CN102898582A - Micron-sized polymer microsphere, and preparation method and light diffusion plate thereof - Google Patents
Micron-sized polymer microsphere, and preparation method and light diffusion plate thereof Download PDFInfo
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- CN102898582A CN102898582A CN2011102105589A CN201110210558A CN102898582A CN 102898582 A CN102898582 A CN 102898582A CN 2011102105589 A CN2011102105589 A CN 2011102105589A CN 201110210558 A CN201110210558 A CN 201110210558A CN 102898582 A CN102898582 A CN 102898582A
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Abstract
The invention provides a micron-sized polymer microsphere. The micron-sized polymer microsphere is a copolymer of a monomer and a crosslinking agent, wherein the monomer is selected from styrene and/or divinylbenzene, the crosslinking agent is a multifunctional acrylate, and the molar ratio of the monomer to the crosslinking agent is 5-50:50-95. The invention also provides a preparation method of the micron-sized polymer microsphere and a light diffusion plate adopting the micron-sized polymer microsphere. The micron-sized polymer microsphere provided by the invention is micron-sized, the preparation method of the micron-sized polymer microsphere is simple, and the light diffusion plate adopting the micron-sized polymer microsphere has a high light transmittance and a high haze.
Description
Technical field
The invention belongs to the light diffusing sheet technical field, relate in particular to a kind of micrograde polymer microsphere and preparation method thereof and light diffusing sheet.
Background technology
Take resin as main material, light diffusing sheet with light diffusion perviousness has the brightness of homogeneous.Therefore, light diffusing sheet is widely used in the purposes such as illuminating cover, interior lighting formula billboard, penetrating type indicating meter.In recent years, to the surface light source unit of using as the downward back light modulation of liquid-crystal display or LCD TV, the demand of light diffusing sheet increases.
At present, light diffusing sheet commonly used mainly is to utilize the organic/inorganic compound particle to join in the transparent plastics matrix as light diffusing agent to form.Inorganic compound particle commonly used such as barium sulfate, calcium sulfate, silicon-dioxide, aluminum oxide are during as light diffusing agent, and the product of acquisition often has less-than-ideal transmittance, so more be to adopt organic polymer particles as light diffusing agent in the current product.
For example, a kind of polymer particle is disclosed among the CN101331153A, this polymer particle is by being the system of adding polymerizable monomer, polymerization starter, suspension dispersive agent and peptizer in the latex of polymer particles of 1-50 μ m toward volume average particle size, and carries out granulation and suspension polymerization obtains.The particle diameter of the polymer particle that the method obtains is larger, and monodispersity is poor.Adopt suspension agent in the method simultaneously, make the stable then initiating chamical reaction of polymerizable monomer form polymer particle; But this suspension agent is difficult to remove from system after reaction, can have a strong impact on the light diffusing energy, so that adopt transmittance and the mist degree of light diffusing sheet product of this polymer particle still lower.
Summary of the invention
The invention solves the polymer particle particle diameter that exists in the prior art large, owing to adopting suspension agent to be difficult to remove to cause that the preparation method is complicated, transmittance and the lower technical problem of mist degree of the light diffusing sheet that causes adopting this polymer particle.
The invention provides a kind of micrograde polymer microsphere, described micrograde polymer microsphere is the multipolymer of monomer and linking agent; Described monomer is selected from vinylbenzene and/or divinylbenzene, and described linking agent is polyfunctional acrylic ester; The mol ratio of monomer and linking agent is 5-50:50-95.
The present invention also provides the preparation method of described micrograde polymer microsphere, comprises first monomer and linking agent are dissolved in the acetonitrile in proportion, adds initiator and carries out copolyreaction, and drying obtains described micrograde polymer microsphere.
At last, the invention provides a kind of light diffusing sheet, described light diffusing sheet comprises resin base material and the light diffusing agent that is scattered in the resin base material, and described light diffusing agent is micrograde polymer microsphere provided by the invention.
Micrograde polymer microsphere provided by the invention, suitably select by kind and consumption to monomer and linking agent, make it that preliminary polymerization occur in acetonitrile solvent, generate oligopolymer and from acetonitrile, be precipitated out to be suspended in and form micelle in the acetonitrile, micelle continues to absorb monomer, initiator and linking agent, carry out further crosslinking polymerization, particle diameter increases gradually and forms micron-sized polymkeric substance, namely obtain micrograde polymer microsphere of the present invention, so that the particle diameter of micrograde polymer microsphere of the present invention is controlled, can form monodispersed polymer microballoon; In addition, the specific refractory power of micrograde polymer microsphere of the present invention can suitably be regulated by the content of monomer and linking agent, thereby but Effective Raise adopts the transmittance of the light diffusing sheet of this micrograde polymer microsphere.Simultaneously, in the micrograde polymer microsphere preparation process provided by the invention, because the low automatically precipitation of the solubleness of oligopolymer in acetonitrile, and need not to adopt stablizer or suspension agent, technique is simplified greatly.Adopt the light diffusing sheet of micrograde polymer microsphere provided by the invention, guaranteeing that mist degree is under the prerequisite of 97.0-99%, its transmittance reaches more than 80%.
Embodiment
Among the present invention, described " functionality " refers to the number of functional group, and described polyfunctionality refers to that the number of described functional group is more than two.
The invention provides a kind of micrograde polymer microsphere, described micrograde polymer microsphere is the multipolymer of monomer and linking agent; Described monomer is selected from vinylbenzene and/or divinylbenzene, and described linking agent is polyfunctional acrylic ester; The mol ratio of monomer and linking agent is 5-50:50-95.
Micrograde polymer microsphere provided by the invention is suitably selected by kind and consumption to monomer and linking agent, on the one hand so that the particle diameter of micrograde polymer microsphere of the present invention is controlled, can form monodispersed polymer microballoon; On the other hand, by the synergy of benzene ring structure unit and acrylate structural unit, regulate the specific refractory power of described micrograde polymer microsphere in suitable scope, thereby so that adopt the light diffusing sheet of micrograde polymer microsphere to have higher transmittance.Particularly, among the present invention, described monomer is vinylbenzene and/or divinylbenzene, and described linking agent is polyfunctional acrylic ester; The mol ratio of monomer and linking agent is 5-50:50-95.
Under the preferable case, described polyfunctional acrylic ester is selected from one or more in ethylene glycol dimethacrylate (EGDMA), trimethylolpropane trimethacrylate (TMPTMA), pentaerythritol triacrylate (PETRA), tetramethylol methane tetraacrylate (PETEA), ethoxylated trimethylolpropane triacrylate (EO-TMPTA), propoxylation Viscoat 295 (PO-TMPTA), propoxylation triglycerin three propylenes (PO-GLYTA), the double pentaerythritol C5 methacrylate (DPEPA).
The median size of micrograde polymer microsphere of the present invention is 0.1-8 μ m.
The present invention also provides the preparation method of described micrograde polymer microsphere, comprises first monomer and linking agent are dissolved in the acetonitrile in proportion, adds initiator and carries out copolyreaction, and drying obtains described micrograde polymer microsphere.
Micrograde polymer microsphere provided by the invention, suitably select by kind and consumption to monomer and linking agent, make it that preliminary polymerization occur in acetonitrile solvent, generate oligopolymer and from acetonitrile, be precipitated out to be suspended in and form micelle in the acetonitrile, micelle continues to absorb monomer, initiator and linking agent, carry out further crosslinking polymerization, particle diameter increases gradually and forms micron-sized polymkeric substance, namely obtain micrograde polymer microsphere of the present invention, so that the particle diameter of micrograde polymer microsphere of the present invention is controlled, can form monodispersed polymer microballoon.Simultaneously, in the micrograde polymer microsphere preparation process provided by the invention, because the low automatically precipitation of the solubleness of oligopolymer in acetonitrile, and need not to adopt stablizer or suspension agent, technique is simplified greatly.
Among the present invention, described copolyreaction is carried out in solvent, and described solvent is acetonitrile.The present inventor finds by great many of experiments, if adopt other all kinds of SOLVENTS commonly used in the prior art for example when alcohols, ketone among the present invention, the particle diameter of resulting polymer microballoon is uncontrollable, can not obtain monodispersed polymer microballoon; Although the particle diameter control to microballoon behind the dispersion agent of commonly using in the adding prior art plays a role, this dispersion agent was difficult to remove in the later stage, and product transmittance and mist degree can reduce.
Under the preferable case, take the acetonitrile of 100 weight parts as benchmark, the total mass of monomer and linking agent is the 1-30 weight part.More preferably in the situation, take the acetonitrile of 100 weight parts as benchmark, the total mass of monomer and linking agent is the 3-10 weight part.
Among the present invention, the polyreaction of described monomer and linking agent is carried out in the presence of initiator, i.e. copolyreaction of the present invention is free radicals copolymerization reaction.Wherein, initiator is used for providing free radical, thereby makes C=C and the C=C in the linking agent in the monomer that crosslinking polymerization occur, and particle diameter increases gradually in the crosslinking polymerization process, forms described micrograde polymer microsphere.
Described initiator can adopt various initiators commonly used in the prior art, for example, can be azo-initiator or peroxide initiator.Wherein, described azo-initiator is oil-soluble initiator, can be selected from Diisopropyl azodicarboxylate (AIBN), 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN), 2,2'-Azobis(2,4-dimethylvaleronitrile) (AMBN), the azo-bis-iso-dimethyl (AIBME) one or more.The kind of described peroxide initiator is conventionally known to one of skill in the art, for example can adopt in benzoyl peroxide (BPO), peroxidized t-butyl perbenzoate (TBPB), the di-tert-butyl hydrogen peroxide (DTBP) one or more.The content of described initiator need not too much, and enough trigger monomers and linking agent reaction get final product.Under the preferable case, take the total mass of monomer and linking agent as benchmark, the consumption of initiator is 0.5-5%.
Described copolyreaction is Raolical polymerizable, and reaction conditions comprises: temperature is 50-140 ℃, and the time is 3-12h.
As a kind of preferred implementation of the present invention, described copolyreaction is carried out under inert atmosphere, can effectively prevent the initiator inactivation.The gas that described inert atmosphere adopts can be selected from various rare gas elementes or the nitrogen that those skilled in the art commonly use.Wherein, rare gas element is various gases corresponding to periodic table of elements neutral element.
At last, the invention provides a kind of light diffusing sheet, described light diffusing sheet comprises resin base material and the light diffusing agent that is scattered in the resin base material, and described light diffusing agent is micrograde polymer microsphere provided by the invention.
Described resin base material can adopt those skilled in the art's various resins commonly used, for example can be polycarbonate (PC) or polystyrene resin.The content proportioning of described resin base material and light diffusing agent in the prior art content range all can, the present invention does not have particular determination.For example, take the resin base material of 100 weight parts as benchmark, the content of light diffusing agent is the 0.5-5 weight part.
As those skilled in the art's common practise, also can also have various auxiliary agents according to the processing needs in the described light diffusing sheet, described auxiliary agent is scattered in the resin base material.Described auxiliary agent is selected from least a in oxidation inhibitor, fire retardant, the whitening agent.
Wherein, oxidation inhibitor can adopt various oxidation inhibitor common in the prior art or its mixture.For example, described oxidation inhibitor can adopt phosphite ester kind antioxidant, for example can be selected from two [2-methyl-4,6-two (1,1 '-dimethyl ethyl) phenol] phosphoric acid ethyl ester (Irgafos 38), 2,2', 2 " nitrilo triethyl-three [3; 3'; 5; 5'-tetra-tert-1; 1'-phenylbenzene-2; 2'-two bases] phosphorous acid ester (Irgafos 12), [three (nonyl phenyl) phosphorous acid ester] (Irgafos TNPP), [four (2,4-di-tert-butyl-phenyl-4,4'-xenyl) bisphosphonate] (Irgafos PEPQ), three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester (Irgafos 168), [two (octadecyl) pentaerythritol diphosphites] (Weston 618), [two diphosphorous acid two (2, the 4-tert-butyl-phenyl) esters of tetramethylolmethane] (Ultranox 626).Described oxidation inhibitor also can adopt the monothioester kind antioxidant of vapour Bagong department, for example can be selected from 3,3 '-propane thioic acid bay alcohol ester (Irganox PS 800), 3, the hard ester alcohol ester of 3 '-propane thioic acid (Irganox PS 802), Cytec company 3, the two tetradecyl alcohol esters (Cyanox MTDP) of 3 '-thio-2 acid, perhaps be selected from 3 of two key companies, the Hostanox SE-10 of 3 '-propane thioic acid ficocerylic acid ester (CHINOX S1600) and β-dodecyl propane thioic acid pentaerythritol ester (CHINOX S4P), Clariant company.Take the resin base material of 100 weight parts as benchmark, the consumption of oxidation inhibitor is 0.01-1%, is preferably 0.02-0.5%.
Fire retardant can adopt the fluorine flame retardant, for example can adopt FR7080.The fluorine flame retardant has advantages of that addition is little, flame retarding efficiency is high and does not affect transmittance.Take the resin base material of 100 weight parts as benchmark, the fire retardant addition is 0.01%～1%.
Whitening agent can be selected from OB, one or more among KSB, KSN and the KCB.Described whitening agent adds and too much can cause light diffusing sheet to be easy to xanthochromia, if very little then do not have the effect that brightens.Under the preferable case, take the resin base material of 100 weight parts as benchmark, the consumption of whitening agent is 0.1-1%, more preferably 0.2-0.5%.
The preparation method of light diffusing sheet provided by the invention can adopt common method of the prior art, for example the mixture that contains resin base material, light diffusing agent, contains or do not contain auxiliary agent can be mixed the general injection grade of rear employing injection molded.Shot size is selected according to actual needs, and the present invention does not have particular determination.Adopt the light diffusing sheet of micrograde polymer microsphere provided by the invention, guaranteeing that mist degree is under the prerequisite of 97.0-99%, its transmittance reaches more than 80%.
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearer, below in conjunction with embodiment, the present invention is further elaborated.The raw material that adopts all is commercially available in embodiment and the Comparative Examples.
Embodiment 1
(1) with 0.2g vinylbenzene (MW=104.15gmol
-1) and 3g linking agent TMPTMA (MW=338.4 gmol
-1) be dissolved in the 100mL acetonitrile, the mol ratio of monomer styrene and linking agent is 17.8:82.2; Add again 0.063g initiator A IBN, pass into N
2Then deoxygenation 10min is heated to system 70 ℃ and carries out copolyreaction, and the reaction times is 8h; After reaction is finished, filter, vacuum-drying 24h, obtain the micrograde polymer microsphere S1 of the present embodiment.
(2) above-mentioned micrograde polymer microsphere S1,100 weight part polycarbonates, the oxidation inhibitor PEPQ of 0.15 weight part and the fire retardant FR 7080 of 0.01 weight part fluorescent whitening agent OB and 0.08 weight part with 1 weight part adopts high-speed mixer to mix, then be extruded into the light diffusing sheet that thickness is 1.5mm with three roller forcing machines, be designated as S11.
Embodiment 2
Adopt the step identical with embodiment 1 to prepare the micrograde polymer microsphere S2 of the present embodiment and the light diffusing sheet S22 that thickness is 1.5mm, difference is:
In the step (1), monomer: 0.2g vinylbenzene, linking agent: 12.35g EGDMA, the mol ratio of monomer and linking agent is 5:95.
Embodiment 3
Adopt the step identical with embodiment 1 to prepare the micrograde polymer microsphere S3 of the present embodiment and the light diffusing sheet S33 that thickness is 1.5mm, difference is:
In the step (1), monomer: 0.3g divinylbenzene (MW=130.19gmol
-1), linking agent: 1.21g PETRA (MW=524.52gmol
-1), the mol ratio of monomer and linking agent is 50:50.
Embodiment 4
Adopt the step identical with embodiment 1 to prepare the micrograde polymer microsphere S4 of the present embodiment and the light diffusing sheet S44 that thickness is 1.5mm, difference is:
In the step (1), monomer: 0.2g vinylbenzene and 0.1g divinylbenzene, linking agent: 8.19g PETRA, the mol ratio of monomer and linking agent is 10:90.
Embodiment 5
Adopt the step identical with embodiment 1 to prepare the micrograde polymer microsphere S5 of the present embodiment and the light diffusing sheet S55 that thickness is 1.5mm, difference is:
In the step (1), the consumption of acetonitrile is 100mL, and initiator is 0.063g BPO.
Embodiment 6
Adopt the step identical with embodiment 1 to prepare the micrograde polymer microsphere S6 of the present embodiment and the light diffusing sheet S66 that thickness is 1.5mm, difference is:
In the step (1), the copolyreaction temperature is 140 ℃, and the time is 8h.
Embodiment 7
Micrograde polymer microsphere S1 among employing and the embodiment 1 prepares the light diffusing sheet S77 of the present embodiment, difference is: adopt high-speed mixer to mix micrograde polymer microsphere S1,100 weight part polycarbonates, the oxidation inhibitor PEPQ of 0.15 weight part and the fire retardant FR 7080 of 0.01 weight part fluorescent whitening agent OB and 0.08 weight part of 1.5 weight parts, then be extruded into the light diffusing sheet of 1.5mm with three roller forcing machines, be designated as S77.
Comparative Examples 1
Adopt the step identical with embodiment 1 to prepare micrograde polymer microsphere DS1 and the light diffusing sheet DS11 of the present embodiment, difference is:
In the step (1), adopt the acetonitrile among the ethanol replacement embodiment 1.
Comparative Examples 2
Adopt the step identical with embodiment 1 to prepare micrograde polymer microsphere DS2 and the light diffusing sheet DS22 of the present embodiment, difference is:
In the step (1), monomer: 0.2g vinylbenzene, linking agent: 0.42g TMPTMA, the mol ratio of monomer and linking agent is 60:40.
Comparative Examples 3
Disclosed method prepares polymer microballoon DS3 and the light diffusing sheet DS33 of this Comparative Examples among the employing CN101331153A embodiment 1.
Performance test:
1, polymer microballoon median size test:
Polymer microballoon sample S1-S6 and DS1-DS3 are scattered in respectively in the dehydrated alcohol, measure respectively the median size of each sample with static laser light scattering, the laser particle instrument that adopts is the BI-200SM that Brooker Hai Wen instrument company produces.
2, light diffusing sheet mist degree and transmittance test:
The WGT-S of Nereid section transmittance mist degree determinator is tested light diffusing sheet sample S11-S77 and DS11-DS33 in the employing.
Test result is as shown in table 1.
Table 1
| The microballoon sample | Median size (μ m) | The light diffusing sheet sample | Mist degree (%) | Transmittance (%) |
| S1 | 5.0 | S11 | 98 | 81 |
| S2 | 6.5 | S22 | 97 | 82 |
| S3 | 2.5 | S33 | 99 | 85 |
| S4 | 0.8 | S44 | 99 | 87 |
| S5 | 4.0 | S55 | 98.5 | 83 |
| S6 | 2.3 | S66 | 99 | 85 |
| - | - | S77 | 99 | 80 |
| DS1 | 0.05 | DS11 | 3 | 88 |
| DS2 | 4.0 | DS22 | 60 | 84 |
| DS3 | 330 | DS33 | 40 | 79 |
By the test result of upper table 1 as can be known, adopting the median size of the polymer microballoon that method provided by the invention makes is 0.8-6.5 μ m.Simultaneously, adopt the light diffusing sheet of this micrograde polymer microsphere to have higher transmittance and mist degree, obviously be better than each sample in the Comparative Examples.
Relatively can find out with the test result of Comparative Examples 1-2 from embodiment 1, among the present invention, described monomer and linking agent need just can make micrograde polymer microsphere in content range of the present invention, and the solvent that adopts in the described micrograde polymer microsphere of preparation among simultaneously the present invention is acetonitrile.
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (13)
1. a micrograde polymer microsphere is characterized in that, described micrograde polymer microsphere is the multipolymer of monomer and linking agent; Described monomer is selected from vinylbenzene and/or divinylbenzene, and described linking agent is polyfunctional acrylic ester; The mol ratio of monomer and linking agent is 5-50:50-95.
2. micrograde polymer microsphere according to claim 1, it is characterized in that, described polyfunctional acrylic ester is selected from one or more in ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, pentaerythritol triacrylate, tetramethylol methane tetraacrylate, ethoxylated trimethylolpropane triacrylate, propoxylation Viscoat 295, propoxylation triglycerin three propylenes, the double pentaerythritol C5 methacrylate.
3. micrograde polymer microsphere according to claim 1 is characterized in that, the median size of described micrograde polymer microsphere is 0.1-8 μ m.
4. the preparation method of micrograde polymer microsphere claimed in claim 1 is characterized in that, comprises first monomer and linking agent are dissolved in the acetonitrile in proportion, adds initiator and carries out copolyreaction, and drying obtains described micrograde polymer microsphere.
5. preparation method according to claim 4 is characterized in that, take the acetonitrile of 100 weight parts as benchmark, the total mass of monomer and linking agent is the 1-30 weight part.
6. preparation method according to claim 4 is characterized in that, take the total mass of monomer and linking agent as benchmark, the consumption of initiator is 0.5-5%.
7. according to claim 4 or 6 described preparation methods, it is characterized in that, described initiator is azo-initiator or peroxide initiator; Described azo-initiator is selected from one or more of Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-iso-dimethyl, and described peroxide initiator is selected from one or more in benzoyl peroxide, peroxidized t-butyl perbenzoate, the di-tert-butyl hydrogen peroxide.
8. preparation method according to claim 4 is characterized in that, the condition of copolyreaction comprises: temperature is 50-140 ℃, and the time is 3-12h.
9. preparation method according to claim 4 is characterized in that, described copolyreaction is carried out under inert atmosphere.
10. light diffusing sheet, described light diffusing sheet comprise resin base material and be scattered in light diffusing agent in the resin base material, and it is characterized in that, described light diffusing agent is each described micrograde polymer microsphere of claim 1-3.
11. light diffusing sheet according to claim 10, described resin base material are polycarbonate or polystyrene resin.
12. light diffusing sheet according to claim 10, take the resin base material of 100 weight parts as benchmark, the content of light diffusing agent is the 0.5-5 weight part.
13. according to claim 10 or 12 described light diffusing sheets, described light diffusing sheet also comprises the auxiliary agent that is scattered in the resin base material; Described auxiliary agent is selected from least a in oxidation inhibitor, fire retardant, the whitening agent.
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