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ContentslistsavailableatScienceDirect

Chemical Engineering Research and Design

journal homepage:www.elsevier.com/locate/cherd

Biodieselproductionfromcastorplantintegrating
ethanolproductionviaabioreneryapproach
a,b,
a,c,
HamedBateni
,KeikhosroKarimi
a

DepartmentofChemicalEngineering,IsfahanUniversityofTechnology,Isfahan84156-83111,Iran
ChemicalandBiomolecularEngineeringDepartment,OhioUniversity,Athens,OH45701,UnitedStates
c
InstituteofBiotechnologyandBioengineering,IsfahanUniversityofTechnology,Isfahan84156-83111,Iran
b

article

info

abstract

Articlehistory:

Biodiesel, a promising alternative fuel, is not a completely renewable fuel, as it currently uses

Received 21 April 2015

oil-based methanol for its industrial production. Integrated biodiesel and bioethanol produc-

Received in revised form 5 August

tion in a biorenery unit can overcome this challenge together with an improved economy.

2015

In this study, castor plant was applied to an integrated biodiesel and ethanol production.

Accepted 17 August 2015

The extracted oil was transesteried with ethanol produced through simultaneous saccha-

Available online xxx

rication and fermentation of the castor plant residue. An alkaline pretreatment using 8%

w/v sodium hydroxide at 100 C

for 60min was applied to improve the ethanol produc-

Keywords:

tion yield from 27.2 to 71.0%. An experimental design using response surface methodology

Castor plant

(RSM) was used to optimize the biodiesel production yield. The optimum biodiesel yield was

Biodiesel

85.0 1.0%, obtained at 62.5

C using an ethanol to oil mass ratio of 0.29:1 for 3.46h, which

Ethanol

was in agreement with the predicted yield (84.4%). Accordingly, 1kg of castor plant resulted

Alkali pretreatment

in production of 149.6 g biodiesel and at least 30.1 g ethanol as the nal products with no

Integrated process

extra alcohol feedstock requirement.

2015 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1.

Introduction

(Ng and Sadhukhan, 2011; Martine z -Hern ande z et al., 2014).

Therefore, biodiesel production using bioethanol results in
a completely renewable biofuel (Lam and Lee, 2011). Global
Biodiesel has attracted a great deal of attention over the
biodiesel and ethanol production were about 25 and 87 billast few decades due to its environmental compatibility and
biodegradability (Aarthy et al., 2014; Reyero et al., 2014). Trans-lion liter s in 2 010, respectively, predicted to correspondingly
esterication of triglycerides u sing methanol in the presence incr ease to over 58 and 161 billion liters by 2020 (Pinto,
2011). According to the U.S. Department of Energy, ethanol,
of an alkaline catalyst is the most common process for
biodiesel production (Haigh et al., 2014; Perdomo et al., 2014). biodiesel, and regular diesel prices were around $0.42, $1.06,
Ethanol can be used as a harmless substitute for methanol in and $0.82 pe r liter at the beginning of 2015, demonstrating
that biodiesel still cannot compete with diesel in the martransesterication reaction besides its individual application
ket (U.S. Department of Energy, 2015). Over 70% of biodiesel
as a renewable alternative fuel. Furthermore, ethanol is procost is c orrelated to oil f eedstock which can be vegetable
duced through the fermentation of renewable biomass while
oil (edible or non-edible), waste cooking oil, or animal fat
methanol is industrially produced from fossil fuel sources.
(Dias et al., 2013). The use of inexpensive non-edible oil, as
However, the production of methanol from biomass with an
a second generation feedstock, not only is economically more
integrated biorenery prospective has been widely studied

Correspondingauthorat :ChemicalandBiomolecularEngineeringDepartment,OhioUniversity,Athens,OH45701,UnitedStates.
Tel.: +1 7405925650; fax: +1 7405930873.

Corresponding author at : Ins titute of Biotechnology an d Bioengineering, Isf ahan Univer sity of Technology , Isfahan 84156-83111, Iran.
Tel.: +98 3113915623; fax: +98 3113912677.
E-mail addresses: hamed.bateni@gmail.com, hb683413@ohio.edu (H. Bateni), karimi@cc.iut.ac.ir (K. Karimi).
http://dx.doi.org/10.1016/j.cherd.2015.08.014
0263-8762/ 2015 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

Please cite this article in press as: Bateni, H., Karimi, K., Biodiesel production from castor plant integrating ethanol production via a biorenery
approach. Chem. Eng. Res. Des. (2015), http://dx.doi.org/10.1016/j.cherd.2015.08.014

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The d evelopment of biof uels production is still limited due

to lack of economic prociency (Zhu and Zhuang, 2012; Karimi
and Pandey, 2014). Biorenery, which is a facility with inteANOVA analysis of variance
grated, efcient and exible biomass processing to various
CCD
central composite design
value-ad ded products and energy , can suppress the ecoGC
gas chromatograph
nomic barriers and lead to the procient biofuel production
HPLC
high performance liquid chromatograph
(Sadhukhan et al., 2014; Luo et al., 2010; Zhu et al., 2014). The
RSM
response surface methodology
concept of biorenery was deve loped analogous to the curSEM
scanning electron microscopy
rent complex crude oil reneries leading to multiple fuels and
SSF
simultaneous saccharication and fermentavalue-added chemicals (Sadhukhan et al., 2014).
tion
Castor plant is an important non-edible oilseed crop which
can toler ate various climate condi tions (humid tropic to
dry subtropic) and has a wide range industrial a pplications
favorable but also can reduce food versus fuel conict (Bateni (Ramanj aneyu lu et al., 2013). Currently, the average global caset al., 2014). However, precise planning and management are tor se ed production yield is about 1.1t/ha (Scholz and da Silva,
2008) with a productivity of 470 kg oil/ha considering seed oil
needed to identify and minimize further challenges toward
contents in a range of 4555% (Santana et al., 2010). Castor
sustainable development of biodiesel production (Sukkasi
et al., 2010). In fact, it should be considered that cultivation of plant cul tivation under f avorable conditions can boost the
non-edible oil cr op may be associated with using arable lan d seed yield to 45t/ha, leading to promising oil productivity
(Scholz and da Silva, 2008).
and consequently increasing load on soil, water and biodiCastor oil consists mainly of ricinoleic acid (12-hydroxyversity (Antizar-Ladislao and Turrion-Gomez, 2008). However,
cis-o ctadec-9-enoic acid), an hydroxylated fatty acid with one
some of the non-edible plants, e.g., castor oil plant, can be
double bond. Th e presence of ricin oleic acid in castor oil
cultivate d in the wastelands irrigated by w astewater which
can suppress the aforementioned challenges (Chakrabarti and results in some unique prop erties, e.g., very high solubility in
alcohol (Perdomo et al., 2013). Therefore castor oi l can be conAhmad, 2008; Tsoutsos et al., 2013).
verted to biodiesel (Klc et al., 2013; Perdomo et al., 2013) even
Ethanol is industrially produced from sugar and starch
at low te mperature (Bateni et al., 2014). Castor biodiesel has
based materials; however, it can be produced from inexa hi gh caloric value and high cetane number (Scholz and da
pensive and abundant l ignocellulosic substrates such as
Silva, 2008). Howeve r , some properties of the nal biodiesel,
agriculturalresidue,forestresidue,and municipal solid wastes
e.g., high kinematic viscosity, may complicate its engine per(Du et al., 2009; Karimi et al., 2013; Misailidis et al., 2009).
Lignocell uloses are dominantly composed of cellulose , along form ance (Berman et al., 2011; Scholz and da Silva, 2008).
Castor b iodiesel can be dilu ted or blended with conventional
with he micell ulose and lignin in a highly compact structure
(Karimi and Chisti, 2015; Karimi and Pandey,2014; Karimi et al., diesel to produce an appropriate fuel for diesel motors (Scholz
2013).Therefore, a pretreatment process is required to remove and da Silva, 2008).
The presence of ricinoleic acid in the castor seed cake
lignin and hemicell ulose and increase the accessibility o f the
results in a more limited application compared to the other
enzyme to cellulose prior to the hydrolysis and fermentation
processes (Asgher et al., 2014; Bateni et al., 2014). Alkaline pre-seed cakes. Castor seed cake can be use d for production of
organic nitrogenous fertilizer due to their nitrogen, phostreatment is one of the most promising chemical processes
which can effectively facilitate further processes. Alkaline pre- phorous and potassium content (Ramachandr an et al., 2007).
How ever, it cannot be directly used for animal feed du e to
treatment using sodium hydroxide was frequently ap plied for
softwoo ds, hardwoods, and agricultu r al residues to improve the p oisenous and allergic properties (Ogunniyi, 2006; Adedeji
ethanol yield and showed promising results (Goshadrou et al., et a l., 2006). Previous study (Bateni et al., 2014) showed the
2011; Mirahmadi et al., 2010; Mohsenzadeh et al., 2011; Nievesgreat potential of castor seed cake for biogas production.
Previous studies have investigated the inuence of reacet al., 2011; Salehi et al., 2012; Salehian and Karimi, 2013).
tion parameters incl uding temperature , reaction time , catalys t
Sodium hydroxide pretreatment resulted in lignin removal,
biomass swelling, more surface reacti v e functional groups likeconc entr ation, and alcohol content on transesterication of
hydroxyl grou ps, and surface roughness improvement in the castor o il (Ca v alcante et al., 2010; Da Silva et al., 2006; De
Oliveira et al., 2005; Jeong and Park, 2009; Ramezani et al.,
pretreated substrate (Islam et al., 2012; Teghammar et al.,
2010). De Oliveira et al. (2005) used the Taguchi e xperimen2010). Although alkaline pretreatment, e.g., NaOH pretreatment, is associated with high alkali loading an d a large volume tal desig n to evaluate the effect of reaction conditions on
commercial rened castor oil. They (De Oliveira et al.,
of waste water for washing, it received great interest since it

C)
does not need complicated reactors (Wan et al., 2011). Sodium 2005) deduced that increasing reaction temperature (3070
hydroxide pretreatment are classied into dilute and concen- and time (13 h) positively affected the reaction conversion,
whereas increasing catalyst concentration (0.51.5 w/w%)
trated treatments. High concentration of sodium hydroxide
yielded a negative effect. In addition, it was conclud ed that
is applied at moderate conditions, i.e., ambient pressure and
increasi ng the a lcohol concentration had no signicant effect
relatively low temperatures. Dissolution of cellulose at these
on the conversion (De Oliveira et al., 2005). Da Silva et al.
conditions is the main phenomenon, resulting in changing
cellulose I (c rystalline cellulose ) to amorphous cellulose with (2006) used response surface methodology to optimize the
low degree of polymerization amenable to enzymatic hydroly- transestrication parameters of a commercial castor oil.
sis (Karimi et al., 2013). Moreover, high concentration sodium Optimum results were achieved with the lowest tem perature and the h i ghest alcohol concentra tion in the presence of
hydroxide provides an opportunity to recover and reuse the
pretreat ment solution, resulting in lower chemical waste dis - 0.81.3 w/w% sodium methoxide as a catalyst (Da Silva et al.,
2006). Ramezani et al. (2010) evaluated the potential of difposal and consequently less environmental concerns (Karimi
ferent basic catalysts (NaOCH3 , KOCH3 , NaOH, KOH) together
et al., 2013; Mirahmadi et al., 2010; Wan et al., 2011).
Nomenclature

Please cite this article in press as: Bateni, H., Karimi, K., Biodiesel production from castor plant integrating ethanol production via a biorenery
approach. Chem. Eng. Res. Des. (2015), http://dx.doi.org/10.1016/j.cherd.2015.08.014

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with different reaction conditions to optimize the methyl ester

synthesis from rened castor oil. The optimum b iodiesel
yield wa s obt ained at 65 C using 8:1 alcohol to o il molar
ratio after 2h in the presence of 0.5% KOCH
3 (Ramezani et al.,
2010). On the other hand, Dias et al. (2013) used raw castor
oil for biodiesel production and evaluated the effects of time
and temperature on the conversion using a central composite
experimental design in the presence of a 6:1 methanol to oil
molar ratio and 1% w/w KOH. The highest yield of 73.62 w/w%

and purity of 83.41 w/w% appeared at 65

C for 8h.
Although many research studies have been carried out on
the biodiesel production from castor oil using ethanol, to the
best of our knowledge, none of them used the ethanol produced from the castor plant residues to covert the raw castor
oil to biodiesel using a biorening approach. Within this context, this study seeks to evaluate the potential of castor plant
for biodiesel production with no external alcohol requirement via an integrated process leading to ethanol production
as a byproduct. Alkaline pretreatment using 8% w/v sodium
hydroxide was used to improve the ethanol production yield.
Further optimization was performed using response surface
methodology (RSM) to get the best biodiesel yield due to the
lack of agreement in the literature for the optimum conditions
of castor oil transesterication.

consisted of holding at an initial temperature of 150 C for

3min , increasing the temperature to 210 C with a 5 C/min

ramp, holding for 6min, increasing to 240 C at

a rate of
5 C/min, and holding for 10min. The temperatures of injector and detector were set at 230 and 250 C, respectively.
The fatty acid methyl esters (FAMEs) were prepared through
the methylation reaction with 0.5N sodium methoxide.
The FAMEs content was calculated by a calibration curve
considering the peak area.
The extractive content and the composition (carbohydrates
and lign in content) of the untreated and p retreated castor
residues were measured using a NREL/TP-510-42618 (Sluiter
et al., 2008) and NREL/TP-510-42619 (Sluiter et al., 2005) methods, respectively.
A high-performance liquid chromatograph (HPLC)
equipped with UV/Vis (Jasco International Co., Tokyo, Japan)
and an ion-exchange Aminex HPX-87P column (Bio-Rad,
USA) at 85C was employed to measure the sugar content for
carbohydrate analysis. Deionized water with a ow rate of
0.6mL/min was used as a mobile phase.
Scanning electron microscopy (SEM, ZEISS, Germany) was
performed at 15kV to investigate the effect of pretreatment
on the surface. The substrates were coated with gold (BAL-TEC
SCD 005, Leica Microsystems, USA) before SEM analysis.

2.

Experimental

2.2.

2.1.

Feedpreparation

Ethanolproduction

Simultaneous saccharication and fermentation (SSF) processes were conducted at 37 C and 130rpm under anaerobic
conditions for 96h in 2.5L glass bottles. A occulating strain
The castor plant was collected from land in Isfahan, Iran. All
of Saccharomyces cerevisiae (CCUG 53310, Culture Collection
parts of the plant were dried using an oven at 35 C for 96h,
and the castor seeds were then separated and dried in an oven of Gothenburg University, Sweden) was used as a fermentat 70C for an extra 24h . Casto r oil was extracted by Soxhlet ing microorganism. Fermentation media were prepared using
5g/L yeast extract, 3.5 g/L (NH 4) 2SO 4, 0.75 g/L MgSO 47H2O,
extractor using n -hexane through the method presented by
1g/L CaCl22H2O, and 50g/L substrates in 50mM buffer citrate.
Perdomo et al. (2013) for 8h. The solvent was then recovThe mixture pH was adjusted to 5, poured into the fermentaered by a vacuum rotary evaporator. Thereafter, the castor
tion bottle, and autoclaved at 121 C for 20min. After cooling
residues, i.e., the ste m, seed cake , and le aves, were milled and
screened to achieve a uniform substrate size within a range of the suspension to roomtemperature,1g/L S. cerevisiae together
with 15 F PU cellulase and 30 IU
-glucosidase per gram of sub0.10.8mm (Bateni et al., 2014).
strates (based on dry weight) were added to the fermenter
2.1.1. Alkalinepretreatment
(Bateni et al., 2014). The ethanol production yield was calcuAlkaline pretreatment using 8% w/v NaOH solution at 100C
lated using the following equation (Salehian and Karimi, 2013):
for 60min was used as an effective pretreatment method p rior
to ethan ol pro duction. The pretreatment involves the followProduced ethanol (g/ L)
ing steps but the details can be found elsewhere (Bateni et al., Ethanol yield (%) =
1.111
0.51 50 (g/ L) glucan (%)
2014):
100
(1)
1. The residues were mixed with 8% (w/v) sodium hydroxide
Ethanol production was conducted using untreated and presolution.
treated castor plant residue to conrm the ethanol yield
2. The slurry was placed in a bath at 100 C and periodically
improvement. The produced ethanol was puried using three
mixed.
sequence distillation steps followed by a dehydration step by
3. After 60min, the suspension was ltered and rinsed with
SigmaAldrich). An HPLC equipped with
molecular sieves (4A,
distilled water until neutral pH.
UV/Vis
(Jasco
International
Co., Tokyo, Japan) and an Aminex
4. The washed substrate was dried using a freeze dryer
HPX-87H column (Bio-Rad, USA) at 60 C was used to analyze
(Christ, Alpha 1-2 LDplus Model, Germany) and kept in
the SSF samples for determination of ethanol content. Sulfuresealable bags until use.
ric acid (5mM) with a ow rate of 0.6mL/min was used as an
eluent.
2.1.2. Feedcharacterization
A gas chromatograph (GC) equipped with a ame ionization
detector (Beijing Beifen-Ruili, Series Sp-3420A, China) and
2.3.
Biodieselproduction
a capillary column (60m 0.25mm 0.25 m, SolGel-WAX,
SGE, UK) was used to determine the fatty acid composition of
Prior to t he transest erication reaction, castor oil was rst lthe castor oil. Pure nitrogen gas with a ow rate of 30mL/min tered by an 80 mesh sieve to remove the solid particles (Bateni
was applied as a carrier gas. The GC temperature program
et al., 2014) and then preheated at80 C for 60min to eliminate
Please cite this article in press as: Bateni, H., Karimi, K., Biodiesel production from castor plant integrating ethanol production via a biorenery
approach. Chem. Eng. Res. Des. (2015), http://dx.doi.org/10.1016/j.cherd.2015.08.014

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Table1Experimentalconditionsforthesurface
responseanalysis.
Levels

1
0
1

Temperature ( C)

X1

X2

1
3
5

50
60
70

(2015)

xxxxxx

Table2Characteristicsofextractedcastoroil.
Properties/components

Factors
Time (h)

xxx

Ethanol to oil
mass ratio
X3
0.2
0.3
0.4

Properties
Viscosity
Free fatty acid
Components
Ricinoleic acid
Linoleic acid
Linolenic acid
Oleic acid

Content
236.7 1.4mm 2/s
1.0 0.3%
89.2 1.2%
4.7 0.7%
3.8 0.5%
0.4 0.2%

2.5.
Costestimation
the extra moisture (Berman et al., 2011). A 500 mL jacketed
batch reactor equipped with a condenser and mechanical
Final et hanol and b iod iesel costs were rou ghly estimated
mixer was used for biodiesel production. Ethanol produced in
according to the economic evaluations performed by Shaei
the previous step was applied to the transesterication reaction inthe presence of 1% w/w KOH. Theeffects of temperature et al. (2011) and Santana et al. (2010), respectively. The NMMO
(5070 C), time (15 h), and ethanol to oil mass ratio (0.20.4) was replaced with 8% NaOH solution in Shaei et al. (2011)
study as the ethanol production yield was very close to
on the biodiesel yield were evaluated. The range s of reaction
the present study. It was assumed that castor residue and
parameters were selected according to the previous studies
considering an economic point of view (Dias et al., 2013). Th e spruc e wood has approximately the same price. In the case
product was le ft in a separation funnel overnight to separate of biodiesel production, ethano l content was consid ered as a
biodiesel (upper phase) from glycerol (lower phase) (Klc et al.,dominant factor on the biodiesel price. Therefore, the amount
2013). Next, the biodiesel was was hed with hot distilled water . and price of ethanol in Santana et al. (2010) study was replaced
by the optimum ethanol content and estimated ethanol price
The yield was determined using the following equation based
on dehydrated biodiesel (Bateni et al., 2014; Klc et al., 2013): of the current study, respectively. The effects of other parameters were neglected in the biodiesel price estimation.
Biodiesel yield (%)=

Produced biodiesel (g)

100
Raw oil (g)

(2)

3.

Resultsanddiscussion

Further characterizations were performed on the sample

3.1.
Rawmaterialcharacterization
with the hi ghest yield. Free fatty acid content of the sample
oil and biodiesel were measured using the method presented
The extracted oil, whi ch repre sented 17.6% w/w of the whole
by Sadasivam and Manickam (2005). Flash point, kinematic
dried castor plant, dominantly consisted of ricinoleic acid
viscosity, free glyc erin, and water and sediment content were (89.2 1.2%). Table 2 exhibits other castor oil characteristics.
measured, and the results were compared to the standard
Extractive, carbohydrate, and lignin con t ent of c astor plant
values in A STM D6751 (2003). The heating value (heat of com- residue were measured before and after the pretreatment,
bustion) was measured using the standard method presented
and the results are presented in Fig. 1. The pretreatment
in ASTM D240 (2003).
reduced the ethanol extractive of the residue from 7.4 0.3
to 4.5 0.1%; however, its effect on the water extractive content was not signicant. A relatively high ethanol extractive
2.4.
Experimentaldesign
content of castor residue indicated the presence of remaining
oil in the seed cake. Alkaline solution (the liquid fraction of
A response surface methodology (RSM) using Minitab 16 was
employed to evaluate the inuence of reaction parameters on the pretreatment process) was an appropriate medium for a
saponication reaction betweenthe remaining oil inthe castor
the biodiesel yield. The experimental design for the reaction
was carried out using a central composite design (CCD) with
three factors, three levels, and six central point repetition. The
value of (alpha) was limited at level 1; therefore, the low est
and highest levels are assigned to be1 and +1, respectively.
The experimental design factors are presented in Table 1.
A general second order polynomial equation was used to
t a correlation between the response (biodiesel yield) and the
independent variables:
k

Y = a+

i=1

ci Xi2 +

bi Xi +
i=1

dijX iX j

(3)

i=1 j>1

where Y is the response, a i , b

are intercept,
d
linear,
i , c ,ijand
quadratic, and interaction constant coefcient, respectively;
k is the number of factors studied and optimized in the
experiment; Xi and Xj are the independent variables. Reaction temperature, time, and ethanol to oil mass ratio were the
independent variables in this study.

Fig.1 Composition ofcastorplantresiduebefore(dark

graybars)andafter(lightgraybars)alkalinepretreatment

using8%(w/v)sodiumhydroxideat 100
Cfor60min.

Please cite this article in press as: Bateni, H., Karimi, K., Biodiesel production from castor plant integrating ethanol production via a biorenery
approach. Chem. Eng. Res. Des. (2015), http://dx.doi.org/10.1016/j.cherd.2015.08.014

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Fig.2 SEMimagesofcastorplantresiduebeforeandafterpretreatmentusing8%(w/v)sodiumhydroxideat 100

Cfor
60min.

residues and sodium hydroxide. A reduction in th e ethanol

81.1 1.6g ethanol (82.2 g with the purity of 98.7%) per kg
extractive content of the pretreated castor residue reected
castor. According to the previous study (Bateni et al., 2014),
the progress of the saponication reaction (Bateni et al., 2014). around 86g ethanol per each kg castor plant was expected,
Cellulose was the dominant carbohydrate in the plant
this means around 7.59.7% ethanol was lost through the
residue, and the pretreatment boosted its content from
glassware equipment during the distillation process. Puried
31.2 0.3 to 44.2 0.2%. Moreover, the li gnin c ontent of the
ethanol was used to investigate the effect of temperature,
residue decreased from 39.2 0.6 to 32.7 0.4% after the
time, and alcohol content on the transesterication yield in
sodium hydroxide pretreatment. Fig. 2 shows the SEM images the presence of 1% KOH.
of the castor residue before and after the pretreatment. A compact structure with a negligible porosity was observed for the
untreated castor residue, while the alkaline pretreatment sig- 3.3.
Biodieselproduction
nicantly opened up the structure and created a sponge-like
shape su bstrate . Higher por osity of the castor residues pro- The experimental design matrix and results are presented
vided a more accessible area for further microbial process
in Table 3. The rst three columns of the factors are coordi(Karimi et al., 2013).
nated to dimensionless (coded) levels of the factors and the
next three columns give the factor levels on a natural scale
(uncoded).
3.2.
Ethanolcharacterization
A quadratic polynomial equation was obtained from the
experimental design and data analysis, and the following
Ethanol was produced using a simultaneous saccharication
equation was obtained to predict the biodiesel yield in terms
and fermentation of the untreated and pretreated castor
of the uncoded factors:
plant residue. The pretreatment increased the ethanol
production yield from 27.2 to 71.0%. The purity of ethanol
produced from the pretreated residue was increased from
Y = 338.146+ 54.167t + 9.837T + 147.290R 5.486t2
8.9 1.1 to 75.5 0.8% after three sequenced distillation
0.072T2 189.545R2 0.218tT 8.937tR + 0.088TR (4)
steps. Further dehydration by molecular sieves resulted in
Table3Experimentalmatrixofthreefactorsinthreelevelsandtheresults.
Run order

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Coded factors

Uncoded factors

Biodiesel yield (%)

X1

X2

X3

t (h)

T ( C)

1
1
1
1
1
1
1
1
1
1
0
0
0
0
0
0
0
0
0
0

1
1
1
1
1
1
1
1
0
0
1
1
0
0
0
0
0
0
0
0

1
1
1
1
1
1
1
1
0
0
0
0
1
1
0
0
0
0
0
0

1
5
1
5
1
5
1
5
1
5
3
3
3
3
3
3
3
3
3
3

50
50
70
70
50
50
70
70
60
60
50
70
60
60
60
60
60
60
60
60

0.2
0.2
0.2
0.2
0.4
0.4
0.4
0.4
0.3
0.3
0.3
0.3
0.2
0.4
0.3
0.3
0.3
0.3
0.3
0.3

29.7
62.7
47.1
63.9
34.1
61.2
52.4
60.8
48.7
73.0
70.7
80.4
82.7
79.1
81.9
81.5
82.1
82.4
84.0
83.1

X1 , t :time; X2 , T :temperature;3X , R :ethanoltooilmassratio.

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Table4Analysisofvarianceforresponsesurfacequadraticmodel.
Source
Regression
Linear
Square
Interaction
Residual error
Lack-of-t
Pure error
Total

Degree of freedom

Sum of squares

9
3
3
3
10
5
5
19

5567.23
1414.88
3974.47
177.87
18.39
14.25
4.14
5585.62

Mean square
618.58
642.11
1324.82
59.29
1.84
2.85
0.83

F -value

P -value

336.40
349.2
720.48
32.24

0.000
0.000
0.000
0.000

3.44

0.101

2
2
S =1.35603;2R =99.67%;
R (pred)=97.72%;
R (adj)=99.37%.

where Y , R , T , and t are the biodiesel yield (%), ethanol to oil

reaction (Lam and Lee, 2011). The same results were reported
mass ratio, temperature( C), and time (h), respectively. Analy- in pr evious studies (Bateni et al., 2014; Leung et al., 2010).
sis of variance (ANOVA) was used to evaluate the adequacy of
Higher alcohol content is favorable in the transestericathe empirical mod el, and the results are presented in Table 4. tion process since it can facilitate triglyceride conversion to
The model was also validated using four sets of data, premonoglycerides. However, monoglyceride can increase glycsented in Fig. 3. As can be seen, the model agreed well w ith
erol solubility in the biodiesel, which not only make s the
the experimental results. The RSM t and parameter estimaseparati on process more challe nging but also results in glyctions for the empirical model are summarized in Table 5. The
erolysis reaction leading back to triglyceride (Lam and Lee,
ANOVA results indicate a statistically signicant correlation
2011; Silva et al., 2011).
between the biodiesel yield and the three factors studied with
The con tour p l ots for the predicted values of the biodiesel
a condence level of 95%. The P -values and T -values were used
yield as a function of the reaction parameters are presented
to checkthe signicance ofthe corresponding coefcients. The in Fig. 4. Fig. 4a shows the contour plot as a function of time
larger magnitude of the T -values and smaller P -value repre- and temperature at a 0.3:1 ethanol to oil mass ratio. Fig. 4b
sent the higher signicance of the corresponding coefcient.
represen ts the contour plot as a function of temperature and
Accordingly, all factors (except the corresponding parameter
ethanol to oil mass ratio for a 3h transesterication reaction.
to the temperature and ethanol content ( T R ) interaction) were Fig. 4c displays the predicted response values as a function of
shown to ha vea sign icant effect. Moreover,the lack-of-t was time and ethanol to oil mass ratio at a temperature of 60C.
insignicant due to the relatively high P -value (0.101).
According to the experimental design results, the potential

Table 5 shows that the rst-order (linear) parameters had

optimum biodiesel yield was 84.4% at 62.5
C using ethanol to
a positive effect on the yield; however, all the interactions can oil mass ratio of 0.29:1 for 3.46h. The predicted biodiesel yield
1.0%.
negatively affect the yield. Moreover, all of the second-order
was in agreement with the practical yield of 85.0
(quadratic) coefcients are negative, resulting in a reduction
The presence of water in the ethanol ( 1.3%) might be
in the response (biodiesel yield) at very high values for the
anot her barrier for higher biodiesel production yield; however,
reaction parameters. Ve r y high reactio n temperatures acceler-the best production yield (85.0%) is still in an acceptable range
ate both transesterication and saponication reaction (Leung compared to the previous study on the transesterication of
et al., 201 0; Silva et al., 2011), which not only led to ester and raw castor oil using ethanol (Dias et al., 2013).
fatty acids lost but also complicated the separation process
Further characterizations were performed o n the optimum
(Snchez et al., 2015).
biodiesel, and the results are presented in Table 6. Accordingly,
Besides the temperature, reaction duration showed a sigall the measured properties met the ASTM D6571 standard
nicant effect on the biodiesel production yield. Similarly, a
except the viscosity, which was three times greater than the
marked increase in the reaction duration resulted in a reducmaximum standard amount.
tion in the biodiesel yield, probably due to saponication

3.4.

Massbalanceandeconomicestimations

Under optimum conditions, 149.6 1.4g biodiesel/kg castor plant was produced, consuming around 51.0 g ethanol.

Table5TheRSMtandparameterestimations.
Term

Fig.3 Comparisonbetw ee ntheexperimentalbiodiesel

yieldandthepredictedyieldby theempiricalmodel
describedinEq.(4).

Constant
t
T
R
t2
T2
R2
tT
tR
TR

Coefcient
338.146
54.167
9.837
147.290
5.486
0.072
189.545
0.218
8.937
0.088

Standard error
28.4538
2.0338
0.9953
57.4868
0.2044
0.0082
81.7715
0.0240
2.3971
0.4794

T -value

P -value

11.884
26.634
9.884
2.562
26.838
8.861
2.318
9.099
3.728
0.183

0.000
0.000
0.000
0.028
0.000
0.000
0.043
0.000
0.004
0.859

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Fig.4 Contourplotsofbiodieselyieldasafunctionof:(a)temperatureandtimeforthereactionusing0.3:1ethanoltooil
massratio,(b)temperatureandethanoltooilmassratiofor3hreaction,and(c)ofethanoltooilmassratioandtimeforthe

reactionat 60
C(allinthepresenceof1%KOHascatalyst).
subsequently improve the ethanol production. The integrated
castor plant processing for biodiesel and ethanol production
has both economic and environmental benets. However, a
Properties
Biodiesel sample
ASTM D6751
precise investigation is needed for waste treatment and recovFlash point ( C)
156 3
130(min)
ery units of the biorenery plant.
Kinematic viscosity (mm2/s)
18.1 0.3
1.96.0
The empirical model developed for biodiesel production
Free glycerin (%)
0.010 0.01
0.020
was in a good agreement with the experimental results. HowWater and sediment (%)
0.02 0.02
0.050
ever, a wide range of experimental data can be used to evaluate
Heating value (MJ/kg)
33.4 2.6

and readjust the parameters to get a better model.

A rough estimate based on optimum results of the current
study showed that integrated ethanol and biodiesel producTherefore, 30.1 g ethanol/kg cas tor plant is produced as a
tion through the proposed technology cost around $0.35/L
value-added byproduct of the process.
Santana et al. (2010) estimated the castor biodiesel cost for and $1.47/kg, respectively. However, further detailed technoa plant with a capacity of 1000kg/h castor oil, where 591.3kg/h economical investigation is necessary to determine a more
ethanol was used. They estimated the nal cost of biodiesel at accurate estimation about the feasibility of the technology and
about $1.52 per kg biodiesel, considering the price of castor oil economic details.
3
and ethanol for $1157/ton and $354.21/m
, respectively. However, according to the current optimum conditions, the best
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