Plasmon-Assisted Photothermal Catalysis of Low-Pressure CO2 Hydrogenation to Methanol over Pd/ZnO Catalyst

Article abstract of DOI:10.1002/cctc.201802081

In this work, we report a novel strategy to promote the industrial methanol production from CO₂ hydrogenation at low pressure (12 bar) over a Pd/ZnO catalyst via introducing light irradiation into a modified continuous-flow fixed-bed reactor. The methanol yield was significantly enhanced by a photothermal synergistic effect and visible light was confirmed as the major contributor (>90 %) due to the localized surface plasmon resonance of Pd.

Full text of DOI:10.1002/cctc.201802081

Accepted Article
Title: Plasmon-assisted photothermal catalysis of low-pressure CO2
hydrogenation to methanol over Pd/ZnO catalyst
Authors: Dengdeng Wu, Kaixi Deng, Bing Hu, Qingye Lu, Guoliang Liu,
and Xinlin Hong
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10.1002/cctc.201802081
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Plasmon-assisted photothermal catalysis of low-pressure CO2
hydrogenation to methanol over Pd/ZnO catalyst
Dengdeng Wu,a Kaixi Deng,a Bing Hu,a Qingye Lu,b Guoliang Liu*a, and Xinlin Hong*a
Abstract: In this work, we report a novel strategy to promote the
industrial methanol production from CO2 hydrogenation at low
pressure (12 bar) over a Pd/ZnO catalyst via introducing light
irradiation into a modified continuous-flow fixed-bed reactor. The
the high capability of H2 dissociation over Pd [11-15]. However,
these systems still suffer from low methanol yield at low pressure.
Thus, the development of efficient catalytic low-pressure
methanol synthesis remains highly desirable.
methanol yield was significantly enhanced by
a photothermal
It is well accepted that the dissociative CO2 adsorption is the
initial step in CO2 reduction and the C-O bond is activated by
electron transfer from the d-band of the metal into the antibonding
synergistic effect and visible light was confirmed as the major
contributor (>90%) due to the localized surface plasmon resonance of
Pd.
δ-
orbital of CO2 to form e.g. CO2 [16,17]. Apart from thermal
excitation, hot electrons can be also generated by photoexcitation
of semiconductors or metals with a photon response, which
enables the photocatalytic CO2 reduction to happen under mild
conditions [18-20]. Inspired by the photo-induced CO2 activation, we
here took a novel attempt to introduce light irradiation to the
traditional catalysis of CO2 hydrogenation to methanol, aiming to
promote CO2 conversion and methanol production under low
pressure condition. Pd/ZnO was employed as a model catalyst
and a pressure of as low as 12 bar was used. Both CO2
conversion and methanol yield were significantly promoted by the
introduction of light illumination. To the best of our knowledge, this
is the first study of photothermal methanol synthesis from CO2
hydrogenation in an industrial-style continuous flow fixed-bed
reactor. We at last demonstrate that the localized surface
plasmon resonance (LSPR) effect of Pd nanoparticles (NPs)
mainly contributes to the activity enhancement under light
irradiation.
The global warming has gained increasing concern in recent
years. Given that carbon dioxide (CO2) is the primary greenhouse
gas from the combustion of fossil fuels, it would be attractive to
utilize CO2 as a raw carbon source to produce useful industrial
products [1,2]. For example, methanol can serve as a chemical
platform for future fuels and valuable chemical production [3]. The
hydrogenation of CO2 to methanol (Equation 1) is the key initial
reaction for the so-called “methanol economy” in the post-oil era
[3]. Considering “clean” hydrogen can be obtained from water
splitting driven by solar or redundant electric source or from
renewable biomass, the methanol synthesis reaction (MSR)
would also be regarded as a means of hydrogen storage in a more
energy-dense and transportable form.
CO2 + 3H2 → CH3OH + H2O ΔH298K = -49.5 kJ mol-1 (1)
CO2 + H2 → CO + H2O
ΔH298K = 41.2 kJ mol-1
(2)
The Pd/ZnO catalyst was prepared by using conventional
impregnation method (see SI). The representative transmission
electron microscopy (TEM) images in Figure 1a and Figure S1
shows an even distribution of Pd NPs dispersed on ZnO
substrates. The size of Pd NPs in this catalyst is about 6.1±0.8
nm on the average. The high resolution (HR) TEM image in Figure
1b clearly shows the typical lattice fringes of ZnO (100) and Pd
(111), suggesting the formation of Pd-ZnO interface. Interestingly,
a d-spacing of 0.219 nm at Pd-ZnO interface is also evidenced for
bimetallic PdZn (111) facet, revealing the formation of PdZn alloy,
as described in Figure 1b and Figures S1-2. It is believed that,
upon H2 treatment, Zn atoms from ZnO gradually migrate onto Pd
surface and intermix with Pd atoms to form bimetallic PdZn phase
at Pd-ZnO interface [21]. Such strong-metal-support-interaction
(SMSI) enables the wetting of Pd NPs on ZnO and the formation
of interfacial PdZn alloy phase. X-ray diffraction (XRD) pattern of
reduced Pd-ZnO in Figure 1c shows a series of strong peaks for
wurtzite ZnO (JCPDS#36-1451) and small PdZn (111) diffractions
(PDF#06-0620), along with a weak shoulder peak at 40.1o (Pd
(111) diffraction). PdZn alloy evolves from Pd upon H2 reduction
(Figure S3), well consistent with above TEM results. Moreover, X-
ray photoelectron spectroscopy (XPS) spectrum of Pd 3d is
deconvoluted into two Pd species: monometallic Pd at 334.5 eV
and PdZn alloy at 335.5 eV [22,23]. Alloying Pd with Zn results in a
chemical shift to higher binding energy by 0.6–1 eV due to
electron modification. Such alloying can shift the d-band structure
Thus far, extensive and continuous studies have been
conducted on the hydrogenation of CO2 to methanol in the past
decades [4-9]. Commercial Cu/ZnO/Al2O3 catalysts have been
widely studied for this reaction at both elevated pressure and
temperature ranging from 50 to 100 bar and 200 to 300 oC for over
50 years [4-6]. Thermodynamically, a condition of high pressure
and low temperature favors the methanol production reaction over
the reverse water gas shift reaction (RWGS, Equation 2).
However, the high pressure condition is a significant barrier for
industry to overcome because first, elevating pressure increases
operational cost and second, the catalytic procedure at high
pressure cannot be coupled with the upstreaming low-pressure
CO2/H2 mixture (at or below 20 bar) produced from low-
temperature aqueous phase reforming of biomass derivatives [10]
.
To explore low-pressure or even atmospheric-pressure methanol
synthesis, which has become an attractive topic in recent years,
Pd based catalysts have been developed by a few groups, due to
[a]
[b]
College of Chemistry and Molecular Sciences, Wuhan University,
Wuhan, 430072, P. R. China. E-mail: hongxl@whu.edu.cn;
liugl@whu.edu.cn
Department of Chemical and Petroleum Engineering, University of
Calgary, Calgary, AB T2N 1N4, Canada
Supporting information for this article is given via a link at the end of
the document.
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10.1002/cctc.201802081
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of Pd towards a behaviour of Cu. The PdZn alloy is generally
believed as the main active sites for methanol synthesis from CO2
hydrogenation [24]. CO pulse chemisorption further confirms the
formation of surface PdZn alloy because of a significant decrease
in the CO adsorption capability after H2 treatment (Figures S4 and
S5).
eV and it can absorb the UV region of light (wavelength below 420
nm), as confirmed by the diffuse reflectance spectra (DRS) of
Pd/ZnO and pure ZnO in Figure 3. After absorption of UV energy,
electron transition would happen from valence band (VB) to
conduction band (CB). The hot electrons may migrate from the
CB in ZnO to the Pd-ZnO interfaces (e.g., PdZn alloy) for catalysis.
Our previous work reported that the electron promotion of ZnO by
the doping of CdSe favors the selective hydrogenation of CO2 to
methanol over Cu/ZnO catalysts [27]. Therefore, we speculate the
increase in electron density of ZnO under light irradiation may be
a reason for the enhancement and thus it should be considered
first.
Figure 2. (a) Conversion of CO2 and (b) STY of methanol and CO in CO2
hydrogenation over the Pd/ZnO catalyst at a reaction temperature ranging from
190 to 270 oC before and after light irradiation. Reaction conditions: gas hourly
space velocity (GHSV) = 20400 mL h-1 gcat-1, CO2:H2 = 1:3 with a pressure of 12
bar, two 500W high-pressure mercury lamps as the light source.
Figure 1. (a) TEM image and Pd size distribution (inset a) and (b) high resolution
TEM image, (c) XRD pattern and (d) deconvolution of Pd 3d XPS spectrum of
the reduced Pd/ZnO catalyst.
We next performed the photo-thermal catalysis of CO2
hydrogenation under light irradiation with UV block by using a filter
to cut off the wavelength shorter than 420 nm. According to the
results in Figure 3a, when the UV region is blocked, the yields of
methanol and CO over Pd/ZnO still account for 93.5% and 90.4%
of those under full spectra irradiation, respectively. The slight drop
is probably due to the loss of the illumination intensity after the
cutoff of UV waves. It implies that visible light is more important
than UV for the photo promotion effect. Considering ZnO cannot
be excited by visible light, we deduce that the Pd component plays
a decisive role in the activity promotion via the utilization of a wide
range of visible light. To provide further evidence, we carried out
a control experiment using a referenced Pd/Al2O3 catalyst (Pd
loading of 5 wt%, close to the loading of Pd in Pd/ZnO catalyst of
5.2 %, Table S1) under the same conditions. Al2O3 is an inert
support and it cannot be excited by the light source due to a large
band gap (8.8 eV). It has been shown that CO is the sole product
in CO2 hydrogenation over Pd/Al2O3 because Pd itself is only
favorable for the RWGS reaction [28]. However, this does not
prevent us from getting useful information about the mechanism
of photo-induced promotion. With full light on, the promotion of
CO yield by 200% was obtained, as depicted in Figure 2d. After
UV block, the Pd/Al2O3 catalyst still performed the major activity,
with a CO yield slightly lower than that under the full spectra. This
highlights the crucial role of Pd in our photocatalytic CO2
We next examined if the light irradiation can affect the catalytic
performance of CO2 hydrogenation over the Pd/ZnO catalyst. CO
and methanol are the only carbonaceous products detected by
gas chromatography. Figure
2
compares the catalytic
performance with and without light irradiation. Over a temperature
range from 190 to 270 oC, light irradiation can significantly
enhance the CO2 conversion by more than two times (Figure 2a).
This is probably because the light irradiation improves the
electron density of active metal surface and thus facilitates the
electron transfer from the metal d-band into the antibonding orbital
δ-
of CO2 to form e.g. CO2 in the initial CO2 activation.16,17 Figure
2b shows the variation trend of product space-time yield (STY).
The STYs of both methanol and CO are promoted by light
irradiation and the promotion degree varies with the reaction
temperature. The increment ratios (STY under irradiation/STY
under dark) for both products are described in Table S2. The
methanol activity is promoted by 1.5~3.0 times, while the CO STY
by 1.6-4.7 times. It seems that the RWGS reaction is more
sensitive to light irradiation than MSR, especially at reaction
temperatures of above 200 oC. At 250 oC, light irradiation
promotes methanol STY by 1.8 times but CO STY by 4.2 times.
We have shown that the light irradiation greatly promoted the
catalytic activity in the industrial CO2 hydrogenation, and further
studies were conducted to figure out how the light irradiation
promotes the hydrogenation of CO2. To address such a question,
we initially speculated that the semi-conducting ZnO component
may play an important role for the improvement as ZnO has been
widely used as a photocatalyst [25, 26]. ZnO has a band gap of 3.2
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hydrogenation. So how did the Pd species react with light for the
promotion?
MSR. The LSPR brings an electron rich state in bare Pd surface
(without contact with supporting ZnO), which further leads to the
great promotion towards CO formation (see more discussion in
ESI). This is also confirmed by the increased CO yield over
referenced Pd-Al2O3 catalyst.
Figure 3. (a) STY of methanol and CO over the Pd-ZnO and referenced Pd-
Al2O3 at 250 oC under different light illumination conditions. (b) Normalized UV-
vis diffuse reflectance spectrum of Pd/ZnO compared with pure ZnO.
Generally, free electrons of a nanostructured metal are capable
of interacting with the incident light and generate a localized
surface plasmon resonance (LSPR) [20,29]. The LSPR effect of the
metals such as Ag and Au has been extensively studied in
photocatalysis due to the fact that the LSPR is found in the visible
part of the solar spectrum, which can increase the light harvesting
ability of high-band-gap photocatalysts after surface decoration
and thus increase their overall activity [30, 31]. Nanosized Pd was
also reported to exhibit a LSPR, but it is mainly located in the UV
region of spectrum (300 nm), which impedes the development of
the LSPR of Pd [32]. The LSPR adsorption center can be
influenced by not only the size of Pd NPs but also the used
supports.[33-35] Recently, Lacerda et al. reported TiO2 supported
Pd NPs with the size of 3-5 nm have a board LSPR absorption in
the visible region centered at 456 nm [33]. It is verified that the
LSPR position for supported Pd could red shift by up to 100 nm
from UV to visible region [34, 35]. Such efforts provide an interesting
new approach to visible light photocatalysis with Pd since Pd
shows excellent catalytic activity compared with Au and Ag. As for
our Pd/ZnO sample, the adsorption is rather broad and weak, and
the LSPR center further shifts to around 570 nm, as confirmed
from the DRS spectrum in Figure 3. The significant red shift of
LSPR position may be due to the strong metal-support interaction
via the formation of PdZn alloy at the Pd-ZnO interface. We
believe that the LSPR could promote the photothermal CO2
hydrogenation in our experiment via a similar mechanism to that
for LSPR assisted photocatalysis.
Scheme 1. Mechanism for the photo-induced promotion in CO2 hydrogenation
to methanol.
In summary, we have demonstrated a novel plasmon-induced
promotion effect in the traditional CO2 hydrogenation in a
modified continuous-flow fixed-bed photothermal reactor. With
light illumination, the conversion of CO2 increases significantly
by up to 200%. Despite the decrease in methanol selectivity, the
yield of methanol is still promoted by 1.5~3 times at 190~250 oC.
More importantly, we find the visible light region of the spectrum
mainly contributes to the major promotion. The LSPR effect of
Pd is proposed as the main reason for the photothermal synergy
in the hydrogenation of CO2. Hopefully, this work would provide
a novel approach to the promotion of thermal CO2 hydrogenation
via the LSPR effect towards the wide utilization of solar energy.
Experimental Section
Preparation of Catalysts
The loading of Pd onto commercial ZnO or Al2O3 support was
achieved by using an impregnation method. Briefly, ZnO or Al2O3
powder was immersed into a Pd(NO3)2 solution in ethanol and the
mixture was kept at 50 °C under stirring until the solvent was
evaporated. The obtained powder was then calcined at 400 °C for
2 h. The catalyst was pre-reduced in 10% H2/Ar at 250 °C for 2 h
before further characterizations.
Given the above results, we propose a mechanism as showed
in Scheme 1. Under light irradiation, Pd nanoparticles adsorb
visible light and hot electrons are generated on Pd surfaces due
to the LSPR effect. These electrons would migrate to the Pd-ZnO
interface where the PdZn bimetallic phase is formed, as confirmed
by TEM and XPS analysis (Figure 1). The PdZn alloy sites are
generally believed as active sites for methanol synthesis from
thermal-type CO2 hydrogenation [14,24]. The increased electron
density at PdZn active sites would facilitate the dissociative
adsorption of CO2 via electron injection to the antibonding orbital
of CO2 and thus promotes the activation of CO2.[16,17] This can
explain the enhancement in the methanol STY and increased CO2
conversion (see more discussion in ESI). We believe this
represents a new type of photothermal synergy in catalysis. On
the other hand, monometallic Pd is more active for RWGS than
Photothermal catalytic tests
The reactor is composed of a quartz tube and two metal caps
with fluororubber O-ring to avoid leaking. The quartz tube has a
length of 35 cm, outside diameter of 24 mm and wall thickness of
8.5 mm. A thermocouple detector is equipped in the quartz tube
directly contacting the tested catalyst. The reaction temperature
(based on catalyst) is well controlled either under light irradiation
or under dark. The quartz tube can be heated up by a surrounding
furnace. The catalyst is fixed by quartz fiber in the tube at the
corresponding height of light source. The light source consists of
two high-pressure mercury lamps equipped with a quartz-made
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Entry for the Table of Contents (Please choose one layout)
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COMMUNICATION
A
localized
surface
promotes
plasmon
industrial
Dengdeng Wu,a Kaixi Deng,a Bing Hu,a
Qingye Lu,b Guoliang Liu*a, and Xinlin
Hong*a
resonance
methanol production from CO2
hydrogenation at low pressure over
Pd/ZnO catalyst via the introduction of
Page No. – Page No.
light irradiation into
continuous-flow fixed-bed reactor.
a
modified
Plasmon-assisted photothermal
catalysis of low-pressure CO2
hydrogenation to methanol over
Pd/ZnO catalyst
Layout 2:
COMMUNICATION
Author(s), Corresponding Author(s)*
((Insert TOC Graphic here))
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Title
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