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Method for preparing hierarchical porous material based on rapid solvent evaporation in inverse microemulsion system

An inverse microemulsion, multi-level pore technology, applied in carbon preparation/purification, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of long and complex reaction process and high cost

Inactive Publication Date: 2020-03-27
CAPITAL NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problems of lengthy and complicated reaction process and high cost in the existing solvent evaporation method, and proposes a method for preparing hierarchical porous materials with low cost and greatly reduced reaction time

Method used

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  • Method for preparing hierarchical porous material based on rapid solvent evaporation in inverse microemulsion system
  • Method for preparing hierarchical porous material based on rapid solvent evaporation in inverse microemulsion system
  • Method for preparing hierarchical porous material based on rapid solvent evaporation in inverse microemulsion system

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Take 0.8g of tri-block surfactant polyether F127 and dissolve it in 8ml of methyl methacrylate. After F127 is completely dissolved, add 0.5ml of ethanol and 0.2ml of water drop by drop. The formation of water nuclei was observed in the methyl ester, and then continued to stir until the solution was completely dissolved and clarified, then added 0.246g of resorcinol and 0.204g of terephthalaldehyde as carbon source precursors, and after it was completely dissolved, added 0.0056g of carbonic acid Sodium is used as the catalyst of the reaction to adjust the pH value to 12, followed by stirring for 6 hours until the solution turns dark red, and the high-temperature solvent is evaporated at 120°C for 10 minutes to obtain a black solid product, which is passed through a tube furnace for 800 ℃ high temperature calcination to obtain the final carbon porous material.

Embodiment 2

[0031] Take 0.8g of tri-block surfactant polyether F127 and dissolve it in 8ml of methyl methacrylate. After F127 is completely dissolved, add 0.5ml of ethanol and 0.2ml of water drop by drop. The formation of water nuclei was observed in the methyl ester, and then the stirring was continued until the solution was completely dissolved and clarified, then 1.04 g of tetraethyl orthosilicate, 0.246 g of resorcinol and 0.204 g of terephthalaldehyde were added as precursors of silicon and carbon sources , after it is completely dissolved, add 0.0056g of sodium carbonate as a reaction catalyst to adjust the pH value to 12, then stir for 6 hours, evaporate the solvent at 130°C for 10 minutes to obtain a black solid product, and the solid product is in the tube After being calcined at a high temperature of 800°C in a furnace, the calcined product is corroded by a 5wt% HF solution to obtain the final silicon-carbon hierarchical porous material. Depend on Figure 7 It can be seen that ...

Embodiment 3

[0033] Take 0.8g of tri-block surfactant polyether F127 and dissolve it in 8ml of methyl methacrylate. After F127 is completely dissolved, add 0.5ml of ethanol and 0.2ml of water drop by drop. The formation of water nuclei was observed in the methyl ester, and then continued to stir until the solution was completely dissolved and clear, then added 8 mmmol of 1,4 (bistriethoxysilyl) benzene and 0.02 ml of concentrated HCl, adjusted the pH to 2, and stirred thoroughly for 12 hours Finally, the high-temperature solvent was evaporated at 140°C for 10 minutes, and the obtained white solid product was refluxed for 24 hours in a solution of concentrated HCl and ethanol with a volume ratio of 3.6:120 to obtain a silicon hierarchical porous material. Depend on Figure 8 It can be seen that the prepared silicon material is hierarchically porous.

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Abstract

The invention discloses a method for preparing a hierarchical porous material based on rapid solvent evaporation in an inverse microemulsion system. According to the method, resorcinol, phloroglucinoland terephthalaldehyde are adopted to replace common phenol and formaldehyde to synthesize phenolic resin such that the reaction time can be shortened; esters such as methyl methacrylate, triblock non-ionic surfactants such as polyether F127, F108 and P123 or ionic surfactants such as hexadecyl trimethyl ammonium bromide and the like are used for forming an inverse microemulsion as a reaction system, the hierarchical porous material can be obtained by directly evaporating a high-temperature solvent, the subsequent hydrothermal curing process is omitted, the reaction time can be greatly shortened, and the product obtained by using the inverse microemulsion system has an ordered mesoporous structure.

Description

technical field [0001] The invention belongs to the technical field of organic polymer preparation, and in particular relates to a method for preparing a hierarchical porous material based on rapid solvent evaporation in an inverse microemulsion system. Background technique [0002] At present, there are two main methods for preparing hierarchical porous carbons using amphiphilic triblock copolymers as soft templates and phenolic resins as carbon sources. One is the reaction in aqueous solution at 100 °C, and the other is evaporation-induced self-assembly in organic solvents. In comparison, the hydrothermal process is time-consuming and complicated, and the hydrothermal temperature and time are greater than 100°C and 48 hours, respectively. Therefore, the EISA method is currently one of the most commonly used methods for preparing hierarchical porous carbons because it is a fast and simple process that facilitates the formation of porous carbons only through the evaporation...

Claims

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Application Information

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IPC IPC(8): C01B32/05C01B33/021
CPCC01B33/021C01B32/05
Inventor 李伟侯晓健栾森郭赞武李文秀宋意
Owner CAPITAL NORMAL UNIVERSITY
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