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Nitrogen-doped ordered mesoporous carbon material and preparation method thereof

A mesoporous carbon and nitrogen doping technology, applied in the field of mesoporous materials, can solve the problems of high price, high nitrogen source corrosiveness, high catalyst cost, etc., and achieve the effects of low price and simple operation method.

Inactive Publication Date: 2017-06-23
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the past, roasting was carried out in a vacuum furnace, which inevitably increased the cost of equipment
In addition, ammonia (Applied Surface Science 393 (2017) 144-150), concentrated nitric acid (Applied Catalysis B: Environmental 147 (2014) 633-641), pyrrole (Nanoscale, 8 (2016) 19086 -19092) or phthalocyanine (Journal of Power Sources 293 (2015) 511-518; Journal of Power Sources 264 (2014) 114-122) as nitrogen precursors, these nitrogen sources are either highly corrosive, or expensive, and the source Rare, although the synthesized nitrogen-containing mesoporous carbon materials can be used in fuel cells, the high catalyst cost is not conducive to its large-scale application

Method used

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  • Nitrogen-doped ordered mesoporous carbon material and preparation method thereof
  • Nitrogen-doped ordered mesoporous carbon material and preparation method thereof

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Effect test

Embodiment 1

[0026] Preparation of a nitrogen-doped ordered mesoporous carbon material N2-OMC in this embodiment (2 is the mass ratio of melamine and OMC):

[0027] Weigh 0.14g of concentrated sulfuric acid, 1.25g of sucrose and 5g of deionized water, mix well and add 1g of SBA-15 silicon-based solid to obtain a milky white suspension, then place the milky white suspension in a blast drying oven and dry at 90°C After 7 hours, the temperature was raised to 160°C for carbonization for 6 hours. The brown solid was taken out and ground into powder, and 0.09 g of concentrated sulfuric acid, 0.8 g of sucrose and 5 g of deionized water were added thereto, and the above drying and carbonization operations were repeated. The carbonized product was heated to 900° C. in a tube furnace under nitrogen atmosphere for 5 hours of high-temperature calcination. Then, the template agent SBA-15 was removed by heating under reflux with an ethanol aqueous solution containing 2mol / L NaOH (ethanol:water=1:1, vol...

Embodiment 2

[0031] Preparation of a nitrogen-doped ordered mesoporous carbon material N5-OMC in this embodiment (5 is the mass ratio of melamine and OMC):

[0032] Weigh 0.14g of concentrated sulfuric acid, 1.25g of sucrose and 5g of deionized water, mix well and add 1g of SBA-15 silicon-based solid to obtain a milky white suspension, then place the milky white suspension in a blast drying oven and dry at 100°C After 6 hours, the temperature was raised to 170°C for carbonization for 5 hours. The brown solid was taken out and ground into powder, and 0.09 g of concentrated sulfuric acid, 0.8 g of sucrose and 5 g of deionized water were added thereto, and the above drying and carbonization operations were repeated. The carbonized product was heated to 1000° C. in a tube furnace under nitrogen atmosphere for 3 hours of high-temperature calcination. Then, the template agent SBA-15 was removed by heating under reflux with an ethanol aqueous solution containing 2mol / L NaOH (ethanol:water=1:1, v...

Embodiment 3

[0036] Preparation of a nitrogen-doped ordered mesoporous carbon material N10-OMC in this embodiment (10 is the mass ratio of melamine and OMC):

[0037] Weigh 0.14g of concentrated sulfuric acid, 1.25g of sucrose and 5g of deionized water, mix well and add 1g of SBA-15 silicon-based solid to obtain a milky white suspension, then place the milky white suspension in a blast drying oven and dry at 100°C After 7 hours, the temperature was raised to 150°C for carbonization for 8 hours. The brown solid was taken out and ground into powder, and 0.09 g of concentrated sulfuric acid, 0.8 g of sucrose and 5 g of deionized water were added thereto, and the above drying and carbonization operations were repeated. The carbonized product was heated to 900° C. in a tube furnace under nitrogen atmosphere for 4 hours of high-temperature calcination. Then, the template agent SBA-15 was removed by heating under reflux with 1 mol / L NaOH aqueous ethanol solution (ethanol:water=1:1, volume ratio)...

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Abstract

The invention belongs to the field of mesoporous materials and discloses a nitrogen-doped ordered mesoporous carbon material and a preparation method thereof. The preparation method comprises the following steps: after uniformly mixing concentrated sulfuric acid, saccharose and deionized water, adding a silicon-based mesoporous material SBA-15 to obtain a milk white suspended liquid A; drying A at 90-100 DEG C, and then raising the temperature to 150-170 DEG C to be carbonized to obtain a solid B; grinding the solid B into powder and then adding concentrated sulfuric acid, saccharose and deionized water to be uniformly mixed, repeating the drying and carbonizing processes, and then roasting the mixture at 900-1000 DEG C to obtain a solid C; and removing a SBA-15 template from the solid C to obtain ordered mesoporous carbon, and then uniformly grinding and mixing the carbon with a nitrogen source, and roasting the mixture for 3-6 hours at 900-1000 DEG C to obtain a product. The method provided by the invention not only can avoid roasting in a vacuum condition, but also can effectively simplify the operating process and greatly lower the preparation cost of the material.

Description

technical field [0001] The invention belongs to the field of mesoporous materials, in particular to a nitrogen-doped ordered mesoporous carbon material and a preparation method thereof. Background technique [0002] Ordered mesoporous carbon (OMC) has been widely used in the research of oxygen reduction reaction catalysts as a new type of conductive support. OMC supports have the advantages of high surface area, large pore volume, concentrated pore size distribution and good pore stability, which are conducive to the molecular transfer of reactants and products, and can effectively improve the electrochemical catalytic activity in the application of fuel cells. In addition, with the deepening of the understanding of non-metallic heteroatoms, some non-metallic elements, such as nitrogen, boron, phosphorus and fluorine, are doped into the mesoporous channels of OMC, and many non-metallic heteroatom doping emerge as the times require. Carbon materials have been expected to rep...

Claims

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Application Information

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IPC IPC(8): C01B32/05
CPCC01P2004/04C01P2006/12C01P2006/14C01P2006/17
Inventor 王秀军黄伟豪何珍珍李白滔
Owner SOUTH CHINA UNIV OF TECH
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