10.1002/asia.202100740
Chemistry - An Asian Journal
FULL PAPER
General procedure for the synthesis of Pd@ZIF-8-n (n = 1~3)
catalyst
Acknowledgements
This work was supported by Natural Science Foundation of China
(21703129), Scientific Research Start-up Funds of Shanxi
University (023151801002), Natural Science Foundation for
Young Scientists of Shanxi Province (2015021051) and Scientific
and Technological Innovation Programs of Higher Education
Institutions in Shanxi (2019L0108). And we are also very grateful
for the test platform provided by Shanxi University of Scientific
Instrument Center.
With different amount of Pd(OAc)2 (5.6 mg (0.025 mmol), 11.2 mg (0.05
mmol) and 23 mg (0.1 mmol)) were added to 30 mL of methanol separately
followed by ultrasonicated for 2 min. The resultant solutions were stirred
at 25 oC for 60 min and then 1.314 g (16 mmol) of 2-methyl imidazole was
added into the above mixture, keeping stirred for another 10 min.
Subsequently, three portions of 1.19 g (4 mmol) of Zn(NO3)2·6H2O
dissolved in 15 mL of methanol were added dropwise and the resultant
solutions were stirred for 3 h and left them stand for another 20 h. The gray
products were collected by centrifugation, washed three times with DMF
and methanol separately, and vacuum-dried overnight at 50 oC. The
obtained products were denoted as Pd@ZIF-8-1, Pd@ZIF-8-2, Pd@ZIF-
8-3, respectively.
Conflict of Interest
Catalytic hydrogenation of 1-octene/cyclooctene using as-
prepared catalysts
The authors declare no competing financial interest.
Hydrogenation of olefins (1-octene or cis-cyclooctene) was carried out in
ethanol solution in a 1 atm of H2 balloon at room temperature. Typically,
20 mg of catalyst, 1 mmol of 1-octene (or cis-cyclooctene) and 5 mL of
ethanol were loaded in a 20 mL reaction tube. Subsequently, residual air
in the reactor was expelled by flushing three times with hydrogen to keep
the reactor at 1 atm of hydrogen filled in a balloon. The reaction mixture
was stirred at 25 oC for given time separately (1~6 h). Samples were taken
away from the reactor, centrifuged and the filtrate was analyzed by gas
chromatograph.
Keywords: One-pot method
• solvent reduction • in-situ
encapsulation • Pd@ZIF-8 nanocomposites • size-selective
hydrogenation
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General procedure for the catalyst recycling
40 mg of Pd@ZIF-8-60 min, 2 mmol of 1-octene and 10 mL of ethanol
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reactor was expelled by flushing three times with hydrogen to keep the
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Characterization
Transmission electron microscope (TEM) was carried out on a FEI Tecnai
G2 F20S-Twin using an accelerating voltage of 200 kV. XRD
measurements were conducted on a Rigaku Ultima IV diffractometer using
Cu-Kα radiation as the X-ray source in the 2θ range of 5-90o. FT-IR spectra
was collected by a Nicolet IS5 IR spectrometer with KBr pellet. The N2
adsorption-desorption isotherms were obtained on a Quantachrome
autosorb iQ2 analyzer. Before measurement, the samples were degassed
under vacuum at 423 K for 8 h. The Pd loading amount of Pd@ZIF-8-60
min catalyst was determined by NexION 350 inductively coupled plasma
mass spectrometry (ICP-MS). The X-ray photoelectron spectra (XPS) was
analyzed on the PHI-5702 instrument and the C1s line at 284.5 eV was
used as the binding energy reference. Gas chromatograph (FULI 9790Ⅱ)
was equipped with a HP-5 column and FID detector to monitor olefins
hydrogenation progress.
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