CN103589387B - LED high strength bonding self-vulcanizing organic silicon potting adhesive and preparation method thereof - Google Patents
LED high strength bonding self-vulcanizing organic silicon potting adhesive and preparation method thereof Download PDFInfo
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- CN103589387B CN103589387B CN201310590767.XA CN201310590767A CN103589387B CN 103589387 B CN103589387 B CN 103589387B CN 201310590767 A CN201310590767 A CN 201310590767A CN 103589387 B CN103589387 B CN 103589387B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 68
- 239000010703 silicon Substances 0.000 title claims abstract description 68
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 34
- 239000000853 adhesive Substances 0.000 title claims abstract description 29
- 238000004382 potting Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- -1 methyl vinyl Chemical group 0.000 claims abstract description 47
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 44
- 239000001257 hydrogen Substances 0.000 claims abstract description 44
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 41
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 239000011347 resin Substances 0.000 claims abstract description 38
- 239000012530 fluid Substances 0.000 claims abstract description 33
- 229920002545 silicone oil Polymers 0.000 claims abstract description 22
- 229920002554 vinyl polymer Polymers 0.000 claims description 50
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 40
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 24
- 150000002431 hydrogen Chemical class 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 238000004821 distillation Methods 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
- 239000003054 catalyst Substances 0.000 claims description 2
- 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
- 239000000565 sealant Substances 0.000 abstract description 18
- 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
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 125000003700 epoxy group Chemical group 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 19
- 238000005516 engineering process Methods 0.000 description 9
- LSWYGACWGAICNM-UHFFFAOYSA-N 2-(prop-2-enoxymethyl)oxirane Chemical compound C=CCOCC1CO1 LSWYGACWGAICNM-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 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
- 238000012360 testing method Methods 0.000 description 6
- 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
- 125000002496 methyl group Chemical group [H]C([H])([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
- 238000005286 illumination 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
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000003283 Pachira macrocarpa Nutrition 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 241001083492 Trapa Species 0.000 description 1
- 235000014364 Trapa natans Nutrition 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 235000009165 saligot Nutrition 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
Abstract
The invention discloses a kind of LED high strength bonding self-vulcanizing organic silicon potting adhesive, this joint sealant comprises A, B two-pack, and vinyl-terminated silicone fluid, containing hydrogen silicone oil, methyl vinyl MQ silicon resin are mixed obtained component A by the weight ratio of 100:8 ~ 100:15 ~ 50; Vinyl-terminated silicone fluid, methyl vinyl MQ silicon resin, catalyzer, tackifier are mixed obtained B component by the weight ratio of 100:15 ~ 50:0.02 ~ 3:2 ~ 24.The present invention adopts methyl vinyl MQ silicon resin and the hydrogeneous cyclosiloxane compound of tackifier, containing epoxide group and siloxane groups, effectively raise the mechanical property of this ambient temperature curable joint sealant, adhesiveproperties and optical property, the step of preparation process simultaneously provided is terse and without the need to the equipment of harshness, be thus applicable to suitability for industrialized production.
Description
Technical field
The present invention relates to Electronic Packaging joint sealant field, specifically a kind of LED high strength bonding self-vulcanizing organic silicon potting adhesive and preparation method thereof.
Background technology
Flourish along with LED illumination industry, and the continuing to bring out of the illumination level LED component of high-power, high brightness, long life requirement, 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, become the LED encapsulation material of a new generation.And existing organic silicon potting adhesive frangibility, mechanical property does not also reach the requirement of LED.In addition, cementability can not meet the requirement of LED substrate bonding, addition-type silicon rubber is general without cementability, if can cementability be improved, silica gel after solidification and will space do not had between base material, the fault that can prevent the long-time water vapor permeable occurred from causing, ensures the use properties of electronic devices and components under harshness and unforeseen circumstances.
Summary of the invention
The object of the invention is the defect in order to overcome the existence of above-mentioned prior art and a kind of LED high strength bonding self-vulcanizing organic silicon potting adhesive and preparation method thereof is provided, after the solidification of this joint sealant, there is excellent optical property, mechanical property and adhesive property, easy to use, output rating and the work-ing life of LED light source can be significantly improved.
The present invention also aims to the preparation method that a kind of LED high strength bonding self-vulcanizing organic silicon potting adhesive is provided.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A preparation method for LED high strength bonding self-vulcanizing organic silicon potting adhesive, comprises the steps:
A, vinyl-terminated silicone fluid, containing hydrogen silicone oil, methyl vinyl MQ silicon resin are mixed obtained component A by the weight ratio of 100:8 ~ 100:15 ~ 50;
B, vinyl-terminated silicone fluid, methyl vinyl MQ silicon resin, catalyzer, tackifier are mixed obtained B component by the weight ratio of 100:15 ~ 50:0.02 ~ 3:2 ~ 24;
C, be that 1 ~ 5:5 ~ 1 mixes by weight by described Part A components and B component, vacuum defoamation, solidifies at ambient temperature, obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive;
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, react 1 ~ 3 hour under the condition of 20 ~ 40 DEG C, then react 1 ~ 3 hour under the condition of 40 ~ 80 DEG C; Mixture underpressure distillation obtains finished product.
For realizing the object of the invention further, preferably, described underpressure distillation is in temperature lower than 60 DEG C, and pressure is 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 represents methyl; 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 represents methyl; R represents methyl or hydrogen base or hydroxyl; P and n represents the polymerization degree; Preferred Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Described methyl vinyl MQ silicon resin refers to that molecule medium vinyl massfraction is the Vinyl MQ silicon resin of 2.5 ~ 4%, and viscosity is 4000 ~ 10000mPas, and preferred Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Described tackifier are the hydrogeneous cyclosiloxane compound containing epoxide group and siloxane groups.
A kind of LED high strength bonding self-vulcanizing organic silicon potting adhesive, is obtained by above-mentioned preparation method.
The present invention compared with prior art possesses following advantage:
1) the present invention is by methyl vinyl MQ silicon resin, and hydrogeneous both the cyclosiloxane compound containing epoxide group and siloxane groups add simultaneously, can improve organic silicon potting adhesive cross-linking set;
2) joint sealant mechanical property of the present invention significantly improves, and also enhances the adhesiveproperties with materials such as metal, PPA plates, and refractive index close, do not affect its high transmission rate.
3) step of preparation process of the present invention is terse, and without the need to the equipment of harshness, is applicable to suitability for industrialized production, has saved energy consumption, 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 the vinyltrimethoxy silane weight ratio by 100:30:40 is mixed, react 3 hours at 20 DEG C, react 1 hour at 80 DEG C again, then distillation removing small molecules under being the condition of-0.1MPa at temperature, the pressure of 60 DEG C, the tackifier of obtained faint yellow oily thickness.
Preparation LED high strength bonding self-vulcanizing organic silicon potting adhesive:
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.16% by vinyl massfraction be 0.3% containing hydrogen silicone oil, vinyl massfraction be 4% methyl vinyl MQ silicon resin mix by the weight ratio of 100:25:15, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.16% by vinyl massfraction be 4% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:15:0.05:7, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 3000ppm, and silicone Science and Technology Ltd. of Shenzhen produces.CMX-30 type
In the present embodiment, vinyl-terminated silicone fluid viscosity is 5000mPas, 206-5000 type, and 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, 202-03 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicon resin viscosity is 4000mPas, ASIBO-MVDQ4000 type, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
During use, component A and B component carried out mixing and stirring by weight for 1:1, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED 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, react 2 hours at 30 DEG C, then react 2 hours at 60 DEG C.Then distillation removing small molecules under being the condition of-0.5MPa at temperature, the pressure of 30 DEG C, the tackifier of obtained faint yellow oily thickness.
Preparation LED high strength bonding self-vulcanizing organic silicon potting adhesive:
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.23% by vinyl massfraction be 1.6% containing hydrogen silicone oil, vinyl massfraction be 3% methyl vinyl MQ silicon resin mix by the weight ratio of 100:10:20, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.23% by vinyl massfraction be 3% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:20:0.02:2, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 7000ppm, CMX-70 type, and silicone Science and Technology Ltd. of Shenzhen produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 3000mPas, 206-3000 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is hydroxy-end capped polymethyl hydrogen siloxane viscosity is 40mPas, 202-16 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicon resin viscosity is 6000mPas, ASIBO-MVDQ6000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Component A and B component carried out mixing and stirring by weight for 1:3, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 3
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively the weight ratio of above-mentioned raw materials by 100:30:80 is mixed, react 1 hour at 40 DEG C, then react 3 hours at 70 DEG C.Then distillation removing small molecules under being the condition of-0.3MPa at temperature, the pressure of 10 DEG C, the tackifier of obtained faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.3% by vinyl massfraction be 0.5% containing hydrogen silicone oil, vinyl massfraction be 2.7% methyl vinyl MQ silicon resin mix by the weight ratio of 100:55:25, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.3% by vinyl massfraction be 2.7% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:25:0.02:3, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 6000ppm, CMX-60 type, and silicone Science and Technology Ltd. of Shenzhen produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 1000mPas, 206-1000 type, and 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, 202-05 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicon resin viscosity is 8000mPas, ASIBO-MVDQ8000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Component A and B component carried out mixing and stirring by weight for 1:5, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 4
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively the weight ratio of above-mentioned raw materials by 100:70:40 is mixed, react 3 hours at 30 DEG C, then react 1 hour at 50 DEG C.Then distillation removing small molecules under being the condition of-0.5MPa at temperature, the pressure of 20 DEG C, the tackifier of obtained faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.48% by vinyl massfraction be 0.8% containing hydrogen silicone oil, vinyl massfraction be 2.5% methyl vinyl MQ silicon resin mix by the weight ratio of 100:10:30, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.48% by vinyl massfraction be 2.5% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:30:0.1:20, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 4000ppm, CMX-40 type, and silicone Science and Technology Ltd. of Shenzhen produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 500mPas, 206-500 type, and 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, 202-08 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicon resin viscosity is 10000mPas, ASIBO-MVDQ10000 type, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Component A and B component carried out mixing and stirring by weight for 3:1, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 5
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively the weight ratio of above-mentioned raw materials by 100:50:60 is mixed, react 2 hours at 40 DEG C, then react 2 hours at 80 DEG C.Then distillation removing small molecules under being the condition of-0.4MPa at temperature, the pressure of 50 DEG C, the tackifier of obtained faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.16% by vinyl massfraction be 0.8% containing hydrogen silicone oil, vinyl massfraction be 2.5% methyl vinyl MQ silicon resin mix by the weight ratio of 100:8:35, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.16% by vinyl massfraction be 2.5% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:35:3:24, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 2000ppm, CMX-20 type, and silicone Science and Technology Ltd. of Shenzhen produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 5000mPas, 206-5000 type, and 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, 202-08 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicon resin viscosity is 10000mPas, ASIBO-MVDQ10000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Component A and B component carried out mixing and stirring by weight for 5:1, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 6
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively the weight ratio of above-mentioned raw materials by 100:50:40 is mixed, react 1 hour at 20 DEG C, then react 3 hours at 70 DEG C.Then distillation removing small molecules under being the condition of-0.1MPa at temperature, the pressure of 60 DEG C, the tackifier of obtained faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.23% by vinyl massfraction be 0.3% containing hydrogen silicone oil, vinyl massfraction be 2.7% methyl vinyl MQ silicon resin mix by the weight ratio of 100:100:40, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.23% by vinyl massfraction be 2.7% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:40:0.15:4, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 3000ppm, CMX-30 type, and silicone Science and Technology Ltd. of Shenzhen produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 3000mPas, 206-3000 type, and 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, 202-03 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicon resin viscosity is 8000mPas, ASIBO-MVDQ8000 type, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Component A and B component carried out mixing and stirring by weight for 1:4, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 7
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively the weight ratio of above-mentioned raw materials by 100:50:80 is mixed, react 2 hours at 20 DEG C, then react 2 hours at 40 DEG C.Then distillation removing small molecules under temperature, the pressure lower than 60 DEG C is the condition of-0.2MPa, the tackifier of obtained faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.3% by vinyl massfraction be 0.5% containing hydrogen silicone oil, vinyl massfraction be 3% methyl vinyl MQ silicon resin mix by the weight ratio of 100:45:45, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.3% by vinyl massfraction be 3% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:45:0.1:3, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 5000ppm, CMX-50 type, and silicone Science and Technology Ltd. of Shenzhen produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 1000mPas, 206-1000 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Containing hydrogen silicone oil is hydroxy-end capped polymethyl hydrogen siloxane, and viscosity is 70mPas, 202-05 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces.
Methyl vinyl MQ silicon resin viscosity is 6000mPas, ASIBO-MVDQ6000, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces.
Component A and B component carried out mixing and stirring by weight for 1:2, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive.
Embodiment 8
By tetramethyl-ring tetrasiloxane, by glycidyl allyl ether, vinyltrimethoxy silane, then successively the weight ratio of above-mentioned raw materials by 100:30:60 is mixed, react 1 hour at 40 DEG C, then react 3 hours at 60 DEG C.Then distillation removing small molecules under temperature, the pressure lower than 60 DEG C is the condition of-0.1MPa, the tackifier of obtained faint yellow oily thickness.
This joint sealant comprises A, B component, wherein, vinyl-terminated silicone fluid, active hydrogen massfraction that component A is 0.48% by vinyl massfraction be 1.6% containing hydrogen silicone oil, vinyl massfraction be 4% methyl vinyl MQ silicon resin mix by the weight ratio of 100:15:50, and to pack; Vinyl-terminated silicone fluid, vinyl massfraction that B component is 0.48% by vinyl massfraction be 4% methyl vinyl MQ silicon resin, catalyzer, tackifier mix by the weight ratio of 100:50:0.02:3, and pack.
The present embodiment catalyzer is platinum-vinyl siloxane title complex, and platinum content is 7000ppm, CMX-70 type, and silicone Science and Technology Ltd. of Shenzhen produces.
In the present embodiment, vinyl-terminated silicone fluid viscosity is 500mPas(206-500 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces).
Containing hydrogen silicone oil is the polymethyl hydrogen siloxane of trimethylammonium end-blocking, and viscosity is 40mPas(202-16 type, and Zhejiang Xinan Chemical Industry Group Co.Ltd produces).
Methyl vinyl MQ silicon resin viscosity is 4000mPas(ASIBO-MVDQ4000 type, and Shanghai Aishibo Organosilicon Material Co., Ltd. produces).
Component A and B component carried out mixing and stirring by weight for 2:1, inject among mould, allow its natural levelling, vacuum defoamation, solidifies at ambient temperature and obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive.
LED high strength bonding self-vulcanizing organic silicon potting adhesive after solidifying embodiment 1 ~ embodiment 8 does performance test, and embodiment 1 ~ embodiment 8 obtains the concrete test result of LED high strength bonding self-vulcanizing organic silicon potting adhesive in table 1.Table 1 obtains shown in LED high strength bonding self-vulcanizing organic silicon potting adhesive the performance test results table 1 for embodiment 1 ~ embodiment 8.
Hardness test: by GB/T 531.1 ?2008 standard dehydrated alcohol wiping specimen surface, measures the hardness of sample with Shanghai six water chestnut instrument plant LX ?A type durometer.
Tensile property is tested: by GB/T 528 ?2009 standards be cut into standard test specimen, measure the tensile property of sample with German Zwick/Roell company Z010 type universal testing machine, rate of extension is 500mm/min.
Adhesiveproperties is tested: by GB/T 7124 ?2008 standards, measure the bonding tensile shear strength of sample to aluminium flake and PPA with German Zwick/Roell company Z010 type universal testing machine, evaluate the adhesiveproperties of joint sealant with this.
Electrical performance testing: by GB/T 1692 ?2008 standards, measure the volume specific resistance of sample with U.S. Keithley company 6517B type megger.By GB/T 1693 ?2007 standards, measure specific inductivity and the dielectric loss angle tangent of sample.
Transmittance is tested: at 25 DEG C, with Japanese Hitachi company UV ?3010 type Zi Wai ?visible spectrophotometer measure the transmittance of sample in 200 ~ 800nm visible wavelength range.
As seen from Table 1, compare with patent CN 102850804 A, joint sealant prepared by the present invention possesses more superior tensile property, transmittance and bonding strength, and has excellent electrical insulation capability.In raw material of the present invention methyl vinyl MQ silicon resin be between organic and inorganic between material, containing the vinyl groups that can participate in solidifying, silicon rubber effective " Concentrative crosslinking " can be made, thus improve the tensile property of joint sealant significantly.And contain the hydrogeneous cyclosiloxane compound of epoxide group and siloxane groups, because the silicon hydrogen base contained 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 silicon 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 (4)
1. a LED preparation method for high strength bonding self-vulcanizing organic silicon potting adhesive, is characterized in that comprising the steps:
A, vinyl-terminated silicone fluid, containing hydrogen silicone oil, methyl vinyl MQ silicon resin are mixed obtained component A by the weight ratio of 100:8 ~ 100:15 ~ 50; Described vinyl-terminated silicone fluid is the polydimethylsiloxane of bi-vinyl end-blocking, and the mass content of molecule medium vinyl is 0.16 ~ 0.48%, and viscosity is 500 ~ 5000mPas; 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, and viscosity is 30 ~ 85mPas;
B, vinyl-terminated silicone fluid, methyl vinyl MQ silicon resin, catalyzer, tackifier are mixed obtained B component by the weight ratio of 100:15 ~ 50:0.02 ~ 3:2 ~ 24;
C, be that 1 ~ 5:5 ~ 1 mixes by weight by described Part A components and B component, vacuum defoamation, solidifies at ambient temperature, obtains LED high strength bonding self-vulcanizing organic silicon potting adhesive;
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, react 1 ~ 3 hour under the condition of 20 ~ 40 DEG C, then react 1 ~ 3 hour under the condition of 40 ~ 80 DEG C; Mixture underpressure distillation obtains finished product.
2. the preparation method of LED high strength bonding self-vulcanizing organic silicon potting adhesive according to claim 1, is characterized in that: described underpressure distillation is in temperature lower than 60 DEG C, and pressure is distill under the condition of-0.1 ~-0.5MPa.
3. the preparation method of LED high strength bonding self-vulcanizing organic silicon potting adhesive according to claim 1, it is characterized in that: described methyl vinyl MQ silicon resin is the Vinyl MQ silicon resin of the mass content 0.1 ~ 6.5% of molecule medium vinyl, and viscosity is 4000 ~ 10000mPas.
4. a LED high strength bonding self-vulcanizing organic silicon potting adhesive, is characterized in that it is obtained by preparation method described in any one of claim 1-3.
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| CN112778968A (en) * | 2021-01-04 | 2021-05-11 | 株洲时代新材料科技股份有限公司 | Organic silicon pouring sealant and preparation method thereof |
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