CN103627178A - Liquid silicone rubber composition for LED (Light Emitting Diode) packaging and preparation method of composition - Google Patents
Liquid silicone rubber composition for LED (Light Emitting Diode) packaging and preparation method of composition Download PDFInfo
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Abstract
The invention relates to a liquid silicone rubber composition for LED (Light Emitting Diode) packaging and a preparation method of the composition. The liquid silicone rubber composition for LED packaging comprises the following components in parts by weight: 60-120 parts of organopolysiloxane containing aliphatic unsaturated bonds, 2-45 parts of organic hydrogen polysiloxane, 5-30 parts of special functional polysiloxane, 0.01-0.5 part of a platinum complex catalyst, 0.01-0.05 part of an inhibitor and 0.5-3 parts of a tackifier. The invention further relates to the preparation method of the liquid silicone rubber composition for LED packaging. According to the liquid silicone rubber composition, special functional polysiloxane is added to take the high-strength reinforcing effect, so that the mechanical properties of the product such as tensile strength, tear strength and elongation at break are greatly improved. The product is good in cohesiveness, and the light transmittance is greater than or equal to 99%.
Description
Technical field
The present invention relates to a kind of LED encapsulation liquid silicon rubber composition and preparation method thereof, belong to liquid silastic preparing technical field.
Background technology
The advantages such as photodiode (Light Emitting Diode is called for short LED), has efficiency high, and photochromic pure, energy consumption is little, and the life-span is long, and response is fast, pollution-free, all solid state, are a kind of novel illumination light sources, be known as green " solid-state illumination ".Development and maturation along with LED technology, the light efficiency of white light LEDs has has met or exceeded the light efficiency level of ordinary incandescent lamp, optical throughput is also significantly increasing, this make LED be expected to become after incandescent light, luminescent lamp, high-intensity gas discharge lamp the 4th generation lighting source.
Common LED encapsulation mainly comprises epoxy resin, polycarbonate, polymethylmethacrylate, thermosetting epoxy resin and optics nylon etc. with material, along with the increasing of LED power and the raising of brightness, these materials because of thermotolerance bad, easily produce xanthochromia, cause light decay, the performance requriements of power type LED chip cannot be met, therefore, new equivalent material need to be sought.Organosilicon material has the advantages such as cold-hot impact, resistance to xanthochromia, water white transparency, low-stress, is the best materials of LED encapsulation use.
Ordinary silicon rubber is during without reinforcement, and intensity is lower, substantially there is no use properties.Adopt gas-phase silica to carry out reinforcement, because the specific refractory power of gas-phase silica and organosilicon material differs larger, can reduce the transmittance of LED packaged material, and the increase with gas-phase silica consumption, compound viscosity sharply increases, and causes operational difficulty, affects gluing process.While only using the reinforcement of MQ silicone resin, although can make the tensile strength of silicon rubber make moderate progress,, there is certain limitation in the raising for tear strength and tensile yield, the LED encapsulation that can not meet the demands higher.
Chinese patent literature CN102344684A(application number 201110233591.3) introduce the vinyl silicone oil that vulcabond modification, end are hydroxyl and prepared LED module packaging organo-silicone rubber, improved the tear resistance of silicon rubber, but not obvious for the raising of tensile strength and tensile yield.
Chinese patent literature CN103146202A(application number 201310087259.X) introduced end-vinyl ultra-branching polysiloxane, be applied in LED package with in liquid silastic, for mechanical property, improve, but still can not meet the LED encapsulation of requirements at the higher level.
Chinese patent literature CN102181159A(application number 201110061714.X) POSS is applied in LED packaged material, due to preparation, POSS not only needs to use solvent, and complex process, and cost is higher.
In addition, add the LED rubber composition of tackifier, there is cohesiveness in various degree with a lot of materials, therefore, while using metal die or glass mold sulfuration preparation test specimens, tend to allow LED silica gel be difficult to the demoulding, can not get complete silicon rubber testing plate, need to add releasing agent or plastic film mulch on mould.Add releasing agent can make easily sticky dust of silastic surface, affect transmittance, plastic film mulch is easily shifted, and causes LED silica gel piece surface to occur ditch ditch bank, unfairness, the accuracy of the data that affect the mechanical properties.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of LED encapsulation liquid silicon rubber composition and preparation method thereof is provided.
Summary of the invention
A kind of LED provided by the invention liquid silicon rubber composition and preparation method thereof for encapsulation, in liquid silicon rubber composition, to have added easy acquisition, lower-cost features based polysiloxane high strength reinforcement component, obtain the liquid silastic product that the mechanical mechanics properties such as tensile strength, tear strength, tensile yield are greatly improved, adopt tetrafluoroethylene mould to prepare test specimens simultaneously.
Detailed Description Of The Invention
A LED encapsulation liquid silicon rubber composition, component is as follows, is weight part:
60～120 parts of the organopolysiloxanes that contains aliphatics unsaturated link(age) (A), 2～45 parts of organic hydrogen polysiloxanes (B) parts, 5～30 parts of features based polysiloxanes (C), 0.01～0.5 part of platinum complex catalyst (D), 0.01～0.05 part, inhibitor (E), 0.5～3 part of tackifier (F);
The organopolysiloxane (A-2) of the resin structure that contains 2 above alkenyls in the straight chain organopolysiloxane (A-1) that the described organopolysiloxane that contains aliphatics unsaturated link(age) (A) is alkenyls more than containing 2 in molecule and/or molecule;
The organic hydrogen polysiloxanes (B-2) of the resin structure that contains 2 above H atoms in the straight chain organic hydrogen polysiloxanes (B-1) that described organic hydrogen polysiloxanes (B) is H atoms more than containing 2 in molecule and/or molecule;
Described features based polysiloxane (C), for containing polysiloxane (C-1) and/or the hydroxyl vinyl polysiloxane (C-2) of many vinylcyclosiloxanes base in molecule;
The general formula of polysiloxane that contains many vinylcyclosiloxanes base in molecule is as follows:
In formula: R
1for the cyclosiloxane base that contains many vinyl, k1=2,3 or 4, k2=2,3 or 4, k3=2,3 or 4, R wherein
1be positioned at the end of molecular chain and/or the sidepiece of molecular chain; R
2, R
2' be methyl, ethyl, propyl group and/or phenyl; Link number a=10～1000, b=0～1000, c=5～1000, viscosity is 1000-20000mPa.s;
The general formula of hydroxyl vinyl polysiloxane is as follows:
Me represent methylidene wherein; Link number s=0～1000, t=1～100, q=1～1000; Viscosity is 10～10000mPa.s;
Described platinum complex catalyst (D) is platinum water or Ka Shi platinum catalyst;
Described inhibitor (E) is alkynol class inhibitor, and tackifier (F) are methyl silicone rubber tackifier or phenyl siloxane rubber tackifier.
Preferred according to the present invention, LED encapsulation liquid silicon rubber composition, component is as follows, is weight part:
80～100 parts of the organopolysiloxanes that contains aliphatics unsaturated link(age) (A), 7～30 parts of organic hydrogen polysiloxanes (B), 5～15 parts of features based polysiloxanes (C), 0.015～0.03 part of platinum complex catalyst (D), 0.015～0.02 part, inhibitor (E), 1～2 part of tackifier (F).
Preferred according to the present invention, the straight chain organopolysiloxane (A-1) that contains 2 above alkenyls in described molecule is selected from vinyl silicone oil and/or phenyl-vinyl silicon oil, and viscosity is 3000～15000mPa.s; The organopolysiloxane (A-2) that contains the resin structure of 2 above alkenyls in described molecule is selected from vinyl polysiloxane and/or phenyl vinyl polysiloxane, and viscosity is 5000～20000mPas;
Preferred according to the present invention, the straight chain organic hydrogen polysiloxanes (B-1) that contains 2 above H atoms in described molecule is selected from containing hydrogen silicone oil and/or phenyl hydrogen-containing silicon oil, and viscosity is 20～100mPas; The viscosity that the organic hydrogen polysiloxanes (B-2) that contains the resin structure of 2 above H atoms in described molecule is selected from Silicon Containing Hydrogen resin and/or phenyl Silicon Containing Hydrogen resin is 20～1500mPas.
Preferred according to the present invention, described R
1for in many vinyl three cyclosiloxane bases, many vinyl Fourth Ring siloxanes, many vinyl five rings siloxanes one or more with arbitrarily than combination; Further preferred, R
1for many vinyl three cyclosiloxane bases, many vinyl Fourth Ring siloxanes one or more with arbitrarily than combination;
Preferred according to the present invention, described R
1a=10～100 are counted in the link of the polysiloxane that contains many vinylcyclosiloxanes base, b=50～500, c=10～500;
Preferred according to the present invention, the platinum content of described platinum complex catalyst (D) is 3000～10000ppm.
Preferred according to the present invention, the value that t and s are counted in the link of described hydroxyl vinyl polysiloxane is s=0～200, t=20～50, q=30～200;
Preferred according to the present invention, described LED encapsulation is with in liquid silicon rubber composition, and the mol ratio of Si-Vi:Si-H is 1:(1～1.8), wherein Si-Vi represents that silico ethylene base, Si-H represent silicon hydrogen base, further preferred, the mol ratio of Si-Vi:Si-H is 1:(1.1～1.5).
Preferred according to the present invention, described inhibitor is propiolic alcohol, 1-ethynyl-1-hexalin, 2-phenyl-3-butyne-2-alcohol, methylbutynol.
Preferred according to the present invention, the polysiloxane (C-1) of described many vinylcyclosiloxanes base can adopt this area ordinary method synthetic, also can be prepared as follows:
(1) respectively dimethyl cyclosiloxane and methyl phenyl ring siloxane are removed after moisture, 90:(0～1 in mass ratio) or 1:(18.5～37) mix, in 0.08～0.1 ratio of dimethyl cyclosiloxane and methyl phenyl ring siloxane total mass, add again the vitriol oil of the mass concentration 98% of dry hydrogeneous ring body, hydrogeneous double-seal head and gross weight 0.5～1.5%, polyreaction 3～5h at 30～50 ℃, add in sodium bicarbonate extremely neutral with pH, filter, de-low, obtain hydrogen containing siloxane;
(2) in the hydrogen containing siloxane making to step (1), add 5 times of tetrem thiazolinyl tetramethyl-ring siloxanes more than quality, add again platinum catalyst, the concentration that makes platinum catalyst is 15～25ppm, under the condition of 80～100 ℃, react 4～6h, be warming up to 140～150 ℃ of low molecules of vacuum removal, obtain the polysiloxane (C-1) of many vinylcyclosiloxanes base;
Further preferred, described hydrogeneous ring body is selected from methylhydracyclosiloxane; Described hydrogeneous double-seal head is selected from tetramethyl-dihydro base sily oxide.
Preferred according to the present invention, described hydroxyl vinyl polysiloxane (C-2) can adopt this area ordinary method synthetic, also can be prepared as follows:
By dimethyl cyclosiloxane, methyl phenyl ring siloxane and methyl ethylene cyclosiloxane remove moisture at 35～40 ℃ respectively, then press dimethyl cyclosiloxane, methyl phenyl ring siloxane is 10:(0～0.005 with the mass ratio of methyl ethylene cyclosiloxane): (1～1.2) or 1:(18.4～37.5): mix (0.1～0.12), add alkali glue, polyase 13～5h under the condition of 90～100 ℃, add again 0.18～0.20g water, be warming up to 140～160 ℃, decomposition catalyst 3～5h, again through the de-low molecule of vacuum, obtain hydroxyl vinyl polysiloxane (C-2),
Further preferred, described alkali glue is selected from the silicon alkoxide of Tetramethylammonium hydroxide.
A preparation method for liquid silicon rubber composition for above-mentioned LED encapsulation, comprises the steps:
After the organopolysiloxane that contains aliphatics unsaturated link(age) (A), organic hydrogen polysiloxanes (B) and features based polysiloxane (C) are mixed in proportion, add again platinum complex catalyst, inhibitor, tackifier, mix, make LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned LED encapsulation, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 5～30min, is placed in tetrafluoroethylene mould; Through at 50～80 ℃ of sulfuration 0.5～1.5h, then at 100～200 ℃ of sulfuration 0.5～4h, or, through at 100～200 ℃ of sulfuration 2h, obtain test specimens.
Beneficial effect
1, the present invention has added features based polysiloxane in liquid silicon rubber composition, it has played the effect of high strength reinforcement, greatly improved the mechanical mechanics property such as tensile strength, tear strength, tensile yield of product, and product there is good cohesiveness, transmittance >=99%;
2, the features based polysiloxane that the present invention adds in liquid silicon rubber composition, easily obtains, and cost is lower;
3, preparation method of the present invention adopts tetrafluoroethylene mould to prepare test specimens, and the demoulding is easy, and preparation process is simple, and product surface is clean;
4, the liquid silicon rubber composition that the present invention makes, is very suitable for embedding, the paster type encapsulation of LED, can also be applied to the fields such as optical lens, solar cell substrate, touch-screen.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is further elaborated, but institute of the present invention protection domain is not limited to this.
Raw material explanation
The polysiloxane (C-1) of many vinylcyclosiloxanes base of described embodiment 1～4 and comparative example 3 is adopted preparation with the following method:
Dimethyl cyclosiloxane is removed after moisture, in the clean there-necked flask of 500mL, add dimethyl cyclosiloxane 370g, the vitriol oil that adds again hydrogeneous ring body (methylhydracyclosiloxane), the hydrogeneous double-seal head of 1.34g (tetramethyl-dihydro base sily oxide) and 4g mass concentration 98% that 30g is dry, polymerization 4h at 40 ℃, add in 12g sodium bicarbonate extremely neutral with pH, filter, de-low, obtain 360g hydrogen containing siloxane; 360g hydrogen containing siloxane, 1720g tetrem thiazolinyl tetramethyl-ring siloxanes and 0.04g platinum catalyst are added in 3000mL, at 90 ℃ of reaction 6h, be warming up to 150 ℃ of low molecules of vacuum removal, obtain the polymethyl siloxane (C-1) of 640g vinylcyclosiloxanes base; Viscosity is 5200mPa.s;
The polysiloxane (C-1) of many vinylcyclosiloxanes base of described embodiment 5～6 is adopted preparation with the following method:
Respectively dimethyl cyclosiloxane, methyl phenyl ring siloxane are removed after moisture, in the clean there-necked flask of 500mL, add dimethyl cyclosiloxane 5g, methyl phenyl ring siloxane 136g, the vitriol oil that adds again hydrogeneous ring body (methylhydracyclosiloxane), the hydrogeneous double-seal head of 1.8g (tetramethyl-dihydro base sily oxide) and 1.5g mass concentration 98% that 22g is dry, polymerization 5h at 30 ℃, add in 4.5g sodium bicarbonate extremely neutral with pH, filter, de-low, obtain 140g phenyl hydrogen containing siloxane; 140g phenyl hydrogen containing siloxane, 680g tetrem thiazolinyl tetramethyl-ring siloxanes and 0.016g platinum catalyst are added in the there-necked flask of 1000mL, at 80 ℃ of reaction 6h, be warming up to 150 ℃ of low molecules of vacuum removal, obtain the phenyl silicone (C-1) of many vinylcyclosiloxanes of 250g base; Viscosity is 9100mPa.s;
The hydroxyl vinyl polysiloxane (C-2) of described embodiment 1～4 and comparative example 3 is adopted preparation with the following method:
Dimethyl cyclosiloxane, methyl ethylene cyclosiloxane are removed to moisture at 40 ℃ respectively, then in the clean there-necked flask of 500mL, add dimethyl cyclosiloxane 150g and the methyl ethylene cyclosiloxane 6.50g that removes moisture, add alkali glue (silicon alkoxide of Tetramethylammonium hydroxide), polymerization 4h at 100 ℃, the water that adds again 0.20g, be warming up to 150 ℃ of decomposition catalyst 4h, then through the de-low molecule of vacuum, obtain 110g hydroxyl vinyl polymethyl siloxane (C-2); Viscosity is 2300mPa.s.
The hydroxyl vinyl polysiloxane (C-2) of described embodiment 5～6 is adopted preparation with the following method:
Dimethyl cyclosiloxane, methyl phenyl ring siloxane, methyl ethylene cyclosiloxane are removed to moisture at 35 ℃ respectively, then in the clean there-necked flask of 500mL, add dimethyl cyclosiloxane 20g, methyl phenyl ring siloxane 350g and the methyl ethylene cyclosiloxane 5.95g that removes moisture, add alkali glue (silicon alkoxide of Tetramethylammonium hydroxide), polyase 13 h at 100 ℃, the water that adds again 0.20g, be warming up to 140 ℃ of decomposition catalyst 5h, through the de-low molecule of vacuum, obtain 300g hydroxyl vinyl phenyl silicone (C-2) again; Viscosity is 5600mPa.s.
Vinyl silicone oil, phenyl-vinyl silicon oil, common commercially available prod, viscosity is 3000～15000mPa.s.
Vinyl polysiloxane, phenyl vinyl polysiloxane, common commercially available prod, viscosity is 5000～20000mPa.s.
Containing hydrogen silicone oil, phenyl hydrogen-containing silicon oil, common commercially available prod, viscosity is 20～100mPas.
Silicon Containing Hydrogen resin, phenyl Silicon Containing Hydrogen resin, common commercially available prod, viscosity is 20～1500mPa.s.
Propiolic alcohol, 1-alkynyl-1-hexalin, 2-phenyl-3-butyne-2-alcohol, methylbutynol, be analytical reagent, common commercially available prod.
Methyl silicone rubber tackifier, phenyl siloxane rubber tackifier, common commercially available prod.
Platinum water, Ka Shi platinum catalyst, common commercially available prod.
Embodiment 1
A preparation method for liquid silicon rubber composition for LED encapsulation, comprises the steps:
In 50.0g vinyl silicone oil, add 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.50g3000ppm, the polymethyl siloxane that 5.92g gained contains many vinylcyclosiloxanes base (C-1), 3.55g gained hydroxyl vinyl polymethyl siloxane (C-2), 0.017g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 0.65g, mix, and then add 4.50g containing hydrogen silicone oil, integral body mixes rear discharging, makes LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned LED encapsulation, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 2h, obtain the product test sample of smooth cleaning.
Embodiment 2
A preparation method for liquid silicon rubber composition for LED encapsulation, comprises the steps:
In 50.0g vinyl silicone oil, add 30.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.36g3000ppm, the polymethyl siloxane that 4.2g contains many vinylcyclosiloxanes base (C-1), 2.5g hydroxyl vinyl polymethyl siloxane (C-2), 0.012g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 0.90g, mix, and finally add 3.50g Silicon Containing Hydrogen resin, integral body mixes rear discharging, makes LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned LED encapsulation, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Embodiment 3
A preparation method for liquid silicon rubber composition for LED encapsulation, comprises the steps:
In 50.0g vinyl silicone oil, add 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.27g5000ppm, the polymethyl siloxane that 9.80g contains many vinylcyclosiloxanes base (C-1), 5.50g hydroxyl vinyl polymethyl siloxane (C-2), 0.018g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 2.76g, mix, and finally add 7.50g containing hydrogen silicone oil, integral body mixes rear discharging, makes LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned LED encapsulation, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 4h, obtain the product test sample of smooth cleaning.
Embodiment 4
A preparation method for liquid silicon rubber composition for LED encapsulation, comprises the steps:
In 10.0g vinyl silicone oil, add 80g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.22g5000ppm, the polymethyl siloxane that 10.00g contains many vinylcyclosiloxanes base (C-1), 5.00g hydroxyl vinyl polymethyl siloxane (C-2), 0.015g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 2.30g, mix, and finally add 9.75g containing hydrogen silicone oil, integral body mixes rear discharging, makes LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned LED encapsulation, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Embodiment 5
A preparation method for liquid silicon rubber composition for LED encapsulation, comprises the steps:
In 50.0g phenyl-vinyl silicon oil, add 50.0g phenyl vinyl polysiloxane, the Ka Shi platinum catalyst of 0.03g10000ppm, the phenyl silicone that 14.00g contains many vinylcyclosiloxanes base (C-1), 5.00g hydroxyl vinyl phenyl silicone (C-2), 0.015g1-ethynyl-1-hexalin, the phenyl siloxane rubber tackifier of 0.81g, mix, and finally add 43.30g phenyl hydrogen-containing silicon oil, integral body mixes rear discharging, makes LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned LED encapsulation, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Embodiment 6
A preparation method for liquid silicon rubber composition for LED encapsulation, comprises the steps:
In 50.0g phenyl vinyl polysiloxane, the Ka Shi platinum catalyst that adds 0.015g10000ppm, the phenyl silicone that 4.50g contains many vinylcyclosiloxanes base (C-1), 1.60g hydroxyl vinyl phenyl silicone (C-2), 0.0075g1-ethynyl-1-hexalin, the phenyl siloxane rubber tackifier of 1.72g, mix, finally add 30.00g phenyl Silicon Containing Hydrogen resin, integral body mixes rear discharging again, makes LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned LED encapsulation, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Comparative example 1
In 50.0g vinyl silicone oil, add 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.50g3000ppm, 0.017g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 0.65g, mix, and then add 3.75g containing hydrogen silicone oil, integral body mixes rear discharging, makes contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned contrast LED encapsulation, step is as follows:
By the contrast LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 2h, obtain the product test sample of smooth cleaning.
Comparative example 2
In 50.0g vinyl silicone oil, add 30.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.36g3000ppm, 0.012g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 0.90g, mix, finally add again 2.65g Silicon Containing Hydrogen resin integral body to mix rear discharging, make contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned contrast LED encapsulation, step is as follows:
By the contrast LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 10min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Comparative example 3
In 50.0g vinyl silicone oil, add 65.0g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.27g5000ppm, the polymethyl siloxane that 9.80g contains many vinylcyclosiloxanes base (C-1), 5.50g hydroxyl vinyl polymethyl siloxane (C-2), 0.018g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 2.76g, mix, and finally add 7.50g containing hydrogen silicone oil again, integral body mixes rear discharging, makes contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned contrast LED encapsulation, step is as follows:
By the contrast LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, is placed in metal die, levelling; At 80 ℃, vulcanize 1h, then, at 150 ℃ of sulfuration 4h, obtain product test sample.
Comparative example 4
To 10.0g vinyl silicone oil, add 80g vinyl polysiloxane, the Ka Shi platinum catalyst of 0.22g5000ppm, 0.015g1-ethynyl-1-hexalin, the methyl silicone rubber tackifier of 2.30g, mix, and finally add 8.65g containing hydrogen silicone oil again, integral body mixes rear discharging, makes contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned contrast LED encapsulation, step is as follows:
By the contrast LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 20min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Comparative example 5
In 50.0g phenyl-vinyl silicon oil, add 50.0g phenyl vinyl polysiloxane, the Ka Shi platinum catalyst of 0.03g10000ppm, 0.015g1-ethynyl-1-hexalin, the phenyl siloxane rubber tackifier of 0.81g, mix, and finally add 34.40g phenyl hydrogen-containing silicon oil again, integral body mixes rear discharging, makes contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned contrast LED encapsulation, step is as follows:
By the contrast LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Comparative example 6
In 50.0g phenyl vinyl polysiloxane, the Ka Shi platinum catalyst that adds 0.015g10000ppm, 0.0075g1-ethynyl-1-hexalin, the phenyl siloxane rubber tackifier of 1.72g, mix, finally add 30.00g phenyl Silicon Containing Hydrogen resin, integral body mixes rear discharging again, makes contrast LED encapsulation liquid silicon rubber composition.
The preparation method of the test specimens of liquid silicon rubber composition for above-mentioned contrast LED encapsulation, step is as follows:
By the contrast LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 30min, is placed in tetrafluoroethylene mould, levelling; At 80 ℃, vulcanize 1h, then at 150 ℃ of sulfuration 3h, obtain the product test sample of smooth cleaning.
Test example
Tensile strength and the tensile yield of the product test sample that above embodiment and comparative example make are tested according to GB/T528-1998, tear strength is tested according to GB/T529-1999, hardness is according to GB/T531-1999, specific refractory power adopts Abbe refractometer to test at 25 ℃, and transmittance adopts the thick testing plate of ultraviolet-visible spectrophotometer test 1mm.
After testing, result is as shown in table 1.
Table 1
From table 1 embodiment 1～2 and 4～6 and the detected result contrast of comparative example 1～2 and 4～6, embodiment 1～2 and 4～6 is owing to having added features based polysiloxane, make for LED encapsulation the mechanical mechanics properties such as the tensile strength of liquid silastic, tear strength, tensile yield have significantly raising than the silicon rubber of common reinforcement (comparative example 1～2 and 4～6), wherein, tensile strength has improved more than 35%, tear strength has improved more than 40%, tensile yield has improved more than 30%, and hardness is also slightly improved.
In addition, by embodiment 3 and comparative example 3, can be found out, the liquid silicon rubber composition of same component, same vulcanization process condition, adopts tetrafluoroethylene mould better than the mechanical mechanics property of the silicon rubber test specimens that adopts metal die to prepare, and transmittance is also high, this is mainly because the test specimens that adopts tetrafluoroethylene mould to prepare, the demoulding is easy, surface cleaning, flawless defect.
Claims (10)
1. a LED encapsulation liquid silicon rubber composition, is characterized in that, component is as follows, is weight part:
60～120 parts of the organopolysiloxanes that contains aliphatics unsaturated link(age) (A), 2～45 parts of organic hydrogen polysiloxanes (B) parts, 5～30 parts of features based polysiloxanes (C), 0.01～0.5 part of platinum complex catalyst (D), 0.01～0.05 part, inhibitor (E), 0.5～3 part of tackifier (F);
The organopolysiloxane (A-2) of the resin structure that contains 2 above alkenyls in the straight chain organopolysiloxane (A-1) that the described organopolysiloxane that contains aliphatics unsaturated link(age) (A) is alkenyls more than containing 2 in molecule and/or molecule;
The organic hydrogen polysiloxanes (B-2) of the resin structure that contains 2 above H atoms in the straight chain organic hydrogen polysiloxanes (B-1) that described organic hydrogen polysiloxanes (B) is H atoms more than containing 2 in molecule and/or molecule;
Described features based polysiloxane (C), for containing polysiloxane (C-1) and/or the hydroxyl vinyl polysiloxane (C-2) of many vinylcyclosiloxanes base in molecule;
The general formula of polysiloxane that contains many vinylcyclosiloxanes base in molecule is as follows:
In formula: R
1for the cyclosiloxane base that contains many vinyl, k1=2,3 or 4, k2=2,3 or 4, k3=2,3 or 4, R wherein
1be positioned at the end of molecular chain and/or the sidepiece of molecular chain; R
2, R
2' be methyl, ethyl, propyl group and/or phenyl; Link number a=10～1000, b=0～1000, c=5～1000, viscosity is 1000-20000mPa.s;
The general formula of hydroxyl vinyl polysiloxane is as follows:
Me represent methylidene wherein; Link number s=0～1000, t=1～100, q=1～1000; Viscosity is 10～10000mPa.s;
Described platinum complex catalyst (D) is platinum water or Ka Shi platinum catalyst;
Described inhibitor (E) is alkynol class inhibitor, and tackifier (F) are methyl silicone rubber tackifier or phenyl siloxane rubber tackifier.
2. LED encapsulation liquid silicon rubber composition as claimed in claim 1, is characterized in that, component is as follows, is weight part:
80～100 parts of the organopolysiloxanes that contains aliphatics unsaturated link(age) (A), 7～30 parts of organic hydrogen polysiloxanes (B), 5～15 parts of features based polysiloxanes (C), 0.015～0.03 part of platinum complex catalyst (D), 0.015～0.02 part, inhibitor (E), 1～2 part of tackifier (F).
3. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterized in that, the straight chain organopolysiloxane (A-1) that contains 2 above alkenyls in described molecule is selected from vinyl silicone oil and/or phenyl-vinyl silicon oil, and viscosity is 3000～15000mPa.s; The organopolysiloxane (A-2) that contains the resin structure of 2 above alkenyls in described molecule is selected from vinyl polysiloxane and/or phenyl vinyl polysiloxane, and viscosity is 5000～20000mPas.
Preferred according to the present invention, the straight chain organic hydrogen polysiloxanes (B-1) that contains 2 above H atoms in described molecule is selected from containing hydrogen silicone oil and/or phenyl hydrogen-containing silicon oil, and viscosity is 20～100mPas; The viscosity that the organic hydrogen polysiloxanes (B-2) that contains the resin structure of 2 above H atoms in described molecule is selected from Silicon Containing Hydrogen resin and/or phenyl Silicon Containing Hydrogen resin is 20～1500mPas.
Preferred according to the present invention, described R
1for in many vinyl three cyclosiloxane bases, many vinyl Fourth Ring siloxanes, many vinyl five rings siloxanes one or more with arbitrarily than combination; Further preferred, R
1for many vinyl three cyclosiloxane bases, many vinyl Fourth Ring siloxanes one or more with arbitrarily than combination.
4. LED encapsulation liquid silicon rubber composition as claimed in claim 1, is characterized in that described R
1a=10～100 are counted in the link of the polysiloxane that contains many vinylcyclosiloxanes base, b=50～500, c=10～500.
5. LED encapsulation liquid silicon rubber composition as claimed in claim 1, is characterized in that, the platinum content of described platinum complex catalyst (D) is 3000～10000ppm.
6. LED encapsulation liquid silicon rubber composition as claimed in claim 1, is characterized in that, the value that t and s are counted in the link of described hydroxyl vinyl polysiloxane is s=0～200, t=20～50, q=30～200.
7. LED encapsulation liquid silicon rubber composition as claimed in claim 1, it is characterized in that, described LED encapsulation is with in liquid silicon rubber composition, and the mol ratio of Si-Vi:Si-H is 1:(1～1.8), further preferred, the mol ratio of Si-Vi:Si-H is 1:(1.1～1.5);
Preferred according to the present invention, described inhibitor is propiolic alcohol, 1-ethynyl-1-hexalin, 2-phenyl-3-butyne-2-alcohol, methylbutynol.
8. LED encapsulation liquid silicon rubber composition as claimed in claim 1, is characterized in that, the polysiloxane (C-1) of described many vinylcyclosiloxanes base is adopted preparation with the following method:
(1) respectively dimethyl cyclosiloxane and methyl phenyl ring siloxane are removed after moisture, 90:(0～1 in mass ratio) or 1:(18.5～37) mix, in 0.08～0.1 ratio of dimethyl cyclosiloxane and methyl phenyl ring siloxane total mass, add again the vitriol oil of the mass concentration 98% of dry hydrogeneous ring body, hydrogeneous double-seal head and gross weight 0.5～1.5%, polyreaction 3～5h at 30～50 ℃, add in sodium bicarbonate extremely neutral with pH, filter, de-low, obtain hydrogen containing siloxane;
(2) in the hydrogen containing siloxane making to step (1), add 5 times of tetrem thiazolinyl tetramethyl-ring siloxanes more than quality, add again platinum catalyst, the concentration that makes platinum catalyst is 15～25ppm, under the condition of 80～100 ℃, react 4～6h, be warming up to 140～150 ℃ of low molecules of vacuum removal, obtain the polysiloxane (C-1) of many vinylcyclosiloxanes base;
Further preferred, described hydrogeneous ring body is selected from methylhydracyclosiloxane; Described hydrogeneous double-seal head is selected from tetramethyl-dihydro base sily oxide.
Preferred according to the present invention, described hydroxyl vinyl polysiloxane (C-2) is adopted preparation with the following method:
By dimethyl cyclosiloxane, methyl phenyl ring siloxane and methyl ethylene cyclosiloxane remove moisture at 35～40 ℃ respectively, then press dimethyl cyclosiloxane, methyl phenyl ring siloxane is 10:(0～0.005 with the mass ratio of methyl ethylene cyclosiloxane): (1～1.2) or 1:(18.4～37.5): mix (0.1～0.12), add alkali glue, polyase 13～5h under the condition of 90～100 ℃, add again 0.18～0.20g water, be warming up to 140～160 ℃, decomposition catalyst 3～5h, again through the de-low molecule of vacuum, obtain hydroxyl vinyl polysiloxane (C-2),
Further preferred, described alkali glue is selected from the silicon alkoxide of Tetramethylammonium hydroxide.
9. described in claim 1, LED encapsulates the preparation method with liquid silicon rubber composition, it is characterized in that, comprises the steps:
After the organopolysiloxane that contains aliphatics unsaturated link(age) (A), organic hydrogen polysiloxanes (B) and features based polysiloxane (C) are mixed in proportion, add again platinum complex catalyst, inhibitor, tackifier, mix, make LED encapsulation liquid silicon rubber composition.
10. described in claim 1, LED encapsulates the preparation method by the test specimens of liquid silicon rubber composition, it is characterized in that, step is as follows:
By the LED encapsulation making with liquid silicon rubber composition at ambient temperature, vacuum defoamation 5～30min, is placed in tetrafluoroethylene mould; Through at 50～80 ℃ of sulfuration 0.5～1.5h, then at 100～200 ℃ of sulfuration 0.5～4h, or, through at 100～200 ℃ of sulfuration 2h, obtain test specimens.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0848779A (en) * | 1994-08-03 | 1996-02-20 | Shin Etsu Chem Co Ltd | Production of organopolysiloxane |
| CN1155562A (en) * | 1995-10-11 | 1997-07-30 | 陶氏康宁公司 | Curable organopolysiloxane compositions with improved adhesion |
| CN101712800A (en) * | 2009-11-06 | 2010-05-26 | 陈俊光 | Organic silicon resin encapsulant of large power LED and preparing method thereof |
| CN102344684A (en) * | 2011-08-15 | 2012-02-08 | 王昌归 | Organic silicon rubber used for LED module packaging and preparation method thereof |
| CN102532900A (en) * | 2010-12-20 | 2012-07-04 | 常州化学研究所 | Organosilicon lens material for power type light-emitting diode (LED) packaging |
| JP2013067677A (en) * | 2011-09-20 | 2013-04-18 | Sumitomo Bakelite Co Ltd | Silicone rubber curable composition, method of manufacturing silicone rubber, silicone rubber, compact, and medical tube |
| CN103351624A (en) * | 2013-05-10 | 2013-10-16 | 浙江炬泰新材料科技有限公司 | High temperature mixing silicon rubber and production process |
-
2013
- 2013-11-29 CN CN201310624813.3A patent/CN103627178B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0848779A (en) * | 1994-08-03 | 1996-02-20 | Shin Etsu Chem Co Ltd | Production of organopolysiloxane |
| CN1155562A (en) * | 1995-10-11 | 1997-07-30 | 陶氏康宁公司 | Curable organopolysiloxane compositions with improved adhesion |
| CN101712800A (en) * | 2009-11-06 | 2010-05-26 | 陈俊光 | Organic silicon resin encapsulant of large power LED and preparing method thereof |
| CN102532900A (en) * | 2010-12-20 | 2012-07-04 | 常州化学研究所 | Organosilicon lens material for power type light-emitting diode (LED) packaging |
| CN102344684A (en) * | 2011-08-15 | 2012-02-08 | 王昌归 | Organic silicon rubber used for LED module packaging and preparation method thereof |
| JP2013067677A (en) * | 2011-09-20 | 2013-04-18 | Sumitomo Bakelite Co Ltd | Silicone rubber curable composition, method of manufacturing silicone rubber, silicone rubber, compact, and medical tube |
| CN103351624A (en) * | 2013-05-10 | 2013-10-16 | 浙江炬泰新材料科技有限公司 | High temperature mixing silicon rubber and production process |
Cited By (23)
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|---|---|---|---|---|
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Address after: 256401 Tangshan, Shandong, Huantai Town, Zibo Co-patentee after: Institute of Process Engineering, Chinese Academy of Sciences Patentee after: Shandong Dongyue organosilicon material Limited by Share Ltd Address before: 256401 Tangshan, Shandong, Huantai Town, Zibo Co-patentee before: Institute of Process Engineering, Chinese Academy of Sciences Patentee before: Shandong Dongyue Silicon Material co., Ltd. |
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