CN102504613A - Preparation method of modified fumed silica for LED packaging reinforcement - Google Patents
Preparation method of modified fumed silica for LED packaging reinforcement Download PDFInfo
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- CN102504613A CN102504613A CN201110356195XA CN201110356195A CN102504613A CN 102504613 A CN102504613 A CN 102504613A CN 201110356195X A CN201110356195X A CN 201110356195XA CN 201110356195 A CN201110356195 A CN 201110356195A CN 102504613 A CN102504613 A CN 102504613A
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Abstract
The invention relates to a preparation method of modified fumed silica for LED packaging reinforcement. The preparation method comprises the following steps: 1, pre-activating the fumed silica in a 120DEG C vacuum; 2, mixing water and ethanol according to a mass ratio of 1:5-1:8, adding a certain proportion of an ethylene and phenyl contained alkoxysilane coupling agent, adjusting the pH value of the obtained solution to 3-5 by an organic acid; and 3, adding the activated fumed silica to the obtained system, stirring for 1.5-3h at 100-120DEG C under refluxing, and removing low molecules in a 150DEG C vacuum to obtain the modified fumed silica. The modified fumed silica obtained through the method of the invention has the following advantages: the dispersibility of the fumed silica in a sizing material is improved; the content of the phenyl contained alkoxysilane coupling agent for surface processing is adjusted to adjust the refractive index of the fumed silica; and the use of the organic acid for adjusting the pH value of the system makes the content of inorganic ions in the modified fumed silica be low, so the modified fumed silica is suitable for the packaging of electronic devices. The modified fumed silica of the invention is especially suitable for being used as a reinforcement filler in an LED packaging material.
Description
Technical field
The present invention relates to a kind of preparation method of modified white carbon black, be meant that specifically a kind of LED of can be used for encapsulated strengthening is with modification vapor phase process Preparative Method of White Carbon Black.
Background technology
Along with the progress of science and technology, the development of society, energy problem has become a great difficult problem of face of mankind, and people more will pay attention to save energy when continually developing new forms of energy.At present, China's illumination consumes and accounts for 20% of whole power consumption, and therefore, reducing electric consumption on lighting is an important channel saving electric energy.And superhigh brightness LED (Light Emitting Diode LED) compares with traditional light source, and the electric energy of its consumption only is 1/10 of a conventional light source, and simultaneously, it also has energy-saving and environmental protection, safety, life-span length, low consumption, light beam and advantage such as concentrates.Therefore, through the development of decades, LED has been widely used in aspects such as decorative illumination, automotive lighting, traffic lights, Backlight For Liquid Crystal Display Panels.
At present the packaged material that uses of LED device mainly contains two kinds of bisphenol A-type transparent epoxy resin and organosilicon materials.Along with the development of white light LEDs,, need outer packaged material when keeping the visible region high transparent, can also higher specific absorption be arranged, to prevent the leakage of UV-light to UV-light especially based on the development of the white light LEDs of UV-light; In addition, packaged material also need have stronger ageing resistance by ultraviolet light ability.But the xanthochromia phenomenon can take place in epoxy resin inevitably under the UV-irradiation of led chip emission behind life-time service, causes its transmittance to descend, and then has reduced the brightness of LED device.Organosilicon material (comprising Zylox and silicone resin) then has the transmittance height, and specific refractory power is big, good stability, and advantage such as stress is little, and water absorbability is low, as the packaged material of LED device, its performance is far superior to epoxy resin.
As the packaged material of LED device, except requiring high refractive index (n
D 20>=1.50), high transmission rate and beyond the excellent resistance to ultraviolet(ray) radiation ability, also require it that certain rigidity and tensile strength will be arranged.But the weakness that Zylox is fatal is that the cross-linked rubber intensity of not reinforcement is extremely low, wants to have good physical strength, just must add reinforced filling.As everyone knows, be thermal silica to Zylox system reinforcing effect filler better and commonly used, but there are shortcomings such as mixing difficulty, big, the easy structurizing of dust in the thermal silica of non-modified.Therefore, thermal silica is normal before use earlier to carry out surface-treated to it, and the method for surface-treated mainly contains dry method modification and wet-process modified two kinds.Dry method be adopt exsiccant WHITE CARBON BLACK and treatment agent steam in fixed reactor drum or fluidized-bed reactor under hot conditions contact reacts.Wet-process modifiedly also mainly contain two kinds of methods, the one, with the solution heated and boiled that the exsiccant WHITE CARBON BLACK is formed with properties-correcting agent and organic solvent, back flow reaction, dry then.The 2nd, the exsiccant WHITE CARBON BLACK is mixed with the solution slurry, add water-miscible organic solvent such as alcohols or tensio-active agent etc., add properties-correcting agent then and carry out the organic-silylation reaction.Compare with dry method, it is simple that wet method has technology, advantages such as the easy control of quality product.European patent EP 0382370 (A1) discloses the method for using vinyltrimethoxy silane and phenyltrimethoxysila,e dry method modification thermal silica, and the thermal silica after the modification can improve performances such as compression set property and the thermal ageing of Zylox.U.S. Pat 5942571 discloses the method for using the thermal silica reinforcement Zylox after organosilane-modified, can obtain hardness JIS-A 40, tensile strength 50kgf/cm
2, the silicone rubber products of elongation at break 500%.And patent EP1424363 and US7838117 also disclose and to have adopted the encapsulation of using it for the LED device behind the thermal silica reinforcement Zylox.But, have only 1.46 based on the refractive index of thermal silica, only be applicable to the silicone rubber products that refractive index is close, if use it for the Zylox reinforcement of high refractive index, then can't make product reach high transmittance.If want to make thermal silica to be used for high refractive index Zylox, then must improve the refractive index of thermal silica.
Summary of the invention
To the deficiency that exists in the prior art, the invention discloses and a kind ofly thermal silica is carried out the surface-treated method with silane coupling agent.Utilize the reaction of organism and silicon hydroxyl; Be connected to the surface of thermal silica to organic group, reduced the silicon hydroxyl quantity on thermal silica surface, make it become hydrophobicity by wetting ability; Thereby improved it and organic consistency, and then increased its dispersiveness in polymkeric substance.Owing to the introducing of phenyl, can improve the refractive index of thermal silica simultaneously, use it for the reinforced filling of organosilicon LED packaged material, can satisfy the requirement of LED packaged material high refractive index, high transmission rate.
Its concrete preparation method is following:
A. at first select for use specific surface area to be about 200m
2/ g, median size is thermal silica dry 5h in 120 ℃ of vacuum of 15nm, removes its contained humidity as far as possible;
B. prepare aqueous ethanolic solution, after mixing than water: ethanol=1:5～1:8 by quality, add 8～12 parts of silane coupling agents, using the organic acid adjust pH then is 3～5;
C. in above-mentioned system, add 100 parts of thermal silicas after the activation, 1.5～3h are stirred in 100～120 ℃ of backflows down;
D. remove the thermal silica after low molecule promptly gets modification under 150 ℃ of vacuum.
As preferably; Vinyl coupling agent described in the above-mentioned preparation method is one or more in vinyltrimethoxy silane, vinyltriethoxysilane, methyl ethylene dimethoxy silane, methyl ethylene diethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, and the octadecyloxy phenyl TMOS is one or more in phenyltrimethoxysila,e, phenyl triethoxysilane, dimethoxydiphenylsilane, the phenylbenzene diethoxy silane.
The add-on of silane coupling agent is to add 8～12 parts of silane coupling agents in per 100 parts of thermal silicas among the above-mentioned preparation method.If the add-on of silane coupling agent exceeds this scope, mainly can have influence on the mechanical property of organosilicon encapsulating material.As more preferably selecting, should add 9～10.5 parts of silane coupling agents in per 100 parts of thermal silicas.
As preferably, the ratio of vinyl alkoxy silane and octadecyloxy phenyl TMOS is 0.9:1～2.4:1 in the silane coupling agent that adds among the above-mentioned preparation method.Can get the product of different refractive index through the ratio of regulating both.
As preferably, the organic acid described in the above-mentioned preparation method is formic acid, acetate, oxalic acid, tartrate, phenylformic acid, P-TOLUENE SULFO ACID 99 or Whitfield's ointment etc.As more preferably selecting, described organic acid is an acetate.
Because the utilization of technique scheme, compared with prior art, the present invention has the following advantages: 1. it is wet-process modified preparing the used method of modification thermal silica among the present invention, and it is simple that this method has technology, advantages such as the easy control of quality product.
2. the consistency of the modification thermal silica of the present invention's preparation and organosilicon material is good, and the add-on of WHITE CARBON BLACK is increased.
3. the modification thermal silica refractive index of the present invention's preparation is high, is used for LED and uses organosilicon encapsulating material, can make LED keep higher transmittance with organosilicon encapsulating material.
4. what use among the present invention is organic acid, can not introduce Cl
-And SO
4 2-Deng mineral ion.Simultaneously, used coupling agent is an organoalkoxysilane and without chlorosilane, also further avoided the introducing of cl ions, makes product be applicable to the encapsulation of electron device more.
5. the reagent that uses in the present invention's reaction is nontoxic, pollution-free.
Embodiment
Embodiment 1
Earlier a certain amount of specific surface area is about 200m
2/ g, median size is that the thermal silica of 15nm is subsequent use behind the dry 5h in 120 ℃ of vacuum.After water and ethanol pressed mass ratio=1:5～1:8 and mix, add a certain proportion of organoalkoxysilane coupling agent that contains vinyl and phenyl, using the acetate adjust pH then is 3～5.In this system, add the thermal silica after the above-mentioned activation again, stirring 1.5～3h removes low molecule at last under 150 ℃ of vacuum under 100～120 ℃ of backflows, promptly gets the thermal silica powder after the modification.Can make the product of different refractive index through the vinyl coupling agent in the adjusting silane coupling agent and the ratio of octadecyloxy phenyl TMOS.
Get absolute ethyl alcohol 200g, water 40g mixes the back and adds the 5.7g vinyltrimethoxy silane, the 2.6g dimethoxydiphenylsilane, and the pH value of using the acetic acid regulation system then is 3～5.In this system, add the thermal silica after the 100g activation, 110 ℃ of refluxed stir 2h, under 150 ℃ of vacuum, remove low molecule at last, promptly get the white powder of the thermal silica after the modification, survey its refractive index n
D 20=1.4816
Embodiment 2
Present embodiment and embodiment 1 something in common repeat no more, and difference is to get absolute ethyl alcohol 210g, and water 40g mixes the back and adds 6.8g methyl ethylene dimethoxy silane, 2.9g phenylbenzene diethoxy silane, and the pH that uses the formic acid regulation system then is 3～5.In this system, add the thermal silica after the 100g activation, 120 ℃ of refluxed stir 2h, under 150 ℃ of vacuum, remove low molecule at last, promptly get the white powder of the thermal silica after the modification, survey its refractive index n
D 20=1.4871.
Embodiment 3
Present embodiment and embodiment 1 something in common repeat no more; Difference is to get absolute ethyl alcohol 210g; Water 30g mixes the back and adds 4.6g vinyltriethoxysilane, 1.9g methyl ethylene dimethoxy silane; 3.2g the phenylbenzene diethoxy silane, the pH that uses the acetic acid regulation system then is 3～5.In this system, add the thermal silica after the 100g activation, 120 ℃ of refluxed stir 2h, under 150 ℃ of vacuum, remove low molecule at last, promptly get the white powder of the thermal silica after the modification, survey its refractive index n
D 20=1.4950.
Embodiment 4
Present embodiment and embodiment 1 something in common repeat no more, and difference is to get absolute ethyl alcohol 220g, water 40g; Mix the back and add the 5.2g vinyltrimethoxy silane; 1.4g phenyltrimethoxysila,e, the 2.8g dimethoxydiphenylsilane, the pH that uses the oxalic acid regulation system then is 3～5.In this system, add the thermal silica after the 100g activation, 110 ℃ of refluxed stir 3h, under 150 ℃ of vacuum, remove low molecule at last, promptly get the white powder of the thermal silica after the modification, survey its refractive index n
D 20=1.5032.
Embodiment 5
Present embodiment and embodiment 1 something in common repeat no more; Difference is to get absolute ethyl alcohol 210g; Water 35g mixes the back and adds 4.9g methyl ethylene diethoxy silane, 1.6g phenyl triethoxysilane; 3.4g dimethoxydiphenylsilane, the pH that uses the phenylformic acid regulation system then is 3～5.In this system, add the thermal silica after the 100g activation, 100 ℃ of refluxed stir 3h, under 150 ℃ of vacuum, remove low molecule at last, promptly get the white powder of the thermal silica after the modification, survey its refractive index n
D 20=1.5081.
Embodiment 6
Present embodiment and embodiment 1 something in common repeat no more; Difference is to get absolute ethyl alcohol 230g, and water 35g mixes the back and adds 6.9g vinyl three ('beta '-methoxy oxyethyl group) silane; 3.1g the phenylbenzene diethoxy silane, the pH that uses the acetic acid regulation system then is 3～5.In this system, add the thermal silica after the 100g activation, 120 ℃ of refluxed stir 1.5h, under 150 ℃ of vacuum, remove low molecule at last, promptly get the white powder of the thermal silica after the modification, survey its refractive index n
D 20=1.5140.
Embodiment 7
Present embodiment and embodiment 1 something in common repeat no more; Difference is to get absolute ethyl alcohol 220g, and water 30g mixes the back and adds 7.4g vinyl three ('beta '-methoxy oxyethyl group) silane; 4.5g dimethoxydiphenylsilane, the pH that uses the acetic acid regulation system then is 3～5.In this system, add the thermal silica after the 100g activation, 110 ℃ of refluxed stir 2h, under 150 ℃ of vacuum, remove low molecule at last, promptly get the white powder of the thermal silica after the modification, survey its refractive index n
D 20=1.5216.
The contrast experiment
Selecting refractive index for use is 1.5263 (n
D 20), viscosity is the vinyl silicone oil (self-control) of 2000 mPas (25 ℃), adds the thermal silica in untreated thermal silica and the foregoing description therein respectively, after thorough mixing stirs.Use digital rotational viscosimeter (SNB-2-J, Shanghai Geoscience Instrument Inst.) and ultraviolet-visible pectrophotometer (Tianjin, island UV1750) to survey its viscosity and respectively in the light transmittance values at 450nm place.Concrete outcome following table: table 1
Visible from contrast experiment's result: consistency and the dispersiveness of the WHITE CARBON BLACK after (1) modification silicone oil is improved.When untreated WHITE CARBON BLACK was 10% when add-on, the viscosity of system had just reached 13520 mPas; And added 20% o'clock through the thermal silica after the modification, the viscosity of system also has only about 4000 mPas.(2) unmodified WHITE CARBON BLACK is because refractive index has only 1.46, so and high refractive index (n
D 20=1.5263) transmittance of meeting reduction system after silicone oil mixes, as when add-on is 10%, the transmittance of system has only 88.7%; And the WHITE CARBON BLACK after the modification because refractive index is improved, therefore with it with after the silicone oil of high refractive index mixes, compare with untreated WHITE CARBON BLACK, when add-on is identical, influence little to the transmittance of system.Reached 1.5216 like the refractive index through the thermal silica after the modification among the embodiment 7, with the close (n of refractive index of vinyl silicone oil
D 20=1.5263), therefore when add-on was 20%, the transmittance of system also can reach 98.1%.
Claims (7)
1. one kind is used for the LED encapsulated strengthening with modification vapor phase process Preparative Method of White Carbon Black, it is characterized in that it may further comprise the steps:
(1) with thermal silica dry 5h in 120 ℃ of vacuum, the thermal silica after the activation is subsequent use;
(2) prepare aqueous ethanolic solution, after mixing than water: ethanol=1:5～1:8 by quality, add 8～12 parts of silane coupling agents, using the organic acid adjust pH then is 3～5; Said silane coupling agent is vinyl alkoxy silane and octadecyloxy phenyl TMOS;
(3) in above-mentioned system, add 100 parts of thermal silicas after the activation, 1.5～3h are stirred in 100～120 ℃ of backflows down;
Remove the thermal silica after low molecule promptly gets modification under (4) 150 ℃ of vacuum.
2. preparation method according to claim 1 is characterized in that the specific surface area of described thermal silica is about 200m
2/ g, median size is 15nm.
3. preparation method according to claim 1 is characterized in that described vinyl alkoxy silane is one or more in vinyltrimethoxy silane, vinyltriethoxysilane, methyl ethylene dimethoxy silane, methyl ethylene diethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane.
4. according to claim 1 or 2 or 3 described preparing methods, it is characterized in that the octadecyloxy phenyl TMOS is one or more in phenyltrimethoxysila,e, phenyl triethoxysilane, dimethoxydiphenylsilane, the phenylbenzene diethoxy silane.
5. preparation method according to claim 1 is characterized in that said silane coupling agent is 9～10.5 parts.
6. according to claim 1 or 5 described preparing methods, it is characterized in that the ratio of vinyl alkoxy silane and octadecyloxy phenyl TMOS is 0.9:1～2.4:1 in the silane coupling agent.
7. preparation method according to claim 1 is characterized in that described organic acid is a kind of in formic acid, acetate, oxalic acid, tartrate, phenylformic acid, P-TOLUENE SULFO ACID 99 or the Whitfield's ointment.
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| CN103087556A (en) * | 2012-12-31 | 2013-05-08 | 东莞市万钧化工新材料科技有限公司 | Surface treatment method and application of heat-conducting packing |
| CN103113761A (en) * | 2013-01-31 | 2013-05-22 | 沈阳化工股份有限公司 | Surface modified fumed silica for improving powder fluidity and production method thereof |
| CN104693843A (en) * | 2015-02-16 | 2015-06-10 | 扬州佩恩橡胶科技有限公司 | Preparation method of environment-friendly white carbon black |
| CN107686564A (en) * | 2017-10-30 | 2018-02-13 | 无锡恒诚硅业有限公司 | A kind of preparation method of hydrophabic silica |
| CN109294514A (en) * | 2018-09-29 | 2019-02-01 | 烟台德邦先进硅材料有限公司 | A kind of LED chip organosilicon crystal-bonding adhesive |
| CN109628037A (en) * | 2018-12-14 | 2019-04-16 | 烟台德邦科技有限公司 | Hybrid die attach adhesive for LED chip |
| CN110387145A (en) * | 2019-07-18 | 2019-10-29 | 常州大学 | A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement |
| CN114045152A (en) * | 2021-11-05 | 2022-02-15 | 南京科矽新材料科技有限公司 | Organic silicon die bonding adhesive for die bonding of LED |
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| CN103087556A (en) * | 2012-12-31 | 2013-05-08 | 东莞市万钧化工新材料科技有限公司 | Surface treatment method and application of heat-conducting packing |
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| CN109294514A (en) * | 2018-09-29 | 2019-02-01 | 烟台德邦先进硅材料有限公司 | A kind of LED chip organosilicon crystal-bonding adhesive |
| CN109628037A (en) * | 2018-12-14 | 2019-04-16 | 烟台德邦科技有限公司 | Hybrid die attach adhesive for LED chip |
| CN110387145A (en) * | 2019-07-18 | 2019-10-29 | 常州大学 | A kind of preparation method of the high abrasion white carbon black for butadiene-styrene rubber reinforcement |
| CN114045152A (en) * | 2021-11-05 | 2022-02-15 | 南京科矽新材料科技有限公司 | Organic silicon die bonding adhesive for die bonding of LED |
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