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Preparation method of nitrogen-doped hollow porous carbon

A porous carbon material and nitrogen-doped technology, which is applied in the preparation/purification of carbon, can solve problems such as unreasonable pore size distribution, damage to reaction vessels, and complicated and lengthy environments, and achieve obvious environmental protection benefits, avoiding environmental hazards, The effect of simple synthesis process

Inactive Publication Date: 2017-05-17
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Some porous carbon materials currently commercially used have not yet met the above requirements due to their unreasonable pore size distribution and complicated and lengthy synthesis process that is not friendly to the environment.
For example, supercapacitor electrode materials, for supercapacitors, existing electrode materials, such as Chinese patent 201610272051.9, require special reaction materials such as graphene oxide and ionic liquids that have not yet achieved industrial mass production, and need to be activated before they can be used. Others Some patents, such as Chinese patent 201410705947.2, also need to activate the material at high temperature with alkaline substances to obtain a porous structure, but high-temperature etching of alkaline substances will damage the reaction vessel, and the synthesis process will also affect the environment
Few Chinese patents in this field involve recycling of by-products of synthesis products

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 0.7g KMnO 4 , 1.4 g MnSO 4 , dissolved in 70ml of water. The solution was poured into a hydrothermal kettle and kept at 150° C. for 12 hours. After it was cooled to room temperature, the obtained product was washed with suction and dried at 60° C. The brown powder obtained at this time is the attached figure 1 Manganese dioxide nanotubes are shown.

[0030] Take 400 mg of the prepared manganese dioxide nanotubes, 0.152 ml of aniline, and 0.116 ml of pyrrole, add them into 180 ml of water, stir for 20 min, put the solution in a refrigerator (3-5°C) and freeze for 30 min, take it out and add 1 ml of H 2 SO 4 , stirred for 0.5min, put it in a refrigerator (3-5°C) for 8h reaction, suction filtered the product until the filtrate was neutral, and dried at 60°C. The black product obtained at this time is the attached figure 2 Intermediates shown.

[0031] Take 400 mg of the intermediate product, place it in a tube furnace, and raise the temperature to 900 °C at a ...

Embodiment 2

[0034] Take 0.7g KMnO 4 , 1.5g MnSO 4 , dissolved in 70ml of water. The solution was poured into a hydrothermal kettle and kept at 120° C. for 5 hours. After it was cooled to room temperature, the obtained product was washed with suction and dried at 60° C. get attached at this time Figure 5 The three-dimensional manganese dioxide shown.

[0035] Take 200mg of manganese dioxide, 0.38ml of aniline, and 0.29ml of pyrrole, add them into 60ml of water, stir for 20min, put the solution in the refrigerator (3-5℃) and freeze for 30min, take it out and add 15ml of pre-frozen containing 1ml Concentrated H 2 SO 4 The aqueous solution was stirred for 0.5 min, put into the refrigerator (3-5°C) and reacted for 8h, the product was suction filtered until the filtrate was neutral, and dried at 60°C to obtain an intermediate product.

[0036] Take 200 mg of the intermediate product, place it in a tube furnace, and raise the temperature to 900°C at a rate of 5°C / min under a nitrogen atmo...

Embodiment 3

[0038] Take 0.7g KMnO 4 , 1.5g MnSO 4 , dissolved in 70ml of water. The solution was poured into a hydrothermal kettle and kept at 160° C. for 12 hours. After it was cooled to room temperature, the obtained product was washed by suction filtration and dried at 60° C. At this time, one-dimensional nanowire manganese dioxide is obtained.

[0039] Take 400mg of manganese dioxide, 0.38ml of aniline, and 0.29ml of pyrrole, add them into 60ml of water, stir for 20min, put the solution in the refrigerator (3-5°C) and freeze for 30min, take it out and add 15ml of pre-frozen containing 2ml h 2 SO 4The aqueous solution was stirred for 0.5 min, put into the refrigerator (3-5°C) and reacted for 8h, the product was suction filtered until the filtrate was neutral, and dried at 60°C to obtain an intermediate product.

[0040] Take 200 mg of the intermediate product, put it in a tube furnace, and raise the temperature to 900°C at a rate of 5°C / min under a nitrogen atmosphere, keep it war...

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Abstract

The invention relates to a preparation method of nitrogen-doped porous carbon. The preparation method specifically comprises the following steps of firstly, preparing a manganese dioxide precursor, preparing a mixing solution containing a certain ratio of aniline and pyrrole monomers, dispersing a manganese dioxide powder into the mixing solution, cooling the dispersing liquid to the temperature below 10 DEG C, adding an acid solution into the dispersing liquid, reacting for a period of time at low temperature, and separating, so as to obtain a product; finally, carbonizing at high temperature under the protection atmosphere, so as to obtain the nitrogen-doped hollow porous carbon material. The preparation method has the characteristics that the synthesis technology is simple, the safe, green and pollution-free effects are realized in the synthesis process, the byproducts can be recycled, the preparation method is suitable for industrial production, and the like; the property of the nitrogen-doped porous carbon is excellent, the specific surface area is higher, and the nitrogen-doped porous carbon can be widely applied to the fields of energy storage, catalysis, adsorption, such as supercapacitors.

Description

technical field [0001] The invention belongs to the field of porous material preparation, and in particular relates to a preparation method of nitrogen-doped hollow porous carbon material. Background technique [0002] In recent years, porous carbon materials have attracted the attention of more and more researchers because of their advantages such as high electrical conductivity, large specific surface area, and low price, and have been studied more and more widely. Used as electrode materials for supercapacitors, negative electrode materials for lithium-ion batteries, gas adsorption materials, and catalyst support materials, etc., and nitrogen-doped porous carbon materials with a hollow structure have macropores (>50nm), mesoporous (2- 50nm) and micropores (<2nm), the complete pore system can meet the needs of different application fields. At the same time, the presence of nitrogen atoms after nitrogen doping can significantly improve the electrochemical performance ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01P2004/03C01P2004/80C01P2006/12C01P2006/14C01P2006/40
Inventor 王建淦刘红震张智勇周蕊谢科予魏秉庆
Owner NORTHWESTERN POLYTECHNICAL UNIV
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