In-situ nitrogen-doped porous carbon material and preparation method thereof

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

Active Publication Date: 2020-08-11
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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  • In-situ nitrogen-doped porous carbon material and preparation method thereof
  • In-situ nitrogen-doped porous carbon material and preparation method thereof
  • In-situ nitrogen-doped porous carbon material and preparation method thereof

Examples

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 preparation method of an in-situ nitrogen-doped porous carbon material, belonging to the technical field of material science. According to the method, magnesium-aluminum hydrotalcite synthesized in situ serves as an auxiliary pore forming agent, phenols or methyl substituted phenols, formaldehyde and nitrogen-containing monomers are copolymerized, a nitrogen-doped carbonprecursor is generated through a one-pot hydrothermal method, and then high-temperature roasting and acid treatment are carried out to prepare the porous carbon material. The specific surface area, pore size distribution and nitrogen doping amount of the nitrogen-doped porous carbon are regulated and controlled by controlling the molar ratio of phenolic aldehyde, the dosage of nitrogen-containingpolymeric monomers, the ratio of magnesium-aluminum to a phenol polymeric monomers and hydrothermal reaction conditions; and the prepared material is high in carbon residue rate and narrow in pore size distribution range. The method can avoid usage of hydrofluoric acid, and is high in operability and friendly to environment.

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 Applications(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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