Method for preparing transition metal doped mesoporous carbon material

A transition metal and mesoporous carbon technology, applied in the field of mesoporous carbon materials, achieves the effects of simple method, reduced preparation cost and wide application range

Inactive Publication Date: 2009-12-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above-mentioned methods prepare pure carbon materials. If they are to be used in catalysis and other fields, the pure carbon materials need to be modified or compounded with other active components.

Method used

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  • Method for preparing transition metal doped mesoporous carbon material
  • Method for preparing transition metal doped mesoporous carbon material
  • Method for preparing transition metal doped mesoporous carbon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Phenol (65 grams) and molybdic acid (5 grams) were placed in the beaker, stirred and heated up to 60 ° C, reacted at this temperature for 0.5 hours, added (46 grams) 37% (567 mmol) formaldehyde solution and catalyst oxalic acid 1 g. Continue to stir, reflux for 2 hours, add distilled water, wash away the unreacted reactants, remove the water layer, and distill the remaining water at 150°C under reduced pressure to remove the residual water, discharge the material, and obtain a dark green solid after cooling. The phenolic resin is soluble in ethanol and acetone and is purple in color.

[0042] Get above-mentioned molybdenum-doped phenolic resin 4 grams and be dissolved in 20 milliliters of ethanols, templating agent (triblock polymer Pluronic F127, EO 106 PO 70 EO 106 ) 5 grams were dissolved in 110 milliliters of ethanol, mixed at room temperature, stirred for 2 hours, added 0.92 grams of curing agent hexamethylenetetramine, continued to stir for 24 hours, and static...

Embodiment 2

[0044] Phenol (65 g) and tungstic acid (7.75 g) were placed in a beaker, stirred and heated to 70° C., after reacting at this temperature for 3 hours, added (46 g) 37% (567 mmol) formaldehyde solution and 1 g oxalic acid. Continue to stir, reflux for 1.5 hours, add distilled water, wash away the unreacted reactants, remove the water layer, and distill the remaining water at 150°C under reduced pressure to remove the residual water, discharge the material, and obtain a yellow-green solid after cooling. The phenolic resin is soluble in ethanol and acetone.

[0045] Dissolve 4 grams of the above-mentioned metal-doped phenolic resin in 20 milliliters of ethanol, dissolve 5 grams of template agent triblock polymer Pluronic F127 in 110 milliliters of ethanol, mix at room temperature, stir for 3 hours, add 0.92 grams of curing agent, and continue stirring After 72 hours, the solvent was evaporated to obtain a polymer monolith. After curing, the template agent is removed by firing a...

Embodiment 3

[0047] Phenol (65 grams) and zirconium oxychloride (5.5 grams) were placed in the beaker, stirred and heated up to a certain temperature of 50 ° C, after reacting at this temperature for 0.5 hours, added (46 grams) of 37% (567 mmol) formaldehyde aqueous solution and 1 g of oxalic acid. Continue to stir, reflux for 2.5 hours, add distilled water, wash away the unreacted reactants, remove the water layer, remove the remaining water under reduced pressure at 150°C, discharge the material, and obtain an orange solid after cooling. The phenolic resin is soluble in ethanol and acetone.

[0048] Dissolve 4 grams of the above-mentioned metal-doped phenolic resin in 25 milliliters of ethanol, dissolve the three-block polymer Pluronic F127 (5 grams) of template agent in 110 milliliters of ethanol, mix at room temperature for 3 hours, add 0.92 grams of curing agent, and continue stirring After 24 hours, the solvent was evaporated to obtain a polymer monolith. After curing, the template...

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Abstract

The invention belongs to a mesoporous carbon material, and particularly relates to a method for preparing a transition metal doped mesoporous carbon material with high specific surface area. The method takes a transition metal doped polymer as a carbonization precursor, takes a block polymer as a pore former, and utilizes a supramolecular self-assembly structure formed by the carbonization precursor and the pore former in a volatile solvent to cure at certain temperature in the existence of a curing agent to form a transition metal doped polymer meso-structure. A transition metal doped mesoporous polymer material can be prepared by roasting to remove the pore former under inert atmosphere. The prepared transition metal doped mesoporous polymer material is subjected to high-temperature carburization in the inert atmosphere to obtain the transition metal doped mesoporous carbon material.

Description

technical field [0001] The invention relates to a mesoporous carbon material, in particular to a preparation method of a transition metal-doped mesoporous carbon material with a high specific surface area. Background technique [0002] In 1992, Mobil Corporation reported the M41S series of mesoporous silicon materials with regular channels. Extending the regular pore size of molecular sieves from micropores to mesoporous range greatly expands the application of porous materials, and at the same time injects new vitality into the development of material science. Ryoo and Hyeon et al. successfully used mesoporous silica (aluminum) materials as templates to successfully prepare mesoporous carbon materials SUN-1 and CMK-1 respectively. Since then, ordered mesoporous carbon materials with different structures have come out one after another, using mesoporous silicon with different structures as templates. In recent years, ordered mesoporous carbon materials have shown many exce...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 包信和王春雷马丁
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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