loaded on activated carbon
RD reactive distillation
xR reaction conversion

Biodiesel is formed by transesterificating triglycerides with short-chain alcohol, typically methanol and ethanol,
by addition of catalyst [7]. Beside biodiesel, this process also obtains glycerol as by-product [8], which can be utilized
as raw materials for producing anti-knocking agent [9]. Conventionally, the transesterification of oils is reacted in
batch reactor and the most common catalyst is homogeneous liquid base catalyst. The using of batch reactor in large
scale biodiesel production faces several problems because of high capital investment and operational cost [2].
However, the using of homogenous liquid base catalyst in the biodiesel production requires neutralization process
followed by washing or separation step to remove the remaining catalyst and salts in organic phase [7]. Besides that,
the homogeneous catalyst cannot be regenerated after the reaction [10]. Thus, the conventional process is high cost
process due to complex unit series, involving reactor and several separation units [11].
Continuous process may be possible to reduce the production cost and improve energy efficiency [12] of batch
reactor, making the price of biodiesel competitive to petroleum diesel [13]. One of promising technologies in biodiesel
production is continuous reactive distillation (RD). RD is designed to integrate reaction and separation process in a
single column, thus intensifying the mass transfer and simplifying the process flowsheet and operation [14]. This
technology offers many benefits over the conventional process: higher conversion, improving reaction selectivity,
lower energy consumption, elimination of solvents in separation step and voidance of azeotropes [11].
Furthermore, the use of heterogeneous solid catalyst is proposed as a potential solution to these problems. By using
this catalyst, the process can be simplified in separation and neutralization unit. Besides that, the catalyst is reusable,
environmentally friendly and less corrosive to the equipment [15]. Potassium is one of nominated actives species
loaded on catalyst support for transesterification reaction. Recently, there has been increasing study of heterogeneous
potassium catalyst for transesterification reaction, such as potassium on Al2O3 [16], potassium on NaY [17], potassium
on bentonite [10], etc. Meanwhile, activated carbon is one of catalyst support that has been used for some process,
such as cobalt support in advance oxidation process [17] and platinum support in ortho-nitrochlorobenzene
hydrogenation process [18]. By loading potassium on activated carbon, the new heterogeneous potassium catalyst has
been introduced for transesterification reaction, namely potassium loaded on activated carbon (K/AC).
This study was focused on the biodiesel production from refined palm oil in continuous RD by using heterogeneous
K/AC catalyst. There are several process parameters which may influence transesterification process. In this paper,
the effects of various reaction temperatures and methanol-palm oil molar ratio on the reaction conversion were
investigated.
744 Yano Surya Pradana et al. / Energy Procedia 143 (2017) 742–747
Author name / Energy Procedia 00 (2017) 000–000 3

2. Experimental

2.1. Materials

Refined palm oil used in this study was produced by PT. Salim Ivomas Pratama, Tbk. (Indonesia). Meanwhile,
methanol (purity ≥ 99.8%) was purchased from PT. Brataco Chemika, Yogyakarta (Indonesia). K/AC catalysts were
also prepared from coconut-shell activated carbon in 20 to 30 mesh of particle size.

2.2. Procedures

Transesterification process using K/AC catalyst was run in a set of continuous RD as in Fig. 1. Palm oil storage
and methanol storage were filled palm oil and methanol, respectively. Heating water and cooling water flow were
turned on. Control valves of palm oil and methanol were then set the molar ratio of reactants and the liquid flow into
column. Magnetic stirrer and heater in pre-mixing process were turned on with 1000 rpm of stirring speed. Zero time
(t = 0) was started when the liquid first drop went into the upper column. Re-boiling flask was turned on and set at
68oC of temperature and 400 rpm of stirring speed. The first sample was then taken when the first product stream flow
out from reboiling flask by itself. The samples were taken in one hour interval and were then centrifuged. In this
research, the temperatures were varied at 50, 55 and 60oC, and the methanol-palm oil molar ratios were varied at 4:1,
6:1 and 8:1.

Nomenclature:
1. Palm oil storage
2. Vent
3. Palm oil “on/off” valve
4. Palm oil control valve
5. Pre-mixing condenser
6. Pre-mixing flask
7. Magnetic stirrer + heater
8. Methanol storage
9. Methanol control valve
10. Methanol “on/off” valve
11. Reactive-distillation condensor
12. Reactive-distillation column 1
13. Reactive-distillation column 2
14. Inert packing
15. Solid catalyst
16. Inert packing
17. Solid catalyst
18. Reboiling flask
19. Magnetic stirrer + heater

Fig. 1. Schematic diagram of continuous reactive distillation.

2.3. Analysis

The methyl ester produced from the transesterification process was analyzed by iodometry method to determine
the reaction conversion. Total glycerol content in biodiesel sample was measured by completely esterifying it with
 Yano Surya Pradana et al. / Energy Procedia 143 (2017) 742–747 745
4 Author name / Energy Procedia 00 (2017) 000–000

KOH and methanol. Chloroform and glacial acetic acid were added and then shaken. Distilled water was put to
separate the mixture. Periodic acid and potassium iodate were reacted with aquatic sample and it was then titrated
with sodium thiosulfate solution. As a comparison, the need of sodium thiosulfate solution was tested in distilled water
after mixing it with periodic acid and potassium iodate. Free glycerol content was measured by the same method with
total glycerol measurement without esterification step. The reaction conversion (XR) can be calculated by using
Equation 1.

xR 
G
T  GF  feed  GT  GF sample  (1)
GT  GF  feed
Where GT is total glycerol content; GF is free glycerol content.

3. Results and discussion

The effects of reaction temperature and methanol-palm oil molar ratio on the reaction conversion were analyzed in
this study.

3.1. Effect of reaction temperature

The effect of reaction temperature on the reaction conversion is shown in Fig. 2. The reaction conversions tended
to be at steady state condition. Higher reaction temperature accelerated an increase in reaction conversion. However,
reaction temperature should be limited to the boiling point of methanol to avoid the lower reaction rate caused by
vaporization. Based on these results, the RD system can be utilized for improving conversion of biodiesel production
using K/AC catalyst. Raharningrum et al. [19] reported that the maximum conversion of biodiesel production using
K/AC in batch system was 0.2271. Meanwhile, the maximum reaction conversion for the biodiesel production in
continuous RD using K/AC catalyst was obtained at 60oC in the value of 0.8269.

Fig. 2. Effect of reaction temperature on the reaction conversion.

3.2. Effect of methanol-palm oil molar ratio

Fig. 3 shows the effect of methanol-palm oil molar ratio on the reaction conversion. The values of reaction
conversion at methanol-palm oil molar ratio of 4:1 and 6:1 show significant differences. In contrast, the values of
746 Yano Surya Pradana et al. / Energy Procedia 143 (2017) 742–747
Author name / Energy Procedia 00 (2017) 000–000 5

reaction conversion at 6:1 and 8:1 show slight differences. This phenomena is caused by mass transfer of methanol
and the number of available active site on the catalyst surface as controlling factors [20]. Generally, the reaction
conversion was increase when the methanol-palm oil molar ratio was increase. The maximum reaction conversion
was 0.8394, obtained at 8:1 of methanol-palm oil molar ratio. It can be explained that the higher methanol-palm oil
molar ratio would drive the adsorption of methanol onto the catalyst surface, thus favoring the reaction [5]. Although
the highest reaction conversion was obtained at 8:1, the optimum methanol-palm oil molar ratio was 6:1 in the value
of 0.8269 of reaction conversion. The reducing methanol to 6:1 in methanol-palm oil ratio was not affected
significantly to reaction conversion.

Fig. 3. Effect of methanol-palm oil molar ratio on reaction conversion.

4. Conclusion

Biodiesel production by using continuous RD and heterogeneous catalyst has been intensively studied to solve the
problems in conventional system. From this research, the optimum reaction conversion of biodiesel production in
continuous RD using K/AC catalyst was 0.8269 obtained at 60°C of reaction temperature and 6:1 of methanol-palm
oil molar ratio. It has proven that the continuous RD posses an enhanced performance on the biodiesel production,
compared to batch reactor.

Acknowledgements

The authors would thank for the financial support for this study from the Ministry of Research, Technology and
Higher Education of the Republic of Indonesia by the research scheme of International Joint Research and Publication.
The authors are also grateful to Prof. Panut Mulyono and Dr. Ahmad Tawfiequrrahman Yuliansyah for providing
suggestions in this study.

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