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Preparation method of homopolymerized organosilicon resin microspheres

A technology of resin microspheres and polyorganosilicon, which is applied in the chemical industry, can solve the problems of wide particle size distribution and limited application, and achieve the effect of strong production process continuity, narrow particle size distribution and particle size reduction.

Inactive Publication Date: 2020-06-16
QUZHOU ZHONGTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The silicone resin microspheres provided by the above technologies and existing patents have too wide particle size distribution, which limits their application in some fields

Method used

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  • Preparation method of homopolymerized organosilicon resin microspheres
  • Preparation method of homopolymerized organosilicon resin microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of homopolymeric silicone resin microspheres, the operation steps are:

[0024] Put 80g of methyltrimethoxysilane and 350g of deionized water into the reactor, add hydrochloric acid with a mass percentage concentration of 10 to adjust the pH value to 3, stir evenly, heat up to 40°C, and keep it warm for 60min for hydrolysis reaction; then add 0.1g of Metal silane particle size control agent, after stirring and mixing evenly, add 0.3g of 8% NaOH solution, adjust the pH value to 8, and carry out polycondensation reaction; after heat preservation polycondensation reaction for 60 minutes, add 5%-dilute sulfuric acid to adjust the pH value to neutral, and discharge , dehydration; then washing the slurry, drying at 100° C., and crushing to obtain the homopolymeric silicone resin microspheres.

[0025] Described metallocene silane particle size control agent is processed according to the following methods:

[0026] Get 3g of 2-methyl-2-[(1-oxo-2-propenyl)...

Embodiment 2

[0032] A preparation method of homopolymeric silicone resin microspheres, the operation steps are:

[0033] Put 90g of methyltrimethoxysilane and 50g of deionized water into the reactor, add hydrochloric acid with a mass percentage concentration of 14 to adjust the pH value to 5, stir evenly, heat up to 60°C, and keep it warm for 80min for hydrolysis reaction; then add 0.5g of Metal silane particle size control agent, after stirring and mixing evenly, add 0.5g of 10% NaOH solution, adjust the pH value to 9, and carry out polycondensation reaction; after heat preservation polycondensation reaction for 90min, add 8% dilute sulfuric acid to adjust the pH value to neutral, discharge, Dehydration; then washing the slurry, drying at 110°C, and crushing to obtain the homopolymeric silicone resin microspheres.

[0034] Described metallocene silane particle size control agent is processed according to the following methods:

[0035] Get 5g of 2-methyl-2-[(1-oxo-2-propenyl)amino]-1-pro...

Embodiment 3

[0043] A preparation method of homopolymeric silicone resin microspheres, the operation steps are:

[0044] Put 100g of methyltrimethoxysilane and 800g of deionized water into the reactor, add hydrochloric acid with a mass percentage concentration of 20 to adjust the pH value to 6, stir evenly, heat up to 80°C, and keep it warm for 90min for hydrolysis reaction; then add 1g of metallocene Silane particle size control agent, after stirring and mixing evenly, add 0.6g of 12% NaOH solution, adjust the pH value to 10, and carry out polycondensation reaction; after 120 minutes of heat preservation polycondensation reaction, add 10% dilute sulfuric acid to adjust the pH value to neutral, discharge, Dehydration; then washing the slurry, drying at 120°C, and crushing to obtain the homopolymeric silicone resin microspheres.

[0045] Described metallocene silane particle size control agent is processed according to the following methods:

[0046] Get 8g of 2-methyl-2-[(1-oxo-2-propenyl...

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Abstract

The invention relates to the field of chemical engineering, and in particular, relates to a preparation method of homopolymerized organosilicon resin microspheres. The method comprises the steps: hydrolyzing methyltrimethoxysilane under acidic conditions, and carrying out a homopolymerization reaction in an alkaline environment in the presence of a metallocene silane particle size control agent. The invention relates to the preparation method of the homopolymerized organosilicon resin microspheres. According to the method, the metallocene silane particle size control agent is added, so that the particle size of the resin microspheres can be effectively controlled under normal pressure, the particle size distribution of the produced microspheres is narrow, the organosilicon resin microspheres can be efficiently produced by the method, the production process is high in continuity and operability, and the method has quite high production value. High temperature and high pressure are not used in the production process, safety and reliability are achieved, and the green production process is compounded.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for preparing homopolymerized silicone resin microspheres. Background technique [0002] Silicone polymers can also be made into nanomaterials to have some special properties and uses. [0003] 201210226121.9 involves a high-efficiency method for producing silicone resin microspheres, which includes: (1) adding silane with three or four hydrolyzable groups into a high-temperature and high-pressure reactor, adding water, and stirring; (2) Inert gas is introduced into the reactor so that the gas pressure in the reactor is 760×1-7600×10mmHg; (3) Heating the reactor until the temperature is between (the boiling point of water under the corresponding pressure -10°C) to the temperature under the corresponding pressure Within the range of the boiling point of water, carry out hydrolysis reaction; (4) Under heat preservation and pressure, add alkali, adjust the pH of the reacta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/22C08G77/20C08G77/06C08G77/08C08J3/03C08L83/08B01J13/14B01J13/04
CPCB01J13/04B01J13/14C08G77/06C08G77/08C08G77/20C08G77/22C08J3/03C08J2383/08
Inventor 许益生吴哥德许丽斯
Owner QUZHOU ZHONGTONG CHEM
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