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A kind of silicone resin for one-component addition type silicone dipping paint and its preparation method and application

A silicone impregnation and addition technology, applied in the direction of coating, can solve the problems of difficult control, dehydrogenation reaction, environmental pollution and so on

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] Charge 2 mol (480 g) of PhSi(OEt) in a 5000 ml glass bottle equipped with stirrer, heating, condenser distillation and dropping funnel 3 、1mol(134g)MeHSi(OEt) 2 , 1mol (160g) MeViSi (OEt) 2 , 0.5mol (52g) Me 3 SiOMe, heated to 60 °C. Under stirring, 699g of 15% hydrochloric acid (containing 105g of HCl and 594g of water) was added dropwise through the dropping funnel, and the dropping time was 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 510 g of silane hydrolyzate.

[0052] Add 500 g of ethyl acetate and 25 g of trimethylchlorosilane to the above 510 g of silane hydrolyzate, raise the temperature to 60...

Embodiment 2

[0062] Charge 6 mol (1188 g) of PhSi(OMe) in a 10000 ml glass bottle equipped with stirrer, heating, condenser distillation and dropping funnel 3 、3mol(402g)MeHSi(OEt) 2 , 1mol (132g) MeViSi (OMe) 2 , 2.0mol (236g) Me 3 SiOEt, heated to 30 °C. Under stirring, 3874g of 3% hydrochloric acid (containing 116g of HCl and 3758g of water) was added dropwise through the dropping funnel for 30 minutes. 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 1370 g of silane hydrolyzate.

[0063] Add 700 g of dichloromethane and 15 g of trimethylchlorosilane to the above 1370 g of silane hydrolyzate, raise the temperature...

Embodiment 3

[0073] Charge 3.0 mol (720 g) PhSi(OEt) in a 5000 ml glass bottle equipped with stirrer, heating, condenser distillation and dropping funnel 3 , 1.5mol (201g) MeHSi (OEt) 2 , 1mol (160g) MeViSi (OEt) 2 , 1.5mol (177g) Me 3 SiOEt, heated to 45 °C. Under stirring, 1271g of 8% hydrochloric acid (containing 101g of HCl and 1170g of water) was added dropwise through the dropping funnel for 20 minutes. 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 750 g of silane hydrolyzate.

[0074] Add 700g of petroleum ether (boiling range 60-90) and 25g of trimethylchlorosilane to the above 750g of silane hydro...

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Abstract

The invention discloses an organic silicone resin for a single-component addition organosilicon impregnating varnish and a preparation method thereof, and application of the organic silicone resin topreparation of the low-volatilization single-component addition organosilicon impregnating varnish. The organic silicone resin for the single-component addition organosilicon impregnating varnish hasa structural formula of (Me<3>SiO<0.5>)<m>(MeHSiO)<n>(MeViSiO)<q>(PhSiO<1.5>)<t>, wherein m is an integer in a range of 1 to 20, n is an integer in a range of 1 to 30, q is an integer in a range of 1to 10, and t is an integer in a range of 2 to 60. The preparation method comprises the following steps: with an alkoxysilane mixture as a raw material, successively carrying out a hydrolysis-condensation reaction, a capping reaction and post-treatment so as to obtain the organic silicone resin. The organic silicone resin prepared by using the method is narrow in molecular weight distribution and low in the content of residual hydrogen chloride; and the single-component addition organosilicon impregnating varnish prepared with the organic silicone resin as a raw material has extremely low volatilization amount at 200 DEG C / 1 h.

Description

technical field [0001] The invention relates to the technical field of silicone resins, in particular to a silicone resin for a one-component addition type silicone dipping varnish, a preparation method thereof and its application in the preparation of a low-volatile 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 wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/20C08G77/12C09D183/07C09D183/05
CPCC08G77/12C08G77/20C08G77/70C08G77/80C09D183/04
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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