CN105001422A - Tackifier for addition silicone, preparation method of tackifier and addition silicone - Google Patents
Tackifier for addition silicone, preparation method of tackifier and addition silicone Download PDFInfo
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- CN105001422A CN105001422A CN201510367129.0A CN201510367129A CN105001422A CN 105001422 A CN105001422 A CN 105001422A CN 201510367129 A CN201510367129 A CN 201510367129A CN 105001422 A CN105001422 A CN 105001422A
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Abstract
The invention discloses a tackifier for addition silicone, a preparation method of the tackifier and addition silicone. The preparation method comprises adding high hydrogen content phenyl silicone oil and toluene into a reactor, carrying out heating, adding a platinum catalyst into the reactor at a temperature of 60-100 DEG C, carrying out full mixing, adding KH570 into the mixture at a temperature of 60-100 DEG C, carrying out a reaction process at a temperature of 60-100 DEG C for 1h or more, adding allyl glycidyl ether into the reaction product at a temperature of 60-100 DEG C, carrying out a reaction process a temperature of 60-100 DEG C for 1h or more, and removing low-boiling-point substances at a temperature of 80-100 DEG C at a vacuum degree of 0.001-0.01MPa so that the tackifier is obtained. The tackifier for addition silicone is a colorless and transparent liquid, has no peculiar smell, has good stability and can be stored for a long time. The tackifier for addition silicone can improve adhesion of the addition silicone cured at a middle temperature to the base material.
Description
Technical field
The present invention relates to addition-type silicon rubber technical field, particularly relate to a kind of addition-type silicon rubber tackifier and preparation method thereof and addition-type silicon rubber.
Background technology
Addition-type silicon rubber is a kind of nonpoisonous and tasteless, organosilicon material with excellent weather resistance and electrical insulating property, be development in recent years one of high-grade organosilicon kind faster, be applied to the industries such as electronic apparatus, machinery, automobile, building more and more widely at present.
But because addition-type silicon rubber self-molecules present polarity is low, it solidifies rear and base material, and especially the adhesiveproperties of plastic basis material is poor.When using as sealing, embedding, coating, inserts, injecting forming material, for improving addition-type silicon rubber to the cementability of institute's contact material, usually can do primary coat process to base material in advance or add tackifier in addition-type silicon rubber.Silane coupling agent is expensive and add production process, reduces production efficiency, and containing inflammable organic solvent in silane coupling agent, adds the danger in accumulating, use procedure.And in addition-type silicon rubber formula, add the problem that tackifier do not have above-mentioned use silane coupling agent, can improve the cementability of silicon rubber and base material preferably, therefore, tackifier are the focuses that raising addition-type silicon rubber and substrate bonding are studied always.
A series of silicon nitrogen heterocyclic tackifier that US Patent No. 5945555 is synthesized, add in addition-type silicon rubber, although solidification is rear and base material, especially PC has good cementability, but silicon rubber has impact in low-temperature curing, only solidify at the temperature of relatively high (120 DEG C) and just can have bonding with base material.Higher solidification value is unfavorable for energy-conservation on the one hand, likely damages on the other hand to plastic basis material itself, produces defect.
Japanese patent discloses of patent No. Unexamined Patent 8-311340 " 3-glycidoxy Trimethoxy silane and quaternary ammonium salt are also used as the tackifier of addition-type silicon rubber ", said composition also can promote the cohesive force of addition-type silicon rubber, adhesive surface is also comparatively wide, but can affect the curing performance of glue; Quaternary ammonium salt has certain alkalescence, also has a certain impact to the extended storage stability of glue.
CN 101605857A discloses a kind of composition, said composition contains reaction product or is made up of this reaction product, and wherein said reaction product is obtained by the reaction mixture of the epoxy radicals silicone hydride comprising the aminosilane of following formula (I), the hydrosulphonyl silane of formula (II) and formula (III):
Above-mentioned composition is suitable as tackifier, particularly the tackifier of priming paint form.They have good adhesivity and are particularly suitable for low application and are particularly suitable for bonding glass.But stability when above tackifier are added in product and cohesive force still can not meet existing needs.
Therefore, prior art need development.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of addition-type silicon rubber tackifier and preparation method thereof and addition-type silicon rubber, described addition-type silicon rubber tackifier may be used for increasing the bonding force of addition-type silicon rubber to metal and PC base material, are intended to solve addition-type silicon rubber tackifier in prior art and there is good not etc. the problem of unstable and cohesive force.
Technical scheme of the present invention is as follows:
A preparation method for addition-type silicon rubber tackifier, wherein, comprises the following steps:
A, the high hydrogeneous phenyl silicone oil of 100 ~ 150 mass parts and 50 ~ 100 mass parts toluene are added reactor;
B, intensification, add 0.1 ~ 0.6 mass parts platinum catalyst under 60 ~ 100 DEG C of conditions, after mixing, adds 25 ~ 75 mass parts KH570 under 60 ~ 100 DEG C of conditions;
C, reaction more than 1 hour under 60 ~ 100 DEG C of conditions; 25 ~ 75 mass parts glycidyl allyl ethers are added under 60 ~ 100 DEG C of conditions;
D, reaction more than 1 hour under 60 ~ 100 DEG C of conditions;
E, 100 DEG C, under vacuum tightness is the condition of 0.01MPa, sloughs low-boiling-point substance, obtain tackifier.
The preparation method of described addition-type silicon rubber tackifier, wherein, in the hydrogeneous phenyl silicone oil of described height, in per molecule ,-SiH is greater than 10 moles, and phenyl content is at 1%-30% mole.
The preparation method of described addition-type silicon rubber tackifier, wherein, in the hydrogeneous phenyl silicone oil of described height in per molecule-SiH content is 20-50 mole, phenyl content is 5%-25% mole.
The preparation method of described addition-type silicon rubber tackifier, in the hydrogeneous phenyl silicone oil of wherein said height in per molecule-SiH content is 30 moles, phenyl content is 20% mole.
The preparation method of described addition-type silicon rubber tackifier, wherein, described platinum catalyst to be massfraction be 0.3% Platinic chloride toluene solution.
The preparation method of described addition-type silicon rubber tackifier, wherein, in step b, KH570 added complete in 30 minutes; In step c, glycidyl allyl ether added complete in 30 minutes.
The preparation method of described addition-type silicon rubber tackifier, wherein, in step b, c, d, temperature of reaction is 80 DEG C.
A kind of addition-type silicon rubber tackifier, wherein, adopt the preparation method of addition-type silicon rubber tackifier as above to prepare.
A kind of addition-type silicon rubber, wherein, described addition-type silicon rubber requires the addition-type silicon rubber tackifier described in 8 containing, for example right profit.
Beneficial effect: the preparation method that the invention provides a kind of new addition-type silicon rubber tackifier, adopt the addition-type silicon rubber tackifier colourless transparent liquid that this method prepares, without any peculiar smell, good stability, can long-term storage.The addition-type silicon rubber tackifier obtained can improve additional organosilicon rubber good bonding after intermediate temperature setting with base material, especially can improve the cementability to polycarbonate (PC) base material.By obtained addition-type silicon rubber tackifier, add in dual composition addition type silicone resin, gained addition-type silicon rubber resin is without any peculiar smell, strong to PC bonding force, solves PC and glass and intermetallic bonding problem simultaneously.
Embodiment
The invention provides a kind of addition-type silicon rubber tackifier and preparation method thereof and addition-type silicon rubber, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The preparation method of a kind of addition-type silicon rubber tackifier provided in the present invention, comprises the following steps:
(1) high for 100 ~ 150 mass parts hydrogeneous phenyl silicone oil and 50 ~ 100 mass parts toluene are added reactor;
(2) heat up, under 60 ~ 100 DEG C of conditions, slowly add 0.1 ~ 0.6 mass parts platinum catalyst, stir 30 minutes; To be mixed evenly after, under 60 ~ 100 DEG C of conditions, slowly add 25 ~ 75 mass parts KH570;
(3) react more than 1 hour under 60 ~ 100 DEG C of conditions; 25 ~ 75 mass parts glycidyl allyl ethers are slowly added under 60 ~ 100 DEG C of conditions;
(4) react more than 1 hour under 60 ~ 100 DEG C of conditions;
(5) 80 ~ 100 DEG C, under vacuum tightness is the condition of 0.001 ~ 0.01MPa, sloughs low-boiling-point substance, obtain tackifier.
Further, reactor described in step (1) is four mouthfuls of glass reaction bottles with speed-adjustable stir, thermometer and reflux condensing tube, and whole reaction process is carried out under condensing reflux condition.
In the hydrogeneous phenyl silicone oil of described height, in per molecule ,-SiH is greater than 10 moles, is preferably 20-50 mole, is particularly preferably 30 moles.In the hydrogeneous phenyl silicone oil of described height, phenyl content is at 1%-30% mole, is preferably 5%-25% mole, is particularly preferably 20% mole.
In step (2), KH570 adds after platinum catalyst is uniformly dispersed, and being incorporated as of KH570 slowly adds, and can add complete in 30 minutes.Described KH570 and γ-methacryloxypropyl trimethoxy silane, it is a kind of organo functional silanes's coupling agent, be mainly used in the adhesiveproperties improving organic materials and inorganic materials, be specially adapted to the polyester rubber that radical is crosslinked, polyolefine, polystyrene and in photochromics as auxiliary agent.
In step (3), glycidyl allyl ether adds after KH570 reacts completely again, and being incorporated as of glycidyl allyl ether slowly adds, and can add complete in 30 minutes.
In step (2) (3) (4), temperature of reaction is 60 ~ 100 DEG C.Preferably, temperature of reaction is 80 DEG C, fully reacts and can avoid being cross-linked.
In step (5), the optimum condition sloughing low-boiling-point substance is 80 ~ 100 DEG C, vacuum tightness is under the condition of 0.001 ~ 0.01MPa, sloughs low-boiling-point substance, obtains tackifier.
The addition-type silicon rubber tackifier adopting the inventive method to prepare need seal preservation.Product is colourless transparent liquid, and without any peculiar smell, good stability, can long-term storage.The addition-type silicon rubber tackifier obtained can improve additional organosilicon rubber good bonding after intermediate temperature setting with base material, especially can improve the cementability to polycarbonate (PC) base material.By obtained addition-type silicon rubber tackifier, add in dual composition addition type silicone resin, gained addition-type silicon rubber resin is without any peculiar smell, strong to PC bonding force, solves PC and glass and intermetallic bonding problem simultaneously.
Therefore, also provide a kind of addition-type silicon rubber tackifier in the present invention, described addition-type silicon rubber tackifier adopt above-mentioned preparation method to prepare.Also provide a kind of addition-type silicon rubber in the present invention, in described addition-type silicon rubber, also have described addition-type silicon rubber tackifier.
Below by way of specific embodiment, the present invention will be further described.
Embodiment 1
High for 150 mass parts hydrogeneous phenyl silicone oil and 75 mass parts toluene are added reactor; Heat up, slowly add at 80 DEG C the platinum catalyst that 0.23 mass parts massfraction is the Platinic chloride of 0.3%, stir 30 minutes; To be mixed evenly after slowly add 40 mass parts KH570 at 80 DEG C in slow 30 minutes; 80 DEG C of reactions more than 1 hour; 40 mass parts glycidyl allyl ethers are slowly added in slow 30 minutes at 80 DEG C; 80 DEG C of reactions 1 hour; 100 DEG C of vacuum tightnesss are that 0.01MPa sloughs low-boiling-point substance, obtain water white transparency tackifier.
Embodiment 2
High for 120 mass parts hydrogeneous phenyl silicone oil and 75 mass parts toluene are added reactor; Heat up, slowly add at 80 DEG C the platinum catalyst that 0.23 mass parts massfraction is the Platinic chloride of 0.3%, stir 30 minutes; To be mixed evenly after slowly add 40 mass parts KH570 at 80 DEG C in slow 30 minutes; 80 DEG C of reactions more than 1 hour; 40 mass parts glycidyl allyl ethers are slowly added in slow 30 minutes at 80 DEG C; 80 DEG C of reactions 1 hour; 100 DEG C of vacuum tightnesss are that 0.01MPa sloughs low-boiling-point substance, obtain water white transparency tackifier.
Embodiment 3
High for 150 mass parts hydrogeneous phenyl silicone oil and 75 mass parts toluene are added reactor; Heat up, slowly add at 60 DEG C the platinum catalyst that 0.23 mass parts massfraction is the Platinic chloride of 0.3%, stir 30 minutes; To be mixed evenly after slowly add 40 mass parts KH570 at 60 DEG C in slow 30 minutes; 60 DEG C of reactions more than 8 hours; 40 mass parts glycidyl allyl ethers are slowly added in slow 30 minutes at 60 DEG C; 60 DEG C of reactions 8 hours; 80 DEG C of vacuum tightnesss are that 0.001MPa sloughs low-boiling-point substance, obtain water white transparency tackifier.
Comparative example 1
High for 150 mass parts hydrogeneous phenyl silicone oil and 75 mass parts toluene are added reactor; Heat up, slowly add at 80 DEG C the platinum catalyst that 0.23 mass parts massfraction is the Platinic chloride of 0.3%, stir 30 minutes; To be mixed evenly after slowly add 40 mass parts KH570 at 80 DEG C in slow 30 minutes; 60 ~ 100 DEG C of reactions more than 1 hour; 100 DEG C of vacuum tightnesss are that 0.01MPa sloughs low-boiling-point substance, obtain water white transparency tackifier.
Comparative example 2
High for 150 mass parts hydrogeneous phenyl silicone oil and 75 mass parts toluene are added reactor; Heat up, slowly add at 80 DEG C the platinum catalyst that 0.23 mass parts massfraction is the Platinic chloride of 0.3%, stir 30 minutes; To be mixed evenly after slowly add 40 mass parts glycidyl allyl ethers at 80 DEG C in slow 30 minutes; 80 DEG C of reactions 1 hour; 100 DEG C of vacuum tightnesss are that 0.01MPa sloughs low-boiling-point substance, obtain water white transparency tackifier.
Comparative example 3
150 mass parts height containing hydrogen silicone oils and 75 mass parts toluene are added reactor; Heat up, slowly add at 80 DEG C the platinum catalyst that 0.23 mass parts massfraction is the Platinic chloride of 0.3%, stir 30 minutes; To be mixed evenly after slowly add 40 mass parts KH570 at 80 DEG C in slow 30 minutes; 80 DEG C of reactions more than 1 hour; 40 mass parts glycidyl allyl ethers are slowly added in slow 30 minutes at 80 DEG C; 80 DEG C of reactions 1 hour; 100 DEG C of vacuum tightnesss are that 0.01MPa sloughs low-boiling-point substance, obtain water white transparency tackifier.
Be more than comparative example, in the tackifier that comparative example 1 is synthesized, introduce epoxy group(ing) without allyl group; Without the ester group that KH570 introduces in comparative example 2; Introduce without phenyl in comparative example 3.
The addition-type silicon rubber of following methods to embodiment and comparative example is adopted to carry out bond strength test.The preparation of add-on type liquid silicon rubber: at 100 parts of viscosity 10000mPas, by CH
2cH (CH
3)
2siO
1/2in the polydimethylsiloxane of chain link end-blocking, add 30 parts of specific surface area 200m
2the thermal silica of/g, 5 parts of hexamethyldisilazanes and 2 parts of water; In kneader mixing homogeneous after, reduce pressure lower 170 DEG C of mixing 2h, is made into base-material.In 100 parts of cooled base-materials, add the tackifier 1.5 parts of above-mentioned synthesis.1.6 parts of viscosity 20mPas, (CH
3)
3siO
1/2(the CH of chain link end-blocking
3)
2siO/CH
3hSiO multipolymer (in 1 molecule containing 20 SiH yls), 0.06 part of alkynol, 0.3 part of platinum massfraction is the platinum-vinyl siloxane title complex of 0.2%, mixes homogeneous, is made into add-on type liquid silicon rubber.
Select the bonding sample of the following base material of 100mm × 20mm × 3mm, before painting silicon rubber, first remove the bonding plane of base material with acetone; Silicon rubber is coated in substrate bonding face; Then two pieces of substrate bonding faces closed up and pressurize gently, making the distance between bonding plane be 1mm; It is steadily placed, within 3 minutes, becomes 150 DEG C of sulfurations.Rubber layer is manually peeled off from one-piece type goods.According to cohesive failure assessment binding property.Result is shown shown in following table 1.As can be seen from the detected result of table 1, the cohesive force of addition-type silicon rubber to PC, Al, Cu glass that with the addition of embodiment 1,2,3 tackifier is best.
Table 1
| Base material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| PC | Ο | Ο | Ο | × | Δ | Δ |
| Al | Ο | Ο | Ο | Δ | Δ | ×/Δ |
| Cu | Ο | Ο | Ο | ×/Δ | × | ×/Δ |
| Glass | Ο | Ο | Ο | × | Δ | ×/Δ |
Wherein, the implication of symbol is: Ο: cohesive failure >=80%; Δ: 30%≤cohesive failure <80%; ×/Δ: 0%< cohesive failure <30%; ×: cohesive failure=0% (stripping).
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (9)
1. a preparation method for addition-type silicon rubber tackifier, is characterized in that, comprises the following steps:
A, the high hydrogeneous phenyl silicone oil of 100 ~ 150 mass parts and 50 ~ 100 mass parts toluene are added reactor;
B, intensification, add 0.1 ~ 0.6 mass parts platinum catalyst under 60 ~ 100 DEG C of conditions, after mixing, adds 25 ~ 75 mass parts KH570 under 60 ~ 100 DEG C of conditions;
C, reaction more than 1 hour under 60 ~ 100 DEG C of conditions; 25 ~ 75 mass parts glycidyl allyl ethers are added under 60 ~ 100 DEG C of conditions;
D, reaction more than 1 hour under 60 ~ 100 DEG C of conditions;
E, 80 ~ 100 DEG C, under vacuum tightness is the condition of 0.001 ~ 0.01MPa, sloughs low-boiling-point substance, obtain tackifier.
2. the preparation method of addition-type silicon rubber tackifier according to claim 1, is characterized in that, in the hydrogeneous phenyl silicone oil of described height, in per molecule ,-SiH is greater than 10 moles, and phenyl content is at 1%-30% mole.
3. the preparation method of addition-type silicon rubber tackifier according to claim 2, is characterized in that, in the hydrogeneous phenyl silicone oil of described height in per molecule-SiH content is 20-50 mole, phenyl content is 5%-25% mole.
4. the preparation method of addition-type silicon rubber tackifier according to claim 3, is characterized in that, in the hydrogeneous phenyl silicone oil of described height in per molecule-SiH content is 30 moles, phenyl content is 20% mole.
5. want the preparation method of the addition-type silicon rubber tackifier described in 1 according to right, it is characterized in that, described platinum catalyst to be massfraction be 0.3% Platinic chloride toluene solution.
6. want the preparation method of the addition-type silicon rubber tackifier described in 1 according to right, it is characterized in that, in step b, KH570 added complete in 30 minutes; In step c, glycidyl allyl ether added complete in 30 minutes.
7. want the preparation method of the addition-type silicon rubber tackifier described in 1 according to right, it is characterized in that, in step b, c, d, temperature of reaction is 80 DEG C.
8. addition-type silicon rubber tackifier, is characterized in that, adopt as arbitrary in claim 1 ~ 7 as described in the preparation method of addition-type silicon rubber tackifier prepare.
9. an addition-type silicon rubber, is characterized in that, described addition-type silicon rubber is containing, for example addition-type silicon rubber tackifier according to claim 8.
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| CN106279700A (en) * | 2016-08-08 | 2017-01-04 | 岳胜武 | Add-on type liquid silicon rubber viscosifier, preparation method and applications |
| CN107674608A (en) * | 2017-10-19 | 2018-02-09 | 张恩天 | Silicon rubber tackifier, liquid two-component addition-type silicon rubber prepared therefrom and its application |
| CN108164705A (en) * | 2017-12-18 | 2018-06-15 | 深圳市康利邦科技有限公司 | A kind of odorlessness add-on type liquid silicon rubber tackifier and its preparation method and application |
| CN109722028A (en) * | 2018-12-11 | 2019-05-07 | 安徽太平洋电缆股份有限公司 | Addition-type silicon rubber |
| CN110922601A (en) * | 2019-11-22 | 2020-03-27 | 新安天玉有机硅有限公司 | Liquid silicone rubber made of bi-component self-adhesive PC material and preparation method thereof |
| CN111117560A (en) * | 2020-01-08 | 2020-05-08 | 东莞新东方科技有限公司 | Preparation method of addition type liquid silicone rubber with specific adhesion to PC material |
| CN116855083A (en) * | 2023-06-12 | 2023-10-10 | 中国南方电网有限责任公司超高压输电公司广州局 | High-heat-conductivity silicon rubber for transistor and preparation process thereof |
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| CN106279700A (en) * | 2016-08-08 | 2017-01-04 | 岳胜武 | Add-on type liquid silicon rubber viscosifier, preparation method and applications |
| CN107674608A (en) * | 2017-10-19 | 2018-02-09 | 张恩天 | Silicon rubber tackifier, liquid two-component addition-type silicon rubber prepared therefrom and its application |
| CN107674608B (en) * | 2017-10-19 | 2020-07-17 | 张恩天 | Silicone rubber tackifier, liquid two-component addition type silicone rubber prepared from silicone rubber tackifier and application of silicone rubber tackifier |
| CN108164705A (en) * | 2017-12-18 | 2018-06-15 | 深圳市康利邦科技有限公司 | A kind of odorlessness add-on type liquid silicon rubber tackifier and its preparation method and application |
| CN109722028A (en) * | 2018-12-11 | 2019-05-07 | 安徽太平洋电缆股份有限公司 | Addition-type silicon rubber |
| CN110922601A (en) * | 2019-11-22 | 2020-03-27 | 新安天玉有机硅有限公司 | Liquid silicone rubber made of bi-component self-adhesive PC material and preparation method thereof |
| CN111117560A (en) * | 2020-01-08 | 2020-05-08 | 东莞新东方科技有限公司 | Preparation method of addition type liquid silicone rubber with specific adhesion to PC material |
| CN116855083A (en) * | 2023-06-12 | 2023-10-10 | 中国南方电网有限责任公司超高压输电公司广州局 | High-heat-conductivity silicon rubber for transistor and preparation process thereof |
| CN116855083B (en) * | 2023-06-12 | 2024-03-12 | 中国南方电网有限责任公司超高压输电公司广州局 | High-heat-conductivity silicon rubber for transistor and preparation process thereof |
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Effective date of registration: 20190306 Address after: 324012 No. 62 Nianhua Road, Quzhou City, Zhejiang Province Patentee after: Zhejiang Sunri Silicone Material Co., Ltd. Address before: 518000 Factory Building I and C of Sifangpu Village, Nianfeng Community, Pingdi Street, Longgang District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Square Silicone Co., Ltd. |