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Preparation method of nitrogen-doped porous carbon-supported metal monoatomic material

A nitrogen-doped porous carbon and metal-loaded technology, which is applied in the field of materials science and engineering, can solve the problems of low metal content, poor adjustability, and complicated operation, and achieve rich research, wide application, and meet the requirements of experimental diversification. Effect

Active Publication Date: 2018-09-28
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Based on the characteristics and disadvantages of metal single atom preparation methods based on wet chemical method, deposition method and pyrolysis method, the purpose of the present invention is to provide a controllable preparation method of nitrogen-doped porous carbon-supported metal single atom material to solve the existing problems. Problems such as low metal content, few types, poor adjustability and complicated operation in technology

Method used

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  • Preparation method of nitrogen-doped porous carbon-supported metal monoatomic material
  • Preparation method of nitrogen-doped porous carbon-supported metal monoatomic material
  • Preparation method of nitrogen-doped porous carbon-supported metal monoatomic material

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Experimental program
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Effect test

Embodiment 1

[0037] Add TPP in 100 ml polytetrafluoroethylene lining: PtTPP = 0.922 g : 0.008 g (99 wt% : 1wt%), 30 ml dichloromethane, 3.195 g anhydrous aluminum chloride; Magnetic stirring in a stainless steel reactor, reaction The temperature was 60 °C, and the reaction time was 48 h; after the Friedel-Crafts alkylation reaction, the Soxhlet extraction and purification were performed with THF, acetone, and methanol, and vacuum 80 o C dried overnight. The polymer product of the Friedel-Crafts alkylation reaction was carbonized at 600 °C in a tube furnace, the gas flow of carbonization was selected from argon, the carbonization time was 5 h, and Pt was obtained after cooling to room temperature. 1 / N-C metal single atom. ICP quantification: Pt—0.06 wt%. Spherically aberration-corrected TEM such as figure 2 As shown in A.

Embodiment 2

[0039] Add TPP in 100 ml polytetrafluoroethylene liner: PtTPP = 0.922 g : 0.015 g (98 wt% : 2wt%), 30 ml methylene chloride, 3.195 g anhydrous aluminum chloride; magnetic stirring in a stainless steel reactor, reaction The temperature was 60 °C, and the reaction time was 48 h; after the Friedel-Crafts alkylation reaction, the Soxhlet extraction and purification were performed with THF, acetone, and methanol, and vacuum 80 o C dried overnight. The polymer product of the Friedel-Crafts alkylation reaction was carbonized at 600 °C in a tube furnace, the gas flow of carbonization was selected from argon, the carbonization time was 5 h, and Pt was obtained after cooling to room temperature. 1 / N-C metal single atom. ICP quantification: Pt—0.21 wt%. Spherically aberration-corrected TEM such as figure 2 Shown in B.

Embodiment 3

[0041] Add TPP in 100 ml polytetrafluoroethylene lining: PtTPP = 0.922 g : 0.030 g (97 wt% : 3wt%), 30 ml dichloromethane, 3.195 g anhydrous aluminum chloride; Magnetic stirring in a stainless steel reactor, reaction The temperature was 60 °C, and the reaction time was 48 h; after the Friedel-Crafts alkylation reaction, the Soxhlet extraction and purification were performed with THF, acetone, and methanol, and vacuum 80 o C dried overnight. The polymer product of the Friedel-Crafts alkylation reaction was carbonized at 600 °C in a tube furnace, the gas flow of carbonization was selected from argon, the carbonization time was 5 h, and Pt was obtained after cooling to room temperature. 1 / N-C metal single atom. ICP quantification: Pt—0.58 wt%. Spherically aberration-corrected TEM such as figure 2 C shown.

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Abstract

The present invention relates to a controllable preparation method of a nitrogen-doped porous carbon-supported metal monoatomic material, and belongs to the technical field of material science and engineering. According to the present invention, porphyrin and a metalloporphyrin are polymerized through a polymerization reaction. The proportions of the porphyrin and the metalloporphyrin are regulated to regulate a metal content (0.06-4.00wt%), and monoatomic metal types (A type, AB type, ABC type) are regulated by regulating different types of metalloporphyrins. According to the present invention, controllable preparation of a metal monoatomic material is realized with good expansibility and reproducibility; meanwhile, the problems of low metal content, few types and the like in the prior art are solved, and researches in the related fields such as the synthetic methodology of metal monoatomic materials and the like.

Description

technical field [0001] The invention relates to the technical field of material science and engineering, in particular to a method for preparing a nitrogen-doped porous carbon-supported metal single-atom material. Background technique [0002] Single-atom catalysts are highly dispersed metals on a certain carrier in the form of atoms, reaching the limit of metal dispersion and maximizing the utilization of atoms. Single-atom catalysts have the advantages of "isolated sites" of homogeneous catalysts and stable and easy-to-separate structures of heterogeneous catalysts. They can closely link heterogeneous catalysis and homogeneous catalysis, and serve as a bridge between heterogeneous catalysis and homogeneous catalysis. and ties. The preparation of single-atom catalysts greatly reduces the amount of precious metals used and reduces production costs. Under certain conditions, its catalytic performance, selectivity, and stability are significantly better than traditional suppo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08B01J35/10
CPCB01J27/24B01J37/084B01J37/086B01J35/23B01J35/617
Inventor 纪红兵何晓辉肖华健何千
Owner SUN YAT SEN UNIV
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