Preparation method of foaming ordered mesoporous carbon integral material with graded tunnel structure

A monolithic material and foam-like technology, which is applied in the field of preparation of foam-like ordered mesoporous carbon monolithic materials with hierarchical pore structure, can solve the problem of uneven distribution of carbon sources, difficulty in controlling the shape and size of bulk silicon templates, and large size of residual solvents. cracks and other problems, to achieve the effect of easy operation, easy amplification, and easy parameters

Inactive Publication Date: 2011-11-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has been studied more, however, compared with the use of powder templates, bulk templates have many shortcomings: for example, during the preparation of ordered mesoporous silicon templates, the removal of residual solvents is always accompanied by serious problems. Shrinkage produces large-sized cracks and the shape and size of bulk silicon templates are difficult to control.
Meanwhile, in order to avoid damaging the bulk templates, the impregnation process needs to be carried out without stirring, which may lead to uneven carbon source distribution.

Method used

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  • Preparation method of foaming ordered mesoporous carbon integral material with graded tunnel structure
  • Preparation method of foaming ordered mesoporous carbon integral material with graded tunnel structure
  • Preparation method of foaming ordered mesoporous carbon integral material with graded tunnel structure

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Prepare a furfuryl alcohol solution with a mass concentration of 0.05 oxalic acid; prepare a suspension according to the weight ratio of the powdered ordered mesoporous silicon material SBA-15 to the furfuryl alcohol solution of oxalic acid at a weight ratio of 1:10, and stir the suspension for 1 hour; Immerse the fat foam in the obtained suspension for 10 minutes, squeeze out the excess suspension; polymerize and solidify at 180°C for 5 hours to obtain a composite foam, place the above composite foam in a nitrogen atmosphere, and heat it at 0.01°C·min -1 The temperature is raised to 700° C. for carbonization treatment for 1 hour to obtain a composite material of foamy ordered mesoporous silicon material and carbon. The composite material was soaked in 48% hydrofluoric acid for 24 hours, washed until neutral, and dried to obtain a foamy ordered mesoporous carbon monolith.

[0021] The resulting foamy ordered mesoporous carbon monolith has a macropore diameter of 500 mic...

Embodiment 2

[0023] Prepare a furfuryl alcohol solution with a mass concentration of 0.1 oxalic acid; prepare a suspension according to the weight ratio of the powdered ordered mesoporous silicon material SBA-15 to the furfuryl alcohol solution of oxalic acid at a weight ratio of 1:6, and stir the suspension for 10 hours; Immerse the fat foam in the obtained suspension for 2 minutes, squeeze out the excess suspension; polymerize and solidify at 80°C for 1 hour to obtain a composite foam, place the above composite foam in a nitrogen atmosphere, and heat at 2°C·min -1 The temperature is raised to 700° C. for carbonization treatment for 1 hour to obtain a composite material of foamy ordered mesoporous silicon material and carbon. The composite material was soaked in 48% hydrofluoric acid for 24 hours, washed until neutral, and dried to obtain a foamy ordered mesoporous carbon monolith.

[0024] The resulting foamy ordered mesoporous carbon monolith has a macropore diameter of 500 microns and ...

Embodiment 3

[0026] Prepare a furfuryl alcohol solution with a mass concentration of 0.05 oxalic acid; prepare a suspension according to the weight ratio of the powdered ordered mesoporous silicon material SBA-15 to the furfuryl alcohol solution of oxalic acid at a weight ratio of 1:8, and stir the suspension for 4 hours; the phenolic resin used as the template Immerse the foam in the obtained suspension for 2 minutes, squeeze out the excess suspension; polymerize and solidify at 80°C for 1 hour to obtain a composite foam, place the above composite foam in a nitrogen atmosphere, -1 The temperature was raised to 900° C. for carbonization treatment for 1 hour to obtain a composite material of foamy ordered mesoporous silicon material and carbon. The composite material was soaked in 48% hydrofluoric acid for 24 hours, washed until neutral, and dried to obtain a foamy ordered mesoporous carbon monolith.

[0027] The resulting foamy ordered mesoporous carbon monolith has a macropore diameter of...

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Abstract

A preparation method of a foaming ordered mesoporous carbon integral material with a graded tunnel structure belongs to the technical field of inorganic nonmetal carbon material. According to the invention, a powdered ordered mesoporous silicon material is used as a template, and furfuryl alcohol is used as a carbon source; the carbon source is introduced into a tunnel of the ordered mesoporous silicon material, treated with thermalpolymerization under catalysis of oxalic acid and charred into a silicon carbon composite material; and silicon template is washed out by hydrofluoric acid, so as to obtain the foaming ordered mesoporous carbon integral material. The integral material with a graded tunnel structure has a highly open macroporous cell structure, an ordered and even-size mesoporous structure; and a pore structure, density and intensity of the foaming integral composite material can be easily adjusted. A preparation process is simple; equipment requirement is not high; parameters are easily to control; operations are easy and are apt to be amplified. The material can be applied to fields of absorption material, cell substrate and fixed bed filling material, etc.

Description

technical field [0001] The invention relates to a method for preparing a foamy ordered mesoporous carbon monolithic material with hierarchical pore structure, and belongs to the scientific and technical field of carbon materials, a branch of inorganic non-metallic material science and technology. Background technique [0002] Ordered mesoporous carbon is a new type of carbon material with a three-dimensional nanostructure. It has a wide range of applications in many fields such as separation and electrochemistry, so it has attracted people's attention. So far, the research work on ordered mesoporous carbons has mostly focused on the synthesis of new three-dimensional ordered structures and the control of pore size. The monolithic multi-level pore structure is considered to have a wide range of applications in fields such as monolithic high-performance liquid chromatography because of its faster mass and heat transfer rates. [0003] The overall structurally ordered mesopor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/02
Inventor 邱介山肖南周颖凌铮赵宗彬
Owner DALIAN UNIV OF TECH
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