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Microwave assisted method for rapidly synthesizing ordered mesoporous carbon

A microwave-assisted, mesoporous carbon technology, which is applied in the field of carbon nanomaterial preparation technology, can solve the problems of consuming a lot of time and energy, and not forming a system.

Inactive Publication Date: 2009-05-27
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the more common one-step template method currently adopts oven thermal polymerization (R.L.Liu Y.F.Shi, Y.Wan, et al. Triconstituent co-assembly to ordered mesostructured polymer-silica and carbon-silica nanocomposites and large-pore mesoporous carbons with high surface areas .J.Am.Chem.Soc., 2006, 128(35): 11652-11662.), this method is relatively mature, the disadvantage is that it consumes a lot of time and energy, and the research on this work has not yet formed a system, and it still needs to be studied Further improvement and development

Method used

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  • Microwave assisted method for rapidly synthesizing ordered mesoporous carbon
  • Microwave assisted method for rapidly synthesizing ordered mesoporous carbon
  • Microwave assisted method for rapidly synthesizing ordered mesoporous carbon

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Experimental program
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specific Embodiment 2

[0015] In the early stage of the experiment, phenol and formaldehyde were used to polymerize under alkaline conditions to obtain a low molecular weight (less than 500) resol resin precursor, which was formulated into a phenolic resin ethanol solution with a mass fraction of 20% for later use. Dissolve 1.0 g of template agent F127 in 10.0 g of absolute ethanol, add 1.0 g of 0.2 mol / L HCl solution dropwise, and stir at 40°C for 1 h to form a transparent solution. Slowly add 2.08g tetraethyl orthosilicate and 2.5g ethanol solution (20%) of phenolic resin dropwise, stir for 2h to make it evenly mixed. The mixture was transferred to a flat-bottomed Petri dish, and the solvent was evaporated at room temperature (25° C.) for 5-8 h to form a uniform film. Transfer to a microwave oven for microwave polymerization with a microwave power of 200W for 30 minutes. Carbonization was carried out in an atmosphere tube furnace with nitrogen gas flow. Incubate at 350°C for 5 hours, 500°C and 6...

specific Embodiment 3

[0017] In the early stage of the experiment, phenol and formaldehyde were used to polymerize under alkaline conditions to obtain a low molecular weight (less than 500) resol resin precursor, which was formulated into a phenolic resin ethanol solution with a mass fraction of 20% for later use. Dissolve 1.0 g of template agent F127 in 10.0 g of absolute ethanol, add 1.0 g of 0.2 mol / L HCl solution dropwise, and stir at 40°C for 1 h to form a transparent solution. Slowly add 2.08g tetraethyl orthosilicate and 2.5g ethanol solution (20%) of phenolic resin dropwise, stir for 2h to make it evenly mixed. The mixture was transferred to a flat-bottomed Petri dish, and the solvent was evaporated at room temperature (25° C.) for 5-8 h to form a uniform film. Transfer to a microwave oven for microwave polymerization with a microwave power of 600W for 60 minutes. Carbonization was carried out in an atmosphere tube furnace with nitrogen gas flow. Incubate at 350°C for 5 hours, at 500°C an...

specific Embodiment 4

[0019]Specific embodiment four (comparative examples):

[0020] (1) In the early stage of the experiment, phenol and formaldehyde were used to polymerize under alkaline conditions to obtain a low molecular weight (less than 500) resole resin precursor, and a phenolic resin ethanol solution with a mass fraction of 20% was prepared for future use. Dissolve 1.0 g of template agent F127 in 10.0 g of absolute ethanol, add 1.0 g of 0.2 mol / L HCl solution dropwise, and stir at 40°C for 1 h to form a transparent solution. Slowly add 2.08g tetraethyl orthosilicate and 2.5g ethanol solution (20%) of phenolic resin dropwise, stir for 2h to make it evenly mixed. The mixture was transferred to a flat-bottomed Petri dish, and the solvent was evaporated at room temperature (25° C.) for 5-8 h to form a uniform film. Put it into a vacuum oven for thermal polymerization at 100°C for 24 hours, and carbonize it in an atmosphere tube furnace with nitrogen flow. Insulate at 350°C for 5 hours, at ...

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Abstract

The invention discloses a method for microwave-assisted rapid synthesis of ordered mesoporous carbon, which belongs to a preparation process of a nanometer carbon material. The method comprises the following steps: a surfactant F127, a phenolic resin and ethyl orthosilicate are mixed evenly; a uniform transparent solution is formed in acid medium by heating and stirring, and is transferred into an evaporating dish to form a thin film; the microwave is utilized to heat and polymerize, the power is between 200 and 600W, and the time is between 30 and 60min; and the high-temperature carbonization is performed under the protection of nitrogen or argon. The utilization of the method can improve the preparation efficiency of the ordered mesoporous carbon and obtain excellent structural performance at the same time.

Description

technical field [0001] The invention relates to the rapid synthesis of ordered mesoporous carbon by using microwave energy, which belongs to the preparation process of carbon nanomaterials. technical background [0002] Mesoporous materials have high pore volume storage and excellent surface condensation properties. They have important application prospects in the fields of shape-selective separation, high-efficiency catalysis, sensing, and optics, electricity, and magnetism. The research and development of ordered mesoporous carbon has greatly enriched the synthesis methods and types of porous carbon materials, broadened the application fields, provided and established new catalyst support materials, energy storage materials and adsorption materials, etc. In addition to the broad application prospects of mesoporous carbon itself, mesoporous carbon materials can be used as catalyst supports and have a wide range of applications. After loading metal nanoparticles (such as Pt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/08
Inventor 何建平狄志勇王道军周建华王涛孙盾
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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