Method for synthesizing high-temperature resistant organic silicon resin

A synthesis method, silicone technology, applied in the field of chemical materials, can solve the problems of poor temperature resistance, high cost, complex synthesis process, etc., and achieve the effect of good stability, low cost and simple process

Inactive Publication Date: 2011-11-23
DALIAN JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to develop a synthetic method of organic silicon resin with low cost, simple process and convenient industrial production according to the current complex synthetic process of silicone resin, various synthetic raw materials, high cost, and poor temperature resistance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Using 190.72g of methyltrimethoxysilane and 146.64g of phenyltrimethoxysilane as starting materials, they were added to a glass reactor equipped with a reflux device. Raise the temperature to 70°C at a certain stirring speed and keep it at this temperature. After stirring evenly, slowly add 97.2g of deionized water into the reaction kettle dropwise for about 10min to 12min. After the dropwise addition was completed, the mixture was reacted for 4 hours and 30 minutes at 70° C. under a constant stirring speed condition. After finishing, remove reflux device, be warming up to 150 ℃, stirring speed is constant, carry out evaporation, polycondensation reaction, reaction is carried out 50 minutes and stops reaction, cooling, adds 93.2g diethylene glycol butyl ether and 3.6g zinc isooctanoate (11% ), and 319.24 g of a colorless and transparent silicone resin solution could be obtained after stirring at 120° C. for 30 min. The R / Si value of the resin was 1.3, and the Ph / (Ph+Me...

Embodiment 2

[0035] Using 136.22g of methyltrimethoxysilane and 134.40g of phenyltrimethoxysilane as starting materials, weigh 13.53g of ethanol and add them together into a glass reactor equipped with a reflux device. Raise the temperature to 70°C at a certain stirring speed and keep it at this temperature. After stirring evenly, slowly add 73.8g of deionized water to the reaction kettle dropwise for about 10min to 12min. After the dropwise addition was completed, the mixture was reacted for 4 hours and 30 minutes at 70° C. under a constant stirring speed condition. After finishing, remove reflux device, be warming up to 150 ℃, stirring speed is constant, carry out evaporation, polycondensation reaction, react and stop reaction in 60 minutes, cooling, add 83.94g n-butanol and 0.83g zinc isooctanoate (11%), at 120 After stirring for 30 minutes at °C, 280.54 g of a colorless and transparent silicone resin solution was obtained. The R / Si value of the resin was 1.35, and the Ph / (Ph+Me) value...

Embodiment 3

[0037] Using 136.22g of methyltrimethoxysilane and 134.40g of phenyltrimethoxysilane as starting materials, weigh 13.53g of acetone and add them together into a glass reactor equipped with a reflux device. Raise the temperature to 70°C at a certain stirring speed and keep it at this temperature. After stirring evenly, slowly add 73.8g of deionized water to the reaction kettle dropwise for about 10min to 12min. After the dropwise addition was completed, the reaction was carried out at 70°C for 5 hours at a constant stirring speed. After finishing, remove reflux device, be warming up to 150 ℃, stirring speed is constant, carry out evaporation, polycondensation reaction, reaction is carried out 1 hour stop reaction, cooling, add 73g diethylene glycol butyl ether and 2.88g zinc isooctanoate (11%) After stirring at 120°C for 30 minutes, 258.84 g of a colorless and transparent silicone resin solution can be obtained. The R / Si value of the resin is 1.35, and the Ph / (Ph+Me) value is ...

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Abstract

The invention discloses a method for synthesizing high-temperature resistant organic silicon resin, which comprises the following steps of: determining the proportion of methyltrimethoxy silane and dimethoxydiphenyl silane serving as initiative raw materials in a ratio of R / Si of 1.3-1.4 and a ratio of Rh / (Ph+Me) of 0.45-0.60, and adding the raw materials into a reaction kettle with a reflux device; adding a certain amount of ethanol or acetone into the reaction kettle at the same time; dripping a certain amount of deionized water into the reaction kettle with stirring at the temperature of between 65 and 75 DEG C; after the dripping is finished, continuously stirring and refluxing the solution for 4 to 6 hours; removing the reflux device, and performing evaporation and condensation polymerization reaction at the temperature of between 145 and 155 DEG C till the water and the solvent are completely evaporated; and reducing the temperature, adding a solvent into the reaction product to adjust the solid content, then adding a curing agent into the reaction product, stirring the mixture uniformly, and then cooling the mixture to obtain the high-temperature resistant organic silicon resin. The method for synthesizing the resin has the advantages of simple raw materials, low cost and simple process; and the synthesized silicon resin has excellent temperature resistance, and is suitable for mass preparation and industrialized production.

Description

technical field [0001] The invention relates to a method for synthesizing a high-temperature-resistant organic silicon resin. The resin is used as a matrix resin for high-temperature-resistant paints and inks, and belongs to the technical field of chemical materials. Background technique [0002] Silicone resin is a polymer with a highly cross-linked network structure. The structure contains both organic groups and inorganic structures. This special composition and molecular structure is a combination of organic and inorganic properties. It has a unique Physical and chemical properties. Therefore, it has broad market prospects in metallurgy, petrochemical, energy, new materials and other industries. [0003] Silicone resin has silicon-oxygen bonds as the main chain, and its unique physical and chemical properties make it widely used as a base material for heat-resistant coatings, weather-resistant coatings and electrical insulation materials. At present, the heat-resistant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06
Inventor 李国军张炳任瑞铭
Owner DALIAN JIAOTONG UNIVERSITY
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