Surface functionalized ordered mesopore nitrogen-doped carbon material and preparation method thereof

A surface functionalization and mesoporous technology, which is applied in the field of preparation of ordered mesoporous nitrogen-doped carbon materials, can solve the problems of low specific surface area and porosity, restricting applications, affecting the self-assembly process of carbon source and soft template, etc. The method is simple, the interaction is improved, and the effect of large application value

Active Publication Date: 2014-10-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the carbon materials obtained by the direct hydrothermal method only have a very low specific surface area and porosity, which limits the application of this type of carbon materials in adsorption separation, catalysis, energy storage / conversion, drug loading, etc.
In addition, the hydrothermal process involves many reactions such as hydrolysis and degradation, which affect the self-assembly process of carbon sources and soft templates.

Method used

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  • Surface functionalized ordered mesopore nitrogen-doped carbon material and preparation method thereof
  • Surface functionalized ordered mesopore nitrogen-doped carbon material and preparation method thereof
  • Surface functionalized ordered mesopore nitrogen-doped carbon material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1: Take melamine sulfate as precursor

[0040]Add 50mL of 0.2M sulfuric acid and 6g of F127 into a 100mL beaker, stir to dissolve. The mixed solution was transferred to a three-necked flask containing 1.26 g (0.01 mol) of melamine, and stirred and refluxed at 92° C. for 24 h. Add 5.4g (0.03mol) of fructose and continue to reflux for 10min. The obtained solution was transferred to a reaction kettle, placed in an oven at 130°C, and reacted for 3d. After the reaction, the product is suction filtered, washed with distilled water several times, and dried to obtain the corresponding carbon material. Then the material is calcined by the above two-step method (the specific steps of the two-step method are: the dried hydrothermal product is first calcined in air at 400°C for 2h to remove the soft template, and then calcined at 900°C for 1h) to obtain ordered mesoporous nitrogen-doped carbon material.

[0041] The scanning electron micrographs of the ordered mesopo...

Embodiment 2

[0050] Embodiment 2: Taking melamine phosphate as a precursor

[0051] Add 50mL of 0.2M phosphoric acid and 6g of F127 into a 100mL beaker, stir to dissolve. The mixed solution was transferred to a three-necked flask containing 1.26 g (0.01 mol) of melamine, and stirred and refluxed at 92° C. for 24 h. Add 5.4g (0.03mol) of fructose and continue to reflux for 10min. The obtained solution was transferred to a reaction kettle, placed in an oven at 130°C, and reacted for 3d. After the reaction, the product is suction filtered, washed with distilled water several times, and dried to obtain the corresponding carbon material. Then the material was calcined by the above-mentioned two-step method (same as Example 1) to obtain an ordered mesoporous nitrogen-doped carbon material. Its scanning electron microscope image (SEM) is shown in Figure 7(a), and its transmission electron microscope image (TEM) is shown in Figure 7(b).

Embodiment 3

[0052] Embodiment 3: Taking melamine oxalate as a precursor

[0053] Add 50mL of 0.1M oxalic acid and 6g of F127 into a 100mL beaker, stir to dissolve. The mixed solution was transferred to a three-necked flask containing 1.26 g (0.01 mol) of melamine, and stirred and refluxed at 92° C. for 24 h. Add 5.4g (0.03mol) of fructose and continue to reflux for 10min. The obtained solution was transferred to a reaction kettle, placed in an oven at 130°C, and reacted for 3d. After the reaction, the product is suction filtered, washed with distilled water several times, and dried to obtain the corresponding carbon material. Then the material was calcined by the above-mentioned two-step method (same as Example 1) to obtain an ordered mesoporous nitrogen-doped carbon material. Its scanning electron microscope image (SEM) is shown in Figure 8(a), and its transmission electron microscope image (TEM) is shown in Figure 8(b).

[0054] The ordered mesoporous nitrogen-doped carbon material ...

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Abstract

The invention discloses a preparation method of a surface functionalized ordered mesopore nitrogen-doped carbon material. The preparation method of the surface functionalized ordered mesopore nitrogen-doped carbon material comprises the following steps: dissolving a carbohydrate raw material in a melamine salt aqueous dispersion system, carrying out hydrothermal reaction at the temperature of 120-200 DEG C while an amphiphilic triblock copolymer is taken as a soft template, filtering, washing and drying hydrothermal reaction products to obtain a porous carbon material, and carrying out high-temperature calcination to obtain a carbohydrate derived ordered mesopore nitrogen-doped carbon material. The invention also discloses a surface functionalized ordered mesopore nitrogen-doped carbon material product obtained by adopting the preparation method. The preparation method of the surface functionalized ordered mesopore nitrogen-doped carbon material has the advantages that a self-assembly process of the carbohydrate and the soft template is completed on the surface of an indissolvable organic salt precursor, the precursor can be copolymerized with a carbon source, so that a carbonized material is automatically transformed, and interaction between the carbohydrate and the soft template is improved, so that large-scale preparation of ordered mesopore and functionalized carbon materials by virtue of the carbohydrate can come true.

Description

technical field [0001] The invention belongs to the technical field of porous material preparation, and in particular relates to a preparation method and product of a surface-functionalized ordered mesoporous nitrogen-doped carbon material. Background technique [0002] With the discovery of new carbon materials such as fullerenes, carbon nanotubes and graphene, scientists are increasingly aware of the important role of carbon materials in scientific development and human progress. In addition to the high thermal conductivity and chemical stability of general carbon materials, ordered mesoporous carbon materials also have appropriate pore diameters (2-50nm), ordered pore tunnels, large specific surface area and porosity, It is beneficial to the adsorption and transport of substances, and is widely used in many fields such as adsorption separation, catalysis, energy storage / conversion, and drug loading. [0003] Through the efforts of scientists for many years, two methods o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 王勇王世萍韩传龙王静朱明蕾
Owner ZHEJIANG UNIV
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