CN104086772A - Uramido modified MQ silicon resin, and preparation method and application thereof - Google Patents
Uramido modified MQ silicon resin, and preparation method and application thereof Download PDFInfo
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- CN104086772A CN104086772A CN201410290272.XA CN201410290272A CN104086772A CN 104086772 A CN104086772 A CN 104086772A CN 201410290272 A CN201410290272 A CN 201410290272A CN 104086772 A CN104086772 A CN 104086772A
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Abstract
The invention discloses a uramido modified MQ silicon resin, and a preparation method and application thereof. The silicon resin is prepared from the following raw materials in percentage by weight: 20-40% of tetra-functionality silicon monomer, 5-30% of siloxane blocking agent, 15-30% of uramido silane coupling agent, 1-10% of catalyst, 5-20% of alcohol and 10-15% of deionized water. The preparation method comprises the following steps: stirring the deionized water, alcohol, catalyst and siloxane blocking agent at 70-80 DEG C to react; dropwisely adding the tetra-functionality silicon monomer/uramido silane coupling agent mixed solution, and reacting while controlling the temperature at 70-80 DEG C; after the dropwise addition, continuing stirring to react for 0.5-2 hours; and extracting, washing, and distilling under reduced pressure to obtain the uramido modified MQ silicon resin. The uramido modified MQ silicon resin has favorable compatibility with silicon rubber and silicon oil, and can obviously enhance the tracking resistance and mechanical properties of the addition-type liquid silicon rubber.
Description
Technical field
The present invention relates to the changing-nature and application of MQ silicone resin, particularly relate to a kind of preparation method of urea groups modification MQ silicone resin and the application in add-on type liquid silicon rubber thereof.
Background technology
Because both there is organic group in its structure in silicone resin, contain again inorganic structure, integrate inorganics and organic characteristic, there is good high-low temperature resistant, weather-resistant, electric insulation, resistance to ozone, difficult combustion, the advantage such as nontoxic and corrosion-free, be widely used in the fields such as defence and military, electric, mechanical, building and communications and transportation.
MQ silicone resin is the silicone resin that a class has tridimensional network, by the silica unit (R of single functionality
3si
1/2, i.e. M unit) and the silica unit (SiO of four functionality
2, i.e. Q unit) and hydrolytic condensation forms, and has excellent thermotolerance, lower temperature resistance, film-forming properties, snappiness, water resisting property and adhesive property, mainly as the tackifier of siloxanes pressure sensitive adhesive and the supporting material of addition-type silicon rubber.According to the needs in different application field, people contain the end-blocking monomer of different functional groups side group by introducing, synthesize containing not isoplastic MQ silicone resin such as vinyl, hydrogen base, phenyl and amino, thereby give MQ silicone resin special performance.Simultaneously, can in MQ silicone resin, introduce some special organic groups such as two functional groups (D unit) and (or) trifunctional (T unit), expanded to the silicone resin of MDQ or MTQ structure, met special demand thereby make it have some property.For example, epoxide modified MQ silicone resin can be used as tackifier and bonding surface treatment agent; The alkali video picture corrosion-resistant material of microfabrication when phenolic group modification MQ silicone resin can be used as large-scale integrated circuit production; Long chain alkyl modified MQ silicone resin can be used for additive and the inner pattern releasing agent applicable of organic resin, has the effect that alleviates internal stress; Polyether-modified MQ silicone resin can be prepared fibre finish.Therefore the MQ silicone resin that, development contains specific function group becomes quite concerned research topic.
US Patent No. 5406245 has reported that urea and derivative thereof are class arc quenching materials, decomposites a large amount of non-combustible gas and play electric arc quenching effect in arc discharge process, is widely used in the equipment such as isolating switch, high-tension fuse and transformer.Chinese patent CN103694709 has reported that the silane compound that contains urea groups can effectively improve the anti creepage trace performance of add-on type liquid silicon rubber.If urea groups is introduced in MQ silicone resin, make urea groups modification MQ silicone resin, can be used for improving the anti creepage trace performance of silicon rubber, have a wide range of applications in fields such as electric outer insulating materials.But not yet find to be so far correlated with paper and patent are delivered.
Summary of the invention
The object of the present invention is to provide a kind of urea groups modification MQ silicone resin and preparation method thereof.
The present invention also aims to provide the application of described urea groups modification MQ silicone resin in add-on type liquid silicon rubber.
Object of the present invention is achieved through the following technical solutions:
A kind of urea groups modification MQ silicone resin, by percentage to the quality, the synthesis material of described urea groups modification MQ silicone resin comprises following component:
Described ureido silane coupling agent is following structural formula:
Wherein R
1, R
2wei ?H, ?(CH
2)
ncH
3huo ?Ph, the integer that n is 0～8; R
3wei ?CH
3huo ?CH
2cH
3;
Described four functionality silicon monomers are the one in methyl silicate, tetraethoxy or water glass;
Described siloxane blocking agent is one or more in hexamethyldisiloxane, tetramethyl divinyl siloxanes or tetramethyl disiloxane;
Described catalyzer is the one in hydrochloric acid, sulfuric acid or tosic acid;
Described alcohol is one or more in ethanol, Virahol or propyl carbinol.
When preparation, be stirring reaction under (70～80) DEG C condition by deionized water, alcohol, catalyzer and siloxane blocking agent in temperature; The mixed solution that drips four functionality silicon monomers and ureido silane coupling agent, temperature of reaction is controlled at (70～80) DEG C; Dropwise rear continuation stirring reaction (0.5～2) h; Extraction, washing, underpressure distillation, obtains urea groups modification MQ silicone resin.
For further realizing object of the present invention, preferably, by percentage to the quality, the synthesis material of described raw material urea groups modification MQ silicone resin also comprises two functionality silicon monomers 0～5%, and described two functionality silicon monomers are one or more in dimethyldimethoxysil,ne, dimethoxydiphenylsilane, aminomethyl phenyl dimethoxy silane, dimethyldiethoxysilane, phenylbenzene diethoxy silane or aminomethyl phenyl diethoxy silane.
By percentage to the quality, the synthesis material of described raw material urea groups modification MQ silicone resin also comprises three-functionality-degree silicon monomer 0～5%; Described three-functionality-degree silicon monomer is one or more in methyltrimethoxy silane, propyl group trimethoxy silane, vinyltrimethoxy silane, phenyltrimethoxysila,e, Union carbide A-162, propyl group three ethoxy silane, vinyltriethoxysilane or phenyl triethoxysilane.
The preparation method of described urea groups modification MQ silicone resin, comprises the following steps:
(1) in reactor, add deionized water, alcohol, catalyzer and siloxane blocking agent, be stirring reaction (0.5～2) h under (70～80) DEG C condition in temperature;
(2) dropwise add the mixed solution of four functionality silicon monomers and ureido silane coupling agent, time for adding is controlled at (2～6) h, and temperature of reaction is controlled at (70～80) DEG C; After dropwising, at (70～80) DEG C, continue stirring reaction (0.5～2) h;
(3) extraction, washing, underpressure distillation, except desolventizing and low-boiling-point substance, obtains urea groups modification MQ silicone resin.
Preferably, in the time that described synthesis material also comprises two functionality silicon monomers and/or three-functionality-degree silicon monomer, described two functionality silicon monomers and/or three-functionality-degree silicon monomer and four functionality silicon monomers and ureido silane coupling agent composition mixed solution.
Preferably, described extraction is for adding toluene extraction.
Preferably, described washing is for extremely neutral mutually with deionized water wash toluene.
The application of described urea groups modification MQ silicone resin in add-on type liquid silicon rubber: 100 mass parts vinyl silicone oils, 40 mass parts thermal silicas and 3～15 mass parts hexamethyldisilazanes are mixed in vacuum kneader, at room temperature stir, be heated to temperature of charge (170 ?180) DEG C continuation mixing, pumping vacuum and mixing again, cooling rear grinding, obtains add-on type liquid silicon rubber sizing; And then add successively containing hydrogen silicone oil, 0.004～0.03 mass parts 1 ?Yi Que Ji ?1 ?the urea groups modification MQ silicone resin, the divinyl tetramethyl disiloxane complex compound of Platinic chloride that platinum content is 3000ppm of hexalin, 1～10 mass parts, at room temperature mix sulfuration (0.1～5) h at (100～150) DEG C; In described containing hydrogen silicone oil, in si-h bond and vinyl silicone oil and urea groups modification MQ silicone resin, the mol ratio of carbon-carbon double bond summation is 1:1～1.8:1; Described platinum atom content accounts for (2～40) ppm of total quality of material.
With respect to prior art, tool of the present invention has the following advantages:
1) the present invention is taking siloxane blocking agent, four functionality silicon monomers, three-functionality-degree silicon monomer, two functionality silicon monomers and ureido silane coupling agent etc. as raw material, hydrolysis-condensation reaction has obtained urea groups modification MQ silicone resin, this modification MQ silicone resin and silicon rubber, silicone oil consistency are good, can significantly improve the anti creepage trace performance of add-on type liquid silicon rubber, in add-on type liquid silicon rubber, add a small amount of (being generally less than 5 mass parts) urea groups modification MQ silicone resin, its anti creepage trace just can reach 1A4.5 level; Meanwhile, mechanical property and hydrophobic performance to add-on type liquid silicon rubber also improve, and curability on add-on type liquid silicon rubber and processing characteristics impact little.
2) the present invention is by progressively dripping controlled hydrolysis speed method, and a step obtains urea groups modification MQ silicone resin, and preparation technology is easy, and process safety is stable, raw material is cheap and easy to get, is easy to realize suitability for industrialized production.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of material; Wherein (a) is that urea groups modification MQ silicone resin 1, (b) are that urea groups modification MQ silicone resin 2, (c) are that urea groups modification MQ silicone resin 3, (d) are that urea groups modification MQ silicone resin 4, (e) are urea groups modification MQ silicone resin 5.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, the present invention is further illustrated, but embodiments of the present invention are not limited to this.
Embodiment 1
By percentage to the quality, the synthesis material of urea groups modification MQ silicone resin 1 comprises following component:
Preparation method: in reactor, adding deionized water, ethanol, concentrated hydrochloric acid, hexamethyldisiloxane and the tetramethyl divinyl disiloxane of above-mentioned raw materials formula, is stirring reaction 0.5h under 80 DEG C of conditions in temperature; Dropwise add tetraethoxy and 3 ?the mixed solution of (di-isopropyl urea groups) propyl-triethoxysilicane, time for adding is controlled at 4h, temperature of reaction is controlled at 80 DEG C; After dropwising, be to continue stirring reaction 0.5h under 80 DEG C of conditions in temperature; Add toluene to extract, with deionized water wash toluene, mutually to neutral, underpressure distillation, except desolventizing and low-boiling-point substance, obtains urea groups modification MQ silicone resin 1.
By 100 mass parts vinyl silicone oils (viscosity at 25 DEG C is 20000mPas, and contents of ethylene is 0.12wt%), (specific surface area is 260m to 40 mass parts thermal silicas
2/ g), 6 mass parts hexamethyldisilazanes mix in vacuum kneader, at room temperature stir 2h, being heated to 170 DEG C of temperature of charge and continuing mixing 2h, then pumping vacuum and mixing 1h, grinds through three-roller after cooling, obtains add-on type liquid silicon rubber basis glue;
In above-mentioned 100 mass parts sizings, (viscosity at 25 DEG C is 160mPas to add 2.68 mass parts urea groups modification MQ silicone resin 1,2.59 mass parts containing hydrogen silicone oils, hydrogen content is 0.5wt%), 0.01 mass parts 1 ?Yi Que Ji ?1 ?the divinyl tetramethyl disiloxane complex compound (platinum content is 3000ppm) of hexalin and 0.25 mass parts Platinic chloride, at room temperature stir, mold pressing 10min at 120 DEG C, make the film that 6mm and 2mm are thick, carry out respectively anti creepage trace test and Mechanics Performance Testing.The performance of sample is as shown in table 1.
Embodiment 2
By percentage to the quality, the synthesis material of urea groups modification MQ silicone resin 2 comprises following component:
Preparation method: in reactor, adding deionized water, ethanol, the vitriol oil, hexamethyldisiloxane and tetramethyl divinyl disiloxane, is stirring reaction 0.5h under 70 DEG C of conditions in temperature; Dropwise add methyl silicate and 3 ?the mixed solution of (di-isopropyl urea groups) propyl-triethoxysilicane, time for adding is controlled at 3h, temperature of reaction is controlled at 70 DEG C; After dropwising, be to continue stirring reaction 1h under 70 DEG C of conditions in temperature; Add toluene to extract, with deionized water wash toluene, mutually to neutral, underpressure distillation, except desolventizing and low-boiling-point substance, obtains urea groups modification MQ silicone resin 2.
Urea groups modification MQ silicone resin 1 in embodiment 1 is become to urea groups modification MQ silicone resin 2, and consumption is 3.57 mass parts, and the consumption of corresponding containing hydrogen silicone oil is increased to 2.88 mass parts.The performance of sample is as shown in table 1.
Embodiment 3
By percentage to the quality, the synthesis material of urea groups modification MQ silicone resin 3 comprises following component:
Preparation method: in reactor, adding deionized water, propyl carbinol, concentrated hydrochloric acid, hexamethyldisiloxane and tetramethyl divinyl disiloxane, is stirring reaction 2h under 70 DEG C of conditions in temperature; Dropwise add tetraethoxy, dimethyldimethoxysil,ne and 3 ?the mixed solution of (di-isopropyl urea groups) propyl-triethoxysilicane, time for adding is controlled at 6h, temperature of reaction is controlled at 70 DEG C; After dropwising, be to continue stirring reaction 2h under 70 DEG C of conditions in temperature; Add toluene to extract, with deionized water wash toluene, mutually to neutral, underpressure distillation, except desolventizing and low-boiling-point substance, obtains urea groups modification MQ silicone resin 3.
Urea groups modification MQ silicone resin 1 in embodiment 1 is become to urea groups modification MQ silicone resin 3, and consumption is 3.57 mass parts, and the consumption of corresponding containing hydrogen silicone oil is increased to 3.03 mass parts.The performance of sample is as shown in table 1.
Embodiment 4
By percentage to the quality, the synthesis material of urea groups modification MQ silicone resin 4 comprises following component:
Preparation method: in reactor, adding deionized water, ethanol, the vitriol oil, hexamethyldisiloxane and tetramethyl divinyl disiloxane, is stirring reaction 1h under 80 DEG C of conditions in temperature; The mixed solution that dropwise adds tetraethoxy and 3 ?(phenyl urea groups) propyl-triethoxysilicane, time for adding is controlled at 2h, and temperature of reaction is controlled at 80 DEG C; After dropwising, be to continue stirring reaction 2h under 80 DEG C of conditions in temperature; Add toluene to extract, with deionized water wash toluene, mutually to neutral, underpressure distillation, except desolventizing and low-boiling-point substance, obtains urea groups modification MQ silicone resin 4.
Urea groups modification MQ silicone resin 1 in embodiment 1 is become to urea groups modification MQ silicone resin 4, and consumption is 3.57 mass parts, and the consumption of corresponding containing hydrogen silicone oil is increased to 3.13 mass parts.The performance of sample is as shown in table 1.
Embodiment 5
By percentage to the quality, the synthesis material of urea groups modification MQ silicone resin 5 comprises following component:
Preparation method: in reactor, adding deionized water, Virahol, tosic acid, hexamethyldisiloxane and tetramethyl divinyl disiloxane, is stirring reaction 2h under 80 DEG C of conditions in temperature; The mixed solution that dropwise adds tetraethoxy, methyltrimethoxy silane and 3 ?(phenyl urea groups) propyl-triethoxysilicane, time for adding is controlled at 4h, and temperature of reaction is controlled at 80 DEG C; After dropwising, be to continue stirring reaction 2h under 80 DEG C of conditions in temperature; Add toluene to extract, with deionized water wash toluene, mutually to neutral, underpressure distillation, except desolventizing and low-boiling-point substance, obtains urea groups modification MQ silicone resin 5.
Urea groups modification MQ silicone resin 1 in embodiment 1 is become to urea groups modification MQ silicone resin 5, and consumption is 3.57 mass parts, and the consumption of corresponding containing hydrogen silicone oil is increased to 3.11 mass parts.The performance of sample is as shown in table 1.
Comparative example 1
By 100 mass parts vinyl silicone oils (viscosity at 25 DEG C is 20000mPas, and contents of ethylene is 0.12wt%), (specific surface area is 260m to 40 mass parts thermal silicas
2/ g) He 12 mass parts hexamethyldisilazanes mix in vacuum kneader, at room temperature stir 2h, are heated to 170 DEG C of mixing 2h of temperature of charge, then pumping vacuum and mixing 1h, grind after cooling through three-roller, obtain add-on type liquid silicon rubber basis glue;
In above-mentioned 100 mass parts sizings, (viscosity at 25 DEG C is 160mPas to add 1.08 mass parts containing hydrogen silicone oils, hydrogen content is 0.5wt%), 0.01 mass parts 1 ?Yi Que Ji ?1 ?the divinyl tetramethyl disiloxane complex compound of hexalin and the 0.25 mass parts platinum content Platinic chloride that is 3000ppm, at room temperature stir, mold pressing 10min at 120 DEG C, make the film that 6mm and 2mm are thick, carry out respectively anti creepage trace test and Mechanics Performance Testing.The performance of sample is as shown in table 1.
For embodiment 1 ?the 5 urea groups modification MQ silicone resin that obtain carried out infrared measurement, infrared spectra is as shown in Figure 1.For the infrared spectra of urea groups modification MQ silicone resin 1, urea groups modification MQ silicone resin 2 and urea groups modification MQ silicone resin 3,2973cm
?1～2885cm
-1for the C of methyl or methylene radical ?H stretching vibration peak; 1253cm
?1, 843cm
?1and 756cm
?1occurred M cell S i ?CH
3charateristic avsorption band, at 3052cm
?1occurred M cell S i ?CH=CH
2charateristic avsorption band; 1200cm
?1～980cm
?1the strong broad peak at place corresponding to Si ?O ?the stretching vibration peak of Si; 3342cm
?1for N in urea groups ?H stretching vibration peak, 1629cm
?1and 1524cm
?1for C=O in urea groups and C ?the stretching vibration peak of N, show to contain urea groups in urea groups modification MQ silicone resin.For the infrared spectra of urea groups modification MQ silicone resin 4 and urea groups modification MQ silicone resin 5,2961cm
?1～2899cm
?1for the C of methyl or methylene radical ?H stretching vibration peak; 1253cm
?1, 843cm
?1and 756cm
?1occurred M cell S i ?CH
3charateristic avsorption band, at 3052cm
?1occurred M cell S i ?CH=CH
2charateristic avsorption band; 1598cm
?1near peak is C=C stretching vibration peak on phenyl ring; 1200cm
?1～980cm
?1the strong broad peak at place corresponding to Si ?O ?the stretching vibration peak of Si; 3342cm
?1for N ?H stretching vibration peak, 1630cm
?1and 1525cm
?1for C=O in urea groups and C ?the stretching vibration peak of N, show to contain urea groups in urea groups modification MQ silicone resin.
As can be seen from Table 1, not adding the add-on type liquid silicon rubber of urea groups modification MQ silicone resin fails by the anti creepage trace test (seeing comparative example 1) of 4.5kV, and the add-on type liquid silicon rubber that adds the synthetic urea groups modification MQ silicone resin of the present invention has all passed through anti creepage trace test, anti creepage trace reaches 1A4.5 level, shows that the urea groups modification MQ silicone resin of synthesized can improve the anti creepage trace performance of add-on type liquid silicon rubber significantly.This is mainly to play electric arc quenching effect because the urea groups of introducing decomposites a large amount of non-combustible gas in dry band arc discharge process, thereby improves add-on type liquid silicon rubber anti creepage trace performance.In addition, the urea groups modification MQ silicone resin that adds synthesized does not only worsen the mechanical property of add-on type liquid silicon rubber, makes on the contrary mechanical property improve.This may be because the urea groups modification MQ silicone resin structure of synthesized contains vinyl, can participate in the sulfuration of add-on type liquid silicon rubber, forms Concentrative crosslinking structure, thereby has improved the mechanical property of silicon rubber.
In table 1, product performance testing method is as follows:
1, according to GB/T528 ?2009 tensile strength and the elongation at breaks of measuring silicon rubber.
2, according to GB/T529 ?2008 tear strengths of measuring silicon rubber.
3, according to GB/T531 ?2008 Shore A hardness of measuring silicon rubber.
4, according to GB/T6553 ?2003 carry out the anti creepage traces test of silicon rubber.Adopt constant-voltage method, trial voltage is
4.5kV; Endpoint is selected " the endpoint method A " in this test method: in the time that in high tension loop, the electric current by sample exceedes 60mA as having reached terminal.
The mechanical property of table 1 add-on type liquid silicon rubber and anti creepage trace performance
Claims (8)
1. a urea groups modification MQ silicone resin, is characterized in that, by percentage to the quality, the synthesis material of described urea groups modification MQ silicone resin comprises following component:
Described ureido silane coupling agent is following structural formula:
Wherein R
1, R
2wei ?H, ?(CH
2)
ncH
3huo ?Ph, the integer that n is 0～8; R
3wei ?CH
3huo ?CH
2cH
3;
Described four functionality silicon monomers are the one in methyl silicate, tetraethoxy or water glass;
Described siloxane blocking agent is one or more in hexamethyldisiloxane, tetramethyl divinyl siloxanes or tetramethyl disiloxane;
Described catalyzer is the one in hydrochloric acid, sulfuric acid or tosic acid;
Described alcohol is one or more in ethanol, Virahol or propyl carbinol.
When preparation, be stirring reaction under (70～80) DEG C condition by deionized water, alcohol, catalyzer and siloxane blocking agent in temperature; The mixed solution that drips four functionality silicon monomers and ureido silane coupling agent, temperature of reaction is controlled at (70～80) DEG C; Dropwise rear continuation stirring reaction (0.5～2) h; Extraction, washing, underpressure distillation, obtains urea groups modification MQ silicone resin.
2. urea groups modification MQ silicone resin claimed in claim 1, it is characterized in that, by percentage to the quality, the synthesis material of described raw material urea groups modification MQ silicone resin also comprises two functionality silicon monomers 0～5%, and described two functionality silicon monomers are one or more in dimethyldimethoxysil,ne, dimethoxydiphenylsilane, aminomethyl phenyl dimethoxy silane, dimethyldiethoxysilane, phenylbenzene diethoxy silane or aminomethyl phenyl diethoxy silane.
3. the urea groups modification MQ silicone resin described in claim 1 or 2, is characterized in that, by percentage to the quality, the synthesis material of described raw material urea groups modification MQ silicone resin also comprises three-functionality-degree silicon monomer 0～5%; Described three-functionality-degree silicon monomer is one or more in methyltrimethoxy silane, propyl group trimethoxy silane, vinyltrimethoxy silane, phenyltrimethoxysila,e, Union carbide A-162, propyl group three ethoxy silane, vinyltriethoxysilane or phenyl triethoxysilane.
4. the preparation method of urea groups modification MQ silicone resin claimed in claim 1, is characterized in that, comprises the following steps:
(1) in reactor, add deionized water, alcohol, catalyzer and siloxane blocking agent, be stirring reaction (0.5～2) h under (70～80) DEG C condition in temperature;
(2) dropwise add the mixed solution of four functionality silicon monomers and ureido silane coupling agent, time for adding is controlled at (2～6) h, and temperature of reaction is controlled at (70～80) DEG C; After dropwising, at (70～80) DEG C, continue stirring reaction (0.5～2) h;
(3) extraction, washing, underpressure distillation, except desolventizing and low-boiling-point substance, obtains urea groups modification MQ silicone resin.
5. the preparation method of urea groups modification MQ silicone resin according to claim 4, it is characterized in that, in the time that described synthesis material also comprises two functionality silicon monomers and/or three-functionality-degree silicon monomer, described two functionality silicon monomers and/or three-functionality-degree silicon monomer and four functionality silicon monomers and ureido silane coupling agent composition mixed solution.
6. the preparation method of urea groups modification MQ silicone resin according to claim 4, is characterized in that, described extraction is for adding toluene extraction.
7. the preparation method of urea groups modification MQ silicone resin according to claim 6, is characterized in that, described washing is for extremely neutral mutually with deionized water wash toluene.
8. the application of urea groups modification MQ silicone resin claimed in claim 1 in add-on type liquid silicon rubber, it is characterized in that: 100 mass parts vinyl silicone oils, 40 mass parts thermal silicas and 3～15 mass parts hexamethyldisilazanes are mixed in vacuum kneader, at room temperature stir, be heated to temperature of charge (170 ?180) DEG C continuation mixing, pumping vacuum and mixing again, cooling rear grinding, obtains add-on type liquid silicon rubber sizing; And then add successively containing hydrogen silicone oil, 0.004～0.03 mass parts 1 ?Yi Que Ji ?1 ?the urea groups modification MQ silicone resin, the divinyl tetramethyl disiloxane complex compound of Platinic chloride that platinum content is 3000ppm of hexalin, 1～10 mass parts, at room temperature mix sulfuration (0.1～5) h at (100～150) DEG C; In described containing hydrogen silicone oil, in si-h bond and vinyl silicone oil and urea groups modification MQ silicone resin, the mol ratio of carbon-carbon double bond summation is 1:1～1.8:1; Described platinum atom content accounts for (2～40) ppm of total quality of material.
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| CN106380603A (en) * | 2016-09-09 | 2017-02-08 | 华南理工大学 | Bis-amino-containing MQ silicone resin, and preparation method and application thereof |
| CN106543734A (en) * | 2016-10-25 | 2017-03-29 | 华南理工大学 | A kind of high-performance anti creepage trace add-on type liquid silicon rubber and preparation method thereof |
| CN107915843A (en) * | 2017-11-14 | 2018-04-17 | 万华化学集团股份有限公司 | A kind of modified MQ silicones and preparation method thereof |
| CN109776806A (en) * | 2019-01-11 | 2019-05-21 | 湖北新四海化工股份有限公司 | A kind of hydrophily MQ silicone resin and its synthetic method |
| CN110423351A (en) * | 2019-07-29 | 2019-11-08 | 中科广化（重庆）新材料研究院有限公司 | A kind of Vinyl MQ silicon resin and preparation method thereof |
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| CN111410744A (en) * | 2019-01-04 | 2020-07-14 | 中昊晨光化工研究院有限公司 | MDQ silicon resin containing phenyl and preparation method thereof |
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| CN106543734A (en) * | 2016-10-25 | 2017-03-29 | 华南理工大学 | A kind of high-performance anti creepage trace add-on type liquid silicon rubber and preparation method thereof |
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| CN112226089A (en) * | 2020-09-30 | 2021-01-15 | 华南理工大学 | Tracking-resistant addition type liquid silicone rubber composition and preparation method and application thereof |
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| CN114574157A (en) * | 2022-03-15 | 2022-06-03 | 广州布鲁奥申新材料科技有限公司 | General organic silicon pressure-sensitive adhesive with high peel strength and preparation method thereof |
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