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Nitrogen-doped porous carbon supported metal M@CN composite catalytic material, preparation method and application

A nitrogen-doped porous carbon, catalytic material technology, applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of a large amount of waste, harsh reaction conditions, etc. Mild, high catalytic activity

Inactive Publication Date: 2019-06-21
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In general, high-pressure hydrogen is used as a reducing agent, or stoichiometric transition metals are used as a reducing agent (such as iron, tin, zinc, and metal sulfides), and the reaction conditions are relatively harsh, or a large amount of waste will be generated

Method used

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  • Nitrogen-doped porous carbon supported metal M@CN composite catalytic material, preparation method and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Co(NO 3 ) 2 ·6H 2 O, H 2 Dissolve BDC and BPY in a mixed solution of 10mL methanol and 20mL DMF, and fully dissolve to obtain a clear solution. The concentrations of the above three substances in the solution are 0.04mol / L, 0.05mol / L, and 0.02mol / L, respectively;

[0030] Seal the above solution in a hydrothermal reaction kettle and put it in an oven at 130°C for 72 hours; after the reaction, the hydrothermal reaction kettle was slowly lowered to room temperature in the oven, opened and filtered to obtain the product Co 2 (BDC) 2 (BPY). Wash several times with DMF to remove unreacted substances attached to the surface.

[0031] In an inert atmosphere, the above product was heated to 600 °C at a rate of 4 °C / min in a tube furnace, kept at a constant temperature for 4 hours, and then lowered to room temperature to prepare Co@CN composite catalytic material A.

Embodiment 2

[0033] Cu(NO 3 ) 2 ·3H 2 O, H 2 Dissolve BDC and BPY in a mixed solution of 20mL methanol and 10mL DMF, and fully dissolve to obtain a clear solution. The concentrations of the above three substances in the solution are 0.05mol / L, 0.05mol / L, and 0.03mol / L, respectively;

[0034] Seal the above solution in a hydrothermal reaction kettle and put it in an oven at 140°C to react for 48 hours; after the reaction, the hydrothermal reaction kettle was slowly lowered to room temperature in the oven, opened and filtered to obtain the product Cu 2 (BDC) 2 (BPY). Wash several times with DMF to remove unreacted substances attached to the surface.

[0035] In an inert atmosphere, the above product was heated to 700 °C at 2 °C / min in a tube furnace, kept at a constant temperature for 3 hours, and then lowered to room temperature to prepare Cu@CN composite catalytic material B.

Embodiment 3

[0037] Ni(NO 3 ) 2 ·6H 2 O, H 2 Dissolve BDC and BPY in a mixed solution of 15mL methanol and 15mL DMF, and fully dissolve to obtain a clear solution. The concentrations of the above three substances in the solution are 0.10mol / L, 0.10mol / L, and 0.05mol / L, respectively;

[0038] Seal the above solution in a hydrothermal reaction kettle and put it in a 120°C oven for 24 hours of reaction; after the reaction, the hydrothermal reaction kettle was slowly lowered to room temperature in the oven, opened and filtered to obtain the product Ni 2 (BDC) 2 (BPY). Wash several times with DMF to remove unreacted substances attached to the surface.

[0039] In an inert atmosphere, the above product was heated to 400 °C at a rate of 3 °C / min in a tube furnace, kept at a constant temperature for 2 hours, and then lowered to room temperature to prepare Ni@CN composite catalytic material C.

[0040] The above nitrogen-doped porous carbon-supported metal-supported M@CN composite catalytic m...

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Abstract

The invention discloses a nitrogen-doped porous carbon supported metal M@CN composite catalytic material, a preparation method and application, and belongs to the field of new materials. The compositecatalytic material is obtained by carbonizing a double-ligand MOF material M2 (BDC) 2 (BPY) synthesized by a nitrogen-containing organic ligand at a high temperature, wherein BDC is terephthalic acid, BPY is 4, 4'-bipyridine, and metal is one or more of copper, cobalt and nickel. The MOF material M2 (BDC) 2 (BPY) of the nitrogen-containing organic ligand is carbonized at a high temperature of 400-800 DEG C for 2-8 hours to obtain the composite catalytic material M@CN. The catalytic material is used for reduction reaction of p-nitrobenzene, and has the advantages of small catalyst use amount,mild reaction conditions and high catalytic activity.

Description

technical field [0001] The invention belongs to the field of new materials, and relates to a novel metal catalyst, namely a composite catalytic material of nitrogen-doped porous carbon-supported metal, which consists of a double-ligand MOF material M synthesized by nitrogen-containing organic ligands. 2 (BDC) 2 (BPY) (BDC = terephthalic acid, BPY = 4,4'-bipyridine) is obtained by carbonization at high temperature. The invention also relates to the application of the composite catalytic material. Background technique [0002] The selective reduction of nitrobenzene is a very important reaction in organic synthesis, because the products of this reaction are aniline, azobenzene and azobenzene oxide, which are used in the synthesis of medicines, dyes, functional polymers, agricultural chemicals and fine chemicals. Main raw materials and key intermediates. Generally, high-pressure hydrogen is used as a reducing agent, or stoichiometric transition metals are used as a reducing ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C07C209/36C07C211/46C07C245/08
Inventor 田福平乔晨霞贾文兰李心怡候潇涵易凯王樱锦
Owner DALIAN UNIV OF TECH
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