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Large-scale prepared particle size-controllable nitrogen and oxygen doped carbon microsphere and preparation method and application thereof

A technology for large-scale preparation and carbon microspheres, which is applied in the preparation/purification of carbon, nanotechnology for materials and surface science, nanotechnology, etc. It can solve the problems of difficult large-scale preparation, complicated steps, and high cost. The preparation method is simple and easy, the mesopore volume is increased, and the yield is high.

Active Publication Date: 2019-05-21
ZIBO VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It solves the problems of complex steps, long time-consuming, high cost and difficult large-scale preparation in the existing carbon microsphere preparation process

Method used

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  • Large-scale prepared particle size-controllable nitrogen and oxygen doped carbon microsphere and preparation method and application thereof
  • Large-scale prepared particle size-controllable nitrogen and oxygen doped carbon microsphere and preparation method and application thereof
  • Large-scale prepared particle size-controllable nitrogen and oxygen doped carbon microsphere and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A Synthesis of precursor polymer microspheres (controlling the particle size of microspheres by adjusting the solvent composition)

[0031] Add 5g of diallyl phthalate, 7g of divinylbenzene, 5g of acrylonitrile and 80g of solvent into a 250ml three-neck flask. The three-necked flask was placed in an oil bath at 70°C with an electric digital display constant-speed stirring device, and condensed and refluxed. After stirring evenly, it was filled with nitrogen atmosphere for protection. Then, 0.2 g of azobisisobutyronitrile was added to start the polymerization reaction. After 3 hours, the reaction was completed, and the solid product was separated by centrifugation, washed and dried to obtain the precursor polymer microspheres. The rotating speed of the electric digital display constant speed stirring device is 900r / min, and the mass ratios of absolute ethanol and deionized water in the solvent are 2:3, 1:1, 3:2, 7:3, 4:1, 9: 1. According to formula 1, the average yiel...

Embodiment 2

[0040] A. Synthesis of precursor polymer microspheres (control the particle size of the microspheres by adjusting the stirring rate composition during the synthesis)

[0041] Add 7g of diallyl phthalate, 5g of divinylbenzene, 5g of acrylonitrile, and 80g of solvent into a 250ml three-necked flask. The three-necked flask was placed in an oil bath at 70°C with an electric digital display constant-speed stirring device, and condensed and refluxed. After stirring evenly, it was filled with nitrogen atmosphere for protection. Then, 0.2 g of azobisisobutyronitrile was added to start the polymerization reaction. After 3 hours, the reaction was completed, and the solid product was separated by centrifugation, washed and dried to obtain the precursor polymer microspheres. The mass ratio of ethanol to deionized water in the solvent is 9:1, and the stirring speeds of the electric digital display constant speed stirring device are 300, 600, 900, 1200 r / min respectively. Calculated accor...

Embodiment 3

[0048] A. Synthesis of precursor polymer microspheres

[0049] Take two 250ml three-necked flasks, numbered A and B respectively. Add 7g diallyl phthalate, 2g methyl acrylate, 3g ethyl acrylate, 5g acrylonitrile to bottle A; add 7g diallyl phthalate, 2g styrene, 3g methacrylic acid to bottle B Methyl ester, 5g acrylonitrile. Then 80 g of solvent were added separately. The three-necked flask was placed in an oil bath at 70°C with an electric digital display constant-speed stirring device, and condensed and refluxed. After stirring evenly, it was filled with nitrogen atmosphere for protection. Then, 0.2 g of azobisisobutyronitrile was added to start the polymerization reaction. After 3 hours, the reaction was completed, and the solid product was separated by centrifugation, washed and dried to obtain the precursor polymer microspheres. The mass ratio of ethanol to deionized water in the solvent is 9:1, and the stirring rate of the electric digital display constant speed stir...

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Abstract

The invention discloses a method for large-scale preparation of nitrogen and oxygen doped carbon microspheres. The method comprises the following steps of: stirring 2-8 parts of diallyl phthalate, 5-10 parts of acrylonitrile, 5-30 parts of a polymerizable monomer, 70-80 parts of a solvent and 0.2-1 part of azodiisobutyronitrile by weight under 70-80 DEG C for 3-5 hours, and carrying out centrifugal separation to obtain a solid powder product; heating the solid powder obtained in the step A to 800-900 DEG C at a certain speed under the protection of inert gas so as to obtain constant-temperature carbonization, and washing and drying the obtained black solid powder to obtain the nitrogen and oxygen doped carbon microspheres. The carbon microspheres are high in mesoporous content, high in specific area and favorable in capacitive performance, and can be used as a supercapacitor electrode material.

Description

Technical field: [0001] The invention relates to the technical field of micro-nano special configuration carbon materials. More specifically, the present invention relates to a method for large-scale preparation of nitrogen-oxygen-doped carbon microspheres with controllable particle size and its application in supercapacitors. Background technique: [0002] Among the many supercapacitor electrode materials, carbon materials often have large specific surface area, good pore size distribution, excellent conductivity, and low production cost, and have always been favored by scientific researchers. At present, new carbon materials mainly include activated carbon, carbon fiber, carbon nanotube, carbon microsphere, carbon aerogel and graphene. Among them, carbon microspheres have advantages that other carbon materials do not have, such as extremely regular morphology, controllable pore size and particle size distribution. This feature greatly reduces the ion diffusion resistance...

Claims

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Application Information

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IPC IPC(8): H01G11/24H01G11/30H01G11/36H01G11/38B82Y30/00B82Y40/00C01B32/05
CPCY02E60/13
Inventor 王小梅
Owner ZIBO VOCATIONAL INST
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