CN104650795A - Preparation method and application of organosilicone pouring sealant adhesive - Google Patents
Preparation method and application of organosilicone pouring sealant adhesive Download PDFInfo
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- CN104650795A CN104650795A CN201510096454.8A CN201510096454A CN104650795A CN 104650795 A CN104650795 A CN 104650795A CN 201510096454 A CN201510096454 A CN 201510096454A CN 104650795 A CN104650795 A CN 104650795A
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Abstract
The invention discloses a preparation method of an organosilicone pouring sealant adhesive. The preparation method of the organosilicone pouring sealant adhesive comprises the following steps: firstly mixing hydroxy methacrylate with titanate uniformly at the room temperature; subsequently adding a silane coupling agent, heating and reacting; and finally removing low-boiling-point substances to obtain the adhesive. The adhesive can be applied to preparation of an LED organosilicone pouring sealant and the preparation method of the LED organosilicone pouring sealant comprise the following steps: adding vinyl silicone oil, methyl vinyl MQ resin, the adhesive, hydrogen-containing silicone oil and 1-acetenyl-cyclohexanol into a kneading machine, uniformly stirring at the room temperature, subsequently adding divinyl-tetramethyl-disiloxane complex of chloroplatinic acid, uniformly stirring, defoaming in vacuum, and finally curing and forming. The adhesive is capable of greatly improving the adhesion of the pouring sealant to a substrate and does not affect the light transmittance of the pouring sealant; the method is simple in construction process; the production efficiency can be greatly improved.
Description
Technical field
The present invention relates to and belongs to electronics adhesive techniques field, is specifically related to the preparation of glue caking agent and utilizes binding agent to prepare the method for organic silicon potting adhesive.
Technical background
Compared with the light sources such as traditional incandescent light, luminescent lamp, LED working current is very little, the electric energy consumed is only 1/10 of conventional light source, do not use the mercury of serious environment pollution, there is the advantages such as energy-saving and environmental protection, volume is little, light, the life-span is long, be expected to the forth generation lighting source become after incandescent light, luminescent lamp, high-intensity gas discharge lamp.Encapsulation is one of important procedure of LED, and it can strengthen the globality of LED, prevents moisture, dust and obnoxious flavour to the erosion of LED, improves the resistibility to external shock, vibrations, extends the work-ing life of LED.
Compared with epoxy resin, organic silicon potting adhesive has and can keep elasticity for a long time at-60 ~ 200 DEG C, does not absorb heat, not heat release during solidification, and solidification post-shrinkage ratio is little, can water-fast, resistance to ozone, weather-proof, the plurality of advantages such as excellent electrical property and chemical stability.But still there are some problem demanding prompt solutions in himself.The additional organosilicon joint sealant sulfuration rear surface overwhelming majority is nonpolar organic group; surface energy is low; thus poor to the cementability of other material; moisture easily causes corrosion and failure of insulation by the infiltration LED inside, space between silicon rubber and base material in use; vibrations may allow itself and base material come off, and make LED lose seal protection.
In order to solve the problem, the cementability of current raising LED organosilicon embedding and base material mainly contains two kinds of methods: one is access cohesiveness group on MQ resin, vinyl MQ resin or ethenylphenyl MQ resin, as epoxy group(ing), ester group etc., the method requires harshness to preparation technology, and promote that the cohesiveness of organic silicon potting adhesive and base material is limited, be difficult to realize industrialization; Two is add small molecules binding agent, as silane coupling agent and titanic acid ester mixture.
The cohesive strength that the binding agent that Chinese patent CN103589387A discloses a kind of tetramethyl-ring tetrasiloxane, glycidyl allyl ether and vinyltrimethoxy silane reaction preparation improves LED organic silicon potting adhesive and base material reaches 0.4MPa; the joint sealant of binder free does not have cohesive strength; but this cohesiveness is still less; need to improve joint sealant cohesive strength further to arrive better seal protection effect, postpone the work-ing life of LED.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of organic silicon potting adhesive binding agent and preparation method thereof is provided, make organic silicon potting adhesive not only have excellent adhesive property, also there is good translucidus, and easy handling.
In order to realize above object, the technical scheme that the present invention takes is: a kind of preparation method of organic silicon potting adhesive binding agent, specifically comprises the following steps: by methacrylic acid hydroxyl ester and weight ratio be first 0.5 ~ 5% titanic acid ester mixed at room temperature even; Add silane coupling agent again, be warming up at 60 ~ 110 DEG C, and react 1 ~ 8h; Finally under temperature 70 ~ 120 DEG C, vacuum tightness 0.06 ~ 0.1MPa condition, slough low-boiling-point substance, obtain binding agent.
Further, methacrylic acid hydroxyl ester is one or more in methacrylic acid-2-hydroxy methacrylate, methacrylic acid-2-hydroxy propyl ester, methacrylic acid-4-hydroxybutyl.
Silane coupling agent is the silane coupling agent containing epoxy group(ing) and alkoxyl group.
Silane coupling agent is glycidyl ether organoalkoxysilane.
Glycidyl ether organoalkoxysilane is one or more in γ-glycidyl ether oxygen propyl trimethoxy silicane, β-(3,4 epoxycyclohexyl)-ethyl triethoxysilane, γ-glycidyl ether oxygen propyl methyldiethoxysilane.
The mol ratio of methacrylic acid hydroxyl ester and silane coupling agent is 1:1 ~ 3:1.
Titanic acid ester is one or more in tetrabutyl titanate, titanium isopropylate, metatitanic acid four tert-butyl ester, the different monooctyl ester of metatitanic acid.
A kind of application of organic silicon potting adhesive binding agent, preparation for organic silicon potting adhesive: divide the 1-ethynyl-1-hexalin of containing hydrogen silicone oil and 0.004 ~ 0.03 mass parts to add kneader the binding agent of the methyl vinyl MQ resin of the vinyl silicone oil of 100 mass parts, 10 ~ 25 mass parts, 0.5 ~ 5 mass parts, 20 ~ 50 quality successively, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound of Platinic chloride of 0.01 ~ 1 mass parts, stir, in vacuum defoamation, at 100 ~ 150 DEG C, finally solidify 1 ~ 5h shaping.
Utilize binding agent prepared by the present invention, directly join organic silicon potting adhesive, significantly can improve the cohesiveness of joint sealant to base material, and not affect the transmittance of joint sealant, the method construction technology is simple, can significantly enhance productivity.
Compared with prior art, the present invention has the following advantages:
1, preparation method of the present invention is easy, easy suitability for industrialized production;
2, consumption of binder of the present invention is less, and the adding the transmittance of organic silicon potting adhesive without impact of binding agent;
3, binding agent is added machine silicon joint sealant and significantly can improve its cohesive strength to aluminium, PPA, LED support by the present invention.
Embodiment
Embodiment 1
The preparation method of organic silicon potting adhesive binding agent is: join in the there-necked flask being with prolong and thermometer by the methacrylic acid-2-hydroxy methacrylate (HEMA) of 13.01g and the tetrabutyl titanate of 0.37g, 25 DEG C stir; Then under agitation slowly add 23.6g γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560), be warming up to 80 DEG C and react 2h; Reaction mixture 80 DEG C, under vacuum tightness 0.08MPa underpressure distillation to steaming without low-boiling-point substance, obtain pale yellow transparent binding agent.
The method that LED organic silicon potting adhesive prepared by application organic silicon potting adhesive binding agent is: be the vinyl silicone oil of 500mPas by 100 mass parts viscosity successively, 25 mass parts methyl vinyl MQ resins, the binding agent A of 0.5 mass parts, 20 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 8min under vacuum tightness 0.1MPa, 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.
Embodiment 2
The preparation method of organic silicon potting adhesive binding agent is: join in the there-necked flask being with condenser and thermometer by the methacrylic acid-2-hydroxy methacrylate (HEMA) of 13.01g and the tetrabutyl titanate of 0.12g, 25 DEG C stir; Then under agitation slowly add the γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) of 11.8g, be warming up to 60 DEG C and react 8h; Reaction mixture 70 DEG C, under vacuum tightness 0.1MPa underpressure distillation to steaming without low-boiling-point substance, obtain pale yellow transparent binding agent.
The method that LED organic silicon potting adhesive prepared by application organic silicon potting adhesive binding agent is: be the vinyl silicone oil of 1000mPas by 100 mass parts viscosity successively, 17.5 mass parts methyl vinyl MQ resin, the binding agent A of 2.5 mass parts, 35 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 0.01 mass parts platinum content is the Platinic chloride of 2600ppm, stir, deaeration 8min under vacuum tightness 0.1Pa, finally at 100 DEG C, solidify 5h shaping.The performance of sample is as shown in table 1, and testing method illustrates in table 1.
Embodiment 3
The preparation method of organic silicon potting adhesive binding agent is: join in the there-necked flask being with prolong and thermometer by the methacrylic acid-2-hydroxy methacrylate (HEMA) of 13.01g and the tetrabutyl titanate of 1.04g, 25 DEG C stir; Then under agitation slowly add the γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560) of 7.87g, be warming up to 110 DEG C and react 1h; Reaction mixture 120 DEG C, under vacuum tightness 0.06MPa underpressure distillation to steaming without low-boiling-point substance, obtain pale yellow transparent binding agent.
The method that LED organic silicon potting adhesive prepared by application organic silicon potting adhesive binding agent is: be the vinyl silicone oil of 4000mPas by 100 mass parts viscosity successively, 10 mass parts methyl vinyl MQ resins, the binding agent A of 5 mass parts, 50 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 1 mass parts platinum content is the Platinic chloride of 2600ppm, stir, deaeration 8min under vacuum tightness 0.1Pa, finally at 150 DEG C, solidify 1h shaping.The performance of sample is as shown in table 1, and testing method illustrates in table 1.
Embodiment 4
The preparation method of organic silicon potting adhesive binding agent is: join in the there-necked flask being with prolong and thermometer by the methacrylic acid-2-hydroxy propyl ester (HPMA) of 14.42g and the titanium isopropylate of 0.38g, 25 DEG C stir; Then under agitation slowly add β-(3,4 epoxycyclohexyl)-ethyl triethoxysilane of 24.64g, be warming up to 80 DEG C and react 2h; Reaction mixture 80 DEG C, under vacuum tightness 0.08MPa underpressure distillation to steaming without low-boiling-point substance, obtain pale yellow transparent binding agent.
The method that LED organic silicon potting adhesive prepared by application organic silicon potting adhesive binding agent is: be the vinyl silicone oil of 500mPas by 100 mass parts viscosity successively, 25 mass parts methyl vinyl MQ resins, the binding agent A of 5 mass parts, 20 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 0.38 mass parts platinum content is the Platinic chloride of 2600ppm, stir, deaeration 8min under vacuum tightness 0.1Pa, finally at 150 DEG C, solidify 1h shaping.The performance of sample is as shown in table 1, and testing method illustrates in table 1.
Embodiment 5
The preparation method of organic silicon potting adhesive binding agent is: join in 250mL there-necked flask by metatitanic acid four tert-butyl ester of the methacrylic acid-4-hydroxybutyl of 15.83g and 0.41g, 25 DEG C stir; Then under agitation slowly add the γ-glycidyl ether oxygen propyl methyldiethoxysilane of 24.84g, be warming up to 80 DEG C and react 2h; Reaction mixture 80 DEG C, under vacuum tightness 0.08MPa underpressure distillation to steaming without low-boiling-point substance, obtain pale yellow transparent binding agent.
The method that LED organic silicon potting adhesive prepared by application organic silicon potting adhesive binding agent is: be the vinyl silicone oil of 500mPas by 100 mass parts viscosity successively, 25 mass parts methyl vinyl MQ resins, the binding agent A of 5 mass parts, 20 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 0.38 mass parts platinum content is the Platinic chloride of 2600ppm, stir, deaeration 8min under vacuum tightness 0.1MPa, finally at 150 DEG C, solidify 1h shaping.The performance of sample is as shown in table 1, and testing method illustrates in table 1.
Conventional example
Be the vinyl silicone oil of 500mPas successively by 100 mass parts viscosity, 10 mass parts methyl vinyl MQ resins, 20 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 solidifies 2h shaping at 130 DEG C.The performance of sample is as shown in table 1, and testing method illustrates in table 1.
In table 1, product performance testing method is as follows:
1, transmittance: at 25 DEG C, measures the transmittance of sample at 200 ~ 800nm visible wavelength range with ultraviolet-visible spectrophotometer.
2, cohesive strength: according to the bonding tensile shear strength of GB/T 13936-1992 mensuration silicon rubber with aluminium, PPA.
3, tensile strength and elongation at break: the tensile strength and the elongation at break that measure silicon rubber according to GB/T 528-2009.
4, Shao A hardness: the Shore A hardness measuring silicon rubber according to GB/T 531-2008.
Table 1 LED organic silicon potting adhesive the performance test results
As shown in Table 1, after adding the LED organic silicon potting adhesive of the binding agent of the present invention's synthesis, the shearing resistance of joint sealant improves 4.5 times than minimum during non-adding additives, than cohesive strength 0.37MPa disclosed in patent CN103589387A, improve at least 1.7 times, show that the binding agent prepared by method of the present invention significantly can improve the adhesive property of LED organic silicon potting adhesive; And such binding agent on the transmittance of joint sealant substantially without impact.
Claims (8)
1. a preparation method for organic silicon potting adhesive binding agent, is characterized in that specifically comprising the following steps:
By methacrylic acid hydroxyl ester and weight ratio be first 0.5 ~ 5% titanic acid ester mixed at room temperature even;
Add silane coupling agent again, be warming up at 60 ~ 110 DEG C, and react 1 ~ 8h;
Finally under temperature 70 ~ 120 DEG C, vacuum tightness 0.06 ~ 0.1MPa condition, slough low-boiling-point substance, obtain binding agent.
2. the preparation method of the organic silicon potting adhesive binding agent according to right 1, is characterized in that described methacrylic acid hydroxyl ester is one or more in methacrylic acid-2-hydroxy methacrylate, methacrylic acid-2-hydroxy propyl ester, methacrylic acid-4-hydroxybutyl.
3. the preparation method of the organic silicon potting adhesive binding agent according to right 1, is characterized in that described silane coupling agent is the silane coupling agent containing epoxy group(ing) and alkoxyl group.
4. the preparation method of the organic silicon potting adhesive binding agent according to right 3, is characterized in that described silane coupling agent is glycidyl ether organoalkoxysilane.
5. the preparation method of the organic silicon potting adhesive binding agent according to right 4, it is characterized in that described glycidyl ether organoalkoxysilane is one or more in γ-glycidyl ether oxygen propyl trimethoxy silicane, β-(3,4 epoxycyclohexyl)-ethyl triethoxysilane, γ-glycidyl ether oxygen propyl methyldiethoxysilane.
6. the preparation method of the organic silicon potting adhesive binding agent according to right 1, is characterized in that the mol ratio of described methacrylic acid hydroxyl ester and silane coupling agent is 1:1 ~ 3:1.
7. the preparation method of the organic silicon potting adhesive binding agent according to right 1, is characterized in that described titanic acid ester is one or more in tetrabutyl titanate, titanium isopropylate, metatitanic acid four tert-butyl ester, the different monooctyl ester of metatitanic acid.
8. the application of an organic silicon potting adhesive binding agent, it is characterized in that the preparation for organic silicon potting adhesive: successively by the vinyl silicone oil of 100 mass parts, the methyl vinyl MQ resin of 10 ~ 25 mass parts, the binding agent of 0.5 ~ 5 mass parts, 20 ~ 50 quality divide the 1-ethynyl-1-hexalin of containing hydrogen silicone oil and 0.004 ~ 0.03 mass parts to add kneader, at room temperature stir, and then add the divinyl tetramethyl disiloxane complex compound of Platinic chloride of 0.01 ~ 1 mass parts, stir, in vacuum defoamation, at 100 ~ 150 DEG C, finally solidify 1 ~ 5h shaping.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001813A (en) * | 2015-07-17 | 2015-10-28 | 六淳胶粘制品（深圳）有限公司 | Organosilicone-modified acrylic pressure-sensitive adhesive and preparation method thereof |
| CN105713201A (en) * | 2016-02-04 | 2016-06-29 | 华南理工大学 | Organosilicon bonding promoter for LED packaging high-refractive-index addition-type silica gel and preparation method and application of organosilicon bonding promoter |
| CN114456383A (en) * | 2022-02-15 | 2022-05-10 | 广东皓明有机硅材料有限公司 | Organic silicon adhesion promoter for LED packaging and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102516775A (en) * | 2011-12-07 | 2012-06-27 | 唐山三友硅业有限责任公司 | High adhesiveness silicone gel for embedding precision electron component |
| CN102898972A (en) * | 2012-10-29 | 2013-01-30 | 华南理工大学 | Preparation method of tackifier for addition type silicone pouring sealant |
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2015
- 2015-03-05 CN CN201510096454.8A patent/CN104650795A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516775A (en) * | 2011-12-07 | 2012-06-27 | 唐山三友硅业有限责任公司 | High adhesiveness silicone gel for embedding precision electron component |
| CN102898972A (en) * | 2012-10-29 | 2013-01-30 | 华南理工大学 | Preparation method of tackifier for addition type silicone pouring sealant |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105001813A (en) * | 2015-07-17 | 2015-10-28 | 六淳胶粘制品（深圳）有限公司 | Organosilicone-modified acrylic pressure-sensitive adhesive and preparation method thereof |
| CN105713201A (en) * | 2016-02-04 | 2016-06-29 | 华南理工大学 | Organosilicon bonding promoter for LED packaging high-refractive-index addition-type silica gel and preparation method and application of organosilicon bonding promoter |
| CN114456383A (en) * | 2022-02-15 | 2022-05-10 | 广东皓明有机硅材料有限公司 | Organic silicon adhesion promoter for LED packaging and preparation method and application thereof |
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Application publication date: 20150527 |