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Preparation method of nitrogen content-adjustable nitrogen-doped ordered mesoporous carbon

A nitrogen-containing, porous carbon technology is applied in the field of preparation of nitrogen-doped ordered mesoporous carbon, which can solve the problems of long aging time, high reaction temperature, time-consuming and energy consumption, and achieves simple process, mild reaction conditions, The effect of short reaction time

Active Publication Date: 2018-01-09
RES INST OF FORESTRY NEW TECH CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are still many problems in the preparation of nitrogen-doped ordered mesoporous carbons by the conventional self-assembled soft template method: for example, the self-assembly induced by solvent evaporation needs to evaporate a large amount of solvent, which is very time-consuming and energy-consuming; Assembly requires high reaction temperature; liquid-phase self-assembly often requires very long aging time

Method used

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  • Preparation method of nitrogen content-adjustable nitrogen-doped ordered mesoporous carbon

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Effect test

Embodiment 1

[0017] 28 mg Na at 20°C 2 CO 3 Dissolve 1.68 g of bis-nitrile amine with 11.3 g of 37% formaldehyde solution, add 11.0 g of resorcinol under stirring, and stir for 4 h. Subsequently, the above mixed solution was added to 8.0 g of F127 solution dissolved in 40 mL of water and 64 mL of ethanol, and 5 mL of hydrochloric acid with a concentration of 2 mol / L was added rapidly, and the reaction was stirred for 2 h. After aging at room temperature for 12 h, the supernatant was discarded and dried at 100 °C for 12 h. The dried samples were placed in a tube furnace and carbonized at 600 °C for 3 h under the protection of nitrogen. Nitrogen-doped ordered mesoporous carbon was obtained by heating at 600 °C for 3 h at a rate of 2 °C / min and cooling to room temperature naturally.

Embodiment 2

[0019] 28 mg Na at 20°C 2 CO 3 Dissolve 2.52 g of bis-nitrile amine with 11.3 g of 37% formaldehyde solution, add 11.0 g of resorcinol under stirring, and stir for 3 h. Subsequently, the above mixed solution was added to 8.0 g of F127 solution dissolved in 40 mL of water and 64 mL of ethanol, and 5 mL of hydrochloric acid with a concentration of 2 mol / L was added quickly, and the reaction was stirred for 1 h. After aging at room temperature for 12 h, the supernatant was discarded and dried at 100 °C for 12 h. The dried samples were placed in a tube furnace and carbonized at 600 °C for 3 h under the protection of nitrogen. Nitrogen-doped ordered mesoporous carbon was obtained by heating at 600 °C for 3 h at a rate of 2 °C / min and cooling to room temperature naturally.

Embodiment 3

[0021] 28 mg Na at 20°C 2 CO 3 and 3.36 g of bis-nitrile amine were dissolved with 11.3 g of 37% formaldehyde solution, and 11.0 g of resorcinol was added under stirring, and the reaction was stirred for 2 h. Subsequently, the above mixed solution was added to 8.0 g of F127 solution dissolved in 40 mL of water and 64 mL of ethanol, and 5 mL of hydrochloric acid with a concentration of 2 mol / L was added quickly, and the reaction was stirred for 1 h. After aging at room temperature for 12 h, the supernatant was discarded and dried at 100 °C for 12 h. The dried samples were placed in a tube furnace and carbonized at 600 °C for 3 h under the protection of nitrogen. Nitrogen-doped ordered mesoporous carbon was obtained by heating at 600 °C for 3 h at a rate of 2 °C / min and cooling to room temperature naturally.

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Abstract

The invention discloses a preparation method of nitrogen content-adjustable nitrogen-doped ordered mesoporous carbon. The preparation method comprises the following steps dissolving a mixture of a nitrogen-containing compound and inorganic base in a formaldehyde solution, adding m-dihydroxybenzene with stirring, and stirring for reacting; adding the prepared mixed solution into F127 dissolved in amixed solvent of ethanol and water, adding hydrochloric acid for catalyzing a reaction, and stirring continually for 0.5 to 4 hours; aging the mixed solution at room temperature after finishing the stirring, pouring out supernatant, and drying to obtain a sample; controlling the heating rate of a tube furnace under the protection of nitrogen gas, carbonizing the prepared sample to obtain the nitrogen-doped ordered mesoporous carbon. The method has the characteristics of mild reaction condition, short reaction time, simple process, and adjustable and controllable nitrogen doping content and the like, and is more suitable for producing the nitrogen-doped ordered mesoporous carbon on a large scale.

Description

technical field [0001] The invention belongs to the technical field of carbon materials in inorganic non-metallic materials, and in particular relates to a preparation method of nitrogen-doped ordered mesoporous carbon with adjustable nitrogen content. Background technique [0002] Ordered mesoporous carbons (Ordered mesoporous carbons, OMCs) refer to a new type of carbon material with ordered pores and pore diameter distribution in the range of 2-50 nm. Due to its high specific surface area, large pore volume, and adjustable The pore size and narrow pore size distribution, good ion and molecule transport performance, and high chemical and thermal stability have a wide range of applications in the fields of adsorption, separation, catalyst loading, and energy storage. [0003] The properties of ordered mesoporous carbons are not only affected by pore size and arrangement, but also affected by surface functional groups and chemical composition. Nitrogen-doped ordered mesop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
Inventor 王傲蒋剑春孙康陈超许伟朱光真卢辛成
Owner RES INST OF FORESTRY NEW TECH CHINESE ACAD OF FORESTRY
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