Cerium Doped Pt/TiO2 for Catalytic Oxidation of Low Concentration Formaldehyde at Room Temperature

Article abstract of DOI:10.1007/s10562-019-02684-z

Abstract: Formaldehyde is a carcinogenic and teratogenic toxic gas. With the extensive use of a variety of building materials, indoor formaldehyde has seriously threatened human health and environment. The catalytic oxidation is considered the most promising method for the removal of formaldehyde from air. In this work, we report a Pt/TiO₂ catalyst with Ce modification, and investigate its activity of catalytic oxidation of low concentration formaldehyde at room temperature. The experimental results show that the trace formaldehyde (20?mg/m³) could be completely degraded at 55?min by using Pt–Ce/TiO₂ catalyst. In view of multiple characterizations, such as BET, XRD, TEM, STEM, XPS and CO adsorption, it is indicated that the modification of Ce can effectively improve the dispersion of Pt particles in the surface and reduction of Pt particle size from 2.9 to 2.2?nm. Moreover, XPS results show that the Ce in the catalyst could enhance the binding energies of Pt, provide abundant oxygen vacancies, and could increase the ratio of adsorbed oxygen atoms to lattice oxygen atoms, which is conducive to the adsorption of oxygen, leading to the improvement of catalytic activity. Graphical Abstract: [Figure not available: see fulltext.].

Full text of DOI:10.1007/s10562-019-02684-z

Catalysis Letters (2019) 149:1319–1325
https://doi.org/10.1007/s10562-019-02684-z
Cerium Doped Pt/TiO2 for Catalytic Oxidation of Low Concentration
Formaldehyde at Room Temperature
Yuanyuan Shi1 · Zhiwei Qiao1 · Zili Liu1 · Jianliang Zuo1
Received: 3 October 2018 / Accepted: 30 December 2018 / Published online: 20 February 2019
© Springer Science+Business Media, LLC, part of Springer Nature 2019
Abstract
Formaldehyde is a carcinogenic and teratogenic toxic gas. With the extensive use of a variety of building materials, indoor
formaldehyde has seriously threatened human health and environment. The catalytic oxidation is considered the most prom-
ising method for the removal of formaldehyde from air. In this work, we report a Pt/TiO2 catalyst with Ce modification, and
investigate its activity of catalytic oxidation of low concentration formaldehyde at room temperature. The experimental results
show that the trace formaldehyde (20 mg/m3) could be completely degraded at 55 min by using Pt–Ce/TiO2 catalyst. In view
of multiple characterizations, such as BET, XRD, TEM, STEM, XPS and CO adsorption, it is indicated that the modifica-
tion of Ce can effectively improve the dispersion of Pt particles in the surface and reduction of Pt particle size from 2.9 to
2.2 nm. Moreover, XPS results show that the Ce in the catalyst could enhance the binding energies of Pt, provide abundant
oxygen vacancies, and could increase the ratio of adsorbed oxygen atoms to lattice oxygen atoms, which is conducive to the
adsorption of oxygen, leading to the improvement of catalytic activity.
Graphical Abstract
Keywords Low concentration formaldehyde · Room temperature · Platinum · Titania · Ce modification
1 Introduction
Formaldehyde (HCHO) is a kind of colorless poisonous gas
with strong pungent odor, the main source of indoor for-
maldehyde is interior decoration materials, such as artifi-
cial synthesis plank, emulsioni paint, carpet fabric and resin
decorations and furniture. The formaldehyde can be slowly
* Zili Liu
gzdxlzl@gmail.com
Extended author information available on the last page of the article
Vol.:(0123456789)
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Y. Shi et al.
released from the materials, and the release period could
exceed by 3–15 years, leading to the concentration of for-
maldehyde in the house keeping higher than the outside [1].
Prolonged exposure to low concentrations of formaldehyde
can cause chronic respiratory diseases, chromosomal abnor-
malities, and even nasopharyngeal cancer or fetal malforma-
tion. The eliminating indoor formaldehyde from the source
is unable to achieved perfectly at present, thus the removal
of indoor formaldehyde is widely paid attention by many
researchers. In recent years, the techniques for removing the
indoor formaldehyde mainly include adsorption [2, 3], plant
purification, plasma technique [4], photocatalytic oxidation
technique [5, 6] and catalytic oxidation technique [7–9].
The catalytic oxidation technique has no secondary pollu-
tion with advantages of high efficiency, complete treatment
and extremely effective treatment for low concentration for-
maldehyde. Therefore, the catalytic oxidation is considered
to be the most promising and effective technique to remove
formaldehyde from indoor air.
catalytic oxidation of formaldehyde. Valden et al. [20] stud-
ied the influence of the size of gold nanoparticles on cata-
lytic activity by using scanning tunnel (STM/STS) technique
on Au/TiO2 catalyst, they found that gold nanoparticles with
non-metallic characteristic size (~3.5 nm) had the highest
catalytic activity. In the Shen et al.’s work [21], it was found
that the increase of Pd particle diameter led to the reduc-
tion of catalyst activity. The previous comparative experi-
ments showed that [22], the Pt catalyst supported on TiO2
had better catalytic oxidation activity than other carriers.
TiO2 not only had the excellent reducibility, but also had
strong electron interaction with the active site [23], such as
Qi et al. [24] used high-surface mesoporous Pt/TiO2 hollow
chains for efficient formaldehyde decomposition, the hollow
chain-like structure, high specific surface area, numerous
mesopores, and high volume of TiO2 are main reasons for
efficient formaldehyde oxidation. Furthermore, they synthe-
sized hierarchically macro-/mesoporous Pt/TiO2 catalyst for
formaldehyde decomposition, the high catalytic activity is
mainly attributed to hierarchically macro-/mesoporous struc-
tures of the TiO2 support with large specific surface area and
optimal pore size [25]. However, the low surface area was
an obvious defect in the application of conventional TiO2 as
a catalytic carrier, which cannot guarantee the high disper-
sion of Pt nanoparticles in the loading process and cannot
provide sufficient reaction space related to the adsorption
or diffusion of reactants [26]. However, some researches
[27, 28] showed that, adding different amounts of rare earth
oxides can improve effectively the dispersion of supported
noble metal catalysts and can make the particle size of active
components become much smaller than that of unmodified
ones, such as in the Shen et al.’s work [29], it was found that
Pt/ZSM-5 through a facile nickel cation exhibits an excellent
catalytic activity and stability for formaldehyde removal.
Considering the high cost of precious metal Pt and low eco-
nomic benefits, in this work, we use the commercial TiO2
to support nano-Pt particles, and the rare earth metal Ce is
doped to modify the defect of low activity of the catalyst.
The loading of Pt in all of catalysts is controlled below 0.5%.
The catalysts are prepared and explored their performance
for the removal of formaldehyde with low concentration at
room temperature.
In the past decades, the technology of catalytic oxidation
to remove formaldehyde has made considerable progress
[10–13]. At present, the precious metal catalysts used in the
catalytic oxidation of formaldehyde mainly included Pt, Au,
Pd, Ag, Ru etc [8, 9, 14–16]. While, due to very high conver-
sion rate and long life of catalytic oxidation of formaldehyde
under low temperature, the Pt-supported catalyst has been
paid attention by most of researchers. In the preparation
of supported precious metal catalyst, the support plays an
important role for its activity, and the choice of different
supports has important influence on the dispersion and size
of loaded precious metal particles. Besides, the activity of
catalyst is also reflected in the numbers of oxygen vacancy
and the interactions between the supports and precious met-
als. Yan et al. [17] used the combination of AlOOH and
CeO2 as the carrier to support the noble metal platinum.
The catalyst showed an excellent activity and stability for
the catalytic oxidation of formaldehyde at room temperature,
the main reason is the rich hydroxyl groups on the surface
of CeO2, the high dispersion of Pt particles and the high
adsorption capacity of AlOOH to formaldehyde. Kim et al.
[18] found that the Pt/TiO2 catalyst prepared by reduction
pretreatment, the oxygen consumption area on the catalyst
surface was correlated with the proportion of Pt species,
and the activated oxygen on the catalyst surface had impact
on the activity of catalytic oxidation of formaldehyde. Cui
et al. [19] found that acid-treated TiO2 nanobelt supported
platinum catalyst shows highly efficient activity for the cata-
lytic oxidation of formaldehyde, due to the acid treated TiO2
could possess more defect sites and more rougher surface
and produce stronger interaction between Pt nanoparticles
and hydroxyl species.
2 Experimental
2.1 Catalyst Preparation
First, TiO2 was modified by various amounts of Ce (0,
1, 5 and 7 wt%) by a impregnation method. For exam-
ple, 0.279 g Ce(NO3)3 was dissolved in a certain amount
of deionized water and then under constant stirring 1.5 g
TiO2 was added to the Ce(NO3)3 solution. After stirring
Furthermore, the size and dispersion of noble metal par-
ticles on the support are closely related to the activity of
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Cerium Doped Pt/TiO2 for Catalytic Oxidation of Low Concentration Formaldehyde at Room…
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for 2 h, excess water was removed in a rotary evaporator
at 80 °C. The samples were dried at 110 °C for 12 h and
then calcined at 450 °C for 4 h. This catalyst was marked
as x wt%Ce/TiO2. (x = 0, 1, 5 or 7).
2.3 Activity Test
Formaldehyde removal test was carried out in an organic
glass sealed box (60 L) at room temperature, the wall of
box was covered with a layer of aluminum foil and a free
passage of air was created using a 5 W electric-fan. 200 mg
catalysts were dispersed on a glass petri dish, which is
placed at the bottom of catalytical reaction apparatus,
covered with a glass slide; and formaldehyde detector was
placed next to it. Before the test, 5 µl solution including
37% formaldehyde solution was injected into the reactor
and reached its gas phase equilibrium under the circulat-
ing fam flow.
Secondly, nano-Pt particles were loaded on Ce doped
TiO2 carrier by precipitation deposition method, and the
Pt content of catalyst was 0.5%. Typically, 1.5 g x wt%Ce/
TiO2 was dissolved in 25 ml deionized water, and then
a certain volume of H2PtCl6 solution was added to the
mixture and stir for 1 h. Then 0.1 mol/l NaOH solution
was added to adjust ph to 10, aging at 60 C for 2 h under
constant stirring. Subsequently, 2.5 ml 0.1 mol/l NaBH4
solution was added to the mixture and stir for 0.5 h, the
suspension was centrifuged and washed three times by
deionized water, and then dried at 80 °C for 12 h. The final
catalyst was denoted as 0.5% Pt-x wt% Ce/TiO2 (x = 0, 1,
5 or 7).
The initial gas concentration of HCHO was controlled to
keep 20 2 mg/m3, and then the glass cover was removed
from dish and start the catalytic activity measurement.
3 Results and Discussion
2.2 Catalyst Characterization
3.1 Characterization of the Catalysts
The crystal structure of catalysts was analyzed by a MASAL
XD-3 diffractometer (Beijing Purkinje Company). The test
conditions were as follows: Cu Kα ray (λ = 0.15406 nm),
tube voltage and tube current were 36 KV, and 20 mA
respectively. Scanning speed was 8°/min. Scans were col-
lected over a range of 2θfrom 0° to 80°.
The structural properties of TiO2 and Pt supported
catalysts were studied by X-ray diffraction charac-
terization. Figure 1 shows that five diffraction peaks
at 2θ = 25.3°(101), 37.8°(004), 48°(200), 53.9°(105),
55.1°(211), are typical for the anatase TiO2 crystal-
line phase. Three diffraction peaks at 2θ = 27.5°(110),
36.1°(101), 41.2°(111) belong to rutile crystalline phase.
The diffraction peaks belonging to CeO2 species are not
observed in the diffraction patterns of modified TiO2 and
Pt-loaded catalyst. This indicates that CeO2 species are
highly dispersed on the surface of TiO2.
Transmission electron microscope (TEM) and high
angle dark field scanning transmission electron microscope
(HAADF-STM) images were measured at 200 KV on a field
emission transmission electron microscope Tecnai G2 F20
S-TWIN (FEI USA).
Micromeritics ASAP-2020 system was used to deter-
mine the N2 adsorption–desorption isotherms of sam-
ple. Brunauer–Emmett–Teller (BET) method was used to
calculate the specific surface area of samples, and Bar-
rett–Joyner–Halenda (BJH) method was used to calculate
the pore diameter distribution.
X-ray photoelectron spectroscopy (XPS) was performed
using a multi-functional X-ray photoelectron spectrometer
(Shimadzu Axis Ultra DLD, Kratos, UK). The spectra were
obtained at ambient temperature. The binding energies were
calibrated using the C1s peak of graphite at 284.6 eV as
reference.
CO adsorption was measured on an AutoChem II2920
to analyze the Pt dispersion of the catalysts. Sample was
firstly pretreated in hydrogen at 150 °C for 1 h and purged
with helium for 1 h at the same temperature. And then, the
catalyst was cooled to room temperature and CO pulses were
injected from a calibrated online sampling valve. CO adsorp-
tion was assumed to be completed after three successive
peaks showed the same peak areas. A CO/Pt stoichiometry
of 1 was used for calculations.
Fig. 1 Powder XRD patterns of TiO2 and supported Pt catalysts
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Y. Shi et al.
Moreover, there is no diffraction peak of Pt species on the
Pt-5%Ce/TiO2 catalysts. The particle size of Pt is calcu-
lated by TEM and STEM images, showed in Figs. 3 and
4, and the degree of Pt dispersion is determined by CO
adsorption characterization, listed in Table 1. Figures 3
and 4 show that Pt nanoparticles have no agglomera-
tion and have high dispersion on the surface of supports.
The average diameter of Pt particles in Pt/TiO2 catalyst
is 2.91 nm, but the Pt diameter in Ce modified catalyst
decreases to 2.2 nm. Furthermore, CO adsorption results
show that the dispersion of Pt particles is significantly
improved after the modification of Ce. All of characteri-
zations indicated that Ce modification could stabilizes Pt
nanoparticles with small size and prevent agglomeration
of Pt particles. A large amount of small Pt nanoparticles
can increase the number of surface defects (ladders, bor-
ders, and corners), leading to exposure of active Pt nano-
particles on the catalyst surface. Thus, more active sites
are provided for the oxidation reaction of formaldehyde at
room temperature.
Pt-loaded catalysts, reason is mainly the low Pt loading of
(0.5 wt%) and the high dispersion of Pt nanoparticles on the
supports, which is further confirmed in both Transmission
Electron Microscopy and CO adsorption analysis.
To understand the physical properties of TiO2, Pt-
loaded catalysts and Ce doping catalysts, N2 adsorp-
tion–desorption isotherm of each sample is measured and
analyzed in Fig. 2 and Table 1. All of the N2 adsorption
isotherms show IV isotherm with H3 type hysteresis in
the figure, this indicates that the sample possess a certain
mesopores. Moreover, Table 1 shows that TiO2 has the
maximum specific surface area of 50 m2/g, and its surface
area slightly decreases after doping 0.5 wt%Pt, whereas
both SBET of TiO2 drop to 43 m2/g after modified by the
Ce and Pt. The reason for decreasing of SBET is that Pt and
CeO2 particles enter into the pore of carrier and cause a
blockage in it.
To explain the effect of Ce doping on the size and dis-
persion of Pt nanoparticles, TEM, STEM and CO adsorp-
tion characterization are performed to analyze Pt/TiO2 and
The important factors of HCHO oxidation at room tem-
perature, as Huang et al. reported, were both the mobility of
activated chemisorbed oxygen on the catalyst surface and the
strong interaction between the support and precious metal
[30]. The mobility of chemisorbed oxygen is more important
to enhance the performance of catalyst than that of lattice
oxygen. Furthermore, several previous works study dem-
onstrated that the gas-phase oxygen could be dissociated
and adsorbed at the oxygen vacancies, and could form the
highly active species for the oxidation reaction [31]. Thus,
in our work X-ray photoelectron spectroscopies of Pt/TiO2
and Pt-Ce/TiO2 catalysts are carried out to analyze the effect
of Ce modification on the binding energies of Pt with O.
Figure 7 shows that the binding energies between Pt 4f and
O1s, and the atomic radios of adsorbed O to lattice O are
calculated by the XPS data of the modified and unmodified
catalysts.
In Fig. 5, for the Pt/TiO2 and Pt-Ce/TiO2 catalysts, the
binding energy peaks of Pt 4f7/2 and Pt 4f5/2 are found at
70.8/74.0 eV and 70.9/74.1 eV, respectively. Comparing
with Pt 4f7/2 standard binding energy of Pt0, Pt2+ and
Pt4+ 71.1 and 72.4/74.2 eV, it indicates that there exist
Fig. 2 N2 adsorption–desorption isotherms of TiO2 and supported Pt
catalysts
Table 1 Physicochemical
properties of TiO2 and
supported Pt catalysts
Simple
SBETa (m2/g)
Pore volume
(cm3/g)
Pore size (nm)
Pt dispersionb Pt particle
(%)
sizec (nm)
Nano TiO2
5 wt%Ce–TiO2
Pt/TiO2
50
43
49
43
0.17
0.36
0.39
0.35
34.9
21.2
21.7
21.4
–
–
–
–
15.63
45.33
2.91
2.21
Pt/5 wt%Ce–TiO2
aCalculated by BET method
bCalculated by CO adsorption
cDetermined by TEM
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Cerium Doped Pt/TiO2 for Catalytic Oxidation of Low Concentration Formaldehyde at Room…
1323
Fig. 3 TEM images of Pt/TiO2 (1, 2) and Pt/5 wt% Ce–TiO2 (3, 4) and their Pt particle size
Fig. 4 HAADF-STEM images of Pt/TiO2 (1, 2) and Pt/5 wt% Ce–TiO2 (3, 4)
both Pt0 and Pt4+ in the catalysts. Moreover the incor-
poration of Ce makes the binding energy of Pt 4f go up
0.1 eV, and cause to the deviation of electron cloud of Pt.
The peak area of Pt doped with Ce is much larger than that
of unmodified Pt, leading to increasing of the number of
electronegativity atoms in Pt microenvironment and fur-
ther increasing of oxygen vacancy. It is consistent with
the XPS data of O.
peak of ~ 530.8 eV, which is attributed to the chemical
adsorption oxygen, denoted as Oads
.
Compared with the O-1s spectra of unmodified Pt/TiO2,
the O-1s peak of Pt–Ce/TiO2 is wider, thus, the chemical
bonds of atoms on the Pt–Ce/TiO2 surface are unsaturated,
and there are more oxygen vacancies. The SOads/SOlat ratio
are calculated by the peak area and listed in Table 2, it is
found that SOads/SOlat of modified Pt–Ce/TiO2 is much
larger than the unmodified Pt/TiO2. This is because CeO2
has an incomparable oxygen storage capacity, which can
provide a large number of oxygen vacancy and can promote
the adsorption of oxygen to generate more Oads. Therefore
In the O 1s spectra of Pt/TiO2 and Pt–Ce/TiO2, both the
O 1s spectral lines can be divided into two peaks, one is the
main peak of ~529.8 eV, which is mainly attributed to the
lattice oxygen in TiO2, denoted as Olat, the other is shoulder
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Y. Shi et al.
Fig. 6 Activity of catalysts under different Ce doping amounts
Fig. 5 XPS analysis of Pt/TiO2 (1) and Pt-5 wt% Ce/TiO2 (2). a Pt 4f;
b O 1s
the performance of Pt–Ce/TiO2 catalyst is significantly
enhanced after Ce doping.
Fig. 7 Catalytic performance of Pt/TiO2 and Pt-5%Ce/TiO2 and sta-
bility test for HCHO oxidation
3.2 Catalytic Activity
Figure 6 compares the activity of catalysts with different
mass fraction of Ce doping (0%, 1%, 3%, 5%, 7%) by the
residual and time curves of HCHO oxidation at room tem-
perature. During the experiment, the error of HCHO detec-
tor is 1%. As shown in the Fig. 6, the catalytic performance
of catalysts for formaldehyde oxidation has been improved
whatever the ratio of Ce is used to modify. But the 5% Ce-
doped catalyst possesses best catalytic activity. This Pt-
5%Ce/TiO2 catalyst could completely oxidize HCHO in the
reactor within 55 min. To test the stability of catalyst for
HCHO oxidation, we set a 2-h reaction cycle and monitor
the oxidation rate of HCHO in 15 cycles. As shown in Fig. 7,
the Pt-5%Ce/TiO2 catalyst could reach the oxidation rate of
100% in 15 cycles. The activity of Pt/TiO2 catalyst rapidly
decreased in the second cycle, because the active centers (Pt
atom) of the catalyst start to deactivate. Thus, the catalysts
after Ce doping exhibit stronger stability than unmodified
catalysts.
Table 2 XPS results of Pt/TiO2
Sample
Pt 4f BE (eV)
Ti 2p BE
O 1s BE (eV)
SOads/SOlat
and Pt–Ce/TiO2 catalysts
4f5/2
4f7/2
(eV)
Oads
Olat
Pt/TiO2
Pt/5 wt%Ce–TiO2
74.0
74.1
70.8
70.9
458.5
458.8
531.1
530.8
529.8
529.6
0.18
0.32
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Cerium Doped Pt/TiO2 for Catalytic Oxidation of Low Concentration Formaldehyde at Room…
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4 Conclusions
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In this work, we report that the Ce modification can greatly
improve the activity of Pt/TiO2 catalyst for low concentra-
tion HCHO oxidation at room temperature as well as the
stability of the catalyst. The catalyst with Ce doping amount
of 5% possesses the best performance and can completely
degrade the 20 mg/m3 of HCHO in 55 min. After the catalyst
is modified by Ce, the diameter of Pt nanoparticles would
change from 2.9 to 2.2 nm, and the dispersion of Pt nano-
particles is enhanced by CO adsorption measurement. The
addition of Ce can provide abundant oxygen vacancies on
the catalyst surface, by the data of XPS characterization.
This is conductive to chemisorb the oxygen from the air, and
then promotes the catalytic oxidation of HCHO, leading to
improvement of the activity of the catalyst. Therefore, the
Pt/TiO2 catalyst with the Ce doping possesses the excellent
performance and a potential commercial value for removing
low concentration of formaldehyde from indoor air.
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Conflict of interest All authors declare that they have no conflict of
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Affiliations
Yuanyuan Shi1 · Zhiwei Qiao1 · Zili Liu1 · Jianliang Zuo1
1
Yuanyuan Shi
School of Chemistry and Chemical Engineering, Guangzhou
867492350@qq.com
University, Guangzhou, Guangdong, China
Zhiwei Qiao
gzdxqzw@gmail.com
Jianliang Zuo
gzdxzjl@gmail.com
1 3