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Method for preparing micron spherical mesoporous silicon dioxide

A mesoporous silica, spherical technology, applied in the direction of silicon oxide, etc., can solve the problem of low yield and achieve a wide range of effects

Inactive Publication Date: 2005-02-16
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Agnes E.Ostafin etc. used cationic surfactants to synthesize mesoporous silica spheres of 60-740nm under alkaline conditions, but the reaction was carried out in a dilute solution and the yield was low [Robert I.Nooney, Dhanasekaran Thirunavukkarasu, Yimei Chen, Robert Josephs, and Agnes E. Ostafin Chem. Mater. 2002, 14(11), 4721-4728]

Method used

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  • Method for preparing micron spherical mesoporous silicon dioxide
  • Method for preparing micron spherical mesoporous silicon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) prepare hydrochloric acid solution, the concentration of hydrochloric acid is 2.0 mol / liter.

[0022] (2) prepare the solution of surfactant, add surfactant in step (1), make the concentration of cetyltrimethylammonium bromide in the mixed solution be 0.05 mole / liter; The concentration of polyvinyl alcohol is 8.0 g / L; the concentration of poly(oxyethylene)-poly(oxypropylene)-poly(oxyethylene) is 3.5×10 -4 mol / liter.

[0023] (3) Ethyl orthosilicate is added to the mixed solution obtained in step (2), so that the concentration of ethyl orthosilicate after mixing is 0.50 mol / liter, continue to stir for 7 minutes, and then stand for a period of time to obtain white The precipitated solution was centrifuged, washed, dried, and calcined at 600°C to obtain mesoporous silica with an average particle size of 1.3 μm and a specific surface area of ​​860 m 2 / g, the mesopore size is 4.4nm.

Embodiment 2

[0025] (1) prepare nitric acid solution, the concentration of nitric acid is 6.0 mol / liter.

[0026] (2) prepare the solution of surfactant, add surfactant in (1), make the concentration of cetyltrimethylammonium chloride in the solution after mixing and dissolving be 0.040 mole / liter; The concentration of polyvinyl alcohol is 6.0 g / L; the concentration of poly(oxyethylene)-poly(oxypropylene)-poly(oxyethylene) is 6×10 -4 mol / liter.

[0027] (3) Ethyl orthosilicate is added to the mixed solution obtained in step (2), so that the concentration of methyl orthosilicate after mixing is 4.0 mol / liter, continue to stir for 15 minutes, and then stand for a period of time to obtain white The precipitated solution was centrifuged, washed, dried, and calcined at 550°C to obtain mesoporous silica with an average particle size of 2.1 μm and a specific surface area of ​​920 m 2 / g, the mesopore size is 2.7nm.

Embodiment 3

[0029] With embodiment 1, change the hydrochloric acid in the step (1) into sulfuric acid, other conditions are constant, obtain mesoporous silica, average particle diameter is 3.1 μ m, specific surface area is 1090m 2 / g, the mesopore size is 2.3nm.

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Abstract

The invention belongs to the field of semiconductor material's preparation and application technology, especially round silicon dioxide. Utilizing surfactant as template and silicate ester as silicon source, hydrolytic condensation is done under acidity condition. The invention has not only low energy consumption and a good dispersity, but also the aperture can be controlled by adding bulk agent.

Description

field of invention [0001] The invention belongs to the technical field of preparation and application of semiconductor materials, in particular to a preparation method of micron-sized spherical mesoporous silicon dioxide. Background technique [0002] Mesoporous silica is a kind of porous solid, which is a porous solid between microporous (pore diameter > 2nm) and macroporous (pore diameter > 50nm) solids. Mesoporous silica is an attractive research object in the field of nanomaterials science in recent years. Due to the huge specific surface area (usually 1000m 2 / g) and uniform pore size, it has important applications in catalysis and separation science, such as chromatography, catalyst support, selective absorption of molecules, sieving, catalysis, etc. The mesopore size makes it possible to deal with larger molecules or genes and has great application prospects in electronics, optics and micromechanics, especially mesoporous solids are u...

Claims

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Application Information

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IPC IPC(8): C01B33/113
Inventor 唐芳琼庞雪蕾
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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