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Synthesis of organosilicon resin

A synthesis method and organosilicon technology, which is applied in the field of silicone resin preparation, can solve problems such as strong corrosion of equipment, environmental pollution, and small-scale production and application constraints, and achieve the effects of easy preservation, convenient and easy synthesis method, and good stability

Active Publication Date: 2006-08-02
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In known synthetic methods, although chlorosilanes such as methyltrichlorosilane, phenyltrichlorosilane, etc. can be hydrolyzed in toluene to synthesize the toluene solution of silicone resin, this method will produce a large amount of hydrogen chloride, which is caused by The strong corrosion effect on the equipment and the pollution to the environment caused by this have made the method subject to certain restrictions in small-scale production applications.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Starting from 1555g methyltriethoxysilane and 780g tetraethyl orthosilicate, add 520g water, 7g0.1N hydrochloric acid and 800g toluene, heat up to 77°C under stirring, keep reflux for 3.5 hours, then at the same temperature Ethanol 845g was evaporated, and the reaction was stopped after aging for 1 hour. After adding 45g of toluene, a colorless and transparent silicone resin solution was obtained. The resin R / Si value was 0.7.

Embodiment 2

[0023] Starting from 534g of methyltriethoxysilane and 49g of dimethyldiethoxysilane, add 222g of water, 1.94g of 0.1N hydrochloric acid and 900g of toluene, raise the temperature to 74-79°C while stirring, and keep refluxing for 6 hours , then add about 1g of hexamethyldisilazane, stop heating and continue stirring for about half an hour, then raise the temperature to 74-89°C to evaporate ethanol and part of the solvent, stop the reaction after aging for 40 minutes, cool to obtain colorless and transparent Silicone resin solution 570g, resin R / Si value is 1.1.

Embodiment 3

[0025] Using 1753g methyltriethoxysilane and 364g dimethyldiethoxysilane as starting materials, add 620g water, 4.87g 0.1N hydrochloric acid and 1058g toluene, raise the temperature to 74~79℃ under stirring, and keep reflux for 4.5 hours , then add about 2.6g of hexamethyldisilazane, stop heating and continue stirring for about half an hour, then raise the temperature to 75-116°C to evaporate ethanol and part of the solvent, stop the reaction after aging for 2 hours, cool, and add 1000g After toluene, 1940 g of colorless transparent silicone resin solution was obtained, and the resin R / Si value was 1.2.

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Abstract

The synthesis of organosilicon resin includes the following steps: selecting at least one kind of alkyl trialkoxy silane RSi(OR1)3 with R / Si ration of 0.7-1.5 as the initial material, where R is one-valent alkyl radical, one-valent aryl radical, one-valent unsaturated group, etc; and R1 represents C1-C4 alkyl radical; adding water, weak polarity or non-polyarity solvent ad 0.1 N hydrochloric acid solution, refluxing under stirring at 60-100 deg.c of 1-6 hr, further stirring for 0.5 hr after stopping heating, re-heating to 65-130 deg.c, curing for 40-120 min, stopping reaction, and cooling to obtain colorless transparent homogeneous organosilicon resin solution. The process has no HCl produced, no corrosion to the apparatus and no environmental pollution, and can meet the special requirement of coating or soaking with organosilicon resin with little water content.

Description

technical field [0001] The present invention relates to the preparation method of silicone resin, specifically, the present invention relates to a kind of synthesis method of the silicone resin solution that can be dissolved in weak polar or non-polar solvents such as toluene. Background technique [0002] In some special applications, such as controlling the low dielectric loss of the product, it is necessary to carry out special moisture-proof coating treatment on the product interface. When using a silicone resin solution as a coating or composite impregnating solution, it is required that no moisture can be brought in. Therefore, a silicone resin solution in a polar solvent such as ethanol is not allowed. In the existing silicone resin synthesis methods, the silicone resin solutions synthesized from alkoxysilanes such as methyltriethoxysilane and phenyltriethoxysilane as raw materials all use ethanol as a solvent. Because the hydrolysis of alkoxysilane directly produces...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/06
Inventor 周远建唐小斗姜承永
Owner CHINA BLUESTAR CHENGRAND CO LTD
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