Journal of Molecular Catalysis A: Chemical 408 (2015) 221227

Contents lists available at ScienceDirect

Journal of Molecular Catalysis A: Chemical

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

Catalytic oxidation of benzene over MnOx /TiO2 catalysts and the

mechanism study
Junlin Zeng a,b , Xiaolong Liu a , Jian Wang a,c , Hanlei Lv a , Tingyu Zhu a,
a
Beijing Research Centre of Process Pollution Control, National Engineering Laboratory for Hydrometallurgical Cleaner Production Technology,
Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China
b
Chemistry and Chemical Engineering, Guizhou University, Guiyang, Guizhou 550025, China
c
University of Chinese Academy of Sciences, Beijing 100049, China

a r t i c l e

i n f o

Article history:
Received 5 June 2015
Received in revised form 16 July 2015
Accepted 18 July 2015
Available online 29 July 2015
Keywords:
Catalytic oxidation
Benzene
Manganese
Reaction mechanism

a b s t r a c t
MOx /TiO2 composites with various metal species (M = Mn, Ce, Co, Fe) were synthesized and employed as
in the catalytic oxidation of benzene. Among those materials, MnOx /TiO2 showed the highest catalytic
efciency. The catalytic activities of MnOx /TiO2 with different MnOx contents were also studied. XRD,
BET, SEM, TEM, and XPS characterizations were conducted to analyze the physiochemical properties of
the MnOx /TiO2 catalysts. Moreover, the reaction mechanism of benzene oxidation over MnOx /TiO2 was
studied through the in situ FTIR experiments.
2015 Elsevier B.V. All rights reserved.

1. Introduction
Volatile organic compounds (VOCs) emitted from industrial process and transportation activities are harmful to the atmosphere
and human health [13]. Among the strategies explored for VOCs
removal, catalytic oxidation is regarded as the most promising
pathway to reduce VOCs emissions due to its advantages of high
efciency, low temperature, and high selectivity to harmless products [4,5].
In recent years, numerous catalysts have been explored, including noble metals [68] and transition-metal oxides [919]. The
noble metal catalysts such as Pd and Pt-based catalysts have
attracted increasing attention for their excellent catalytic activities.
However, the drawbacks of high costs and being likely to produce
multi-chlorinated byproducts have greatly restricted their applications. Non-noble metal catalysts (mainly Co, Mn, Ce and Fe) have
also demonstrated a great catalytic performance in VOCs oxidations
[2022]. Moreover, the catalysts showed great advantages of lower
costs and higher resistance to poison [23,24].
Within the non-noble metal catalysts developed, MnOx -based
materials have gained increasing importance because of its high

Corresponding author.
E-mail address: tyzhu@ipe.ac.cn (T. Zhu).
http://dx.doi.org/10.1016/j.molcata.2015.07.024
1381-1169/ 2015 Elsevier B.V. All rights reserved.

efciency, which was ascribed to the reactive oxygen species

of MnOx . Aguero et al. [25] prepared the MnOx /Al2 O3 and the
material revealed as a well-dened catalyst in binary VOCs oxidation. For MnOx -containing composites, Wang et al. [26] reported
CeO2 MnOx catalytic oxidation of benzene with high efciency,
and CeO2 enhance the transfer ability of oxygen species. The mesoporous MnCe composite exhibited higher catalytic activity in the
total oxidation of VOCs [27].
Based on previous work, the Mn-containing materials are useful for developing a stable catalyst with low costs and high activity,
and the mechanism study are helpful to optimize the MnOx -based
catalytic system. However, the mechanism research such as the
organic intermediates, the interaction between the Mn active center and organic species, and the reaction path, are far less explored.
Herein, we present MnOx /TiO2 catalyzed benzene oxidation and its
mechanism studies.

2. Experimental
2.1. Catalyst preparation
MOx /TiO2 catalysts were prepared using impregnation method
with the weight percentages of MOx and TiO2 being 3 wt.%
and 97 wt.%, respectively. In a typical preparation for CeO2 /TiO2 ,
Ce(NO3 )2 6H2 O (0.391 g, 0.9 mmol) was dissolved in 20 mL of

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J. Zeng et al. / Journal of Molecular Catalysis A: Chemical 408 (2015) 221227

100

MnOx(3%)/TiO2
CeO2(3%)/TiO2

Conversion%

80

Co3O4(3%)/TiO
Fe2O3(3%)/TiO2

60

TiO2

40

20

(a)

100

100

Conversion%

80

150

200

250
300
350
o
Temperature/ C

400

450

MnOx(1%)/TiO2
MnOx(3%)/TiO2
MnOx(5%)/TiO2
MnOx(10%)/TiO2

60

MnOx(15%)/TiO2
MnOx(20%)/TiO2

40

20

(b)

0
100

150

200

250

300

350

400

Temperature/ C
Fig. 1. Benzene conversions as a function of reaction temperature over (a) MOx /TiO2
(M = Mn, Ce, Co, Fe) and (b) MnOx (y)/TiO2 (y = 1%, 3%, 5%, 10%, 15%, 20%).
Fig. 2. XRD patterns of (a) MOx /TiO2 (M = Mn, Ce, Co, Fe) and (b) MnOx (y)/TiO2
(y = 1%, 3%, 5%, 10%, 15%, 20%).

deionized water, and the solution was then added into 80 mL of

aqueous suspension of TiO2 (5 g, 62.6 mmol). The mixture was
stirred for 2 h at 60 C. The solvent was then removed with rotary
evaporation at 60 C and kept for 2 h. The resulting sample was
dried at 110 C for 10 h and calcined at 500 C for 4 h, giving the
expected CeO2 /TiO2 catalyst. Similarly, MnOx /TiO2 , Co3 O4 /TiO2 ,
Fe3 O4 /TiO2 catalysts were prepared adopting the same method.
Additionally, MnOx (y)/TiO2 catalysts were prepared through the
same method, where y represents the weight percentage MnOx
(y = 1%, 3%, 5%, 10%, 15%, 20%).

2.2. Catalyst characterization

The samples were characterized using the following equipments. X-ray diffraction (XRD) patterns were recorded by Cu K
radiation on Netherlands PANalytical X Pert PRO diffractometer
for phase identication in the samples. Specic surface areas (BET)
were recorded by the US Quanta Chromes Autosorb-iQ automatic
instrument. Scanning electron microscope (SEM) images were
obtained using Hitachi S-4800. Transmission electron microscope
(TEM) images and high-resolution transmission electron microscope (HRTEM) images were taken on JEOL JEM-2100 microscope
operated at 120 kV. X-ray photoelectron spectroscopy (XPS) measurements were conducted on Thermo escalab 250Xi X-ray using
an Al K source.

Table 1
The physical properties of MnOx (y)/TiO2 .
Sample

Specic surface
area/(m2 g1 )

Particle size
(nm)a

Particle size
(nm)b

TiO2
MnOx (1%)/TiO2
MnOx (3%)/TiO2
MnOx (5%)/TiO2
MnOx (10%)/TiO2
MnOx (15%)/TiO2
MnOx (20%)/TiO2

51.3
50.2
49.7
49.5
49.6
48.2
48.4

25.0
25.3
25.5
25.1
25.6
26.0
25.9

25.0
25.0
25.0
25.0
25.0
25.0
25.0

a
Data determined based on the XRD results according to the Scherrer equation
using the FWHM of the peak at 25.4 (2).
b
Data determined based on the TEM results.

2.3. Catalytic evaluation

Catalytic activities of the catalysts were evaluated in a continuous ow xed-bed quartz microreactor (i.d. = 4 mm) from 100
to 450 C with 100 mg of catalyst (6080 mesh). Benzene was
introduced into reactant ow with its concentration of 500 ppm,
and the O2 concentration is 20%. The total ow ratio of the reactant mixture was 100 mL/min with the weight hourly space velocity
(WHSV) of 60,000 mL/(gh). Analysis of the reactants and products
were performed on-line with a gas chromatographymass spectrometry (GCMS-QP2010 Plus, Shimadzu).

J. Zeng et al. / Journal of Molecular Catalysis A: Chemical 408 (2015) 221227

223

Fig. 3. TEM images (a, d, g represent y = 5%, 10%, 15%, respectively), HRTEM images (b, e, h represent y = 5%, 10%, 15%, respectively) and EDX spectra (c, f, i represent y = 5%,
10%, 15%, respectively) of the MnOx (y)/TiO2 .

2.4. In situ FTIR experiments

FTIR spectra were collected with an FTIR spectrometer (Nicolet
6700, Thermo) equipped with an MCT detector (cooled by liquid
nitrogen) and a stainless steel IR cell (CaF2 windows). Primarily, the
IR cell was ushed by owing Ar (100 mL/min for 2 h) to ensure that
it was clean. Then the powder sample (about 45 mg) was pressed
into a supported disk and oxidized at 300 C for 1 h in a 20% O2 /Ar
(100 mL/min) stream. Subsequently, the sample was cooled down
to desired temperature and collected background in owing 20%
O2 /Ar stream. Eventually, the IR spectra were collected at different times in owing 20% O2 /Ar and 50% benzene (100 mL/min)
stream.
In order to examine the effect of the absorbed oxygen in catalytic
oxidation of benzene, the powder sample was pressed into a supported disk and desorbed at 300 C for 1 h in an Ar (100 mL/min)
stream. Then the sample was cooled down to desired temperature and collected background in owing Ar. Finally, the IR spectra
were collected at different times in owing Ar and 50% benzene
(100 mL/min) stream.

Table 2
The XPS data of MnOx (y)/TiO2 catalysts.
Catalyst

Mn2+
(%)

Mn3+
(%)

Mn4+
(%)

Olatt
(%)

Oads
(%)

Osur
(%)

Oads /Olatt

MnOx
MnOx
MnOx
MnOx

7
6.6
7
1.66

22.8
64.1
77.46
83.3

70.2
29.3
15.49
15.01

67.6
70.76
78.26
85.09

25.35
20
18.8
14.58

7.04
9.23
2.8
0.92

0.375
0.283
0.24
0.17

(1%)/TiO2
(5%)/TiO2
(15%)/TiO2
(20%)/TiO2

3. Results and discussion

3.1. Catalytic performance
The catalytic oxidation of benzene over all catalysts was established within 100450 C. As shown in Fig. 1a, the catalytic activity
increased in sequence of TiO2 , CeO2 /TiO2 , Fe2 O3 /TiO2 , Co3 O4 /TiO2 ,
and MnOx /TiO2 , and T50 (50% benzene conversion rate corresponding to the reaction temperature) for the catalysts were 418 C,
417 C, 332 C, 320 C, and 295 C, respectively. MnOx /TiO2 showed
the lowest complete oxidation temperature of 350 C, revealing

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J. Zeng et al. / Journal of Molecular Catalysis A: Chemical 408 (2015) 221227

O1s

MnOx(1%)/TiO2

536

Intensity(a.u.)

Intensity(a.u.)

O1s

Olatt

Osur

Oads

534

532

530

MnOx(5%)/TiO2
Olatt
Oads

536

528

Osur

534

530

528

O1s

Intensity(a.u.)

Intensity(a.u.)

O1s

MnOx(15%)/TiO2
Oads

Olatt

Osur

536

532

Binding energy(eV)

Binding energy(eV)

534

Olatt
MnOx(20%)/TiO2
Oads
Osur

532

530

528

Binding energy(eV)

536

534

532

530

528

Binding energy(eV)

Fig. 4. XPS spectra of O 1s for MnOx (y)/TiO2 of (a), (b), (c), (d) (y = 1%, 5%, 15%, 20%).

that the Mn-based catalyst exhibit the highest catalytic activity. Accordingly, a series of MnOx /TiO2 catalysts with different
MnOx contents (120 wt.%) were prepared. The samples were then
employed in the catalytic oxidation of benzene and the results
were shown in Fig. 1b. It can be seen that the catalytic activity rose as the increase of the MnOx weight percentage within
the range of (110 wt.%). MnOx (10%)/TiO2 contributed the lowest
complete oxidation temperature of 325 C. However, the samples
of MnOx (10%)/TiO2 , MnOx (15%)/TiO2 and MnOx (20%)/TiO2 showed
similar catalytic performance, revealing that further increase of the
MnOx amount led to no higher efciency. Noteworthy, no byproducts were observed in our experiments. In order to evaluate the
catalytic stability of the samples, on-stream benzene oxidation
experiments were performed at 325 C for 12 h. The results are
shown in Fig. S1. The samples of MnOx (10%)/TiO2 , MnOx (15%)/TiO2 ,
and MnOx (20%)/TiO2 gave the complete oxidation, whereas the
conversions for MnOx (3%)/TiO2 and MnOx (5%)/TiO2 were 83% and
92%, respectively and it was consistent with Fig. 1b. Therefore, it
was disclosed that the MnOx (y)/TiO2 have extremely stability.
3.2. Characterization results and analysis
From the XRD patterns of the as-prepared MOx /TiO2 samples
in Fig. 2a, it can be seen that these materials exhibited 25.4 ,
48.1 , 53.6 , 55.2 (2) peaks due to anatase TiO2 (PDF 21-1272),
and 27.5 , 36.2 , 54.4 (2) peaks attributable to rutile TiO2 (PDF

21-1276). Any MnOx , CeO2 , Co3 O4 , and Fe2 O3 phases were not
observed, possibly because that little MOx was loaded leading to
well-dispersion of the small crystallite particles [2830]. The XRD
patterns of MnOx (y)/TiO2 catalysts were shown in Fig. 2b. For
the samples with MnOx contents above 5%, the diffraction peaks
at 28.8 , 42.9 , 56.7 (2) ascribed to MnO2 (PDF 24-0735) were
observed, and the peak intensity was gradually strengthened as
the increasing content of MnOx . When the MnOx content reached
to 20%, the diffraction peaks at 33.0 , 55.3 , 65.9 (2) characteristic of Mn2 O3 (PDF 41-1442) appeared. Therefore, MnOx (20%)/TiO2
sample contains at least two valence states of Mn (Mn4+ , Mn3+ ). For
other catalysts, multiple valence states might also exist, whereas
the XRD diffraction signals could not be detected possibly due to
their less multi-valence contents or the detection limitation.
The N2 adsorptiondesorption isotherms and BJH pore size distribution analysis were performed to evaluate the specic surface
area and the particle size of the MnOx (y)/TiO2 catalysts. As shown
in Table 1, with the increased of MnOx contents, the specic surface
area showed a very slight decreasing tendency. The particles size
determined based on XRD and TEM results were also illustrated
with an average value of 25 nm, showing no signicant difference.
The SEM images of MnOx (1%)/TiO2 and MnOx (20%)/TiO2 are
listed as Fig. S2. As shown in Fig.S2a, the sample presents a uniform size and round structure, and the particles are well dispersed.
The morphology of MnOx (1%)/TiO2 showed no apparent difference
from that of MnOx (20%)/TiO2 shown in Fig.S2b. Hence, it could be

T=275 C

h
g

-6

-1

TOF(x10 S )

15

1313

1425
1410
1383
1377
1354

0.05a.u.

20

225

1581
1572

J. Zeng et al. / Journal of Molecular Catalysis A: Chemical 408 (2015) 221227

10

T=225 C

b
a

1800
0.20

0.25

0.30

0.35

1700

0.40

1400

1300

1200

Wavenumbers(cm )
Fig. 6. In situ FTIR spectra of TiO2 collected at 250 C after (a) 10, (b) 30 min on
500 ppm benzene/Ar stream and MnOx (5%)/TiO2 collected at 250 C after (c) 1, (d)
3, (e) 10, (f) 20, (g) 30, (h) 60 min on 500 ppm benzene/Ar stream.

1572

in Oads /Olatt molar ratio. TOF were calculated according to the molar
amount of Mn in total catalyst. Accordingly, a higher Oads concentration was benecial for improving catalytic performance [40],
since surface adsorbed oxygen could attack an organic molecule
[41]. As shown in Table 2, with the increase of Mn content, the Oads
concentration and Oads /Olatt molar ratio decreased. However, the
catalysts with lower Mn loadings gave the higher Oads /Olatt ratios,
and generally also better Mn dispersion. Therefore, Mn is more easily exposed for the catalytic oxidation. Hence, it was also reasonable
that better Mn dispersion was responsible for higher TOF value,
which might be the reason behind the correlation between TOF
and Oads /Olatt ratios. Elaborately designed work would be needed
to further explore the correlations.
As shown in Fig. 6a and b, FTIR spectra were collected with
different time intervals during the adsorption of benzene/Ar onto
the pure titania support at 250 C and no band was observed. For
MnOx (5%)/TiO2 /Ar, FTIR spectra were collected with different time
distances during the adsorption of benzene/Ar at 250 C, and the
results were shown in Fig. 6ch. In particular, band at 1572 cm1
was assigned to the surface phenolate species (C C stretching
vibrations) [42], and bands at 1425, 1313 cm1 were assigned
to the maleate species (Olen rocking vibration) [4346]. In

1425
1407
1383
1376
1368
1354

0.05a.u.

concluded that the increase of the MnOx content within the range
of (120%) basically led to no obvious morphology change of the
MnOx (y)/TiO2 samples.
Fig. 3a, d and g showed the TEM images of MnOx (5%)/TiO2 ,
MnOx (10%)/TiO2 , and MnOx (15%)/TiO2 and all the catalysts showed
an average diameter of 25 nm, which is consistent with the Scherrer formula calculated value. With the increase of the MnOx
contents, no signicant aggregation was observed, and the samples showed little difference in morphology. Fig. 3b, e and h
presented the HRTEM images of MnOx (5%)/TiO2 , MnOx (10%)/TiO2 ,
and MnOx (15%)/TiO2 , respectively. As shown in the HRTEM images,
anatase nanocrystals with 0.35 nm lattice spacing of (1 0 1) facet
and rutile nanocrystals with 0.32 nm lattice spacing of (1 1 0) facet
were observed. In addition, no crystalline manganese oxide with
clear lattice spacings were observed. In order to analyze the MnOx
species, their corresponding EDX spectra were collected and illustrated as Fig. 3c, f and i. The EDX spectra exposed that Ti, O, Mn were
detected, and with the increase of MnOx loadings, the Mn contents
heightened obviously. It has been reported that MnOx mainly exists
with an amorphous structure in the MnOx -based materials [21],
which makes the surface MnOx hard to identify in the regular
TEM images. Fig. S3 showed the TEM images of MnOx (5%)/TiO2 ,
MnOx (10%)/TiO2 , and MnOx (15%)/TiO2 before (S3ac) and after
(S3df) the reaction, and the morphologies showed no apparent
difference.
Table 2 showed the XPS results of MnOx (y)/TiO2 and it could be
conrmed the coexistence of three kinds of Mn species [31], Mn2+ ,
Mn3+ , Mn4+ and three sorts of oxygen species [3133,28], surface
lattice oxygen (Olatt , O2 ), adsorbed oxygen (Oads , e.g.,O2 , O2 2 , or
O ), and adsorbed OH groups or molecular water, on the surface of
the catalysts.
The XPS spectra of Mn 2p are displayed in Fig. S4. As shown
in Fig. S4a and b, the spectrum of Mn 2p is one asymmetrical signal which can be decomposed into three components at BE = 640.8,
641.8, 641.3 eV which are assigned to the surface Mn2+ , Mn3+ , Mn4+
species [34]. The surface Mn (Mn2+ , Mn3+ , Mn4+ ) contents were calculated by quantitative analysis method in Table 2. It showed that
Mn3+ and Mn4+ dominate in the catalysts, and they were generally
considered as catalytically active components, and higher surface
Mn3+ and Mn4+ concentrations will introduce more active oxygen
which is related to the catalytic performance [3436]. The spectra
of O 1s were described in Fig. 4a and b. The O 1s spectra deconvolve
into three components at BE = 529.8, 531.4, 533.3 eV, assignable to
Olatt , Oads , Osur species [3739], respectively. As shown in Fig. 5, the
TOF per MnOx species at each temperature increased with the rise

1500

-1

Oads/Olatt molar ratio (mol/mol)

Fig. 5. TOF per MnOx at different temperature as a function of Oads /Olatt molar ratio
of MnOx (y)/TiO2 (y = 1%, 5%, 15%, 20%).

1600

1313

0
0.15

d
c

f
e
d
c
b
a

1800

1700

1600

1500

1400

1300

1200

-1

Wavenumbers(cm )
Fig. 7. In situ FTIR spectra of MnOx (5%)/TiO2 collected at 250 C after (a) 1, (b) 3, (c)
10, (d) 20, (e) 30, (f) 60 min on 500 ppm benzene/20%O2 /Ar stream.

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J. Zeng et al. / Journal of Molecular Catalysis A: Chemical 408 (2015) 221227

Fig. 8. Proposed mechanism for the catalytic oxidation of benzene over MnOx /TiO2 catalysts.

addition, bands at 1383 (CH in plane bending), 1377 (CH2 stretching vibration), 1354 (CH3 stretching vibration) cm1 were assigned
to the acetate species [47,48] and band at 1410 cm1 was assigned
to o-benzoquinone [45], respectively. As the reaction proceeding, a
low intensity band at 1581 cm1 was emerged that can be deemed
the unsaturated species (C C stretching vibrations) [49,50], and in
this research it could be phenolate other than benzene. If the band
at 1581 cm1 was ascribed to benzene, it should be observed in
the Fig. 6a and b. Consequently, it could be concluded that benzene decomposed over MnOx (5%)/TiO2 at 250 C under Ar, and
phenolate, o-benzoquinone, maleate, and acetate species were
accordingly produced. In combination with the XPS analysis, it was
believed that the Oads species (active oxygen) play a major role in
the oxidation process.
As shown in Fig. 7af, MnOx (5%)/TiO2 FTIR spectra were collected during the adsorption of benzene/20%O2 /Ar at 250 C. In
comparison to Fig. 6, similar bands at 1572, 1425, 1383, 1377,
1354, 1313 cm1 due to different organic species were found
in Fig. 7. Meanwhile, band at 1410 cm1 shifted to 1407 cm1 ,
band at 1368 cm1 was emerged and band at 1581 cm1 disappeared. Hence, it could be proposed that benzene was oxidized
into phenolate, o-benzoquinone, maleate and acetate species over
MnOx (5%)/TiO2 at 250 C in the presence of an O2 /Ar mixture. By the
comparison of Figs. 6 and 7, it could be concluded that the oxidation
of benzene proceeds in the same path under oxygen-rich or oxygenfree conditions. It was believed that benzene reacted with the active
oxygen species of the catalyst, other than the gas oxygen. While
the active oxygen was consumed, the gas oxygen was adsorbed
on the catalyst and transformed into active oxygen species,
accomplishing the catalytic oxidation process on the catalyst
surface.
Based on the results of in situ FTIR experiments, a reaction mechanism was proposed and shown in Fig. 8. As one can see, benzene (A)
rst reacts with the active Mn center, giving phenolate (B) species
with two conjugated structures (C). The oxygen-containing group is
generally considered as an electron-donating and ortho-para positioned director. Accordingly, the phenolate species can be easily
oxidized into o-benzoquinone (D) and p-benzoquinone (E). However, p-benzoquinone (E) was not observed possibly due to its high
reactivity. The quinone species were then further oxidized. With
the catalyst promoting and the attack of the active oxygen species,
a ring opening occurred, affording the small molecule intermediates, such as maleate (F) and acetate (G) species, which were
indeed observed in the in situ experiments. Furthermore, oxidation of maleate (F) and acetate (G) species gave the nal inorganic
products of CO2 , CO, and H2 O.

4. Conclusion
MOx /TiO2 (M = Mn, Ce, Co, Fe) samples with certain contents
were prepared and employed as the catalysts for benzene oxidation, and MnOx /TiO2 showed the highest catalytic efciency. As
the MnOx content increased, the catalytic activity also showed an
increasing tendency. However, the catalytic activity increased little when the MnOx content was above 5%. XPS characterizations
revealed that Oads species (active oxygen) play a major role in the
oxidation process. Many organic intermediates were observed in
the in situ FTIR experiments. Accordingly, a reaction mechanism
for the catalytic oxidation of benzene over MnOx /TiO2 was proposed, which is meaningful to the future development of the VOCs
removal catalysts.
Acknowledgements
This work was supported by Project of the Natural Science Foundation of China (No. 21177129), and the Strategic Priority Research
Program of the Chinese Academy of Sciences (No. XDB05050100).
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in
the online version, at http://dx.doi.org/10.1016/j.molcata.2015.07.
024
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