CN101649158B - Organosilicon insulating impregnating varnish and preparation method thereof - Google Patents

Organosilicon insulating impregnating varnish and preparation method thereof Download PDF

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CN101649158B
CN101649158B CN2009100343725A CN200910034372A CN101649158B CN 101649158 B CN101649158 B CN 101649158B CN 2009100343725 A CN2009100343725 A CN 2009100343725A CN 200910034372 A CN200910034372 A CN 200910034372A CN 101649158 B CN101649158 B CN 101649158B
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impregnating varnish
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顾嫒娟
张北京
梁国正
袁莉
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Suzhou University
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Abstract

The invention discloses an organosilicon insulating impregnating varnish and a preparation method thereof. The organosilicon insulating impregnating varnish comprises a component A and a component B in a weight ratio of 1:1, wherein the component A comprises 100 parts of polymethylphenylvinylsiloxane and 0.9-1.5 parts of platinum catalyst and the component B comprises 30-75 parts of polyhedral oligomeric silsesquioxane with ethylene group and 40-60 parts of hyperbranched polysiloxane with Si-H bond. The polymethylphenylvinylsiloxane synthesized in the preparation method of the invention adopts ethanol as solvent and is no non-toxic and non-harmful; when the prepared impregnating varnish is solidified, no by-product with low molecular weight is discharged, thus not affecting the electric performance of the insulating material; in addition the impregnating varnish has good post impregnation effect, high temperature resistance and environmental friend.

Description

A kind of organic silicon insulation impregnating varnish and preparation method thereof
Technical field
The present invention relates to a kind of organic silicon insulation impregnating varnish; Be particularly related to a kind of high temperature resistant, solvent-free organic silicon insulation impregnating varnish and preparation method thereof, it be a kind of with polyphenylmethyl base vinylsiloxane be base resin, to contain vinyl polyhedral oligomeric silsesquioxane (POSS-Vi) be the heatproof auxiliary agent, contain LV that si-h bond hyperbranched polyorganosiloxane (HBPSi-H) is thinner and linking agent, high temperature resistant, solvent-free, solidify the bi-component organic silicon insulating impregnating varnish soon.
Background technology
Continuous progress along with science and technology; Equipment such as electrical equipment and electrical are towards high-power, frequency conversionization, miniaturization and, highly efficient durable and intelligent direction development; Simultaneously, the power transmission and transformation product develops to high-voltage, large vol and long-distance transmissions direction, and insulation system is for realizing that above-mentioned target is most important; Therefore, the q&r of raising insulating material is very urgent.
At present, the silicone impregnating varnish of report is main both at home and abroad has two big types:
First kind is that the solvent-type organosilicon insulating impregnating varnish is arranged, and curing mechanism is prepolymer further condensation and the crosslinking curing under heating and catalyst action that contains Si-OH, Si-OR, Si-H key.Like product DC-901, the DC-980 of Dow corning company, product TSR-103, the TSR-104 of organosilicon company of Japanese Toshiba, product 955 of Chinese morning twilight chemical research institute etc.This type impregnating varnish exist difficult dry, after-tack and shortcoming such as degree of crosslinking is wayward, and be solvent mostly with YLENE or toluene, have solvent to emit during curing, contaminate environment, harm humans is healthy; The micromolecular water that generates is prone to produce bubble, influences the final performance of paint film.And this type of impregnating varnish mostly is H level (180 ℃), can't satisfy the request for utilization of big motor of present high pressure and high-temperature electric machine.
Second kind is the no-solvent type organic silicon insulation impregnating varnish, and curing mechanism is that siloxanes that contains the Si-Vi key and the siloxanes (linking agent) that contains the Si-H key under the platinum catalyst effect hydrogen silication addition reaction take place and crosslinked.Such impregnating varnish is suitable for vacuum pressure impregnation (VPI) technology, like the TJ1173 of China, the H62C of Germany, the SIB3551 of Switzerland, the KR2019 of Japan etc.The solvent-free organic silicon impregnating varnish does not contain solvent, and condition of cure is gentle, does not have low molecule by product and emits, and can realize zero volatilization, and have high temperature high voltage resistant, anti-corona, hydrophobic nature is good, insulativity is excellent and advantage such as environmental protection.But no-solvent type silicone impregnating varnish viscosity is too big at present, and temperature tolerance needs further to improve, and when synthesizing base resin, still uses toluene to be solvent mostly, contaminate environment, and harm humans is healthy.
In sum, there are some problems in the prior art for preparing silicone impregnating varnish.Therefore, providing a kind of nontoxic, LV that the base resin degree of crosslinking is easy to control, environmentally friendly, heat-resistant solvent-free organic silicon insulation impregnating varnish and preparation method thereof to have important use is worth and academic significance.
Summary of the invention
In order to overcome the deficiency that prior art exists, the object of the present invention is to provide a kind of nontoxic, LV that the base resin degree of crosslinking is easy to control, environmentally friendly, heat-resistant solvent-free organic silicon insulation impregnating varnish and preparation method thereof.
Realize that the technical scheme that the object of the invention adopted is: a kind of organic silicon insulation impregnating varnish, by weight, it comprises A, B component, wherein the A component comprises 100 parts polyphenylmethyl base vinylsiloxane and 0.9~1.5 part platinum catalyst; The B component comprise 30~75 parts contain vinyl polyhedral oligomeric silsesquioxane and 40~60 parts contain the si-h bond hyperbranched polyorganosiloxane; A, B component are equal proportion.
A kind of preparation method of solvent-free organic silicon insulation impregnating varnish, its step is following:
(1) preparation A component:
By weight, 65~100 parts of methyltrimethoxy silanes, 280~420 parts of dimethoxydiphenylsilanes and 100~150 parts of vinyltrimethoxy silanes are dissolved in 260~400 parts of ethanol, slowly drip 85~120 parts of deionized waters; Using hydrochloric acid to regulate pH is 2.8~3.5, after 7~9 hours, obtains not end capped polyphenylmethyl base vinylsiloxane solution through 2~3 hours, 70~80 ℃ condensation reactions of 30~50 ℃ of hydrolysis treatment again;
By weight, 40~60 parts SWS-F 221s and 5~10 parts of deionized waters are dissolved in 20~60 parts of ethanol, adding hydrochloric acid adjusting pH is 3.0~6.0; In hydrolysis treatment under 30~80 ℃ the temperature condition after 1~3 hour; Slowly join resulting solution in the above-mentioned not end capped polyphenylmethyl base vinylsiloxane solution, reaction is 6~8 hours under 70~80 ℃ temperature condition, standing demix; Obtain layer oily matter, be polyphenylmethyl base vinylsiloxane;
The platinum catalyst of 100 parts of above-mentioned polyphenylmethyl base vinylsiloxanes and 0.9~1.5 part is mixed, obtain the A component;
(2) preparation B component:
By weight; 100~150 parts of vinyltrimethoxy silanes or 130~200 parts of vinyltriethoxysilanes are dissolved in 260~390 parts of ethanol; Slowly drip 40~60 parts of deionized waters, using hydrochloric acid to regulate pH is 3.0~3.5, reacts 10 hours down at the temperature condition of nitrogen atmosphere and 60 ℃; Reaction finishes the back steams and desolventizes, and adds acetone, and what promptly get the white crystal shape after the sedimentation contains the vinyl polyhedral oligomeric silsesquioxane;
By weight; 100~150 parts of Trimethoxy silanes or 120~180 parts of triethoxyl silanes are dissolved in 130~330 parts of methyl alcohol; Slowly drip 17~40 parts of deionized waters; Using hydrochloric acid to regulate pH is 3.0~6.0, is hydrolysis 2~3 hours under 0~30 ℃ of condition in nitrogen atmosphere, temperature, obtains first solution; 80~120 parts SWS-F 221s and 10~15 parts of deionized waters are dissolved in 60~90 parts of ethanol, and adding hydrochloric acid adjusting pH is 3.0~6.0, and hydrolysis treatment obtained second solution in 1~3 hour under 30~80 ℃ temperature condition; Second solution is slowly joined in the first solution, and reaction is 6~10 hours under 60~80 ℃ temperature condition, and standing demix obtains layer oily matter, is to contain the si-h bond hyperbranched polyorganosiloxane;
The above-mentioned si-h bond hyperbranched polyorganosiloxane that contains that 30~75 parts above-mentioned is contained vinyl polyhedral oligomeric silsesquioxane and 40~60 parts mixes, and obtains the B component;
(3) A, B component equal proportion are mixed, obtain solvent-free organic silicon insulation impregnating varnish.
Solvent-free organic silicon insulation impregnating varnish provided by the invention solidifies through the addition reaction between the active function groups on the molecular chain, and its reaction formula is represented as follows:
Figure G2009100343725D00031
The present invention is directed to that the solvent-type organosilicon impregnating varnish exists when being used for the VPI technology insulation processing of motor; Can not get not having the globality insulation system of air gap; In use discharge a large amount of organic solvents, and solvent-free organic silicon impregnating varnish viscosity is too big, the whole weak effect that soaks; Temperature tolerance waits not enough inadequately, and a kind of heat-resistant solvent-free organic silicon insulation impregnating varnish and preparation method thereof is provided.Institute's synthetic polyphenylmethyl base vinylsiloxane with ethanol is solvent, and is nontoxic, harmless, and in addition, prepared impregnating varnish does not have low molecule by product when solidifying emits, and does not influence the electric property of insulating material, and puts in order and soak effective, high temperature resistant, environmental protection.
Embodiment
Below in conjunction with embodiment the present invention is further described:
Embodiment 1
1) polyphenylmethyl base vinylsiloxane is synthetic: 65 parts of methyltrimethoxy silanes, 280 parts of dimethoxydiphenylsilanes, 100 parts of vinyltrimethoxy silanes are dissolved in 260 parts of ethanol; Slowly drip 85 parts of de-ionizeds; And use hydrochloric acid adjusting pH is 3.5; After 7 hours, get solution 1# through 2 hours, 80 ℃ condensation reactions of 50 ℃ of hydrolysis reaction; 40 parts of SWS-F 221s and 5 parts of deionized waters are dissolved in 20 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 3.0,80 ℃ of hydrolysis got solution 2# in 1 hour; Solution 2# is slowly poured among the solution 1#, 70 ℃ the reaction 8 hours after standing demix get layer oily matter, be polyphenylmethyl base vinylsiloxane;
2) contain the synthetic of vinyl polyhedral oligomeric silsesquioxane: 100 parts of vinyltrimethoxy silanes are dissolved in 260 parts of ethanol; Slowly drip 40 parts and add deionized water and a certain amount of hydrochloric acid; Regulating pH is 3.5, under nitrogen atmosphere and 60 ℃ of conditions, reacts 10 hours, steams solvent; Add a certain amount of acetone sedimentation, promptly get and contain vinyl polyhedral oligomeric silsesquioxane white crystal;
3) contain the synthetic of si-h bond hyperbranched polyorganosiloxane: 100 parts of Trimethoxy silanes are dissolved in 130 parts of methyl alcohol, and slowly drip 17 parts of deionized waters and a certain amount of hydrochloric acid, regulating pH is 3.0, and hydrolysis got solution 3# in 2 hours under nitrogen atmosphere and condition of ice bath; 80 parts of SWS-F 221s and 10 parts of deionized waters are dissolved in 60 ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 3.0,50 ℃ of hydrolysis got solution 4# in 2 hours; Solution 4# is slowly poured among the solution 3#, 60 ℃ of reactions after 10 hours standing demix get layer oily matter, be and contain the si-h bond hyperbranched polyorganosiloxane;
4) preparation of solvent-free organic silicon insulation impregnating varnish: by weight, 100 parts of polyphenylmethyl base vinylsiloxanes and 0.9 part of platinum catalyst are mixed formation A component; Containing vinyl polyhedral oligomeric silsesquioxane and 40 parts with 30 parts contains the si-h bond hyperbranched polyorganosiloxane and mixes and form the B component; A, B component are packed respectively, and equal proportion is mixed during use, can obtain solvent-free organic silicon insulation impregnating varnish.
Embodiment 2
1) polyphenylmethyl base vinylsiloxane is synthetic: 80 parts of methyltrimethoxy silanes, 340 parts of dimethoxydiphenylsilanes, 120 parts of vinyltrimethoxy silanes are dissolved in 300 parts of ethanol; Slowly drip 90 parts of deionized waters and a certain amount of hydrochloric acid; Regulating pH is 3.0; After 9 hours, get solution 1# through 30 ℃ of hydrolysis 3 hours, 70 ℃ of condensation reactions; 50 parts of SWS-F 221s and 7 parts of deionized waters are dissolved in 35 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is about 4, and 50 ℃ of hydrolysis got solution 2# in 2 hours; Solution 2# is slowly poured among the solution 1#, 80 ℃ the reaction 6 hours after standing demix get layer oily matter, be polyphenylmethyl base vinylsiloxane.
2) contain the synthetic of vinyl polyhedral oligomeric silsesquioxane: 110 parts of vinyltrimethoxy silanes are dissolved in 290 parts of ethanol; Slowly drip 45 parts and add deionized water and a certain amount of hydrochloric acid; Regulating pH is 3.3, under nitrogen atmosphere and 60 ℃ of conditions, reacts 10 hours, steams solvent; Add a certain amount of acetone sedimentation, promptly get and contain vinyl polyhedral oligomeric silsesquioxane white crystal.
3) contain the synthetic of si-h bond hyperbranched polyorganosiloxane: 120 parts of Trimethoxy silanes are dissolved in 175 parts of methyl alcohol, and slowly drip 25 parts of deionized waters and a certain amount of hydrochloric acid, regulating pH is 4, under nitrogen atmosphere and 5 ℃ of conditions hydrolysis 2 hours solution 3#; 100 parts of SWS-F 221s and 12 parts of deionized waters are dissolved in 72 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 5.5,30 ℃ of hydrolysis got solution 4# in 3 hours; Solution 4# is slowly poured among the solution 3#, 80 ℃ of reactions after 6 hours standing demix get layer oily matter, be and contain the si-h bond hyperbranched polyorganosiloxane;
4) preparation of solvent-free organic silicon insulation impregnating varnish: by weight, 100 parts of polyphenylmethyl base vinylsiloxanes and 1.1 parts of platinum catalysts are mixed formation A component; With 50 parts contain vinyl polyhedral oligomeric silsesquioxane and 50 parts contain the si-h bond hyperbranched polyorganosiloxane mix form B component A, the B component is packed respectively, equal proportion is mixed and is got final product during use.
Embodiment 3
1) polyphenylmethyl base vinylsiloxane is synthetic: 90 parts of methyltrimethoxy silanes, 390 parts of dimethoxydiphenylsilanes, 135 parts of vinyltrimethoxy silanes are dissolved in 300 parts of ethanol; Slowly drip 100 parts of deionized waters and a certain amount of hydrochloric acid; Regulating pH is 2.8; After 8 hours, get solution 1# through 40 ℃ of hydrolysis 2.5 hours, 75 ℃ of condensation reactions; 55 parts of SWS-F 221s and 8 parts of deionized waters are dissolved in 40 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 6.0,30 ℃ of hydrolysis got solution 2# in 3 hours; Solution 2# is slowly poured among the solution 1#, 75 ℃ the reaction 7 hours after standing demix get layer oily matter, be polyphenylmethyl base vinylsiloxane;
2) contain the synthetic of vinyl polyhedral oligomeric silsesquioxane: 130 parts of vinyltriethoxysilanes are dissolved in 260 parts of ethanol; Slowly drip 40 parts of deionized waters and a certain amount of hydrochloric acid; Regulating pH is 3.0, under nitrogen atmosphere and 60 ℃ of conditions, reacts 10 hours, steams solvent; Add a certain amount of acetone sedimentation, promptly get and contain vinyl polyhedral oligomeric silsesquioxane white crystal;
3) contain the synthetic of si-h bond hyperbranched polyorganosiloxane: 120 parts of triethoxyl silanes are dissolved in 170 parts of methyl alcohol, and slowly drip 17 parts of deionized waters and a certain amount of hydrochloric acid, regulating pH is 6.0, under nitrogen atmosphere and 30 ℃ of conditions hydrolysis 2 hours solution 3#; 100 parts of SWS-F 221s and 12 parts of deionized waters are dissolved in 70 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 4.1,70 ℃ of hydrolysis got solution 4# in 2 hours; Solution 4# is slowly poured among the solution 3#, 70 ℃ of reactions after 8 hours standing demix get layer oily matter, be and contain the si-h bond hyperbranched polyorganosiloxane;
4) preparation of solvent-free organic silicon insulation impregnating varnish: by weight, 100 parts of polyphenylmethyl base vinylsiloxanes and 1.2 parts of platinum catalysts are mixed formation A component; With 60 parts contain vinyl polyhedral oligomeric silsesquioxane and 60 parts contain the si-h bond hyperbranched polyorganosiloxane mix form B component A, the B component is packed respectively, equal proportion is mixed and is got final product during use.
Embodiment 4
1) polyphenylmethyl base vinylsiloxane is synthetic: 100 parts of methyltrimethoxy silanes, 420 parts of dimethoxydiphenylsilanes, 150 parts of vinyltrimethoxy silanes are dissolved in 400 parts of ethanol; Slowly drip 120 parts of deionized waters and a certain amount of hydrochloric acid; Regulating pH is 3.2; After 8 hours, get solution 1# through 40 ℃ of hydrolysis 2.5 hours, 75 ℃ of condensation reactions; 60 parts of SWS-F 221s and 10 parts of deionized waters are dissolved in 60 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is about 5, and 70 ℃ of hydrolysis got solution 2# in 2 hours; Solution 2# is slowly poured among the solution 1#, 75 ℃ the reaction 7 hours after standing demix get layer oily matter, be polyphenylmethyl base vinylsiloxane;
2) contain the synthetic of vinyl polyhedral oligomeric silsesquioxane: 150 parts of vinyltrimethoxy silanes are dissolved in 390 parts of ethanol; Slowly drip 60 parts and add deionized water and a certain amount of hydrochloric acid; Regulating pH is 3.5, under nitrogen atmosphere and 60 ℃ of conditions, reacts 10 hours, steams solvent; Add a certain amount of acetone sedimentation, promptly get and contain vinyl polyhedral oligomeric silsesquioxane white crystal;
3) contain the synthetic of si-h bond hyperbranched polyorganosiloxane: 150 parts of Trimethoxy silanes are dissolved in 330 parts of methyl alcohol, and slowly drip 40 parts of deionized waters and a certain amount of hydrochloric acid, regulating pH is 5.0, under nitrogen atmosphere and 10 ℃ of conditions hydrolysis 2 hours solution 3#; 120 parts of SWS-F 221s and 15 parts of deionized waters are dissolved in 90 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 6.0,50 ℃ of hydrolysis got solution 4# in 2.5 hours; Solution 4# is slowly poured among the solution 3#, 80 ℃ of reactions after 6 hours standing demix get layer oily matter, be and contain the si-h bond hyperbranched polyorganosiloxane;
4) preparation of solvent-free organic silicon insulation impregnating varnish: by weight, 100 parts of polyphenylmethyl base vinylsiloxanes and 1.5 parts of platinum catalysts are mixed formation A component; Containing vinyl polyhedral oligomeric silsesquioxane and 46 parts with 40 parts contains the si-h bond hyperbranched polyorganosiloxane and mixes and form the B component; A, B component are packed respectively, and the equal proportion mixing gets final product during use.
Embodiment 5
1) polyphenylmethyl base vinylsiloxane is synthetic: 100 parts of methyltrimethoxy silanes, 400 parts of dimethoxydiphenylsilanes, 140 parts of vinyltrimethoxy silanes are dissolved in 300 parts of ethanol; Slowly drip 120 parts of deionized waters and a certain amount of hydrochloric acid; Regulating pH is 3.5; After 8 hours, get solution 1# through 30 ℃ of hydrolysis 3 hours, 75 ℃ of condensation reactions; 60 parts of SWS-F 221s and 10 parts of deionized waters are dissolved in 60 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 4.5,40 ℃ of hydrolysis got solution 2# in 2.5 hours; Solution 2# is slowly poured among the solution 1#, 75 ℃ the reaction 7 hours after standing demix get layer oily matter, be polyphenylmethyl base vinylsiloxane.
2) contain the synthetic of vinyl polyhedral oligomeric silsesquioxane: 200 parts of vinyltriethoxysilanes are dissolved in 350 parts of ethanol; Slowly drip 60 parts and add deionized water and a certain amount of hydrochloric acid; Regulating pH is 3.1, under nitrogen atmosphere and 60 ℃ of conditions, reacts 10 hours, steams solvent; Add a certain amount of acetone sedimentation, promptly get and contain vinyl polyhedral oligomeric silsesquioxane white crystal.
3) contain the synthetic of si-h bond hyperbranched polyorganosiloxane: 180 parts of triethoxyl silanes are dissolved in 300 parts of methyl alcohol, and slowly drip 40 parts of deionized waters and a certain amount of hydrochloric acid, regulating pH is 3.0, under nitrogen atmosphere and 20 ℃ of conditions hydrolysis 3 hours solution 3#; 120 parts of SWS-F 221s and 15 parts of deionized waters are dissolved in 90 parts of ethanol, and add a certain amount of hydrochloric acid, regulating pH is that 3.6,80 ℃ of hydrolysis got solution 4# in 1 hour; Solution 4# is slowly poured among the solution 3#, 80 ℃ of reactions after 8 hours standing demix get layer oily matter, be and contain the si-h bond hyperbranched polyorganosiloxane.
4) preparation of solvent-free organic silicon insulation impregnating varnish: by weight, 100 parts of polyphenylmethyl base vinylsiloxanes and 1.0 parts of platinum catalysts are mixed formation A component; Containing vinyl polyhedral oligomeric silsesquioxane and 52 parts with 75 parts contains the si-h bond hyperbranched polyorganosiloxane and mixes and form the B component; A, B component are packed respectively, and the equal proportion mixing gets final product during use.

Claims (2)

1. the preparation method of an organic silicon insulation impregnating varnish is characterized in that step is following:
(1) preparation A component:
By weight, 65~100 parts of methyltrimethoxy silanes, 280~420 parts of dimethoxydiphenylsilanes and 100~150 parts of vinyltrimethoxy silanes are dissolved in 260~400 parts of ethanol, slowly drip 85~120 parts of deionized waters; Using hydrochloric acid to regulate pH is 2.8~3.5, after 7~9 hours, obtains not end capped polyphenylmethyl base vinylsiloxane solution through 2~3 hours, 70~80 ℃ condensation reactions of 30~50 ℃ of hydrolysis treatment again;
By weight, 40~60 parts SWS-F 221s and 5~10 parts of deionized waters are dissolved in 20~60 parts of ethanol, adding hydrochloric acid adjusting pH is 3.0~6.0; In hydrolysis treatment under 30~80 ℃ the temperature condition after 1~3 hour; Slowly join resulting solution in the above-mentioned not end capped polyphenylmethyl base vinylsiloxane solution, reaction is 6~8 hours under 70~80 ℃ temperature condition, standing demix; Obtain layer oily matter, be polyphenylmethyl base vinylsiloxane;
The platinum catalyst of 100 parts of above-mentioned polyphenylmethyl base vinylsiloxanes and 0.9~1.5 part is mixed, obtain the A component;
(2) preparation B component:
By weight; 100~150 parts of vinyltrimethoxy silanes or 130~200 parts of vinyltriethoxysilanes are dissolved in 260~390 parts of ethanol; Slowly drip 40~60 parts of deionized waters, using hydrochloric acid to regulate pH is 3.0~3.5, reacts 10 hours down at the temperature condition of nitrogen atmosphere and 60 ℃; Reaction finishes the back steams and desolventizes, and adds acetone, and what promptly get the white crystal shape after the sedimentation contains the vinyl polyhedral oligomeric silsesquioxane;
By weight; 100~150 parts of Trimethoxy silanes or 120~180 parts of triethoxyl silanes are dissolved in 130~330 parts of methyl alcohol; Slowly drip 17~40 parts of deionized waters; Using hydrochloric acid to regulate pH is 3.0~6.0, is hydrolysis 2~3 hours under 0~30 ℃ of condition in nitrogen atmosphere, temperature, obtains first solution; 80~120 parts SWS-F 221s and 10~15 parts of deionized waters are dissolved in 60~90 parts of ethanol, and adding hydrochloric acid adjusting pH is 3.0~6.0, and hydrolysis treatment obtained second solution in 1~3 hour under 30~80 ℃ temperature condition; Second solution is slowly joined in the first solution, and reaction is 6~10 hours under 60~80 ℃ temperature condition, and standing demix obtains layer oily matter, is to contain the si-h bond hyperbranched polyorganosiloxane;
The above-mentioned si-h bond hyperbranched polyorganosiloxane that contains that 30~75 parts above-mentioned is contained vinyl polyhedral oligomeric silsesquioxane and 40~60 parts mixes, and obtains the B component;
(3) A, B component equal proportion are mixed, obtain solvent-free organic silicon insulation impregnating varnish.
2. organic silicon insulation impregnating varnish, it is characterized in that: by weight, it comprises A, B component, wherein the A component comprises 100 parts polyphenylmethyl base vinylsiloxane and 0.9~1.5 part platinum catalyst; The B component comprise 30~75 parts contain vinyl polyhedral oligomeric silsesquioxane and 40~60 parts contain the si-h bond hyperbranched polyorganosiloxane; A, B component are equal proportion; Said polyphenylmethyl base vinylsiloxane, contain the vinyl polyhedral oligomeric silsesquioxane and contain the si-h bond hyperbranched polyorganosiloxane and adopt the preparation method of claim 1 to prepare.
CN2009100343725A 2009-08-25 2009-08-25 Organosilicon insulating impregnating varnish and preparation method thereof Expired - Fee Related CN101649158B (en)

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