CN102994004B - Add-on type liquid silicon rubber adhesion promoters with strengthening action and its preparation method and application - Google Patents
Add-on type liquid silicon rubber adhesion promoters with strengthening action and its preparation method and application Download PDFInfo
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Abstract
The invention discloses add-on type liquid silicon rubber adhesion promoters with strengthening action and its preparation method and application, this adhesion promoters is simultaneously containing the silicone compounds of polyene-based, epoxy group(ing) and alkoxyl group, during preparation, the polyene-based ether compound of hydroxyl and epoxy group(ing) silicone compounds are at room temperature stirred, add catalyzer, be warmed up to 60 ~ 130 DEG C of reaction 1 ~ 10h, then continue reaction 1 ~ 6h at reduced pressure conditions and prepare.Preparation technology of the present invention is easy, and raw material is cheap and easy to get, environmental protection, is easy to realize suitability for industrialized production.Adhesion promoters prepared by the present invention can significantly improve the adhesiveproperties of add-on type liquid silicon rubber, be conducive to the filling of filler in silicon rubber and dispersion, improve the mechanical property of silicon rubber, have a wide range of applications in fields such as electron device package, semi-conductor chip coating and photovoltaic component encapsulatings.
Description
Technical field
The present invention relates to the bonding and Strengthening Technology field of organosilicon material, in more detail can improve the adhesion promoters of add-on type liquid silicon rubber adhesiveproperties and mechanical property.The invention still further relates to the preparation method and application of described adhesion promoters.
Background technology
The world today, scientific and technical fast development, the mankind have entered the electronic information epoch.Along with the continuous progress of electronic technology, electronic component, logical circuit are tending towards integrated day by day, miniaturization and modularization, and Working environment is harsher, has higher requirement to the stability in use of electron device.Encapsulation is one of important procedure of electronic devices and components, it can the globality of strengthening electronic device, prevents moisture, dust and obnoxious flavour to the erosion of electronic devices and components, improves the resistibility to external shock, vibrations, stablize component parameter, and be conducive to miniaturization and the lightweight of device.
Electronic package material conventional at present mainly contains epoxy resin, urethane and organosilicon material three major types.Wherein, add-on type liquid silicon rubber can keep elasticity for a long time at-60 ~ 200 DEG C, does not absorb heat, not heat release during solidification, do not shrink after solidification, and there is excellent electrical property and chemical stability, and can water-fast, resistance to ozone, weather-proof, become one of high performance packaged material.Although add-on type liquid silicon rubber has the incomparable advantage of other packaged material, himself also has some problems.As add-on type liquid silicon rubber after curing surface the overwhelming majority be nonpolar organic group, show low internal cohesive energy (Siliconesealantsandstructuraladhesives.InternationalJour nalofAdhesion & Adhesives, 2001, 21 (5): 411-422), thus poor to the cementability of other material, moisture easily causes corrosion and failure of insulation by the space infiltration inside of electronic component between silicon rubber and base material in use, even can come off with base material in the environment of harshness, electron device is made to lose seal protection, limit its range of application to a certain extent.
In order to solve the problem, the cementability how improving add-on type liquid silicon rubber and base material be carried out some both at home and abroad and having studied.At present, mainly contain three kinds of methods: one is process substrate surface, comprise with silane coupling agent pretreating substrates surface, use the measures such as Cement Composite Treated by Plasma substrate surface, shortcoming needs additional production process, reduces production efficiency, add production cost; Two is the molecular structures by changing polysiloxane, makes add-on type liquid silicon rubber itself have cementability, but due to this preparation process more complicated, realizes suitability for industrialized production and apply being subject to larger restriction; Three is by adding adhesion promoters, obtains cementability after add-on type liquid silicon rubber is solidified.
Chinese patent CN102408869A discloses one vinyl front three (second) TMOS and γ-(2,3-epoxy third oxygen) propyl group front three (second) TMOS reacts by hydrolysis reaction or both hydrolysis reaction products and γ-aminopropyl front three (second) TMOS add-on type liquid silicon rubber adhesion promoters aluminium being had to certain cementability prepared, but there is the bad control of hydrolysis reaction condition of siloxanes, reaction process easily produces gel, and nitrogenous compound easily makes the shortcomings such as Pt catalyst poisoning.European patent EP 2158285B1 reports a kind of silicoorganic compound with at least one benzene ring structure, at least one alicyclic epoxy base and at least one Si-H base utilizing addition reaction of silicon with hydrogen to synthesize, and is added in silicon rubber the sealing material that can obtain and the electrolytic thin-membrane in fuel cell be produced to good bonding.Chinese patent CN102010598A also report a kind of utilize addition reaction of silicon with hydrogen to synthesize every 1 molecule trimerization isocyanide acyl ring has the organo-siloxane of allyl group, epoxy group(ing) and organic siloxy-containing trimerization isocyanide acyl ring; by adding this adhesion promoters to silicon rubber, the thermoplasticss such as itself and liquid crystalline polymers can be made to produce good bonding.But all there is the bad control of addition reaction of silicon with hydrogen condition, the shortcomings such as difficulty removed by platinum catalyst.
Although to the adhesion promoters improving add-on type liquid silicon rubber cementability, there are reports at present, but these work only study adhesiveproperties mostly, for the report that the adhesion promoters that can improve add-on type liquid silicon rubber adhesiveproperties and mechanical property is but not relevant simultaneously.Because organo-silicone rubber has amorphism structure, its macromolecular chain is very submissive, and interchain interaction power is weak, and the organo-silicone rubber intensity without reinforcement is extremely low, almost has no value for use.Therefore, develop the add-on type liquid silicon rubber adhesion promoters with strengthening action to have great importance.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of add-on type liquid silicon rubber adhesion promoters with strengthening action and preparation method thereof is provided.
The invention still further relates to the application of adhesion promoters in add-on type liquid silicon rubber, this adhesion promoters is added in add-on type liquid silicon rubber, good adhesive property and mechanical property can be obtained.
Object of the present invention is achieved through the following technical solutions:
Have an add-on type liquid silicon rubber adhesion promoters for strengthening action, simultaneously containing the silicone compounds of polyene-based, epoxy group(ing) and alkoxyl group, its general molecular formula is:
Wherein R
1for-CH (CH
2oCH
2cH=CH
2)
2,-CH
2c (CH
2cH
3) (CH
2oCH
2cH=CH
2)
2or-CH
2c (CH
2oCH
2cH=CH
2)
3; R
2for-CH
3or-CH
2cH
3; R
3for-CH
3,-CH
2cH
3,-OCH
3or-OCH
2cH
3; R
4for-CH
2cH
2cH
2oCH
2r
5or-CH
2cH
2r
6, wherein R
5for epoxy group(ing), R
6it is 3,4-epoxy group(ing)-cyclohexyl.
There is the preparation method of the add-on type liquid silicon rubber adhesion promoters of strengthening action: the polyene-based ether compound of hydroxyl and epoxy group(ing) silicone compounds are at room temperature stirred at 0.8: 1 ~ 1.4: 1 in molar ratio, then the organic titanate catalyzer of 0.5 ~ 4% of reactant total mass is added under agitation, under temperature is 60 ~ 130 DEG C of conditions, reacts 1 ~ 10h, under vacuum tightness is 0.01 ~ 30kPa condition, continues reaction 1 ~ 6h obtains add-on type liquid silicon rubber adhesion promoters;
The polyene-based ether compound of described hydroxyl is one or more in glycerol diallyl ether, trimethylolpropane allyl ether and pentaerythritol triallyl ether; Structural formula is respectively:
Glycerol diallyl ether trimethylolpropane allyl ether pentaerythritol triallyl ether
Described epoxy group(ing) silicone compounds is 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 3-(2,3-epoxy third oxygen) hydroxypropyl methyl dimethoxysilane, 3-(2,3-epoxy third oxygen) propyl-triethoxysilicane, 3-(2,3-epoxy third oxygen) hydroxypropyl methyl diethoxy silane, 2-(3,4-epoxy cyclohexane base) one or more in ethyl trimethoxy silane and 2-(3,4-epoxy cyclohexane base) ethyl triethoxysilane;
Described organic titanate catalyzer be tetraethyl titanate, titanium isopropylate, tetrabutyl titanate, metatitanic acid four tert-butyl ester and bis(acetylacetonate) titanium acid diisopropyl ester in one or more.
Further, the polyene-based ether compound of described hydroxyl and the mol ratio of epoxy group(ing) silicone compounds are preferably 1: 1 ~ 1.2: 1.Described temperature is the time of reacting under 60 ~ 130 DEG C of conditions be preferably 1.5 ~ 7.5h.Described vacuum tightness is the time of continuing under 0.01 ~ 30kPa condition to react be preferably 2 ~ 4h.
The application of described adhesion promoters in add-on type liquid silicon rubber: successively the 1-ethynyl-1-hexalin of the adhesion promoters of the aluminum oxide of the vinyl silicone oil of 100 mass parts, 120 ~ 200 mass parts, 0.8 ~ 6 mass parts, containing hydrogen silicone oil and 0.004 ~ 0.03 mass parts is added kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound that platinum content is the Platinic chloride of 1500 ~ 4500ppm, stir, deaeration 8 ~ 25min under vacuum tightness 0.5 ~ 50kPa, finally solidifies 1 ~ 5h shaping at 110 ~ 150 DEG C; In described containing hydrogen silicone oil, in si-h bond and vinyl silicone oil and adhesion promoters, the mol ratio of double bond summation is 1: 1 ~ 1.6: 1; Described platinum atom content accounts for 2 ~ 40ppm of total quality of material.
Compared with prior art, tool has the following advantages in the present invention:
1, the adhesion promoters that prepared by the present invention can significantly improve the adhesiveproperties of add-on type liquid silicon rubber, and in silicon rubber, add a small amount of (being generally less than 2.5 mass parts) adhesion promoters, bonding strength can improve more than 150%.
2, the adhesion promoters that prepared by the present invention can significantly improve the mechanical property of add-on type liquid silicon rubber.This adhesion promoters contains polyene-based, can form Concentrative crosslinking structure when add-on type liquid silicon rubber solidifies, and the ability making add-on type liquid silicon rubber resist external force strengthens, and intensity improves.
3, the adhesion promoters that prepared by the present invention can improve the consistency of filler and add-on type liquid silicon rubber, is conducive to the filling of filler in silicon rubber and dispersion, improves processing characteristics.
4, preparation technology of the present invention is easy, and raw material is cheap and easy to get, environmental protection, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of the adhesion promoters 1 of preparation in embodiment 1;
Fig. 2 is the nucleus magnetic hydrogen spectrum of the adhesion promoters 1 of preparation in embodiment 1;
Fig. 3 is the infrared spectrum of the adhesion promoters 6 of preparation in embodiment 6;
Fig. 4 is the nucleus magnetic hydrogen spectrum of the adhesion promoters 6 of preparation in embodiment 6.
Embodiment
For a better understanding of the present invention, below in conjunction with embodiment, further explanation is done to the present invention, but embodiments of the present invention are not limited thereto.
Embodiment 1
By 12.82g pentaerythritol triallyl ether (APE) and 11.82g3-(2,3-epoxy third oxygen) propyl trimethoxy silicane (KH-560) adds there-necked flask with thermometer and condensing reflux pipe, at room temperature stir, then 0.25g tetrabutyl titanate is dripped under agitation, be warming up to 80 DEG C of reaction 2h, under vacuum tightness 0.5kPa, finally continue reaction 2h obtain product adhesion promoters 1.
The infrared spectrum (Fig. 1) of adhesion promoters 1 is analyzed, at 2844cm
-1there is the absorption peak of methoxyl group in place, at 1646cm
-1there is the absorption peak of double bond in place, at 922cm
-1there is the absorption peak of C-H absorption peak in thiazolinyl and epoxy group(ing) in place.
The nucleus magnetic hydrogen spectrum (Fig. 2) of adhesion promoters 1 is analyzed, the peak at chemical shift 5 ~ 6ppm place is produced by the Hydrogen Proton in double bond, the peak at chemical shift 3.54ppm place is produced by the Hydrogen Proton in methoxyl group, and the peak at chemical shift 2.5 ~ 3.2ppm place is produced by the Hydrogen Proton in epoxy group(ing).
Can determine that adhesion promoters 1 is the compound simultaneously containing polyene-based, epoxy group(ing) and alkoxyl group by infrared spectrum and nucleus magnetic hydrogen spectrum.Wherein, polyene-based can participate in the solidification of add-on type liquid silicon rubber, forms Concentrative crosslinking structure, improves the mechanical property of silicon rubber; And epoxy group(ing), alkoxyl group isopolarity group can improve the reactive force of add-on type liquid silicon rubber and base material, silicon rubber is made to have good cementability.Above-mentioned preparation process can adopt reaction formula to be expressed as:
Be the vinyl silicone oil of 300mPas by 40 mass parts viscosity successively, the vinyl silicone oil of 60 mass parts 1000mPas, 150 mass parts median sizes are the aluminum oxide of 5 μm, the adhesion promoters 1 of 2 mass parts, 7.12 mass parts hydrogen contents be 0.5% containing hydrogen silicone oil and 0.01 mass parts 1-ethynyl-1-hexalin add kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound that 0.38 mass parts platinum content is the Platinic chloride of 2600ppm, stir, deaeration 15min under vacuum tightness 2kPa, finally at 130 DEG C, solidify 2h shaping.The performance of sample is as shown in table 1, and testing method illustrates in table 1.Its bonding tensile shear strength (is called for short shearing resistance, lower same) be 1.19MPa, tensile strength is 3.19MPa, improve 250% and 43% respectively relative to the shearing resistance (0.34MPa) of comparative example 1 and tensile strength (2.23MPa), illustrate that the adhesion promoters 1 prepared with APE and KH-560 can improve adhesiveproperties and the mechanical property of add-on type liquid silicon rubber significantly.
Embodiment 2
By 12.82gAPE and 18.02g2-(3,4-epoxy cyclohexane base) ethyl triethoxysilane (KH-567) adds there-necked flask with thermometer and condensing reflux pipe, at room temperature stir, then 0.15g tetrabutyl titanate is dripped under agitation, be warming up to 130 DEG C of reaction 1h, under vacuum tightness 0.01kPa, finally continue reaction 1h obtain product adhesion promoters 2.
Carrying out infrared spectrum and nucleus magnetic hydrogen spectrum to adhesion promoters 2 analyzes known, and its structure is:
Be the vinyl silicone oil of 300mPas by 40 mass parts viscosity successively, the vinyl silicone oil of 60 mass parts 1000mPas, 120 mass parts median sizes are the aluminum oxide of 5 μm, the adhesion promoters 2 of 2.5 mass parts, 6.33 mass parts hydrogen contents be 0.5% containing hydrogen silicone oil and 0.004 mass parts 1-ethynyl-1-hexalin add kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound that 0.3 mass parts platinum content is the Platinic chloride of 1500ppm, stir, deaeration 25min under vacuum tightness 50kPa, finally at 110 DEG C, solidify 5h shaping.The performance of sample is as shown in table 1, its shearing resistance is 0.81MPa, tensile strength is 2.89MPa, to compare with tensile strength (2.06MPa) with the shearing resistance (0.31MPa) of comparative example 2 and improve 161% and 40% respectively, illustrate that the adhesion promoters 2 prepared with APE and KH-567 can improve adhesiveproperties and the mechanical property of add-on type liquid silicon rubber preferably.
Embodiment 3
The present embodiment difference from Example 1 is KH-560 to be changed into 2-(3,4-epoxy cyclohexane base) ethyl trimethoxy silane (KH-566), and its consumption is 12.32g, obtained adhesion promoters 3.
Carrying out infrared spectrum and nucleus magnetic hydrogen spectrum to adhesion promoters 3 analyzes known, and its structure is:
Adhesion promoters 1 is changed into adhesion promoters 3, and its consumption is 1.5 mass parts, the consumption of corresponding containing hydrogen silicone oil is reduced to 6.3 mass parts, and the consumption of the divinyl tetramethyl disiloxane complex compound of Platinic chloride changes into 1.52 mass parts.The performance of solidification sample is as shown in table 1, its shearing resistance is 0.96MPa, tensile strength is 3.01MPa, improve 182% and 35% respectively relative to the shearing resistance of comparative example 1 and tensile strength, illustrate that adhesion promoters 3 that KH-566 replaces KH-560 to prepare significantly can improve adhesiveproperties and the mechanical property of add-on type liquid silicon rubber.
Embodiment 4
By 10.72g trimethylolpropane allyl ether (TMPDE) and 9.94g3-(2,3-epoxy third oxygen) propyl-triethoxysilicane (KH-561) adds there-necked flask with thermometer and condensing reflux pipe, at room temperature stir, then 0.83g tetrabutyl titanate is dripped under agitation, be warming up to 60 DEG C of reaction 10h, under vacuum tightness 30kPa, finally continue reaction 6h obtain product adhesion promoters 4.
Carrying out infrared spectrum and nucleus magnetic hydrogen spectrum to adhesion promoters 4 analyzes known, and its structure is:
Be the vinyl silicone oil of 300mPas by 40 mass parts viscosity successively, the vinyl silicone oil of 60 mass parts 1000mPas, 200 mass parts median sizes are the aluminum oxide of 5 μm, the adhesion promoters 4 of 6 mass parts, 13.88 mass parts hydrogen contents be 0.5% containing hydrogen silicone oil and 0.03 mass parts 1-ethynyl-1-hexalin add kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound that 2.84 mass parts platinum contents are the Platinic chloride of 4500ppm, stir, deaeration 8min under vacuum tightness 0.5kPa, finally at 150 DEG C, solidify 1h shaping.The performance of sample is as shown in table 1, its shearing resistance is 1.43MPa, tensile strength is 3.34MPa, improve 297% and 27% respectively compared with comparative example 3, illustrate that the adhesion promoters 4 prepared with TMPDE and KH-561 can improve adhesiveproperties and the mechanical property of add-on type liquid silicon rubber significantly.
Embodiment 5
The present embodiment difference from Example 1 is KH-560 to change into KH-561, and its consumption is 13.92g, accordingly tetrabutyl titanate consumption is brought up to 0.27g, obtained adhesion promoters 5.
Carrying out infrared spectrum and nucleus magnetic hydrogen spectrum to adhesion promoters 5 analyzes known, and its structure is:
Adhesion promoters 1 is changed into adhesion promoters 5, and its consumption is 1.5 mass parts, the consumption of corresponding containing hydrogen silicone oil is reduced to 6.22 mass parts.The performance of sample is as shown in table 1, its shearing resistance is 1.04MPa, tensile strength is 3.15MPa, improve 206% and 41% respectively relative to the shearing resistance of comparative example 1 and tensile strength, adhesiveproperties and the mechanical property that can improve add-on type liquid silicon rubber with the adhesion promoters 5 that KH-561 replaces KH-560 to prepare significantly are described.
Embodiment 6
The present embodiment difference from Example 1 is APE to change into TMPDE, and its consumption is 10.72g, accordingly tetrabutyl titanate consumption is reduced to 0.22g, obtained adhesion promoters 6.Carry out infrared spectrum (Fig. 3) to adhesion promoters 6 and nucleus magnetic hydrogen spectrum (Fig. 4) is analyzed known, its structure is:
Adhesion promoters 1 is changed into adhesion promoters 6, and its consumption is 1.5 mass parts, the consumption of corresponding containing hydrogen silicone oil is reduced to 5.73 mass parts, and the consumption of the divinyl tetramethyl disiloxane complex compound of Platinic chloride changes into 0.76 mass parts.The performance of sample is as shown in table 1, its shearing resistance is 0.92MPa, tensile strength is 3.06MPa, to compare with tensile strength with the shearing resistance of comparative example 1 and improve 170% and 37% respectively, adhesiveproperties and the mechanical property that can improve add-on type liquid silicon rubber with the adhesion promoters 6 that TMPDE replaces APE to prepare preferably are described.
Comparative example 1
Be the vinyl silicone oil of 300mPas successively by 40 mass parts viscosity, the vinyl silicone oil of 60 mass parts 1000mPas, 150 mass parts median sizes to be aluminum oxide, the 4.03 mass parts hydrogen contents of 5 μm be 0.5% containing hydrogen silicone oil and 0.01 mass parts 1-ethynyl-1-hexalin add kneader, stir at 30 DEG C, and then add the vinylsiloxane complex compound that 0.38 mass parts platinum content is the Platinic chloride of 2600ppm, stir, deaeration 20min under vacuum tightness is 2kPa, finally at 130 DEG C, solidify 2h shaping, the performance of sample is as shown in table 1.
Comparative example 2
Be the vinyl silicone oil of 300mPas by 40 mass parts viscosity successively, the vinyl silicone oil of 60 mass parts 1000mPas, 120 mass parts median sizes are the aluminum oxide of 5 μm, 3.39 mass parts hydrogen contents be 0.5% containing hydrogen silicone oil and 0.004 mass parts 1-ethynyl-1-hexalin add kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound that 0.3 mass parts platinum content is the Platinic chloride of 1500ppm, stir, deaeration 25min under vacuum tightness 50kPa, finally at 110 DEG C, solidify 5h shaping, the performance of sample is as shown in table 1.
Comparative example 3
Be the vinyl silicone oil of 300mPas by 40 mass parts viscosity successively, the vinyl silicone oil of 60 mass parts 1000mPas, 200 mass parts median sizes are the aluminum oxide of 5 μm, 5.37 mass parts hydrogen contents be 0.5% containing hydrogen silicone oil and 0.03 mass parts 1-ethynyl-1-hexalin add kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound that 2.71 mass parts platinum contents are the Platinic chloride of 4500ppm, stir, deaeration 8min under vacuum tightness 0.5kPa, finally at 150 DEG C, solidify 1h shaping, the performance of sample is as shown in table 1.
In table 1, product performance testing method is as follows:
1, according to the viscosity of GB/T2794-1995 with rotary viscosity design determining silicon rubber.
2, according to the bonding tensile shear strength of GB/T13936-1992 mensuration silicon rubber with aluminium.
3, tensile strength and the elongation at break of silicon rubber is measured according to GB/T528-2009.
4, the Shore A hardness of silicon rubber is measured according to GB/T531-2008.
Table 1 add-on type liquid silicon rubber the performance test results
Claims (6)
1. there is an add-on type liquid silicon rubber adhesion promoters for strengthening action, it is characterized in that: promotor is that its general molecular formula is simultaneously containing the silicone compounds of polyene-based, epoxy group(ing) and alkoxyl group:
Wherein R
1wei ?CH (CH
2oCH
2cH=CH
2)
2, ?CH
2c (CH
2cH
3) (CH
2oCH
2cH=CH
2)
2huo ?CH
2c (CH
2oCH
2cH=CH
2)
3; R
2wei ?CH
3huo ?CH
2cH
3; R
3wei ?CH
3, ?CH
2cH
3, ?OCH
3huo ?OCH
2cH
3; R
4wei ?CH
2cH
2cH
2oCH
2r
5huo ?CH
2cH
2r
6, wherein R
5for
r
6be 3,4 ?Huan Yang Ji ?cyclohexyl.
2. the preparation method with the add-on type liquid silicon rubber adhesion promoters of strengthening action according to claim 1, it is characterized in that: by the polyene-based ether compound of hydroxyl and epoxy group(ing) silicone compounds in molar ratio 0.8:1 ~ 1.4:1 at room temperature stir, then the organic titanate catalyzer of 0.5 ~ 4% of reactant total mass is added under agitation, under temperature is 60 ~ 130 DEG C of conditions, reacts 1 ~ 10h, under vacuum tightness is 0.01 ~ 30kPa condition, continues reaction 1 ~ 6h obtains add-on type liquid silicon rubber adhesion promoters;
The polyene-based ether compound of described hydroxyl is one or more in glycerol diallyl ether, trimethylolpropane allyl ether and pentaerythritol triallyl ether;
Described epoxy group(ing) silicone compounds be 3 ?(2,3 ?epoxy third oxygen) propyl trimethoxy silicane, 3 ?(2,3 ?epoxy third oxygen) hydroxypropyl methyl dimethoxysilane, 3 ?(2,3 ?epoxy third oxygen) propyl-triethoxysilicane, 3 ?(2,3 ?epoxy third oxygen) hydroxypropyl methyl diethoxy silane, 2 ?(3,4 ?epoxy cyclohexane base) ethyl trimethoxy silane and 2 ?one or more in (3,4 ?epoxy cyclohexane base) ethyl triethoxysilane;
Described organic titanate catalyzer be tetraethyl titanate, titanium isopropylate, tetrabutyl titanate, metatitanic acid four tert-butyl ester and bis(acetylacetonate) titanium acid diisopropyl ester in one or more.
3. preparation method according to claim 2, is characterized in that: the polyene-based ether compound of described hydroxyl and the mol ratio of epoxy group(ing) silicone compounds are 1:1 ~ 1.2:1.
4. preparation method according to claim 2, is characterized in that: described temperature is the time of reacting under 60 ~ 130 DEG C of conditions is 1.5 ~ 7.5h.
5. preparation method according to claim 2, is characterized in that: described vacuum tightness is the time of continuing under 0.01 ~ 30kPa condition to react is 2 ~ 4h.
6. the application of adhesion promoters according to claim 1 in add-on type liquid silicon rubber, it is characterized in that: successively by the vinyl silicone oil of 100 mass parts, the aluminum oxide of 120 ~ 200 mass parts, the adhesion promoters of 0.8 ~ 6 mass parts, containing hydrogen silicone oil and 0.004 ~ 0.03 mass parts 1 ?Yi Que Ji ?1 ?hexalin add kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound that platinum content is the Platinic chloride of 1500 ~ 4500ppm, stir, deaeration 8 ~ 25min under vacuum tightness 0.5 ~ 50kPa, at 110 ~ 150 DEG C, finally solidify 1 ~ 5h shaping, in described containing hydrogen silicone oil, in si-h bond and vinyl silicone oil and adhesion promoters, the mol ratio of double bond summation is 1:1 ~ 1.6:1, by platinum content note, the consumption of the divinyl tetramethyl disiloxane complex compound of described Platinic chloride accounts for 2 ~ 40ppm of total quality of material.
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| CN109852282A (en) * | 2019-01-30 | 2019-06-07 | 惠州市勤洲建治光学材料有限公司 | A kind of additional organosilicon pressure sensitive adhesive tackifier and preparation method |
| CN112318893B (en) * | 2020-10-19 | 2022-06-28 | 广西北海跃达玻璃钢制品有限公司 | Preparation method of glass fiber reinforced plastic sand inclusion pipe |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1496990A (en) * | 2002-10-07 | 2004-05-19 | 通用电气公司 | Method for preparing organo-silicon composition containing epoxy ethane |
| CN102408869A (en) * | 2011-08-04 | 2012-04-11 | 绵阳惠利电子材料有限公司 | Halogen-free flame-retardant addition type organosilicon potting compound for electronic appliances |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1496990A (en) * | 2002-10-07 | 2004-05-19 | 通用电气公司 | Method for preparing organo-silicon composition containing epoxy ethane |
| CN102408869A (en) * | 2011-08-04 | 2012-04-11 | 绵阳惠利电子材料有限公司 | Halogen-free flame-retardant addition type organosilicon potting compound for electronic appliances |
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