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Preparation method and application of metal-loaded nitrogen-doped wrinkled graphene

A technology of supporting metals and graphene, applied in the field of nanomaterials, can solve the problems of large-scale preparation and popularization and application of unfavorable materials, complex preparation steps, and high equipment dependence, and achieves changes in catalytic and electrochemical performance. Actionable effect

Pending Publication Date: 2020-04-28
JIANGSU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] There are many existing methods for preparing nitrogen-doped wrinkled graphene, such as gel method, spinning method, spray drying method, etc., and the methods for loading metals on it mainly include impregnation method, etc., but the existing methods are generally dependent on equipment. High density, complex preparation steps, harsh conditions and other disadvantages are not conducive to the large-scale preparation and application of this type of material

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  • Preparation method and application of metal-loaded nitrogen-doped wrinkled graphene
  • Preparation method and application of metal-loaded nitrogen-doped wrinkled graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1, the preparation of a kind of nitrogen-doped wrinkled graphene

[0027] (1) Ultrasonic disperse 100 mg graphene oxide in 40 mL solvent, stir for 20 min, and make a homogeneous suspension;

[0028] (2) Dissolve 100 mg of ethylenediamine-capped polyethyleneamine (molecular weight: 1500) into 40 mL of solvent and stir for 20 min;

[0029] (3) Mix the above two solutions, stir for 30 min, transfer to a 100 mL hydrothermal reaction kettle with a polytetrafluoroethylene liner, heat at 180°C for 36 h, collect the solid by centrifugation after cooling, and wash with pure water and ethanol in turn , 60 ° C vacuum drying to obtain a solid powder.

[0030] (4) The obtained product is 112 mg of wrinkled nitrogen-doped graphene, elemental analysis C: 72.1%, N: 9.1%, H: 4.3%, BET test shows that the specific surface area is 756 m 2 / g.

Embodiment 2

[0031] Embodiment 2, the preparation of a kind of nitrogen-doped wrinkled graphene

[0032] (1) Ultrasonic disperse 100 mg graphene oxide in 40 mL solvent, stir for 20 min, and make a homogeneous suspension;

[0033] (2) Dissolve 50 mg of ethylenediamine-capped polyethyleneamine (molecular weight: 1500) in 40 mL of solvent and stir for 20 min;

[0034] (3) Mix the above two solutions, stir for 30 min, transfer to a 100 mL hydrothermal reaction kettle with a polytetrafluoroethylene liner, heat at 180 °C for 36 h, and centrifuge to collect the solid after cooling. Washing, vacuum drying at 60°C to obtain solid powder;

[0035] (4) Put the above solid into a quartz boat and place it in a tube furnace, then pass nitrogen gas for 10~30 min, the air flow rate is 50mL / min, raise the temperature to 700°C at a speed of 2°C / min, keep it warm for 240 min, and cool To room temperature, 86 mg of nitrogen-doped graphene rich in wrinkles was obtained, elemental analysis C: 84.5%, N: 5.9%, ...

Embodiment 3

[0036] Example 3, Preparation of a nitrogen-doped wrinkled graphene loaded with metal cobalt

[0037] (1) Ultrasonic disperse 100 mg graphene oxide in 40 mL solvent, stir for 20 min, and make a homogeneous suspension;

[0038] (2) Dissolve 100 mg of ethylenediamine-capped polyethyleneamine (molecular weight: 1500) in 40 mL of solvent, stir for 20 min, and add 5 mg of cobalt acetate;

[0039] (3) Mix the above two solutions, stir for 30 min, transfer to a 100 mL hydrothermal reaction kettle with a polytetrafluoroethylene liner, heat at 180 °C for 36 h, and centrifuge to collect the solid after cooling. Washing, vacuum drying at 60°C to obtain solid powder;

[0040] (4) The obtained product is nitrogen-doped wrinkled graphene loaded with metal cobalt, elemental analysis C: 71.4%, N: 9.7%, H: 4.4%, BET test shows that the specific surface area is 743 m 2 / g, ICP tests show that the loading of metal cobalt is 0.67%.

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Abstract

The invention discloses a preparation method and application of metal-loaded nitrogen-doped wrinkled graphene. Graphene oxide, ethylenediamine-terminated polyvinylamine and corresponding metal salt are used as raw materials. The preparation method comprises the following steps: dispersing graphene oxide into a certain solvent to form a solution A; preparing an ethylenediamine-terminated polyvinylamine solution with a certain concentration, adding a certain amount of a metal salt into the solution to form a solution B, mixing and stirring the solution A and the solution B, carrying out a hydrothermal reaction in a hydrothermal reaction kettle, collecting a solid after cooling, washing the solid, and drying the solid to obtain the final product. The experimental process is simple, the operability is high, and industrial popularization is facilitated; the prepared metal-loaded nitrogen-doped wrinkled graphene has the advantages of large specific surface area, a large number of wrinkles and pores, good structure retentivity, uniform nitrogen doping and uniform metal loading, greatly changes the catalytic and electrochemical properties of graphene, and widens the application of graphenein the fields of catalysis and energy storage.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a preparation method and application of metal-loaded nitrogen-doped wrinkled graphene. Background technique [0002] Carbon materials have become the most widely used materials in the world due to their many forms. As a kind of carbon materials, graphene has ultra-high electrical conductivity, high mechanical strength, huge specific surface area and good chemical stability. Therefore, it is considered as an ideal support for single-atom dispersed catalysts. Graphene is a two-dimensional carbon nanomaterial composed of carbon atoms with sp² hybrid orbitals forming a hexagonal honeycomb lattice. Due to its atomic-level thickness, graphene exhibits a unique electronic structure, which in turn exhibits peculiar macroscopic physical properties. chemical properties. [0003] However, pure graphene will agglomerate or even re-stack due to van der Waals force and π-π stacking, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184B01J27/24B01J35/10C07C51/15C07C57/24C07C209/34C07C211/46
CPCC01B32/184B01J27/24C07C51/15C07C209/34C01B2204/22B01J35/60C07C57/42C07C211/46
Inventor 毛武涛倪萍张子祥张少杰丁一鸣马超李茂龙鲍克燕
Owner JIANGSU UNIV OF TECH
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