Monatomic copper catalyst as well as gram-level preparation method and application thereof to selective reduction of functional organic molecules

A copper catalyst and atomic technology, which is applied in the field of synthesis of non-noble metal single-atom materials, can solve the problems of low utilization rate of catalytic active sites, difficulty in multiple recycling, low hydrogenation selectivity, etc., and achieve simple operation, low raw material cost, The effect of high experimental repetition rate

Active Publication Date: 2020-11-24
XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to overcome the difficult problem of above-mentioned existing copper salt and copper nanomaterial catalytic technology, provide a kind of single-atom copper catalyst and its gram-level preparation method and the application of selective reduction function organic molecule, be used to solve the problem in the prior art Copper salts and copper nano-catalysts are difficult to recycle multiple times, the utilization rate of catalytic active sites is low, and they are easy to agglomerate, and they are also used to solve the technical problem of low selectivity for selective hydrogenation of functional organic molecules

Method used

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  • Monatomic copper catalyst as well as gram-level preparation method and application thereof to selective reduction of functional organic molecules
  • Monatomic copper catalyst as well as gram-level preparation method and application thereof to selective reduction of functional organic molecules
  • Monatomic copper catalyst as well as gram-level preparation method and application thereof to selective reduction of functional organic molecules

Examples

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Effect test

Embodiment 1

[0040] 1) Place 10g of melamine in a two-necked flask, add anhydrous methanol, ultrasonically disperse for 10min, add 3mL of glyoxal aqueous solution and ultrasonically disperse for 30min, place the two-necked flask on a magnetic heating stirrer, and connect the mouth of the two-necked flask The condenser tube, the other end of the condenser tube is plugged with a rubber stopper, and it is condensed and refluxed in an oil bath at 70°C for 2 hours to obtain process product A; process product A is centrifuged and dried to obtain product B; among which process product A is separated The centrifugation speed is 4000r / min, and the centrifugation time is 2 times, each centrifugation time is 7min; the centrifugal product A is dried at 60°C for 24h to remove the reaction solvent methanol; the volume ratio of the mass of melamine to anhydrous methanol is 1g:5mL; The concentration of the glyoxal aqueous solution is 8.8 mol / L; the molar ratio of glyoxal to melamine in the glyoxal aqueous s...

Embodiment 2

[0046] 1) Place 10g of melamine in a two-necked flask, add anhydrous methanol, ultrasonically disperse for 10min, add 3mL of glyoxal aqueous solution and ultrasonically disperse for 30min, place the two-necked flask on a magnetic heating stirrer, and connect the mouth of the two-necked flask The condenser tube, the other end of the condenser tube is plugged with a rubber stopper, and it is condensed and refluxed in an oil bath at 70°C for 2 hours to obtain process product A; process product A is centrifuged and dried to obtain product B; among which process product A is separated The centrifugal speed is 4000r / min, the centrifugation is 4 times, and the time of each centrifugation is 4min; the centrifugal product A is dried at 60°C for 24h to remove the reaction solvent methanol; the volume ratio of the mass of the melamine to the anhydrous methanol is 1g:5mL; The concentration of the glyoxal aqueous solution is 8.8 mol / L; the molar ratio of glyoxal to melamine in the glyoxal aq...

Embodiment 3

[0051] 1) Place 10g of melamine in a two-necked flask, add anhydrous methanol, ultrasonically disperse for 10min, add 3mL of glyoxal aqueous solution and ultrasonically disperse for 30min, place the two-necked flask on a magnetic heating stirrer, and connect the mouth of the two-necked flask The condenser tube, the other end of the condenser tube is plugged with a rubber stopper, and it is condensed and refluxed in an oil bath at 70°C for 2 hours to obtain process product A; process product A is centrifuged and dried to obtain product B; among which process product A is separated The centrifugal speed is 4000r / min, the centrifugation is 3 times, and the centrifugation time is 5min each time; the centrifugal product A is dried at 60°C for 24h to remove the reaction solvent methanol; the volume ratio of the mass of melamine to the anhydrous methanol is 1g:5mL; The concentration of the glyoxal aqueous solution is 8.8 mol / L; the molar ratio of glyoxal to melamine in the glyoxal aque...

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Abstract

The invention discloses a monatomic copper catalyst as well as a gram-level preparation method and application thereof to selective reduction of functional organic molecules. According to the method,glyoxal and melamine are subjected to condensation reaction to form a Schiff base functional group, so that the Schiff base functional group can be efficiently complexed with a copper source; furtherthe complexed copper source is sintered into a monatomic copper catalyst, so that monatomic copper is stably embedded into a framework of carbon nitride; according to the method, a common copper source and melamine are adopted as reaction raw material agents, so that the raw material of the synthesis reaction is low in cost and easy to obtain, an easily complexed Schiff base functional group is formed through the condensation reaction of glyoxal and melamine, the copper source is uniformly dispersed in a ligand skeleton, and the ligand is sintered to form a carbon nitride skeleton to stabilizethe copper source.

Description

【Technical Field】 [0001] The invention belongs to the technical field of synthesis of non-noble metal monoatomic materials, and specifically relates to a monoatomic copper catalyst, a gram-level preparation method thereof, and application of selective reduction of functional organic molecules. 【Background technique】 [0002] In recent years, the selective hydrogenation of functional organic molecules (multiple reducible functional groups, such as 4-nitrostyrene) has attracted the attention of extensive scientific research. In addition, the selective hydrogenation products of functional organic molecules have great application potential in medicines, dyes, and fine chemicals. The biggest problem in the selective hydrogenation of functional organic molecules lies in the development of highly selective and highly active catalysts. In the past ten years, noble metal-based catalysts such as gold, palladium and platinum have been reported successively, but noble metal-based catalysts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J27/24B01J37/08C07C209/36C07C211/45
CPCB01J23/72B01J27/24B01J35/0013B01J37/086C07C209/36C07C211/45Y02P20/584
Inventor 刘虎陈双莉孙小琴
Owner XI'AN UNIVERSITY OF ARCHITECTURE AND TECHNOLOGY
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