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Method for preparing nitrogen-doped porous carbon material by two-step method and application thereof

A nitrogen-doped porous carbon and two-step technology, which is applied in the field of hydrogen storage materials and new energy materials, can solve the problems of large mesopores and achieve the effects of increased low-temperature hydrogen storage, good reversible adsorption performance, and stability maintenance

Inactive Publication Date: 2009-09-16
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Recently, the preparation of porous carbon or carbon-nitrogen materials by the template method has attracted widespread attention, but the porous materials synthesized by the single-step method contain a certain amount of micropores, and there are also a large number of relatively large mesopores.

Method used

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  • Method for preparing nitrogen-doped porous carbon material by two-step method and application thereof
  • Method for preparing nitrogen-doped porous carbon material by two-step method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Using molecular sieve 13X as a template, nitrogen-doped porous carbon was prepared by template carbonization by introducing carbon or carbon-nitrogen precursors through a two-step method, using furfuryl alcohol and acetonitrile as carbon or carbon-nitrogen precursors for liquid impregnation and vapor deposition, respectively. The specific surface area of ​​the 13X used is 674m 2 / g, the pore volume is 0.32cm 3 / g. First weigh 4g 13X and immerse it into a solution consisting of 1.5ml furfuryl alcohol, 10ml absolute ethanol and 0.01g oxalic acid, stir at room temperature for 4h to fully mix, then heat at 60°C and 80°C for 16h, respectively, to obtain The yellow-brown solid powder was put into a tube furnace, and then heated at 150 °C under N 2 Heating under the atmosphere for 3h to complete the pre-polymerization of furfuryl alcohol, then the temperature was raised to 700 ° C, followed by 70cm 3 N / min 2 Pass acetonitrile gas into the gas carrier, and heat for 4 hours ...

Embodiment 2

[0021] The method of this example is basically the same as that of Example 1, except that the temperature is raised to 700° C., and then heated for 8 hours under an acetonitrile atmosphere to complete the carbonization of furfuryl alcohol and the deposition of acetonitrile. Figure 1 shows the transmission electron microscope picture of the nitrogen-doped porous carbon material, and the ordered micropore structure can be seen. Figure 2 shows the change of the hydrogen absorption capacity of the nitrogen-doped porous material under different pressures, and it can be seen that the hydrogen absorption capacity increases as the pressure increases. Figure 3 shows the hydrogen absorption and dehydrogenation changes of the nitrogen-doped porous material under different pressures. It can be seen that the entire adsorption process is reversible and can quickly reach the equilibrium of adsorption and desorption. Figure 4 shows the variation of the specific capacitance of the electrode ma...

Embodiment 3

[0023] The method of this example is basically the same as that of Example 1, except that 4g of 13X is immersed in a solution consisting of 3.0ml of furfuryl alcohol, 10ml of absolute ethanol and 0.02g of oxalic acid. The specific test results of the electrode material can be obtained from FIG. 4 and Table 2.

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Abstract

The invention relates to a method for preparing a nitrogen-doped porous carbon material by a two-step method and application thereof, and belongs to the field of hydrogen storage materials and new energy materials. The nitrogen-doped porous carbon material is prepared by adopting a template carbonization method, which comprises that: firstly, a microporous molecular sieve such as ZSM-5, 3A, 5A, 13X, Y, beta and the like is used as a template, and then nitrogen-doped porous carbon material is prepared by adopting the two-step method combining liquid-phase impregnation and chemical precipitation. The liquid-phase impregnation uses sucrose, furfuryl alcohol, polyacrylonitrile and the like as a carbon or carbon-nitrogen precursor which is impregnated in the template, and the chemical precipitation comprises that propylene, acetonitrile, phenyl ethylene, methylbenzene and the like are precipitated on the template by a CVD method in turn. And then, nitrogen-doped porous carbon is further obtained through the process steps such as high temperature carbonization, template removal and the like. The nitrogen-doped porous carbon material with different structures can be obtained by controlling process conditions. The nitrogen-doped porous carbon material prepared by the method has the advantages of high specific surface area, large pore volume, narrow aperture distribution and adjustable pore structure, and can be used for the hydrogen storage materials and super-capacitor electrode materials.

Description

technical field [0001] The invention belongs to the field of hydrogen storage materials and new energy materials, and provides a two-step method for preparing nitrogen-doped porous carbon materials and its application in hydrogen storage materials and supercapacitor electrode materials. Background technique [0002] Porous carbonaceous materials have attracted a lot of attention due to their low density, high specific surface area, good chemical stability, good electrical conductivity, controllable pore structure, and undemanding application conditions. They have become hydrogen storage materials and supercapacitor electrodes. One of the important objects of material research. [0003] In the field of hydrogen storage materials, because the storage of porous materials utilizes the physical adsorption of hydrogen molecules, this porous material can achieve large mass storage in a small volume. Theoretically, the higher the specific surface area of ​​carbon materials, the gre...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 高秋明王焕磊
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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