CN103275617B - The preparation method of organosilicon photo-diffusion particle and application thereof - Google Patents
The preparation method of organosilicon photo-diffusion particle and application thereof Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method and application thereof of organosilicon photo-diffusion particle, the preparation method of organosilicon photo-diffusion particle of the present invention, comprise the following steps: that the silane of non-polar group is hydrolyzed in sour water, after being condensed into silicone resin spherical particle again in alkaline water, surface treatment is done with the silane with polar group in drying course, silicone hydroxyl with the alkoxyl group in the silane of polar group and silicone resin spherical particle remained on surface is reacted, remove alcohols, form covalent linkage, thus improve silicone resin spherical particle surface polarity.Organosilicon photo-diffusion particle prepared by the present invention, be suitable for making cloth of coating-type optical diffusion film, optical efficiency is higher compared with PMMA base light diffusion particle, and is suitable for making cloth of coating-type optical diffusion film, also can avoid because light diffusion particle assembles the defect caused, simultaneously with cured glue water in conjunction with firm.
Description
Technical field
The present invention relates to a kind of optical diffusion film field, particularly relate to a kind of preparation method and application thereof of organosilicon photo-diffusion particle, the preparation method of described organosilicon photo-diffusion particle, for making coating class optical diffusion film, replaces methyl methacrylate (PMMA) base light diffusion particle.
Background technology
Optical diffusion film is just being widely used in the various liquid-crystal displays such as TV, computer monitor, smart mobile phone and in the semiconductor lighting progressively expanded in recent years.The basic structure of most diffusion barrier is that (mould as thin in PET) two sides or one side are coated with the glue and solvent that contain light diffusion particle over the transparent substrate, specific refractory power and the PET(ethylene glycol terephthalate of light diffusion particle) different, light therethrough is using PET as the diffusion layer of base material, and pass in the medium of different refractivity, make light that many refractions, reflection and the phenomenon of scattering occur, the light uniformly effect that spreads to reach optics of area source can be revised.
Light diffusion (mist degree) efficiency depends on the refractive index difference between different media, and particle dia etc., waiting under particle dia, specific refractory power difference is larger, and light deflection angle is larger, and mist degree is higher, efficiency is also higher: namely under the light diffusion particle prerequisite adding equivalent, mist degree is larger, or obtains identical mist degree, and the add-on of light diffusion particle can reduce.
The specific refractory power of organic silica-based smooth diffusion particle is 1.42, the specific refractory power of methyl methacrylate (PMMA) base light diffusion particle is 1.49, the specific refractory power of PET is 1.58, so the specific refractivity of organosilicon, PMMA base light diffusion particle and PET is respectively 1.58-1.42=0.16 and 1.58-1.49=0.09, this significant difference directly causes the efficiency of organic silica-based smooth diffusion particle higher than methyl methacrylate (PMMA) base light diffusion particle.This Plastic add formula application in generally confirmed.
But in cloth of coating-type application, light diffusion particle needs first to be uniformly dispersed in ethyl acetate, butylacetate equal solvent, vinylformic acid glue, be applied to oven dry in PET film again to make, the surface characteristic (polymethylmethacrylate structure) of PMMA light diffusion particle is close with ethyl acetate solvent, vinylformic acid glue etc., be easy to dispersion according to close compatible principle, few appearance assembles the defects such as the white point caused due to light diffusion particle.Organosilicon photo-diffusion particle surface mostly is and ethyl acetate, butyl acetate solvent, the different larger methyl polysilicone alkyl structure of vinylformic acid glue equal difference, polarity is lower, so when its concentration in ethyl acetate, butylacetate equal solvent, vinylformic acid glue is slightly large, just there will be large-area gathering white-spot defects, be also not so good as PMMA light diffusion particle with the combination of solidifying rear vinylformic acid glue firm simultaneously.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of preparation method and application thereof of organosilicon photo-diffusion particle, for solving problem in prior art.Organosilicon photo-diffusion particle prepared by the present invention can go up organic silica-based smooth diffusion particle that is dispersed, coating at plastic film (such as PET film), obtains higher efficiency, transmittance and mist degree.
For achieving the above object and other relevant objects, first aspect present invention provides a kind of preparation method of organosilicon photo-diffusion particle, comprises the following steps:
The silane of non-polar group is hydrolyzed in sour water, then be condensed into silicone resin spherical particle in alkaline water after, in drying course, does surface treatment with the silane with polar group.
The surface treatment of drying process, silicone hydroxyl (Si-OH) with the alkoxyl groups such as the methoxyl group (-OCH3) in the silane of polar group, oxyethyl group (-OCH2CH3) and silicone resin spherical particle remained on surface is reacted, remove alcohols, form covalent linkage.Thus improve silicone resin spherical particle surface polarity.
The described silane with polar group is the silane with polar group except alkoxyl group.
Preferably, the described silane with polar group is selected from: one or more the mixing in methacryloxypropyl trimethoxy silane, methacryloxypropyl, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, acryloxypropyl Trimethoxy silane, acryloxypropyl triethoxyl silane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane.
The silane of described non-polar group can be selected from: one or more the mixing in methyltrimethoxy silane, Union carbide A-162, ethyl trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, tetraethoxysilane or tetramethoxy-silicane.
Described sour water obtains, as added aqueous hydrochloric acid, aqueous sulfuric acid etc. by acid adding in reaction solution or aqueous acid.The pH value of described sour water is 5-6.
Described alkaline water obtains, as added lithium hydroxide, sodium hydroxide, potassium hydroxide, ammoniacal liquor etc. by the aqueous solution adding alkali or alkali in reaction solution.The pH value of described alkaline water is 10-12.
When the silane of non-polar group is hydrolyzed in sour water, the silane of described non-polar group and the weight ratio of water are: 1:50 – 1:2.
Other conditions of hydrolysis reaction and condensation reaction adopt routine or utilize and in closed reactor, are filled with rare gas element increase pressure to the method raising temperature under 130-150 DEG C, 2-5 normal atmosphere, accelerate to be hydrolyzed and condensation process.
Be specially do surface treatment with the silane with polar group in drying course: in drying course, add the silane with polar group accounting for silicone resin spherical particle weight 0.1-10% and stir.Can disposablely before facing oven dry add, and baking limit, back is stirred; Also can add constantly in the process of drying, and baking limit, limit is stirred.
Organosilicon photo-diffusion particle specific refractory power of the present invention is: 1.42-1.45, and in ethyl acetate, butylacetate or the two mixture, good dispersion is not reunited.
A kind of organosilicon photo-diffusion particle of second aspect present invention, is obtained by aforementioned preparation process.
Third aspect present invention provides the purposes of described organosilicon photo-diffusion particle in optical diffusion film field.
More specifically, described organosilicon photo-diffusion particle can be used for preparing coating type (cloth of coating-type) optical diffusion film.
Fourth aspect present invention provides a kind of optical diffusion film, and the basic structure of described optical diffusion film is scribble organosilicon photo-diffusion particle of the present invention on the two sides of transparent substrate or one side.
Further, described transparent substrate is PET(ethylene glycol terephthalate) film.
Fifth aspect present invention provides a kind of preparation method of optical diffusion film, comprises the steps:
1) light diffusion particle prepared by method of the present invention is evenly spread in solvent obtain mixed liquor I;
2) in the mixed liquor I of step 1), add coating resin and solidifying agent, mix and obtain mixed liquor I I;
3) mixed liquor I I even spread is also dry over the transparent substrate.
Concrete, described solvent can be selected from ethyl acetate, butylacetate or their mixing equal solvent.
Described coating resin can be acrylic resin.
Described solidifying agent can be isocyanate curing agent.
Described transparent substrate can be: PET film.
Further, in step 1), the weight ratio of light diffusion particle and solvent is: 1:2-1:10.
Step 2) in, the gross weight of coating resin and solidifying agent and the weight ratio of solvent are: 1:3-1:10
Step 2) in, the weight ratio of coating resin and solidifying agent is 100:2-5
In step 3), dry employing normal condition, preferably for dry at 80-100 DEG C with circulation dryer.
The present invention is that the surface characteristic by changing organosilicon photo-diffusion particle makes it easily in ethyl acetate, is uniformly dispersed, thus is suitable for use as the production of cloth of coating-type optical diffusion film in butylacetate equal solvent, vinylformic acid glue.
As mentioned above, organosilicon photo-diffusion particle prepared by the present invention, be suitable for making cloth of coating-type optical diffusion film, optical efficiency is higher compared with PMMA base light diffusion particle, and be suitable for making cloth of coating-type optical diffusion film, equally with PMMA base light diffusion particle avoid because light diffusion particle assembles the defect caused, simultaneously with cured glue water in conjunction with firm.With the coating material prepared by organosilicon photo-diffusion particle provided by the present invention, under the prerequisite of its optical diffusion film transmittance 89-91%, mist degree can reach 89%, without white-spot defects.
Embodiment
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Embodiment 1
1. material:
1) methyltrimethoxy silane
2) deionized water
3) acid: hydrochloric acid, the strong acid such as sulfuric acid
4) alkali: lithium hydroxide, sodium hydroxide, potassium hydroxide, ammoniacal liquor etc.
5) methacryloxypropyl trimethoxy silane
2. making method:
1) methyltrimethoxy silane: deionized water=1:50 – 1:2
2) acid: appropriate
3) alkali: appropriate
4) add in deionized water by methyltrimethoxy silane in proportion, it is completely transparent that acid adding to pH value is that 5-6 is stirred to system
5) adding alkali to pH value is 10-12, stirs stopping in 3-5 minute, static 4-5 hour, or utilization is filled with rare gas element increase pressure to the method raising temperature under 130-150 DEG C, 2-5 normal atmosphere in closed reactor, accelerates hydrolysis and condensation process.
6) filter
7) methacryloxypropyl trimethoxy silane adding particle weight 0.1-10% in drying course fully stirs, the finished product after oven dry, and finished product specific refractory power is: 1.42-1.45.
8) methacryloxypropyl trimethoxy silane 7) can change methacryloxypropyl into, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, acryloxypropyl Trimethoxy silane, acryloxypropyl triethoxyl silane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilanes etc. are with the silane of polar group except alkoxyl group.Methyltrimethoxy silane can partly or entirely be substituted by Union carbide A-162, ethyl trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, tetraethoxysilane or tetramethoxy-silicane.Design parameter is chosen and is referred to following table:
Embodiment 2 distributed test
Respectively the organosilicon photo-diffusion particle prepared by example 1-6 in embodiment 1 is mixed by weight 1:3 with butyl acetate solvent, add the vinylformic acid glue of weight of solvent 1/3 again, stir 120 minutes with paddle agitator, be coated onto in PET film and dry, whether basis of microscopic observation reunites.
Simultaneous test: nonpolar smooth diffusion particle EL500(gushes strange material)
Result organosilicon photo-diffusion particle of the present invention is all reunited, and contrasts nonpolar smooth diffusion particle and occur every 100 square centimeters and there will be the white points reunion of more than at least 10.
In each example, methacryloxypropyl trimethoxy silane uses methacryloxypropyl respectively, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, acryloxypropyl Trimethoxy silane, acryloxypropyl triethoxyl silane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane substitutes, or methyltrimethoxy silane uses Union carbide A-162 respectively, ethyl trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, the organosilicon photo-diffusion particle that tetraethoxysilane or tetramethoxy-silicane substitute rear acquisition all can mix with 1:3 weight ratio with ethyl acetate or butylacetate, add the vinylformic acid glue of weight of solvent 1/3 again, do not reunite after stirring abundant mixing in 120 minutes with paddle agitator.
The preparation of embodiment 3 optical diffusion film
1. use material:
I. light diffusion particle
Ii. coating resin: acrylic resin
Iii. solidifying agent: isocyanate curing agent
Iv. base material film: optical grade PET film, thickness 100um
V. solvent: butylacetate
2. use equipment:
Vi. coating roll
Vii. circulation dryer
3. making method:
Viii. in solvent 400 grams, add light diffusion particle 40-170 gram prepared by each example in embodiment 1 respectively, stir and evenly spread in solvent to light diffusion particle for more than 2 hours
Ix. in said mixture i, add 40-100 gram of coating resin and solidifying agent, fully stir
X. with coating roll, ii is uniformly coated on base material film
Xi. circulation dryer is used at 80-100 DEG C dry 3 minutes.
Haze detection instrument: upper Nereid section transmittance mist degree tester
White-spot defects detection method: adopt Shanghai opticinstrument one factory, detects microscope 8XB range estimation
Under the prerequisite of the optical diffusion film transmittance 89-91% of gained coating material, detect mist degree and white-spot defects.
Result is as shown in the table:
In sum, the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (7)
1. a preparation method for organosilicon photo-diffusion particle, comprises the following steps:
The silane of non-polar group is hydrolyzed in sour water, when the silane of non-polar group is hydrolyzed in sour water, the silane of described non-polar group and the weight ratio of water are: 1:50 – 1:2, after being condensed into silicone resin spherical particle again in alkaline water, the pH value of described alkaline water is 10-12, surface treatment is done with the silane with polar group in drying course, silicone hydroxyl with the alkoxyl group in the silane of polar group and silicone resin spherical particle remained on surface is reacted, remove alcohols, form covalent linkage, thus improve silicone resin spherical particle surface polarity, the described silane with polar group is selected from: methacryloxypropyl trimethoxy silane, methacryloxypropyl, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, acryloxypropyl Trimethoxy silane, acryloxypropyl triethoxyl silane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, one or more mixing in mercaptopropyltriethoxysilane, the silane of described non-polar group is selected from: one or more the mixing in methyltrimethoxy silane, Union carbide A-162, ethyl trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, tetraethoxysilane or tetramethoxy-silicane.
2. preparation method as claimed in claim 1, it is characterized in that, be specially do surface treatment with the silane with polar group in drying course: in drying course, add the silane with polar group accounting for silicone resin spherical particle weight 0.1-10% and stir.
3. an organosilicon photo-diffusion particle, is obtained by the preparation method described in the arbitrary claim of claim 1-2.
4. the purposes of organosilicon photo-diffusion particle in cloth of coating-type optical diffusion film field as claimed in claim 3.
5. an optical diffusion film, the basic structure of described optical diffusion film is that the two sides of transparent substrate or one side scribble organosilicon photo-diffusion particle according to claim 3.
6. a preparation method for optical diffusion film, comprises the steps:
1) smooth diffusion particle according to claim 3 is evenly spread in solvent obtain mixed liquor I;
2) to step 1) mixed liquor I in add coating resin and solidifying agent, mix obtain mixed liquor I I;
3) mixed liquor I I even spread is also dry over the transparent substrate.
7. the preparation method of optical diffusion film as claimed in claim 6, is characterized in that, also meets following optional one or more feature:
1) described solvent is ethyl acetate, butylacetate or the two mixture;
2) described coating resin is acrylic resin;
3) described solidifying agent is isocyanate curing agent;
4) described transparent substrate is: PET film.
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| CN104900790A (en) * | 2015-05-13 | 2015-09-09 | 福建泉州世光照明科技有限公司 | LED light source atomization package colloid and atomization LED light source |
| CN105694042B (en) * | 2016-04-26 | 2021-04-13 | 京东方科技集团股份有限公司 | Light diffusion powder, preparation method of light diffusion powder, quantum dot photoresist and quantum dot color film |
| CN106928476B (en) * | 2017-02-28 | 2019-04-02 | 江苏晨光涂料有限公司 | A kind of preparation method of the silicon rubber microballoon for light diffusing agent |
| CN109608939B (en) * | 2018-10-16 | 2022-02-01 | 苏州星烁纳米科技有限公司 | Quantum dot ink and quantum dot color film |
| CN110423562A (en) * | 2019-09-09 | 2019-11-08 | 常州斯威克光伏新材料有限公司 | A kind of EVA white glue film containing light diffusion particle |
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| CN1696179A (en) * | 2005-06-03 | 2005-11-16 | 哈尔滨工业大学 | Method for grafting modifying silicone resin |
| CN101070384A (en) * | 2007-06-20 | 2007-11-14 | 胡孟进 | Process for preparing non-adhesive resin special for organic brick |
| CN101735618A (en) * | 2008-11-26 | 2010-06-16 | 信越化学工业株式会社 | Room temperature curable organopolysiloxane composition |
| CN102627770A (en) * | 2012-03-16 | 2012-08-08 | 深圳市惠乐光电有限公司 | Organosiloxane polymer, preparation method of the organosiloxane polymer, color photoresist for color filter, color filter and preparation method of the color filter |
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| JP5526468B2 (en) * | 2006-09-29 | 2014-06-18 | 大日本印刷株式会社 | Anti-reflection laminate |
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Patent Citations (4)
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|---|---|---|---|---|
| CN1696179A (en) * | 2005-06-03 | 2005-11-16 | 哈尔滨工业大学 | Method for grafting modifying silicone resin |
| CN101070384A (en) * | 2007-06-20 | 2007-11-14 | 胡孟进 | Process for preparing non-adhesive resin special for organic brick |
| CN101735618A (en) * | 2008-11-26 | 2010-06-16 | 信越化学工业株式会社 | Room temperature curable organopolysiloxane composition |
| CN102627770A (en) * | 2012-03-16 | 2012-08-08 | 深圳市惠乐光电有限公司 | Organosiloxane polymer, preparation method of the organosiloxane polymer, color photoresist for color filter, color filter and preparation method of the color filter |
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