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Heteroatom-doped porous carbon hollow microspheres and preparation method thereof

A technology of hollow microspheres and porous carbon, which is applied in the field of inorganic carbon nanometers, can solve the problems of difficult structure, negative impact on material performance, uneven pore size distribution of hollow microspheres, etc., and achieve uniform material structure, large specific surface area and high output. Effect

Active Publication Date: 2017-07-18
上海鸿鹄骥航科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The pore size distribution of the hollow microspheres prepared by this technology is uneven, and the structure is difficult to control, which has a serious negative impact on the performance of the material.

Method used

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  • Heteroatom-doped porous carbon hollow microspheres and preparation method thereof
  • Heteroatom-doped porous carbon hollow microspheres and preparation method thereof
  • Heteroatom-doped porous carbon hollow microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] This embodiment includes the following steps:

[0036] 1) In a 150mL dry single-necked flask, dissolve 1.0g of 4,4'-thiobisthiophenol in 60mL of acetonitrile and disperse evenly by ultrasonication. Add 1mL of triethylamine to the above reaction solution and continue the reaction for 30 minutes. This reaction liquid is added in the polytetrafluoroethylene digestion tank that contains 0.5g hexachlorocyclotriphosphazene and 0.5g p-phenylenediamine, in the system, add appropriate amount of triethylamine as acid-binding agent, then the digestion tank is sealed, 160 ℃ for 3 hours. After the reaction, the product was filtered, washed with water and ethanol to obtain polyphosphazene hollow microspheres.

[0037] 2) Put the polyphosphazene microspheres into a porcelain boat, place it in the middle of the furnace cavity of the tube furnace, seal the tube furnace, and pass inert gas for 1 hour to replace the oxygen in the furnace cavity.

[0038] In this embodiment, the heating ...

Embodiment 2

[0043] This embodiment includes the following steps:

[0044] 1) In a 150mL dry single-necked flask, dissolve 1.0g of 4,4'-thiobisthiophenol in 60mL of acetonitrile and disperse evenly by ultrasonication. Add 0.5mL of triethylamine to the above reaction solution and continue the reaction for 30 minutes. Add the reaction solution into a polytetrafluoroethylene digestion tank containing 0.5g hexachlorocyclotriphosphazene and 1.0g 4,4'-diaminodiphenylmethane, add an appropriate amount of triethylamine as an acid-binding agent in the system, and then Seal the digestion tank and react at 160°C for 3 hours. After the reaction, the product was filtered, washed with water, and washed with ethanol to obtain polyphosphazene hollow microspheres

[0045] 2) Put the polyphosphazene microspheres into a porcelain boat, place it in the middle of the furnace cavity of the tube furnace, seal the tube furnace, and pass inert gas for 1 hour to replace the oxygen in the furnace cavity.

[0046] ...

Embodiment 3

[0050] This embodiment includes the following steps:

[0051] 1) In a 150mL dry single-necked flask, dissolve 1.0g of 4,4'-thiobisthiophenol in 60mL of acetonitrile, and disperse evenly with ultrasound (150W, 50°C), add 1mL of triethylamine to the above reaction solution, The reaction was continued for 30 minutes. Add the reaction solution into a flask containing 0.5g of hexachlorocyclotriphosphazene and 1.1g of 4,4'-dihydroxydiphenylsulfone, and disperse it evenly by ultrasonication. The reaction was carried out for 3 hours. After the reaction, the product was filtered, washed with water, and washed with ethanol to obtain polyphosphazene hollow microspheres

[0052] 2) Put the polyphosphazene microspheres into the porcelain boat, and place it in the middle of the cavity of the tube furnace.

[0053] In this embodiment, the heating setting of the tube furnace is as follows: the temperature is raised from normal temperature to 350°C at a rate of 5°C / min, kept at this tempera...

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Abstract

The invention provides heteroatom doped hollow porous carbon microspheres and a preparation method thereof. A micro-nano capsule formed by 4,4'-thiobisbenzenethiol and triethylamine is taken as a template, hollow polyphosphazene microspheres are prepared by coating and modifying the surface of the template through polyphophazene, finally, carbonization and activation treatment are performed in an inert atmosphere, and the heteroatom doped hollow porous carbon microspheres are obtained. The following complicated template removal process of a hard template method is avoided; a large quantity of non-carbon atoms in the polyphophazene molecular structure provide a necessary condition for formation of the heteroatom doped structures in the hollow carbon microspheres. According to the preparation method, the yield is high, the material structure is uniform, the specific surface area is large, and the preparation method is an efficient method for preparation of the heteroatom doped hollow porous carbon microspheres.

Description

technical field [0001] The invention relates to a technology in the field of inorganic carbon nanometers, in particular to a heteroatom-doped porous carbon hollow microsphere and a preparation method thereof. Background technique [0002] Carbon hollow microspheres have broad application prospects in the fields of catalysis and electrochemical energy storage. At present, the main preparation method of carbon hollow microspheres is the hard template method. In this method, carbonaceous precursors are first assembled, complexed or adsorbed on the periphery of the hard template, and then hollow carbon microspheres are obtained through processes such as carbonization and removal of the template. Due to the process of removing the template, the process is complicated. For example, using an etchant such as hydrofluoric acid to etch the template is cumbersome and can cause great harm to the environment. Therefore, it is of great economic value to realize the controllable and effi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/318
CPCC01P2002/72C01P2002/82C01P2004/04C01P2004/34
Inventor 黄小彬陈奎永高转刘洪
Owner 上海鸿鹄骥航科技有限公司
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