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A nitrogen-cobalt co-doped porous carbon-supported sulfur-zinc-cobalt catalytic material and its preparation method and application

A catalytic material and co-doping technology, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of expensive precursors, complicated preparation processes, and difficulty in scaling up production, and achieve improved hydrogenation. High efficiency, improved catalytic activity, good versatility

Inactive Publication Date: 2021-04-20
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Unfortunately, the precursors are expensive and the preparation process is complicated, which makes it difficult to scale up both for production and practical application

Method used

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  • A nitrogen-cobalt co-doped porous carbon-supported sulfur-zinc-cobalt catalytic material and its preparation method and application
  • A nitrogen-cobalt co-doped porous carbon-supported sulfur-zinc-cobalt catalytic material and its preparation method and application
  • A nitrogen-cobalt co-doped porous carbon-supported sulfur-zinc-cobalt catalytic material and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation of Co@NPC: 10g bovine serum albumin was dissolved in 20mL double distilled water, and then 1.75g ​​CoCl 2 ·6H 2 O was mixed in the above solution and stirred magnetically for 1 h. The resulting protein complex was lyophilized for 24 hours to yield a solid. The lyophilized solid was then ground into a powder and then heated at 5°C min -1 The heating rate of the powder is pyrolyzed to 800°C, and at 800°C flowing nitrogen (40mL min -1 ) atmosphere for 2h, then naturally cooled to room temperature. Automatically grind the obtained solid into carbon powder with agate mortar, then add it into 1M HCl aqueous solution, stir vigorously at 80°C for 8 hours, filter the obtained black dispersion on an organic microporous membrane, rinse with deionized water until the pH is neutral, Then use absolute ethanol. The filtered solid was dried overnight in a vacuum oven at 40°C.

Embodiment 2

[0044] CoN x -Co x Preparation of ZnS@NPC-0.5: 10g of bovine serum albumin was dissolved in 20mL of double distilled water, and then 1.75g ​​of CoCl 2 ·6H 2 O was mixed in the above solution and stirred magnetically for 1 h. Then dissolve a certain mass ratio of zinc chloride in water. The above two solutions were mixed and stored under magnetic stirring at room temperature for 1 h. The resulting pink protein complex was lyophilized for 24 hours to give a light blue solid. The mass ratio of zinc salt to bovine serum albumin is 0.5 / 1. The lyophilized solid was then ground into a powder and then heated at 5°C min -1 The heating rate of the powder is pyrolyzed to 800°C, and at 800°C flowing nitrogen (40mL min -1 ) atmosphere for 2h, then naturally cooled to room temperature. Automatically grind the obtained solid into carbon powder with agate mortar, then add it into 1M HCl aqueous solution, stir vigorously at 80°C for 8 hours, filter the obtained black dispersion on an o...

Embodiment 3

[0046] CoN x -Co x Preparation of ZnS@NPC-1: 10g of bovine serum albumin was dissolved in 20mL of twice distilled water, and then 1.75g ​​of CoCl 2 ·6H 2 O was mixed in the above solution and stirred magnetically for 1 h. Then dissolve a certain mass ratio of zinc chloride in water. The above two solutions were mixed and stored under magnetic stirring at room temperature for 1 h. The resulting pink protein complex was lyophilized for 24 hours to give a light blue solid. The mass ratio of zinc salt to bovine serum albumin is 1 / 1. The lyophilized solid was then ground into a powder and then heated at 5°C min -1 The heating rate of the powder is pyrolyzed to 800°C, and at 800°C flowing nitrogen (40mL min -1 ) atmosphere for 2h, then naturally cooled to room temperature. Automatically grind the obtained solid into carbon powder with agate mortar, then add it into 1M HCl aqueous solution, stir vigorously at 80°C for 8 hours, filter the obtained black dispersion on an organi...

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Abstract

The invention discloses a nitrogen-cobalt co-doped porous carbon loaded Co x ZnS catalytic material and its preparation method and application. Nitrogen-cobalt co-doped porous carbon supported Co x The ZnS catalytic material consists of protein-metal ions (Zn 2+ / Co 2+ ) complexes were obtained after pyrolysis and acid washing. Nitrogen-cobalt co-doped porous carbon supported Co x ZnS catalytic materials have highly efficient active centers (CoN x and Co x ZnS) and unique porous structure, high efficiency and good selectivity in the catalytic hydrogenation reaction of nitro compounds, under mild conditions (90 ° C, 5 bar H 2 ), especially at normal temperature and pressure (25°C, 1bar H 2 ) can realize catalytic nitro hydrogenation, so that nitro compounds can be efficiently and selectively catalyzed into the corresponding amine compounds, and the catalytic material is sensitive to CO and H 2 S intoxication showed remarkable tolerance. In addition, the catalytic material has a simple synthesis method and has broad application prospects in the technical field of catalytic hydrogenation.

Description

technical field [0001] The invention relates to a catalytic material, in particular to a nitrogen-cobalt co-doped porous carbon loaded Co x ZnS catalytic material (CoN x -Co x ZnS@NPCs), also involves the utilization of protein-zinc / cobalt ions (Zn 2+ / Co 2+ ) network precursor to construct nitrogen-cobalt co-doped porous carbon-supported Co x Methods of ZnS catalytic materials, and methods involving nitrogen-cobalt co-doped porous carbon-supported Co x The application of ZnS catalytic material to selective hydrogenation of nitro compounds under mild conditions belongs to the technical field of heterogeneous catalytic materials. Background technique [0002] Amines and their derivatives are important bulk chemicals and industrial intermediates used in the production of pharmaceuticals, pigments, agrochemicals, dyes and fine chemicals. The reduction of nitro compounds provides an extremely important route to the production of amines, and catalytic hydrogenation reaction...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/02B01J35/10C07C209/36C07C211/46
CPCB01J27/24B01J35/0073B01J35/026B01J35/1004B01J35/1061C07C209/36C07C211/46
Inventor 刘又年安平张广吉王立强唐飞鹰
Owner CENT SOUTH UNIV