Single-atom metal photocatalyst and its preparation method and application in carbon-oxygen cross-coupling reaction

A catalyst and metal light technology, applied in the research and development of single-atom metal photocatalysts, can solve the problems of poor cycle utilization, limited electron or energy transfer efficiency in the initiation step, and deactivation of metal deposition, so as to improve atomic efficiency and avoid Deposition of inactivation to achieve the effect of recycling

Active Publication Date: 2021-12-31
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, due to the limited electron or energy transfer efficiency in the initiation step, the light-driven coupling reaction rate needs to be further improved. In addition, the reaction usually requires a higher amount of metal complexes, and there are problems such as inactivation of metal deposition and poor recycling rate.

Method used

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  • Single-atom metal photocatalyst and its preparation method and application in carbon-oxygen cross-coupling reaction
  • Single-atom metal photocatalyst and its preparation method and application in carbon-oxygen cross-coupling reaction
  • Single-atom metal photocatalyst and its preparation method and application in carbon-oxygen cross-coupling reaction

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Experimental program
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Effect test

Embodiment 1

[0044] 10g of urea was heated to 500°C at a heating rate of 2°C / min, and kept at 500°C in air for 2 hours. The obtained yellow solid product was triturated and washed with water and ethanol. The sample was vacuum dried for 12 h to obtain C 3 N 4 . By adding 1mmol / L nickel chloride hexahydrate, C 3 N 4 (2g / L) was dispersed in a suspension of 50mL DMAc and reacted for 6 hours. It was then centrifuged, and the solid product was washed twice, then dried under vacuum for 12 h. get C 3 N 4 Loaded mononuclear nickel.

Embodiment 2

[0046] 10mg C 3 N 4 -Ni and 0.02 mmol of auxiliary ligand imidazole, 0.18 mmol of organic base, 0.1 mmol of p-bromoacetophenone and 6 mmol of methanol were added to (DMAc), and the total volume of the reaction solution was 5 mL. The reaction mixture was then purged with argon for at least 15 minutes under magnetic stirring to remove oxygen. Photoreactions were performed under the illumination of a xenon lamp equipped with a 400 nm stop filter. The reaction temperature was maintained at 25°C with circulating water cooling. After 8 hours of irradiation, the product p-methoxyacetophenone was obtained with a yield of 97%.

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Abstract

The invention belongs to the field of photocatalysis / metal-catalyzed organic synthesis, and provides a carbon-based single-atom metal catalytic material and its preparation method and application. The catalyst system constructed by the catalytic material realizes the light-driven carbon-oxygen synthesis of aromatic halogenated compounds and alcohols. Coupling reaction to synthesize ether compounds. The catalyst includes a graphite-type carbon nitride substrate, a metal center, and a sheet morphology with uniformly distributed metal atoms, and the metal is anchored on the substrate surface in the form of ions. The catalyst developed by the invention has the advantages of low reaction temperature, fast conversion rate, wide range of applicable substrates, and less side reactions, and has significant advantages compared with existing catalysts in terms of conversion number, metal utilization efficiency, preparation cost and recycling. .

Description

technical field [0001] The invention relates to the field of light / metal catalytic synthesis, in particular to the research and development of a single-atom metal photocatalyst for cross carbon-oxygen coupling synthesis of ether / phenol. Background technique [0002] Cross-coupling reactions such as carbon-carbon, carbon-oxygen, and carbon-nitrogen are important reactions in the preparation of pharmaceuticals and fine chemical products. Traditional catalysts are mainly metal palladium complexes with complex ligand structures; in addition, strong organic bases, such as potassium tert-butoxide, etc. are required or the temperature is raised to complete the reaction. An important breakthrough in catalytic systems for heterocoupling reactions in recent years is the combination of photocatalysis and metal catalysis to realize light-driven coupling reactions. The photocatalyst can choose molecular dyes or semiconductor materials, replace noble metal palladium with the first transi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/22B01J31/22C07C45/64C07C49/84
CPCB01J27/22B01J31/1815B01J35/004C07C45/64B01J2231/4288B01J2531/847C07C49/84
Inventor 赵进才刘天骄宋文静赵鑫孟涤籍宏伟马万红陈春城车延科盛桦章宇超
Owner INST OF CHEM CHINESE ACAD OF SCI
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