CN102993753B - A kind of composite hybridization organosilicon LED encapsulation material and its preparation method and application - Google Patents

A kind of composite hybridization organosilicon LED encapsulation material and its preparation method and application Download PDF

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CN102993753B
CN102993753B CN201210484569.0A CN201210484569A CN102993753B CN 102993753 B CN102993753 B CN 102993753B CN 201210484569 A CN201210484569 A CN 201210484569A CN 102993753 B CN102993753 B CN 102993753B
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organosilicon
composite hybridization
encapsulation material
led encapsulation
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CN102993753A (en
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刘伟区
韩敏健
闫振龙
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Guangzhou Chemical Co Ltd of CAS
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Abstract

The invention discloses a kind of composite hybridization organosilicon LED encapsulation material and its preparation method and application.The present invention is by mixing 10 ~ 100 parts by weight of silica phenyl organosilicon composite hybridization things, 0 ~ 48 parts by weight of ethylene based polysiloxane, 0.00001 ~ 0.0002 part by weight of catalyst A, 1.6 ~ 32 weight part hydrogen containing siloxanes, under 80 ~ 110 DEG C of vacuum conditions, react 1 ~ 8h, obtain composite hybridization organosilicon LED encapsulation material.Organosilicon composite hybridization material provided by the invention not only preparation method is simple, and raw materials environmental protection is easy to get, and has the advantage that high refractive index, high-transmission rate, high strength etc. meet LED requirement.The composite hybridization organosilicon LED encapsulation material prepared mainly is used as the packaged material of great power LED and white light LEDs.

Description

A kind of composite hybridization organosilicon LED encapsulation material and its preparation method and application
Technical field
The present invention relates to a kind of LED encapsulation material, particularly a kind of composite hybridization organosilicon LED encapsulation material and its preparation method and application.
Background technology
LED encapsulation material comprises the high transparent materials such as epoxy resin, polycarbonate, polymethylmethacrylate, organosilicon, and wherein polycarbonate and polymethylmethacrylate are used as LED outer layer lens material, and epoxy and organosilicon are mainly as packaged material.Epoxy resin is because it has excellent cohesiveness, electrical insulating property, stopping property and dielectric properties, and cost compare is low, flexible and changeable, the high mainstay material becoming LED of production efficiency of filling a prescription.But, along with the improving constantly and the development of white light LEDs of power of LED, higher requirement is also proposed to the packaged material of LED, such as high refractive index, high-transmission rate, high thermal conductivity, resistance to ultraviolet and thermal ageing ability and low thermal coefficient of expansion, low ion content and low-stress etc.The water absorbability that epoxy self exists, easily aging, high temperature and short wavelength light are according to not enough work-ing lifes that then can greatly affect and shorten LED component such as lower internal stress easy to change, solidification are large.Compared with epoxy resin, organosilicon material then has the good transparency, weathering resistance, insulativity and strong hydrophobicity etc., becomes the ideal chose of LED encapsulation material, also receives the concern of domestic and international investigator simultaneously.
At present, the research of organosilicon encapsulating material concentrates on and improves specific refractory power and strengthen the aspects such as mechanical strength.Although adopting containing benzene siloxanes is the packaged material that organosilicon encapsulating material prepared by raw material can obtain high-transmission rate and high refractive index, its mechanical property does not get a promotion.The mode of chemistry or physical blending is adopted to be doped into organosilicon encapsulating material nano silicon or titanium dioxide separately, although the performances such as LED encapsulation material mechanical property and ultraviolet aging resistance can be made to be improved, but along with the increase of nanoparticle addition, nanoparticle and the blended insufficient homogeneity that result in organosilicon encapsulating material of other raw materials are deteriorated, and the optical properties such as the transmissivity of organosilicon encapsulating material and specific refractory power are obviously declined.
Summary of the invention
For overcoming shortcoming and defect of the prior art, primary and foremost purpose of the present invention is the composite hybridization organosilicon LED encapsulation material providing a kind of high refractive index, high-transmission rate, high strength.
Another object of the present invention is to the preparation method that above-mentioned composite hybridization organosilicon LED encapsulation material is provided.
Another object of the present invention is the application providing above-mentioned composite hybridization organosilicon LED encapsulation material.
Object of the present invention is achieved through the following technical solutions:
A kind of composite hybridization organosilicon LED encapsulation material, is prepared from by following raw material by weight:
Described silicon-dioxide phenyl organosilicon composite hybridization thing is obtained by the method comprising following steps: by 10 ~ 100 weight parts containing the mixing of benzene siloxanyl monomers, 1.50 ~ 27.2 parts by weight of ethylene radical siloxane monomers, 0.1 ~ 6 weight part nano silicon, 0.1 ~ 1 part by weight of catalyst B, 1.5 ~ 10 weight parts waters and 20 ~ 280 weight parts organic solvent, 5 ~ 9h is reacted at 50 ~ 70 DEG C, at 60 ~ 85 DEG C, rotary evaporation 0.5 ~ 3h is except anhydrating and organic solvent, obtains silicon-dioxide phenyl organosilicon composite hybridization thing;
Described is one in phenyl three (dimethyl siloxane) silane, phenyl three (trimethylsiloxane group) silane, dimethoxydiphenylsilane, dimethoxydiphenylsilane, phenyltrimethoxysila,e and phenyl triethoxysilane or at least two kinds containing benzene siloxanyl monomers;
Described vinylsiloxane monomer is one in vinyltrimethoxy silane, vinyltriethoxysilane, propenyl trichlorosilane, γ-(methacryloxypropyl) propyl trimethoxy silicane, vinyl three tert-butoxy silane and vinyltriacetoxy silane or at least two kinds;
The particle size range of described nano silicon is 7 ~ 410nm;
Described catalyst B is one in hydrochloric acid, sulfuric acid, phosphoric acid, boric acid, nitric acid, alkali metal hydroxide, alkali-metal oxide compound, organic amine, quaternary ammonium salt, dibutyl tin acetate, dibutyl tin dilaurate, stannous octoate, phosphorus trichloride, boron trichloride, iron trichloride, ferric bromide, zinc chloride, tin tetrachloride and titanium tetrachloride or at least two kinds;
Described organic solvent is one in dimethylbenzene, vinyl acetic monomer, tetrahydrofuran (THF), toluene and propyl carbinol or at least two kinds;
Described catalyst A is platinum complex, the dicyclopentadiene platinum dichloride (Cp of tetramethyl divinyl disiloxane coordination 2ptCl 2), two (triphenylphosphine) ((PPh of the platinum complex of diethyl phthalate coordination, dichloro 3) 2cl 2) platinum complex of coordination, tetrahydrofuran (THF) make the H of solvent 2ptCl 6, Virahol makes the H of solvent 2ptCl 6with four (triphenylphosphine) platinum (Pt (PPh 3) 4) in one or at least two kinds;
Described hydrogeneous organopolysiloxane is preferably the hydrogeneous organopolysiloxane that hydrogeneous massfraction is 0.1 ~ 1.5%;
Described vinyl organopolysiloxane is preferably the vinyl organopolysiloxane that vinyl massfraction is 0.1 ~ 6.0%;
The preparation method of described composite hybridization organosilicon LED encapsulation material, comprise following steps: by hydrogeneous to 10 ~ 100 parts by weight of silica phenyl organosilicon composite hybridization things, 0 ~ 48 parts by weight of ethylene based polysiloxane, 0.00001 ~ 0.0002 part by weight of catalyst A and 1.6 ~ 32 weight parts organopolysiloxane mixing, under 80 ~ 110 DEG C of vacuum conditions, react 1 ~ 8h, obtain composite hybridization organosilicon LED encapsulation material;
Described composite hybridization organosilicon LED encapsulation material is applied in the encapsulation field of LED, in particular as the packaged material of great power LED and white light LEDs.
The present invention has following advantage and effect relative to prior art:
(1) composite hybridization organosilicon LED encapsulation material provided by the present invention, adopt the nano-silicon dioxide particle of hydroxyl and contain benzene siloxanes, vinylsiloxane hydrolytic condensation, the silicon-dioxide phenyl organosilicon composite hybridization thing synthesized on this basis achieves three's high efficiency composition hydridization, well solve nano-silicon dioxide particle in packaged material, disperse uneven problem, solidify with hydrogen containing siloxane again, the composite hybridization LED encapsulation material obtained, improves the optical properties such as the specific refractory power of packaged material while strongthener mechanical property.
(2) composite hybridization organosilicon LED encapsulation material provided by the present invention, by improving nano silicon and the consumption containing benzene siloxanyl monomers in silicon-dioxide phenyl organosilicon composite hybridization thing, increase the organosilicon composite hybridization thing cross-linking density of corresponding preparation, there is high refractive index and the feature such as transmissivity, high strength.
Embodiment
Below in conjunction with embodiment, further detailed description is done to the present invention, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) loading of 120g dimethoxydiphenylsilane, 25g γ-(methacryloxypropyl) propyl trimethoxy silicane, 6g nano silicon (120 ± 10nm), 0.80g dibutyl tin dilaurate, 10g distilled water and 150g tetrahydrofuran (THF) is possessed in the reactor of stirrer, condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 9h at 50 DEG C, at 80 DEG C, rotary evaporation 1h is except anhydrating and tetrahydrofuran (THF), obtains the silicon-dioxide phenyl organosilicon composite hybridization thing that contents of ethylene is 0.57%;
(2) silicon-dioxide phenyl organosilicon composite hybridization thing 100g in step (1) is got, two (triphenylphosphine) ((PPh of 0.20mg dichloro 3) 2cl 2) platinum complex, the hydrogeneous organopolysiloxane of 1.60g (202 types of coordination, technical grade, hydrogen content 1.5%,) be placed in open container, stir under normal temperature, then obtained composite hybridization organosilicon LED encapsulation material A after 5h is reacted at being placed in 90 DEG C under vacuum, performance test project and the results are shown in Table 1.
Embodiment 2
(1) loading of 15g mono-phenyltrimethoxysila,e, 1.50g vinyltriethoxysilane, 0.91g nano silicon (7 ~ 40nm), 0.10g dibutyl tin acetate, 1.50g distilled water and 20g toluene is possessed in the reactor of stirrer, condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 6h at 65 DEG C, at 70 DEG C of rotary evaporation 2h except anhydrating and toluene, obtain the silicon-dioxide phenyl organosilicon composite hybridization thing that contents of ethylene is 1.90%;
(2) silicon-dioxide phenyl organosilicon composite hybridization thing 10g, 10g vinyl polysiloxane (SiVi-300 in step (1) is got, 300mPas, vinyl molar fraction is 1.92%, Xin An chemical inc, Zhejiang), 0.01mg tetrahydrofuran (THF) makes the H of solvent 2ptCl 6(Solute mass fraction is 0.2%) and 9.00g hydrogen containing siloxane (202 types, technical grade, hydrogen content 0.18%) be placed in open container, stir under normal temperature, obtained composite hybridization organosilicon LED encapsulation material B react 4h under vacuum condition at 95 DEG C after, performance test project and the results are shown in Table 1.
Embodiment 3
(1) loading of 75.50g diphenyl diethoxy silane, 21.50g vinyl three tert-butoxy silane, 5.95g nano silicon (400 ± 10nm), 0.40g stannous octoate, 7.2g distilled water and 110g propyl carbinol is possessed in the reactor of stirrer, condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 7h at 60 DEG C, at 85 DEG C, rotary evaporation 30min is except anhydrating and propyl carbinol, obtains the silicon-dioxide phenyl organosilicon composite hybridization thing that contents of ethylene is 2.75%;
(2) get silicon-dioxide phenyl organosilicon composite hybridization thing 50g, 10g vinyl polysiloxane (SiVi-1000,1000mPas, vinyl molar fraction is 0.8%, Xin An chemical inc, Zhejiang) in step (1), H that 0.06mg Virahol makes solvent 2ptCl 6(Solute mass fraction is 0.3%) and 4.20g hydrogen containing siloxane (202 types, technical grade, hydrogen content 0.54%) be placed in open container, stir under normal temperature, obtained composite hybridization organosilicon LED encapsulation material C react 8h under vacuum condition at 80 DEG C after, performance test project and the results are shown in Table 1.
Embodiment 4
(1) 46g phenyl-trichloro-silicane, 12.60g vinyltrimethoxy silane, 4.5g nano silicon (200 ± 10nm), 0.40g stannous octoate, 5.0g distilled water and 75g dimethylbenzene mixing loading is possessed in the reactor of stirrer, condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 5h at 70 DEG C, at 60 DEG C, rotary evaporation 3h is except anhydrating and dimethylbenzene, obtains the silicon-dioxide phenyl organosilicon composite hybridization thing that contents of ethylene is 1.82%;
(2) silicon-dioxide phenyl organosilicon composite hybridization thing 40g in step (1) is got, 30g vinyl polysiloxane (SiVi-500, 500mPas, vinyl molar fraction is 1.2%, Xin An chemical inc, Zhejiang), the platinum complex of 0.05mg diethyl phthalate coordination, 11.12g hydrogen containing siloxane (end containing hydrogen silicone oil, technical grade, available hydrogen content 0.1%, Kaihua County brothers' silicone material factory) be placed in open container, stir under normal temperature, obtained composite hybridization organosilicon LED encapsulation material D react 1h under vacuum condition at 110 DEG C after, performance test project and the results are shown in Table 1.
Embodiment 5
(1) loading of 58g diphenyl dichlorosilane, 27.20g vinyltriacetoxy silane, 0.1g nano silicon (30 ± 5nm), 0.40g dibutyl tin dilaurate, 6.10g distilled water and 100g tetrahydrofuran (THF) is possessed in the reactor of stirrer, condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 8h at 55 DEG C, at 75 DEG C, rotary evaporation 1.5h is except anhydrating and tetrahydrofuran (THF), obtains the silicon-dioxide phenyl organosilicon composite hybridization thing that vinyl is 5.36%;
(2) silicon-dioxide phenyl organosilicon composite hybridization thing 54g, 48g vinyl polysiloxane (SiVi-300 in step (1) is got, 300mPas, vinyl molar fraction is 1.92%, Xin An chemical inc, Zhejiang), 0.04mg dicyclopentadiene platinum dichloride (Cp 2ptCl 2), 32.00g hydrogen containing siloxane (202 types, technical grade, hydrogen content 0.54%) be placed in open container, stir under normal temperature, obtained composite hybridization organosilicon LED encapsulation material E react 3h under vacuum condition at 98 DEG C after, performance test project and the results are shown in Table 1.
Embodiment 6(comparative examples)
(1) get 63g tetraethoxy, 8g vinyltriethoxysilane, 0.40g dibutyl tin dilaurate, 5g distilled water, 100g toluene load possess in the reactor of stirrer, condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 7h at 60 DEG C, at 75 DEG C, rotary evaporation 1.5h is except anhydrating and toluene, obtains the organosilicon that contents of ethylene is 1.5%;
(2) get organosilicon that 25g step (1) obtains, H that 15g hydrogen containing siloxane (end containing hydrogen silicone oil, technical grade, available hydrogen content 0.1%, Kaihua County brothers' silicone material factory), 0.10mg Virahol make solvent 2ptCl 6(Solute mass fraction is 0.4%) is placed in open container, stirs, obtain organosilicon material F under 90 DEG C of vacuum conditions after reacting 5h under normal temperature, performance test project and the results are shown in Table 1.
The performance of the organosilicon composite hybridization material A ~ F prepared by embodiment 1 ~ 6 is in table 1:
Table 1
Transmissivity arepresent the transmissivity of material after UV-irradiation 500h
Organosilicon composite hybridization material A ~ F prepared by embodiment 1 ~ 5 and comparative examples 6 is carried out the process of batten sanding and polishing, and testing method is as follows:
Transmissivity: measure by GB/T2410-2008;
Specific refractory power: measure by GB/T6488-2008;
Hardness: measure by GB/T 2411-2008;
Tensile strength: measure by GB/T 2951.42-2008;
Transmissivity a: i.e. resistance to ultraviolet test, measures by GB/T 18950-2003;
Can judge in table 1, from the contrast of organosilicon composite hybridization material A ~ E and F, find to the addition of silicon-dioxide, along with the increase of phenyl content, A ~ E shows the feature such as high refractive index and transmissivity, higher intensity, resistance to ultraviolet, reaches the technology of the present invention and improves effect.
Comparative example 1:
Composite hybridization organosilicon LED encapsulation material of the present invention specifically contrast implement formula and performance in table 2:
Table 2
Formula Proportioning A/B/C Transmissivity Specific refractory power Hardness Tensile strength Transmissivity a
7 100(A7)/35/20 93% 1.50 35A 2.1MP 91%
8 100(A8)/35/20 95% 1.52 47A 2.9MP 92%
9 100(A9)/35/20 96% 1.55 61D 3.7MP 93%
10 100(A10)/35/20 94% 1.53 73D 4.3MP 90%
11 100(A11)/35/20 90% 1.48 82D 5.2MP 87%
Transmissivity arepresent the transmissivity of material after UV-irradiation 500h
A7, A8, A9, A10, A11 represent that silicon-dioxide phenyl organosilicon composite hybridization thing is containing benzene siloxanyl monomers, and the weight of synthesizing the important source material dimethoxydiphenylsilane of A7, A8, A9, A10, A11, γ-(methacryloxypropyl) propyl trimethoxy silicane and nano silicon (120nm ± 10nm) is respectively 100/19.9/0.1,100/19.5/0.5,100/19/1,100/15/5,100/10/10.B represents the polysiloxane of hydrogeneous 0.5%, and C represents other components.
Transmissivity: measure by GB/T2410-2008;
Specific refractory power: measure by GB/T6488-2008;
Hardness: measure by GB/T 2411-2008;
Tensile strength: measure by GB/T 1701-2001;
Transmissivity a: i.e. resistance to ultraviolet test, measures by GB/T 18950-2003;
Table 2 A7 components silica phenyl organosilicon composite hybridization thing in 7 of filling a prescription is obtained by the method comprising following steps: by 100 weight part dimethoxydiphenylsilanes, 19.9 weight part γ-(methacryloxypropyl) propyl trimethoxy silicane, 0.1 weight part nano silicon (120nm ± 10nm), 1 weight part dibutyl tin dilaurate, 3 weight part distilled water and the loading of 150 weight part tetrahydrofuran (THF)s possess stirrer, in the reactor of condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 9h at 50 DEG C, at 80 DEG C, rotary evaporation 1h is except anhydrating and tetrahydrofuran (THF), obtaining contents of ethylene is 1.57% silicon-dioxide phenyl organosilicon composite hybridization thing,
The preparation method of composite hybridization LED encapsulation material, comprise following steps: get 100 parts by weight of silica phenyl organosilicon composite hybridization things (in corresponding above-mentioned comparative example 1 formula component A), 20 parts by weight of ethylene based polysiloxane (SiVi-300,300mPas, vinyl molar fraction is 1.92%, Xin An chemical inc, Zhejiang), 0.00005 weight part tetrahydrofuran (THF) makes the H of solvent 2ptCl 6(Solute mass fraction is 0.2%), 32 weight part hydrogen containing siloxanes (202 types, technical grade, hydrogen content 0.54%) are placed in open container, stir under normal temperature, obtained composite hybridization organosilicon LED encapsulation material react 4h under vacuum condition at 95 DEG C after;
Table 2 other components in 8 ~ 11 of filling a prescription are constant, only change the relative usage of γ-(methacryloxypropyl) propyl trimethoxy silicane and nano silicon (120 ± 10nm).
Fill a prescription a kind of composite hybridization organosilicon of 7 ~ 11 the present invention provided LED encapsulation material relatively from table 2, under same materials conditions of mixture ratios, along with the increase preparing nano silicon consumption in silicon-dioxide phenyl organosilicon composite hybridization thing in formula, hardness and the tensile strength of composite hybridization organosilicon LED encapsulation material enlarge markedly, physical and mechanical property is significantly improved, the over-all properties of material is significantly improved, and has fully demonstrated technology of the present invention and has improved effect.
Comparative example 2:
Another group of composite hybridization organosilicon LED encapsulation material of the present invention concrete contrast enforcement formula and performance thereof are in table 3:
Table 3
Formula Proportioning A/B/C Transmissivity Specific refractory power Hardness Tensile strength Transmissivity a
12 100(A12)/25/0.1 96% 1.55 63D 1.8MP 93%
13 100(A13)/25/0.1 94% 1.54 60D 1.9MP 90%
14 100(A14)/25/0.1 93% 1.52 55A 1.6MP 91%
15 100(A15)/25/0.1 90% 1.49 59A 1.5MP 88%
16 100(A16)/25/0.1 88% 1.47 57A 1.7MP 85%
Transmissivity arepresent the transmissivity of material after UV-irradiation 500h
A12, A13, A14, A15, A16 represent that silicon-dioxide phenyl organosilicon composite hybridization thing is containing benzene siloxanyl monomers, the weight of synthesis important source material one phenyltrimethoxysila,e of A12, A13, A14, A15, A16, vinyltriethoxysilane and nano silicon (80nm ± 10nm) is respectively 100/10/1,90/20/1,60/50/1,30/80/1,10/100/1.B represents hydrogeneous 0.9% polysiloxane, C represents the H that Virahol dissolves 2ptCl 6.
Transmissivity: measure by GB/T2410-2008;
Specific refractory power: measure by GB/T6488-2008;
Hardness: measure by GB/T 2411-2008;
Tensile strength: measure by GB/T 1701-2001;
Transmissivity a: i.e. resistance to ultraviolet test, measures by GB/T 18950-2003;
Table 3 A12 components silica phenyl organosilicon composite hybridization thing in 12 of filling a prescription is obtained by the method comprising following steps: by 100 weight part phenyltrimethoxysila,e, 10 parts by weight of ethylene ethyl triethoxy silicane alkane, 1 weight part nano silicon (80nm ± 10nm), 0.5 weight part dibutyl tin acetate, 5 weight part distilled water and the loading of 280 parts by weight of toluene possess stirrer, in the reactor of condensing reflux pipe and thermometer, mix and stir, then condensing reflux reaction 6h at 65 DEG C, at 70 DEG C of rotary evaporation 2h except anhydrating and toluene, obtain the silicon-dioxide phenyl organosilicon composite hybridization thing that contents of ethylene is 1.95%,
The preparation of composite hybridization LED encapsulation material, comprises following steps: get 100 parts by weight of silica phenyl organosilicon composite hybridization things (corresponding above-mentioned comparative example 2 fill a prescription in component A), H that 0.0002 parts by weight of isopropyl alcohol makes solvent 2ptCl 6(Solute mass fraction is 0.4%), 25 weight part hydrogen containing siloxane (202 types, technical grade, hydrogen content 0.54%) be placed in open container, stir under normal temperature, obtained composite hybridization organosilicon LED encapsulation material after reacting 5h at being then placed in 90 DEG C under vacuum;
13 ~ 16 other components of filling a prescription in table 3 are constant, only change the relative usage of phenyltrimethoxysila,e and vinyltriethoxysilane, obtain the silicon-dioxide phenyl organosilicon composite hybridization thing that contents of ethylene is 1.95%.
Fill a prescription a kind of composite hybridization organosilicon of 12 ~ 16 the present invention provided LED encapsulation material relatively from table 3, under same materials conditions of mixture ratios, along with the increase preparing phenyl siloxane consumption in silicon-dioxide phenyl organosilicon composite hybridization thing in formula, transmissivity and the specific refractory power of material been significantly enhanced thereupon.The over-all properties of material effectively improves, and has fully demonstrated technology of the present invention and has improved effect.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (8)

1. a composite hybridization organosilicon LED encapsulation material, is characterized in that: be prepared from by following raw material by weight:
Described silicon-dioxide phenyl organosilicon composite hybridization thing is obtained by the method comprising following steps: by 10 ~ 100 weight parts containing the mixing of benzene siloxanyl monomers, 1.50 ~ 27.2 parts by weight of ethylene radical siloxane monomers, 0.1 ~ 6 weight part nano silicon, 0.1 ~ 1 part by weight of catalyst B, 1.5 ~ 10 weight parts waters and 20 ~ 280 weight parts organic solvent, 5 ~ 9h is reacted at 50 ~ 70 DEG C, at 60 ~ 85 DEG C, rotary evaporation 0.5 ~ 3h is except anhydrating and organic solvent, obtains silicon-dioxide phenyl organosilicon composite hybridization thing;
Described catalyst B is one in hydrochloric acid, sulfuric acid, phosphoric acid, boric acid, nitric acid, alkali metal hydroxide, alkali-metal oxide compound, organic amine, quaternary ammonium salt, dibutyl tin acetate, dibutyl tin dilaurate, stannous octoate, phosphorus trichloride, boron trichloride, iron trichloride, ferric bromide, zinc chloride, tin tetrachloride and titanium tetrachloride or at least two kinds;
The H that described catalyst A is the platinum complex of tetramethyl divinyl disiloxane coordination, dicyclopentadiene platinum dichloride, the platinum complex of diethyl phthalate coordination, the platinum complex of two (triphenylphosphine) coordination of dichloro, tetrahydrofuran (THF) make solvent 2ptCl 6, Virahol makes the H of solvent 2ptCl 6with the one in four (triphenylphosphine) platinum or at least two kinds.
2. composite hybridization organosilicon LED encapsulation material according to claim 1, is characterized in that: described is one in phenyl three (dimethyl siloxane) silane, phenyl three (trimethylsiloxane group) silane, dimethoxydiphenylsilane, dimethoxydiphenylsilane, phenyltrimethoxysila,e and phenyl triethoxysilane or at least two kinds containing benzene siloxanyl monomers.
3. composite hybridization organosilicon LED encapsulation material according to claim 1, is characterized in that: described vinylsiloxane monomer is one in vinyltrimethoxy silane, vinyltriethoxysilane, propenyl trichlorosilane, γ-(methacryloxypropyl) propyl trimethoxy silicane, vinyl three tert-butoxy silane and vinyltriacetoxy silane or at least two kinds.
4. composite hybridization organosilicon LED encapsulation material according to claim 1, is characterized in that: the particle size range of described nano silicon is 7 ~ 410nm.
5. composite hybridization organosilicon LED encapsulation material according to claim 1, is characterized in that: described organic solvent is one in dimethylbenzene, vinyl acetic monomer, tetrahydrofuran (THF), toluene and propyl carbinol or at least two kinds.
6. the preparation method of the composite hybridization organosilicon LED encapsulation material described in any one of Claims 1 to 5, it is characterized in that: by 10 ~ 100 parts by weight of silica phenyl organosilicon composite hybridization things, 0 ~ 48 parts by weight of ethylene based polysiloxane, 0.00001 ~ 0.0002 part by weight of catalyst A, the hydrogeneous organopolysiloxane mixing of 1.6 ~ 32 weight part, under 80 ~ 110 DEG C of vacuum conditions, react 1 ~ 8h, obtain composite hybridization organosilicon LED encapsulation material.
7. the application of the composite hybridization organosilicon LED encapsulation material described in any one of Claims 1 to 5, is characterized in that: described composite hybridization organosilicon LED encapsulation material is applied to the encapsulation field of LED.
8. the application of composite hybridization organosilicon LED encapsulation material according to claim 7, is characterized in that: described composite hybridization organosilicon LED encapsulation material is used as the packaged material of great power LED and white light LEDs.
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