Micron-sized monodispersed porous silica microsphere and preparation method thereof

A technology of porous silicon dioxide and silicon dioxide, applied in the directions of silicon dioxide, silicon oxide, nanotechnology, etc., can solve problems such as application field limitations, and achieve low cost of raw materials, adjustable particle size and pore structure, and acceptable conditions. Strong control effect

Active Publication Date: 2019-03-01
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the pore size of the material prepared by the molecular template method is generally less than 4nm, wh

Method used

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  • Micron-sized monodispersed porous silica microsphere and preparation method thereof
  • Micron-sized monodispersed porous silica microsphere and preparation method thereof
  • Micron-sized monodispersed porous silica microsphere and preparation method thereof

Examples

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Example Embodiment

[0023] Example 1

[0024] Preparation of silica microspheres using polymethylsilsesquioxane microspheres as template

[0025] (1) Add 20 g of methyltrimethoxysilane to 100 mL of deionized water, add 0 μL of pH 1 hydrochloric acid solution, and stir and react for 1 hour at room temperature to obtain a polysilsesquioxane hydrolysate;

[0026] (2) Add 10 μL of concentrated ammonia to the polysilsesquioxane hydrolysate, stir well, let stand for 4 hours, filter to remove the mother liquor, collect the microspheres, wash with 95% ethanol to obtain polysilsesquioxane gel micro ball;

[0027] (3) Disperse 1 g of polysilsesquioxane gel microspheres in 10 mL of 80% ethanol at a mass-to-volume ratio of 0.1, and mix;

[0028] (4) Add sodium hydroxide to the mixed solution obtained in step (3) to make the concentration 0.05M, mix well, shake in a 70℃ water bath for 10 hours, filter to remove the solvent, and wash the microspheres alternately with 95% ethanol and water. Until the filtrate is neutra...

Example Embodiment

[0031] Example 2

[0032] Preparation of silica microspheres with different pore diameters using polymethylsilsesquioxane microspheres as templates

[0033] (1) Add 20 g of methyltrimethoxysilane to 100 mL of deionized water, add 0 μL of pH 1 hydrochloric acid solution, and stir and react for 1 hour at room temperature to obtain a polysilsesquioxane hydrolysate;

[0034] (2) Add 10 μL of concentrated ammonia to the polysilsesquioxane hydrolysate, stir well, let stand for 4 hours, filter to remove the mother liquor, collect the microspheres, wash with 95% ethanol to obtain polysilsesquioxane gel micro ball;

[0035] (3) Disperse 1 g of polysilsesquioxane gel microspheres in 10 mL of 80% ethanol at a mass-to-volume ratio of 0.1, and mix;

[0036] (4) Add sodium hydroxide to the mixed solution obtained in step (3) to make the concentration of 0.01 and 0.025M respectively, mix well, shake in a 70℃ water bath for 10h, filter to remove the solvent, and use 95% ethanol and water for the micro...

Example Embodiment

[0041] Example 3

[0042] Preparation of silica microspheres with different particle diameters using polymethylsilsesquioxane microspheres as templates

[0043] (1) Add 20 g of methyltrimethoxysilane to 100 mL of deionized water, add 0 μL of pH 1 hydrochloric acid solution, and stir and react for 1 hour at room temperature to obtain a polysilsesquioxane hydrolysate;

[0044] (2) Add 5, 20, and 50 μL of concentrated ammonia to the polysilsesquioxane hydrolysate, stir well, and let stand for 4, 3, and 2 hours respectively, filter to remove the mother liquor, collect the microspheres, and wash with 95% ethanol. Obtaining polysilsesquioxane gel microspheres of different particle sizes;

[0045] (3) Disperse 1 g of polysilsesquioxane gel microspheres in 10 mL of 80% ethanol at a mass-to-volume ratio of 0.1, and mix;

[0046] (4) Add sodium hydroxide to the mixed solution obtained in step (3) to make the concentration respectively 0.05, 0.1, 0.6M, mix well, shake in a water bath at 70℃ for 1...

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Abstract

The invention discloses a preparation method of a micron-sized monodispersed porous silica microsphere. A novel porous polysilsesquioxane microsphere is taken as a template, direct calcinations is conducted for removing organic components, and thus a monodispersed porous silica microsphere material with the controllable particle size and hole diameter. The invention further discloses the micron-sized monodispersed porous silica microsphere prepared through the preparation method, the particle size of the silica microsphere is 3-10 [mu]m, the pore volume is 0.3-0.9 cm<3>/g, the specific surface area is 100-400 m<2>/g, and the hole diameter is 3-100 nm. Compared with a traditional process, the preparation method is simple, the economical effect is achieved, graded screening is not needed, and the prepared porous silica microsphere is round and normal in shape and uniform in particle size distribution, has a mesoporous structure, can be directly applied to high performance liquid chromatography stationary phases, and can also be applied to the fields such as catalytic carriers, coating and cosmetic additives.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-efficiency liquid phase monodisperse mesoporous silica microspheres, and in particular relates to a micron-scale monodisperse porous silica microsphere and a preparation method thereof, especially relates to high-performance liquid chromatography immobilization A method for preparing monodisperse porous silica microspheres with a particle size distribution of 3-10 μm. Background technique [0002] Monodisperse porous silica microspheres are widely used in the fields of biomedicine, cosmetics, coatings, chemistry and chromatography due to their high mechanical strength, large specific surface area, mesoporous structure and abundant functionalized silanol on the surface. application prospects. Monodisperse porous silica microspheres with a particle size in the range of 3-10 μm play an important role in the high-efficiency liquid phase stationary phase, which can effectively reduce the f...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B33/18C01P2004/32C01P2006/17C01P2006/14C01P2006/12C01P2004/61C01P2004/52
Inventor 陈磊霍志霞万谦宏
Owner TIANJIN UNIV
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