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A kind of addition type organosilicon resin and its preparation method and application

An addition-type, silicone technology, applied in the direction of coating, etc., can solve problems such as equipment corrosion, unsatisfactory volatile content, and reduction of hydrogen content in silicone resin.

Active Publication Date: 2020-09-29
浙江博菲电气股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this technical solution is that the silicone impregnating varnish consists of two main components, that is, a two-component addition type silicone impregnating varnish, the industrial preparation of which involves extremely high costs and complex In addition, the volatile content of the silicone impregnating paint is at least 0.9% at 180-200 ° C. Although it meets the national standard GB15022-2007, it cannot meet some technical fields that have higher requirements for volatile content.
[0006] Another example is that the Chinese patent literature with the publication number CN 101070386 A discloses a method for preparing a one-component H-siloxane-containing addition-crosslinkable silicone resin, which is composed of a one-component silicone resin, but has the disadvantage of Because all the raw materials use chlorosilane mixture, a large amount of HCl is released during the hydrolysis process, which is very easy to cause environmental pollution and equipment corrosion, and the reaction is violent and difficult to control
Although a 0.01-1.0% concentration aqueous solution of a base with a pH value of 7.0-8.5 is used in this preparation process to wash the phase comprising a one-component H-siloxane-containing addition-crosslinkable silicone resin to reduce the residual HCl content, However, this washing process is prone to dehydrogenation reaction, which reduces the hydrogen content in silicone resin.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Fill 33mol (594g) of water into a 5000ml glass bottle equipped with a stirrer, heating, condenser distillation and dropping funnel, and heat to 60°C. Under stirring, drop 2mol (480g) PhSi(OEt) through the dropping funnel 3 、1mol(134g)MeHSi(OEt) 2 , 1mol (160g) MeViSi (OEt) 2 , 0.5mol (54.3g) Me 3 SiCl mixture, the dropping time is 25min. Raise the temperature to 80°C and react for 8h. After the reaction was completed, it was cooled to room temperature, and 900 g of ethyl acetate was added. Stir, let stand, and divide the acid water. The organic layer was washed 500 mL×3 times until neutral, and ethyl acetate was distilled off. The temperature was raised to 150° C., and the vacuum pressure was maintained at 50 hPa for 3 hours to obtain 500 g of silane hydrolyzate.

[0052] Add 500 g of ethyl acetate and 25 g of trimethylchlorosilane to the above silane hydrolyzate, raise the temperature to 60° C., and react for 4 hours. Add 45g of absolute ethanol and continue th...

Embodiment 2

[0062] Put 208mol (3744g) of water in a 10000ml glass bottle equipped with a stirrer, heating, condenser distillation and dropping funnel and heat it to 30°C. Under stirring, drop 6mol (1188g) PhSi(OMe) through the dropping funnel 3 、3mol(402g)MeHSi(OEt) 2 , 1mol (132g) MeViSi (OMe) 2 , 2.0mol (217g) Me 3 SiCl mixture, the dropping time is 30min. Raise the temperature to 60°C and react for 3h. After the reaction was completed, it was cooled to room temperature, and 1000 g of dichloromethane was added. Stir, let stand, and divide the acid water. The organic layer was washed 1000 mL×3 times with water until neutral, and dichloromethane was distilled off. The temperature was raised to 50° C., and the vacuum pressure was maintained at 80 hPa for 4 hours to obtain 1200 g of silane hydrolyzate.

[0063] Add 700 g of dichloromethane and 15 g of trimethylchlorosilane to the above 1200 g of silane hydrolyzate, raise the temperature to 30° C., and react for 8 hours. Add 10g of a...

Embodiment 3

[0073] Fill 65mol (1170g) of water into a 5000ml glass bottle equipped with a stirrer, heating, condenser distillation and dropping funnel, and heat to 45°C. Under stirring, drop 3.0mol (720g) PhSi(OEt) through the dropping funnel 3 , 1.5mol (201g) MeHSi (OEt) 2 , 1mol (160g) MeViSi (OEt) 2 , 1.5mol (162.8g) Me 3 SiCl mixture, the dropwise addition time is 20min. Raise the temperature to 70°C and react for 5h. After the reaction is completed, cool to room temperature, and add 1500 g of petroleum ether (boiling range 60-90). Stir, let stand, and divide the acid water. The organic layer was washed 500 mL×3 times with water until neutral, and the petroleum ether was distilled off. The temperature was raised to 80° C., and the vacuum pressure was maintained at 30 hPa for 2 hours to obtain 780 g of silane hydrolyzate.

[0074] Add 700g of petroleum ether (boiling range 60-90) and 25g of trimethylchlorosilane to the above 780g of silane hydrolyzate, raise the temperature to 6...

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Abstract

The invention discloses addition type organic silicon resin, a preparation method of the addition type organic silicon resin and application of the addition type organic silicon resin to preparation of low-volatilization single-ingredient addition organic silicon impregnating varnish. The addition type organic silicon resin has a structure general formula of (Me3SiO0.5)m(MeHSiO)n(MeViSiO)q(PhSiO1.5)t, wherein the m is an integer being 1 to 20; the n is an integer being 1 to 30; the q is an integer being 1 to 10; the t is an integer being 2 to 60. The preparation method is characterized in thata silane mixture containing alkoxy silane and chlorosilane is used as a raw material; the raw material is sequentially subjected to hydrolysis-condensation reaction, end capping reaction and aftertreatment to prepare the addition type organic silicon resin. The addition type organic silicon resin with narrow molecular weight distribution and extremely low residual hydrogen chloride content is prepared by the process; the addition organic silicon impregnating varnish is prepared by using the addition type organic silicon resin as raw materials; the volatile quantity at 200 DEG C / 1h is extremely low.

Description

technical field [0001] The invention relates to the technical field of silicone resins, in particular to an addition-type silicone resin and its preparation method and its application in the preparation of low-volatility one-component addition-type silicone dipping varnish. Background technique [0002] Silicone impregnating varnish is a kind of important insulating material based on silicone resin. It is a kind of thermosetting polysiloxane system with highly cross-linked structure. A polyorganosiloxane with a highly cross-linked network structure. Silicone dipping varnish can be divided into condensation type and addition type according to different crosslinking and curing methods. Condensation-type silicone impregnating varnish is a silicone resin prepolymer containing Si—OH, Si-OR and other groups, which is further condensed and cross-linked into a solid product under the action of a catalyst or heated; The polysiloxane with -Vi bond and the siloxane with Si-H bond und...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/04C08G77/06C09D183/04
CPCC08G77/04C08G77/06C09D183/04
Inventor 吴化军李美江许坤来国桥秦长春侯新瑞
Owner 浙江博菲电气股份有限公司
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