Thermally conductive SiC as support of aluminum fluoride for the catalytic dehydrofluorination reaction

Article abstract of DOI:10.1016/j.catcom.2020.106033

Aluminum fluoride (AlF₃) is a typical catalyst for dehydrofluorination of hydrofluorocarbons (HFCs) to fluoroolefins with high heat of reaction. Consequently, heat supply and sintering are the key challenges for AlF₃-based catalysts. Herein, SiC with high thermal conductivity and resistance to HF corrosion is suggested as a candidate support of AlF₃ catalyst. The interaction between AlF₃ and SiC leads to uniform distribution of the catalytic phase, and as a result of this, AlF₃/SiC exhibits high catalytic activity and stability for the dehydrofluorination of 1,1-difluoroethane to vinyl fluoride. This study proposes a novel catalyst support (SiC) for strong endothermic catalytic reactions involving HFCs for the first time to the best of our knowledge.

Full text of DOI:10.1016/j.catcom.2020.106033

CatalysisCommunications142(2020)106033
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Catalysis Communications
journal homepage: www.elsevier.com/locate/catcom
Short communication
Thermally conductive SiC as support of aluminum fluoride for the catalytic
dehydrofluorination reaction
Jiaqin Lu, Wenfeng Han⁎, Wei Yu, Yongnan Liu, Hong Yang, Bing Liu, Haodong Tang, Ying Li
Industrial Institute of Catalysis, Zhejiang University of Technology, Hangzhou 310032, People's Republic of China
A R T I C L E I N F O
A B S T R A C T
Keywords:
Silicon carbide
Aluminum fluoride
Thermal conductivity
Dehydrofluorination
Aluminum fluoride (AlF3) is a typical catalyst for dehydrofluorination of hydrofluorocarbons (HFCs) to fluor-
oolefins with high heat of reaction. Consequently, heat supply and sintering are the key challenges for AlF3-
based catalysts. Herein, SiC with high thermal conductivity and resistance to HF corrosion is suggested as a
candidate support of AlF3 catalyst. The interaction between AlF3 and SiC leads to uniform distribution of the
catalytic phase, and as a result of this, AlF3/SiC exhibits high catalytic activity and stability for the dehydro-
fluorination of 1,1-difluoroethane to vinyl fluoride. This study proposes a novel catalyst support (SiC) for strong
endothermic catalytic reactions involving HFCs for the first time to the best of our knowledge.
1. Introduction
dehydrofluorination of hydrofluorocarbons (HFCs) is hindered both
thermodynamically and kinetically [12]. Therefore, it necessitates the
Global warming has been one of the major challenges for the whole
society which is attracting increasing attention recently [1]. In addition
to CO2, typical greenhouse gases, hydrofluorocarbons (HFCs) also play
a significant role with increasing emissions, which are usually of high
global warming potential (GWP) [2]. For instance, the GWP of 1,1-di-
fluoroethane (HFC-152a) is 1300 times larger than that of CO2 [3]. The
emission of these gases is regulated by the Montreal Protocol and its
amendments, especially the recent Kigali Amendment [4]. As reported
in the literature [5–7], dehydrofluorination of HFCs to hydro-
fluoroolefins (HFOs), the monomers used for manufacturing various
fluorinated polymers, is the most efficient route for converting these
greenhouse gases into value-added and environmentally benign che-
micals.
Besides, dehydrofluorination of HFC-152a can benefit the manu-
facturing of polyvinyl fluoride (PVF),which is a typical polymer mate-
rial with excellent resistance to weathering, chemically inert nature,
suitable mechanical strength, low permeability and light transmittance
[8,9], and it is widely adopted in packaging, glazing and electrical
applications [10]. At present, as the feedstock of PVF, the monomer of
vinyl fluoride (VF) is mainly produced via hydrofluorination of acet-
ylene and dehydrofluorination of HFC-152a. During the hydro-
fluorination of acetylene, HFC-152a would be generated as the by-
product with large quantity [3,11]. Consequently, dehydrofluorination
of HFC-152a plays an important role in the preparation of VF.
However, due to the high stability of CeF bond,
development of effective and proper catalysts. It is well accepted that
the catalysts should be Lewis acid catalysts, including fluorinated Cr, Al
and Mg-based catalysts. However, strong Lewis acid catalysts usually
suffer from coke formation [13]. Clearly, the Lewis acid sites function
as both active sites and coking sites leading to catalyst deactivation. As
a response to this, pre-deposition of carbon over the AlF3 catalyst before
reaction can improve significantly the stability for dehydrofluorination
of 1, 1, 1, 3, 3-pentafluoropropane [14]. Moreover, besides the fluori-
nated monomers, HF is also the major product of the dehydro-
fluorination of HFCs. Due to the presence of the highly corrosive HF,
there is very few choices left for the development of dehydrofluorina-
tion catalysts.
In addition to the challenge in selecting appropriate catalytic ma-
terials, heat transfer is another problem for dehydrofluorination reac-
tions. Clearly, the dehydrofluorination catalytic process includes the
cleavage of extremely stable CeF bonds with dissociation energies
higher than 450 kJ mol−1, which is one of the highest bond energies. As
a result, all the dehydrofluorination reactions are highly endothermic.
In order to provide enough heat to the reaction zone, superheated steam
or excessive dilution of N2 was preferred for the pyrolysis of HFCs and
HCFCs [15]. In the case of catalytic pyrolysis of HFCs, it will be fa-
vorable for the catalyst to be a very good thermally conductive mate-
rial.
Silicon carbide (SiC) is a typical ceramic material with strong cor-
rosion resistance, and high thermal conductivity [16]. Due to its
⁎ Corresponding author.
E-mail address: hanwf@zjut.edu.cn (W. Han).
https://doi.org/10.1016/j.catcom.2020.106033
Received 11 February 2020; Received in revised form 30 April 2020; Accepted 30 April 2020
Availableonline04May2020
1566-7367/©2020ElsevierB.V.Allrightsreserved.

J. Lu, et al.
CatalysisCommunications142(2020)106033
excellent stability and thermal conductivity, SiC was considered as
proper support of catalysts [17–20], and the catalytic selectivity and
resistance to sintering of the supported active phase can be significantly
improved [21]. In addition, SiC was found to be stable under the cor-
rosion of HF acid [22]. Consequently, Al-based catalysts supported on
SiC could be proposed that can effectively transfer heat to the reaction
occurred on the supported phase, reduce the temperature of the catalyst
bed, and prevent catalysts from sintering and carbon deposition at high
reaction temperatures.
In this work, aluminum fluoride (AlF3) supported on silicon carbide
(SiC) was synthesized and evaluated as a highly efficient catalyst for the
dehydrofluorination of HFC-152a toward fluoroolefins production. The
catalytic activity and stability of carbon-supported AlF3 (reference
catalyst) were also investigated and compared with that of SiC-sup-
ported AlF3.
(Philips-FEI Company).
Specific surface areas (m2/g) of the supports were determined by
the BET method making use of the N2 adsorption isotherms at liquid
nitrogen temperature (−195.7 °C) obtained using an Autosorb-1/C gas
adsorption analyzer (Quantachrome Instruments).
X-ray photoelectron spectroscopy (XPS) measurements were per-
formed on an ESCALAB210 (VG Co., monochromatized micro-focused
Mg Ka X-ray source) to study the metal oxidation states and surface
composition of the catalytic phase. Finally, solid state 27Al NMR was
adopted to explore better the structure of the catalysts.
2.4. Catalytic activity measurements
Catalytic activity measurements were carried out on a fixed bed
reactor (stainless steel, 8 mm (i.d), L = 400 mm) under atmospheric
pressure. The blank experiments (without a catalyst) showed no ob-
vious reactions. Prior to the reaction, 2 mL of the catalyst (20–40 mesh)
was loaded into the reactor and heated at 300 °C for 30 min in N2 gas
with a flow rate of 5 mL min−1. Then, HFC-152a /N2 gas mixture was
fed into the reactor (HFC-152a/N2 of 1/1, total flow rate of
10 mL min−1, SV = 300 h−1). The reaction products exit gas stream
was passed through a KOH solution to trap HF, and then the gaseous
products were analyzed by online gas chromatography (Fuli GC9790
chromatograph equipped with a PoraPLOT Q column and a TCD de-
tector). Since the selectivity to VF was higher than 99.8% for all the
catalysts, the selectivity data in dehydrofluorination activity test is not
shown.
2. Experimental
2.1. Reagents and chemicals
Silicon carbide (SiC, 99.0% with particle size between 0.5 and
0.7 μm), aluminum nitrate (Al(NO3)3·9H2O, > 98%) and ammonium
fluoride (NH4F, > 98%) were purchased from Aladdin Company,
Shanghai, China. All other required chemicals with analytical purity
were obtained from Sigma Aldrich, USA.
2.2. Synthesis of SiC-supported AlF3 catalyst
Silicon carbide supported aluminum fluoride catalyst was prepared
by the wet impregnation technique. 3 g of fine SiC powder was first
gradually dried at 120 °C for 12 h in the oven. Then, 0.7124 g alu-
minum nitrate and 0.2132 g ammonium fluoride were dissolved in 3 mL
deionized water. The obtained liquid mixture was then added dropwise
and mixed with 3 g of fine SiC powder using a micropipette. After aging
for 12 h, aluminum nitrate was fluorinated into aluminum fluoride.
Finally, a homogeneous paste was obtained. The paste was initially
dried at 120 °C and then annealed at 400 °C for 3 h in nitrogen gas
atmosphere. As a reference, activated carbon-supported AlF3 was pre-
pared with exactly the same procedure.
3. Results and discussion
According to reaction (1), simple dehydrofluorination of HFC-152a
leads to the formation of vinyl fluoride (VF). After the removal of by-
product HF with water scrubber, almost pure VF would be obtained.
However, due to the high stability of CeF bonds, no reaction was de-
tected at elevated temperatures in the absence of catalyst. Clearly, it is
necessary to develop a proper catalyst for this process. In addition, the
enthalpy change of this reaction is as high as 84.4 kJ mol−1
Consequently, heat supply for this ⊙reaction is another key challenge.
.
CH3CHF2 → CH2 = CHF + HFΔr H298 = 84.4kJmol−1
(1)
2.3. Characterization of catalysts
As a response, SiC with high thermal conductivity and resistance to
HF corrosion was selected as a support of AlF3 catalyst for the first time
to the best of our knowledge. As shown in Fig. 1a, no noticeable AlF3
diffraction peaks were observed in the XRD pattern of 5 wt% AlF3/SiC
catalyst, in good agreement with the PDF card (74–1302) of cubic SiC
(6H-SiC) without observing any other peaks. Clearly, SiC used in the
present study was well crystalized. Since the detection limit of powder
XRD for crystalline size determination is less than ~4 nm, the absence
of AlF3 diffraction peaks may suggest that AlF3 was well dispersed on
SiC. No change in the XRD pattern was noticed for the spent AlF3/SiC
The catalysts were characterized by powder X-ray diffraction (XRD)
using
a Thermo ARL X'TRA diffractometer (Cu-Kα radiation,
λ = 0.154056 nm) at room temperature, which was equipped with a Si
(Li) solid detector at 40 kV/40 mA and a monochromator.
Transmission electron microscopy (TEM), energy dispersive X-ray
spectrometry (EDXS) mapping and high-resolution transmission elec-
tron microscopy (HRTEM) images were recorded to further explore the
microstructure of catalysts over a Tecnai G2 F30 S-Twin at 300 kV
(b)
(a)
AlF3/SiC-spent
AlF3/C-Fresh
AlF3/SiC-fresh
AlF3/C-Spent
PDF#84-1672 (AlF3)
PDF#74-1302 (SiC)
10 20 30 40 50 60 70 80
2-Theta
10 20 30 40 50 60 70 80
2-Theta
Fig. 1. XRD patterns of (a) fresh and spent 5 wt% AlF3/SiC catalysts, (b) fresh and spent 5 wt% AlF3/C catalysts.
2

J. Lu, et al.
CatalysisCommunications142(2020)106033
Fig. 2. TEM images along with EDX elemental mapping. (a) AlF3/SiC-fresh and (b) AlF3/C-fresh catalysts.
catalyst (after reaction).
Hence, SiC contains impurities such as Si and SiO2 which are facilely
fluorinated by fluorine -containing species.
By contrast, clear AlF3 diffraction peaks were detected over AlF3/C
indicating the formation of AlF3 crystallites (Fig. 1b). Based on the XRD
pattern, the crystal size of AlF3 was determined to be 24.6 nm for the
fresh AlF3/C catalyst according to the Scherrer equation. After reaction,
the crystal size of spent AlF3/C increased to 28.7 nm, indicating sig-
nificant sintering of AlF3 over the activated carbon support.
Both AlF3/SiC and AlF3/C catalysts were further characterized by
TEM and EDX mapping. As shown in Fig. 2, because of the poor contrast
between AlF3, SiC and activated carbon, no AlF3 particles could be
clearly observed in TEM images. However, with the help of EDX map-
ping, the elemental distribution could be completely disclosed. For the
AlF3/SiC catalyst, the elements including C, Si, Al and F were identified.
Carbon (C) (Fig. 2a) and Si (Fig. S1) were observed all over the particle.
In addition, Al and F were dispersed uniformly. The EDX spectra of the
AlF3/C showed the presence of C, F and Al (Fig. 2b). However, AlF3
with large particle size was found with concentrated distribution of Al
and F. The above results were well consistent with the observations
from XRD. Clearly, the TEM examination and EDX elemental mapping
results proved that the desired loading of AlF3 had been successfully
achieved.
After reaction, Si concentration in spent AlF3/SiC catalyst was re-
duced significantly (Fig. S2), which can be attributed to coke deposition
or etching of Si by HF during reaction. However, comparing the map-
ping of the C element in Fig. 2a and Fig. S2, only slight increase in C
content can be noticed, while more AlF3 (Al and F elements in Fig. S2)
were exposed. Therefore, some of Si element can be etched by the HF
product during the dehydrofluorination of HFC-152a. By contrast,
carbon content increased significantly in spent AlF3/C, while more
sintered AlF3 particles can be found (Fig. S3), indicating the coke for-
mation on AlF3/C during reaction. Elemental compositions of the fresh
and spent 5 wt% AlF3/C and 5 wt% AlF3/SiC determined by mapping in
Table S1 reinforce the above discussion.
As discussed previously, SiC is stable under the corrosion of HF
[22]. We suggested that the etching of Si should not be contributed by
SiC. As demonstrated in Fig. S4, significant amount of Si was fluori-
nated by NH4F during catalyst preparation (XPS, binding energy of
102.3 eV), in addition to SiC (XPS, binding energy of 100.3 eV) [23].
The presence of AlF3 over AlF3/SiC and AlF3/C catalysts is re-
inforced by HRTEM studies. Clear lattice fringes for both AlF3/SiC and
AlF3/C catalysts were detected (Fig. S5). The lattice spacing of fringe
along (200) direction is 0.35 nm, and that of fringe along (002) di-
rection is 0.36 nm in the AlF3 crystal structure [24]. Part of the AlF3
crystals are highlighted with yellow circles (Fig. S5). As disclosed by
HRTEM, the crystalline size of AlF3 in the fresh AlF3/SiC catalyst is
~6–8 nm, which is larger than the determination by XRD (Fig. S6a),
probably because of the difficult to detect smaller crystalline particles
in the HRTEM due to the strong lattice fringes of SiC. After reaction, the
crystalline size of AlF3 slightly increased to 9 nm (Fig. S6b). By contrast,
this was increased from 6 to 13 nm for the AlF3/C catalyst (Fig. S6c and
d), suggesting that AlF3 tends to sinter more significantly over AlF3/C
than over AlF3/SiC, which agrees well with the results of XRD and EDX
mapping.
The high dispersion of AlF3 over SiC is not ascribed to its surface
area. As indicated in Fig. S7, type-III adsorption isotherm and H3
hysteresis loop can be identified for SiC, suggesting that the surface
texture was characteristic of a nonporous solid. Actually, the surface
area of SiC estimated in the present study was only 1.4 m2/g. However,
the surface area of activated carbon is extremely high. A type-II ad-
sorption isotherm and H4 hysteresis loop with specific surface area of
~1100 m2/g were found (Fig. S7b). Clearly, the distribution of AlF3 is
most likely attributed to the interaction between AlF3 and SiC.
Therefore, XPS experiments were further conducted for AlF3/SiC and
AlF3/C catalysts to obtain deeper insight into the interactions of AlF3
and its supports.
As shown in Fig. 3, compared with Al 2p in AlF3/C, the binding
energy in AlF3/SiC decreases from 77.49 eV to 77.12 eV, shifting to-
ward lower energy by 0.37 eV. Clearly, the strong AleF bond is wea-
kened over the SiC support. The shift indicates that F element of AlF3
has been interacted with Si of SiC. This conclusion can be reinforced by
the change of F 1 s binding energy. The binding energy of F in AlF3/SiC
(688.60 eV) is 0.45 eV higher than that in AlF3/C (688.15 eV), which
confirms the strong interaction between AlF3 and SiC with F atoms.
Moreover, this interaction can be further confirmed by the change in
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J. Lu, et al.
CatalysisCommunications142(2020)106033
4. Conclusions
688.15
×5
(a)
(b)
77.49
Aluminum fluoride (AlF3) supported on silicon carbide (SiC) was
successfully synthesized as potential catalyst for practical dehydro-
fluorination reaction. As the dehydrofluorination involves the dis-
sociation of CeF bond, large amount of reaction heat is required. With
SiC as the support, its thermal conductivity facilitates the transfer of
reaction heat to and from the supported catalytic phase. Consequently,
less sintering of AlF3 can be achieved compared with the AlF3/C cata-
lyst. Although its surface area is extremely low, the interaction between
AlF3 and SiC can contribute to the uniform dispersion of AlF3. The
catalytic performance of aluminum fluoride loaded on silicon carbide in
the dehydrofluorination of 1,1-difluoroethane to vinyl fluoride can be
significantly higher than that of AlF3 supported on activated carbon.
The present results indicated that SiC is a potential and efficient support
for catalysts of fluoroalkane dehydrofluorination. This study proposed a
novel catalyst support (SiC) with high thermal conductivity and stabi-
lity for the carrying strong endothermic catalytic reactions involving
HFCs.
AlF /C
3
AlF /C
3
×5
688.60
77.12
AlF /SiC
3
AlF /SiC
3
680
684
688
692
696
70 72 74 76 78 80 82 84
Binding Energy (eV)
Bending Energy (eV)
Fig. 3. XPS spectra of fresh 5 wt% AlF3/SiC and 5 wt% AlF3/C for (a) Al 2p and
(b) F 1 s.
Declaration of Competing Interest
70
(a)
60
50
40
30
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influ-
ence the work reported in this paper.
Acknowledgements
5% AlF3/SiC
20
We thank the Zhejiang Provincial Natural Science Foundation of
China (Grant No. LY19B060009) for financial support.
5% AlF3/C
10
SiC
0
Appendix A. Supplementary data
0
10
20
30
40
Time on Stream (h)
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.catcom.2020.106033.
Fig. 4. Conversion of HFC-152a over different catalysts as a function of time on
stream (atmospheric pressure, 300 °C, GHSV of 300 h−1, feed gas composition:
50 vol% HFC-152a and 50 vol% N2).
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