Journal of Natural Gas Chemistry 21(2012)194–199

Weakening internal diffusion effect in selective hydrodesulfurization of

FCC gasoline by novel designed eggshell CoMoS/Al2O3 catalysts
Bin Liu, Yongming Chai∗ , Yajing Wang, Yunqi Liu, Chenguang Liu∗
State Key Laboratory of Heavy Oil Processing, Key Laboratory of Catalysis, China National Petroleum Corp. (CNPC),
China University of Petroleum (East China), Qingdao 266555, Shandong, China
[ Manuscript received July 25, 2011; revised October 24, 2011 ]

Abstract
A simple method for preparation of presulfided eggshell CoMoS/γ-Al2 O3 catalysts with sharp boundary is developed, through which the
eggshell thicknesses of Co and Mo could be easily regulated by controlling the impregnation time. According to the results characterized by
EDS, XRD, HRTEM and FT-IR of adsorbed CO, the active component structures, the nature and/or the amount of active sites on the eggshell
catalyst are similar to these on the uniform catalyst. The evaluation results of the catalytic performance in selective hydrodesulfurization (HDS)
of FCC gasoline show the presence of significant internal diffusion inhibition effect on HDS of S-compounds especially in the uniform catalyst.
Compared with uniform catalyst, the eggshell catalyst could remarkably reduce such an internal diffusion inhibition effect due to a shortened
diffusion path of the reactants, thus showing higher HDS activity and selectivity.
Key words
CoMoS/γ-Al2 O3 ; eggshell catalyst; uniform catalyst; internal diffusion; hydrodesulfurization

1. Introduction The internal diffusion resistance within the pores of cata-

The increasing need for ultra-clean gasoline requires to
drastically improve the efficiency of hydrotreating process.
Besides major sulfur content, FCC gasoline also contains
large content of olefins which are attributable to the high oc-
tane number of the final product, however, the olefins usu-
ally be easily hydrogenated in the hydrodesulfurization (HDS)
units [1]. Therefore, preparation of catalysts with high activ-
ity and selectivity in the HDS of FCC gasoline is a arguably
preferable solution. In order to realized higher use efficiency
of active components, the active components with eggshell
distribution supported on porous supports have been widely
studied and applied in oxidation [2], Fischer-Tropsch synthe-
sis [3,4], hydrogenation [5,6], automotive exhaust purification
[7] and other fields [8,9]. Moreover, the eggshell distribution
has been theoretically and experimentally proved to eliminate
the adverse intra-particle mass transfer limitation effectively
in some cases [10−12].
lysts can cause the reactant concentration and reaction temper-
ature gradient in the different region of the catalyst particle,
and thus affected catalytic activity and selectivity [13−16].
After studying the intra-particle diffusion effect on HDS
of dibenzothiophenic compounds with full-size and crushed
NiMo/Al2 O3 hydrotreating catalysts, Chen et al. [11] pro-
posed that significant intra-particle diffusion resistance could
reduce the reaction rate of sulphur removal. In addition, we
also prepared the eggshell MoS2 /Al2 O3 catalysts previously,
which could remarkably reduce the internal diffusion resis-
tance and showed higher total sulfur removal activity [17].
However, conventional HDS catalysts are generally consti-
tuted of alumina-supported small MoS2 slabs promoted by
cobalt. Hence, it is reasonably speculated that the catalysts
with similar eggshell thicknesses of Co and Mo, which show
perfect synergetic effect, would display the best catalytic per-
formance in selective HDS reaction.
For the preparation of eggshell catalysts, various methods
have been developed, such as coating method [18], deposition

∗ Corresponding author. Tel: +86-532-86981716; Fax: +86-532-86981787; E-mail: cgliu.upc.edu.cn@gmail.com, ymchai.upc.edu.cn@gmail.com

This work was supported by grants from the Major State Basic Research Development Program of China (“973” Program, 2010CB226905), the National
Natural Science Foundation of China (Grant Nos. 21006128 and 21106185), the Research Fund for the Doctoral Program of Higher Education of China (Grant
No. 20100133120007), the Shandong Provincial Natural Science Foundation of China (ZR2011BQ002), the Fundamental Research Funds for the Central
Universities and the Graduate Innovation Project of China University of Petroleum (Grant No. CXZD11-06).

Copyright©2012, Dalian Institute of Chemical Physics, Chinese Academy of Sciences. All rights reserved.
doi:10.1016/S1003-9953(11)60354-X
 Journal of Natural Gas Chemistry Vol. 21 No. 2 2012
precipitation [19−21], pressing-disk technique [16], spray-
ing method [22] and diffusion-adsorption [23−25]. How-
ever, some drawbacks also exist in the normal preparation
of eggshell catalysts, including the long preparation period,
difficulty in control of the eggshell thickness and the content
of the active component, the high solvent cost and the low
mechanical strength.
In this study, we described a novel method of preparing
presulfided eggshell CoMoS/Al2 O3 catalysts and also evalu-
ated the activity and selectivity of the as-prepared catalysts in
selective HDS of FCC gasoline in a fixed-bed high pressure
micro-reactor, further revealing the effects of the reactant in-
ner diffusion on the catalysts performance.
2. Experimental
2.1. Preparation of eggshell catalysts
CoMoS/γ-Al2O3 catalysts were prepared as follows. So-
lution A was obtained by dissolving 3.82 g ammonium tre-
trathiomolybdate in 5 mL ethanolamine. A clear solution
B of 2.4 g cobalt nitrate, 2.4 g ethylenediamine tetracetic
acid and 3 mL ammonia water was obtained. Then, the co-
impregnation solution C was got by adding solution B to solu-
tion A under stirring. Next, the cylindrical γ-Al2 O3 extrudates
(20 g) with an external diameter of 1.3 mm, an average length
of 3 mm, a BET surface area of 269 m2 /g, a pore volume
of 0.64 cm3 /g and a BJH average pore diameter of 7.2 nm,
were impregnated with solution C and extrudate samples were
removed at various time intervals, which were subsequently
dried in an evaporator at 100 ◦ C for 30 min and finally calci-
nated at 500 ◦ C under a nitrogen flow (100 mL/min) for 3 h.
The average eggshell thickness was determined by scanning
electron microscopy (SEM) through examining the cross sec-
tion of five impregnated samples with random orientations.
The resulting CoMoS/γ-Al2O3 catalyst with eggshell thick-
ness of 0.2 mm was denoted as Egg-0.2 and the MoO3 and
CoO contents of the catalyst were 9.5 wt% and 2.5 wt%, re-
spectively.
2.2. Reference catalyst
The uniform CoMoS/γ-Al2 O3 catalyst was prepared by
incipient wetness impregnation of γ-Al2 O3 extrudates (20 g)
with an aqueous solution containing 3.82 g ammonium tre-
trathiomolybdate firstly dissolved in 5 mL ethylenediamine.
The impregnated catalyst was dried in an evaporator at
60 ◦ C for 6 h and calcinated at 250 ◦ C under nitrogen flow
(100 mL/min) for 3 h. Subsequently the loading of Co was
performed by incipient wetness method with a aqueous solu-
tion of 2.4 g cobalt nitrate and 2.4 g ethylenediamine tetracetic
acid, and finally calcinated at 500 ◦ C under a nitrogen flow
(100 mL/min) for 3 h. The uniform catalyst with the MoO3
and CoO contents of 9.5 wt% and 2.5 wt%, was denoted as
Hom-U.
195
2.3. Characterization of catalysts
A detailed description of all characterization techniques
have been provided elsewhere [17], and only a brief sum-
mary was given below. X-ray powder diffraction (XRD)
analysis was carried out using a PANalytical’s X’Pert PRO
diffractometer with Cu Kα radiation operated at 45 kV and
40 mA. The line distribution profiles of Co and Mo in the
cross section of the catalysts were measured by energy-
dispersion X-ray spectroscopy (EDS) on Hitachi S-4800. The
high-resolution transmission electron microscopy (HRTEM)
images of the samples were taken using a JEOL JEM-
2100 UHR microscope. IR spectra of adsorbed CO were
recorded on a Thermo Nicolet NEXUS IR spectrometer
equipped with a MCT detector.
2.4. Catalytic performance test
The catalytic tests for selective HDS of FCC gasoline over
the eggshell and uniform catalysts were carried out in a high-
pressure fixed-bed continuous flow reactor under the follow-
ing conditions: hydrogen pressure of 2 MPa, temperature of
240 to 280 ◦ C, LHSV of 4 h−1 , hydrogen/feed volumetric ra-
tio of 300/1 and catalyst loading of 10 mL.
The hydrocarbon compositions of the reactant feeds (as
seen in Table 1) and products were analyzed using a PONA-
GC (Agilent 7890N). The total sulfur content was determined
by Analytikjenas elemental analysis (Multi EA 3100). The
HDS of S-compounds and conversion of olefin (HYD) were
calculated as follows:
HDS (%) = (S f − S p)/Sf × 100
where, Sf and Sp represent the sulfur contents in the reactant
feeds and products, respectively.
HYD (%) = (Of − Op )/Of × 100
where, Of and Op are the olefin contents in reactant feeds and
products, respectively.
The catalyst selectivity factor S was defined in our previ-
ous study [17] for easily comparing the selectivity of different
catalysts. A catalyst with a larger S value has higher se-
lectivity, indicating a higher HDS rate with same olefin
saturation rate.
HDS selectivity index S = kHDS /kHYD
where, kHDS and kHYD are the apparent reaction rate constants
for the HDS of total sulfur and HYD of olefins, respectively.
Table 1. Properties of FCC gasoline
Properties Value
Density (g/cm3 , 15 ◦ C) 0.731
Sulfur (μg/L) 901.2
Hydrocarbon (vol%)
Paraffins 4.04
Isoparaffins 41.48
Olefins 30.78
Naphthenes 8.50
Aromatics 15.23
196 Bin Liu et al./ Journal of Natural Gas Chemistry Vol. 21 No. 2 2012

3. Results and discussion tributions in the catalyst extrudates, and also the dimension-
less penetration across the particle is a function of impreg-
3.1. Eggshell catalysts nation time. Therefore, the eggshell thicknesses of Co and
Mo could be easily regulated by controlling the impregnation
Figure 1 showsthe effect of impregnation time on the im- time.
pregnation depth. Obviously, CoMoS/γ-Al2 O3 catalysts with
sharp and deep eggshell profiles were prepared, and the im-
pregnation depth increased clearly with the prolonged impreg-
nation time. Meanwhile, in the impregnation process, the im-
pregnation depth is usually influenced by the impregnation
rate. According to the Washburn equation [3], the impreg-
nation rate was calculated from the slope of the linear fitting
of dimensionless penetration depth (ξ) against t1/2 data and
its value was about 0.016 mm/s1/2 .
Figure 2 shows the cross-sectional SEM images together
with Co and Mo line distribution profiles of Egg-0.2 and
Hom-U catalysts. Visibly, Co and Mo showed almost the
same distribution and mainly dispersed at surface layer over
Egg-0.2 catalyst, presenting an eggshell distribution. In com-
parison with that, Co and Mo distributions were very uniform
along the cross section of Hom-U catalyst.
According to the above analysis, we can conclude that the
diffusion rate is a key factor to determine the Co and Mo dis- Figure 1. Effect of impregnation time on impregnation depth

Figure 2. Co and Mo distributions of cross section of Egg-0.2 and Hom-U CoMoS/γ-Al2 O3 catalysts extrudates by EDS analysis
 Journal of Natural Gas Chemistry Vol. 21 No. 2 2012
3.2. Characterization of catalysts
Figure 3 shows the XRD patterns of Egg-0.2 and Hom-U
catalysts. All the samples displayed the similar characteristics
of diffraction peaks to γ-Al2 O3 and no visible new diffraction
peaks were observed. It implied that Co and Mo species
were either completely amorphous or composed of small crys-
tallites. Therefore, the active components were considered
evenly distributed on the surface of the support, indicating that
one-step impregnation method to obtain presulfided eggshell
CoMoS/γ-Al2 O3 catalysts would not affect the dispersion of
the active components, which was also confirmed by HRTEM
analysis.
Figure 3. XRD patterns of Egg-0.2 and Hom-U CoMoS/γ-Al2 O3 catalysts
Representative TEM micrographs of catalysts Egg-0.2
and Hom-U are shown in Figure 4. Accordingly, the
Figure 4. TEM images of Egg-0.2 and Hom-U catalysts
197
micrographs exhibited the well-known MoS2 slab-like struc-
ture. And the slab lengths and stacking numbers of MoS2
slabs of different catalysts were quantitatively compared
based on at least ten micrographs including 250−300 slabs
taken from different parts of each catalyst, and the calculated
average layer number and length of supported MoS2 slabs are
summarized in Table 2. It was found that the predominant slab
number and average length of MoS2 slabs of samples were
similar, and they did not show significant differences in the
dispersion or the morphology of MoS2 slabs.
Table 2. Slab length and stacking number of the catalysts
Samples Average size (nm) Average stacking number
Egg-0.2 4.18 1.98
Hom-U 4.36 1.92
IR spectra of CO adsorbed on Egg-0.2 and Hom-U cat-
alysts are presented in Figure 5. Compared with the spec-
tra obtained after CO adsorbed on presulfided MoS2 /γ-Al2 O3
catalyst [17], a new band at 2061 cm−1 appeared in the spectra
of the catalysts, due to CO adsorption on either Mo or Co cen-
ters related to CoMoS phase. Travert et al. [26] ascribed the
band at 2061 cm−1 to CO interacting either with a Co atom
or with a 5-fold coordinated Mo atom adjacent to a Co. The
relative areas of bands at 2114 cm−1 and 2061 cm−1 , which
showed the information on the nature and relative number of
active sites because of CO selective adsorption on the coordi-
natively unsaturated sites (CUS), were almost the same for the
eggshell and uniform catalysts, indicating minor difference in
the number of active sites for Egg-0.2 and Hom-U catalysts.
Based on the above analysis, the method used for the
preparation of eggshell catalyst would not affect the distribu-
tion or morphology of the active components, as well as the
nature or relative number of the active sites. Thus, it could
be reasonably assumed that the active component structures
of the eggshell and uniform catalysts were similar, and the
differences in activity and/or selectivity could be mainly as-
cribed to the different distributions of the active components
in the catalysts.
Figure 5. IR spectra of CO adsorbed on Egg-0.2 and Hom-U catalysts
198 Bin Liu et al./ Journal of Natural Gas Chemistry Vol. 21 No. 2 2012
3.3. Catalytic performance test
The catalytic performances of presulfided Egg-0.2 and
Hom-U CoMoS/γ-Al2 O3 catalysts are presented in Figure 6.
With the increase of reaction temperatures, the total sul-
fur compounds removal activity increased noticeably. At
the same temperature, the eggshell catalyst (Egg-0.2) always
showed higher HDS conversion compared with that of the uni-
form catalyst (Hom-U), indicating that the substantial inter-
nal diffusion limitation in Hom-U catalyst may cause lower
HDS activity. Similar results were also obtained by Chen
et al. [11], who studied the intra-particle diffusion effect
on HDS of dibenzothiophenic compounds with full-size and
crushed NiMo/Al2 O3 hydrotreating catalysts. Therefore, the
eggshell catalyst with a thin layer of active material supported
on the outer surface of the catalyst particle could shorten the
diffusion path of the reactant and thus weaken the substan-
tial internal diffusion limitation in the uniform catalyst, which
induced higher HDS activity. However, as seen in Figure 6,
Egg-0.2 and Hom-U catalysts showed almost the same olefins
HYD conversion activity, implying that the internal diffusion
resistance effect on HYD of olefins might be neglected. So,
it was possible to improve the HDS of gasoline by eggshell
catalyst to obtain better selective HDS performance.
Figure 6. Catalytic performances of Egg-0.2 and Hom-U catalysts. Reaction
conditions: hydrogen pressure of 2 MPa, gas to liquid ratio of 300 Nm3 /m3 ,
LHSV of 4 h−1
For FCC gasoline, it mainly contains sulfur compo-
nents of thiophenes [27,28] and the HDS activity of thio-
phenes can be influenced by their structures, and therefore
may be affected differently by internal diffusion. More-
over, the effects of internal diffusion resistance on different
structure thiophenes are still unclear. Based on the num-
ber of substituent groups bonded to thiophene molecules,
all the thiophenes (Ts) could be divided into five groups:
thiophene (T), methylthiophenes (MTs), dimethylthiophenes
(DMTs), 3-carbons-alkylthiophenes (3CTs) and 4-carbons-
alkylthiophenes (4CTs) [29]. We compared the catalyst
effectiveness factors of each group Ts removal over the
eggshell and uniform catalysts, and it can be assumed that
the external transmission showed the same effect on the two
catalysts. Thus, the catalyst effectiveness factors, indicating
the intra-particle diffusion effect, were calculated according
to the equation [11]: k = ηkintrinstic , where k and kintrinstic are
the apparent and intrinsic reaction rate constants. Moreover,
intrinsic reaction rate constant was only related to the reaction
temperature. So it was assumed that the eggshell and uni-
form catalysts had the same intrinsic reaction rate constants
under the same reaction conditions. The ratios of the catalyst
effectiveness factors can be obtained by calculating the ratio
of the apparent reaction rate constants.
In Table 3, the relative catalyst effectiveness factors for
each group Ts removal over Egg-0.2 and Hom-U catalysts
are presented. Taking into account of first-order kinetics for
each group Ts, the values given are the ratios of the appar-
ent reaction rate constants of the eggshell and uniform cat-
alysts, and Hom-U catalyst was considered as the reference
catalyst. As seen in Table 3, the values increased with the
increasing reaction temperature, showing that the eggshell
catalyst could effectively reduce the internal diffusion at
higher temperatures. That was because temperature had a
greater impact on the intrinsic rate constant than that on the
effectiveness diffusivity (De ), contributing to the increase of
the Thiele modulus (φ), and thus led to much prominent in-
ternal diffusion effect in uniform catalyst at higher temper-
atures. It was also observed that the highest values in Ta-
ble 3 were estimated for T, next appeared the values of MTs
followed by the values of DMTs, all of which were higher
than those of 3CTs and 4CTs showing the lowest values at
the same temperature. It could be explained as follows: the
intrinsic rate constant of different group Ts varied greatly,
while the differences in effectiveness diffusivity were mi-
nor because of relatively slight differences in molecular size
among all the Ts, and therefore the φ value of each group
Ts was mainly associated with the intrinsic rate constant of
different group Ts. That was to say, the Ts with higher sul-
fur removal rates, such as T and MTs, showed larger φ values
than those with larger steric effects, such as DMTs, 3CTs and
4CTs, indicating more severe internal diffusion effect, which
was consistent with the higher relative catalyst effectiveness
factor values. Hence, the eggshell catalyst could conspicu-
ously decrease the internal diffusion inhibition effect on HDS
of Ts, and apparently the effect decreased in the order of
T>MTs>DMTs>3CTs>4CTs.
Table 3. Relative catalyst effectiveness factors
for thiophenes hydrodesulfurization
t/ ◦ C
S-compounds
240 260 280
T 1.451 1.591 1.802
MTs 1.314 1.449 1.588
DMTs 1.195 1.365 1.479
3CTs 1.127 1.242 1.367
4CTs 1.089 1.215 1.243
Reaction conditions: hydrogen pressure of 2 MPa, gas to liquid ra-
tio of 300 Nm3 /m3 , LHSV of 4 h−1
The catalyst selectivity factor (S) was calculated with a
ratio of the pseudo-second-order reaction rate constants for
 Journal of Natural Gas Chemistry Vol. 21 No. 2 2012
the HDS of total sulfur to the pseudo-first-order reaction rate
constants for the HYD of olefins. The catalyst with larger S
value presented higher selectivity, which is shown in Figure 7.
It could be seen that the eggshell catalyst (Egg-0.2) always
had higher S at different temperatures ranging from 240 ◦ C
to 280 ◦ C, indicating significant intra-particle diffusion effect
on selective HDS of FCC gasoline. At 260 ◦ C, the highest
HDS selectivity index was obtained. That was because the
HYD reaction rate of olefins dramatically increased when the
temperature was higher than 240 ◦ C especially higher than
260 ◦ C [30], and the further enhanced HYD activity of olefins
which was higher than that of S-compounds HDS led to the
decreased selectivity index at higher temperatures. Therefore,
it could be concluded that the eggshell catalyst, in which a thin
layer of active material is supported on the outer surface of the
catalyst particles, could decrease the internal diffusion effect,
thus showing highly selective HDS activity for FCC gasoline.
Figure 7. HDS selectivity index (S) of Egg-0.2 and Hom-U
CoMoS/γ-Al2 O3 catalysts. Reaction conditions: hydrogen pressure of
2 MPa, gas to liquid ratio of 300 Nm3 /m3 , LHSV of 4 h−1
4. Conclusions
The presulfided eggshell CoMoS/γ-Al2 O3 catalyst with
sharp and deep Co and Mo concentration profiles is prepared
by one-step impregnation method. Using this method, the
eggshell thicknesses of Co and Mo could be easily regulated
by controlling the impregnation time. According to the re-
sults characterized by EDS, XRD, HRTEM and FT-IR of ad-
sorbed CO, the catalysts with eggshell and uniform distribu-
tions have almost similar active component structures, nature
and/or amount of active sites, and the differences in activity
and/or selectivity are mainly a consequence of different dis-
tributions of the active components on the catalysts. Catalytic
performance evaluation in selective HDS of FCC gasoline
shows that significant internal diffusion inhibition effect on
HDS of Ts is present especially in the uniform catalyst, which
decreases in the order of T>MTs>DMTs>3CTs>4CTs. The
eggshell catalyst could remarkably reduce such an internal
diffusion inhibition effect because of a short diffusion path
of the reactants, thus showing higher HDS selectivity.
199
Acknowledgements
This work was supported by grants from the Major State
Basic Research Development Program of China (“973” Program,
2010CB226905), the National Natural Science Foundation of China
(Grant Nos. 21006128 and 21106185), the Research Fund for
the Doctoral Program of Higher Education of China (Grant No.
20100133120007), the Shandong Provincial Natural Science Foun-
dation of China (ZR2011BQ002), the Fundamental Research Funds
for the Central Universities and the Graduate Innovation Project of
China University of Petroleum (Grant No. CXZD11-06).
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