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

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Problems solved by technology

However, in the synthesis process, the metal precursor and the mesoporous nitrogen carbide mater

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
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Example Embodiment

[0025] Example 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 under reflux at 60°C for 4h, dry overnight, and then put it in a quartz tube, and at 600°C and 40ml / min pure Heating in nitrogen atmosphere for 2 hours to carbonize the material to obtain brown-black powder; stir the obtained brown-black powder with 50 mL of 25% hydrofluoric acid solution for 3 hours, wash with deionized water and ethanol several times, and dry to obtain the obtained The ordered mesoporous nitrogen carbide materials are described.

[0028] b. Preparation of alkylated halide ion compounds

[0029] Take 0.5 g of ordered mesoporous carbon nitride material, dissolve it in 100 mL of DMF solution, add 5.6 g of methyl iodide, heat under reflux for 0.5 h at 100 °C, and filter with suction. The obtained solids are washed with distilled water and acetone, respectively, a...

Example Embodiment

[0034] Example 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 under reflux at 100°C for 4h, dry overnight, and then put it in a quartz tube, and at 300°C and 40ml / min pure Heating in a nitrogen atmosphere for 4 hours to carbonize the material to obtain brown-black powder; stir the obtained brown-black powder with 50 mL of 25% hydrofluoric acid solution for 4 hours, wash with deionized water and ethanol several times, and dry to obtain the The ordered mesoporous nitrogen carbide materials are described.

[0037] b. Preparation of alkylated halide ion compounds

[0038] Take 0.5 g of ordered mesoporous carbon nitride material, dissolve it in 100 mL of DMF solution, then add 14 g of methyl iodide, heat under reflux at 90°C for 5 hours, and filter with suction. The obtained solids are washed with distilled water and acetone respectively. The...

Example Embodiment

[0043] Example 3

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

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

[0046] b. Preparation of alkylated halide ion compounds

[0047] Take 0.5 g of ordered mesoporous carbon nitride material, dissolve it in 100 mL of DMF solution, then add 7 g of methyl iodide, heat under reflux at 120 ° C for 10 hours, suction filtration, and the obtained solids are washed with distilled water and acetone respectively. Then dr...

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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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