10.1002/cctc.201801946
ChemCatChem
FULL PAPER
was changed to 0.75 mL or 3.0 mL, Pd-Ni(2:1)/NC or Pd-Ni(1:2)/NC was
also prepared, respectively.
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The preparation process of Pd-Fe/NC or Pd-Co/NC was the same as the
synthetic procedures of Pd-Ni/NC, just by replacing Ni2+ solution (2.0 mg
mL−1) with Fe2+ solution (2.0 mg mL−1) or Co2+ solution (2.0 mg mL−1).
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For comparison, Ni supported on NC (Ni/NC) was also prepared, just
with the addition of 1.5 mL Ni2+ solution. The preparation of Pd/NC was
without the addition of M2+ (Fe, Co or Ni) solution, only 1.5 mL Pd2+
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Catalyst test
0.5 mmol phenylacetylene, a certain amount of catalyst was dispersed in
10 mL ethanol under sonication in a round-bottomed flask. Then, a
balloon filled with H2 was connected to the flask, and the air in the flask
was quickly replaced by H2 three times. The reaction was maintained at
25 oC under vigorous stirring. The reaction mixture was collected using a
syringe at a certain time interval, and filtered through the membrane filter,
the filtrate was diluted by absolute ethanol, and the reaction results were
evaluated by an Agilent 5977E gas chromatography–mass spectrometry
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Characterization
The morphology and surface characteristics of the prepared samples
were characterized by TEM using an accelerating voltage of 200 kV
(Tecnai G2 F30) equipped with EDX (Tecnai G2, USA). A Rigaku D/max-
2400 diffractometer equipped with Cu-Kα radiation (λ= 1.5406 Å) was
used to measure the XRD patterns of the samples in the 2θ range of 10–
90o. XPS with X-ray source Al Kα (Perkin-Elmer PHI-5702) was used to
analyze the electronic states of the surface composition, and C 1s peak
was used as the energy reference (284.6 eV). The BET specific surface
areas, pore volume and pore-size distribution of the samples were
analyzed by N2 adsorption–desorption techniques at 77 K using a
TriStar3020 (Micromeritics). PerkinElmer EA2400 II instrument was used
to determine the C, N content of the samples (Elemental analysis results
for the supports were listed in Table S2). The metal contents of the
prepared catalysts were tested by ICP-AES. GC–MS (Agilent 5977E)
was applied to estimate the results of the reactions.
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Acknowledgements
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The authors acknowledge the financial support of the National
Natural Science Foundation of China (21872066 and 21802058),
and the Fundamental Research Funds for the Central
Universities (No. lzujbky-2017-kb11 and lzujbky-2017-107).
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Keywords: Palladium • Iron series elements • Nitrogen-doped
carbon • Simehydrogenation • Phenylacetylene
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