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Preparation method of mesoporous carbon nitride loaded precious nano particle

A technology of mesoporous carbonized nitrogen and nano-particles, which is applied in the field of materials-related preparation methods, can solve the problems of mesoporous materials, weak force, and easy falling off of metal precursors, and achieve good catalytic effects and save raw materials.

Inactive Publication Date: 2013-02-13
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the synthesis process, the metal precursor and the mesoporous nitrogen carbide material are only combined by electrostatic attraction. Porous materials present certain difficulties

Method used

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  • Preparation method of mesoporous carbon nitride loaded precious nano particle
  • Preparation method of mesoporous carbon nitride loaded precious nano particle
  • Preparation method of mesoporous carbon nitride loaded precious nano particle

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] a. Synthesis of ordered mesoporous nitrogen carbide materials

[0027] Mix 1g of SBA-15, 6g of carbon tetrachloride, and 2.7g of ethylenediamine in a certain proportion, heat and reflux at 60°C for 4h, dry overnight, then place it in a quartz tube, and purify at 600°C and 40ml / min Heating in a nitrogen atmosphere, keeping the material for 2 hours to carbonize the material, and obtaining a brown-black powder; stirring the obtained brown-black powder with 50 mL of 25% hydrofluoric acid solution for 3 hours, washing with deionized water and ethanol several times, and drying to obtain the obtained Ordered mesoporous nitrogen carbide materials.

[0028] b, the preparation of alkylated halide ion compound

[0029] Take 0.5g of ordered mesoporous nitrogen carbide material, dissolve it in 100mL of DMF solution, then add 5.6g of methyl iodide, heat to reflux at 100°C for 0.5h, filter with suction, wash the obtained solid with distilled water and acetone, and then dry it.

[00...

Embodiment 2

[0035] a. Synthesis of ordered mesoporous nitrogen carbide materials

[0036] Mix 1g of SBA-15, 6g of carbon tetrachloride, and 2.7g of ethylenediamine in a certain proportion, heat and reflux at 100°C for 4 hours, dry overnight, then place it in a quartz tube, and purify at 300°C and 40ml / min Heating in a nitrogen atmosphere, keeping the material for 4 hours to carbonize the material, and obtaining a brown-black powder; stirring the resulting brown-black powder with 50 mL of 25% hydrofluoric acid solution for 4 hours, washing with deionized water and ethanol several times, and drying to obtain the obtained Ordered mesoporous nitrogen carbide materials.

[0037] b, the preparation of alkylated halide ion compounds

[0038] Take 0.5g of ordered mesoporous nitrogen carbide material, dissolve it in 100mL of DMF solution, then add 14g of methyl iodide, heat and reflux at 90°C for 5 hours, filter with suction, and wash the obtained solid with distilled water and acetone respective...

Embodiment 3

[0044] a. Synthesis of ordered mesoporous nitrogen carbide materials

[0045] Mix 2g of SBA-15, 12g of carbon tetrachloride, and 5.4g of ethylenediamine in a certain proportion, heat and reflux at 100°C for 3 hours, dry overnight, then place it in a quartz tube, and heat it under 500°C and 40ml / min of pure nitrogen Heating in the atmosphere, keeping the material for 4 hours to carbonize the material, and obtaining a brown-black powder; stirring the obtained brown-black powder with 100 mL of 25% hydrofluoric acid solution for 10 h, washing with deionized water and ethanol several times, and drying to obtain the described Ordered mesoporous nitrogen carbide materials.

[0046] b, the preparation of alkylated halide ion compounds

[0047] Take 0.5g of ordered mesoporous nitrogen carbide material, dissolve it in 100mL of DMF solution, then add 7g of methyl iodide, heat and reflux at 120°C for 10 hours, filter with suction, and wash the obtained solid with distilled water and aceton...

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Abstract

The invention discloses a preparation method of a mesoporous carbon nitride loaded precious nano particle, which comprises the steps of: with mesoporous silica as a hard template, preparing a mesoporous nitrogen-doped carbon material by using a nano pouring method; then carrying out alkylation reaction by using halohydrocarbon to ensure that the nitrogen-doped carbon surface is subjected to quaternization; enabling an anion group with precious metals to replace a halide ion by means of an ion exchange method, binding on the surface of the material; and finally reducing metal ions by using a reducing agent, and preparing the mesoporous carbon nitride loaded precious nano particle. According to the method, a precious metal particle precursor and a mesoporous material are tightly combined by means of an ion bond, and the precious metal particle is well dispersed on the ordered mesoporous material to form a precious metal / nitrogen carbon compound material. The mesoporous carbon nitride loaded precious nano particle has the activity of the precious nano particle and is high in specific area and large in hole volume of a mesoporous molecular sieve. The mesoporous carbon nitride loaded precious nano particle has excellent catalysis activity and catalysis stability for cathode oxygen reduction of a fuel cell, and has a potential commercial application prospect.

Description

technical field [0001] The invention relates to a preparation method of the material. Specifically, mesoporous silicon oxide is used as a hard template to prepare a mesoporous carbonized nitrogen material through a nano-casting method, and then the surface of the carbonized nitrogen is quaternized by means of an alkylation reaction using a halogenated hydrocarbon. The way of ion exchange is to make anion groups with noble metals replace halide ions, bind them on the surface of the material, and finally reduce the metal ions with a reducing agent to prepare a method for mesoporous nitrogen carbide-loaded noble metal nanoparticle materials. Background technique [0002] Due to its unique physical and chemical properties, metal particles have attracted extensive attention in the fields of catalysis, separation, magnetism, optoelectronics and microelectronics. The special properties of these metallic particles depend on their size, shape, crystal structure and organizational par...

Claims

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Application Information

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IPC IPC(8): H01M4/88
CPCY02E60/50
Inventor 单永奎孔莹莹孔爱国余友谊张永博韩振董冰
Owner EAST CHINA NORMAL UNIVERSITY
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