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Monodisperse porous polysilsesquioxane microsphere and preparation method thereof

A polysilsesquioxane, monodisperse technology

Inactive Publication Date: 2016-11-09
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the template method can prepare mesoporous microspheres, this method is only applicable to bridged siloxane monomers

Method used

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  • Monodisperse porous polysilsesquioxane microsphere and preparation method thereof
  • Monodisperse porous polysilsesquioxane microsphere and preparation method thereof
  • Monodisperse porous polysilsesquioxane microsphere and preparation method thereof

Examples

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Effect test

Embodiment 1

[0025] Embodiment 1: the preparation method of monodisperse porous polymethylsilsesquioxane microspheres, comprises the following steps:

[0026] (1) Mix deionized water and methyltrimethoxysilane in a 250mL three-neck flask according to different molar ratios of 10, 38, and 150, and stir and react at room temperature for 0.5h to obtain polymethylsilsesquioxane pre- Polymer dispersion system;

[0027] (2) Add concentrated ammonia water to the polymethylsilsesquioxane prepolymer dispersion system obtained in step (1) by volume ratio of 0.00001, after stirring evenly, leave to react for 5h, filter, collect microspheres, and use Washing with absolute ethanol three times to obtain polymethylsilsesquioxane gel microspheres, and calculate the solid content of polysilsesquioxane gel microspheres;

[0028] (3) Add polysilsesquioxane gel microspheres into deionized water according to the mass ratio of 0.01, and mix well;

[0029](4) Add concentrated ammonia water (14.7mol / L) to the p...

Embodiment 2

[0033] Embodiment 2: the preparation method of monodispersity polymethylsilsesquioxane microsphere, comprises the steps:

[0034] (1) Add deionized water (100mL) and methyltrimethoxysilane (20g) to three 250mL there-necked flasks at a molar ratio of 38, mix well, and stir magnetically at room temperature for 0.25, 3, and 10 hours respectively to obtain poly Methylsilsesquioxane prepolymer dispersion system;

[0035] (2) Add concentrated ammonia water to the polymethylsilsesquioxane prepolymer dispersion system obtained in step (1) according to the volume ratio of 0.00001, after stirring evenly, leave to react for 5h, filter, collect microspheres, and use Washing repeatedly with water and ethanol three times; obtaining polymethylsilsesquioxane gel microspheres: and calculating the solid content of polysilsesquioxane gel microspheres;

[0036] Steps (3)-(4) are the same as in Example 1 (3)-(4) to obtain monodisperse porous polymethylsilsesquioxane microspheres.

[0037] Charac...

Embodiment 3

[0040] Embodiment 3: the preparation method of monodisperse porous polymethylsilsesquioxane microspheres, comprises the steps:

[0041] (1) Add deionized water (100mL) and methyltrimethoxysilane (20g) to three 250mL there-necked flasks at a molar ratio of 38, mix well, and stir magnetically at room temperature for 0.5h to obtain polymethylsilsesquisilane Oxyalkylene prepolymer dispersion system;

[0042] (2) Add concentrated ammonia water to the polymethylsilsesquioxane prepolymer dispersion system obtained in step (1) according to the volume ratio of 0.00001, 0.001, and 0.05 respectively, after stirring evenly, let stand for reaction for 5h, filter, Collect the microspheres, wash them repeatedly with absolute ethanol three times; obtain the polymethylsilsesquioxane gel microspheres: and calculate the solid content of the polysilsesquioxane gel microspheres;

[0043] Steps (3)-(4) are the same as in Example 1 (3)-(4) to obtain monodisperse porous polymethylsilsesquioxane micr...

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Abstract

The invention discloses a monodisperse porous polysilsesquioxane microsphere and a preparation method thereof. The monodisperse porous polysilsesquioxane microsphere has an average particle size of 0.5 to 10 [mu]m, a pore volume of 0.3 to 1.2 mL / g, a specific surface area of 272.413 to 823.698 m<2> / g and a pore size of 1.7 to 30 nm. The monodisperse porous polysilsesquioxane microsphere has high porosity, a large specific surface area and good hydrothermal stability; the preparation method is simple in process, easily controllable in conditions and high in product yield; and the monodisperse porous polysilsesquioxane microsphere is applicable as a chromatographic filling material.

Description

technical field [0001] The invention relates to monodisperse porous polysilsesquioxane microspheres and a preparation method thereof, belonging to the preparation technology of porous organic silica gel microspheres. Background technique [0002] Hybrid materials are the fourth generation of materials after single-component materials, composite materials and functionally graded materials. It is a homogeneous heterogeneous composite material, which is compounded at the nanometer level through chemical bonds or intermolecular interactions, so that the phase separation size does not exceed the order of nanometers. Compared with traditional composite materials with larger microphase size, it has obvious difference in structure and performance. Among them, organic-inorganic hybrid materials, as new materials with excellent performance, have broad application prospects in the fields of optics, electronics and biology. The organic and inorganic components that make up the hybrid ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/20C08J9/28
CPCC08G77/06C08G77/20C08J9/28C08J2383/04
Inventor 万谦宏霍志霞陈磊
Owner TIANJIN UNIV