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Preparation method and application of N-doped mesoporous-carbon-loaded metal nano-catalyst

A technology of metal nano and mesoporous carbon, which is applied in the direction of catalytic reaction, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of destroying the structure and composition of active components, increasing the movement tendency of active components, and affecting the service life of catalysts and recycling issues

Active Publication Date: 2019-03-19
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, mesoporous carbon as a catalyst support has a weak interaction with the active components, which increases the movement tendency of the active components during the catalytic process, causing the active components to agglomerate or transfer to the reaction system and lose, destroying the active components. structure and composition, the catalyst exhibits lower stability, thereby affecting the service life and recycling of the catalyst
In addition, the mesoporous carbon support has a simple composition and weak ability to regulate the activity of the catalyst.

Method used

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  • Preparation method and application of N-doped mesoporous-carbon-loaded metal nano-catalyst
  • Preparation method and application of N-doped mesoporous-carbon-loaded metal nano-catalyst
  • Preparation method and application of N-doped mesoporous-carbon-loaded metal nano-catalyst

Examples

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Comparison scheme
Effect test

Embodiment 1

[0038] Example 1: Preparation of Pd@N-MPC and its catalytic bipyridine synthesis

[0039]Get 67.9g of THPP, 5gNaOH and 0.1g of surfactant F127, add it into 100ml of alcohol-water mixed solvent with a volume ratio of 1:1, stir until completely dissolved; add 50ml of formaldehyde solution (37wt%) to the above solution After stirring and mixing evenly, the reaction was continued for 2 hours under heating conditions, and polymer precipitation appeared in the reaction mixture. The above mixture was transferred and sealed into a hydrothermal reactor and placed in a dry oven at 90° C. for 4 h. After the reaction, take out the reactant and adjust the pH of the solution to 6-7 with hydrochloric acid, filter the precipitate and wash it several times with ethanol and distilled water, obtain the covalent organic framework polymer in a 60°C drying oven, and dry it in a vacuum drying oven. The covalent organic framework polymer was pulverized and sieved to obtain a solid with a particle si...

Embodiment 2

[0041] Example 2: Preparation of Pd@N-MPC and its catalytic bipyridine synthesis

[0042] Get 78.3g of Pd-THPP, 5gNaOH and 0.1g of surfactant F127, join in the 100ml alcohol-water mixed solvent containing volume ratio of 1:1, stir until completely dissolved; add 50ml formaldehyde solution (37wt %), after stirring and mixing evenly, the reaction was continued for 2 hours under heating conditions, and polymer precipitation occurred in the reaction mixture. The above mixture was transferred and sealed into a hydrothermal reactor and placed in a dry oven at 90° C. for 4 h. After the reaction, take out the reactant and adjust the pH of the solution to 6-7 with hydrochloric acid, filter the obtained precipitate, wash it several times with ethanol and distilled water, and dry it in a vacuum oven at 60°C to form a metal-coordinated organic framework polymer precursor. 10 g of the precursor was placed in a vacuum tube furnace, and carbonized and reduced at high temperature in a mixed ...

Embodiment 3

[0044] Example 3: Preparation of Pt@N-MPC and its catalytic bipyridine synthesis

[0045] Get 67.9g of THPP, 5gNaOH and 0.1g of surfactant F127, add it into 100ml of alcohol-water mixed solvent with a volume ratio of 1:1, stir until completely dissolved; add 50ml of formaldehyde solution (37wt%) to the above solution After stirring and mixing evenly, the reaction was continued for 2 hours under heating conditions, and polymer precipitation appeared in the reaction mixture. The above mixture was transferred and sealed into a hydrothermal reactor and placed in a dry oven at 90° C. for 4 h. After the reaction, take out the reactant and adjust the pH of the solution to 6-7 with hydrochloric acid, filter the precipitate and wash it several times with ethanol and distilled water, obtain the covalent organic framework polymer in a 60°C drying oven, and dry it in a vacuum drying oven. The covalent organic framework polymer was pulverized and sieved to obtain a solid with a particle s...

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Abstract

The invention discloses a preparation method and application of an N-doped mesoporous-carbon-loaded metal nano-catalyst. The preparation method comprises the steps of with a metal 5,10,15-20-tetra(4-hydroxyphenyl)porphyrin complex (M-THPP for short) as a starting material and a metal covalent organic framework polymer prepared through condensation polymerization of formaldehyde as a precursor, carrying out hydro-thermal synthesis and annealing, so as to obtain the N-doped mesoporous-carbon-loaded metal nano-catalyst M@N-MPC, wherein the nano-catalyst can be directly used for directly couplingpyridine to generate 2,2'-bipyridine, and M can be mono-metal and duplex metal. By virtue of a coordination effect of the catalyst precursor and carrier nitrogen, the metal active components, namely nano-particles are small in particle size and uniformly dispersed and have high catalytic activity to the reaction for directly coupling pyridine to synthesize dipyridyl, the reaction conditions are relatively mild, and the single-pass conversion rate is high; and meanwhile, the carbon catalyst carrier is high in stability and good in recycling cycle performance in a pyridine alkali wash reaction system and is particularly suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a preparation method of an N-doped mesoporous carbon-supported metal nanocatalyst and its application in catalyzing the direct coupling of pyridine to synthesize 2,2'-bipyridine. Background technique [0002] 2,2'-Bipyridine can be used as an important ligand and as an intermediate in the production of the pesticide diquat, and has a wide range of applications. Therefore, the development of green and environmentally friendly bipyridyl has important application value. [0003] At present, there are many routes for the synthesis of bipyridine at home and abroad, mainly including pyridine direct coupling method, alkyne amine or carbonyl compound ring method, chloropyridine Ullmann coupling reaction synthesis method, etc. The carbonyl compound cyclization method studied in the early stage has rare raw materials and long synthetic routes, which are not suitable for industrial production. At present, the most commonly used Ullmann ...

Claims

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Application Information

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IPC IPC(8): B01J31/18B01J31/16C07D213/22
CPCB01J31/1691B01J31/183B01J2231/34B01J2531/16B01J2531/824B01J2531/828B01J2531/847C07D213/22
Inventor 冯乙巳王旭东刘杰徐文艺浦同俊陈威豪
Owner HEFEI UNIV OF TECH
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