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Nitrogen-rich hierarchical pore carbon material and preparation method

A technology of multi-level pores and carbon materials, used in structural parts, electrical components, battery electrodes, etc., can solve the problems of few active sites, can not reflect performance, no micropores, etc., and achieve the effect of reducing costs.

Inactive Publication Date: 2016-08-17
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the pore size distribution of the obtained material is narrow, and there are no macropores for rapid material transport, and no micropores for "confinement effect"; at the same time, the cost of the precursor template is high and cannot be reused, resulting in high cost
[0003] The level of nitrogen content and the uniformity of distribution are another important factor affecting the performance of nitrogen-containing carbon materials. Nitrogen-containing polymer materials are often accompanied by severe decomposition during high-temperature carbonization. After the resin is decomposed, ammonia, nitrogen and nitrogen oxides are often obtained. Gas small molecules, so that the nitrogen content in the final material is below 2%, which often cannot show excellent performance as redox catalysts and adsorbents due to fewer active sites

Method used

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  • Nitrogen-rich hierarchical pore carbon material and preparation method
  • Nitrogen-rich hierarchical pore carbon material and preparation method
  • Nitrogen-rich hierarchical pore carbon material and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: Preparation of nitrogen-rich porous carbon material with cyclohexane and ethanol as reaction solvent

[0026] Take 8 mL of cyclohexane and 20 mL of ethanol in a two-necked flask, control the temperature at 60 °C, mix and disperse evenly for 1 h, add 0.5 g of aniline and disperse for 30 min, then add 1 mL of formaldehyde, and react for 5 h. After the reaction, The obtained product was washed three times with deionized water and three times with cyclohexane, and dried at 80° C. to obtain a nitrogen-rich porous polymer material. Under the protection of inert gas, the purified product was carbonized at 800 °C for 3 h to obtain a nitrogen-rich hierarchical porous carbon material.

[0027] The product was scanned by an electron microscope and identified as having a porous structure. Nitrogen adsorption-desorption proves that it contains hierarchical pore structure and pore distribution.

Embodiment 2

[0028] Embodiment 2: Preparation of nitrogen-rich porous carbon material with isopropanol and water as reaction solvent

[0029] Take 20 mL of isopropanol and 8 mL of water in a two-necked flask, control the temperature at 70 °C, mix and disperse evenly for 1 h, add 0.5 g of m-phenylenediamine and disperse for 30 min, then add 1 mL of formaldehyde, react for 5 h, and react After the end, the obtained product was washed three times with deionized water and three times with cyclohexane, and dried at 80° C. to obtain a nitrogen-rich porous polymer material. Under the protection of inert gas, the purified product was carbonized at 800 °C for 3 h to obtain a nitrogen-rich hierarchical porous carbon material.

[0030] The product was scanned by an electron microscope and identified as having a porous structure. Nitrogen adsorption-desorption proves that it contains hierarchical pore structure and pore distribution.

Embodiment 3

[0031] Example 3: Preparation of nitrogen-rich porous carbon material with tetrahydrofuran and water as reaction solvent

[0032] Take 20 mL of tetrahydrofuran and 8 mL of water in a two-necked flask, control the temperature at 60 °C, mix and disperse evenly for 1 h, add 0.5 g of aniline and disperse for 30 min, then add 1 mL of formaldehyde, and react for 5 h. After the reaction, the obtained product After washing three times with deionized water and three times with cyclohexane, and drying at 80°C, a nitrogen-rich porous polymer material is obtained. Under the protection of inert gas, the purified product was carbonized at 600 °C for 3 h to obtain a nitrogen-rich hierarchical porous carbon material.

[0033] The product was scanned by an electron microscope and identified as having a porous structure. Nitrogen adsorption-desorption proves that it contains hierarchical pore structure and pore distribution.

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Abstract

The invention belongs to the field of material preparation, and specifically relates to a preparation method for a nitrogen-rich hierarchical pore carbon material. The preparation method comprises the following steps of dissolving nitrogen-rich monomers and aldehydes into a solvent I and a solvent II respectively; uniformly dispersing and then mixing, adding a catalyst to adjust the pH value and the reacting temperature; reacting for 2-12h, repeatedly washing the product for 2-3 times by an elution solvent under a centrifuging or ultrasonic effect after the reaction is finished; and drying the product at a temperature of 40-80 DEG C to obtain a nitrogen-rich porous polymer material; and carbonizing the product obtained in the step 1) under the protection of an inert gas at a temperature of 600-1,200 DEG C for 3-8h to obtain the nitrogen-rich hierarchical pore carbon material. The carbon material prepared by the invention contains a large amount of nitrogen elements, and has a quite large specific surface area and a special porous structure; and the carbon material is 200-1,600m<2> / g in the specific surface area, 1-100nm in the pore diameter distribution, and 2-30% in the nitrogen content.

Description

technical field [0001] The invention belongs to the technical field of material preparation, in particular to a method for preparing a nitrogen-rich hierarchical porous carbon material. Background technique [0002] Because nitrogen-rich porous carbon materials retain a large amount of nitrogen and oxygen elements, the carbon materials are hydrophilic and can selectively adsorb polar compounds; moreover, the nitrogen-oxygen bonds distributed in the carbon materials have excellent redox catalytic activity; at the same time, the huge The specific surface area and special hierarchical pore structure make it have broad application prospects in the fields of supercapacitors, highly active oxygen reduction catalysts, adsorbents, and carbon dioxide capture and storage, and has attracted the attention of researchers at home and abroad. The synthesis of nitrogen-containing porous carbon materials is mostly obtained by using nitrogen-containing polymer resins under high-temperature ca...

Claims

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Application Information

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IPC IPC(8): H01M4/96C01B31/02
CPCC01P2004/03C01P2004/61H01M4/96Y02E60/50
Inventor 邹伟唐楷颜杰杨益祥苏桂萍那仁格日勒朱建民
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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