A kind of silver ruthenium double metal doped graphene catalyst and its preparation method and application

A graphene and catalyst technology, applied in the field of silver ruthenium bimetal doped graphene catalyst and its preparation, can solve the problems of difficult control of the reaction process, cumbersome synthesis process, high production cost, etc., achieve good application prospects, and reduce side reaction products , the effect of short reaction time

A graphene and catalyst technology, applied in the field of silver ruthenium bimetal doped graphene catalyst and its preparation, can solve the problems of difficult control of the reaction process, cumbersome synthesis process, high production cost, etc., achieve good application prospects, and reduce side reaction products , the effect of short reaction time

CN112452324BActive Publication Date: 2022-03-11JIANGNAN UNIV
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  • A kind of silver ruthenium double metal doped graphene catalyst and its preparation method and application
  • A kind of silver ruthenium double metal doped graphene catalyst and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0023] Preparation of graphene-supported silver-ruthenium bimetallic catalysts:

[0024] First treat 6.0g of graphite with 5mL of 37% hydrochloric acid, add 1.5g of iodobenzene diacetate to oxidize, then use ultrasonic vibration until the graphene oxide aqueous solution is clear and free of particles, add 1g of dinitrophenylhydrazine and reflux at 50°C for 30h. Filter and dry to obtain graphene, and 1.0g of AgBF 4 with 1.1 g of RuCl 3 Dissolve in 10mL of ethylene glycol, stir in an ice bath, remove the ice bath after all the solids are dissolved; add 5g of graphene, adjust the pH of the mixture to 7, place it under hydrothermal conditions at 80°C, and react for 2 hours; After the reaction, cool, centrifuge, wash, and vacuum dry to obtain the product; roast the product in a high-temperature muffle furnace, first raise the temperature to 500°C, keep the temperature stable for 4 hours, and finally store it in a vacuum desiccator to obtain the silver ruthenium bismuth Metal-dope...

Embodiment 2

[0028] Preparation of graphene-supported silver-ruthenium bimetallic catalysts:

[0029] First treat 9.0g of graphite with 12mL of 37% hydrochloric acid, add 1.5g of iodobenzene diacetate to oxidize, then use ultrasonic vibration until the graphene oxide aqueous solution is clear and free of particles, add 3g of dinitrophenylhydrazine and reflux at 100°C for 10h. Filter and dry to get graphene, and 2.0g of AgBF 4 with 2.2 g of RuCl 3 Dissolve in 14mL of ethylene glycol, stir in an ice bath, remove the ice bath after all the solids are dissolved; add 8g of graphene, adjust the pH of the mixture to 7, place it under hydrothermal conditions at 80°C, and react for 2 hours; After the reaction, cool, centrifuge, wash, and vacuum dry to obtain the product; roast the product in a high-temperature muffle furnace, first raise the temperature to 400°C, keep the temperature stable for 6 hours, and finally store it in a vacuum desiccator to obtain the silver ruthenium bismuth Metal-doped...

Embodiment 3

[0033] Preparation of graphene-supported silver-ruthenium bimetallic catalysts:

[0034] First treat 12.0g of graphite with 15mL of 37% hydrochloric acid, add 1.8g of iodobenzene diacetate for oxidation, then use ultrasonic vibration until the graphene oxide aqueous solution is clear and free of particles, add 5g of dinitrophenylhydrazine and reflux at 50°C for 20h, Filtration, drying to obtain graphene, 3.0g of AgBF 4 with 3.3 g of RuCl 3 Dissolve in 20mL of ethylene glycol, stir in an ice bath, remove the ice bath after all the solids are dissolved; add 10g of graphene, adjust the pH of the mixture to 11, place it under hydrothermal conditions at 80°C, and react for 2 hours; After the reaction, cool, centrifuge, wash, and vacuum dry to obtain the product; roast the product in a high-temperature muffle furnace, first raise the temperature to 300°C, keep the temperature stable for 10 hours, and finally store it in a vacuum desiccator to obtain the silver ruthenium bismuth Me...

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Abstract

The invention discloses a silver-ruthenium bimetal doped graphene catalyst and its preparation method and application. The catalyst includes a graphene carrier, and the graphene carrier is loaded with silver and ruthenium nanoparticles, and the mass ratio of silver and ruthenium nanoparticles is 0.5 ~1: 0.6~1.1, the diameter of silver and ruthenium nanoparticles is 100~800nm. The preparation method of this catalyst comprises the following steps: (1) prepare graphene; (2) make AgBF 4 with RuCl 3 Dissolving in ethylene glycol, adding graphene, and reacting under hydrothermal conditions; (3) cooling, centrifuging, washing, and vacuum drying to obtain the product; (4) roasting. The catalyst is used as a catalyst in the synthesis process of bisphenol F or 1-phenyl-3-p-nitrophenyl-acetone. When the catalyst is used in the synthesis of bisphenol F, it has excellent catalytic performance, significantly improves the yield of bisphenol F, and the side reaction products are effectively reduced; when used in the synthesis of 1-phenyl-3-p-nitrophenyl-acetone It has excellent catalytic performance, the product chemical selectivity is 100%, the yield is greater than 90%, and it can be recycled and reused.

Description

technical field [0001] The present invention relates to a catalyst and its preparation method and application, more specifically, to a silver-ruthenium bimetallic doped graphene catalyst and its preparation method and application. Background technique [0002] Bisphenol F is produced by in-situ condensation of phenol and acetone, and is a very important organic chemical intermediate. Bisphenol F products are mainly composed of 3 isomers of dihydroxydiphenylmethane, its unique chemical structure characteristics, the synthetic polyester resin, polycarbon resin, epoxy resin, and as a phenolic resin modifier and Flame retardants, their heat resistance, moisture resistance, processability and injection molding performance all exceed similar products made of bisphenol A as raw materials. The excellent properties of bisphenol F derivatives make it widely used in the synthesis of electronic-grade epoxy resins, high-solid coatings, special low-viscosity resins for injection molding ...

Claims

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Application Information

Patent Timeline
11 Mar 2022
Publication
CN112452324B
IPC
B01J23/50; B01J35/02; B01J37/10; B01J37/16; B01J37/06; B01J37/12; C07C37/20; C07C39/16; C07C201/12; C07C205/45; B01J35/00
CPC
B01J23/50; B01J37/10; B01J37/16; B01J37/06; C07C37/20; C07C201/12; B01J35/23; B01J35/40
Inventors
王大伟; 胡文康