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Preparation method for carbon nitride supported monodisperse oxidation state metal atom catalytic material

A technology of catalytic materials and metal atoms, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as specific surface area increase, catalyst deactivation, metal surface free energy increase, etc., to achieve Agglomeration inhibition, good dispersibility, and easy-to-control effects

Active Publication Date: 2017-06-20
BEIJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When the metal particles are reduced to the atomic level, the specific surface area increases sharply, which leads to a sharp increase in the free energy of the metal surface, and agglomeration and coupling easily occur during preparation and reaction to form large clusters, which leads to catalyst deactivation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Disperse 2 g of melamine in 100 mL of N,N-dimethylformamide and stir at room temperature for 3 h to obtain a melamine solution. Disperse 10 mg of copper carbonate in 10 mL of N,N-dimethylformamide, and ultrasonically treat it for 30 min to obtain a copper nitrate solution. Transfer the melamine solution to a 250mL round-bottomed flask, then add the copper carbonate solution to the melamine solution, configure a condensation reflux tube, heat to 110°C under nitrogen protection, stir for 48 hours in the dark, and then cool naturally to room temperature. The solvent was removed from the mixed solution by rotary evaporation to obtain a solid metal carbon-nitrogen adduct, which was dried in vacuum for 24 hours and then ground to 80 mesh. Put the solid powder in a ceramic crucible, put it into a tube furnace, and heat it under the condition of nitrogen protection. First, heat to 250°C at a rate of 5°C / min and keep for 1h, then heat to 500°C at a rate of 10°C / min and keep for...

Embodiment 2

[0019] Disperse 2 g of melamine in 100 mL of N,N-dimethylformamide and stir at room temperature for 3 h to obtain a melamine solution. Disperse 20 mg of manganese nitrate in 10 mL of N,N-dimethylformamide, and ultrasonically treat it for 30 min to obtain a manganese nitrate solution. Transfer the melamine solution to a 250mL round bottom flask, then add the manganese nitrate solution into the melamine solution, configure a condensing reflux tube, heat to 110°C under nitrogen protection, stir for 48 hours in the dark, and then cool naturally to room temperature. The solvent was removed from the mixed solution by rotary evaporation to obtain a solid metal carbon-nitrogen adduct, which was dried in vacuum for 24 hours and then ground to 80 mesh. Put the solid powder in a ceramic crucible, put it into a tube furnace, and heat it under the condition of nitrogen protection. First, heat to 300°C at a rate of 2°C / min and keep for 1h, then heat to 500°C at a rate of 5°C / min and keep f...

Embodiment 3

[0021] Disperse 2 g of melamine in 100 mL of methanol and stir at room temperature for 3 h to obtain a melamine solution. Disperse 20mg of iron carbonate in 10mL of methanol and ultrasonically treat it for 30min to obtain an iron carbonate solution. Transfer the melamine solution to a 250mL round-bottomed flask, then add the ferric carbonate solution into the melamine solution, configure a condensation reflux tube, heat to 50°C under nitrogen protection, stir for 24 hours in the dark, and then cool naturally to room temperature. The solvent was removed from the mixed solution by rotary evaporation to obtain a solid metal carbon-nitrogen adduct, which was dried in vacuum for 24 hours and then ground to 80 mesh. Put the solid powder in a ceramic crucible, put it into a tube furnace, and heat it under the condition of nitrogen protection. First, heat to 250°C at a rate of 5°C / min and keep for 2h, then heat to 450°C at a rate of 5°C / min and keep for 4h. Cool down to room tempera...

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Abstract

The invention mainly relates to a preparation method for a carbon nitride supported monodisperse oxidation state metal atom catalytic material, in particular to a preparation method of a layered graphite-phase carbon nitride supported monodisperse oxidation state metal M atom composite (M is one or two or more of Zn, V, Fe, Co, Ni, Sn, Pb, Cu, In and Mn), and belongs to the field of catalytic materials. The method adopts a way of complexation of a metal precursor and a carbon nitrogen precursor to inhibit agglomeration of metal atoms, and employs one-step pyrolysis of a metal carbon nitrogen adduct to prepare the carbon nitride supported monodisperse oxidation state metal atom catalytic material, wherein the metal M exists in the form of partial or complete oxidation state single atoms, and the varieties and composition of the supported metal atoms can be regulated as needed. The method of the invention has the characteristics of simplicity and easy control, and can be used for mass preparation of the carbon nitride supported monodisperse oxidation state metal atom catalytic material.

Description

technical field [0001] The present invention mainly relates to a preparation method of a carbon nitride-supported monodisperse oxidation state metal atom catalytic material, specifically a layered graphite phase carbon nitride supported monodisperse oxidation state metal M atom composite material (M is Zn, V, The preparation method of one or more of Fe, Co, Ni, Sn, Pb, Cu, In, Mn) belongs to the field of catalytic materials. [0002] Background technique: [0003] Single-atom catalysis is of great significance for the practical application of catalysts (X. Yang, A. Wang, B. Qiao, J. Li, J. Liu, T. Zhang. Accounts of Chemical Research, 2013, 46, 1740-1748.) . For high-loaded metal catalysts, only a small number of metal active components play a catalytic role in the catalytic reaction process. In comparison, single-atom catalysis where each metal atom acts as an active site is much more efficient than traditional supported metals. The metal utilization efficiency of the cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24
CPCB01J27/24
Inventor 卞兆勇王辉
Owner BEIJING NORMAL UNIVERSITY
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