Precious metal Carbene polymer catalysts and its preparation method and use
A catalyst and precious metal technology, applied in the field of nano-catalysis, can solve the problems of uneven distribution of metal sites, low metal loading, complicated preparation methods, etc., and achieve the effects of high industrial application value, high catalytic activity, and reduced industrial costs.
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Embodiment 1
[0013] Embodiment 1 (preparation and application of catalyst PNC-1)
[0014] Dissolve 100 mg of palladium acetate in a mixed solution of 10 mL of DMF and acetonitrile (volume ratio 1:2), and then add it to a mixed solution of 70 mL of DMF and acetonitrile containing imidazolium salt TIS, and then react the reaction system at 110 ° C for 1 h, then React at 145°C for 23h. After the reaction, cool to room temperature, centrifuge to separate the obtained yellow solid, wash with acetonitrile and dichloromethane several times, and dry under vacuum to obtain pure spherical catalyst PNC-1.
[0015] The content of Pd in the catalyst PNC-1 is 12.0%, and the thermal stability is at least above 250°C.
[0016] Catalyst PNC-1 is used in the hydrosilylation reaction of benzaldehyde and trimethylsilyl cyanane, the catalyst dosage is 0.2%, the reaction temperature is room temperature, the reaction time is 1 h, the conversion rate is 92%, and there is no by-product. It can be recycled 6 tim...
Embodiment 2
[0017] Embodiment 2 (preparation and application of catalyst PNC-2)
[0018] Dissolve 100 mg of palladium acetate in a mixed solution of 10 mL of DMSO and acetonitrile (volume ratio 1:1), and then add it to a mixed solution of 70 mL of DMSO and acetonitrile containing imidazolium salt TIS, then react the reaction system at 110 ° C for 1 h, and then React at 145°C for 23h. After the reaction is completed, cool to room temperature, no solid is washed out, then add 220mL of a mixed solution of dichloromethane and diethyl ether (volume ratio 1:3) while stirring, and soon a yellow solid precipitates. A yellow solid was obtained by centrifugation, washed several times with acetonitrile and dichloromethane, and dried under vacuum to obtain pure cube-shaped catalyst PNC-2.
[0019] The content of Pd in the catalyst PNC-1 is 12.5%, and the thermal stability is at least above 250°C. Catalyst PNC-2 is used in the hydrosilylation reaction of benzaldehyde and trimethylsilylcyanane, the ...
Embodiment 3
[0020] Embodiment 3 (preparation and application of catalyst PNC-3)
[0021] Dissolve 100mg of palladium acetate in 10mL of DMSO solution, then add it into 70mL of DMSO solution containing imidazolium salt TIS, then react the reaction system at 110°C for 1h, and then react at 145°C for 23h. After the reaction is completed, cool to room temperature, No solid was washed out, and then 220 mL of a mixed solution of dichloromethane and diethyl ether (volume ratio 1:3) was added under stirring, and soon a yellow solid was precipitated, which was centrifuged to obtain a yellow solid, which was then washed with acetonitrile and dichloromethane. After that, it was dried under vacuum to obtain pure product honeycomb catalyst PNC-3.
[0022] The content of Pd in the catalyst PNC-1 is 12.8%, and the thermal stability is at least above 250°C. Catalyst PNC-2 is used in the hydrosilylation reaction of benzaldehyde and trimethylsilyl cyanane, the catalyst dosage is 0.2%, the reaction tempe...
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