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A preparation method of nitrogen-doped porous carbon-supported metal single-atom material

A nitrogen-doped porous carbon and metal-loaded technology, applied in the field of materials science and engineering, can solve the problems of complex operation, low metal content, and few types, and achieve the effect of wide application and large specific surface area.

Active Publication Date: 2021-12-17
SUN YAT SEN UNIV
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  • Summary
  • 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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  • A preparation method of nitrogen-doped porous carbon-supported metal single-atom material
  • A preparation method of nitrogen-doped porous carbon-supported metal single-atom material
  • A preparation method of nitrogen-doped porous carbon-supported metal single-atom material

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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 invention relates to a controllable preparation method of a nitrogen-doped porous carbon-supported metal single-atom material, which belongs to the technical field of material science and engineering. The present invention polymerizes porphyrin-metalloporphyrin through polymerization reaction, regulates the ratio of porphyrin-metalloporphyrin to regulate the metal content (0.06-4.00 wt%), regulates different metalloporphyrin types and regulates metal single atom types (A type, AB type , ABC type). The invention realizes the controllable preparation of metal single-atom materials, has good scalability and reproducibility, solves the problems of low metal content and few types in the prior art, and enriches the synthesis methodology of metal single-atom materials and other related fields Research.

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 Patents(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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