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Biomass and Bioenergy 27 (2004) 477484

Catalytic conversion of palm oil-based fatty acid


mixture to liquid fuel
Yean-Sang Ooi, Ridzuan. Zakaria, Abdul Rahman Mohamed, Subhash Bhatia

School of Chemical Engineering, Universiti Sains Malaysia, Engineering Campus, 14300 Nibong Tebal, SPS Penang, Malaysia
Received 29 May 2003; received in revised form 18 March 2004; accepted 30 March 2004
Abstract
A substantial amount of fatty acid mixture residue is generated in the palm oil-based oleochemical industries in Malaysia.
The recovery of fatty acids residue is dicult and not economical; therefore, its alternative usage is explored. The fatty
acid mixture can be converted to liquid hydrocarbon fuel and chemicals using catalytic technology. In the present study, the
catalytic cracking of fatty acid mixture residue to liquid hydrocarbon fuel was studied over HZSM-5 catalyst in a xed-bed
microreactor at atmospheric pressure. The eect of reaction temperature (400450

C), fatty acid/catalyst ratio (610) and


weight hourly space velocity (2.54:5 h
1
) was studied over the yield of liquid hydrocarbon fuel. Design of experiments
was used to study the eect of operating variables over conversion of fatty acid mixture and yield of hydrocarbon fuel. The
response surface methodology was used to determine the optimum value of the operating variables for maximum conversion
of fatty acid mixture and yield of gasoline fraction in the liquid product obtained.
? 2004 Elsevier Ltd. All rights reserved.
Keywords: Biofuel; Fatty acid mixture residue; HZSM-5; Cracking; Design of experiments (DOE)
1. Introduction
Biofuel production from vegetable oils such as
canola oil [1,2] and palm oil [3,4] are currently being
studied, not only due to the depletion of fossil fuels
but also the stringent regulations on the composition
and quality of the transportation fuels. Biofuel is de-
ned as liquid or gaseous fuel that can be produced
from the utilization of biomass substrates and can
serve as a (partial) substitute for fossil fuels. Liq-
uid biofuel oers alternative fuel option in terms of

Corresponding author. Tel.: +60-4-5937788x6409; fax: +60-


4-5941013.
E-mail address: chbhatia@eng.usm.my (S. Bhatia).
environmental benets since it is free from nitrogen
and sulfur compounds [1]. With biofuel, the green
house eect and air pollution can be minimized.
Biodiesel is one of the alternative fuel produced from
vegetable oils and being used in trucks and buses in
western countries [5]. However, biodiesel can only
be used in diesel engines, and not in gasoline engine.
The direct catalytic conversion of vegetable oils
such as rapeseed oil, canola oil and palm oil to fuel do
not hold much promise since it will depend on the crop
production and the market price of oil. In Malaysia,
palm oil has been utilized not only as cooking oil
and raw material for oleochemical industries but also
in the production biodiesel [3]. The direct conversion
of edible palm oil to fuel may not be economically
0961-9534/$ - see front matter ? 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biombioe.2004.03.003
478 Y.-S. Ooi et al. / Biomass and Bioenergy 27 (2004) 477484
feasible even though the results showed the potential
of obtaining liquid hydrocarbons [3]. In the present
study, palm oil-based fatty acid mixture residue ob-
tained from oleochemical industry is used as the raw
material in catalytic conversion to fuel and chemi-
cals. The fatty acid mixture is a residue after distilla-
tion and recovery of desired fatty acids. The fatty acid
mixture residue cannot be further distilled because of
higher operating cost and low recovery. By converting
fatty acid mixture residue into fuel, a protable system
could be established to provide economic opportuni-
ties and benet the environment without competing
with the edible oil market. At the same time, the fatty
acid mixture residue would be converted to more use-
ful product, an alternative energy source in the form
of biofuel.
In the present research, catalytic cracking of fatty
acid mixture has been studied for the production of
liquid fuel. The catalytic cracking process depends on
the reaction operating condition as well as the choice
of catalyst. In order to predict the optimum operating
conditions in a process to obtain the highest yield of
desired product, a statistical approach has been used
by several researchers [68]. The benets of using
statistical approach with minimum number of experi-
ments to obtain the optimumoperating conditions have
drawn interest of the researcher for complex reactions.
Adjaye et al. [6] identied the signicant reaction con-
ditions as well as interaction factors responsible to
aect the product distribution in canola oil cracking
reaction using statistical study. Twaiq et al. [9] demon-
strated the use of design of experiments (DOE) in the
study of palm oil cracking process to optimize the sig-
nicant reaction parameters.
The objectives of the present research are (a) to
study the catalytic conversion of fatty acid mixture
to liquid hydrocarbon fuel at dierent operating con-
ditions; (b) to optimize the reaction operating condi-
tions for the production of gasoline fraction in liquid
hydrocarbon fuel using DOE and response surface
methodology.
2. Experimental
2.1. Fatty acid mixture residue
The palm oil-based fatty acid mixture residue
was obtained from Acid-Chem International Sdn
Table 1
Composition of fatty acid mixture residue
Fatty Acid Percentage
Lauric acid (C12:0) 3.23
Myristic acid (C14:0) 1.59
Palmitic acid (C16:0) 6.11
Stearic acid (C18:0) 8.25
Oleic acid (C18:1) 68.64
Linoleic acid (C18:2) 7.00
Arachidic acid (C20:0) 1.80
Eicosenoic acid (C20:1) 1.05
Behenic acid (C22:0) 0.59
Lignoceric acid (C24:0) 1.21
Others 0.53
Bhd. (Butterworth, Malaysia). It was received as
dark brown liquid, having mild smell, lighter than
water and free of water and particles. The compo-
nents of the fatty acid mixture residue were identied
by converting fatty acid mixture into methyl esters
and analyzed using GC-MS (Hewlett-Packard Model
5890 Series II/5989A). The column Supelcowax 10
(60 m long 0:25 mm ID, lm thickness 0:25 m)
was used and the temperature was programmed
from 100

C to 230

C. Table 1 shows the concen-


tration of dierent types of fatty acids present in the
mixture.
2.2. Catalyst preparation and characterization
H-ZSM-5 with Si/Al ratio of 50 was obtained from
Sud-Chemie AG, Katalyse-Labor, Munich, Germany.
HZSM-5 sample was calcined in a mue furnace
for 6 h at 600

C before it was used. The catalyst


was characterized for its acidity by temperature pro-
grammed desorption (TPD) of ammonia using Chem-
bet 3000 instrument (Quantachrome) equipped with
TPRWin, version 1 software to calculate the acid-
ity. The BET surface area and pore volume of the
catalyst were measured by nitrogen adsorption using
Autosorb I (Quantachrome Automated Gas Sorption
System). The samples were degassed for 5 h under
vacuum at 300

C prior to the analysis. The physical


and chemical characteristics of HZSM-5 are presented
in Table 2.
Y.-S. Ooi et al. / Biomass and Bioenergy 27 (2004) 477484 479
Table 2
Properties of HZSM-5 catalyst
Si/Al ratio 50
BET surface area (m
2
=g) 430
Pore size (nm) 0:54 0:56
Pore volume (cm
3
=g)
a
0.2519
Acidity (mmol NH
3
=g) 0.25
a
At P=P
0
= 0:5.
2.3. Experimental procedure
The cracking of fatty acid mixture was conducted
at atmospheric pressure in a xed-bed microreactor
(185 mm 10 mm ID) described elsewhere [3]. The
reaction temperature was in the range of 400450

C
and with a fatty acid mixture residue feed rate (weight
hourly space velocity, WHSV) of 2.54:5 h
1
while
the fatty acid mixture to catalyst ratio was varied
between 6 and 10. HZSM-5 (1:0 g) was loaded over
0:2 g of quartz wool supported with a stainless steel
mesh in the microreactor placed in the vertical tube
furnace (model no. MTF 10/25/130, Carbolite) and
the temperature was monitored by a thermocouple
positioned in the center of the catalyst bed. Nitrogen
gas was passed through the reactor for 1 h before
the fatty acid mixture was fed using a syringe pump
(Cole Parmer model no. E-74900-05). Once steady
state had reached in the reactor, the liquid product (or-
ganic and aqueous fractions) was collected in a liquid
sampler while the gaseous product was collected in a
gas-sampling bulb. The process run time of each ex-
periment varied from 2 to 4 h depending on the feed
rate and fatty acid mixture/catalyst ratio. The uncon-
verted fatty acid mixture was separated from the liquid
product in a microdistillation unit (Buchi B850, GKR)
operated at 200

C for 30 min under vacuum (5 Pa).


The residue remaining after the vacuum distillation
was termed as the residual fatty acid mixture. The
gaseous product was analyzed using HP Plot Q capil-
lary column (divinyl benzene/styrene porous polymer,
30 m long 0:53 mm ID 40 m lm thickness)
over gas chromatograph (Hewlett Packard, Model
5890 series II) equipped with thermal conductivity de-
tector (TCD). The organic liquid product (OLP) was
analyzed using a capillary glass column (Petrocol DH
50.2, lm thickness 0:5 m; 50 m long0:2 mm ID)
at a split ratio of 1:100, with a FID detector. The OLP
contains a large number of components of hydro-
carbon compounds therefore the composition of OLP
was dened according to the boiling range of three
types of petroleum products (a) gasoline fraction
(333393 K), (b) kerosene fraction (393453 K)
and (c) diesel fraction (453473 K). The spent cat-
alyst was washed with acetone prior to the coke
analysis. The amount of coke was determined by the
dierence before and after calcination in a mue
furnace.
3. Results and discussion
The important operating variables aecting the con-
version and product distribution were reaction temper-
ature, fatty acid to catalyst ratio and WHSV. Since the
gasoline fraction is the most desired product, thus the
optimumoperating conditions (independent variables)
was determined to maximize its yield (response). The
statistical method of factorial DOE eliminates the sys-
tematic errors with an estimate of the experimental
error and minimizes the number of experiments [8].
Several other responses were also considered in the
factorial design such as the conversion of fatty acid
mixture (P
C
), yield of OLP (Y
OLP
), yield of gaseous
product (Y
Gas
) and yield of gasoline fraction (Y
G
).
The eects of main process variables and their inter-
actions were assessed with specic condence level
and thus leading to a better understanding about the
process studied [10]. A 3
3
full factorial design with
three process variables where each with three levels,
namely low (1), central (0) and high level (1) was
used. Table 3 presents 3
3
full factorial design with the
operating range of each variable. The total numbers
of experiments conducted were 27 and ve experi-
ments were repeated at the central level of each factor
to estimate the experimental error. The base levels of
the factors were chosen based on a priori knowledge
[3,4,7]. Higher reaction temperature and low feed rate
would give higher yield of gaseous product while too
low reaction temperature and high feed rate would
deactivate the catalyst faster. The reaction conditions
chosen in the design of experiments and responses are
presented in Table 4. The conversion and yield are
480 Y.-S. Ooi et al. / Biomass and Bioenergy 27 (2004) 477484
Table 3
Independent variables coded and real values used in the model
Factor Factor code Unit Low level (1) Center level (0) High level (1)
Reaction temperature A

C 400 425 450
Fatty acid/catalyst ratio B g/g cat 6 8 10
WHSV C h
1
2.5 3.5 4.5
Table 4
Experimental matrix and experimental results for 3
3
factorial design
Temperature Fatty acid/catalyst WHSV Treatment combination P
C
Y
OLP
Y
G
Y
Gas
(

C) (g/g cat) (h
1
)
A B C
400 6 2.5 1 1 1 95.1 61.2 38.3 22.2
425 6 2.5 0 1 1 95.0 58.2 40.3 27.4
450 6 2.5 1 1 1 97.8 57.4 41.6 32.5
400 8 2.5 1 0 1 97.4 62.2 39.8 24.0
425 8 2.5 0 0 1 96.0 59.6 40.0 26.6
450 8 2.5 1 0 1 98.3 55.8 40.9 33.4
400 10 2.5 1 1 1 91.4 61.9 38.4 19.3
425 10 2.5 0 1 1 95.4 59.3 42.1 27.0
450 10 2.5 1 1 1 97.9 56.4 36.1 33.1
400 6 3.5 1 1 0 73.8 49.2 34.9 7.9
425 6 3.5 0 1 0 87.9 59.0 42.5 16.7
450 6 3.5 1 1 0 95.3 59.7 41.2 26.7
400 8 3.5 1 0 0 73.8 54.4 39.6 8.5
425 8 3.5 0 0 0 94.9 60.1 42.1 26.0
450 8 3.5 1 0 0 95.7 59.0 42.9 27.2
400 10 3.5 1 1 0 67.3 46.8 34.0 11.0
425 10 3.5 0 1 0 86.7 56.9 41.7 18.0
450 10 3.5 1 1 0 95.1 61.4 44.5 24.4
400 6 4.5 1 1 1 67.6 42.3 31.7 8.0
425 6 4.5 0 1 1 79.8 49.9 34.6 21.5
450 6 4.5 1 1 1 96.0 62.8 42.4 26.2
400 8 4.5 1 0 1 67.3 45.1 28.3 9.1
425 8 4.5 0 0 1 91.6 59.6 44.9 20.5
450 8 4.5 1 0 1 96.2 59.0 42.1 27.1
400 10 4.5 1 1 1 68.2 45.7 33.1 12.0
425 10 4.5 0 1 1 74.3 50.7 35.0 13.8
450 10 4.5 1 1 1 92.4 52.3 40.8 30.9
Repeated trial
425 8 3.5 0 0 0 87.9 57.7 37.6 20.3
425 8 3.5 0 0 0 93.6 61.4 45.3 17.7
425 8 3.5 0 0 0 93.5 64.0 47.6 19.0
425 8 3.5 0 0 0 91.1 64.6 41.8 15.0
425 8 3.5 0 0 0 92.2 61.6 47.1 21.7
Y.-S. Ooi et al. / Biomass and Bioenergy 27 (2004) 477484 481
dened as
Conversion (wt%)
=
[gas (g) + OLP (g) + water (g) + coke (g)]
fatty acid mixture feed(g)
100%; (1)
Yield (wt%) =
desired product (g)
fatty acid mixture feed (g)
100%; (2)
where the OLP represents organic liquid product
and the total products are the sum of products gas,
OLP, water and coke. The major components of the
gaseous products were propane, propylene, butane
and butylenes. The OLP contains liquid hydrocar-
bons, which belong to gasoline fraction, kerosene
fraction and diesel fraction, respectively. The gaso-
line fraction contains hydrocarbons rich in aromatics.
Since it is complex mixture of hydrocarbons therefore
the fraction is based on the boiling point cut rather
than the composition.
Table 4 shows that conversion of fatty acid mixture
was almost constant, which was above 90 wt% at the
feeding rate of 2:5 h
1
. These results indicated that
at low space velocity, the conversion of the fatty acid
mixture was almost independent of the fatty acid to
catalyst ratio and the reaction temperature. However,
the product distribution varied as the temperature and
fatty acid mixture to catalyst ratio were changed. The
yield of gaseous product increased with the tempera-
ture and independent of increase in fatty acid to cata-
lyst ratio, while the OLP yield decreased from 62.2 to
55:9 wt%. The increment of the gas yield was higher
than the increase in OLP yield. Once the feed rate was
increased from 2.5 to 4:5 h
1
, the conversion of the
fatty acid mixture was in the range of 6780 wt% at
lower reaction temperature (400 and 425

C). How-
ever, the yield of organic liquid product as well as the
gasoline fraction increased at the expense the yield of
gaseous product. This was possibly due to the sec-
ondary cracking reaction, which was not active at
lower reaction temperature. However, no signicant
trend in the conversion was observed when the space
velocity was increased from 2.5 to 4:5 h
1
for the re-
action temperature higher than 425

C. The eect of
space velocity was found signicant at lower reaction
temperature (400

C).
Since several variables were studied, thus the con-
ditions which signicantly aected the product distri-
bution were to be identied statistically. Therefore,
the analysis of variance (ANOVA), was performed at
95% level of condence for the designed experiments
using the Design-Expert software (version 6.0.6). The
signicance of the individual and iteration of the fac-
tors were determined by the F-values. Table 5 shows
the summary of the results obtained. It was found that
the combined eects of the three factors were negligi-
ble for all the responses considered. The reaction tem-
perature and space velocity were signicant variables
for conversion as well as the yield of all products and
should be included in the model developed. The fatty
acid mixture to catalyst ratio did not play important
role in the conversion and product distribution except
coke formation (not shown). The coke formation can
be reduced by varying the temperature and WHSV at
constant fatty acid mixture to catalyst ratio.
In order to quantify the curvature eects, the data
from the experimental results were tted to a quadratic
equation. The test of the model adequacy was done
through lack-of-t F-tests [11]. Eqs. (3)(6) were
chosen to t the data after elimination of insignicant
variables and their interactions.
Statistical model (built with the codied factors):
P
C
= 90:68 + 9:04A 1:32B 6:11C
2:59A
2
4:20B
2
+ 2:60C
2
+0:48AB + 5:96AC 0:43BC
1:76B
2
C + 0:35BC
2
; (3)
Y
OLP
= 60:57 + 3:14A 0:45B 3:66C
2:64A
2
2:76B
2
1:50C
2
0:97AB + 4:82AC 0:58BC; (4)
Y
G
= 43:39 + 3:02A 0:081B 1:36C
2:28A
2
1:84B
2
2:29C
2
0:37AB + 2:51AC + 0:32BC; (5)
Y
Gas
= 19:25 + 7:75A + 0:023B 4:25C
0:37A
2
1:17B
2
+ 4:82C
2
0:10AB + 1:81AC + 0:32BC; (6)
482 Y.-S. Ooi et al. / Biomass and Bioenergy 27 (2004) 477484
Table 5
The analysis of variance (ANOVA) for the conversion, OLP yield, gasoline fraction yield and gas yield
Source of variance Sum of squares Degree of freedom Mean square F-value P-value
Conversion, P
C
Mean 2:496 10
5
1 2:496 10
5
Linear 2446 3 815 23.8 0.0001
Quadratic 219 3 73 5.2 0.0071
Cubic 96 7 14 1.0 0.4860
Model 2974 12 248 19.4
Residual 295 20 13
Lack of t 264 15 18 2.9 0.1237
Pure error 31 5 6
Signicant model term: A; C; B
2
; AC
OLP yield, Y
OLP
Mean 1:028 10
5
1 1:028 10
5
Linear 422 3 141 5.7 0.0036
Quadratic 190 3 63 6.6 0.0024
Cubic 76 7 11 1.2 0.3542
Model 906 9 101 10.5 0.0001
Residual 211 22 10
Lack of t 178 17 10 1.6 0.3156
Pure error 33 5 7
Signicant model term: A; C; A
2
; B
2
and AC
Gasoline fraction yield,Y
G
Mean 50653 1 50,653
Linear 198 3 66 4.4 0.0121
Quadratic 160 3 53 6.4 0.0029
Cubic 6 7 1 0.07 0.9992
Model 436 9 48 5.8 0.0004
Residual 185 22 8
Lack of t 112 17 7 0.5 0.8959
Pure error 72 5 14
Signicant model term: A; AC
Gas yield, Y
Gas
Mean 14237 1 14,237
Linear 1405 3 468 35.4 0.0001
Quadratic 169 3 56 7.7 0.0011
Cubic 20 7 3 0.3 0.9401
Model 1614 9 179 24.5 0.0001
Residual 161 22 7
Lack of t 91 17 5 0.4 0.9371
Pure error 70 5 14
Signicant model term: A; C and C
2
where P
C
represents conversion of fatty acid, Y
represents product yield (Y
OLP
for OLP, Y
G
for gaso-
line fraction and Y
Gas
for gas) and the values of
A, B and C are in terms of coded factor, i.e. 1; 0
and 1. In order for a model to be reliable, the re-
sults should be predicted with reasonable accuracy
Y.-S. Ooi et al. / Biomass and Bioenergy 27 (2004) 477484 483
Actual Conversion
P
r
e
d
i
c
t
e
d

C
o
n
v
e
r
s
i
o
n
61.74
71.28
80.81
90.35
99.89
61.74 71.28 80.81 90.35 99.89
R
2
= 0.91
(a)
(b)
Actual OLP Yield
P
r
e
d
i
c
t
e
d


O
L
P

Y
i
e
l
d
42.09
47.73
53.37
59.01
64.64
42.09 47.73 53.37 59.01 64.64
R
2
= 0.81
Fig. 1. Experimental versus predicted values for (a) conversion of
fatty acid mixture; (b) organic liquid product (OLP) yield.
by the model and compared with the experimen-
tal results. A comparison between the experimental
values with the simulated values of conversion and
OLP yield from the model are presented in Fig. 1.
The values of correlation coecient for the con-
version and yield of OLP were 0.91 and 0.81, re-
spectively. Since these values are greater than 80%,
it shows a good agreement between experimental
data and predicted values [6]. Three-dimensional
plots (response surface) for the yield of gaso-
line fraction obtained from Eq. (5) are plotted in
Fig. 2. The gasoline yield was increased with the
31.9
35.1
38.2
41.3
44.4
G
a
s
o
l
i
n
e

Y
i
e
l
d
,

w
t
%
400
425
450
2.5
3.5
4.5
Temperature,
o
C WHSV, h
-1
Fig. 2. Response surface plot for gasoline fraction yield ob-
tained from the statistical model over HZSM-5 for fatty acid
mixture/catalyst ratio of 8.
decrease of WHSV at higher temperatures within
the experimental range. At WHSV between 3.5 and
4:5 h
1
, the maximum gasoline fraction yield of
44:4 wt% was achieved at temperature of 450

C.
The optimum values of reaction temperature of
440

C, fatty acid mixture to catalyst ratio 9.64 and


WHSV 3:66 h
1
were obtained for maximum yield of
OLP and gasoline fraction. An experiment was con-
ducted at these optimum conditions in order to verify
the accuracy of the model proposed. The conversion
of fatty acid mixture was 85:4 wt% as compared to
simulated value of 91:4 wt% which was 6 wt% lower.
The gasoline fraction yield was 41:5 wt% compared
to simulated value of 44:4 wt% which was 3 wt%
lower. The proposed statistical model was adequate
for predicting the conversion and products yield from
catalytic cracking of fatty acid mixture within the
experimental error (5%) and range of operating
conditions.
4. Conclusions
HZSM-5 produced an organic liquid product rich in
gasoline fraction from the catalytic cracking of palm
oil-based fatty acid mixture. The yield of dierent
484 Y.-S. Ooi et al. / Biomass and Bioenergy 27 (2004) 477484
products obtained from cracking process can be ad-
equately predicted using the response surface model.
The most important process variables aecting the
yield of gasoline fraction were reaction temperature
and WHSV. The optimum yield of gasoline fraction
was 44:4 wt% at WHSV of 3:66 h
1
, reaction tem-
perature of 440

C and fatty acid mixture to catalyst


ratio of 9.64 was obtained from DOE coupled with
response surface methodology. The fatty acid mixture
residue can be utilized to produce value added product
such as liquid fuel using catalytic technology.
Acknowledgements
The authors are thankful to Acid-Chem Inter-
national Sdn Bhd. (Butterworth, Malaysia) for provid-
ing fatty acid mixture residue. The nancial support
by the Ministry of Science, Technology and Environ-
ment, Malaysia Government, under long-term IRPA
grant (Project: 02-02-05-2184 EA005) is gratefully
acknowledged.
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