CN103275321A - Preparation method and application of organosilicon photo-diffusion particle - Google Patents
Preparation method and application of organosilicon photo-diffusion particle Download PDFInfo
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Abstract
The invention relates to a preparation method and application of an organosilicon photo-diffusion particle. The preparation method comprises the following steps of: hydrolyzing silane with polar groups in acidic water or co-hydrolyzing silane with polar groups and silane without polar groups in acidic water; and then condensing the hydrolysate into an organosilicon resin spherical particle in alkaline water. The prepared organosilicon photo-diffusion particle is suitable to serve as a coating photo-diffusion membrane, has higher optical efficiency than the PMMA (poly(methyl methacrylate))-based photo-diffusion particle, can also avoid the defects caused by aggregation of photo-diffusion particles, and is simultaneously bonded with cured glue firmly.
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 light diffusion particle, the preparation method of described organosilicon light diffusion particle is used for making coating class optical diffusion film, replaces the basic light diffusion particle of methyl methacrylate (PMMA).
Background technology
Optical diffusion film just be widely used in the various liquid-crystal displays such as TV, computer monitor, smart mobile phone and the semiconductor lighting that progressively enlarges in recent years in.The basic structure of most diffusion barriers is (as the thin mould of PET) two sides or single face burnish gilding diffusion particles on transparent substrate, the specific refractory power of light diffusion particle and PET(ethylene glycol terephthalate) different, light sees through with the diffusion layer of PET as base material, and in the medium of different refractivity, pass, make light that the phenomenon of many refractions, reflection and scattering take place, can revise light and become uniform area light source to reach the effect of optics diffusion.
Light diffusion (mist degree) efficient depends on the refractive index difference between the different media, and particle dia etc., waiting under the particle dia, the specific refractory power difference is more big, and the light deflection angle is more big, and mist degree is just more high, efficient is also just more high: namely under the light diffusion particle prerequisite that adds equivalent, mist degree is bigger, 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 the basic light diffusion particle of methyl methacrylate (PMMA) is 1.49, the specific refractory power of PET is 1.58, so the difference of the specific refractory power 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 efficient of organic silica-based smooth diffusion particle to be higher than the basic light diffusion particle of methyl methacrylate (PMMA).This is generally confirmed in plastics class adding formula is used.
But in cloth of coating-type is used, the light diffusion particle needs to be uniformly dispersed in ethyl acetate, butylacetate equal solvent, vinylformic acid glue earlier, be applied to again to dry on the PET film and make, the surface characteristic of PMMA light diffusion particle (polymethylmethacrylate structure) is close with ethyl acetate, butyl acetate solvent, vinylformic acid glue etc., be easy to disperse few the appearance because the light diffusion particle is assembled the defectives such as white point that cause according to close compatible principle.Organosilicon light diffusion particle surface mostly is and ethyl acetate, butyl acetate solvent, the different bigger methyl polysilicone alkyl structure of vinylformic acid glue equal difference, so it is big slightly to work as its concentration, large-area gathering white-spot defects will appear, and also firm not as PMMA light diffusion particle with the combination of solidifying back vinylformic acid glue simultaneously.
Summary of the invention
The shortcoming of prior art the object of the present invention is to provide a kind of preparation method and application thereof of organosilicon light diffusion particle in view of the above, is used for solving the prior art problem.The prepared organosilicon light diffusion particle of the present invention can be gone up evenly the organic silica-based smooth diffusion particle that disperses, is coated with at plastic film (for example PET film), obtain higher efficient, transmittance and mist degree.
Reach other relevant purposes for achieving the above object, first aspect present invention provides a kind of preparation method of organosilicon light diffusion particle, comprises the following steps:
To have silane hydrolysis in sour water of polar group, or have the silane of polar group and silane cohydrolysis in sour water of nonpolarity group, in alkaline water, be condensed into silicone resin ball-type particle again.
The described silane that has polar group is the silane that has polar group except alkoxyl group.
Preferably, the described silane that has polar group is selected from: the mixing of one or more in methacryloxypropyl trimethoxy silane, methacryloxypropyl triethoxyl silane, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, acryloxy propyl trimethoxy silicane, acryloxy propyl-triethoxysilicane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, the mercaptopropyltriethoxysilane.The silane of described nonpolarity group can be selected from: the mixing of one or more in methyltrimethoxy silane, Union carbide A-162, ethyl trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, tetraethoxysilane or the tetramethoxy-silicane.
Described sour water can obtain by add acid or aqueous acid in reaction solution, as adding aqueous hydrochloric acid, aqueous sulfuric acid etc.The pH value of described sour water is 5-6.
Described alkaline water can obtain by the aqueous solution that adds alkali or alkali in reaction solution, as adding lithium hydroxide, sodium hydroxide, potassium hydroxide, ammoniacal liquor etc.The pH value of described alkaline water is 10-12.
The silane that has a polar group describedly has the silane of polar group and the weight ratio of water is: 1:50 – 1:2 in sour water during hydrolysis.
The silane that has the silane of polar group and a nonpolarity group in sour water during cohydrolysis, the gross weight of the silane of the described silane that has a polar group and nonpolarity group and the weight ratio of water: 1:50 – 1:2.
During cohydrolysis, the silane that has polar group accounts for more than 1% of silane total amount to the silane that has the silane of polar group and a nonpolarity group in sour water.Preferable, the weight ratio of the silane of the described silane that has a polar group and nonpolarity group is: 1:99 – 20:80.Better, the weight ratio of the silane of the described silane that has a polar group and nonpolarity group is: 1:99 – 15:85.
Other conditions of hydrolysis reaction and condensation reaction adopt conventional or utilize the method that charges into rare gas element increase pressure in closed reactor to improve temperature to 130-150 ℃, accelerate hydrolysis and condensation process under 2-5 the normal atmosphere.
After the condensation further filtering drying obtain finished product.
Organosilicon light diffusion particle specific refractory power of the present invention is: 1.42-1.45, good dispersion is not reunited in the mixed solution of ethyl acetate, butylacetate and vinylformic acid glue.
A kind of organosilicon light of second aspect present invention diffusion particle is made by aforementioned preparation method.
Third aspect present invention provides the purposes of described organosilicon light diffusion particle in the optical diffusion film field.
More specifically, described organosilicon light diffusion particle can be used for preparing the cloth of coating-type optical diffusion film.
Fourth aspect present invention provides a kind of optical diffusion film, and described optical diffusion film is that two sides or the single spreading of transparent substrate has organosilicon light diffusion particle of the present invention.
Further, described transparent substrate is the PET(ethylene glycol terephthalate) film.
Fifth aspect present invention provides a kind of preparation method of optical diffusion film, comprises the steps:
1) the light diffusion particle that method of the present invention is prepared evenly spreads to and obtains mixed liquor I in the solvent;
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 is uniformly coated on the transparent substrate and drying.
Concrete, described solvent can be selected from ethyl acetate, the butylacetate equal solvent.
Described coating resin can be acrylic resin.
Described solidifying agent can be isocyanate curing agent.
Described transparent substrate can be: the PET film.
Further, in the 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 the step 3), the dry normal condition that adopts, preferable is dry down at 80-100 ℃ with circulating moisture eliminator.
The present invention easily is uniformly dispersed it by the surface characteristic that changes organosilicon light diffusion particle in ethyl acetate, butylacetate equal solvent, vinylformic acid glue, thereby is suitable for use as the production of cloth of coating-type optical diffusion film.
As mentioned above, the organosilicon light diffusion particle that the present invention is prepared, be suitable for doing the cloth of coating-type optical diffusion film, to compare optical efficiency higher with PMMA base light diffusion particle, and be suitable for doing the cloth of coating-type optical diffusion film, avoid because light diffusion particle assemble the defective that cause the same with PMMA base light diffusion particle, simultaneously firm with the combination of cured glue water.With the prepared coating material of organosilicon light diffusion particle provided by the present invention, under the prerequisite of its optical diffusion film transmittance 90-91%, mist degree can reach 89%, no white-spot defects.
Embodiment
Below by specific specific examples explanation embodiments of the present invention, those skilled in the art can understand other advantages of the present invention and effect easily by the disclosed content of this specification sheets.The present invention can also be implemented or be used by other different embodiment, and the every details in this specification sheets also can be based on different viewpoints and application, carries out various modifications or change under the spirit of the present invention not deviating from.
Embodiment 1
The preparation of organosilicon light diffusion particle
1. material:
1) methacryloxypropyl trimethoxy silane
2) methyltrimethoxy silane
3) deionized water
4) acid: strong acid such as hydrochloric acid, sulfuric acid
5) alkali: lithium hydroxide, sodium hydroxide, potassium hydroxide, ammoniacal liquor etc.
2. making method:
1) methacryloxypropyl trimethoxy silane: methyltrimethoxy silane=1:99 – 20:80
2) (methacryloxypropyl trimethoxy silane+methyltrimethoxy silane): deionized water=1:50 – 1:2
3) acid: an amount of
4) alkali: an amount of
5) in proportion methacryloxypropyl trimethoxy silane, methyltrimethoxy silane mixture are added in the deionized water, it is transparent fully for 5-6 is stirred to system to the pH value to add acid
6) adding alkali to pH value is 10-12, stir to stop in 3-5 minute, and static 4-5 hour, or utilize the method that in closed reactor, charges into rare gas element increase pressure to improve temperature to 130-150 ℃, accelerate hydrolysis and condensation process under 2-5 the normal atmosphere.
7) filter, dry finished product, the finished product specific refractory power is: 1.42-1.45.
8) methacryloxypropyl trimethoxy silane 1) can change the methacryloxypropyl triethoxyl silane into, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, the acryloxy propyl trimethoxy silicane, the acryloxy propyl-triethoxysilicane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilanes etc. have 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.Concrete parameter is chosen and is seen following table for details:
Embodiment 2 distributed tests
Respectively the organosilicon light diffusion particle of pressing example 1-6 preparation among the embodiment 1 is mixed by weight 1:3 with butyl acetate solvent, the vinylformic acid glue that adds weight of solvent 1/3 again, stirred 120 minutes with paddle agitator, be coated onto on the PET film and dry, whether the microscopically observation reunites.
Simultaneous test: nonpolar smooth diffusion particle EL500(gushes strange material)
Result's organosilicon light of the present invention diffusion particle is not all reunited, and contrast nonpolar smooth diffusion particle per 100 square centimeters of white points reunions that can occur more than at least 10 takes place.
In each example, methacryloxypropyl trimethoxy silane is used the methacryloxypropyl triethoxyl silane respectively, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, the acryloxy propyl trimethoxy silicane, the acryloxy propyl-triethoxysilicane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, mercaptopropyltriethoxysilane substitutes, or methyltrimethoxy silane is used Union carbide A-162 respectively, ethyl trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, the organosilicon light diffusion particle that obtains after propyl-triethoxysilicane substitutes all can be in above-mentioned and butyl acetate solvent, do not reunite after the abundant mixing of vinylformic acid glue.
The preparation of embodiment 3 optical diffusion films
1. use material:
I. light diffusion particle
Ii. coating resin: acrylic resin
Iii. solidifying agent: isocyanate curing agent
Iv. base material film: optics level PET film, thickness 100um
V. solvent: butylacetate
2. use equipment:
Vi. coating roll
Vii. circulating moisture eliminator
3. making method:
Viii. the light diffusion particle 40-170 gram that adds each examples preparation among the embodiment 1 in solvent 400 gram respectively stirs more than 2 hours to the light diffusion particle and evenly spreads in the solvent
Ix. in said mixture i, add 40-100 gram coating resin and solidifying agent, fully stir
X. with coating roll ii is uniformly coated on the base material film
It is xi. following dry 3 minutes at 80-100 ℃ with circulating moisture eliminator.
Haze detection instrument: go up Nereid section transmittance mist degree tester
White-spot defects detection method: adopt Shanghai opticinstrument one factory, detect 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.
The result is as shown in the table:
In sum, the present invention has effectively overcome various shortcoming of the prior art and the tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not is used for restriction the present invention.Any person skilled in the art scholar all can be under spirit of the present invention and category, and above-described embodiment is modified or changed.Therefore, have in the technical field under such as and know that usually the knowledgeable modifies or changes not breaking away from all equivalences of finishing under disclosed spirit and the technological thought, must be contained by claim of the present invention.
Claims (11)
1. the preparation method of an organosilicon light diffusion particle comprises the following steps:
Silane hydrolysis in sour water of polar group be will have, or the silane of polar group and silane cohydrolysis in sour water of nonpolarity group had; In alkaline water, be condensed into silicone resin ball-type particle again.
2. preparation method as claimed in claim 1 is characterized in that, the described silane that has polar group is the silane that has polar group except alkoxyl group.
3. preparation method as claimed in claim 1, it is characterized in that the described silane that has polar group is selected from: the mixing of one or more in methacryloxypropyl trimethoxy silane, methacryloxypropyl triethoxyl silane, glycidyl ether oxygen propyl trimethoxy silicane, glycidoxypropyltrietandysilane andysilane, acryloxy propyl trimethoxy silicane, acryloxy propyl-triethoxysilicane, r-chloropropyl trimethoxyl silane, chloropropyl triethoxysilane, mercaptopropyl trimethoxysilane, the mercaptopropyltriethoxysilane; The silane of described nonpolarity group is selected from: the mixing of one or more in methyltrimethoxy silane, Union carbide A-162, ethyl trimethoxy silane, ethyl triethoxysilane, propyl trimethoxy silicane, propyl-triethoxysilicane, tetraethoxysilane or the tetramethoxy-silicane.
4. preparation method as claimed in claim 1, it is characterized in that, the silane that has the silane of polar group and a nonpolarity group is in sour water during cohydrolysis, and the gross weight of the silane of the described silane that has a polar group and nonpolarity group and the weight ratio of water are: 1:50 – 1:2.
5. preparation method as claimed in claim 1 is characterized in that, during cohydrolysis, the silane that has polar group accounts for more than 1% of silane total amount to the silane that has the silane of polar group and a nonpolarity group in sour water.
6. preparation method as claimed in claim 5 is characterized in that, the weight ratio of the silane of the described silane that has a polar group and nonpolarity group is: 1:99 – 15:85.
7. organosilicon light diffusion particle, described preparation method makes by the arbitrary claim of claim 1-6.
8. organosilicon light diffusion particle as claimed in claim 7 is in the purposes in cloth of coating-type optical diffusion film field.
9. optical diffusion film, the basic structure of described optical diffusion film are the two sides of transparent substrate or the single spreading requirement 7 described organosilicon light diffusion particles of having the right.
10. the preparation method of an optical diffusion film comprises the steps:
1) the described smooth diffusion particle of claim 7 is evenly spread to obtains mixed liquor I in the solvent;
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 is uniformly coated on the transparent substrate and drying.
11. the preparation method as optical diffusion film as described in the claim 10 is characterized in that, also satisfies following optional one or multinomial feature:
1) described solvent is ethyl acetate or butylacetate or the mixture of the two;
2) described coating resin is acrylic resin;
3) described solidifying agent is isocyanate curing agent;
4) described transparent substrate is: the PET film.
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| CN104231830A (en) * | 2014-08-08 | 2014-12-24 | 佛山佛塑科技集团股份有限公司 | Preparation method of diffusion film coating composition, preparation method of diffusion film, and corresponding diffusion film |
| CN104610545A (en) * | 2015-02-11 | 2015-05-13 | 广州市晶硅新材料有限公司 | Preparation method of colored organosilicon powder |
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| CN105566579A (en) * | 2015-12-21 | 2016-05-11 | 王金明 | Preparation method of organic silicon light diffusant |
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| CN104610545A (en) * | 2015-02-11 | 2015-05-13 | 广州市晶硅新材料有限公司 | Preparation method of colored organosilicon powder |
| CN105001510A (en) * | 2015-07-02 | 2015-10-28 | 广州科苑新型材料有限公司 | Low temperature resistant halogen-free flame-retardant light scattering polypropylene composition and preparation method thereof |
| CN105001510B (en) * | 2015-07-02 | 2018-06-12 | 广州科苑新型材料有限公司 | A kind of low temperature resistant halogen-free flameproof light diffusion polypropene composition and preparation method thereof |
| CN105254823A (en) * | 2015-09-24 | 2016-01-20 | 浙江衢州万能达科技有限公司 | Preparation method of organosilicon light diffusion microspheres |
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| CN105566568B (en) * | 2015-12-18 | 2017-07-04 | 王金明 | A kind of preparation method of silicon light diffusing agent |
| CN105566568A (en) * | 2015-12-18 | 2016-05-11 | 王金明 | Preparation of fluorine-silicon photodiffusant |
| CN105566579A (en) * | 2015-12-21 | 2016-05-11 | 王金明 | Preparation method of organic silicon light diffusant |
| CN105566579B (en) * | 2015-12-21 | 2018-07-10 | 王金明 | A kind of preparation of organosilicon light diffusing agent |
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| CN105646882B (en) * | 2016-02-24 | 2019-01-22 | 金发科技股份有限公司 | A kind of smooth diffusion particle and preparation method thereof and the thermoplasticity photodiffusion material being made from it and application |
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Effective date of registration: 20200707 Address after: 221300 south of Huancheng North Road and west of Yimeng Mountain Road, Pizhou Economic Development Zone, Xuzhou City, Jiangsu Province Patentee after: JIANGSU YONGXIN MATERIAL TECHNOLOGY Co.,Ltd. Address before: 200433 room 323, No. 601-20, National Road, Shanghai, Yangpu District Patentee before: UNICONE MATERIALS TECHNOLOGY (SHANGHAI) Co.,Ltd. |