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Method for preparing ultrafine porous carbon nanoparticles from metal organic skeleton as precursor

A technology of metal-organic framework and carbon nanoparticles, which is applied in the field of preparation of ultra-microporous carbon nanoparticles, can solve the problems of ultra-microporous carbon materials that have not been seen yet, achieve excellent cycle stability, simple and efficient preparation method, excellent electrochemical performance effect

Active Publication Date: 2017-07-25
上海科漪实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the above-mentioned two difficulties, there have been no reports on the preparation of ultra-microporous carbon materials from metal-organic framework precursors.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Measure zirconium tetrachloride, biphenyl dicarboxylic acid, benzoic acid and N,N-dimethylformamide solution according to the mass ratio of 1:3:5:75, and after ultrasonic mixing, transfer the mixed solution to the reaction Heat treatment at 100 °C for 0.5 d in a kettle to obtain a metal-organic framework (UiO 67 ). In a tube furnace, under the protection of an inert gas, the obtained MOF was heated to 550°C for 5 hours at a heating rate of 1°C / min, and then cooled down to room temperature naturally, and removed with a 10% by mass hydrofluoric acid solution. Metal zirconium, that is, to obtain ultra-microporous carbon nanoparticles.

Embodiment 2

[0018] Measure zirconium tetrachloride, biphenyl dicarboxylic acid, benzoic acid and N,N-dimethylformamide solution at a ratio of 1:3:20:150 parts by mass, and after ultrasonic mixing, transfer the mixed solution to the reaction Heat treatment at 100°C for 1.5 d in a kettle to obtain a metal-organic framework (UiO 67 ). In a tube furnace, under the protection of an inert gas, the obtained MOF was heated to 650°C for 4 hours at a heating rate of 5°C / min, and then cooled down to room temperature naturally, and removed with a 10% by mass hydrofluoric acid solution. Metal zirconium can obtain ultra-microporous carbon nano-particles.

Embodiment 3

[0020] Measure zirconium tetrachloride, biphenyl dicarboxylic acid, benzoic acid and N,N-dimethylformamide solution according to the ratio of 1:3:15:225 parts by mass, and after ultrasonic mixing, transfer the mixed solution to the reaction Heat treatment at 100°C for 2 days in a kettle to obtain a metal-organic framework (UiO 67 ). In a tube furnace, under the protection of an inert gas, the obtained metal organic framework was heated to 900°C for 2 hours at a heating rate of 10°C / min, and then cooled to room temperature naturally, and removed with a 10% by mass hydrofluoric acid solution. Metal zirconium can obtain ultra-microporous carbon nano-particles.

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Abstract

The invention relates to a method for preparing ultrafine porous carbon nanoparticles from a metal organic skeleton as a precursor. The method comprises weighing zirconium tetrachloride, biphenyldicarboxylic acid, benzoic acid and N, N-dimethylformamide solution according to a mass ratio of 1: 1.5-4: 5-20: 70-300, carrying out uniform ultrasonic mixing, transferring the mixed solution into a reactor, carrying out heat treatment at a temperature of 100 DEG C for 0.5-2 d to obtain a metal organic skeleton UiO67, heating the metal organic skeleton UiO67 to 550-900 DEG C in an inert gas protective atmosphere in a tubular furnace at a heating rate of 1-10 DEG C / min, carrying out carbonization for 2-5h, naturally cooling the product to the room temperature, and removing metal zirconium through a hydrofluoric acid solution having a mass fraction of 10% so that ultrafine porous carbon nanoparticles are obtained. The method has simple processes. The ultrafine porous carbon nanoparticles have a high specific surface area and regular ultra-micropores, can be used as supercapacitor electrodes and have excellent electrochemical performances.

Description

technical field [0001] The invention relates to a method for preparing ultramicroporous carbon nanoparticles by using metal organic framework as a precursor. It belongs to the technical field of material preparation technology. Background technique [0002] Supercapacitor has the advantages of high power density, short charging time, good cycle stability, safety and reliability, etc. It is a green and efficient electrochemical energy storage device. Value. The design and development of high-performance electrode materials is a key factor for the practical application of supercapacitors. Porous carbon materials have the advantages of high specific surface area, good electrical conductivity and chemical stability, as well as a wide range of raw material sources and low cost. They are the most widely used electrode materials in supercapacitors in recent years. For example, "Preparation method and application of a hierarchical porous carbon material" (Chinese invention patent...

Claims

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Application Information

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IPC IPC(8): C01B32/05H01G11/86H01G11/36B82Y30/00
CPCY02E60/13H01G11/36B82Y30/00C01P2004/62C01P2006/12C01P2006/16C01P2006/40H01G11/86
Inventor 刘明贤赵方乐甘礼华
Owner 上海科漪实业有限公司
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