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Method for preparing ordered mesoporous hollow silica spheres

A technology of mesoporous silica and silica spheres is applied in the field of preparation of ordered mesoporous silica hollow spheres, which can solve the problems of large-scale synthesis, cumbersome operation process, limited application and other problems that are unfavorable to industrialization, and achieve good industrial Application prospect, simple reaction device, low cost effect

Inactive Publication Date: 2013-03-20
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the sacrificial template method can be used to obtain uniform and adjustable ordered mesoporous silica hollow spheres by controlling the synthesis of the sacrificial template, it is difficult to use a milder post-treatment due to the use of organic polymer micro / nanospheres as templates. method (such as solvent extraction) to remove
Therefore, in practical applications, the existing sacrificial template methods are not suitable for large-scale industrial synthesis due to the relatively cumbersome operation process and high cost, thus limiting their application.

Method used

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  • Method for preparing ordered mesoporous hollow silica spheres
  • Method for preparing ordered mesoporous hollow silica spheres
  • Method for preparing ordered mesoporous hollow silica spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1) In a glass bottle, add 50 mg of silica spheres to 10 mL of water, and obtain a dispersion of silica spheres after ultrasonication for 10 minutes.

[0025] 2) Add the silica sphere dispersion prepared in step 1) to 60 mL of ethanol / water (1:1) mixed solution with a concentration of 1.25 mg / mL cetyltrimethylammonium bromide, and then add 0.275 mL Ammonia water, stirred for 30min, added 0.125mL tetraethyl orthosilicate, stirred at 25°C for 6h, and then centrifuged.

[0026] 3) Redisperse the white precipitate obtained by centrifugation in step 2) in 10 mL of water to obtain a precursor dispersion.

[0027] 4) In a glass bottle, add 212 mg of anhydrous sodium carbonate to the precursor dispersion obtained in step 3), then stir at 50° C. for 8 hours, and finally cool at room temperature.

[0028] 5) The white precipitate treated in step 4) was repeatedly washed twice with water and ethanol, and then dried naturally to obtain a white powder.

[0029] 6) The obtained whit...

Embodiment 2

[0032]1) In a glass bottle, add 50 mg of silica spheres to 10 mL of water, and obtain a dispersion of silica spheres after ultrasonication for 10 minutes.

[0033] 2) Add the silica sphere dispersion prepared in step 1) to 60 mL of ethanol / water (1:1) mixed solution with a concentration of 2.5 mg / mL cetyltrimethylammonium bromide, and then add 0.55 mL of ammonia water, stirred for 30 min, added 0.25 mL of ethyl orthosilicate, stirred at 25°C for 6 h, and then centrifuged.

[0034] 3) Redisperse the white precipitate obtained by centrifugation in step 2) in 10 mL of water to obtain a precursor dispersion.

[0035] 4) In a glass bottle, add 212 mg of anhydrous sodium carbonate to the precursor dispersion obtained in step 3), then stir at 80° C. for 1 h, and finally cool at room temperature.

[0036] 5) The white precipitate treated in step 4) was repeatedly washed twice with water and ethanol, and then dried naturally to obtain a white powder.

[0037] 6) The target product is...

Embodiment 3

[0039] 1) In a glass bottle, add 50 mg of silica spheres to 10 mL of water, and obtain a dispersion of silica spheres after ultrasonication for 20 minutes.

[0040] 2) Add the silica sphere dispersion prepared in step 1) to 60 mL of ethanol / water (2:1) mixed solution with a concentration of 1.25 mg / mL cetyltrimethylammonium bromide, and then add 0.275 mL of ammonia water, stirred for 30 min, added 0.125 mL of tetraethyl orthosilicate, stirred at 25°C for 6 h, and then centrifuged.

[0041] 3) Redisperse the white precipitate obtained by centrifugation in step 2) in 10 mL of water to obtain a precursor dispersion.

[0042] 4) In a glass bottle, add 212 mg of anhydrous sodium carbonate to the precursor dispersion obtained in step 3), then stir at a constant temperature of 45° C. for 12 h, and finally cool at room temperature.

[0043] 5) The white precipitate treated in step 4) was repeatedly washed once with water and ethanol, and then dried naturally to obtain a white powder....

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Abstract

The invention relates to hollow silica spheres and provides a method for preparing ordered mesoporous hollow silica spheres. The method comprises the following steps: adding silica spheres to water and obtaining silica sphere dispersion after ultrasonic treatment; adding the silica sphere dispersion to ethanol solution containing cationic surfactants, adding ammonia water to the obtained solution and then adding tetraethoxysilane and centrifugally collecting precipitate after stirring; and adding the obtained precipitate to water to obtain precursor dispersion, adding an alkali source to the dispersion, carrying out stirring and etching, collecting precipitate after etching and washing and airing the precipitate to obtain white powder and removing the cationic surfactants from the white powder, thus obtaining the ordered mesoporous hollow silica spheres. In the method, the silica spheres are taken as the templates and the core-shell type precursor is synthesized in advance under the action of the surfactants; and the core is selectively etched in the alkaline environment by utilizing the stability difference between the core and the shell layer relative to alkali, thus obtaining the ordered mesoporous hollow silica spheres.

Description

technical field [0001] The invention relates to silica hollow spheres, in particular to a method for preparing ordered mesoporous silica hollow spheres. Background technique [0002] In recent years, mesoporous silica hollow spheres with excellent properties such as high specific surface area, good mechanical and thermal stability, low toxicity, high biocompatibility, high drug loading capacity, and mesoporous channels that can be used as transport substances have been used in catalytic , Drug delivery, sensing and selective adsorption have important research and application value, and have received extensive attention from researchers. Among them, compared with disordered mesoporous silica hollow spheres, ordered mesoporous silica hollow spheres with ordered pores have important research value and Potential application prospects have become a research hotspot now. [0003] The preparation method of existing ordered mesoporous silica hollow spheres (1, H.Blas, M.Save, Pame...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12B01J13/02
Inventor 郑南峰方晓亮陈诚李悦
Owner XIAMEN UNIV