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Preparation method of nitrogen-doped nano porous hollow carbon spheres

A nano-porous, nitrogen-doped technology, applied in nano-carbon, nanotechnology, chemical instruments and methods, etc., can solve the problems of toxicity, complex post-processing, high equipment requirements, etc., and achieve improved reactivity, narrow particle size distribution, The effect of high specific surface area

Active Publication Date: 2017-11-03
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The hydrothermal carbonization method cannot produce products with uniform size and shape on a large scale, and generally requires high pressure, which requires high equipment, and the prepared carbon spheres are prone to agglomeration
The chemical vapor deposition method is relatively easy to industrialize, but this method consumes a lot of energy and costs, and the controllability of the shape and size of nano-carbon spheres is not easy to achieve
The post-processing of the hard template method is more complicated, and the soft template method is difficult to synthesize monodisperse carbon spheres
CN104439237A discloses a method for preparing iron-carbon spheres and hollow carbon spheres. This invention uses iron-containing compounds as catalysts, and plastics or recycled plastics as carbon source materials. The cost is low and the operation is simple, but the prepared carbon spheres poor dispersion
CN101181986A discloses a method for preparing nanoporous carbon spheres. The method utilizes porous starch as a carbon source precursor, and adopts the method of coating carbonization to prepare monodisperse nanoscale porous carbon microspheres under high temperature conditions, but adopts Tin-containing compounds are used as coating agents, which have certain toxicity to the human body and the environment, which affects their industrial applications

Method used

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  • Preparation method of nitrogen-doped nano porous hollow carbon spheres
  • Preparation method of nitrogen-doped nano porous hollow carbon spheres
  • Preparation method of nitrogen-doped nano porous hollow carbon spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1. Preparation of carbon sphere precursor

[0032]Weigh 14.0g styrene, 0.2g polystyrene, 0.8g hexadecane and 0.2g azobisisoheptanonitrile and mix to form an oil phase; weigh 0.2g sodium lauryl sulfate and 0.2g sodium nitrite and dissolve in Form a water phase in 90.0g of water; slowly add the oil phase to the water phase and magnetically stir for 0.5h for pre-emulsification, and then homogeneously emulsify for 5min at a shear rate of 19000rpm in an ice-water bath to form a miniemulsion; transfer the miniemulsion to the container In a three-necked flask with a stirrer, a thermometer and a reflux condenser, pass nitrogen gas for 0.5h, and react at a constant temperature in a water bath at 50°C for 1.0h to obtain polystyrene microspheres; add 10.0g of acrylonitrile dropwise to the obtained polystyrene microspheres Mixture with 0.2g of divinylbenzene, continue to react at constant temperature for 0.5h, then drop 5.0ml of γ-methacryloxypropyl trimethoxysilane into the reacti...

Embodiment 2

[0046] The preparation process of this example is the same as that of Example 1, except that the amount of aqueous phase polymerization inhibitor sodium nitrite is 0.1 g.

[0047] The nitrogen-doped nanoporous hollow carbon spheres obtained in this example have a particle size of about 100 nm and a specific surface area of ​​398 m 2 / g, the pore volume is 0.3cm 3 / g, the pore size is 3.1nm.

Embodiment 3

[0049] The preparation process of this example is the same as that of Example 1, except that the amount of aqueous phase polymerization inhibitor sodium nitrite is 0.05 g.

[0050] The nitrogen-doped nanoporous hollow carbon spheres obtained in this example have a particle size of about 100 nm and a specific surface area of ​​591 m 2 / g, the pore volume is 0.4cm 3 / g, the pore size is 2.9nm.

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Abstract

The invention discloses a preparation method of nitrogen-doped nano porous hollow carbon spheres. The preparation method comprises the following steps: preparing polystyrene / polyacrylonitrile core-shell structural composite microspheres by adopting styrene and acrylonitrile as monomers by virtue of miniemulsion polymerization; dropwise adding a silane coupling agent, and continuously polymerizing to form polystyrene / polyacrylonitrile / polysilane coupling agent dual-layer core-shell composite microspheres; and then pre-oxidizing, carbonizing and removing core-layer silicon dioxide to prepare the nitrogen-doped nano porous hollow carbon spheres. The polystyrene / polyacrylonitrile / polysilane coupling agent dual-layer core-shell composite microspheres prepared by adopting a seed miniemulsion polymerizing method are used as a precursor of the carbon spheres and have the characteristics of narrow distribution of particle size, good single dispersity, controllability in particle size and the like.

Description

technical field [0001] The invention relates to a preparation method of nitrogen-doped nanoporous hollow carbon spheres, belonging to the technical field of composite materials. Background technique [0002] Carbon materials have been active in research hotspots for many years. In addition to the existence of diamond and graphite in nature, researchers have successively prepared fullerene C 60 , carbon nanotubes, graphene, etc., the carbon material system is gradually being improved. The flexible bonding method of carbon materials makes them have various structural forms and has considerable application potential. They are widely used in many national economic fields such as energy, chemical industry, environmental protection, electronics, and aerospace. Spherical carbon materials were first produced from the mesophase spheres formed during the heat treatment of pitch-like compounds. Due to its many excellent properties, such as self-sintering performance, high bulk densit...

Claims

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Application Information

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IPC IPC(8): C01B32/15B82Y40/00B01J20/20B01J20/30B01J20/28
CPCB01J20/0259B01J20/103B01J20/20B01J20/28064B01J20/28071B01J20/28083B01J2220/4812B82Y40/00C01P2002/54C01P2004/34C01P2004/62C01P2004/64C01P2006/12C01P2006/14C01P2006/16C01P2006/40
Inventor 张建安赵静吴庆云吴明元杨建军
Owner ANHUI UNIVERSITY
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