Catalytic Hydro Processing of Cottonseed Oil in Petroleum Diesel Mixtures - 2

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{\phpg\posx5316\pvpg\posy952\absw1467\absh114 \f20 \fs12 \cf0 \f20 \fs12 \cf0 Fuel
88 (2009) 145-149 \par
}
{\phpg\posx3762\pvpg\posy1482\absw4635\absh1136 \f10 \fs15 \cf0 \fi808 \f10
\fs15 \cf0 Contents lists available at{\cf2 ScienceDirect }
\par}{\phpg\posx3762\pvpg\posy1482\absw4635\absh1136 \sl-284 \par\f10 \fs15 \cf0
\fi2036 {\f20 \fs26 Fuel }
journal homepage: www.elsevier.com/locate/fuel \par
}
{\phpg\posx850\pvpg\posy3545\absw9135\absh981 \f20 \fs25 \cf0 \f20 \fs25 \cf0
Catalytic hydroprocessing of cottonseed oil in petroleum diesel mixtures
\par}{\phpg\posx850\pvpg\posy3545\absw9135\absh981 \sl-344 \f20 \fs25 \cf0 for
production of renewable diesel
{\fs20 I.}{\fs20 Sebos}{\up006 \fs13 a}{\fs20 ,}{\fs20 A.}{\fs20 Matsoukas}
{\up006 \fs13 a}{\fs20 ,}{\fs20 V.}{\fs20 Apostolopoulos}{\up006 \fs13 b}{\fs20
,}{\fs20 N.}{\fs20 Papayannakos}{\up006 \fs13 a,}{\dn006 \fs13 * }\par
}
{\phpg\posx850\pvpg\posy4727\absw7568\absh293 \f20 \fs8 \cf0 \f20 \fs8 \cf0 a{\fs12
National}{\fs12 Technical}{\fs12 University}{\fs12 of}{\fs12 Athens,}{\fs12
School}{\fs12 of}{\fs12 Chemical}{\fs12 Engineering,}{\fs12 Heroon}{\fs12
Polytechniou}{\fs12 9,}{\fs12 Zografos,}{\fs12 157}{\fs12 80}{\fs12
Athens,}{\fs12 Greece }
\par}{\phpg\posx850\pvpg\posy4727\absw7568\absh293 \sl-171 \f20 \fs8 \cf0 {\up006
b}{\fs12 MOTOR}{\fs12 OIL}{\fs12 (Hellas),}{\fs12 Corinth}{\fs12
Refineries}{\fs12 SA,}{\fs12 201}{\fs12 00}{\fs12 Corinth,}{\fs12
Greece }\par
}
{\phpg\posx850\pvpg\posy5533\absw1083\absh456 \f20 \fs17 \cf0 \f20 \fs17 \cf0 a r
t i c l e
{\fs12 Article}{\fs12 history: }\par
}
{\phpg\posx2130\pvpg\posy5533\absw606\absh221 \f20 \fs17 \cf0 \f20 \fs17 \cf0 i n
f o \par
}
Received 11 January 2008
\par}{\phpg\posx850\pvpg\posy6085\absw2324\absh577 \sl-171 \f20 \fs12 \cf0 Received
in revised form 29 July 2008
\par}{\phpg\posx850\pvpg\posy6085\absw2324\absh577 \sl-171 \f20 \fs12 \cf0 Accepted
31 July 2008
\par}{\phpg\posx850\pvpg\posy6085\absw2324\absh577 \sl-171 \f20 \fs12 \cf0
Available online 24 August 2008 \par
}
{\phpg\posx4141\pvpg\posy5539\absw7109\absh1679 \f20 \fs17 \cf0 \f20 \fs17 \cf0 a
b s t r a c t
{\fs13 The}{\fs13 conversion}{\fs13 of}{\fs13 the}{\fs13 esters}{\fs13
included}{\fs13 in}{\fs13 refined}{\fs13 cottonseed}{\fs13 oil}{\fs13
into}{\fs13 hydrocarbon}{\fs13 molecules}{\fs13 compatible }
\par}{\phpg\posx4141\pvpg\posy5539\absw7109\absh1679 \sl-191 \f20 \fs17 \cf0 {\fs13
with}{\fs13 petroleum}{\fs13 diesel,}{\fs13 which}{\fs13 are}{\fs13
named}{\fs13 renewable}{\fs13 diesel,}{\fs13 has}{\fs13 been}{\fs13
studied}{\fs13 at}{\fs13 conventional}{\fs13 hydrotreat- }
ment}{\fs13 conditions.}{\fs13 The}{\fs13 vegetable}{\fs13 oil}{\fs13
was}{\fs13 fed}{\fs13 in}{\fs13 mixture}{\fs13 with}{\fs13 desulphurized}
{\fs13 petroleum}{\fs13 diesel}{\fs13 to}{\fs13 the}{\fs13 hyd- }
rotreater}{\fs13 containing}{\fs13 a}{\fs13 conventional}{\fs13
CoMo/Al}{\fs13 O}{\fs13 hydrotreatment}{\fs13 catalyst.}{\fs13
Conversion}{\fs13 of}{\fs13 esters}{\fs13 was }
\par}{\phpg\posx4141\pvpg\posy5539\absw7109\absh1679 \sl-91 \f20 \fs17 \cf0 \fi3190
{\fs9 2}{\fs9 3 }
determined}{\fs13 in}{\fs13 the}{\fs13 temperature}{\fs13 range}{\fs13
of}{\fs13 305-345}{\fs13 �}{\fs13 C,}{\fs13 at}{\fs13 30}{\fs13 bar}{\fs13
and}{\fs13 for}{\fs13 5}{\fs13 h}{\fs13 <}{\fs13 WHSV}{\fs13 <}{\fs13
25}{\fs13 h}{\fs13 .}{\fs13 Catalyst }
deactivation}{\fs13 was}{\fs13 followed}{\fs13 for}{\fs13 a}{\fs13
period}{\fs13 of}{\fs13 450}{\fs13 h}{\fs13 in}{\fs13 operation.}{\fs13
A}{\fs13 simple}{\fs13 kinetic}{\fs13 model}{\fs13 of}{\fs13 ester}{\fs13
conversion }
suitable}{\fs13 for}{\fs13 scale-up}{\fs13 and}{\fs13 simulation}{\fs13
studies}{\fs13 has}{\fs13 been}{\fs13 tested. }
\fi4382 {\fs13 �}{\fs13 2008}{\fs13 Elsevier}{\fs13 Ltd.}{\fs13 All}{\fs13
rights}{\fs13 reserved. }\par
}
{\phpg\posx9284\pvpg\posy6660\absw145\absh118 \f10 \fs9 \cf0 {\f0\fs11
\bullet }\f10 \fs9 \cf0 {\f20 1 }\par
}
}
Keywords:
Renewable diesel
Hydroprocessing
Vegetable oils \par
}
{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \f20 \fs15 \cf0 \f20 \fs15 \cf0 1.
Introduction
\fi232 The increasing energy consumption in the past decades and the
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-208 \f20 \fs15 \cf0 growing
environmental concerns have made renewable fuels an
attractive alternative to conventional petroleum-based ones. Vege-
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-208 \f20 \fs15 \cf0 table
oils and fats constitute a very important source for the pro-
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-209 \f20 \fs15 \cf0 duction
of diesel compatible biofuels. The well-known
conventional biofuel that is currently worldwide used and pro-
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-209 \f20 \fs15 \cf0 duced
from these sources is biodiesel which is associated with
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-208 \f20 \fs15 \cf0 FAMEs
(fatty acid methyl esters) produced by the transesterifica-
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-209 \f20 \fs15 \cf0 tion of
the triglyceride-containing feedstocks{\cf2 [1].} The demand for
biodiesel is expected to increase in the future since European Un-
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-209 \f20 \fs15 \cf0 ion
(EU) is encouraging its member countries to boost the use of
renewable raw materials for the production of transportation fuels
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-209 \f20 \fs15 \cf0 and
biodiesel appears as the only product from oils and fats, being
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-208 \f20 \fs15 \cf0 a good
substitute to fossil diesel{\cf2 [2].} The aim of the EU's biofuel
directive is to raise the proportion of biofuels and other renewable
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-208 \f20 \fs15 \cf0 fuels
to 5.75% of total gasoline and diesel consumption (based on
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-209 \f20 \fs15 \cf0 energy
content) by 2010{\cf2 [2]. }
However, an alternative route for the production of a diesel sub-
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-209 \f20 \fs15 \cf0 stitute
from vegetable oils and fats is recently developed based on
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-208 \f20 \fs15 \cf0 the
hydrotreatment of the triglyceride-containing feedstocks. The
hydrotreatment process has the advantage that it leads to a deox-
ygenated and thus stable product, fully compatible with petroleum
\par}{\phpg\posx850\pvpg\posy8337\absw5022\absh4851 \sl-208 \f20 \fs15 \cf0 derived
diesel fuels, with a high cetane number and low sulphur
content{\cf2 [3]. }\par
}
{\phpg\posx850\pvpg\posy14272\absw4560\absh746 \f20 \fs12 \cf0 \fi100 \f20 \fs12
\cf0 * Corresponding author. Tel.: +30 210 772 3239; fax: +30 210 772
3155.
E-mail address:{\cf2 npap@central.ntua.gr} (N. Papayannakos).
0016-2361/$ - see front matter � 2008 Elsevier Ltd. All rights reserved.

doi:10.1016/j.fuel.2008.07.032 \par
}
\fs15 \cf0 Since the method of producing renewable diesel through the
hydrotreatment process is recently introduced there is an increas-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-209 \f20 \fs15 \cf0 ing
interest in and tackling with this subject. Krause et al.{\cf2 [4-7] }
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 have
studied the reaction of hydrodeoxygenation of model com-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-209 \f20 \fs15 \cf0 pounds
resembling the ester group containing compounds of
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 wood-
derived bio-oil as aliphatic esters and acids. Similar tests
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-209 \f20 \fs15 \cf0 have
been performed by Laurent and Delmon{\cf2 [8,9],} who focused
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 on the
catalytic performance of CoMo sulfide catalysts of various
supports for the hydrodeoxygenation of oxygen-containing mole-
cules{\cf2 [10-12]. }
Murzin et al.{\cf2 [13],} by using a variety of model compounds
resembling vegetable oils investigated the performance of a num-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-209 \f20 \fs15 \cf0 ber of
catalysts for the production of renewable diesel. According
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 to
their results, Pd supported on active carbon catalysts displayed
superior deoxygenation properties, yielding diesel-like hydrocar-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 bons.
A reaction mechanism and kinetic modeling was also exam-
ined{\cf2 [14-17].} Beside model compounds, the use of vegetable oils
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 either
neat or as a mixture with heavy vacuum oil was examined
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-209 \f20 \fs15 \cf0 by
Corma et al. as feedstock at standard hydrotreating conditions
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-234 \f20 \fs15 \cf0 with
conventional hydrotreating sulphided NiMo/Al {\dn006 \fs10 2}O {\dn006 \fs10
3} catalyst.
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-182 \f20 \fs15 \cf0 Their
results are satisfactory as concerns the production of die-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 sel-
like-hydrocarbons{\cf2 [18]. }
Many companies investigate and plan to apply hydrotreatment
technologies for the production of renewable diesel fuel from veg-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 etable
oils and animal fats. They either take advantage of existing
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-209 \f20 \fs15 \cf0 plants
(oil refineries) by hydroconverting in HDT units blends of
triglyceride-containing material with diesel streams derived from
various units of a refinery (atmospheric distillation, FCC, de-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-208 \f20 \fs15 \cf0 layed
coker, etc.){\cf2 [19,20],} or construct new plants for the produc-
\par}{\phpg\posx6230\pvpg\posy8337\absw5022\absh5603 \sl-209 \f20 \fs15 \cf0 tion
of neat renewable diesel fuel blending stock which can be \par
}
\sect\sectd\pard\plain
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5e5ff00c58458ff00f395a3fe21e8f0f7fd262ffe0bcbff008b08b1ff00e72b5fd0bd1401fcf47fc43d
1e1eff00a4c5ff00c1797ff161163ffce56bf6c7f679f825a37ece3f057e1d7c11d03c6ff167e25e9df
0f3c3f1e8c7e21fc76f897e26f8bff17fc73a8cd7573a9eb5e2cf1ffc42f16dddd6a7adf883c41ad5f6
a1aa5c5b5947a4f857c3f15d43e1af037867c27e0ad1fc3fe18d23d9a8a0028a28a0028a28a0028a28a
28a0028a28a0028a28a0028a28a00fffd9
}}\par}{\phpg\posx654\pvpg\posy957\absw229\absh114 \f20 \fs11 \cf0 \f20 \fs11 \cf0
146 \par
}
{\phpg\posx4729\pvpg\posy957\absw2251\absh114 \f20 \fs11 \cf0 \f20 \fs11 \cf0 I.
Sebos et al. / Fuel 88 (2009) 145-149 \par
}
Nomenclature \par
}
{\phpg\posx853\pvpg\posy1940\absw174\absh1406 \f20 \fs16 \cf0 \f20 \fs16 \cf0 a
\par}{\phpg\posx853\pvpg\posy1940\absw174\absh1406 \sl-199 \f20 \fs16 \cf0 {\fs14 C
}
\par}{\phpg\posx853\pvpg\posy1940\absw174\absh1406 \sl-198 \f20 \fs16 \cf0 {\fs14 k
}
\par}{\phpg\posx853\pvpg\posy1940\absw174\absh1406 \sl-199 \f20 \fs16 \cf0 {\fs14 m
}
\par}{\phpg\posx853\pvpg\posy1940\absw174\absh1406 \sl-199 \f20 \fs16 \cf0 {\fs14 m
}
{\fs14 _ }
\par}{\phpg\posx853\pvpg\posy1940\absw174\absh1406 \sl-216 \f20 \fs16 \cf0 {\fs14 r
}
R}{\fs9 2 }
\par}{\phpg\posx853\pvpg\posy1940\absw174\absh1406 \sl-199 \f20 \fs16 \cf0 {\fs14 x
}\par
}
activity coefficient
concentration
reaction rate constant
\par}{\phpg\posx1570\pvpg\posy1949\absw1627\absh1398 \sl-199 \f20 \fs14 \cf0 mass
quantity
\par}{\phpg\posx1570\pvpg\posy1949\absw1627\absh1398 \sl-199 \f20 \fs14 \cf0 mass
feed rate
reaction rate
\par}{\phpg\posx1570\pvpg\posy1949\absw1627\absh1398 \sl-198 \f20 \fs14 \cf0 degree
of explanation
\par}{\phpg\posx1570\pvpg\posy1949\absw1627\absh1398 \sl-199 \f20 \fs14 \cf0 ester
conversion \par
}
Subscripts
\par}{\phpg\posx6034\pvpg\posy1949\absw706\absh1219 \sl-199 \f20 \fs14 \cf0 cat
\par}{\phpg\posx6034\pvpg\posy1949\absw706\absh1219 \sl-198 \f20 \fs14 \cf0 est
\par}{\phpg\posx6034\pvpg\posy1949\absw706\absh1219 \sl-199 \f20 \fs14 \cf0 exp
\par}{\phpg\posx6034\pvpg\posy1949\absw706\absh1219 \sl-199 \f20 \fs14 \cf0 HDO
\par}{\phpg\posx6034\pvpg\posy1949\absw706\absh1219 \sl-199 \f20 \fs14 \cf0 i
\par}{\phpg\posx6034\pvpg\posy1949\absw706\absh1219 \sl-198 \f20 \fs14 \cf0 o \par
}
catalyst
estimated
experimental
hydrodeoxygenation
current value
reference value \par
}
{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \f20 \fs14 \cf0 \f20 \fs14 \cf0 used
as cetane number improver of mineral diesel{\cf2 [21-23].} One of
major concerns for the application of the hydro-conversion
\par}{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \sl-209 \f20 \fs14 \cf0 process
is the extent of the vegetable oil conversion at conven-
\par}{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \sl-208 \f20 \fs14 \cf0 tional
hydroprocessing conditions. Blending of the hydrodesulphu-
\par}{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \sl-209 \f20 \fs14 \cf0 rized
diesel with vegetable oils or fats and a subsequent
hydrotreatment of the blend would offer {\f63 \u64258\'3f}exibility in the produc-
scheme and a very good alternative to produce a mixture of
\par}{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \sl-208 \f20 \fs14 \cf0 petro
diesel with renewable diesel. In this case among the most
important parameters for the application of this process is the oil
conversion, the stability of commercial catalysts as well as the
\par}{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \sl-209 \f20 \fs14 \cf0 product
quality.
The scope of the present work is the evaluation of the perfor-
\par}{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \sl-235 \f20 \fs14 \cf0 mance
of a commercial HDS (hydrodesulphurization) CoMo/Al {\dn006 \fs9 2}O{\dn006 \fs9 3
}
catalyst in hydrotreating a mixture of cottonseed oil with desul-
phurized diesel for the production of a diesel fuel with enhanced
\par}{\phpg\posx654\pvpg\posy4355\absw5022\absh3532 \sl-209 \f20 \fs14 \cf0 cetane
number. Experiments were conducted in a bench-scale
trickle-bed reactor and the oil conversion was monitored. The
deactivation of the catalyst was determined and considered in
study of reaction kinetics. \par
}
Experimental
\fi232 Experiments were carried out in an integral, isothermal, labora-
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-208 \f20 \fs14 \cf0 tory
bench-scale trickle-bed reactor. The inner diameter of the
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-209 \f20 \fs14 \cf0 reactor
tube was 2.54 cm and its total length 47.5 cm. The temper-
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-208 \f20 \fs14 \cf0 ature
of the catalyst bed was monitored and controlled via five
thermocouples placed inside a thermowell with an external diam-
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-208 \f20 \fs14 \cf0 eter
of 4 mm. The control of the temperature within �1 �C was
accomplished by software proportional-integral-derivative (PID)
controllers, which, through a system of solid-state relays, supply
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-208 \f20 \fs14 \cf0 with
the appropriate energy every single of the four resistors that
''embrace" the reactor tube.
A piston-bearing pump drives the liquid at the top of the cata-
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-209 \f20 \fs14 \cf0 lyst
bed where it is mixed with the gas and they {\f63 \u64258\'3f}ow co-currently
downward in the reactor. The whole unit resembles commercial
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-209 \f20 \fs14 \cf0 ones,
as it is semi-automated with the operating parameters being
controlled from a main personal computer equipped with a data
acquisition card to digitalize analogue signals, which have been
collected and intensified by a multiplexer card. User-friendly soft-
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-209 \f20 \fs14 \cf0 ware
allows the easy handling of the signals for either their sur-
veillance or control.
The experiments were conducted at temperatures in the range
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-208 \f20 \fs14 \cf0 of 305-
345 �C and total pressure of 30 bar. The minimum mass li-
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-209 \f20 \fs14 \cf0 quid
{\f63 \u64258\'3f}ow rate was 25 g/h and the maximum was 125 g/h, corre-
{\f0\fs12 \bullet }{\f10 \fs9 }{\fs9 1 }
sponding to weight hourly space velocities (WHSV) of 5-25 h .
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-209 \f20 \fs14 \cf0 The
{\f63 \u64258\'3f}ow rate of the hydrogen feed was 23-24 Nl/h while the gas
{\f63 \u64258\'3f}owing through the reactor was a 1 vol% H{\dn006 \fs9
2}S/H{\dn006 \fs9 2} mixture. The par-
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-208 \f20 \fs14 \cf0 tial
pressure of H{\dn006 \fs9 2}S was achieved by adding the respective quantity
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-182 \f20 \fs14 \cf0 of DMDS
in the liquid feed. The liquid feed was a mixture of 10 wt%
\par}{\phpg\posx654\pvpg\posy8659\absw5022\absh5842 \sl-209 \f20 \fs14 \cf0 of
refined cottonseed oil in desulphurized diesel (S < 50 ppm). The
catalyst used was a commercial CoMo/Al {\dn006 \fs9 2}O {\dn006 \fs9 3} in
cylindrical form \par
}
with a mean diameter of 1.4 mm which is mainly suggested by
vendors for the production of ultra deep desulphurized diesel
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 oil.
The diluted catalytic bed was 6.1 cm long and consisted of
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 5 g of
catalyst and 36.2 g of inert carborundum (SiC) particles with
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 a mean
diameter of 0.25 mm. Before and after the catalyst bed, two
impeded zones, one from glass spheres of 3 mm in diameter and
another of 4 mm, secured uniform liquid distribution and sup-
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 ported
the catalyst bed. The loading of the bed was dense as por-
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 tions
of catalyst and diluent carborundum were sequentially
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 added
in the continuously shaken reactor.
The catalyst was dehumidified under hydrogen with a {\f63 \u64258\'3f}ow of
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 15
Nl/h for 2 h at 100 �C. The sulphided catalyst was prepared
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 in
situ by raising the temperature to 340 �C at a rate of 20 �C per
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-235 \f20 \fs14 \cf0 hour
with a gas {\f63 \u64258\'3f}ow of 15 Nl/h H {\dn006 \fs9 2} and a liquid
{\f63 \u64258\'3f}ow of 20 g/h of
diesel. DMDS was added so that S concentration in liquid feed
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 was 1
wt%. Presulphidation was continued for 4 h at 340 �C.
After activating the catalyst, experiments for 43 days lasting for
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 10-12
h per day were conducted. Deactivation was followed by
repetition of standard experiments. In the beginning of each exper-
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 iment,
high liquid and gas {\f63 \u64258\'3f}ow rates were used to wet the catalyst
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 bed
and avoid liquid maldistribution during operation. The steady
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 state
of each experiment was achieved after 4-6 h of continuous
operation depending on liquid and gas {\f63 \u64258\'3f}ow rates. In between the
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 daily
experimental intervals of 10-12 h, the reactor was cooled
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 down
smoothly under hydrogen {\f63 \u64258\'3f}ow and kept under 30 bar pres-
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 sure
overnight at room temperature.
In{\cf2 Table}{\cf2 1,} the composition of cottonseed oil used is shown. The
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 liquid
product of the reaction was collected and its saponification
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 number
was determined according to ASTM D94-02. By comparing
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 it
with the respective number of the feed, we calculate the conver-
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 sion
of the saponifiable material present in the feed. Since the die-
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 sel
used was desulphurized, the only saponifiable material of the
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-208 \f20 \fs14 \cf0 feed
was the fatty triglycerides of the cottonseed oil that has been
verified experimentally. Thus, the relative change of the saponifica-
number can be used as a measure of the conversion of the es-
\par}{\phpg\posx6034\pvpg\posy4355\absw5022\absh7110 \sl-209 \f20 \fs14 \cf0 ter
group containing material that comes from the triglycerides of
feedstock and can also be mono- and di-esters in the partly
converted oils. \par
}
Table 1
Composition of cottonseed oil
Fatty acids type
Palmitic
Palmitoleic
Stearic
\par}{\phpg\posx6034\pvpg\posy12946\absw1779\absh1833 \sl-171 \f20 \fs11 \cf0 Oleic

trans-Oleic
Linoleic
trans-Linoleic
Linolenic \par
}
Form
16:0
\par}{\phpg\posx7878\pvpg\posy13403\absw314\absh1421 \sl-172 \f20 \fs11 \cf0 16:1
18:3 \par
}
Formula
\par}{\phpg\posx9071\pvpg\posy13403\absw550\absh1433 \sl-126 \par\f20 \fs11 \cf0 C
H O
\par}{\phpg\posx9071\pvpg\posy13403\absw550\absh1433 \f20 \fs11 \cf0 \fi78 {\fs7
16}{\fs7 32}{\fs7 2 }
\par}{\phpg\posx9071\pvpg\posy13403\absw550\absh1433 \sl-150 \f20 \fs11 \cf0 C H
O
16}{\fs7 30}{\fs7 2 }
O
18}{\fs7 36}{\fs7 2 }
O
18}{\fs7 34}{\fs7 2 }
O
18}{\fs7 34}{\fs7 2 }
O
18}{\fs7 32}{\fs7 2 }
O
18}{\fs7 32}{\fs7 2 }
O
18}{\fs7 30}{\fs7 2 }\par
}
{\phpg\posx10501\pvpg\posy13403\absw553\absh1421 \f20 \fs11 \cf0 \f20 \fs11 \cf0 %
(kg/kg)
22.96
0.90
2.30
\par}{\phpg\posx10501\pvpg\posy13403\absw553\absh1421 \sl-171 \f20 \fs11 \cf0 16.70

0.10

0.02
0.20 \par
}
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}}\par}{\phpg\posx4925\pvpg\posy957\absw2251\absh114 \f20 \fs11 \cf0 \f20 \fs11
\cf0 I. Sebos et al. / Fuel 88 (2009) 145-149 \par
}
147 \par
}
Results and discussion
\fi232 In order to examine the kinetics of the hydrodeoxygenation
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-208 \f20 \fs14 \cf0 (HDO)
of the triglycerides of the feedstock to obtain diesel-like
hydrocarbons at the conditions of our experiments, it is considered
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-208 \f20 \fs14 \cf0 that
plug {\f63 \u64258\'3f}ow is well approximated within the reactor, since the
dilution of the catalyst bed with fine particles (SiC) ensures the full
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-208 \f20 \fs14 \cf0 wetting
of catalyst particles and the avoidance of liquid maldistri-
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-209 \f20 \fs14 \cf0 bution
or axial dispersion{\cf2 [24,25].} As the normal boiling point of
triglycerides in the vegetable oil used is more than 400 �C
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-209 \f20 \fs14 \cf0 {\cf2
[26],} their evaporation is restricted and the vegetable oil is consid-
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-209 \f20 \fs14 \cf0 ered to
be present only in the liquid phase. Internal mass transfer
restrictions are included in the reaction kinetics described in this
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-209 \f20 \fs14 \cf0 work
and therefore the kinetics presented in the followings is an
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-208 \f20 \fs14 \cf0 overall
kinetics and not an intrinsic one. However, internal diffu-
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-209 \f20 \fs14 \cf0 sion
is not expected to limit the reaction severely as the Weisz
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-208 \f20 \fs14 \cf0 modulus
is calculated less than 1.5 for all the reaction conditions
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-209 \f20 \fs14 \cf0 of this
work.
Furthermore, it is assumed that the HDO of the ester groups is a
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-209 \f20 \fs14 \cf0 first-
order reaction, proportional to the concentration of the ester
\par}{\phpg\posx850\pvpg\posy1366\absw5022\absh3909 \sl-208 \f20 \fs14 \cf0 content
of the feedstock (Eq.{\cf2 (1)) }\par
}
�#{\dn006 \f20 \fs9 HDOr}{\f20 } � �{\f20 k}{\dn006 \f20 \fs9 HDO }\par
}
where{\f10 #}r \par
}
C{\dn006 \fs9 est}{\dn006 \fs7 0 }\par
}
\bullet }\f10 \fs15 \cf0 {\f20 C}{\dn006 \f20 \fs9 est}{\dn006 \f20 \fs7 0 }\par
}
\bullet }\f10 \fs15 \cf0 �{\f20 1} #{\f20 x}�; \par
}
\fs14 \cf0 The activity of the catalyst and ester conversion versus time is
presented in{\cf2 Fig.}{\cf2 1.} During the first 100 h the catalyst
was stabi-
\par}{\phpg\posx6230\pvpg\posy1350\absw5021\absh2402 \sl-209 \f20 \fs14 \cf0 lized
and its activity was followed after this period. The activity
coefficient at 100 hours is set as the reference one ({\fs17 a} = 1). As seen
in{\cf2 Fig.}{\cf2 1,} catalyst activity declines slowly up to 300 h in operation
\par}{\phpg\posx6230\pvpg\posy1350\absw5021\absh2402 \sl-208 \f20 \fs14 \cf0 with a

loss of about 13% in respect to the reference value while it
appears to reach a steady state after this period.
The experimentally obtained conversions along with the esti-
\par}{\phpg\posx6230\pvpg\posy1350\absw5021\absh2402 \sl-209 \f20 \fs14 \cf0 mated
ones, by using the proposed model of hydrodeoxygenation,
\par}{\phpg\posx6230\pvpg\posy1350\absw5021\absh2402 \sl-208 \f20 \fs14 \cf0 are
presented in{\cf2 Figs.}{\cf2 2-4} vs. WHSV for 305, 320 and 335 �C,
respectively. Experimental conversions were corrected from the
in{\f63 \u64258\'3f}uence of catalyst deactivation by using Eqs.{\cf2 (2)}{\cf2
and}{\cf2 (3). }
The goodness of the model was evaluated by the calculation of \par
}
{\phpg\posx8365\pvpg\posy4041\absw69\absh125 \f20 \fs9 \cf0 \f20 \fs9 \cf0 2 \par
}
{\phpg\posx6230\pvpg\posy4069\absw2135\absh221 \f20 \fs14 \cf0 \f20 \fs14 \cf0 the
degree of explanation, R
{\fs15 " }
{\fs15 P }\par
}
{\phpg\posx6230\pvpg\posy4494\absw1294\absh187 \f20 \fs9 \cf0 \fi96 \f20 \fs9 \cf0
2
R}{\f10 \fs15 �}{\fs15 100}{\fs15 %}{\f10 \fs15 #}{\fs15 1}{\f10 \fs15
# }\par
}
�{\f20 x}{\dn006 \f20 \fs9 exp }\par
}
{\phpg\posx7561\pvpg\posy4551\absw175\absh198 \f20 \fs15 \cf0 \f20 \fs15 \cf0 P
\par
}
�{\f20 4}� \par
}
�{\f20 x}{\dn006 \f20 \fs9 exp }\par
}
\bullet }\f10 \fs15 \cf0 {\f20 x}{\dn006 \f20 \fs9 est}�
{\f0\fs19 \bullet }{\f20 }{\dn006 \f20 \fs9 exp}�x \par
}
{\phpg\posx8594\pvpg\posy4376\absw80\absh333 \f20 \fs9 \cf0 \f20 \fs9 \cf0 2
\par}{\phpg\posx8594\pvpg\posy4376\absw80\absh333 \sl-130 \par\f20 \fs9 \cf0 2 \par
}
{\phpg\posx8685\pvpg\posy4243\absw150\absh407 \f20 \fs15 \cf0 \f20 \fs15 \cf0 #
{\f10 ; }\par
}
HDO{\fs14 is}{\fs14 the}{\fs14 rate}{\fs14 of}{\fs14 HDO,}{\fs14 k}
{\dn006 HDO }\par
}
\fs15 \cf0 �{\f20 1}�
{\f20 \fs14 the}{\f20 \fs14 reaction}{\f20 \fs14 rate}{\f20 \fs14
constant, }\par
}
{\phpg\posx1238\pvpg\posy6389\absw4633\absh143 \f20 \fs14 \cf0 \f20 \fs14 \cf0 the
ester group content of the feedstock as determined by \par
}
where subscripts exp and est denote experimental and estimated,
respectively. R {\up006 \fs9 2} values were calculated 92.93%, 96.94% and 94.46%
\par}{\phpg\posx6230\pvpg\posy5020\absw5022\absh1461 \sl-208 \f20 \fs14 \cf0 for
305, 320 and 335 �C, which indicate a satisfactory fitting of
experimental data.
As seen in{\cf2 Figs.}{\cf2 2-4} conversion increases with temperature.
Analysis of the temperature dependency based on the Arrhenius
equation and the proposed model results in a value of activation
\par}{\phpg\posx6230\pvpg\posy5020\absw5022\absh1461 \sl-209 \f20 \fs14 \cf0 energy
equal to 111 kJ/mol (Fig.{\cf2 5). }\par
}
saponification number and x their conversion. As mentioned before,
conversion is determined by the relative change of the saponifica-
number between feedstock and product stream. By implement-
\par}{\phpg\posx850\pvpg\posy6598\absw5022\absh896 \sl-209 \f20 \fs14 \cf0 ing the
rate expression into the mass balance of ester group content,
\par}{\phpg\posx850\pvpg\posy6598\absw5022\absh896 \sl-208 \f20 \fs14 \cf0 Eq.{\cf2
(2)} is obtained, which is the main formula of our model and by \par
}
{\phpg\posx850\pvpg\posy7644\absw856\absh165 \f20 \fs14 \cf0 \f20 \fs14 \cf0 which
k{\dn006 \fs9 HDO }\par
}
k{\dn006 \fs9 HDO }\par
}
{\phpg\posx1759\pvpg\posy7644\absw1407\absh143 \f20 \fs14 \cf0 \f20 \fs14 \cf0 can
be determined \par
}
{\shp\shpleft6475\shptop7771\shpright6635\shpbottom7865
\shpz0\shpfhdr0\shpbxpage\shpbypage\shpwr3\shpwrk0\shpfblwtxt0
{\*\shpinst {\sp{\sn fLine}{\sv 0}}{\sp{\sn shapeType}{\sv 202}}
{\sp{\sn dxTextLeft}{\sv 0}}{\sp{\sn dxTextRight}{\sv 0}}
{\sp{\sn dyTextTop}{\sv 0}}{\sp{\sn dyTextBottom}{\sv 0}}
{\sp{\sn fFilled}{\sv 0}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 x \par}}
{\phpg\posx1230\pvpg\posy7937\absw1716\absh223 \f10 \fs15 \cf0 \f10 \fs15 \cf0 �
#{\f20 ln}�{\f20 1} #{\f20 x}� #{\f20 m_}{\f20 =} m{\f20 }{\dn006 \f20 \fs9
cat}; \par
}
�{\f20 2}� \par
}
{\phpg\posx850\pvpg\posy8265\absw2506\absh143 \f20 \fs14 \cf0 \f20 \fs14 \cf0 where
m is mass feed rate and m \par
}
{\phpg\posx1419\pvpg\posy8264\absw91\absh129 \f20 \fs14 \cf0 \f20 \fs14 \cf0 _ \par
}
cat{\fs14 the}{\fs14 catalyst}{\fs14 mass. }\par
}
\cf0 The deactivation of the catalyst is monitored by calculating the
activity coefficient (Eq.{\cf2 (3))} of each repeated standard experiment.
\par}{\phpg\posx850\pvpg\posy8475\absw5022\absh1084 \sl-209 \f20 \fs14 \cf0 The
conditions of the standard experiments were selected to be:
\par}{\phpg\posx850\pvpg\posy8475\absw5022\absh1084 \sl-208 \f20 \fs14 \cf0 reactor
temperature 320 �C, reactor total pressure 30 bar, partial
pressure of H {\dn006 \fs9 2}S 1 vol%, mass feed rate 40 g/h and H {\dn006 \fs9
2} gas {\f63 \u64258\'3f}ow rate
\par}{\phpg\posx850\pvpg\posy8475\absw5022\absh1084 \sl-182 \f20 \fs14 \cf0 23-24
Nl/h \par
}
{\phpg\posx850\pvpg\posy9806\absw645\absh186 \f20 \fs18 \cf0 \f20 \fs18 \cf0 a{\f10
\fs15 �}{\fs15 k}{\dn006 \fs9 HDO }\par
}
i{\f10 \fs15 =}{\fs15 k}{\dn006 \fs9 HDO}{\f10 \fs15 ;o }\par
}
�{\f20 3}� \par
}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 Conversion, \par}}
experimental
\par}{\phpg\posx7402\pvpg\posy9339\absw687\absh221 \sl-156 \f10 \fs9 \cf0 model
prediction \par
}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 Ester \par}}
\par}{\phpg\posx6758\pvpg\posy7150\absw210\absh2407 \sl-170 \par\f10 \fs14 \cf0 70
\fi49 0 \par
}
\par
}
\par
}
\par
}
\par
}
\par
}
\par}{\phpg\posx9394\pvpg\posy9828\absw210\absh300 \sl-198 \f10 \fs14 \cf0 {\b
\fs10 -1 }\par
}
\par
}
14 \par
}
16 \par
}
where{\fs17 a} is the activity coefficient and subscript o and i denote the
reference and current values, respectively. \par
}
{\phpg\posx6230\pvpg\posy10072\absw5020\absh475 \b \f10 \fs16 \cf0 \fi2432 \b
\f10 \fs16 \cf0 WHSV (h )
\par}{\phpg\posx6230\pvpg\posy10072\absw5020\absh475 \sl-184 \par\b \f10 \fs16 \cf0
{\b0 \f20 \fs11 Fig.}{\b0 \f20 \fs11 2.}{\b0 \f20 \fs11 Conversion}{\b0 \f20
\fs11 of}{\b0 \f20 \fs11 esters}{\b0 \f20 \fs11 vs.}{\b0 \f20 \fs11 WHSV.}
{\b0 \f20 \fs11 Reaction}{\b0 \f20 \fs11 conditions:}{\b0 \f20 \fs11 T}
{\b0 \f20 \fs11 =}{\b0 \f20 \fs11 305}{\b0 \f20 \fs11 �}{\b0 \f20 \fs11 C,}
{\b0 \f20 \fs11 P}{\b0 \f20 \fs11 =}{\b0 \f20 \fs11 30}{\b0 \f20 \fs11
bar, }\par
}
P{\fs7 H }{\dn006 \fs5 2}{\fs7 S}{\f10 � }\par
}
vol%, m{\dn006 \fs7 cat }\par
}
{\phpg\posx7395\pvpg\posy10642\absw3855\absh114 \f20 \fs11 \cf0 \f20 \fs11 \cf0 = 5
g. Feedstock: 10 wt% cottonseed oil in desulphurized diesel. \par
}
\par
}
70 \par
}
0.9 \par
}
60 \par
}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 ) \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 % \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 ( \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \f40 \fs15 \cf0 {\field{\*\fldinst SYMBOL
97 \\f Symbol }} \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 ty, \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 i \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 tiv \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 c \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 A{\b0\dn006 \fs14
0.7 }\par}}
0.8 \par
}
50 \par
}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 on, \par}}
40 \par
}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 ersi \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 v \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 n \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 o \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 C \par}}
0.6 \par
}
30 \par
}
activity coefficient,{\f40 {\field{\*\fldinst SYMBOL 97 \\f Symbol }} }
conversion, x (%) \par
}
\cf0 300
\fs16 Time}{\b \fs16 (h) }\par
}
400 \par
}
0.5 \par
}
\par
}
100 \par
}
200 \par
}
\cf0 20
\par
}

90
80
70
60
50
40
30
20
10
0 \par
}
experimental
prediction
\fi215 {\fs14 5 }\par
}
\par
}
10 \par
}
15 \par
}
20 \par
}
25 \par
}
30 \par
}
{\phpg\posx850\pvpg\posy14631\absw5021\absh422 \f20 \fs11 \cf0 \f20 \fs11 \cf0 Fig.
1. Catalyst activity and conversion vs. time. Conditions of repeated
standard
experiment: T = 320 �C, P = 30 bar, P{\fs7 H }{\dn006 \fs5 2}{\fs7 S}{\f10
�} 1 vol%, m{\dn006 \fs7 cat} = 5 g, WHSV = 8 h . Feed-
\par}{\phpg\posx850\pvpg\posy14631\absw5021\absh422 \sl-171 \f20 \fs11 \cf0 stock:
10 wt% cottonseed oil in desulphurized diesel. \par
}
}
{\phpg\posx6230\pvpg\posy14376\absw5020\absh499 \b \f10 \fs16 \cf0 \fi2432 \b
\f10 \fs16 \cf0 WHSV (h{\up006 \fs10 -1})
{\b0 \f20 \fs11 Fig.}{\b0 \f20 \fs11 3.}{\b0 \f20 \fs11 Conversion}{\b0 \f20
\fs11 of}{\b0 \f20 \fs11 esters}{\b0 \f20 \fs11 vs.}{\b0 \f20 \fs11 WHSV.}
{\b0 \f20 \fs11 Reaction}{\b0 \f20 \fs11 conditions:}{\b0 \f20 \fs11 T}
{\b0 \f20 \fs11 =}{\b0 \f20 \fs11 320}{\b0 \f20 \fs11 �}{\b0 \f20 \fs11 C,}
{\b0 \f20 \fs11 P}{\b0 \f20 \fs11 =}{\b0 \f20 \fs11 30}{\b0 \f20 \fs11
bar, }\par
}
P{\fs7 H }{\dn006 \fs5 2}{\fs7 S}{\f10 � }\par
}
vol%, m{\dn006 \fs7 cat }\par
}
}
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50014514500145145001451450014514500145145001451450014514500145145001451450014514500
1451450014514500145145001451450014514500145145007ca1e23ff0091875eff00b0cea9ff00a5d3
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14514500145145001451450014514500145145001451450014514500145145001451450014514500145
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14500145145001451450014514500145145001451450014514500145145001451450014514500145145
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}}\par}{\phpg\posx654\pvpg\posy957\absw229\absh114 \f20 \fs11 \cf0 \f20 \fs11 \cf0
148 \par
}
{\phpg\posx4729\pvpg\posy957\absw2251\absh114 \f20 \fs11 \cf0 \f20 \fs11 \cf0 I.
Sebos et al. / Fuel 88 (2009) 145-149 \par
}
350 \par
}
90
80
70
60
50
40
30
20
10 \par
}
\par
}
\par
}
400 \par
}
300 \par
}
250 \par
}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 C \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs10 \cf0 o \par}}
200 \par
}
150 \par
}
experimental
prediction \par
}
desulphurised diesel \par
}
product with renewable diesel \par
}
\cf0 100
IBP 5% 10% 20% 30% 40% 50% 60% 70% 80% 85% 90% 95% FBP
{\b \fs16 %}{\b \fs16 vol/vol }
{\f20 \fs11 Fig.}{\f20 \fs11 6.}{\f20 \fs11 Distillation}{\f20 \fs11
curves}{\f20 \fs11 of}{\f20 \fs11 the}{\f20 \fs11 desulphurized}{\f20
\fs11 diesel}{\f20 \fs11 and}{\f20 \fs11 the}{\f20 \fs11 product}
{\f20 \fs11 with }
{\f20 \fs11 renewable}{\f20 \fs11 diesel. }\par
}
Conclusions
\fi232 In this study a commercial CoMo catalyst was tested for the
hydrodeoxygenation of a mixture of 10 wt% cottonseed oil in diesel
\par}{\phpg\posx6034\pvpg\posy5189\absw5021\absh5227 \sl-208 \f20 \fs14 \cf0 at
conditions similar to the ones used in conventional HDS units of
refinery plants. The results are satisfactory as concerns the use of
existing petroleum refinery infrastructure for vegetable oil
conversion to diesel fuel. Summarizing our findings:
\fi23 1. Catalyst performed rather stable, appearing to reach a steady
state after 300 h in operation.
2. Under the conditions examined, a conversion of triglycerides
\fi4487 {\f0\fs12 \bullet }{\f10 \fs9 }{\fs9 1 }
close to 100% can be achieved with WHSV less than 5 h .
3. The assumption that hydrodeoxygenation is a first-order reac-
tion with respect to the ester content, under the conditions of
our tests, results in a satisfactory simulation of experimental
data with degrees of explanation 92-97%.
4. Hydrodeoxygenation is temperature dependent, with an activa-
tion energy of 111 kJ/mol.
5. Hydrotreatment of a 10 wt% mixture of cottonseed oil in diesel
under the conditions examined results in a +3 raise of cetane
number, which implies a cetane number of the hydrodeoxygen-
ated cottonseed oil of 80. Moreover, other quality related prop-
erties of the matrix desulphurized diesel used, as distillation
curve, density and cloud pint, are not affected. Thus, the hydro-
treatment of vegetable oils not only contributes to the produc-
tion of fuel from renewable feedstocks, but also results in the
production of diesel-like hydrocarbons of superior quality. \par
}
\par
}
\par
}
\cf0 15
\fs16 WHSV}{\b \fs16 (h}{\b\up006 \fs10 -1}{\b \fs16 ) }\par
}
\par
}
\par
}
\par
}
{\phpg\posx654\pvpg\posy4708\absw5020\absh116 \f20 \fs11 \cf0 \f20 \fs11 \cf0 Fig.
4. Conversion of esters vs. WHSV. Reaction conditions: T = 335 �C, P = 30
bar, \par
}
{\phpg\posx654\pvpg\posy4879\absw378\absh142 \f20 \fs11 \cf0 \f20 \fs11 \cf0 P{\fs7
H }{\dn006 \fs5 2}{\fs7 S}{\f10 � }\par
}
{\phpg\posx1069\pvpg\posy4879\absw717\absh143 \f20 \fs11 \cf0 \f20 \fs11 \cf0 1 vol
%, m{\dn006 \fs7 cat }\par
}
}
\par
}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 ) \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs10 \cf0 -1 \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 h \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 ( \par}}
{\sp{\sn txflTextFlow}{\sv 2}}}{\shptxt \b \f10 \fs15 \cf0 k \par}}
{\phpg\posx1184\pvpg\posy6859\absw105\absh118 \f10 \fs9 \cf0 \f10 \fs9 \cf0 10 \par
}
{\phpg\posx1186\pvpg\posy8169\absw295\absh188 \f10 \fs9 \cf0 \fi56 \f10 \fs9 \cf0 1

\par
}
{\phpg\posx1743\pvpg\posy8288\absw348\absh118 \f10 \fs9 \cf0 \f10 \fs9 \cf0 0.00162
\par
}
\par
}
\par
}
\par
}
0.0017 \par
}
\par
}
\par
}
{\phpg\posx654\pvpg\posy8473\absw5020\absh498 \b \f10 \fs16 \cf0 \fi2508 \b \f10
\fs16 \cf0 1/T (K {\up006 \fs10 -1})
{\b0 \f20 \fs11 Fig.}{\b0 \f20 \fs11 5.}{\b0 \f20 \fs11 Arrhenius}{\b0 \f20
\fs11 plot}{\b0 \f20 \fs11 for}{\b0 \f20 \fs11 the}{\b0 \f20 \fs11 first-
order}{\b0 \f20 \fs11 reaction}{\b0 \f20 \fs11 constant.}{\b0 \f20 \fs11
Reaction}{\b0 \f20 \fs11 conditions: }\par
}
{\phpg\posx654\pvpg\posy9071\absw1720\absh268 \f20 \fs11 \cf0 \f20 \fs11 \cf0 T =
305-345 �C, P = 30 bar, P
\par}{\phpg\posx654\pvpg\posy9071\absw1720\absh268 \sl-171 \f20 \fs11 \cf0 oil in
desulphurized diesel. \par
}
H{\dn006 \fs5 2} S{\f10 \fs11 � }\par
}
{\phpg\posx2719\pvpg\posy9071\absw726\absh143 \f20 \fs11 \cf0 \f20 \fs11 \cf0 1 vol
%, m{\dn006 \fs7 cat }\par
}
g. Feedstock: 10 wt% cottonseed \par
}
\cf0 In{\cf2 Table}{\cf2 2} and{\cf2 Fig.}{\cf2 6} a comparison between
the mixture con-
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-208 \f20 \fs14 \cf0 taining
the renewable diesel and the desulphurized diesel used
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-209 \f20 \fs14 \cf0 in
preparing the feed mixture of 10 wt% cottonseed oil, is pre-
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-208 \f20 \fs14 \cf0 sented,
for assessing the quality of the hydrotreated product. The
{\f0\fs12 \bullet }{\f10 \fs9 }{\fs9 1 }
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-280 \f20 \fs14 \cf0 and the
ester conversion was 97%. As regards the density, distilla-
curve and cloud point, the product with renewable diesel has
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-208 \f20 \fs14 \cf0 almost
the same behavior as desulphurized diesel. However, ce-
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-209 \f20 \fs14 \cf0 tane
number and index have been significantly improved. More
specifically, the cetane number was determined to be 53 for the
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-209 \f20 \fs14 \cf0 mixture
compared to 50 of the matrix desulphurized diesel. With
assumption that cetane number of the product mixture is a lin-
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-209 \f20 \fs14 \cf0 ear
function of its components, the observed increase corresponds
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-208 \f20 \fs14 \cf0 to a
cetane number of 80 of the hydrotreated cottonseed oil. This
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-209 \f20 \fs14 \cf0 value
is in close agreement with the cetane values referred in liter-
\par}{\phpg\posx654\pvpg\posy9788\absw5022\absh2967 \sl-208 \f20 \fs14 \cf0 ature
for renewable diesels{\cf2 [3,18,23]. }\par
}
mixture tested had been processed at 345 �C and WHSV = 6 h \par
}
Table 2
Properties of the mixture containing the renewable diesel compared to desulphurized
\par}{\phpg\posx654\pvpg\posy13460\absw5021\absh423 \sl-172 \f20 \fs11 \cf0 diesel

used as matrix \par
}
Properties
Density @ 15 �C (g/ml)
\par}{\phpg\posx654\pvpg\posy14089\absw1380\absh806 \sl-171 \f20 \fs11 \cf0 Cetane
number
\par}{\phpg\posx654\pvpg\posy14089\absw1380\absh806 \sl-171 \f20 \fs11 \cf0 Cetane
index
\par}{\phpg\posx654\pvpg\posy14089\absw1380\absh806 \sl-171 \f20 \fs11 \cf0 Cloud
point (�C) \par
}
Desulphurated diesel
0.8533
\par}{\phpg\posx2274\pvpg\posy14089\absw1285\absh804 \sl-171 \f20 \fs11 \cf0 0 \par
}
Mixture with renewable diesel
0.8497
\par}{\phpg\posx3799\pvpg\posy14089\absw1875\absh804 \sl-171 \f20 \fs11 \cf0 0 \par
}
Acknowledgement
\par}{\phpg\posx6034\pvpg\posy11467\absw5021\absh3267 \sl-209 \par\f20 \fs14
\cf0 \fi238 The authors thank Motor-Oil Hellas Refinery for the financial
support of this work and giving permission for publication.
References
\par}{\phpg\posx6034\pvpg\posy11467\absw5021\absh3267 \sl-180 \par\f20 \fs14
\cf0 \fi63 {\fs11 [1]}{\fs11 Barakos}{\fs11 N,}{\fs11 Pasias}{\fs11 S,}
{\fs11 Papayannakos}{\fs11 N.}{\fs11 Transesterification}{\fs11 of}{\fs11
triglycerides}{\fs11 in }
\fi296 {\fs11 high}{\fs11 and}{\fs11 low}{\fs11 quality}{\fs11 oil}{\fs11
feeds}{\fs11 over}{\fs11 an}{\fs11 HT2}{\fs11 hydrotalcite}{\fs11
catalyst.}{\fs11 Bioresource }
\fi296 {\fs11 Technology}{\fs11 2008;99(11):5037-42. }
{\fs11 [2]}{\fs11 Directive}{\fs11 2003/30/EC}{\fs11 of}{\fs11 the}{\fs11
European}{\fs11 Parliament}{\fs11 and}{\fs11 of}{\fs11 the}{\fs11 Council}
{\fs11 of}{\fs11 8}{\fs11 May }
\fi296 {\fs11 2003}{\fs11 on}{\fs11 the}{\fs11 promotion}{\fs11 of}{\fs11
the}{\fs11 use}{\fs11 of}{\fs11 biofuels}{\fs11 and}{\fs11 other}{\fs11
renewable}{\fs11 fuels}{\fs11 for }
\fi296 {\fs11 transport.}{\fs11 Official}{\fs11 J}{\fs11 Eur}{\fs11 Union}
{\fs11 L}{\fs11 123/42,}{\fs11 Brussels,}{\fs11 17.5.2003. }
{\fs11 [3]}{\fs11 Stumborg}{\fs11 M,}{\fs11 Wong}{\fs11 A,}{\fs11 Hogan}
{\fs11 E.}{\fs11 Hydroprocessed}{\fs11 vegetable}{\fs11 oils}{\fs11 for}
{\fs11 diesel}{\fs11 fuel }
\fi296 {\fs11 improvement.}{\fs11 Bioresource}{\fs11 Technol}{\fs11
1996;56:13-8. }
{\fs11 [4]}{\fs11 S�}{\fs11 e}{\fs11 nol}{\fs11 O}{\fs11 _}{\fs11 I,}{\fs11
Viljava}{\fs11 TR,}{\fs11 Krause}{\fs11 AOI.}{\fs11 Hydrodeoxygenation}
{\fs11 of}{\fs11 methyl}{\fs11 esters}{\fs11 on }
\fi296 {\fs11 sulphided}{\fs11 NiMo/}{\fs13 c}{\fs11 -Al }{\dn006 \fs7 2}
{\fs11 O}{\dn006 \fs7 3}{\fs11 and}{\fs11 CoMo/}{\fs13 c}{\fs11 -Al}
{\dn006 \fs7 2}{\fs11 O}{\dn006 \fs7 3}{\fs11 catalysts.}{\fs11 Catal}
{\fs11 Today }
\fi297 {\fs11 2005;100:331-5. }
{\fs11 [5]}{\fs11 S�}{\fs11 e}{\fs11 nol}{\fs11 O}{\fs11 _}{\fs11 I,}{\fs11
Ryymin}{\fs11 EM,}{\fs11 Viljava}{\fs11 TR,}{\fs11 Krause}{\fs11 AOI.}
{\fs11 Reactions}{\fs11 of}{\fs11 methyl}{\fs11 heptanoate }
\fi297 {\fs11 hydrodeoxygenation}{\fs11 on}{\fs11 sulphided}{\fs11
catalysts.}{\fs11 J}{\fs11 Mol}{\fs11 Catal}{\fs11 A:}{\fs11
Chem }
\fi297 {\fs11 2007;268:1-8. }\par
}
ffd8ffe000104a46494600010100000100010000ffdb004300010101010101010101010101010101010
10101010101010101010101010101010101010101010101010101010101010101010101010101010101
010101010101ffdb0043010101010101010101010101010101010101010101010101010101010101010
1010101010101010101010101010101010101010101010101010101010101010101ffc0001108031a02
5303012200021101031101ffc4001f00000105010101010101000000000000000001020304050607080
90a0bffc400b5100002010303020403050504040000017d010203000411051221314106135161072271
14328191a1082342b1c11552d1f02433627282090a161718191a25262728292a3435363738393a43444
5464748494a535455565758595a636465666768696a737475767778797a838485868788898a92939495
0102030405060708090a0bffc400b511000201020404030407050404000102770001020311040521310
61241510761711322328108144291a1b1c109233352f0156272d10a162434e125f11718191a26272829
2a35363738393a434445464748494a535455565758595a636465666768696a737475767778797a82838
0028a28a0028a28a0028a28a0028a28a0028a28
8a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a0028a28a00ffd9
}}\par}{\phpg\posx4925\pvpg\posy958\absw2251\absh114 \f20 \fs12 \cf0 \f20 \fs12
\cf0 I. Sebos et al. / Fuel 88 (2009) 145-149 \par
}
\cf0 [6] S�enol O_I, Viljava TR, Krause AOI. Hydrodeoxygenation of
aliphatic esters on
sulphided NiMo/{\fs14 c}-Al{\dn006 \fs8 2}O{\dn006 \fs8 3} and CoMo/{\fs14 c}-Al
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