Method for preparing poly-organic silsesquioxane microsphere

A technology of sesquioxane and polyorganosilicon, which is applied in the field of preparing polyorganosilsesquioxane microspheres, can solve the problems of cumbersome steps and achieve the effects of simple process, good spherical shape and short production cycle

Active Publication Date: 2010-03-24
ETERNAL CHINA INVESTMENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some of the various existing preparation methods are based on the two-step method of hydrolysis-polycondensation, and some need to add surfactants or sieve to achieve the uniformity of the particle size of the microspheres, and the steps are cumbersome

Method used

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  • Method for preparing poly-organic silsesquioxane microsphere

Examples

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Effect test

Embodiment 1

[0016] Embodiment 1, preparation polyorganosilsesquioxane microsphere

[0017] Mix 70ml of water with 10ml of ethanol, and slowly add 4ml of CH under stirring 3 Si(OCH 3 ) 3 , fully stirred to obtain a clear solution, adding 0.1ml of ammonia water with a mass percentage concentration of 28% to it, stirring continuously for 3 hours, and the silicone resin microspheres obtained after standing for 1 hour precipitated to the bottom of the reactor. Separated by filtration, washed with deionized water, and dried to obtain 1.65 g of methyl silicone resin microspheres with a particle size of 0.6-1 μm, such as figure 1 shown.

Embodiment 2

[0018] Embodiment 2, preparation polyorganosilsesquioxane microsphere

[0019] Take 40ml of water, slowly add 5ml of CH under stirring 3 Si(OCH 3 ) 3 , fully stirred to obtain a clear solution, adding 0.4ml of ammonia water with a mass percentage concentration of 28% to it, stirring continuously for 4 hours, and the silicone resin microspheres obtained after standing for 1 hour precipitated to the bottom of the reactor. Separated by filtration, washed with deionized water, and dried to obtain 2.1 g of methyl silicone resin microspheres with a particle size of 1.5-2 μm, such as figure 2 shown.

Embodiment 3

[0020] Embodiment 3, preparation polyorganosilsesquioxane microsphere

[0021] Mix 70ml of water with 10ml of ethanol, and slowly add 4ml of CH under stirring 3 Si(OCH 3 ) 3 , fully stirred to obtain a clear solution, adding 0.36ml of ammonia water with a mass percentage concentration of 28% to it, stirring continuously for 3 hours, and the silicone resin microspheres obtained after standing for 1 hour precipitated to the bottom of the reactor. Separated by filtration, washed with deionized water, and dried to obtain 1.6 g of methyl silicone resin microspheres with a particle size of 0.5 μm, such as image 3 shown.

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Abstract

The invention discloses a method for preparing poly-organic silsesquioxane microsphere, comprising the following steps: 1) adding mixture of one or arbitrary several kinds selected from compound in structure general formula R1Si(OR2)3 into the mixture solution of water and alcohol, uniformly stirring the mixture, wherein R1 is hydrogen, methyl or vinyl, R2 is C1-C4 alkyl; 2) adding aqueous solution of alkali metal hydroxide or ammonia water into the reaction system and obtaining products after reaction. The method uses one-step method and the reaction is performed at normal temperature withoutcatalyst containing inorganic ion. The technology is simple and the production period is short and the obtained poly-organic silsesquioxane microsphere has good shape and the particle size is in narrow distribution at micro order.

Description

technical field [0001] The invention relates to a method for preparing polyorganosilsesquioxane microspheres. Background technique [0002] Polyorganosilsesquioxane microspheres not only have low relative density, but also have excellent heat resistance, weather resistance, lubricity, water resistance, high hardness, and wear resistance. They can be used in plastics, rubber, coatings, inks, Manufacture of cosmetics and liquid crystal display adjustment pads, light diffusion plates, high-definition video tapes, thermal prints, etc., to improve their lubricity, gloss, hydrophobicity, antifouling, mold release, flame retardancy, etc. At present, many patents have reported the preparation method of silicone resin microspheres. Watanabe T proposed in the Japanese patent (JP4088022) that methyltrimethoxysilane or its partial hydrolyzed polycondensate was dropped into an alkaline aqueous solution to carry out a hydrolyzed polycondensation reaction to make spherical microspheres. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/14C08G77/06C08G77/20C08G77/12
Inventor 刘海云戴珍赵宁张小莉徐坚
Owner ETERNAL CHINA INVESTMENT
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