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MOFs derived three-dimensional hierarchical pore Co/NC composite material and preparation method thereof

A composite material and multi-level pore technology, which is applied in the field of porous materials, can solve the problems of step limitation and application, and achieve the effect of low cost, good practical application value, and improved catalytic reaction activity

Active Publication Date: 2021-03-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing literature reports are to use acid to remove metal components to obtain metal-free porous carbon materials, while metals with excellent catalytic activity need to be loaded on carbon supports through subsequent impregnation-reduction methods, which is limited by complicated steps. The application of such methods in the field of heterogeneous catalysis

Method used

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  • MOFs derived three-dimensional hierarchical pore Co/NC composite material and preparation method thereof
  • MOFs derived three-dimensional hierarchical pore Co/NC composite material and preparation method thereof
  • MOFs derived three-dimensional hierarchical pore Co/NC composite material and preparation method thereof

Examples

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Effect test

Embodiment 1

[0041] This embodiment provides a method for preparing a three-dimensional hierarchically porous Co / NC composite material derived from MOFs, including the following steps:

[0042] (1) 2-methylimidazole (5g) was added in methanol (50mL), dissolved by ultrasonication for 5min to obtain an organic ligand solution; Zn(NO 3 ) 2 ·6H 2 O(1.50g) and Co(NO 3 ) 2 ·6H 2 O (0.20g) was dissolved in methanol (50mL) to obtain a metal salt solution;

[0043] (2) Add the metal salt solution in step (1) to the organic ligand solution to obtain a mixed solution, stir at 25°C for 2 hours to obtain a ZnCo-ZIF suspension, and centrifuge the resulting ZnCo-ZIF suspension at 9500r / min After 8 minutes, the precipitate was taken, and then fully washed with methanol, and dried at 60°C for 12 hours to obtain the ZnCo-ZIF material;

[0044] (3) Weigh 200 mg of the ZnCo-ZIF material obtained in step (2) and disperse it into 5 mL of distilled water, ultrasonicate for 30 minutes to obtain a purple sus...

Embodiment 2

[0051] This embodiment provides a method for preparing a three-dimensional hierarchically porous Co / NC composite material derived from MOFs, including the following steps:

[0052] (1) 2-methylimidazole (5g) was added in methanol (50mL), dissolved by ultrasonication for 5min to obtain an organic ligand solution; Zn(NO 3 ) 2 ·6H 2 O(1.50g) and Co(NO 3 ) 2 ·6H 2 O (0.20g) was dissolved in methanol (50mL) to obtain a metal salt solution;

[0053] (2) Add the metal salt solution in step (1) to the organic ligand solution to obtain a mixed solution, stir at 25°C for 1 h to obtain a ZnCo-ZIF suspension, and centrifuge the resulting ZnCo-ZIF suspension at 9800r / min After 8 minutes, the precipitate was collected, washed thoroughly with methanol, and dried at 60°C for 12 hours to obtain the ZnCo-ZIF material.

[0054] (3) Weigh 200 mg of the ZnCo-ZIF material obtained in step (2) and disperse it into 5 mL of distilled water, ultrasonicate for 30 min to obtain a purple suspension,...

Embodiment 3

[0059] This embodiment provides a method for preparing a three-dimensional hierarchically porous Co / NC composite material derived from MOFs, including the following steps:

[0060] (1) 2-methylimidazole (5g) was added in methanol (50mL), dissolved by ultrasonication for 5min to obtain an organic ligand solution; Zn(NO 3 ) 2 ·6H 2 O(1.50g) and Co(NO 3 ) 2 ·6H 2 O (0.20g) was dissolved in methanol (50mL) to obtain a metal salt solution;

[0061] (2) Add the metal salt solution in step (1) to the organic ligand solution to obtain a mixed solution, stir at 25°C for 12 hours to obtain a ZnCo-ZIF suspension, and centrifuge the resulting ZnCo-ZIF suspension at 6500r / min After 8 minutes, the precipitate was collected, washed thoroughly with methanol, and dried at 60°C for 12 hours to obtain the ZnCo-ZIF material.

[0062] (3) Weigh 200 mg of the ZnCo-ZIF material obtained in step (2) and disperse it into 5 mL of distilled water, ultrasonicate for 30 min to obtain a purple suspen...

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Abstract

The invention discloses an MOFs derived three-dimensional hierarchical pore Co / NC composite material and a preparation method thereof. The method comprises the following steps of: adding an organic ligand solution into a metal salt solution, stirring, centrifuging and drying to obtain a ZnCo-ZIF material; adding the ZnCo-ZIF material into water, then adding a starch suspension, heating and stirring, and carrying out rotary evaporation to obtain a ZnCo-ZIF / ST material; and calcining the ZnCo-ZIF / ST material to obtain the three-dimensional hierarchical pore Co / NC material. Bimetal MOFs are usedas precursors, the three-dimensional hierarchical pore Co / NC material is prepared through a starch limited pyrolysis method, and compared with a traditional template method and an activation method, the method is easy and convenient to operate, safe and environmentally friendly; and meanwhile, due to the introduction of low-boiling-point Zn, the agglomeration of Co nanoparticles at high temperature is reduced, and the material shows excellent catalytic performance in the oxidative esterification reaction of 5-hydroxymethylfurfural and has a good application prospect.

Description

technical field [0001] The invention relates to the field of porous materials, in particular to a three-dimensional hierarchical porous Co / NC composite material derived from MOFs and a preparation method thereof. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOFs) are a new class of porous zeolite-like materials that have emerged in recent years. They are composed of central metal ions or metal clusters and organic ligands through coordination bonds. 3D porous materials. Compared with traditional porous materials, MOFs materials have high specific surface area, controllable pore size and tunable morphology. Porous metal-carbon composites with good thermal and chemical stability can be prepared by pyrolysis of MOFs materials, which has broad application prospects in the field of catalysis. [0003] One of the main problems currently facing is that the derivative carbon materials obtained by direct calcination of MOFs can control the morph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08B01J35/10C07D307/68
CPCB01J27/24B01J37/086B01J37/0018C07D307/68B01J35/23B01J35/61B01J35/651B01J35/647
Inventor 李映伟肖凌寒房瑞琪
Owner SOUTH CHINA UNIV OF TECH
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