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Low-hydroxyl hydrogen-containing vinyl phenyl organic silicon resin and preparation method thereof

A technology of hydrogen vinyl phenyl and silicone, which is applied in the field of low hydroxyl hydrogen-containing vinyl phenyl silicone resin and its preparation, can solve the problems of poor viscosity stability, poor electrical insulation performance, high hydroxyl content, etc., and achieve excellent durability Thermal, mild and controllable reaction process, effect of reducing oligomer and silanol content

Active Publication Date: 2020-08-25
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the high hydroxyl content in the hydrolyzed silicone resin in the prior art, resulting in poor viscosity stability during storage, poor electrical insulation performance after curing, and at the same time, the existing methods for eliminating hydroxyl groups are relatively cumbersome and not environmentally friendly. , provides a low-hydroxyl hydrogen-containing vinyl phenyl silicone resin, which has mild preparation conditions, low silanol content in the product, good viscosity stability, and excellent electrical insulation performance of the organosilicon impregnating varnish prepared from it At the same time, it also provides an environmentally friendly, non-corrosive, and simple post-processing preparation method for the silicone resin

Method used

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  • Low-hydroxyl hydrogen-containing vinyl phenyl organic silicon resin and preparation method thereof
  • Low-hydroxyl hydrogen-containing vinyl phenyl organic silicon resin and preparation method thereof
  • Low-hydroxyl hydrogen-containing vinyl phenyl organic silicon resin and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0050] PO(CH 2 OMe 2 SiC 3 h 6 NCO) 3 preparation

[0051] (a) 140g trihydroxymethyl phosphine oxide is put into reaction flask with three-way valve, stirring and constant pressure dropping funnel, evacuated nitrogen three times, 500ml toluene is injected in the reaction flask, 735g dimethylaminopropyl Dissolve methoxysilane in 200ml of toluene, put it into a constant pressure dropping funnel, and drop it into the reaction flask within 30 minutes. After the dropwise addition, the reaction was heated to reflux for 12h. Reaction finishes, evaporates solvent, excess dimethylaminopropyl methoxy silane and low boiler, obtains 485g PO (CH 2 OMe 2 SiC 3 h 6 NH 2 ) 3 .

[0052] (b) 485g PO(CH 2 OMe 2 SiC 3 h 6 NH 2 ) 3 Put it into a reaction flask equipped with a three-way valve, stirring and a constant pressure dropping funnel, evacuate and pass nitrogen three times, inject 1000ml of benzene and 600g of triethylamine into the reaction flask, and cool to -5°C. Add 2...

Embodiment 2

[0055] 378g water, 83g hydrogen type strongly acidic cation exchange resin, 41g p-toluenesulfonic acid, 450g toluene are charged in the reaction flask equipped with stirrer, heating, condenser distillation and dropping funnel. Under stirring, drop 2mol (480g) PhSi(OEt) through the dropping funnel 3 、1mol(134g)MeHSi(OEt) 2 , 1mol (160g) MeViSi (OEt) 2 , 0.5mol (52g) Me 3 SiOMe mixture, the dropping time is 25min. Raise the temperature to 70°C and react for 3h. After the reaction is complete, cool to room temperature. The solid was filtered off, and the acid water was separated. The organic layer was washed 500 mL×3 times with water until neutral, and the toluene was distilled off. The temperature was raised to 150° C. and maintained at a vacuum pressure of 50 hPa for 4 hours to obtain 450 g of silane hydrolyzate.

[0056] Under nitrogen protection, add 45g PO(CH 2 OMe 2 SiC 3 h 6 NCO) 3 , temperature controlled to 30°C, and reacted for 8h. After the reaction was co...

Embodiment 3

[0064] 4032g of water, 390g of hydrogen-type strongly acidic cation exchange resin, 25g of p-toluenesulfonic acid, and 1900g of benzene were charged into a reaction flask equipped with a stirrer, heating, condenser distillation and dropping funnel, and were stirred by dropping Add 6mol (1188g) PhSi(OMe) dropwise into the funnel 3 、3mol(402g)MeHSi(OEt) 2 , 1mol (132g) MeViSi (OMe) 2 , 2.0mol (236g) Me 3 SiOEt mixture, the dropwise addition time is 30min. Raise the temperature to 50°C and react for 8h. After the reaction is complete, cool to room temperature, filter off the solid, and separate the acid water. The organic layer was washed 1000mL×3 times with water until neutral, and the solvent benzene was distilled off. The temperature was raised to 100° C., and the vacuum pressure was maintained at 80 hPa for 2 hours to obtain 1250 g of organosilicon hydrolyzate.

[0065] Under nitrogen protection, add 108g PO(CH 2 OMe 2 SiC 3 h 6 NCO) 3 , heated up to 80°C, and reac...

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Abstract

The invention relates to the technical field of organic silicon resin, specifically to low-hydroxyl hydrogen-containing vinyl phenyl organic silicon resin. The general structural formula of the low-hydroxyl hydrogen-containing vinyl phenyl organic silicon resin is [Me<3>SiO<0.5>]<m>[MeHSiO]<n>[MeViSiO]<q>[PhSiO<1.5>]<t>[(PO)<1 / 3>(CH<2>OMe<2>SiC<3>H<6>NHCOO<0.5>)], wherein m is an integer in a range of 1 to 10, n is an integer in a range of 1 to 15, q is an integer in a range of 1 to 10, t is an integer in a range of 5 to 30, and p is an integer in a range of 1 to 3. The preparation method comprises the following steps: with an alkoxy silane mixture as a raw material, carrying out a hydrolysis-condensation reaction and PO(CH2OMe<2>SiC<4>H<8>NCO)<3> end-capping reaction under the co-catalysis of hydrogen-type strong-acid cation exchange resin and p-toluenesulfonic acid. The organic silicon resin and the preparation method in the invention overcomes the defects that silicon resin prepared in the prior art has high hydroxyl content and is thus poor in storage viscosity stability and electrical insulation property; and the organic silicon resin prepared in the invention is relativelylow in silicon hydroxyl content and good in viscosity stability in a storage period, and single-component addition type organic silicon impregnating varnish prepared by taking the organic silicon resin as a raw material is excellent in electrical insulation property after being cured.

Description

technical field [0001] The invention relates to the technical field of silicone resins, in particular to a low-hydroxyl hydrogen-containing vinylphenyl silicone resin and a preparation method thereof. Background technique [0002] Silicone resin is a polyorganosiloxane with a highly cross-linked network structure with Si-O-Si as the main chain and organic groups connected to silicon atoms. According to different cross-linking and curing methods, it can be divided into condensation type and addition type. Condensation-type silicone resin 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 under heating; addition-type silicone resin is obtained by containing Si-Vi Bonded siloxane and Si-H bond-containing siloxane undergo a hydrosilylation addition reaction under the action of a catalyst to cross-link. [0003] Compared with condensation-type silicone resins...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06C09D183/07C09D5/25
CPCC08G77/20C08G77/06C09D183/04C09D5/00
Inventor 李美江刘美辰侯新瑞宋华锋
Owner HANGZHOU NORMAL UNIVERSITY
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