Ni-PC@SBA-15 derived from nano-sized Ni-MOF-74 confined in SBA-15 as a highly active catalyst for gas phase catalytic hydrodechlorination of 1,2-dichloroethane

Article abstract of DOI:10.1039/d0cc00998a

A novel catalyst consisting of metallic Ni and porous carbon (PC) confined in SBA-15 was fabricated by the confined pyrolysis of nano-sized Ni-MOF-74 that was in situ grown in the mesopores of SBA-15. Due to the intimate contact between Ni and PC in a fine Ni-PC composite resulting from the confinement effect of mesoporous SBA-15, the catalyst displayed prominent catalytic activity and selectivity in the gas phase catalytic hydrodechlorination of 1,2-dichloroethane. This journal is

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DOI: 10.1039/D0CC00998A
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Ni-PC@SBA-15 derived from nano-sized Ni-MOF-74 confined in
SBA-15 as highly active catalyst for gas phase catalytic
hydrodechlorination of 1,2-dichloroethane
Received 00th
January 20xx,
Xin Ning,a,b Dongzhi Deng,a Heyun Fu*,a Xiaolei Qu,a Zhaoyi Xu,a Shourong Zhenga
Accepted 00th January 20xx
DOI: 10.1039/x0xx00000x
However, the direct pyrolysis of MOFs also results in large
metal particles due to aggregation of metal particles at high
carbonization temperature.5 To enhance the dispersion of
MOFs, hybridizing MOFs with SiO2 or carbonaceous materials
has been explored and the hybrid materials exhibited
promising performances in gas adsorption, storage and
electrochemical reactions.6 Notably, confining nanoparticles in
well-defined channels is an effective approach to enhance
particle dispersion and inhibit particle aggregation. However,
studies using confined MOFs as precursors to prepare
supported catalysts are still very limited in the literature.6f, 6g
Herein, we fabricated highly dispersed Ni-PC composite
located in the pores of an ordered mesoporous silica (i.e., SBA-
15) using nano-sized Ni-MOF-74 confined in SBA-15 as the
precursor. SBA-15 was selected as the matrix to host Ni-PC
particles due to its ordered mesopore structure, high pore
volume and large surface area.7 The preparation route of the
catalysts is described in Scheme 1 and the details of
preparation procedure are given in ESI † . Briefly, a desired
amount of nano-sized Ni-MOF-74 was in-situ grown inside the
mesopores of SBA-15 (denoted as xNi-MOF-74@SBA-15, x=1, 4,
17, where x represented theoretical Ni loading amount).
Subsequently, the highly dispersed Ni-PC composite confined
in SBA-15 pores was readily obtained upon direct pyrolysis of
xNi-MOF-74@SBA-15 at 450 oC under N2 atmosphere. The
resultant catalyst is denoted as xNi-PC@SBA-15. For
comparison, PC supported Ni catalyst (denoted as Ni@PC) was
prepared by direct carbonization of pristine Ni-MOF-74. To
investigate the role of PC, 1Ni-PC@SBA-15 was calcined in air
to obtain a catalyst without carbon (denoted as 1Ni@SBA-15).
A Ni-based catalyst supported on SBA-15 with similar Ni
A novel catalyst consisting of metallic Ni and porous carbon (PC)
confined in SBA-15 was fabricated by the confined pyrolysis of
nano-sized Ni-MOF-74 that was in-situ grown in the mesopores of
SBA-15. Due to the intimate contact between Ni and PC in fine Ni-
PC composite resulting from the confinement effect of
mesoporous SBA-15, the catalyst displayed prominent catalytic
activity and selectivity in the gas phase catalytic
hydrodechlorination of 1,2-dichloroethane.
Gas phase catalytic hydrodechlorination (HDC) is an attractive
avenue to convert chlorinated organic pollutants into less toxic
and valuable hydrocarbons.1 Supported Ni-based catalysts are
cost-effective and highly selective catalysts despite of their
relatively lower catalytic activities as compared with noble
metal catalysts.2 Additionally, carbonaceous materials and SiO2
are widely adopted catalyst supports due to their excellent
resistance against corrosive HCl formed in the HDC processes.
For Ni-based catalysts supported on carbon and SiO2, however,
large metal particles are generally formed and metal particle
growth commonly occurs during the preparation and reaction
processes because of the lack of strong metal-support
interaction, resulting in low catalytic activity. Numerous
hierarchically structured Ni-based catalysts, such as core-shell,
yolk-shell, lamellar and embedded catalysts, have been
explored to enhance metal dispersion and catalytic stability.3
Metal-organic frameworks (MOFs) can be easily converted into
nano-sized metal particles supported on porous carbon (PC)
through pyrolysis under controlled atmosphere, providing
facile and one-step synthesis of supported metal catalysts.4
Ni-MOF-74
Ni-PC
a. State Key Laboratory of Pollution Control and Resource Reuse, School of the
Environment, Nanjing University, Nanjing 210046, China
b. Jiangsu Key Laboratory of Environmental Material and Engineering, School of
Environmental Science and Engineering, Yangzhou University, Yangzhou 225000,
China.
Ni(CH3COO)2
Impregnation
DHTP
in-situ grown
N2
Calcination
Ni-MOF-74@SBA-15
Ni(CH3COO)2@SBA-15
Ni-PC@SBA-15
SBA-15
E-mail: heyunfu@nju.edu.cn; Tel: +86-25-89680373
†Electronic Supplementary Information (ESI) available: Experimental details and Scheme 1. Schematic illustration of the fabrication of Ni-PC@SBA-15
characterization results of the catalysts. See DOI:10.1039/x0xx00000x
catalysts derived from nano-sized Ni-MOF-47 confined in SBA-15.
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o
loading amounts prepared by the conventional impregnation linker decomposition temperature was 355 CViefworArtpiclreisOtnilninee
method was also involved as comparison (denoted as 1Ni/SBA- nano-sized Ni-MOF-74, in agreement DwOIi:t1h0.1t0h3e9/Dli0tCeCra0t0u9r9e8.A8
15). The gas phase catalytic HDC of 1,2-dichloroethane was Probably due to the protection by SBA-15,15 the
used to evaluate the catalytic performances of the catalysts.
decomposition temperature was slightly higher for xNi-MOF-
The contents of Ni in the catalysts were determined by 74@SBA-15 (395-405 oC).
inductively coupled plasma-atomic emission spectrometry
(ICP-AES) and the results are listed in Table S1 in ESI†. Ni@PC
had a Ni content of 73.66 wt.%, significantly higher than that
of xNi-PC@SBA-15 (ranging from 0.89 to 17.0 wt.%). The X-ray
diffraction (XRD) patterns of nano-sized Ni-MOF-74 and xNi-
MOF-74@SBA-15 are presented in Fig. S1a. In consistence with
the previous study,8 pristine Ni-MOF-74 exhibited two weak
and broad peaks at 2θ of 6.8 (110) and 11.9o (300), reflecting
its low crystallinity due to the small crystal size in the
nanometer range (i.e., < 10 nm). As for 17Ni-MOF-74@SBA-15,
diffraction peaks of nano-sized Ni-MOF-74 were indentified
along with that of amorphous SiO2 (the broad peak centered at
2θ of 22.4o), indicating that nano-sized Ni-MOF-74 was formed
in SBA-15. However, the diffraction peaks characteristic of
nano-sized Ni-MOF-74 were not observed in 1Ni-MOF-
74@SBA-15 and 4Ni-MOF-74@SBA-15, likely due to the low
loading amount of nano-sized Ni-MOF-74 and its dilution on
SBA-15 support.9 Similar observations were reported for other
confined MOF nanocrystals.9,10 Ni@PC presented very sharp
and narrow diffraction peaks at 44.4, 51.9 and 76.5o assigned
to metallic Ni,11 reflecting the formation of large and well
crystallized Ni particles on PC upon pyrolysis of nano-sized Ni-
MOF-74. In parallel, the diffraction peaks characteristic of
metallic Ni were clearly observed in 17Ni-PC@SBA-15.
However, peaks of metallic Ni were not identified in 1Ni-
PC@SBA-15 and 4Ni-PC@SBA-15 (see Fig. S1b), suggesting the
formation of small Ni particles with high dispersions.
Consistent results were provided by the X-ray photoelectron
spectra (XPS) of Ni 2p (Fig. S2 in ESI †). As shown in Fig. S2,
besides metallic Ni, NiO and Ni(OH)2 species can also be found
in Ni-based catalysts due to the oxidation of surface metallic Ni
when exposed to air. In Ni@PC, the majority of Ni species were
in the form of metallic Ni. 17Ni-PC@SBA-15 had a lower
content of metallic Ni as compared with Ni@PC. However, the
XPS peaks of metallic Ni were absence in 1Ni-PC@SBA-15 and
4Ni-PC@SBA-15, attributed to their very small Ni particles with
high surface to bulk ratios that were more prone to oxidation
upon exposure to air.
The infrared (IR) spectra of nano-sized Ni-MOF-74 and
xNi-MOF-74@SBA-15 are displayed in Fig. S3a. For pristine
nano-sized Ni-MOF-74, the IR bands characteristic of MOF-74
appeared at 1552, 1416 and 1193 cm-1, which were assigned
to the asymmetric and symmetric stretching vibrations of -
COO- from the carboxylic acid, and the vibrational band of C-O
respectively.10,12,13 As for xNi-MOF-74@SBA-15, besides very
strong bands at 1056 and 809 cm-1 from asymmetric and
symmetric stretching vibrations of Si-O in SBA-15,11,14 the IR
bands of Ni-MOF-74 were also clearly identified. Additionally,
the intensities of IR bands assigned to Ni-MOF-74 increased
with the loading of Ni-MOF-74, confirming the successful
growth of Ni-MOF-74 in SBA-15. The IR spectra of the xNi-
PC@SBA-15 catalysts were similar to that of SBA-15 (see Fig.
S3b, ESI†) and the bands characteristic of organic components
were not visible, suggesting complete decomposition and
carbonization of organic moisture from Ni-MOF-74 after
pyrolysis. Fig. S4 (ESI † ) shows thermogravimetric analysis
(TGA) profiles of Ni-MOF-74 and xNi-MOF-74@SBA-15. The
The diffuse reflectance ultraviolet-visible (DR-UV/Vis)
spectra of xNi-MOF-74@SBA-15 (presented in Fig. S5, ESI†)
were similar to that of pristine nano-sized Ni-MOF-74, which
were also typical for MOF-74.16,17 This further confirmed the
formation of Ni-MOF-74 in SBA-15. Additionally, all UV
absorbance bands of xNi-MOF-74@SBA-15 were slightly blue-
shifted in comparison with Ni-MOF-74, likely attributed to the
formation of smaller crystals of Ni-MOF-74 due to the
confinement effect of SBA-15.18 The N2 adsorption-desorption
isotherms and pore size distributions of SBA-15 and xNi-MOF-
74@SBA-15 are shown in Fig. S6 and the parameters are listed
in Table S2, ESI † . All isotherms displayed clear capillary
condensation with typical IV sorption behavior, attributed to
the mesopore structure of SBA-15. Due to the pore occupation
and lower surface area of nano-sized Ni-MOF-74 with low
crystallinity,8 xNi-MOF-74@SBA-15 possessed lower surface
area than pristine SBA-15. In parallel, the BET surface area and
pore volume of xNi-PC@SBA-15 were also lower as compared
with SBA-15 (Fig. S7 and Table S1), due to the formation of Ni-
PC particles in the mesopores of SBA-15.
Fig. S8 (ESI † ) shows the scanning electron microscopy
(SEM) images of xNi-MOF-74@SBA-15. It is seen that Ni-MOF-
74 was aggregated nanocrystals (Fig. S8a). 1Ni-MOF-74@SBA-
15 and 4Ni-MOF-74@SBA-15 exhibited the ropelike domains
of SBA-15 (Fig. S8b and c), suggesting that Ni-MOF-74 was
mainly dispersed inside the pores of SBA-15 in these two
materials. For 17Ni-MOF-74@SBA-15, a uniform Ni-MOF-74
layer was observed outside SBA-15 (Fig. S8d), indicative of the
growth of partial Ni-MOF-74 on SBA-15 external surface due to
excess Ni-MOF-74 loading. The SEM images and elemental
mapping of Ni@PC and xNi-PC@SBA-15 catalysts are displayed
in Fig. S9. For all Ni-based catalysts, the elemental distributions
were homogeneous.
The morphology of xNi-MOF-74@SBA-15 was further
characterized by the transmission electron microscopy (TEM)
images (presented in Fig. S10 in ESI†). Consistent with previous
observations,8 pristine nano-sized Ni-MOF-74 showed
a
‘continuous’ solid morphology. Ordered arrays of SBA-15
channels were clearly observed in the images of xNi-MOF-
74@SBA-15. In line with the SEM results, nano-sized Ni-MOF-
74 was found both in the pore and on the surface of 17Ni-
MOF-74@SBA-15. TEM images of Ni@PC and xNi-PC@SBA-15
catalysts are shown in Fig. 1. For Ni@PC catalyst, very large Ni
particles (with size in the range of 4-22 nm) could be clearly
identified due to severe metal aggregation, while small Ni
particles were evenly distributed in xNi-PC@SBA-15, attributed
to the effectively confinement effects from SBA-15. Notably, in
1Ni-PC@SBA-15, Ni particles (with size in the range of 0.4-6
nm) were smaller than the pore diameter of SBA-15 (8.09 nm),
reflecting that majority of Ni particles could be confined in the
mesopores of SBA-15. A small portion of Ni particles were
likely located on the external surface of SBA-15 in 4Ni-
PC@SBA-15 and 17Ni-PC@SBA-15, as suggested by their larger
particle sizes. The average Ni particle sizes of the catalysts
2 | J. Name., 2012, 00, 1-3
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30
25
20
15
10
5
30
25
20
15
10
5
catalytic merit. Fig. 2 shows the catalytic HDC of 1,2-
View Article Online
d = 11.88 nm
d = 2.45 nm
dichloroethane on the catalysts as a function of reaction time
DOI: 10.1039/D0CC00998A
on stream (TOS). The conversion of 1,2-dichloroethane
remained nearly constant on all catalysts during the test TOS,
indicative of the high catalytic stability of Ni-based catalysts.
Consistently, the morphologies and Ni particle sizes of the
tested catalysts were not significantly changed after use (see
TEM images in Fig. S13 in ESI †). However, 1,2-dichloroethane
conversions on Ni-based catalysts varied with their structural
0
0
0
5
10
15
20
25
0
5
10
15
20
25
Particle diameter (nm)
Particle diameter (nm)
(a) Ni@PC
(b) 1Ni-PC@SBA-15
30
25
20
15
10
5
30
25
20
15
10
5
d = 4.37 nm
d = 9.88 nm
properties. At 10
h of TOS, the conversions of 1,2-
0
0
0
dichloroethane on 1Ni-PC@SBA-15, 4Ni-PC@SBA-15 and 17Ni-
PC@SBA-15 were 40.3%, 55.9% and 65.5%, respectively. The
gradually increased 1,2-dichloroethane conversion was
ascribed to the increase of active Ni sites with Ni loadings. It
should be noted that the conversions of xNi-PC@SBA-15
catalysts were comparable to or even higher than that of
Ni@PC (43.2%), despite of their much lower Ni loading (4-80
times lower than that in Ni@PC). This suggested the
remarkable enhancement effects on xNi-PC@SBA-15 for
catalytic HDC of 1,2-dichloroethane. The higher catalytic
activities of xNi-PC@SBA-15 catalysts can be tentatively
explained in terms of the dispersion of Ni particles. TEM
results showed that owing to the confinement effects of SBA-
15, much higher Ni dispersion was obtained on xNi-PC@SBA-
15 catalysts than that of Ni@PC. Thus, xNi-PC@SBA-15 had
more active sites and hence higher catalytic activities. The
exceptional advantages of xNi-PC@SBA-15 catalysts were also
manifested in comparison with SBA-15 supported Ni catalyst
prepared by the conventional impregnation method (i.e.,
1Ni/SBA-15, Fig. S14). At 10 h of TOS, the conversion of 1,2-
dichloroethane on 1Ni/SBA-15 was 18.9%, less than half of the
conversion of 1Ni-PC@SBA-15.
To further evaluate the catalytic performances of the
catalysts, turnover frequency (TOF) values were calculated by
normalizing the 1,2-dichloroethane conversion by exposed Ni
sites. The TOF values of Ni@PC, 1Ni-PC@SBA-15, 4Ni-PC@SBA-
15 and 17Ni-PC@SBA-15 were 2.64, 42.04, 21.83, and 14.41 h-
1, respectively. This reflected a catalytic activity order of 1Ni-
PC@SBA-15 > 4Ni-PC@SBA-15 > 17Ni-PC@SBA-15 >> Ni@PC,
which was consistent with their Ni dispersion order. This trend
could be well interpreted in terms of the strong interaction
between Ni particles and supports, which is favorable for the
formation of spilled hydrogens. Previous studies showed that
the spilled hydrogens formed on the metal-support interface
0
5
10
15
20
25
5
10
15
20
25
Particle diameter (nm)
Particle diameter (nm)
(c) 4Ni-PC@SBA-15
(d) 17Ni-PC@SBA-15
30
d = 2.80 nm
25
20
15
10
5
0
0
5
10
15
20
25
Particle diameter (nm)
(e) 1Ni@SBA-15
Fig. 1. The TEM images and Ni particles size distribution of different
Ni-based catalysts.
were further quantified according to a surface area weighted
diameter:19
풅풔 =
풏풊풅ퟑ풊 / 풏풊풅ퟐ풊
∑ ∑
where ni is the number of counted Ni particles with diameter
of di and the total number of particles (ni) is larger than 120.
The average Ni particle sizes of Ni@PC, 1Ni-PC@SBA-15,
4Ni-PC@SBA-15 and 17Ni-PC@SBA-15 were calculated to be
11.88, 2.45, 4.37 and 9.88 nm, respectively. On the basis of Ni
particle sizes, the dispersion of active Ni sites can be further
determined using the equation:20 Dispersion (%) = 96.7/ds (nm).
The dispersions of Ni in 1Ni-PC@SBA-15, 4Ni-PC@SBA-15,
17Ni-PC@SBA-15 and Ni@PC were calculated to be 39.47%,
22.13%, 9.79% and 8.14%, respectively, reflecting a dispersion
order of 1Ni-PC@SBA-15 > 4Ni-PC@SBA-15 > 17Ni-PC@SBA-15
> Ni@PC.
To verify the role of carbon in xNi-PC@SBA-15,
temperature-programmed hydrogen desorption (H2-TPD)
profiles of 1Ni-PC@SBA-15 and 1Ni@SBA-15 are compared
and the results are presented in Fig. S11. Both 1Ni-PC@SBA-15
and 1Ni@SBA-15 displayed two desorption peaks. The
desorption peaks at 50-300 oC were assigned to hydrogens
weakly adsorbed on the surface of Ni particles, while the high
temperature peaks at 400-600 oC were attributed to spilled
hydrogens,21 migrating from Ni metal surface to the surface of
PC and SBA-15. Notably, the ratio of spilled hydrogens to
adsorbed hydrogens of 1Ni-PC@SBA-15 was 44.5, much larger
than that of 1Ni@SBA-15 (26.8). This suggested the
substantially enhanced H-spillover effect of 1Ni-PC@SBA-15.
The marked enhancement of H-spillover effect in 1Ni-PC@SBA-
15 was likely due to the formation of Ni-carbon composites, in
which the intimate contact between Ni particles and carbon
with large interfacial perimeter strongly facilitated H-spillover
from Ni particles into carbon surface.22
Fig. 2. (a) Conversion as a function of time on stream and (b)
The gas phase catalytic HDC of 1,2-dichloroethane was
used to evaluate the catalytic performances of the catalysts.
Besides trace methane and ethane, ethylene was the main
product from the catalytic HDC of 1,2-dichloroethane on Ni-
based catalysts. Ethylene selectivities of all catalysts were
above 90% (Fig. S12 in ESI † ), representing their remarkable
turnover
frequency
for
gas
phase
catalytic
hydrodechlorination of 1,2-dichloroethane over different Ni-
based catalysts.
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J. Name., 2013, 00, 1-3 | 3
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Śrębowata and S. Dzwigaj, Micropor. Mesopor. MaVti.e,w2A0rt1ic3le,O1n6lin9e,
120-127.
played an important role in the HDC reaction on Ni-based
catalysts.23,24 For both Ni@PC and xNi-PC@SBA-15 catalysts, Ni
particles were in intimate contact with the carbonaceous
residual. Furthermore, smaller Ni particle had larger Ni-carbon
interfacial area due to more effective Ni-carbon contact. Thus,
stronger H-spillover effect could be expected on catalysts with
smaller Ni particle size. Accordingly, owing to the higher Ni
dispersion, xNi-PC@SBA-15 catalysts exhibited significantly
higher TOF values than Ni@PC. The crucial role of H-spillover
effect could be further verified by comparing the catalytic
performances of 1Ni-PC@SBA-15 and 1Ni@SBA-15 without
carbon residual. 1Ni@SBA-15 had similar Ni loading amount
and particle size with that of 1Ni-PC@SBA-15 (see Fig. 1 and
Table S1), whereas its conversion of 1,2-dichloroethane (24.5%)
was much lower than that of 1Ni-PC@SBA-15 (40.3%).
Consistently, the TOF value of 1Ni@SBA-15 was 28.86 h-1,
lower than that of 1Ni-PC@SBA-15 (42.04 h-1). H2-TPD results
showed that more effective formation of spilled hydrogens
was evoked on 1Ni-PC@SBA-15 than on 1Ni@SBA-15, clearly
confirming the important role of H-spillover effect.
In summary, we successfully prepared a novel Ni-PC
composite confined in SBA-15 (Ni-PC@SBA-15) by the confined
pyrolysis of nano-sized Ni-MOF-74 that was in-situ grown in
the mesopores of SBA-15, and introduced it for the gas phase
catalytic HDC reaction. In comparison with Ni-PC composite
prepared by direct pyrolysis of Ni-MOF-74 (Ni@PC), very small
Ni particles with even size distribution are achieved on Ni-
PC@SBA-15 due to the confinement effect from ordered
mesopores of SBA-15. Additionally, the intimate contact
between Ni particles and carbon in fine Ni-PC composite
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PC@SBA-15 can be used as a highly active and selective
catalyst in gas phase catalytic HDC reaction. The study also
provides important knowledge to the fabrication of MOFs-
derived materials with high metal dispersion.
This work was supported by the Outstanding Youth
Foundation of Jiangsu Province of China (No. BK20190059) and
the National Natural Science Foundation of China (No. 21, 141-148.
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Conflicts of interest
There are no conflicts to declare.
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DOI: 10.1039/D0CC00998A
Table of contents
Ni-MOF-74
Ni-porous carbon (PC)
Ni(CH3COO)2
Impregnation
DHTP
In-situ grown
N2
Calcination
Ni(CH3COO)2@SBA-15
Ni-porous carbon (PC) @SBA-15
Ni-MOF-74@SBA-15
SBA-15
60
50
40
30
20
10
0
H
H
C
C
Cl
42
Cl
H
H
+H2
H
H
H
C
C
H
2.6
Ni-PC from direct
pyrolysis of Ni-MOF-74
Ni-PC @SBA-15
Novel Ni-porous carbon composite confined in SBA-15 was fabricated for highly effective and
selective gas phase catalytic hydrodechlorination of 1,2-dichloroethane.