Pt/MnO2 Nanoflowers Anchored to Boron Nitride Aerogels for Highly Efficient Enrichment and Catalytic Oxidation of Formaldehyde at Room Temperature

Article abstract of DOI:10.1002/anie.202013667

The catalytic room temperature oxidation of formaldehyde (HCHO) is widely considered as a viable method for the abatement of indoor toxic HCHO pollution. Herein, Pt/MnO₂ nanoflowers anchored to boron nitride aerogels (Pt/MnO₂-BN) were fabricated for the catalytic room temperature oxidation of HCHO. The three-dimensional Pt/MnO₂-BN aerogels demonstrated superior catalytic activity as a result of the improved diffusion of the reactant molecules within the porous structure. Furthermore, the porous aerogels displayed excellent HCHO adsorption capacities, which promote a rapid HCHO gas-phase concentration reduction and a subsequent complete oxidation of the adsorbed HCHO. The combined adsorption and oxidation properties of the Pt/MnO₂-BN aerogels enhance the oxidative removal of HCHO. The optimized Pt/MnO₂-BN demonstrated excellent catalytic activity toward HCHO (200 ppm) at room temperature, achieving a 96 % formaldehyde conversion after 50 min.

Full text of DOI:10.1002/anie.202013667

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Accepted Article
Title: Pt/MnO2 Nanoflowers Anchored to Boron Nitride Aerogels
for Highly Efficient Enrichment and Catalytic Oxidation of
Formaldehyde at Room Temperature
Authors: Dongyun Chen, Guping Zhang, Mengmeng Wang, Najun Li,
Qingfeng Xu, Hua Li, Jinghui He, and Jian-Mei Lu
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Pt/MnO Nanoflowers Anchored to Boron Nitride Aerogels for
2
Highly Efficient Enrichment and Catalytic Oxidation of
Formaldehyde at Room Temperature
Dongyun Chen, Guping Zhang, Mengmeng Wang, Najun Li, Qingfeng Xu, Hua Li, Jinghui He, and
Jianmei Lu*
Abstract: The catalytic room temperature oxidation of formaldehyde
HCHO) is widely considered as a viable method for the abatement
of indoor toxic HCHO pollution. Herein, Pt/MnO nanoflowers
anchored to boron nitride aerogels (Pt/MnO -BN) were fabricated for
the catalytic room temperature oxidation of HCHO. The three-
dimensional Pt/MnO -BN aerogels demonstrated superior catalytic
component in composite materials, the uptake capacities remain
unsatisfactory. From the perspective of the HCHO polarity,
materials possessing large specific surface areas and
hydrophilic surfaces typically act as excellent adsorbents for
(
2
2
[
6]
HCHO removal. Recently, hexagonal boron nitride (BN), as a
graphene analogue, has received extensive research interest in
the fields of environmental remediation and solar energy
conversion owing to hexagonal BN possessing unique
properties such as a two-dimensional (2D) layered structure, a
large specific surface area, excellent electrical insulation, and
2
activity as a result of the improved diffusion of the reactant
molecules within the porous structure. Furthermore, the porous
aerogels displayed excellent HCHO adsorption capacities, which
promote a rapid HCHO gas-phase concentration reduction and a
subsequent complete oxidation of the adsorbed HCHO. The
[
7]
high thermal conductivity. In addition to the large specific
surface area, BN possesses high hydrophilicity, and the
adsorption of HCHO molecules onto BN has also been
combined adsorption and oxidation properties of the Pt/MnO
aerogels synergistically enhance the oxidative removal of HCHO.
The optimized Pt/MnO -BN demonstrated excellent catalytic activity
2
-BN
[
6b]
2
theoretically studied.
Therefore, porous BN is expected to
toward HCHO (200 ppm) at room temperature, achieving a 96%
formaldehyde conversion after 50 min.
demonstrate good adsorption performance toward gaseous
HCHO. However, the maximum capacity of the adsorbent and
hazards associated with desorption during the regeneration
process hinders the effectiveness of adsorbents. Conversely,
Indoor living, studying and working accounts for approximately
catalytic oxidation can continuously and completely covert
75% of people's time, and hence, indoor air quality is essential
[4e-f]
2 2
gaseous HCHO into harmless CO and H O.
to human health. Therefore, there has been a wealth of
interdependent research in recent years focusing on
Principally, there are two catalyst family types for HCHO
oxidation, including supported noble metals (Pt, Au, Rh and
[
1]
improvements to indoor air quality. Volatile organic compounds
[8]
[9]
Pd) and non-noble metal oxides (Ag, Co, Ce and Mn). The
supported noble metal catalysts, such as alkali-metal-doped Na-
(
VOCs) are typical indoor air pollutants, which are principally
[
2]
emitted from used building and decorative materials.
[10a]
[10b]
Pt/TiO
NPs)
2
[8c]
,
Pt/MnO
and Na promoted Pd/TiO
x
-CeO
2
,
2
TiO -supported Pd nanoparticles
Particularly, formaldehyde (HCHO) is widely considered as a
hazardous VOC that is a significant threat to human health.
Long-term continuous exposure to HCHO can result in
numerous serious health problems, including respiratory
[10c]
(
2
,
exhibit outstanding
catalytic performance at ambient temperatures, even at high
space velocities. Additionally, Mn-based catalysts, such as
[11]
MnO
x
-CeO
2
,
MnO
x
/AC and graphene-MnO
2
,
have been
[3]
diseases, skin irritation, and cancer.
Hence, efficiently
extensively studied for HCHO oxidation and are the most active
catalysts among the transition metal oxides. Moreover,
combining the advantages of catalytic oxidation with adsorption
nanomaterials could enhance the efficiency of HCHO treatment.
removing indoor air HCHO is vital to meet air quality
requirements and to reduce public health risks.
Numerous techniques for HCHO removal have been
developed over the past few decades, to include physical
adsorption, chemical adsorption, photocatalytic degradation,
Herein, Pt NPs (~30 nm) were first loaded onto MnO
nanoflowers. The Pt NPs provide unique spatial characteristics
for the MnO nanoflowers, thereby providing stability to the
structure, thus circumventing the disadvantages of aggregation.
Thereafter, the as-prepared Pt/MnO composites were dispersed
2
[
4]
plasma oxidation and thermal catalytic oxidation. Among these
aforementioned techniques, adsorption is considered as a
feasible and convenient strategy because of improved techno-
economics and ease of operation. Numerous adsorbents
2
2
and anchored onto porous aerogels possessing interconnected
networks assembled on curled BN nanosheets (Scheme S1).
The porous structure of the aerogels facilitates HCHO
including activated carbon (AC), AlOOH, and CeO
2
have been
investigated with respect to their ability to remove gaseous
[
5]
HCHO. However, even through surface modification or as a
2
enrichment at the Pt/MnO -BN interface and subsequently
promotes the complete oxidation of the adsorbed HCHO.
X-ray diffraction (XRD) analysis was undertaken to determine
[
*] Prof. D. Y. Chen, G. P. Zhang, M. M. Wang, Prof. N. J. Li, Prof. Q. F.
the crystal structures of the as-prepared Pt/MnO
Pt/MnO -BN and BN samples. We prepared a series of Pt/MnO
BN (dosage of the Pt/MnO solution: 10, 20 and 40 μL), which
were abbreviated as Pt/MnO -BN10, Pt/MnO -BN20, Pt/MnO
2
, series of
Xu, Prof. H. Li, Prof. J. H. He, Prof. J. M. Lu
College of Chemistry, Chemical Engineering and Materials Science
Collaborative Innovation Center of Suzhou Nano Science and Technology
Soochow University
Suzhou 215123 (P. R. China)
E-mail: lujm@suda.edu.cn
2
2
-
2
2
2
2
-
BN40, respectively. The diffraction peaks associated with BN,
presented in Figure S1, are in good agreement with hexagonal
Supporting information for this article is given via a link at the end of the
document.
[6b]
BN (JCPDS card No. 45-0893).
patterns of the Pt/MnO
Furthermore, the XRD
2
composites exhibit four typical diffraction
1
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Angewandte Chemie International Edition
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COMMUNICATION
peaks, which correspond to the (002), (100), (111) and (200)
[12]
crystalline planes of hexagonal δ-MnO
2
.
No obvious XRD
peaks attributed to the Pt NPs are observed because of the low
Pt loadings. Additionally, the peak associated with the (111)
crystal plane of MnO
materials. The (111) peak intensity increases as a function of the
Pt/MnO composite amount in the aerogel materials. The
aforementioned results indicate that the Pt/MnO composites
2 2
is observed in all the Pt/MnO -BN aerogel
2
2
were successfully anchored to the BN aerogels, and furthermore,
that all the prepared samples demonstrate a high degree of
crystallinity with no impurity diffraction peaks observed.
To confirm the presence of Pt NPs in the Pt/MnO
and Pt/MnO -BN samples, both scanning electron microscopy
SEM) and transmission electron microscopy (TEM) were
2
composites
2
(
performed to investigate the morphologies and structures of the
as-prepared catalysts. As exhibited in Figure 1a, the Pt NPs
were first successfully prepared with diameters of ~30 nm.
Additionally, the Pt NPs were observed to be aggregates
comprising smaller nanoclusters. Figure 1b shows that the
Figure 2. (a) Low- and (b) high-magnification scanning electron microscopy
images of the Pt/MnO
2
-BN20 aerogel. (c) TEM micrograph and (d) photograph
2
MnO nanoflowers form a 3D scaffold, which provides a suitable
of the Pt/MnO -BN20 aerogel.
2
environment for Pt NP loading. Additionally, lattice fringes
having spacings of 0.240 nm, 0.290 nm and 0.480 nm are also
observed, which correspond to the (100), (020) and (110) crystal
Then, the SEM image of pure BN aerogel shown in Figure S2
suggests that the BN sheets is connected through thin polymer
layers. Meanwhile, the adsorption-desorption curve reveals a
type-IV isotherm for BN aerogel (Figure S4a) and the
[
12-13]
planes of MnO
2
, respectively (Figure 1c–d).
Furthermore,
high-angle annular dark-field scanning transmission microscopy
and the corresponding energy dispersive x-ray spectroscopy
2
-1
corresponding surface area is up to 80. 05 m g (Table S1).
Similarity, the interconnected highly porous Pt/MnO -BN aerogel
elemental mapping images (Figure 1e) of a single Pt/MnO
composite further suggest the existence of Pt NPs in the
Pt/MnO composites.
2
2
materials are formed when polyvinyl alcohol (PVA) molecules
act as a cross-linker to link the BN nanosheets. As displayed in
Figure 2a–b, both the porous layered structure of the aerogel
and the large BN sheet structure are obviously observed, which
favors reactant and product transfer, thereby accelerating the
oxidation of HCHO. Furthermore, the TEM micrograph
2
demonstrates the Pt/MnO
across the BN nanosheets, confirming the successful anchoring
of Pt/MnO to the aerogels (Figure 2c). Additionally, SEM
2
composites to be evenly distributed
2
elemental mapping characterization demonstrates that B, N, O,
Mn, and Pt are homogeneously distributed throughout the
aerogel matrix (Figure S3), indicating the successful preparation
of the Pt/MnO
possessing a fluffy and brown columnar macrostructure is
presented in Figure 2d. As illustrated in Figure S4b, the N
adsorption-desorption isotherm of the Pt/MnO -BN20 catalyst
2 2
-BN aerogels herein. The Pt/MnO -BN20 aerogel
2
2
exhibited a type-IV isotherm with a H3-type hysteresis loop. By
connecting the various layers to an ordered porous structure, the
interconnected network formed by the PVA molecules promotes
the high surface area of BN and Pt/MnO
2
-BN aerogels (Table
S1). Furthermore, the Pt/MnO -BN20 catalyst exhibits a high
2
surface area, which is beneficial for HCHO adsorption and in
reducing the HCHO concentration during the catalytic oxidation
process. Additionally, the inset of Figure S4b shows the pore
size distributions, which exhibit primary modal pore sizes of ca.
3–5 nm, and with which reveals the existence of mesoporous
structures in the aerogel catalysts. The HCHO uptake and
storage capacities are significantly improved as a result of the
enhanced effective surface areas and ordered porosity within
the internal structure of the aerogels. Such enhanced properties
improve the catalytic activity toward HCHO.
Figure 1. Transmission electron microscopy (TEM) images of (a) Pt
nanoparticles and (b) Pt/MnO composites. High resolution TEM micrographs
of (c–d) Pt/MnO composites. (e) High-angle annular dark-field scanning
transmission microscopy and energy dispersive X-ray spectroscopy elemental
mapping images of Mn, O and Pt of the Pt/MnO composites.
2
2
2
2
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than O
L
H
and O , indicating the larger content of surface
adsorbed oxygen species in Pt/MnO
the result of calculated g value of ~2.004 from ESR test implies
the presence of oxygen vacancies in the prepared Pt/MnO
BN10, Pt/MnO -BN20 and Pt/MnO -BN40 catalysts (Figure 3f).
As reported in the literatures, numerous surface active O
2
-BN20 sample. Besides,
2
-
2
2
–
–
2
species onthe composite surface such as O , O and -OH group,
which result from surface oxygen vacancies, play a significant
role in oxidation reaction and are beneficial for HCHO
[
13]
oxidation.
Figure 3. High-resolution X-ray photoelectron spectroscopy spectra for (a) B
1s, (b) N 1s, (c) Mn 2p, (d) Pt 4f, and (e) O 1s of the Pt/MnO
2
-BN20 sample. (f)
ESR spectra of the as-prepared Pt/MnO
BN40 samples.
2
-BN10, Pt/MnO
2
-BN20 and Pt/MnO -
2
Extensive
characterization was conducted to explore the surface element
compositions and chemical states of the Pt/MnO -BN20 sample.
The survey scan XPS spectrum shown in Figure S5 reveals the
existence of B, N, Mn, O and Pt elements in the Pt/MnO -BN20
X-ray
photoelectron
spectroscopy
(XPS)
Figure 4. (a) Concentration changes of HCHO as a function of reaction time
for the BN aerogel, Pt/MnO -BN and Pt/MnO /BN samples. (b) Real-time
HCHO concentration and corresponding ΔCO of the Pt/MnO -BN20 sample
during five recycling tests. (c) Proposed reaction mechanism for HCHO
oxidation over the Pt/MnO -BN catalysts.
2
2
2
2
2
2
2
The catalytic oxidation performance of the as-prepared
Pt/MnO -BN10, Pt/MnO -BN20, Pt/MnO -BN40, Pt/MnO /BN
sample, which is consistent with the elemental mapping analysis
results (Figure S3). Figure 3a-b shows that the B 1s and N 1s
spectra of the aerogel sample consist of two individual peaks,
derived from BN, at binding energies (BE) = 190.4 eV, 192.0 eV
and 398.0 eV, 398.7 eV, which are assigned to the B-N, B-O
2
2
2
2
and BN aerogel toward gaseous HCHO (200 ppm) conversion
under an air atmosphere was investigated in detail. As displayed
in Figure 4a, the pure BN aerogel is observed to have no
catalytic effect at this experimental temperature. However, the
HCHO concentration decreased and stabilized at 62 ppm after
[
6b, 14]
bonds and the N-B, N-H bonds, respectively.
Figure 3c
shows that the Mn 2p signal of the sample can be divided into
two peaks. The two strong peaks at BE = 641.83 eV and 653.63
eV, with a spin-energy separation of 11.8 eV, are assigned to
2
5 min because of the strong adsorption capacity of the BN
aerogel. Furthermore, the disordered Pt/MnO /BN catalyst
prepared through simple mixing of Pt/MnO and bulk BN
exhibited worse HCHO catalytic performance. However, the
Pt/MnO -BN aerogel materials clearly catalyze the degradation
of HCHO with higher efficiencies, which implies the superiority of
the porous aerogel structure. Among the Pt/MnO -BN aerogel
catalysts, the HCHO concentration on Pt/MnO -BN20 catalyst
decreases the fastest than those on Pt/MnO -BN10 and
Pt/MnO -BN40. After 50 min, we can see that the HCHO
concentration decrease from 200 ppm to 8, 19 and 33 ppm for
Pt/MnO -BN20, Pt/MnO -BN40 and Pt/MnO -BN10, respectively.
Importantly, the Pt/MnO -BN20 realizes a gaseous HCHO
conversion of ~96% into harmless H O and CO at room
temperature, showing the highest catalytic activity. The superior
catalytic performance of the Pt/MnO -BN20 catalyst derives from
the optimum Pt/MnO loading, the porous structure and the
2
4
+
[12]
2
2
Mn and derive from the MnO nanoflowers. As illustrated in
Figure 3d, the XPS spectrum of Pt 4f is deconvoluted into two
main peaks at ~71.25 eV and 74.52 eV, which are assigned to
the Pt 4f7/2 and Pt 4f5/2 binding energies, respectively. The Pt
2
2
4f
7/2 signal relates to the two peaks at 71.25 eV and 71.84 eV.
2
The Pt 4f5/2 signal comprises two components at 74.52 eV and
0
2
7
5.39 eV. The metallic Pt at BE = 71.25 eV and 74.52 eV is
[
6b, 12-13]
2
most prominent.
The bands at 71.84 eV and 75.39 eV are
2
+
attributed to Pt species, such as PtO. Additionally, the actual
Pt content in the Pt/MnO -BN20 sample is obtained through
2
2
2
2
2
inductively coupled plasma-atomic emission spectroscopy
measurements, as shown in Table S1. The actual values are
observed to be slightly lower than the experimental-theoretical
values as a result of the inevitable losses during the preparation
process. The O 1s high-resolution spectrum, as observed in
Figure 3e, comprises three peaks at 529.8, 531.5 and 532.9 eV,
2
2
2
2
larger specific surface area of the aerogel. Therefore, the
combination of catalytic oxidation with adsorption could
significantly enhance the efficiency of HCHO treatment
compared to adsorption or oxidation alone. The prepared
which can be attributed to lattice oxygen species (O
hydroxyl species (O ) and surface adsorbed oxygen species
), resprectively. Notably, the percentage of O is much higher
L
), surface
H
(
O
A
A
3
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COMMUNICATION
Pt/MnO
2
-BN aerogel materials exhibited satisfactory catalytic
of reactants and products, thereby accelerating the HCHO
oxidation process. Additionally, the combined adsorption and
oxidation properties enhance the efficiency of the catalyst to
performance toward removing HCHO in comparison with
previously reported literatures in Table S2. Additionally, for
practical applications, assessing the catalytic stability of
2
reduce the HCHO concentration in air. Thus, the Pt/MnO -BN
Pt/MnO
2
-BN20 is greatly significant. The catalyst cyclability
catalyst exhibits superior catalytic activity toward HCHO (200
ppm) achieving 96% conversion at room temperature.
Furthermore, the 3D Pt/MnO -BN aerogel, as a monolithic
2
toward the catalytic oxidation of HCHO was assessed by
subjecting the catalyst to five reaction-regeneration cycles, as
demonstrated in Figure 4b. The Pt/MnO
demonstrates excellent repeatability, even during the fifth cycle,
where the HCHO removal rate is still maintained at ~92.5%. The
2
-BN20 catalyst
catalyst, is easier to recycle and reuse in comparison with
catalysts in powder form. The monolithic porous composite
herein demonstrates promise as an oxidation catalyst and
provides useful insights into the design of high-performance
catalysts for room temperature HCHO removal.
BET result indicated Pt/MnO
surface area and mesoporous structure after the cycling tests
Figure S4b and Table S1). Meanwhile, the XRD patterns of the
Pt/MnO -BN20 catalyst before and after the cycling tests were
2
-BN20 sample remain the high
(
2
studied and are presented in Figure S7. No appreciable change
was found in the crystalline structure, and the inset SEM image
after the five cycling tests showed that the catalyst still has
original mesoporous structure, further suggesting that the
Acknowledgements
We gratefully acknowledge the financial support provided by the
National Natural Science Foundation of China (21938006,
Pt/MnO
removal HCHO reaction. Besides, the obvious increase of the
generated CO concentration compared to the decrease of the
2
-BN20 catalyst are relatively stable during the catalytic
5
1973148, 21722607, 21776190), Natural Science Foundation
of the Jiangsu Higher Education Institutions of China
17KJA430014, 17KJA150009), and the project supported by
2
(
entered HCHO concentration, which mainly result from the part
of HCHO are desorbed from the surface of the reactor and then
the Priority Academic Program Development of Jiangsu Higher
Education Institutions (PAPD).
oxidized to CO
Additionally, the mechanism for HCHO oxidation over the
Pt/MnO -BN catalyst at room temperature is suggested in
2
.
2
Keywords: Pt/MnO • boron nitride aerogel • formaldehyde •
2
catalytic oxidation
Figure 4c based on previous research. The porous layered
structure structure together with large SBET is beneficial to the
diffusion of HCHO towards the catalyst surface. HCHO reactant
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gas molecules are first adsorbed onto the OH group of the MnO
substrate through hydrogen bonding. Simultaneously,
2
O
2
molecules in the air are adsorbed onto and activated by
negatively charged Pt NPs (step I), which can facilitate the
[
15]
subsequent oxidation of HCHO. Moreover, the surface active
−
−
oxygen (O
2
, O , etc.) and structural hydroxyl groups play a vital
role in this process. The consumed hydroxyls are regenerated
by the dissociation of molecule water through the reaction of O ,
2
[3]
a) M. Chen, H. Yin, X. Li, Y. Qiu, G. Cao, J. Wang, X. Yang, P. Wang, J.
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−
−
[16]
O
(
+H
DOM) is generated through the process and the adsorbed
HCHO molecules are oxidized by activated oxygen species
step II). Thereafter, DOM is quickly oxidized and transformed
into formate species (intermediate) by activated oxygen species
step III). Next, intermediate formate species are further oxidized
to unstable carbonic acid (step IV) that rapidly decomposes into
harmless CO and H O products. Meanwhile, the conversion of
formates to CO and H O is likely the rate-determining step in
2
O → 2-OH.
Then, the intermediate dioxymethylene
(
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intermediates, With the continuous feeding of oxygen, the
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Inorg. Chem. 2018, 57, 8451-8457.
−
−
consumed O
oxygen on the surface vacancies, such as oxygen vacancies
Figure 3f), for further oxidation of formate species. Finally the
products are released from the surface of the Pt/MnO -BN
2
and O will be replenished by the activation of
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(
2
sample (step V) with the simultaneous regeneration of the
catalyst active site. In short, harmful HCHO gas can undergo
[
[
6]
7]
complete catalytic oxidation into harmless CO
the efficient Pt/MnO -BN catalyst.
2 2
and H O through
2
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In summary, a 3D Pt/MnO -BN catalyst was successfully
fabricated through Pt NPs loading onto MnO nanoflowers,
followed by anchoring of the Pt/MnO composites to BN
aerogels. The porous structure is beneficial to the rapid transfer
2
2
2
4
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COMMUNICATION
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Angewandte Chemie International Edition
10.1002/anie.202013667
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Entry for the Table of Contents
Three-dimensional monolithic Pt/MnO
2
-BN catalyst was successfully fabricated by anchoring Pt/MnO
2
nanoflower on boron nitride
(
BN) aerogels. The as-formed porous aerogels catalyst possesses the excellent ability of the combination of adsorption and oxidation
to effecient removal of formaldehyde at room temperature, as well as easier to be recycled and reused in comparison with powdery
ones.
6
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