Iron-nitrogen co-doped mesoporous carbon and preparation method and application thereof

A technology of co-doping and mesoporous carbon, applied in chemical instruments and methods, catalyst activation/preparation, organic chemistry, etc., can solve the problems of limited promotion and application of preparation technology, troublesome catalyst preparation process, poor selectivity of reaction, etc. Achieve the effects of increased yield, simple preparation method, and easy reaction

Active Publication Date: 2017-07-04
永嘉跃龙密封件有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above preparation methods can effectively prepare azobenzene, but there are also many problems. The catalyst used is expensive (Au), or the catalyst preparation process is very troublesome, or the reaction needs to be carried out under high pressure conditions, or the selection of the reaction Poor performance, etc., which limit the promotion and application of existing preparation technology in industry

Method used

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  • Iron-nitrogen co-doped mesoporous carbon and preparation method and application thereof
  • Iron-nitrogen co-doped mesoporous carbon and preparation method and application thereof
  • Iron-nitrogen co-doped mesoporous carbon and preparation method and application thereof

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Effect test

Embodiment 1

[0036] The preparation method of the iron-nitrogen co-doped mesoporous carbon is specifically: 0.02mol of citric acid monohydrate (4.3339g) and 0.01mol of magnesium nitrate hexahydrate (2.59g) are added to 10mL of deionized water, stirred and dissolved, Then put the solution into an oven at 120° C. for 24 hours until a foamy solid, namely the precursor, is obtained. Mix 4g of precursor, 4g of melamine and 4g of potassium ferrocyanide, and then burn the mixture in an atmosphere furnace at 800°C for 1 hour under the protection of nitrogen, and then cool to room temperature to obtain nitrogen and metal iron Co-doped mesoporous carbon.

Embodiment 2

[0038]The preparation method of the nitrogen-doped mesoporous carbon is specifically: 0.02mol of citric acid monohydrate (4.3339g) and 0.01mol of magnesium nitrate hexahydrate (2.59g) are added to 10mL of deionized water, stirred and dissolved, and then The solution was put into an oven at 120° C. for 24 hours until a foamy solid, namely the precursor, was obtained. 4g of the precursor and 4g of melamine were mixed together, and then the mixture was burned in an atmosphere furnace at 800° C. for 1 hour under the protection of nitrogen, and then cooled to room temperature to obtain nitrogen-doped mesoporous carbon.

Embodiment 3

[0040] The preparation method of the nitrogen-doped mesoporous carbon is specifically: 0.02mol of citric acid monohydrate (4.3339g) and 0.01mol of magnesium nitrate hexahydrate (2.59g) are added to 10mL of deionized water, stirred and dissolved, and then The solution was put into an oven at 120° C. for 24 hours until a foamy solid, namely the precursor, was obtained. Under the protection of nitrogen, 4 g of the precursor was burned in an atmosphere furnace at 800° C. for 1 hour, and then cooled to room temperature to obtain mesoporous carbon.

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Abstract

The invention discloses iron-nitrogen co-doped mesoporous carbon and a preparation method and application thereof. The preparation method comprises taking citric acid monohydrate and magnesium nitrate hexahydrate, adding the citric acid monohydrate and magnesium nitrate hexahydrate into deionized water, stirring the solution for dissolution, then placing the solution in an oven, carrying out baking for a period of time to obtain foamy solids as precursors, mixing the precursors, a nitrogen source and an iron salt, firing the mixture in an atmosphere furnace in a nitrogen protective atmosphere, and cooling the product to the room temperature to obtain the iron-nitrogen co-doped mesoporous carbon NMC-Fe. The NMC-Fe has a flower-like structure, petals of the flower-like structure are multi-layer carbon sheets and the iron compound is distributed in the carbon sheets. The iron-nitrogen co-doped mesoporous carbon has high stability and can be used for preparation of aromatic azo compounds. The chemical selectivity of the catalytic reaction is very good so that the yield of the product azobenzene is 94%. Compared with the existing common preparation method, the preparation method provided by the invention has a higher yield.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and relates to a metal catalyst and a preparation method thereof, in particular to an iron-nitrogen co-doped graphene, and a method for preparing arylazo compounds by using the catalyst. Background technique [0002] Aryl azo compounds are important industrial raw materials with a wide range of uses, such as dyes, food additives, display agents and free radical initiators. [0003] At present, azobenzene can be synthesized by various methods, and the most classic method is the coupling reaction of diazonium salt and aromatic compound substituted with electron-donating groups, or the preparation of azobenzene by Mills reaction and Wallach reaction. In addition, there are many documents on the preparation of azobenzene through the reductive coupling reaction of nitrobenzene, which is easy to get and cheap in price. This method usually needs to use a large amount of transition metals, and a large a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C245/08C07C291/08
CPCB01J27/24B01J35/026B01J35/1019B01J35/1061B01J37/082C07C245/08C07C291/08
Inventor 余小春林大杰王舜金辉乐尹德武刘爱丽史重阳白金宝
Owner 永嘉跃龙密封件有限公司
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