Hollow anatase TiO2 nanoparticles with excellent catalytic activity for dichloromethane combustion

Article abstract of DOI:10.1039/c6ra06400k

Toward the design of efficient nanocatalysts, hollow anatase TiO₂ nanoparticles around 11.4 nm in size were prepared by a cetyltrimethylammonium bromide (CTAB)-assisted hydrothermal method. The catalyst showed high catalytic activity for dichloromethane (DCM) combustion, exhibiting 90% DCM conversion at 201 °C. The satisfactory performance of the catalyst was attributed to its hollow texture with many active sites, and the large number of moderately strong acidic sites on the hollow TiO₂ surface.

Full text of DOI:10.1039/c6ra06400k

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Hollow anatase TiO nanoparticles with excellent catalytic activity
2
for dichloromethane combustion
Received 00th 00000 2016,
Accepted 00th 00000 20xx
a
a
a
a
a
b
Haifeng Huang, Xixiong Zhang, Xiaojia Jiang, kang Dou, Zhiyi Ni and Hanfeng Lu *
DOI: 10.1039/x0xx00000x
www.rsc.org/
Toward the design of efficient nanocatalysts, hollow anatase TiO
2
groups of catalysts to form reactive intermediates, which can be
1
7,18
oxidized to carbon dioxide.
It is believed that the activity
nanoparticles with around 11.4 nm were prepared by
cetyltrimethylammonium bromide (CTAB) -assisted hydrothermal
method. This catalyst delivered a high catalytic activity for
dichloromethane (DCM) combustion, in particular, the catalyst
for catalytic combustion of DCM is usually determined by
several key factors such as surface acidity and redox
21, 22
properties.
The strength and the amount of medium and
strong acidic sites would be beneficial for the chemisorption of
exhibited 90% DCM conversion at 201 °C. The satisfactory DCM molecules onto the hydroxyl groups of the catalyst
5, 23
performance of the catalyst can be contributed to the hollow surface.
Metal oxide catalysts with strong acidic surface
show a very high catalytic activity in the combustion of
texture with rich active sites and the high amount of moderately
strong acidic sites on the hollow TiO surface.
2
4ꢀ25
CVOCs,
however, coke formation readily occurs on
2
catalysts, leading to bad stability and restricting their
2
6
development. Therefore, it is meaningful to adjust the
structure of metal oxide materials, such as Al , SiO , and
TiO , to ensure the high catalytic activity and stability for
2
O
3
2
Chlorinated volatile organic compounds (CVOCs) are
poisonous pollutants considered as the most harmful organic
contaminants because of their acute toxicity and strong
bioaccumulation potential. Abatement of alkyl chloride
pollutants, such as dichloromethane (DCM), 1, 2ꢀ
dichloroethane (DCE) and trichloroethylene (TCE), has gained
2
CVOC combustion, especially for TiO
acidic species among metal oxides.
2
who is more resistant to
27ꢀ29
2
TiO have various
crystal structures, which can be readily controlled. Different
TiO crystal structures may exhibit different catalytic activities;
2
thus, regulating and controlling the crystal structures may help
us find an optimum catalyst. Herein, we reported a hollow
considerable attention because of increasing concern for
1
environmental protection.
Among various available
anatase TiO
2 2
(TiO ꢀHA) nanoparticle catalyst prepared by
detoxification techniques, catalytic oxidation is a promising
method to abate these harmful emissions due to its low energy
consumption, high efficiency, and preferred ability of
CTABꢀassisted hydrothermal synthesis. As reference, we also
prepared brookite TiO (TiO ꢀB), rutile TiO (TiO ꢀR), and six
2
2
2
2
2
ꢀ4
2 2
other TiO catalysts. The TiO ꢀHA nanoparticle catalyst shows
converting CVOCs into harmless substances.
Catalyst is
5
the highest activity among all the employed catalysts, including
undoubtedly key factor controlling this technique
a
.
7,17,20
noble metal catalysts reported in other papers.
structure and surface chemical properties of the TiO
The
ꢀHA were
Nowadays, the most frequently investigated catalysts for
CVOCs removal include three typeset of catalysts based on
2
6
ꢀ9
10ꢀ15
16
characterized, and the catalytic behavior was assessed in
relation to a few important parameters of the catalysts such as
7ꢀ19 surface acidity and reducibility. We expect that findings
presented in this paper could provide novel insights into the
design and synthesis of catalysts for catalytic oxidation of
CVOCs.
noble metals , transition metal oxides
, or zeolites . The
catalytic oxidation of DCM, a representative alkyl chloride
1
pollutant, has been widely investigated on these catalysts.
Noble metal catalysts, such as Pt catalysts and Ru catalysts are
more preferentially acceptable than other catalysts. However,
expensive price and shortage of resources limit its industrial
1
,20
Hollow anatase nanoparticles were synthesized through
application.
Therefore, developing an ideal catalyst that is
CTABꢀassisted hydrothermal method. Specific amounts of
precursors, namely, TiOSO ·2H O and CTAB (CTAB/TiOSO
1:12, molar ratio) were dissolved in 50 mL of deionized water
under magnetic stirring at 60 °C. The TiOSO solution was
earthꢀabundant, contains nonꢀnoble metals, and possesses
superior catalytic activity will be a breakthrough in DCM
catalytic combustion. DCM can readily react with the hydroxyl
4
2
4
=
4
added to the CTAB solution under vigorous stirring. The liquid
mixture obtained was then subjected to hydrothermal treatment in a
1
50 mL stainless steel autoclave at 110 °C for 24 h. After the
autoclave was cooled to room temperature, the precipitate was
filtered and washed repeatedly with deionized water and ethyl
alcohol. TiO
2 2
ꢀB and TiO ꢀR were synthesized through modified
30,
hydrothermal method by using previously described method.
3
1
The detailed synthesis of other catalysts was introduced in the
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Table 1 The textures and catalytic performances of TiO catalysts
a
b
d
BET
surface
Pore
volume
Pore
size(nm)
Particle
size(Å)
T
/°C
50
T
90
/°C
catalysts
area
m /g)
3
(cm /g)
2
(
TiO
2
-HA
-B
-R
94.73
36.08
19.51
0.31
0.27
0.26
12.98
29.95
52.68
114
338
390
175 201
241 279
302 411
TiO
TiO
2
2
c
adsorption and activation of DCM molecules on the internal
surface of the catalysts. To investigate the morphology and
dispersion of the samples, the representative TEM patterns of
the catalysts were obtained (TiO
2 2
ꢀHA see Fig.1cꢀd, TiO ꢀB,
TiO ꢀR see Fig.S2). It can be seen that the particles of TiO ꢀHA
2
2
show good dispersion, and the nanoparticles show regular
homogeneous particles with hollow spherical morphology.
2
HRTEM confirms the existence of 8ꢀ20 nm TiO particles. This
Fig. 1 Characterizations of hollow anatase TiO
2
(TiO
2
-HA). (a) the XRD
findings is in good agreement with the average mean diameter
estimated according to the Scherrer equation applied to the<101>
reflection of anatase of the XRD data (see Table 1). The hollow
pore size of the particle corresponds to the mesoporous
pattern of TiO
2
-HA; (b) N
2
adsorption-desorption curves and pore size
-HA.
distribution of TiO
2
-HA; (c, d) HRTEM images of TiO
2
2
distribution shown in Fig.1b (inset). Hence, TiO ꢀHA
supporting material. Almost all precursors prepared were
calcined in air at 500 °C for 4 h. The catalysts were
characterized by sensitive physicoꢀchemical techniques, such as
nanoparticle is a catalyst that belongs to anatase crystalline
phase and possesses hollow spherical morphology. Higher
specific surface area, wider poreꢀsize distribution of
mesoporous, larger pore volume and hollow spherical
morphology may be favorable for the improvement of the
catalytic performance for DCM destruction.
Xꢀray diffraction (XRD),
2
N ꢀphysisorption, transmission
electron microscopy (TEM), and pyridine adsorption followed
by FTꢀIR spectroscopy (FTIRꢀpyridine) analyses.
Catalytic performance tests were performed in a traditional
fixedꢀbed tubular reactor (quartz glass; 6 mm i.d.) at ambient
pressure. Briefly, 200 mg of the catalyst was placed in the
middle of the reactor and diluted with 1800 mg of quartz sand.
The catalytic activity of the TiO
decomposition is shown in fig.2a. The TiO
2
catalysts for DCM
ꢀHA and TiO ꢀB
2
2
catalysts present a high catalytic activity, especially TiO ꢀHA
2
with hollow structure, with T50 and T90 (temperature when 50%
and 90% conversion were obtained) of approximately 175 °C
and 201 °C, respectively (see Table 1). As referential samples,
DCM feed gas was generated by bubbling air (20.8% O and
2
7
9.2% N ) at a suitable flow rate through a saturator in an ice
2
bath. A bypass flow of air was also used to balance total flow
rate to provide the desired gas hourly space velocity (GHSV) in
the catalyst bed. The gas stream was composed of 1000 ppm
2
other three anatase, two brookite and one rutile TiO catalysts
were prepared through different methods, the XRD patterns and
the DCM combustion activity of the samples are shown in Fig.
S1 and the properties are shown in Table 1S. Also we can see
ꢀ1
−1
−1
DCM and air in 50 mL min [GHSV of 15000 mL h (gcat.) ].
The effluent gases were analyzed online with a GCꢀ6890N gas
chromatograph equipped with FID detector and an FTꢀIR
2
that the same crystallineꢀphase TiO catalysts prepared by
different methods significantly differ in terms of activity (see
Fig.S1). Furthermore, the synthesized catalyst was compared
with catalysts recently reported in the literature, and the results
are listed in Table 2. Notably, comparing the results of our
work with those reported in the literature is difficult because the
activity of the tested catalysts is significantly related to the
−
1
spectrometer (Vertex70; scan rate = 32 scans s ; resolution =
−
1
2
.5 cm ). GC–MS analysis was conducted to confirm the
formation of byꢀproducts. The concentrations of Cl and HCl
2
were analyzed by bubbling the effluent through 0.0125 N
NaOH solution. Further detailed analytic process was described
3
2
in a previous study.
Fig.1a presents the XRD pattern of the TiO
The sample shows characteristic diffraction peaks of the
anatase TiO crystalline phase (PDF#21ꢀ1272) and no other
diffraction peaks were detected, also TiO ꢀB and TiO ꢀR
2
operation condition. As listed in Table 2, the TiO ꢀHA
nanoparticle catalyst in the current work shows the highest
2
ꢀHA catalyst.
2
2
2
catalysts respective show the characteristic diffraction peaks of
the brookite and rutile TiO crystalline phase (see Fig.S1). The
texture properties of various catalysts were investigated by N
adsorption / desorption. As shown in Table 1, the TiO ꢀHA
Table 2 some works made on total oxidation of DCM with catalyst
2
Catalyst
DCM Content
ppm
GHSV
T
90/°C
Ref.
2
/
2
-
1
-1
-1
-1
Pt/Al
Ru/7%Ce-Al
Ru/TiO
.42k-2Pt/Al
Ce/TiO
CoCr
Ce1Cr
CuMnO /Zr–Ti–Al
2
O
3
1000
750
750
3000
1000
3000
1000
1200
/
20000 h
10000 h
10000 h
15000 h
3000 h
15000 h
320
260
267
321
315
257
337
470(T100
450(T100
430
17
20
35
7
11
13
10
36
37
38
catalyst exhibits higher BET specific surface area than the two
2
O
3
other catalysts. The N adsorption / desorption isotherms and
2
2
2
the BJH pore size distribution of the TiO ꢀHA catalyst are
0
2
O
3
shown in Fig.1b. The sample exhibits type IV adsorption /
desorption isotherms with H1 hysteresis loops, which are
typical characteristics of mesoporous materials according to the
-1
2
-1
2
O
4
-1 -1
4
9000 mLg h
8000 h
/
15000 h
15000mLg h
3
3, 34
-
1
IUPAC classification.
catalyst possesses
within 5ꢀ25 nm. Moreover, the pore volume of TiO
larger than that of TiO ꢀB or TiO ꢀR, which can promote the
As shown in the inset of Fig.1b, the
symmetrical mesoporous distribution
ꢀHA is
x
)
)
a
H-ZSM-5
Mn/HZSM-5
TiO -HA
-1
2
1000
1000
-1 -1
2
2
2
201
This work
2
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Fig. 2 Catalytic performance of DCM combustion on TiO
2
-HA catalyst. (a) Light-off curves of DCM combustion on TiO
2 2 2
-HA, brookite TiO (TiO -B), rutile
TiO
2
(TiO
2
-R) ; (b) Catalytic Selectivity of DCM combustion on TiO
2
-HA; (c) Stability of TiO -HA for DCM oxidation. Gas composition: 1000 ppm DCM in air,
2
-1
-1
GHSV = 15000 mL h (gcat.) .
4
0
activity among all the employed catalysts, including noble dissociate O
2
.
metal catalysts, such as 0.42Kꢀ2Pt/Al The stability of the TiO ꢀHA catalyst with time on stream
2
O
3
and Ru/7%CeꢀAl
2
O
3
,
2
with T90 of 321 °C and 260 °C, respectively. It should be was also investigated (see Fig.2c). Degradation experiments
noticed that for CVOCs oxidation, high conversion is not only were conducted on the TiO –HA catalyst, which was
2
criterion for good catalyst systems, and selectivity of the maintained for 2 h at 200 °C. The DCM conversion was
products are also important. The desired products in Clꢀ sustained at 90% during the first 90 min of the reaction, but it
containing CVOCs oxidation should be CO
shows the conversion and products distribution of DCM over conversion recovers when the temperature increases to 225 °C,
the TiO ꢀHA catalyst. The detectable final products are CO but still decline later and even below 61%. Similar situation
CO, and HCl with CH Cl. No other Clꢀcontaining organic was observed at 250°C, 275°C and 300 °C. Until the
2
and HCl. Fig.2b sharply decreased from 93% to 61% in the next 30 min. The
2
2
,
3
compounds are detected (see Fig. S3). Though TiO
excellent catalytic activity at a low temperature range (below declines in 1 h. At 350 °C, the DCM conversion maintains 100%
25 °C), DCM conversion generated a large amount of CH Cl in 1 h, we remain the temperature for another 50 h, and no
2
ꢀHA have temperature increase to 325 °C, the conversion only slightly
2
3
until reaching the plateau at 225 °C, indicating that the polar Cꢀ significant deactivation is observed because the conversion still
Cl bonds are much weaker than the CꢀH bonds and were maintains above 90%. The deactivation of the catalyst at a low
3
9
expected to be cleaved at first. It could be found that the temperature which may be related to the Cl species deposited
yields of byꢀproducts decreased and a large amounts of on the active sites in the process of DCM destruction on the
(CO
2 2
+CO) and HCl were generated with the temperature surface of TiO ꢀHA catalyst, and the increase of temperature
raising. In addition, HCl yield rapidly increased at 325 °C, can remove the adsorbed Cl species, hence, more active sites
2
0.35
which could be due to the sudden removal of many adsorbed Cl can be accessible.
2
Thus, at 350 °C for TiO ꢀHA catalyst, the
species in the form of HCl at this temperature. At 350 °C, most DCM removal activity remains without any catalyst
amount of DCM decomposed into simple (CO +CO) and HCl. deactivation on 50 h longꢀtime stability tests, which suggests
2
The ratio of CO
hence, CO dominated in the generated (CO
catalyst, which indicates that the activity for CO oxidation of transformed into HCl, (CO
2
: (CO
2
+CO) was about 29% at this temperature, the presence of balance was found between absorbed Cl species
+CO) for TiO and desorbed Cl species. And at this temperature, the DCM was
+CO) and hardly any CH Cl.
As previously mentioned, the activity for catalytic
2
2
2
3
the catalyst is poor probably owing to the weak ability to
2 2 2 2 2 2
Fig. 3 Pyridine adsorption-temperature programmed desorption FT-IR for TiO . (a) TiO -HA, (b) brookite TiO (TiO -B), (c) rutile TiO (TiO -R).
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combustion of DCM was considered related to the synergy Specialized Research Fund for the Doctoral Program of Higher
between acidic role and oxidization. The acidity is favorable for Education (NO. 20133317110004).
activating CꢀCl bonds. Thus, FTIRꢀpyridine was characterized
the acidity on the catalysts surface (see Fig.3), measured after
evacuation at 30°C, 200°C and 400 °C corresponding
respectively to the amount of weak, midꢀstrong and strong
acidity. The amount of Brønsted sites (B sites) and Lewis
Notes and references
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3
4
5
6
7
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ꢀ1 23,41
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respectively to pyridine adsorbed on B sites and L sites. We
find a very interesting phenomenon. In particular, the TiO ꢀHA
corresponding
2
catalyst (see Fig.3a), possesses both B sites and L sites, and the
increase in the evacuation temperature of pyridine induces a
slight decrease in the peak of adsorbed pyridine on B acid sites
and large decrease in L acid sites at 400°C.This phenomenon
reveals that the B sites of the catalyst are mainly strong B sites
and the L sites are mostly midꢀstrong L sites with a few strong
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Fig.3bꢀc). These observations indicate that the amount of midꢀ
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1
,
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,
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hydroxyl group that leads to the rupture of C–Cl bonds and
freeing one HCl (or the Cl species adsorbed on the surface).
The adsorbed intermediate species could be attacked by the
adjacent activate oxygen species, the chlorine atom is
substituted by oxygen atoms, leading to adsorbed formaldehyde
formation and hemiacetal species, which disproportionate into
methoxy species and formate species. The formaldehyde
species could generate major methoxy species when this
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0 19
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2
2
2
B
CH Cl at low temperature were generated.
3
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2
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Acknowledgements
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We would like to acknowledge the financial support from the
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PleaseRd So Cn oA t da vd aj un s ct ems argins
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DOI: 10.1039/C6RA06400K
RSC Advances
COMMUNICATION
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2 R. W, Van den Brink, R. Louw, P. Minder, Appl. Catal., B, 1998, 16,
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3 R. W, Van den Brink, M. Krzan, M. M. R. FeijenꢀJeurissen, R.
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Louw, P. Minder, Appl. Catal., B, 2000, 24, 255.
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DOI: 10.1039/C6RA06400K
Table of Content (TOC)
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Hollow anatase TiO nanoparticles with around 11.4 nm were prepared by
CTAB-assisted hydrothermal method. This catalyst delivered a high catalytic activity
for dichloromethane (DCM) combustion. In particular, the catalyst exhibited 90%
DCM conversion at 201 °C.
Keywords
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Hollow; Anatase TiO ; DCM; Catalytic combustion;