CN103589387A - High-strength bonding room temperature curing organosilicone potting adhesive for LED (light-emitting diode) and preparation method of adhesive - Google Patents
High-strength bonding room temperature curing organosilicone potting adhesive for LED (light-emitting diode) and preparation method of adhesive Download PDFInfo
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- CN103589387A CN103589387A CN201310590767.XA CN201310590767A CN103589387A CN 103589387 A CN103589387 A CN 103589387A CN 201310590767 A CN201310590767 A CN 201310590767A CN 103589387 A CN103589387 A CN 103589387A
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- vinyl
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- potting adhesive
- led
- strength bonding
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 37
- 239000000853 adhesive Substances 0.000 title claims abstract description 33
- 238000004382 potting Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 52
- -1 methyl vinyl Chemical group 0.000 claims abstract description 47
- 239000001257 hydrogen Substances 0.000 claims abstract description 44
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 44
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 42
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 33
- 239000010703 silicon Substances 0.000 claims abstract description 33
- 229920002545 silicone oil Polymers 0.000 claims abstract description 24
- 239000003054 catalyst Substances 0.000 claims abstract description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 39
- 229920002050 silicone resin Polymers 0.000 claims description 35
- 239000012530 fluid Substances 0.000 claims description 31
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- 150000002431 hydrogen Chemical class 0.000 claims description 21
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004821 distillation Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 12
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 10
- RSNQKPMXXVDJFG-UHFFFAOYSA-N tetrasiloxane Chemical compound [SiH3]O[SiH2]O[SiH2]O[SiH3] RSNQKPMXXVDJFG-UHFFFAOYSA-N 0.000 claims description 10
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 10
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 abstract description 5
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000011347 resin Substances 0.000 abstract 3
- 229920005989 resin Polymers 0.000 abstract 3
- 125000003700 epoxy group Chemical group 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 19
- 238000012856 packing Methods 0.000 description 16
- 239000000565 sealant Substances 0.000 description 16
- 238000012360 testing method Methods 0.000 description 9
- LSWYGACWGAICNM-UHFFFAOYSA-N 2-(prop-2-enoxymethyl)oxirane Chemical compound C=CCOCC1CO1 LSWYGACWGAICNM-UHFFFAOYSA-N 0.000 description 8
- 150000003384 small molecules Chemical class 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 150000002118 epoxides Chemical group 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 229920002379 silicone rubber Polymers 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
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- Adhesives Or Adhesive Processes (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a high-strength bonding room temperature curing organosilicone potting adhesive for an LED (light-emitting diode), which comprises a component A and a component B. The component A is prepared by uniformly mixing terminal vinyl silicone oil, hydrogen silicone oil and methyl vinyl MO silicon resin at a weight ratio of 100:(8-100):(15-50). The component B is prepared by uniformly mixing terminal vinyl silicone oil, methyl vinyl MO silicon resin, a catalyst and a tackifier at a weight ratio of 100:(15-50):(0.02-3):(2-24). With the adoption of the methyl vinyl MO silicon resin and the tackifier, namely a hydrogenous cyclosiloxane compound containing epoxy groups and siloxane groups, the mechanical properties, a bonding property and optical properties of the room temperature curing potting adhesive are effectively improved, and a provided preparation technology has concise steps, does not require demanding equipment and therefore, is suitable for industrial production.
Description
Technical field
The present invention relates to Electronic Packaging joint sealant field, specifically high strength bonding self-vulcanizing organic silicon potting adhesive and preparation method thereof for a kind of LED.
Background technology
Flourish along with LED illuminating industry, and the continuing to bring out of the illumination level LED device that requires of high-power, high brightness, long lifetime, organosilicon material relies on its good in optical property, non-yellowing under hot environment, soft, the advantages such as convenient disassembly, substituted epoxy resin gradually, becomes LED packaged material of new generation.And existing organic silicon potting adhesive frangibility, mechanical property does not also reach the requirement of LED encapsulation.In addition, cementability can not meet the requirement of LED substrate bonding, addition-type silicon rubber is generally without cementability, if can improve cementability, between silica gel after solidifying and base material, will there is no space, can prevent the fault that the long-time water vapor permeable occurring causes, guarantee the use properties of electronic devices and components under harsh and unforeseen circumstances.
Summary of the invention
The object of the invention is provides high strength bonding self-vulcanizing organic silicon potting adhesive and preparation method thereof for a kind of LED in order to overcome the defect of above-mentioned prior art existence, after this joint sealant solidifies, there is good optical property, mechanical property and adhesive property, easy to use, output rating and the work-ing life that can obviously improve LED light source.
The present invention also aims to provide the preparation method of a kind of LED with high strength bonding self-vulcanizing organic silicon potting adhesive.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A preparation method for high strength bonding self-vulcanizing organic silicon potting adhesive for LED, comprises the steps:
A, vinyl-terminated silicone fluid, containing hydrogen silicone oil, methyl vinyl MQ silicone resin are mixed and make A component by the weight ratio of 100:8～100:15～50;
B, vinyl-terminated silicone fluid, methyl vinyl MQ silicone resin, catalyzer, tackifier are mixed and make B component by the weight ratio of 100:15～50:0.02～3:2～24;
C, by described component A component and B component, be that mix 1～5:5～1 by weight, vacuum defoamation, solidifies at ambient temperature, obtains high strength bonding self-vulcanizing organic silicon potting adhesive for LED;
Described catalyzer is platinum catalyst, and platinum content is 2000～7000ppm;
Described tackifier are prepared by the following method: by tetramethyl-ring tetrasiloxane, allyl glycidyl and vinyltrimethoxy silane are mixed by the weight ratio of 100:20～70:30～80, under the condition of 20～40 ℃, react 1～3 hour, then under the condition of 40～80 ℃, react 1～3 hour; Mixture underpressure distillation obtains finished product.
For further realizing the object of the invention, preferably, described underpressure distillation be in temperature lower than 60 ℃, pressure is to distill under the condition of-0.1～-0.5MPa.
Described vinyl-terminated silicone fluid is the polydimethylsiloxane of bi-vinyl end-blocking, and vinyl massfraction is 0.16～0.48%, and viscosity is 500～5000mPas, and structural formula is
Wherein, Me represent methylidene; Vi represents vinyl; N represents the polymerization degree; Zhejiang Xinan Chemical Industry Group Co.Ltd.
Described containing hydrogen silicone oil is trimethylammonium or dimethyl or hydroxy-end capped polymethyl hydrogen siloxane, and active hydrogen massfraction is 0.3～1.6%, and viscosity is 30～85mPas, and structural formula is:
Wherein: Me represent methylidene; R represent methylidene or hydrogen base or hydroxyl; P and n represent the polymerization degree; Preferably Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Described methyl vinyl MQ silicone resin refers to the vinyl MQ silicone resin that molecule medium vinyl massfraction is 2.5～4%, and viscosity is 4000～10000mPas, and preferably Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Described tackifier are the hydrogeneous cyclosiloxane compounds containing epoxide group and siloxane groups.
With a high strength bonding self-vulcanizing organic silicon potting adhesive, by above-mentioned preparation method, made.
The present invention compared with prior art possesses following advantage:
1) the present invention is methyl vinyl MQ silicone resin, and containing the hydrogeneous cyclosiloxane compound of epoxide group and siloxane groups, the two adds simultaneously, can improve organic silicon potting adhesive cross-linking set;
2) joint sealant mechanical property of the present invention obviously improves, and also strengthened the adhesiveproperties with materials such as metal, PPA plates, and specific refractory power is close, does not affect its high transmission rate.
3) step of preparation process of the present invention is terse, and without harsh equipment, is applicable to suitability for industrialized production, has saved energy consumption, has reduced cost.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, but the scope of protection of present invention is not limited to the scope of embodiment statement.
Embodiment 1
Tetramethyl-ring tetrasiloxane, glycidyl allyl ether and vinyltrimethoxy silane are mixed by the weight ratio of 100:30:40, at 20 ℃, react 3 hours, at 80 ℃, react 1 hour again, then under the condition that is-0.1MPa in the temperature of 60 ℃, pressure, small molecules is removed in distillation, makes the tackifier of faint yellow oily thickness.
High strength bonding self-vulcanizing organic silicon potting adhesive for preparation LED:
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.16% by vinyl massfraction, active hydrogen massfraction are 0.3%, vinyl massfraction are 4% mixes by the weight ratio of 100:25:15, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.16% by vinyl massfraction, vinyl massfraction are 4%, catalyzer, tackifier mix by the weight ratio of 100:15:0.05:7, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 3000ppm, and Shenzhen silicone Science and Technology Ltd. produces.CMX-30 type
In the present embodiment, vinyl-terminated silicone fluid viscosity is 5000mPas, and 206-5000 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is the polymethyl hydrogen siloxane of dimethyl end-blocking, and viscosity is 30mPas, and 202-03 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicone resin viscosity is 4000mPas, and ASIBO-MVDQ4000 Xing， Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
During use, A component and B component, by weight for 1:1 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 2
By tetramethyl-ring tetrasiloxane, glycidyl allyl ether, vinyltrimethoxy silane are mixed by the weight ratio of 100:70:80, at 30 ℃, react 2 hours, then at 60 ℃, react 2 hours.Then at temperature, the pressure of 30 ℃, be-condition of 0.5MPa under distillation remove small molecules, make the tackifier of faint yellow oily thickness.
High strength bonding self-vulcanizing organic silicon potting adhesive for preparation LED:
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.23% by vinyl massfraction, active hydrogen massfraction are 1.6%, vinyl massfraction are 3% mixes by the weight ratio of 100:10:20, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.23% by vinyl massfraction, vinyl massfraction are 3%, catalyzer, tackifier mix by the weight ratio of 100:20:0.02:2, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 7000ppm, and CMX-70 Xing， Shenzhen silicone Science and Technology Ltd. produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 3000mPas, and 206-3000 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is that hydroxy-end capped polymethyl hydrogen siloxane viscosity is 40mPas, and 202-16 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicone resin viscosity is 6000mPas, ASIBO-MVDQ6000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
A component and B component, by weight for 1:3 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 3
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively above-mentioned raw materials is mixed by the weight ratio of 100:30:80, at 40 ℃, react 1 hour, then at 70 ℃, react 3 hours.Then at temperature, the pressure of 10 ℃, be-condition of 0.3MPa under distillation remove small molecules, make the tackifier of faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.3% by vinyl massfraction, active hydrogen massfraction are 0.5%, vinyl massfraction are 2.7% mixes by the weight ratio of 100:55:25, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.3% by vinyl massfraction, vinyl massfraction are 2.7%, catalyzer, tackifier mix by the weight ratio of 100:25:0.02:3, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 6000ppm, and CMX-60 Xing， Shenzhen silicone Science and Technology Ltd. produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 1000mPas, and 206-1000 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is the polymethyl hydrogen siloxane of trimethylammonium end-blocking, and viscosity is 70mPas, and 202-05 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicone resin viscosity is 8000mPas, ASIBO-MVDQ8000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
A component and B component, by weight for 1:5 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 4
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively above-mentioned raw materials is mixed by the weight ratio of 100:70:40, at 30 ℃, react 3 hours, then at 50 ℃, react 1 hour.Then at temperature, the pressure of 20 ℃, be-condition of 0.5MPa under distillation remove small molecules, make the tackifier of faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.48% by vinyl massfraction, active hydrogen massfraction are 0.8%, vinyl massfraction are 2.5% mixes by the weight ratio of 100:10:30, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.48% by vinyl massfraction, vinyl massfraction are 2.5%, catalyzer, tackifier mix by the weight ratio of 100:30:0.1:20, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 4000ppm, and CMX-40 Xing， Shenzhen silicone Science and Technology Ltd. produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 500mPas, and 206-500 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is the polymethyl hydrogen siloxane of trimethylammonium end-blocking, and viscosity is 85mPas, and 202-08 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicone resin viscosity is 10000mPas, and ASIBO-MVDQ10000 Xing， Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
A component and B component, by weight for 3:1 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 5
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively above-mentioned raw materials is mixed by the weight ratio of 100:50:60, at 40 ℃, react 2 hours, then at 80 ℃, react 2 hours.Then at temperature, the pressure of 50 ℃, be-condition of 0.4MPa under distillation remove small molecules, make the tackifier of faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.16% by vinyl massfraction, active hydrogen massfraction are 0.8%, vinyl massfraction are 2.5% mixes by the weight ratio of 100:8:35, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.16% by vinyl massfraction, vinyl massfraction are 2.5%, catalyzer, tackifier mix by the weight ratio of 100:35:3:24, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 2000ppm, and CMX-20 Xing， Shenzhen silicone Science and Technology Ltd. produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 5000mPas, and 206-5000 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is the polymethyl hydrogen siloxane of dimethyl end-blocking, and viscosity is 85mPas, and 202-08 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicone resin viscosity is 10000mPas, ASIBO-MVDQ10000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
A component and B component, by weight for 5:1 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 6
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively above-mentioned raw materials is mixed by the weight ratio of 100:50:40, at 20 ℃, react 1 hour, then at 70 ℃, react 3 hours.Then at temperature, the pressure of 60 ℃, be-condition of 0.1MPa under distillation remove small molecules, make the tackifier of faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.23% by vinyl massfraction, active hydrogen massfraction are 0.3%, vinyl massfraction are 2.7% mixes by the weight ratio of 100:100:40, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.23% by vinyl massfraction, vinyl massfraction are 2.7%, catalyzer, tackifier mix by the weight ratio of 100:40:0.15:4, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 3000ppm, and CMX-30 Xing， Shenzhen silicone Science and Technology Ltd. produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 3000mPas, and 206-3000 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is the polymethyl hydrogen siloxane of dimethyl end-blocking, and viscosity is 30mPas, and 202-03 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicone resin viscosity is 8000mPas, and ASIBO-MVDQ8000 Xing， Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
A component and B component, by weight for 1:4 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 7
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively above-mentioned raw materials is mixed by the weight ratio of 100:50:80, at 20 ℃, react 2 hours, then at 40 ℃, react 2 hours.Then at the temperature lower than 60 ℃, pressure, be-condition of 0.2MPa under distillation remove small molecules, make the tackifier of faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.3% by vinyl massfraction, active hydrogen massfraction are 0.5%, vinyl massfraction are 3% mixes by the weight ratio of 100:45:45, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.3% by vinyl massfraction, vinyl massfraction are 3%, catalyzer, tackifier mix by the weight ratio of 100:45:0.1:3, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 5000ppm, and CMX-50 Xing， Shenzhen silicone Science and Technology Ltd. produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 1000mPas, and 206-1000 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is hydroxy-end capped polymethyl hydrogen siloxane, and viscosity is 70mPas, and 202-05 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicone resin viscosity is 6000mPas, ASIBO-MVDQ6000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
A component and B component, by weight for 1:2 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 8
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively above-mentioned raw materials is mixed by the weight ratio of 100:30:60, at 40 ℃, react 1 hour, then at 60 ℃, react 3 hours.Then at the temperature lower than 60 ℃, pressure, be-condition of 0.1MPa under distillation remove small molecules, make the tackifier of faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, the methyl vinyl MQ silicone resin that the containing hydrogen silicone oil that the vinyl-terminated silicone fluid that A component is 0.48% by vinyl massfraction, active hydrogen massfraction are 1.6%, vinyl massfraction are 4% mixes by the weight ratio of 100:15:50, and packing; The methyl vinyl MQ silicone resin that the vinyl-terminated silicone fluid that B component is 0.48% by vinyl massfraction, vinyl massfraction are 4%, catalyzer, tackifier mix by the weight ratio of 100:50:0.02:3, and packing.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 7000ppm, and CMX-70 Xing， Shenzhen silicone Science and Technology Ltd. produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is that 500mPas(206-500 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces).
Containing hydrogen silicone oil is the polymethyl hydrogen siloxane of trimethylammonium end-blocking, and viscosity is that 40mPas(202-16 Xing， Zhejiang Xinan Chemical Industry Group Co.Ltd produces).
Methyl vinyl MQ silicone resin viscosity is that 4000mPas(ASIBO-MVDQ4000 Xing， Shanghai Aishibo Organosilicon Material Co., Ltd. produces).
A component and B component, by weight for 2:1 mixes and stirs, are injected among mould, allowed its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED use high strength bonding self-vulcanizing organic silicon potting adhesive.
LED after embodiment 1～embodiment 8 is solidified does performance test with high strength bonding self-vulcanizing organic silicon potting adhesive, and embodiment 1～embodiment 8 makes LED and uses the concrete test result of high strength bonding self-vulcanizing organic silicon potting adhesive in Table 1.Table 1 is used shown in high strength bonding self-vulcanizing organic silicon potting adhesive the performance test results table 1 for embodiment 1～embodiment 8 makes LED.
Hardness test: press GB/T 531.1 ?2008 standards dehydrated alcohol wiping specimen surfaces, measure the hardness of sample with the LX ?A of Shanghai Liu Ling instrument plant type durometer.
Tensile property test: by GB/T 528 ?2009 standards be cut into standard test specimen, with the tensile property of the German Zwick/Roell Z010 of company type universal testing machine mensuration sample, rate of extension is 500mm/min.
Adhesiveproperties test: press GB/T 7124 ?2008 standards, the bonding tensile shear strength with the German Zwick/Roell Z010 of company type universal testing machine mensuration sample to aluminium flake and PPA, evaluates the adhesiveproperties of joint sealant with this.
Electrical performance testing: press the volume specific resistance that the GB/T 1692 ?2008 standard ，Yong U.S. 6517B of Keithley company type meggers are measured sample.Press GB/T 1693 ?2007 standards, measure specific inductivity and the dielectric loss angle tangent of sample.
Transmittance test: at 25 ℃, with the Japanese Hitachi UV of company ?3010 type Zi Wai ?the transmittance of visible spectrophotometer mensuration sample in 200～800nm visible wavelength range.
As seen from Table 1, with patent CN 102850804 A comparisons, joint sealant prepared by the present invention possesses more superior tensile property, transmittance and bonding strength, and has good electrical insulation capability.In raw material of the present invention methyl vinyl MQ silicone resin be between organic and inorganic between material, contain and can participate in curing vinyl groups, can make silicon rubber effectively " Concentrative crosslinking ", thereby improve significantly the tensile property of joint sealant.And containing the hydrogeneous cyclosiloxane compound of epoxide group and siloxane groups, because the silicon hydrogen base containing can react with joint sealant, hydroxyl, epoxide group can form chemical bond with the hydroxyl on aluminium flake, PPA surface, and the tensile property of joint sealant and bonding strength have further lifting.Methyl vinyl MQ silicone resin and all differ minimum with vinyl-terminated silicone fluid containing the specific refractory power of the hydrogeneous cyclosiloxane compound of epoxide group and siloxane groups, therefore still keep high transmission rate.
Table 1
Claims (6)
1. a preparation method for high strength bonding self-vulcanizing organic silicon potting adhesive for LED, is characterized in that comprising the steps:
A, vinyl-terminated silicone fluid, containing hydrogen silicone oil, methyl vinyl MQ silicone resin are mixed and make A component by the weight ratio of 100:8～100:15～50;
B, vinyl-terminated silicone fluid, methyl vinyl MQ silicone resin, catalyzer, tackifier are mixed and make B component by the weight ratio of 100:15～50:0.02～3:2～24;
C, by described component A component and B component, be that mix 1～5:5～1 by weight, vacuum defoamation, solidifies at ambient temperature, obtains high strength bonding self-vulcanizing organic silicon potting adhesive for LED;
Described catalyzer is platinum catalyst, and platinum content is 2000～7000ppm;
Described tackifier are prepared by the following method: by tetramethyl-ring tetrasiloxane, allyl glycidyl and vinyltrimethoxy silane are mixed by the weight ratio of 100:20～70:30～80, under the condition of 20～40 ℃, react 1～3 hour, then under the condition of 40～80 ℃, react 1～3 hour; Mixture underpressure distillation obtains finished product.
2. the preparation method of high strength bonding self-vulcanizing organic silicon potting adhesive for LED according to claim 1, is characterized in that: described underpressure distillation be in temperature lower than 60 ℃, pressure is to distill under the condition of-0.1～-0.5MPa.
3. the preparation method of high strength bonding self-vulcanizing organic silicon potting adhesive for LED according to claim 1, it is characterized in that: described vinyl-terminated silicone fluid is the polydimethylsiloxane of bi-vinyl end-blocking, the mass content of molecule medium vinyl is 0.16～0.48%, and viscosity is 500～5000m mPas.
4. the preparation method of high strength bonding self-vulcanizing organic silicon potting adhesive for LED according to claim 1, it is characterized in that: described containing hydrogen silicone oil is trimethylammonium or dimethyl or hydroxy-end capped polymethyl hydrogen siloxane, the containing hydrogen silicone oil of hydrogen content 0.3～1.6% in molecule, viscosity is 30～85mPas.
5. the preparation method of high strength bonding self-vulcanizing organic silicon potting adhesive for LED according to claim 1, it is characterized in that: described methyl vinyl MQ silicone resin is the vinyl MQ silicone resin of the mass content 0.1～6.5% of molecule medium vinyl, and viscosity is 4000～10000mPas.
6. a high strength bonding self-vulcanizing organic silicon potting adhesive for LED, is characterized in that it is made by preparation method described in claim 1-5 any one.
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