A kind of in-situ nitrogen-doped porous carbon material and its preparation method

A nitrogen-doped porous carbon, in-situ technology, applied in the field of materials science, can solve problems such as high toxicity and lengthy procedures

Active Publication Date: 2021-09-14
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, regardless of whether silicon oxide is used as a soft template or a hard template, the post-processing process is lengthy, and hydrofluoric acid must be used to etch to remove template agents such as silicon dioxide, which is highly toxic.

Method used

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  • A kind of in-situ nitrogen-doped porous carbon material and its preparation method
  • A kind of in-situ nitrogen-doped porous carbon material and its preparation method
  • A kind of in-situ nitrogen-doped porous carbon material and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0034] (1) Precursor preparation: weigh MgCl 2 ·6H 2 O (12.19g, 60mmol) and AlCl 3 ·6H 2 O (19.3g, 40mmol) was dissolved in 150g deionized water to obtain mixed solution I; NaOH (4g, 0.2mol) and NaOH were weighed 2 CO 3 (8.48g, 0.08mol) was dissolved in 150g deionized water to obtain mixed solution II; at room temperature, mixed solution II was slowly added dropwise to mixed solution I, and then added with a mass concentration of 37% formaldehyde solution 22.1g (formaldehyde The molar weight is 0.272mol), resorcinol 15g (0.136mol), after stirring for 2h, adjust the pH value to 10 with sodium hydroxide solution. The stirring temperature was raised to 40°C for 2 hours, then 3.82 g (0.045 mol) of dicyandiamide was added, transferred to a hydrothermal kettle, and the temperature was continued to rise to 80°C for 18 hours of hydrothermal reaction. After the reaction, a gel was obtained, which was placed in an oven, dried at 110° C. for 12 hours, and then ground into powder to ...

Embodiment 2

[0040] (1) Precursor preparation: weigh MgCl 2 ·6H 2 O (12.19g, 60mmol) and AlCl 3 ·6H 2 O (19.3g, 40mmol) was dissolved in 150g deionized water to obtain mixed solution I; NaOH (4g, 0.2mol) and NaOH were weighed 2 CO 3 (8.48g, 0.08mol) was dissolved in 150g deionized water to obtain mixed solution II; at room temperature, mixed solution II was slowly added dropwise to mixed solution I, and then adding mass concentration was 37% formaldehyde aqueous solution 16.57g (formaldehyde The molar weight is 0.204mol), resorcinol 15g (0.136mol), after stirring for 3h, adjust the pH value to 11 with sodium hydroxide solution. The stirring temperature was raised to 50°C for 2 hours, then 3.82 g (0.045 mol) of dicyandiamide was added, transferred to a hydrothermal kettle, and the temperature was continued to rise to 100°C for 18 hours of hydrothermal reaction. After the reaction, a gel was obtained, which was placed in an oven, dried at 100° C. for 48 hours, and then ground into powde...

Embodiment 3

[0046] (1) Precursor preparation: weigh MgCl 2 ·6H 2 O (12.19g, 60mmol) and AlCl 3 ·6H 2 O (19.3g, 40mmol) was dissolved in 150g deionized water to obtain mixed solution I; NaOH (4g, 0.2mol) and NaOH were weighed 2 CO 3 (8.48g, 0.08mol) was dissolved in 150g deionized water to obtain mixed solution II; at room temperature, mixed solution II was slowly added dropwise to mixed solution I, and then added with a mass concentration of 37% formaldehyde solution 22.1g (formaldehyde The molar weight is 0.272mol), resorcinol 15g (0.136mol), after stirring for 2h, adjust the pH value to 10 with sodium hydroxide solution. The stirring temperature was raised to 40°C for 2 hours, then 11.1 g (0.132 mol) of dicyandiamide was added, transferred to a hydrothermal kettle, and the temperature was continued to rise to 80°C for 48 hours of hydrothermal reaction. After the reaction, a gel was obtained, which was placed in an oven, dried at 150° C. for 12 hours, and then ground into powder to ...

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Abstract

The invention relates to a method for preparing an in-situ nitrogen-doped porous carbon material, belonging to the technical field of material science. Using in-situ synthesized magnesium aluminum hydrotalcite as an auxiliary pore-forming agent, phenols or methyl-substituted phenols, formaldehyde are copolymerized with nitrogen-containing monomers, and a nitrogen-doped carbon precursor is generated by one-pot hydrothermal method, which is then roasted at high temperature and Acid treatment yields porous carbon materials. By controlling the molar ratio of phenolic formaldehyde, the amount of nitrogen-containing polymerized monomers, the ratio of magnesium-aluminum to phenolic polymerized monomers, and the hydrothermal reaction conditions, the specific surface area, pore size distribution, and nitrogen-doped amount of nitrogen-doped porous carbon can be regulated; The prepared material has a high carbon residue rate and a narrow pore size distribution range. The method can avoid the use of hydrofluoric acid, has strong operability and is relatively environment-friendly.

Description

technical field [0001] The invention relates to an in-situ nitrogen-doped porous carbon material and a preparation method thereof, belonging to the technical field of material science. Background technique [0002] Porous carbon materials have the characteristics of low cost, light weight, non-toxicity, surface chemical inertness, high temperature resistance, acid and alkali resistance, high mechanical stability, good electrical conductivity, adsorption, and large specific surface area and pore volume. , hydrogen storage, catalysis, and fuel cells and electrochemical double-layer capacitors have shown great application potential and have attracted much attention. [0003] The porous carbon material prepared by using phenolic resin as the carbon source without auxiliary pore-forming technology is mainly microporous, with a small specific surface area, generally less than 100m 2 / g, the pore volume is less than 0.1cm 3 / g, no matter in the field of fuel cells or catalysis, i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/312C01B32/05
CPCC01B32/05C01B32/312
Inventor 庞思平李佳哲孙成辉严致远宋建伟
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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