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WO2016190560A1 - Light diffusing powder and preparation method therefor - Google Patents

Light diffusing powder and preparation method therefor Download PDF

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Publication number
WO2016190560A1
WO2016190560A1 PCT/KR2016/004602 KR2016004602W WO2016190560A1 WO 2016190560 A1 WO2016190560 A1 WO 2016190560A1 KR 2016004602 W KR2016004602 W KR 2016004602W WO 2016190560 A1 WO2016190560 A1 WO 2016190560A1
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WO
WIPO (PCT)
Prior art keywords
light
powder
light diffusing
polyorganosilsesquioxane
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/KR2016/004602
Other languages
French (fr)
Korean (ko)
Inventor
김주성
김현유
이지영
이윤규
주정규
진영섭
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Lotte Advanced Materials Co Ltd
Original Assignee
Lotte Advanced Materials Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Lotte Advanced Materials Co Ltd filed Critical Lotte Advanced Materials Co Ltd
Priority to JP2017557131A priority Critical patent/JP2018517017A/en
Priority to CN201680031294.1A priority patent/CN107667142B/en
Publication of WO2016190560A1 publication Critical patent/WO2016190560A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L25/00Compositions of, homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Compositions of derivatives of such polymers
    • C08L25/02Homopolymers or copolymers of hydrocarbons
    • C08L25/04Homopolymers or copolymers of styrene
    • C08L25/06Polystyrene
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • C08L83/06Polysiloxanes containing silicon bound to oxygen-containing groups
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/02Diffusing elements; Afocal elements

Definitions

  • the present invention relates to a light diffusing powder and a method of manufacturing the same. More specifically, the present invention relates to a light diffusing powder applied to a light diffusing plate and a manufacturing method thereof.
  • Silicone-based fine particles such as silica and polyorganosilsesquioxane generally have excellent compatibility with various polymer resins and organic materials, and are used as additives for paints, plastics, rubbers, papers, coating liquids, and active agents to improve driving stability of high-definition video tapes. It is used in various ways.
  • the polyorganosilsesquioxane particles have a three-dimensional network structure, but have excellent fluidity and compatibility with resins and have an optically low refractive index. It has been spotlighted as an apparatus backlight, a (light) diffuser of a light diffusion plate, an additive of a light guide plate, and the like.
  • Such polyorganosilsesquioxane particles are variously produced by a sol-gel method comprising a hydrolysis reaction and a condensation reaction mechanism using a methyltrialkoxysilane monomer as in the method disclosed in JP-A-2000-186148.
  • the powdered polyorgano silsesquioxane particles are first prepared from a thermoplastic resin such as styrene resin and a master batch composition.
  • a method of manufacturing a light diffusion plate by mixing and extruding it with a separate thermoplastic resin is used.
  • the polyorganosilsesquioxane fine particles having a particle diameter of about 0.5 ⁇ m or less may be mostly lost in the powdering process (dehydration process, etc.) of the polyorganosilsesquioxane particles, and the method powders the diffusing agent, There is a problem that the process is complicated, such as to prepare a master batch composition containing a high concentration thereof.
  • the present inventors have minimized the loss of polyorganosilsesquioxane particles having a particle diameter of about 0.5 ⁇ m or less, to prepare a light diffusion powder capable of realizing excellent light diffusibility and brightness, and to simplify process to improve processability. It is early to develop the invention.
  • the problem to be solved by the present invention is to provide a light diffusion powder capable of realizing excellent light diffusion and brightness.
  • Another object of the present invention is to provide a method for producing a light-diffusion powder capable of minimizing the loss of polyorganosilsesquioxane particles having a particle diameter of about 0.5 ⁇ m or less.
  • Another problem to be solved by the present invention is to provide a method for producing a light-diffusion powder excellent in economics and fairness.
  • Another object of the present invention is to provide a light diffusion plate to which the light diffusion powder is applied.
  • the light diffusion powder is a polystyrene resin; And polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 ⁇ m.
  • the polyorganosilsesquioxane particles may be included in about 0.1 to about 45 parts by weight based on about 100 parts by weight of the polystyrene-based resin.
  • the polystyrene-based resin may be a continuous phase, and the polyorganosilsesquioxane particles may be a dispersed phase.
  • the polyorganosilsesquioxane particles may comprise from about 30 to about 99.9% by weight of the total polyorganosilsesquioxane particles of the fine particles having a particle diameter of about 0.05 to about 0.5 ⁇ m.
  • the light diffusing powder may have a spherical shape having a particle diameter of about 0.01 to about 10 mm or a granule shape having a long diameter of about 0.01 to about 10 mm.
  • the light diffusion powder may further include a light stabilizer.
  • the light stabilizer may include one or more of benzotriazole-based compound and triazine-based compound.
  • the light stabilizer is a dispersed phase and may be included in an amount of about 0.1 to about 45 parts by weight based on about 100 parts by weight of the polystyrene resin.
  • the preparation method includes mixing a styrene monomer with a polymerization solution (suspension) containing polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 ⁇ m; And polymerizing the styrene-based monomer to prepare a light diffusion powder, wherein the light diffusion powder comprises the polyorganosilsesquioxane particles and the polystyrene resin.
  • a polymerization solution suspension
  • D50 average particle diameter
  • the polyorganosilsesquioxane polymer solution may be prepared by hydrolysis and condensation of an organoalkoxy silane through a sol-gel process.
  • an optical stabilizer may be further added when the polyorganosilsesquioxane polymer solution and a styrene monomer are mixed.
  • dewatering the light diffusing powder may further comprise the step of drying the dehydrated light diffusion powder.
  • the light diffusion powder may be about 5% by weight or less after dehydration.
  • Another aspect of the invention relates to a light diffusion plate manufactured using the light diffusion powder.
  • the present invention can minimize the loss of the light-diffusion powder that can implement excellent light diffusivity and brightness, the polyorganosilsesquioxane fine particles having a particle diameter of about 0.5 ⁇ m or less, and the manufacturing method of the light-diffusion powder with excellent economic efficiency and processability It has the effect of providing the light diffusion plate to which the light diffusion powder is applied.
  • Light diffusion powder according to the present invention is a polystyrene resin; And polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 ⁇ m.
  • the polystyrene resin used in the present invention can be used without limitation the polystyrene resin used in a conventional light diffusion plate, it can be obtained by polymerizing a styrene monomer through a known polymerization method.
  • the styrene monomers include styrene, ⁇ -methylstyrene, ⁇ -methylstyrene, p-methylstyrene, pt-butylstyrene, ethylstyrene, vinylxylene, monochlorostyrene, dichlorostyrene, dibromostyrene, Vinyl naphthalene may be used, but is not limited thereto. These may be applied alone or in mixture of two or more.
  • the polystyrene-based resin may form a continuous phase (matrix) of the light diffusion powder.
  • grains mentioned later, and the said styrene monomer, and polymerizing a styrene-type monomer the said polyorgano silsesquioxane particle (dispersed phase ) can be obtained a polystyrene resin (continuous phase) is dispersed.
  • the polystyrene-based resin may have a weight average molecular weight of about 5,000 to about 50,000 g / mol, for example, about 5,000 to about 30,000 g / mol, measured using gel permeation chromatography (GPC).
  • the polyorgano silses quoxane particles (dispersed phase) may be evenly dispersed in the polystyrene resin (continuous phase) polymerized in the above range, and during diffusion plate extrusion, the light diffusion powder may be evenly distributed and distributed in the matrix.
  • the polyorganosilsesquioxane particles used in the present invention may act as a light diffusing agent, and the average particle diameter (D50) measured by laser scattering particle size analysis is about 0.1 to about 0.9 ⁇ m, eg For example, about 0.3 to about 0.6 ⁇ m. If the average particle diameter of the polyorganosilsesquioxane particles is less than about 0.1 ⁇ m, the permeability may increase more than the diffusivity outside the Rayleigh scattering region, and if the average particle diameter exceeds about 0.9 ⁇ m, the diffusivity And a brightness improving effect may not be obtained, and an excessive amount of the light diffusing agent may be used.
  • D50 average particle diameter measured by laser scattering particle size analysis
  • the polyorganosilsesquioxane particles may comprise a repeating unit of the following formula (1).
  • R is an alkyl group having 1 to 6 carbon atoms, a vinyl group or an aryl group, and x has a range of 0 to 1.5.
  • R may be a methyl group, an ethyl group, a phenyl group, etc., and it is preferable from an industrial viewpoint that it is a methyl group.
  • the polyorganosilsesquioxane particles may be prepared by a sol-gel process (hydrolysis and condensation reaction) using organo alkoxy silane as a monomer, but is not limited thereto.
  • the polyorganosilsesquioxane particles may comprise from about 30 to about 99.9 weight percent, such as from about 40 to about 100 weight percent of the total polyorganosilsesquioxane particles, having a particle diameter of about 0.05 to about 0.5 ⁇ m. About 99% by weight. Since the light diffusion efficiency of the polyorganosilsesquioxane particles in the above range can be excellent, and the input amount of the diffusion agent (polyorganosilsesquioxane particles) introduced into the light diffusion plate at the same transmittance can be reduced, manufacturing cost In addition to the reduction in strength, the reduction in strength and crack increase due to the decrease in compatibility between the diffusion agent and the resin can be reduced.
  • the polyorganosilsesquioxane particles can be in the dispersed phase of the light diffusion powder.
  • a form dispersed in a polystyrene resin continuous phase
  • a form dispersed in a polystyrene resin continuous phase
  • the polyorganosilsesquioxane particles may be included from about 0.1 to about 45 parts by weight, for example from about 3 to about 10 parts by weight based on about 100 parts by weight of the polystyrene-based resin.
  • the light diffusion powder may implement excellent diffusion effects and luminance.
  • the light diffusion powder according to the embodiment of the present invention may further include a light stabilizer.
  • the light stabilizer may be a light stabilizer having an absorbance of at least about 0.25 AU, for example from about 0.5 to about 1.0 AU, at a wavelength of about 380 nm for a concentration of about 20 mg / L in toluene.
  • the optical acid powder prepared in the above range can sufficiently absorb light at wavelengths of about 380 to about 390 nm in external light, and can improve external light stability of the display device by lowering transmittance.
  • the light stabilizer may include one or more of benzotriazole-based compound and triazine-based compound, may be used commercially available light stabilizer.
  • light stabilizers such as Tinuvin-770, Tinuvin-P, Tinuvin-477, Tinuvin-326, etc. may be used, but are not limited thereto.
  • the light stabilizer may be in a form (disperse phase) dispersed in the polystyrene-based resin (continuous phase, matrix).
  • the light stabilizer and the polyorganosilsesquioxane suspension to be described later and the styrene monomers are mixed, and then a styrene monomer is polymerized to form the polyorganosilsesquioxane in the polystyrene resin (continuous phase, matrix).
  • a light-diffusion powder in which particles (dispersed phase) and light stabilizer (dispersed phase) are dispersed can be obtained.
  • about 0.1 to about 45 parts by weight for example about 0.5 to about 30 parts by weight, specifically about 1 to about 20 parts by weight, based on about 100 parts by weight of the polystyrene resin.
  • the transmittance of about 1% or less may be secured at a wavelength of about 380 to about 390 nm to increase external light stability, and an excessive amount of light stabilizer may be included to reduce precipitation of white spots.
  • the light diffusing powder according to the embodiment of the present invention has a spherical particle diameter of about 0.01 to about 10 mm, for example, about 0.03 to about 5 mm, specifically about 0.03 to about 1 mm, or a long diameter of about 0.01 to about 10 mm. mm, for example about 0.1 to about 5 mm, specifically about 0.1 to about 1 mm.
  • the ratio of the long diameter and the short diameter may be about 4: about 1 to about 1: about 1, for example, about 2: about 1 to about 1.5: about 1 have.
  • the light diffusion powder may implement excellent diffusion effects and luminance.
  • a polymerization solution (suspension) containing a polyorganosilsesquioxane particle having an average particle diameter (D50) of about 0.1 to about 0.9 ⁇ m is mixed with a styrene monomer. and; And preparing a light diffusion powder by polymerizing the styrene-based monomer.
  • the polyorganosilsesquioxane polymer solution may be prepared by a sol-gel method using an organoalkoxysilane as a monomer. More specifically, the polyorganosilsesquioxane polymerization liquid can be manufactured by hydrolyzing and condensing organotrialkoxysilane in the presence of an acid or a base catalyst in an aqueous phase.
  • the organotrialkoxysilane may be represented by the following formula (2).
  • R is as defined in Chemical Formula 1, and R 1 is an alkyl group having 1 to 5 carbon atoms.
  • R may be a methyl group, an ethyl group, a phenyl group, or the like, and R 1 may be a methyl group, an ethyl group, a propyl group, or a butyl group.
  • R 1 and R 2 are methyl groups.
  • the sol-gel process (hydrolysis and condensation reactions) is commonly known to those skilled in the art.
  • the hydrolysis and condensation reaction may be performed by mixing a monomer containing an organoalkoxysilane with a predetermined solvent, and may further include a catalyst to control the reaction rate.
  • the catalyst may be an acid catalyst such as hydrochloric acid, acetic acid, hydrogen fluoride, nitric acid, sulfuric acid, chlorosulfonic acid and iodic acid; Base catalysts such as ammonia, potassium hydroxide, sodium hydroxide, barium hydroxide and imidazole; And the like can be used.
  • a base catalyst it can be carried out at a pH of about 8.5 to about 13, for example pH about 10 to about 13 conditions.
  • a polyorganosilsesquioxane polymer solution containing polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 ⁇ m may be obtained.
  • the hydrolysis and condensation reaction may be performed at room temperature for about 1 to about 24 hours, and may be performed at about 60 to about 100 ° C. for about 1 to about 8 hours to promote the reaction, but is not limited thereto.
  • the solvent in the hydrolysis and condensation reaction is not particularly limited.
  • water, methanol, ethanol, propanol, isopropanol, n-butanol, tert-butanol, methoxypropanol and the like may be used alone or in combination of two or more thereof.
  • the polyorganosilsesquioxane polymer solution may be used by adding water to facilitate polymerization of the styrene monomer.
  • the weight ratio of the polyorganosilsesquioxane particles and water may be about 0.02: about 1 to about 0.9: about 1, but is not limited thereto.
  • the polyorganosilsesquioxane polymerization liquid (suspension) is mixed with the styrene monomer, and then the styrene monomer is polymerized to form a light diffusion powder having a polyorgano silsesquioxane dispersed in a polystyrene resin. It can manufacture.
  • the step of preparing the conventionally powdered polyorganosilsesquioxane particles from the polystyrene resin and the master batch composition can be omitted. Therefore, the processability can be improved, and the polyorganosilsesquioxane fine particles of about 0.5 ⁇ m or less lost due to powdering can also contribute to the light diffusion effect, thereby ensuring excellent economic efficiency and light diffusion.
  • Polymerization of the styrene monomers is commonly known to those skilled in the art.
  • a known suspension polymerization method can be used. Specifically, a styrene-based monomer and, if necessary, a polymerization initiator, a chain transfer agent, etc. may be added, and this may be added to an aqueous solution in which a dispersion stabilizer or the like is dissolved to perform suspension polymerization.
  • a styrene-based monomer or the like may be added to the polyorganosilsesquioxane suspension and mixed, and suspension polymerization may be performed.
  • the polymerization temperature and the polymerization time can be appropriately adjusted.
  • the reaction may be performed at a polymerization temperature of about 65 to about 125 ° C, specifically about 70 to about 120 ° C for about 1 to about 8 hours, but is not limited thereto.
  • the polymerization initiator may be used a conventional radical polymerization initiator known in the polymerization art, for example, potassium persulfate, octanoyl peroxide, decanyl peroxide, lauroyl peroxide, benzoyl peroxide Monochlorobenzoyl peroxide, dichlorobenzoyl peroxide, p-methylbenzoyl peroxide, tert-butyl perbenzoate, azobisisobutyronitrile and azobis- (2,4-dimethyl) -valeronitrile and the like can be used. May be, but is not limited thereto.
  • the polymerization initiator may be applied alone or by mixing two or more kinds.
  • the polymerization initiator may include about 0.01 to about 10 parts by weight, for example about 0.03 to about 5 parts by weight, based on about 100 parts by weight of the styrene-based polymer, but is not limited thereto.
  • the above-described light stabilizer may be further added when the polyorganosilsesquioxane suspension and the styrene monomer are mixed.
  • a light-diffusion powder in which the polyorganosilsesquioxane particles (dispersed phase) and the light stabilizer (dispersed phase) are dispersed in a polystyrene resin (continuous phase, matrix) prepared from a styrene monomer can be obtained.
  • a dehydration process of the light diffusing powder may be performed.
  • the dewatering process is purified by the centrifugal separator, filter press, vibrating screen (vibrating screen), etc. after the first dewatered sludge after washing with water, about 60 to about 200 °C, for example about 70 to about 90
  • the light-diffusing powder in the form of a white powder may be prepared by drying using a fluidized bed dryer, a spin flash dryer, a vacuum dryer, a convection oven, or the like within a range of ° C.
  • the powdered light diffusing powder may have a water content of about 5% by weight or less, for example, about 3 to about 5% by weight.
  • the light diffusing plate according to the present invention is prepared using the light diffusing powder.
  • the light diffusion powder of the present invention is applied to the light diffusion plate production, it is possible to implement excellent brightness and light diffusion, the light diffusion plate is particularly useful as a diffusion plate used in LCD-TV.
  • the light diffusion plate may include about 100 parts by weight of the thermoplastic resin and about 0.1 to about 10 parts by weight of the light diffusion powder, for example, about 0.5 to about 8 parts by weight. In the above range, the transmittance of the thermoplastic resin may be reduced to be suitable as the diffusion plate, and the luminance, light diffusing property, and light resistance may be excellent.
  • the thermoplastic resin may be a vinyl chloride resin, a polystyrene resin, a styrene-acrylonitrile resin, a polyacrylic resin, an acrylic-styrene resin, a polyester resin, or an ABS resin, which is used in a conventional diffusion plate.
  • Resin or polycarbonate resin can be used without limitation.
  • the method of manufacturing such a light diffusion plate can be easily carried out by those skilled in the art. For example, after mixing the thermoplastic resin and the light diffusing powder and other additives as necessary, melt extrusion in the extruder to produce a pellet form, and various molding such as injection molding, extrusion molding, vacuum molding, casting molding Through the method, it can be manufactured into various light diffusing plates (molded articles).
  • the prepared light-diffusion powder has a weight ratio (PS: PMSQ) of 100: 3.36 of polystyrene resin and polymethylsilsesquioxane particles, and has a spherical particle diameter of 0.1 to 2 mm measured by laser scattering particle size analysis. And a granule shape having a long diameter of 0.5 to 5 mm.
  • a flat plate specimen was manufactured in the same manner as in Example 1, except that 30 parts by weight of the light diffusing powder of Preparation Example 1 was used. The transmittance and the haze were measured, and the results are shown in Table 1 below.
  • a flat plate specimen was manufactured in the same manner as in Example 1, except that 40 parts by weight of the light diffusing powder of Preparation Example 1 was used. The transmittance and the haze were measured, and the results are shown in Table 1 below.
  • Transmittance (TT) (unit:%): It measured using the haze meter (NDH 5000W, Nippon Denshi Kogyo Co., Ltd.).
  • Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Polystyrene resin 100 100 100 100 100 100 Light Diffusion Powder 24.5 30 40 - - Masterbatch composition - - - 15 20 PMSQ Particle Average Particle Size (D50) 0.3 ⁇ m 0.3 ⁇ m 0.3 ⁇ m 1 ⁇ m 1 ⁇ m PMSQ Particle Content in Specimens (wt%) 0.796 0.975 1.3 1.5 2.0 Transmittance (%) 61.1 62.1 61.1 64.57 60.1 Haze (%) 92.1 92.8 91.8 91.2 86.4
  • the specimen using the light-diffusion powder of the present invention including the polymethylsilsesquioxane particles having an average particle diameter of 0.3 ⁇ m, even if containing a small amount of 1.3% by weight, the diffusion performance is excellent Able to know.
  • Comparative Examples 1 and 2 using polyorganosilsesquioxane particles having an average particle diameter (D50) of 1.0 ⁇ m exhibited low diffusion performance due to high transmittance or low haze, even when an excessive amount was used. Able to know.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)
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Abstract

A light diffusing powder of the present invention comprises: a polystyrene-based resin; and polyorganosilsesquioxane particles having an average diameter (D50) of approximately 0.1-0.9 μm. The light diffusing powder has an excellent light diffusion property and brightness, and a preparation method therefor reduces the loss of polyorganosilsesquioxane microparticles of approximately 0.5 μm or less and has excellent economic efficiency and processability.

Description

광확산 파우더 및 그 제조방법Light Diffusion Powder and Manufacturing Method Thereof

본 발명은 광확산 파우더 및 그 제조방법에 관한 것이다. 보다 구체적으로 본 발명은 광확산판에 적용되는 광확산 파우더 및 그 제조방법에 관한 것이다.The present invention relates to a light diffusing powder and a method of manufacturing the same. More specifically, the present invention relates to a light diffusing powder applied to a light diffusing plate and a manufacturing method thereof.

실리카 및 폴리오가노실세스퀴옥산과 같은 실리콘계 미립자는 일반적으로 각종 고분자 수지 및 유기물과의 상용성이 뛰어나 도료, 플라스틱, 고무, 종이, 코팅액의 첨가제 및 고화질 비디오 테이프의 주행안정성을 높이기 위한 활성제 등으로 다양하게 사용되고 있다.Silicone-based fine particles such as silica and polyorganosilsesquioxane generally have excellent compatibility with various polymer resins and organic materials, and are used as additives for paints, plastics, rubbers, papers, coating liquids, and active agents to improve driving stability of high-definition video tapes. It is used in various ways.

특히, 폴리오가노실세스퀴옥산 입자는 분자구조가 3차원의 망상구조로 되어 있으면서도 수지와의 유동성 및 상용성이 우수하고 광학적으로 낮은 굴절률을 가지고 있는 등 많은 특성 때문에, 조명 커버, 간판, 액정표시장치 백라이트, 광확산판의 (광)확산제, 도광판의 첨가제 등으로 각광 받고 있다.Particularly, the polyorganosilsesquioxane particles have a three-dimensional network structure, but have excellent fluidity and compatibility with resins and have an optically low refractive index. It has been spotlighted as an apparatus backlight, a (light) diffuser of a light diffusion plate, an additive of a light guide plate, and the like.

이러한 폴리오가노실세스퀴옥산 입자는 일본특허공개 제2000-186148호 등에 나타난 방법과 같이 메틸트리알콕시실란 단량체를 이용하여 가수분해반응과 축합반응 메카니즘으로 이루어지는 졸-겔법 등에 의해 다양하게 제조되고 있다.Such polyorganosilsesquioxane particles are variously produced by a sol-gel method comprising a hydrolysis reaction and a condensation reaction mechanism using a methyltrialkoxysilane monomer as in the method disclosed in JP-A-2000-186148.

또한, 기존에는 폴리오가노실세스퀴옥산 입자를 확산제로서 광확산판에 적용하기 위하여, 분체화된 폴리오가노실세스퀴옥산 입자를 스티렌계 수지 등의 열가소성 수지와 마스터 배치 조성물로 먼저 제조한 후, 이를 별도의 열가소성 수지와 다시 혼합하고 압출하여 광확산판을 제조하는 방법이 사용되고 있다. 그러나, 입경 약 0.5 ㎛ 이하의 폴리오가노실세스퀴옥산 미립자는 폴리오가노실세스퀴옥산 입자의 분체화 공정(탈수 공정 등)에서 대부분 손실될 우려가 있으며, 상기 방법은 확산제를 분체화하고, 이를 고농도로 포함하는 마스터 배치 조성물을 제조해야 하는 등 공정이 복잡하다는 문제점이 있다.In addition, in order to apply the polyorgano silsesquioxane particles to the light diffusion plate as a diffusing agent, the powdered polyorgano silsesquioxane particles are first prepared from a thermoplastic resin such as styrene resin and a master batch composition. In addition, a method of manufacturing a light diffusion plate by mixing and extruding it with a separate thermoplastic resin is used. However, the polyorganosilsesquioxane fine particles having a particle diameter of about 0.5 μm or less may be mostly lost in the powdering process (dehydration process, etc.) of the polyorganosilsesquioxane particles, and the method powders the diffusing agent, There is a problem that the process is complicated, such as to prepare a master batch composition containing a high concentration thereof.

이에 본 발명자들은 입경 약 0.5 ㎛ 이하의 폴리오가노실세스퀴옥산 미립자의 손실을 최소화하여, 우수한 광확산성 및 휘도를 구현할 수 있는 광확산 파우더를 제조하고, 복잡한 공정을 단순화시켜 공정성을 개선하고자 본 발명을 개발하기에 이른 것이다.Accordingly, the present inventors have minimized the loss of polyorganosilsesquioxane particles having a particle diameter of about 0.5 μm or less, to prepare a light diffusion powder capable of realizing excellent light diffusibility and brightness, and to simplify process to improve processability. It is early to develop the invention.

본 발명이 해결하고자 하는 과제는 우수한 광확산성 및 휘도를 구현할 수 있는 광확산 파우더를 제공하기 위한 것이다.The problem to be solved by the present invention is to provide a light diffusion powder capable of realizing excellent light diffusion and brightness.

본 발명이 해결하고자 하는 다른 과제는 입경 약 0.5 ㎛ 이하인 폴리오가노실세스퀴옥산 미립자의 손실을 최소화할 수 있는 광확산 파우더의 제조방법을 제공하기 위한 것이다.Another object of the present invention is to provide a method for producing a light-diffusion powder capable of minimizing the loss of polyorganosilsesquioxane particles having a particle diameter of about 0.5 μm or less.

본 발명이 해결하고자 하는 또 다른 과제는 경제성 및 공정성이 뛰어난 광확산 파우더의 제조방법을 제공하기 위한 것이다.Another problem to be solved by the present invention is to provide a method for producing a light-diffusion powder excellent in economics and fairness.

본 발명이 해결하고자 하는 또 다른 과제는 상기 광확산 파우더를 적용한 광확산판을 제공하기 위한 것이다.Another object of the present invention is to provide a light diffusion plate to which the light diffusion powder is applied.

본 발명의 상기 및 기타의 목적들은 하기 설명되는 본 발명에 의하여 모두 달성될 수 있다.The above and other objects of the present invention can be achieved by the present invention described below.

본 발명의 하나의 관점은 광학산 파우더에 관한 것이다. 상기 광확산 파우더는 폴리스티렌계 수지; 및 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛인 폴리오가노실세스퀴옥산 입자를 포함하는 것을 특징으로 한다.One aspect of the invention relates to optical acid powder. The light diffusion powder is a polystyrene resin; And polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 μm.

구체예에서, 상기 폴리오가노실세스퀴옥산 입자는 상기 폴리스티렌계 수지 약 100 중량부에 대하여 약 0.1 내지 약 45 중량부로 포함될 수 있다.In embodiments, the polyorganosilsesquioxane particles may be included in about 0.1 to about 45 parts by weight based on about 100 parts by weight of the polystyrene-based resin.

구체예에서, 상기 폴리스티렌계 수지는 연속상이고, 상기 폴리오가노실세스퀴옥산 입자는 분산상일 수 있다.In an embodiment, the polystyrene-based resin may be a continuous phase, and the polyorganosilsesquioxane particles may be a dispersed phase.

구체예에서, 상기 폴리오가노실세스퀴옥산 입자는 입경이 약 0.05 내지 약 0.5 ㎛인 미립자를 전체 폴리오가노실세스퀴옥산 입자 100 중량% 중 약 30 내지 약 99.9 중량%로 포함할 수 있다.In embodiments, the polyorganosilsesquioxane particles may comprise from about 30 to about 99.9% by weight of the total polyorganosilsesquioxane particles of the fine particles having a particle diameter of about 0.05 to about 0.5 ㎛.

구체예에서, 상기 광확산 파우더는 입경이 약 0.01 내지 약 10 mm인 구형이거나, 장경이 약 0.01 내지 약 10 mm인 그래뉼 형상일 수 있다.In embodiments, the light diffusing powder may have a spherical shape having a particle diameter of about 0.01 to about 10 mm or a granule shape having a long diameter of about 0.01 to about 10 mm.

구체예에서, 상기 광확산 파우더는 광안정제를 더 포함할 수 있다.In embodiments, the light diffusion powder may further include a light stabilizer.

구체예에서, 상기 광안정제는 벤조트리아졸계 화합물 및 트리아진계 화합물 중 1종 이상을 포함할 수 있다.In embodiments, the light stabilizer may include one or more of benzotriazole-based compound and triazine-based compound.

구체예에서, 상기 광안정제는 분산상이고, 상기 폴리스티렌계 수지 약 100 중량부에 대하여 약 0.1 내지 약 45 중량부로 포함될 수 있다.In some embodiments, the light stabilizer is a dispersed phase and may be included in an amount of about 0.1 to about 45 parts by weight based on about 100 parts by weight of the polystyrene resin.

본 발명의 다른 관점은 광확산 파우더의 제조방법에 관한 것이다. 상기 제조방법은 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛인 폴리오가노실세스퀴옥산 입자를 포함하는 중합액(현탁액)과 스티렌계 단량체를 혼합하고; 그리고 상기 스티렌계 단량체를 중합하여 광확산 파우더를 제조하는 단계;를 포함하며, 상기 광확산 파우더는 상기 폴리오가노실세스퀴옥산 입자 및 폴리스티렌계 수지를 포함하는 것을 특징으로 한다.Another aspect of the invention relates to a method for producing a light diffusing powder. The preparation method includes mixing a styrene monomer with a polymerization solution (suspension) containing polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 μm; And polymerizing the styrene-based monomer to prepare a light diffusion powder, wherein the light diffusion powder comprises the polyorganosilsesquioxane particles and the polystyrene resin.

구체예에서, 상기 폴리오가노실세스퀴옥산 중합액은 오가노 알콕시 실란을 졸-겔 공정을 통해 가수분해 및 축합반응시켜 제조하는 것일 수 있다.In an embodiment, the polyorganosilsesquioxane polymer solution may be prepared by hydrolysis and condensation of an organoalkoxy silane through a sol-gel process.

구체예에서, 상기 폴리오가노실세스퀴옥산 중합액과 스티렌계 단량체를 혼합 시 광안정제를 더 첨가할 수 있다.In an embodiment, an optical stabilizer may be further added when the polyorganosilsesquioxane polymer solution and a styrene monomer are mixed.

구체예에서, 상기 광확산 파우더를 탈수하는 단계; 및 상기 탈수된 광확산 파우더를 건조하는 단계를 더 포함할 수 있다.In an embodiment, dewatering the light diffusing powder; And it may further comprise the step of drying the dehydrated light diffusion powder.

구체예에서, 상기 광확산 파우더는 탈수 후, 수분 함량이 약 5 중량% 이하일 수 있다.In embodiments, the light diffusion powder may be about 5% by weight or less after dehydration.

본 발명의 또 다른 관점은 상기 광확산 파우더를 이용하여 제조된 광확산판에 관한 것이다.Another aspect of the invention relates to a light diffusion plate manufactured using the light diffusion powder.

본 발명은 우수한 광확산성 및 휘도를 구현할 수 있는 광확산 파우더, 입경 약 0.5 ㎛ 이하인 폴리오가노실세스퀴옥산 미립자의 손실을 최소화할 수 있고, 경제성 및 공정성이 우수한 광확산 파우더의 제조방법 및 상기 광확산 파우더를 적용한 광확산판을 제공하는 발명의 효과를 가진다.The present invention can minimize the loss of the light-diffusion powder that can implement excellent light diffusivity and brightness, the polyorganosilsesquioxane fine particles having a particle diameter of about 0.5 ㎛ or less, and the manufacturing method of the light-diffusion powder with excellent economic efficiency and processability It has the effect of providing the light diffusion plate to which the light diffusion powder is applied.

이하, 본 발명을 상세히 설명하면, 다음과 같다.Hereinafter, the present invention will be described in detail.

본 발명에 따른 광확산 파우더는 폴리스티렌계 수지; 및 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛인 폴리오가노실세스퀴옥산 입자를 포함하는 것을 특징으로 한다.Light diffusion powder according to the present invention is a polystyrene resin; And polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 μm.

본 발명에 사용되는 폴리스티렌계 수지는 통상의 광확산판에 사용되는 폴리스티렌계 수지를 제한 없이 사용할 수 있으며, 스티렌계 단량체를 공지의 중합방법을 통해 중합하여 얻을 수 있는 것이다.The polystyrene resin used in the present invention can be used without limitation the polystyrene resin used in a conventional light diffusion plate, it can be obtained by polymerizing a styrene monomer through a known polymerization method.

구체예에서, 상기 스티렌계 단량체로는 스티렌, α-메틸스티렌, β-메틸스티렌, p-메틸스티렌, p-t-부틸스티렌, 에틸스티렌, 비닐크실렌, 모노클로로스티렌, 디클로로스티렌, 디브로모스티렌, 비닐나프탈렌 등을 사용할 수 있으나, 이에 제한되는 것은 아니다. 이들은 단독 또는 2종 이상의 혼합물로 적용될 수 있다.In an embodiment, the styrene monomers include styrene, α-methylstyrene, β-methylstyrene, p-methylstyrene, pt-butylstyrene, ethylstyrene, vinylxylene, monochlorostyrene, dichlorostyrene, dibromostyrene, Vinyl naphthalene may be used, but is not limited thereto. These may be applied alone or in mixture of two or more.

구체예에서, 상기 폴리스티렌계 수지는 광확산 파우더의 연속상(매트릭스)을 형성할 수 있다. 예를 들면, 후술될 상기 폴리오가노실세스퀴옥산 입자를 포함하는 폴리오가노실세스퀴옥산 현탁액과 상기 스티렌계 단량체를 혼합 후, 스틸렌계 단량체를 중합함으로써, 상기 폴리오가노실세스퀴옥산 입자(분산상)가 분산된 폴리스티렌계 수지(연속상)를 얻을 수 있다.In an embodiment, the polystyrene-based resin may form a continuous phase (matrix) of the light diffusion powder. For example, after mixing a polyorganosilsesquioxane suspension containing the said polyorgano silsesquioxane particle | grains mentioned later, and the said styrene monomer, and polymerizing a styrene-type monomer, the said polyorgano silsesquioxane particle (dispersed phase ) Can be obtained a polystyrene resin (continuous phase) is dispersed.

구체예에서, 상기 폴리스티렌계 수지는 GPC(gel permeation chromatography)를 사용하여 측정한 중량평균분자량이 약 5,000 내지 약 50,000 g/mol, 예를 들면 약 5,000 내지 약 30,000 g/mol일 수 있다. 상기 범위에서 중합되는 폴리스티렌계 수지(연속상) 내에 폴리오가노 실세스 퀴옥산 입자(분산상)가 고르게 분산될 수 있고, 확산판 압출 시, 광확산 파우더가 매트릭스 내에 고르게 확산 분포될 수 있다.In an embodiment, the polystyrene-based resin may have a weight average molecular weight of about 5,000 to about 50,000 g / mol, for example, about 5,000 to about 30,000 g / mol, measured using gel permeation chromatography (GPC). The polyorgano silses quoxane particles (dispersed phase) may be evenly dispersed in the polystyrene resin (continuous phase) polymerized in the above range, and during diffusion plate extrusion, the light diffusion powder may be evenly distributed and distributed in the matrix.

본 발명에 사용되는 폴리오가노실세스퀴옥산 입자는 광확산제의 역할을 할 수 있는 것으로서, 레이저 스캐터링(laser scattering) 입도 분석법으로 측정한 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛, 예를 들면 약 0.3 내지 약 0.6 ㎛일 수 있다. 상기 폴리오가노실세스퀴옥산 입자의 평균입경이 약 0.1 ㎛ 미만이면, 레일리 산란(Rayleigh scattering) 영역 외로 확산성보다 투과성이 증가할 우려가 있고, 상기 평균입경이 약 0.9 ㎛를 초과하면, 확산성 및 휘도 향상 효과를 얻지 못하고, 광확산제를 과량 사용하여야 할 수 있다.The polyorganosilsesquioxane particles used in the present invention may act as a light diffusing agent, and the average particle diameter (D50) measured by laser scattering particle size analysis is about 0.1 to about 0.9 μm, eg For example, about 0.3 to about 0.6 μm. If the average particle diameter of the polyorganosilsesquioxane particles is less than about 0.1 μm, the permeability may increase more than the diffusivity outside the Rayleigh scattering region, and if the average particle diameter exceeds about 0.9 μm, the diffusivity And a brightness improving effect may not be obtained, and an excessive amount of the light diffusing agent may be used.

구체예에서, 상기 폴리오가노실세스퀴옥산 입자는 하기 화학식 1의 반복단위를 포함할 수 있다.In embodiments, the polyorganosilsesquioxane particles may comprise a repeating unit of the following formula (1).

[화학식 1][Formula 1]

RSiO1.5-x(OH)x RSiO 1.5-x (OH) x

상기 화학식 1에서, R은 탄소수 1 내지 6의 알킬기, 비닐기 또는 아릴기이며, x는 0 내지 1.5의 범위를 갖는다. 예를 들면, R은 메틸기, 에틸기, 페닐기 등일 수 있고, 메틸기인 것이 공업적인 측면에서 바람직하다.In Formula 1, R is an alkyl group having 1 to 6 carbon atoms, a vinyl group or an aryl group, and x has a range of 0 to 1.5. For example, R may be a methyl group, an ethyl group, a phenyl group, etc., and it is preferable from an industrial viewpoint that it is a methyl group.

구체예에서, 상기 폴리오가노실세스퀴옥산 입자는 단량체로서 오가노 알콕시 실란을 이용하여 졸-겔 공정(가수분해 및 축합반응)으로 제조한 것일 수 있으나, 이에 제한되지 않는다.In embodiments, the polyorganosilsesquioxane particles may be prepared by a sol-gel process (hydrolysis and condensation reaction) using organo alkoxy silane as a monomer, but is not limited thereto.

구체예에서, 상기 폴리오가노실세스퀴옥산 입자는 입경이 약 0.05 내지 약 0.5 ㎛인 미립자를 전체 폴리오가노실세스퀴옥산 입자 100 중량% 중 약 30 내지 약 99.9 중량%, 예를 들면 약 40 내지 약 99 중량%로 포함할 수 있다. 상기 범위에서 폴리오가노실세스퀴옥산 입자의 광확산 효율이 우수할 수 있고, 동일 투과도에서 광확산판에 투입되는 확산제(폴리오가노실세스퀴옥산 입자)의 투입량을 감소시킬 수 있으므로, 제조비용을 절감할 수 있을 뿐만 아니라 확산제와 수지와의 상용성 저하에 따른 강도 저하 및 크랙 증가 현상을 감소시킬 수 있다.In embodiments, the polyorganosilsesquioxane particles may comprise from about 30 to about 99.9 weight percent, such as from about 40 to about 100 weight percent of the total polyorganosilsesquioxane particles, having a particle diameter of about 0.05 to about 0.5 μm. About 99% by weight. Since the light diffusion efficiency of the polyorganosilsesquioxane particles in the above range can be excellent, and the input amount of the diffusion agent (polyorganosilsesquioxane particles) introduced into the light diffusion plate at the same transmittance can be reduced, manufacturing cost In addition to the reduction in strength, the reduction in strength and crack increase due to the decrease in compatibility between the diffusion agent and the resin can be reduced.

구체예에서, 상기 폴리오가노실세스퀴옥산 입자는 광확산 파우더의 분산상일 수 있다. 예를 들면, 후술될 폴리오가노실세스퀴옥산 현탁액을 분체화하지 않고, 현탁액 자체를 상기 스티렌계 단량체와 혼합한 후 스티렌계 단량체를 중합함으로써, 폴리스티렌계 수지(연속상)에 분산된 형태(분산상)로 존재할 수 있다.In an embodiment, the polyorganosilsesquioxane particles can be in the dispersed phase of the light diffusion powder. For example, a form dispersed in a polystyrene resin (continuous phase) by mixing the suspension itself with the styrene monomer and then polymerizing the styrene monomer without powdering the polyorganosilsesquioxane suspension described below. May exist.

구체예에서, 상기 폴리오가노실세스퀴옥산 입자는 상기 폴리스티렌계 수지 약 100 중량부에 대하여 약 0.1 내지 약 45 중량부로, 예를 들면 약 3 내지 약 10 중량부로 포함될 수 있다. 상기 범위에서 광확산 파우더가 우수한 확산 효과 및 휘도를 구현할 수 있다.In embodiments, the polyorganosilsesquioxane particles may be included from about 0.1 to about 45 parts by weight, for example from about 3 to about 10 parts by weight based on about 100 parts by weight of the polystyrene-based resin. In the above range, the light diffusion powder may implement excellent diffusion effects and luminance.

본 발명의 일 실시예에 따른 광확산 파우더는 광안정제를 더 포함할 수 있다.The light diffusion powder according to the embodiment of the present invention may further include a light stabilizer.

구체예에서, 상기 광안정제로는 톨루엔 중 약 20 mg/L 농도에 대해 파장 약 380 nm에서 흡광도가 약 0.25 AU 이상, 예를 들면 약 0.5 내지 약 1.0 AU인 광안정제를 사용할 수 있다. 상기 범위에서 제조된 광학산 파우더가 외광 중 파장 약 380 내지 약 390 nm에서의 빛을 충분히 흡수할 수 있으며, 투과율을 낮춤으로써 디스플레이 소자의 외광 안정성을 높일 수 있다.In embodiments, the light stabilizer may be a light stabilizer having an absorbance of at least about 0.25 AU, for example from about 0.5 to about 1.0 AU, at a wavelength of about 380 nm for a concentration of about 20 mg / L in toluene. The optical acid powder prepared in the above range can sufficiently absorb light at wavelengths of about 380 to about 390 nm in external light, and can improve external light stability of the display device by lowering transmittance.

구체예에서, 상기 광안정제는 벤조트리아졸계 화합물 및 트리아진계 화합물 중 1종 이상을 포함할 수 있으며, 상품화된 광안정제를 사용할 수 있다. 구체적으로, Ciba사의 Tinuvin-770, Tinuvin-P, Tinuvin-477, Tinuvin-326 등의 광안정제를 사용할 수 있으나, 이에 제한되지 않는다.In embodiments, the light stabilizer may include one or more of benzotriazole-based compound and triazine-based compound, may be used commercially available light stabilizer. Specifically, light stabilizers such as Tinuvin-770, Tinuvin-P, Tinuvin-477, Tinuvin-326, etc. may be used, but are not limited thereto.

구체예에서, 상기 광안정제는 상기 폴리스티렌계 수지(연속상, 매트릭스)에 분산된 형태(분산상)일 수 있다. 예를 들면, 상기 광안정제 및 후술될 폴리오가노실세스퀴옥산 현탁액과 상기 스티렌계 단량체를 혼합 후, 스틸렌계 단량체를 중합함으로써, 폴리스티렌계 수지(연속상, 매트릭스)에 상기 폴리오가노실세스퀴옥산 입자(분산상) 및 광안정제(분산상)가 분산된 광확산 파우더를 얻을 수 있다.In embodiments, the light stabilizer may be in a form (disperse phase) dispersed in the polystyrene-based resin (continuous phase, matrix). For example, the light stabilizer and the polyorganosilsesquioxane suspension to be described later and the styrene monomers are mixed, and then a styrene monomer is polymerized to form the polyorganosilsesquioxane in the polystyrene resin (continuous phase, matrix). A light-diffusion powder in which particles (dispersed phase) and light stabilizer (dispersed phase) are dispersed can be obtained.

구체예에서, 상기 폴리스티렌계 수지 약 100 중량부에 대하여 약 0.1 내지 약 45 중량부, 예를 들면 약 0.5 내지 약 30 중량부, 구체적으로 약 1 내지 약 20 중량부로 포함될 수 있다. 상기 범위에서 파장 약 380 내지 약 390 nm에서 투과율 약 1% 이하를 확보하여 외광 안정성을 높일 수 있고, 광안정제가 과량 포함되어 백색의 반점으로 석출되는 것을 저감할 수 있다.In embodiments, about 0.1 to about 45 parts by weight, for example about 0.5 to about 30 parts by weight, specifically about 1 to about 20 parts by weight, based on about 100 parts by weight of the polystyrene resin. In the above range, the transmittance of about 1% or less may be secured at a wavelength of about 380 to about 390 nm to increase external light stability, and an excessive amount of light stabilizer may be included to reduce precipitation of white spots.

본 발명의 일 실시예에 따른 광확산 파우더는 입경이 약 0.01 내지 약 10 mm, 예를 들면 약 0.03 내지 약 5 mm, 구체적으로 약 0.03 내지 약 1 mm인 구형이거나, 장경이 약 0.01 내지 약 10 mm, 예를 들면 약 0.1 내지 약 5 mm, 구체적으로 약 0.1 내지 약 1 mm인 그래뉼 형상일 수 있다. 또한, 광확산 파우더가 그래뉼 형상일 경우, 장경 및 단경의 비(장경:단경)는 약 4 : 약 1 내지 약 1 : 약 1, 예를 들면 약 2 : 약 1 내지 약 1.5 : 약 1일 수 있다. 상기 범위에서 광확산 파우더가 우수한 확산 효과 및 휘도를 구현할 수 있다.The light diffusing powder according to the embodiment of the present invention has a spherical particle diameter of about 0.01 to about 10 mm, for example, about 0.03 to about 5 mm, specifically about 0.03 to about 1 mm, or a long diameter of about 0.01 to about 10 mm. mm, for example about 0.1 to about 5 mm, specifically about 0.1 to about 1 mm. In addition, when the light-diffusion powder is granular, the ratio of the long diameter and the short diameter (long diameter: short diameter) may be about 4: about 1 to about 1: about 1, for example, about 2: about 1 to about 1.5: about 1 have. In the above range, the light diffusion powder may implement excellent diffusion effects and luminance.

본 발명의 일 실시예에 따른 광확산 파우더의 제조방법은 상기 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛인 폴리오가노실세스퀴옥산 입자를 포함하는 중합액(현탁액)과 스티렌계 단량체를 혼합하고; 그리고 상기 스티렌계 단량체를 중합하여 광확산 파우더를 제조하는 단계;를 포함할 수 있다.In the method for preparing a light diffusing powder according to an embodiment of the present invention, a polymerization solution (suspension) containing a polyorganosilsesquioxane particle having an average particle diameter (D50) of about 0.1 to about 0.9 μm is mixed with a styrene monomer. and; And preparing a light diffusion powder by polymerizing the styrene-based monomer.

상기 폴리오가노실세스퀴옥산 중합액(현탁액, 라텍스)의 제조방법은 당업자에게 잘 알려져 있다. 예를 들면, 상기 폴리오가노실세스퀴옥산 중합액은 단량체로 오가노알콕시실란을 이용하여 졸-겔법(sol-gel method)에 의해 제조될 수 있다. 보다 구체적으로, 오가노트리알콕시실란을 수상에서 산 또는 염기 촉매의 존재 하에 가수분해 및 축합반응시킴으로써, 폴리오가노실세스퀴옥산 중합액을 제조할 수 있다.Methods of preparing the polyorganosilsesquioxane polymer solution (suspension, latex) are well known to those skilled in the art. For example, the polyorganosilsesquioxane polymer solution may be prepared by a sol-gel method using an organoalkoxysilane as a monomer. More specifically, the polyorganosilsesquioxane polymerization liquid can be manufactured by hydrolyzing and condensing organotrialkoxysilane in the presence of an acid or a base catalyst in an aqueous phase.

구체예에서, 상기 오가노트리알콕시실란은 하기 화학식 2로 표시될 수 있다.In embodiments, the organotrialkoxysilane may be represented by the following formula (2).

[화학식 2][Formula 2]

RSi(OR1)3 RSi (OR 1 ) 3

상기 화학식 2에서, R은 상기 화학식 1에서 정의한 바와 같고, R1은 탄소수 1 내지 5의 알킬기이다. 예를 들면, R은 메틸기, 에틸기, 또는 페닐기 등일 수 있고, R1은 메틸기, 에틸기, 프로필기 또는 부틸기일 수 있다. 구체적으로, R1 및 R2가 메틸기인 것이 공업적인 측면에서 바람직하다.In Chemical Formula 2, R is as defined in Chemical Formula 1, and R 1 is an alkyl group having 1 to 5 carbon atoms. For example, R may be a methyl group, an ethyl group, a phenyl group, or the like, and R 1 may be a methyl group, an ethyl group, a propyl group, or a butyl group. Specifically, it is preferable from an industrial point of view that R 1 and R 2 are methyl groups.

구체예에서, 상기 졸-겔 공정(가수분해 및 축합반응)은 당업자에게 통상적으로 알려져 있다. 구체적으로, 가수분해 및 축합반응은 오르가노알콕시실란을 포함하는 단량체와 소정의 용제를 혼합하여 수행될 수 있는데, 반응 속도를 조절하기 위해 촉매를 더 포함할 수도 있다. 촉매는 염산, 아세트산, 불화수소, 질산, 황산, 클로로술폰산, 요오드산 등의 산 촉매; 암모니아, 수산화칼륨, 수산화나트륨, 수산화바륨, 이미다졸 등의 염기 촉매; 등이 사용될 수 있다. 보다 구체적으로, 염기 촉매를 사용하여, pH 약 8.5 내지 약 13, 예를 들면 pH 약 10 내지 약 13 조건에서 수행될 수 있다. 상기 범위에서 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛인 폴리오가노실세스퀴옥산 입자를 포함하는 폴리오가노실세스퀴옥산 중합액을 얻을 수 있다. 상기 가수분해 및 축합반응은 상온에서는 약 1 내지 약 24시간 동안 수행될 수 있고, 반응을 촉진하기 위해서는 약 60 내지 약 100℃에서 약 1 내지 약 8시간 동안 수행될 수 있지만, 이에 제한되지 않는다. 가수분해 및 축합반응 시 용제는 특별히 제한되지 않는데, 예를 들면 물, 메탄올, 에탄올, 프로판올, 이소프로판올, n-부탄올, tert-부탄올, 메톡시프로판올 등을 단독 또는 2종 이상 혼합하여 사용할 수 있다.In an embodiment, the sol-gel process (hydrolysis and condensation reactions) is commonly known to those skilled in the art. Specifically, the hydrolysis and condensation reaction may be performed by mixing a monomer containing an organoalkoxysilane with a predetermined solvent, and may further include a catalyst to control the reaction rate. The catalyst may be an acid catalyst such as hydrochloric acid, acetic acid, hydrogen fluoride, nitric acid, sulfuric acid, chlorosulfonic acid and iodic acid; Base catalysts such as ammonia, potassium hydroxide, sodium hydroxide, barium hydroxide and imidazole; And the like can be used. More specifically, using a base catalyst, it can be carried out at a pH of about 8.5 to about 13, for example pH about 10 to about 13 conditions. In the above range, a polyorganosilsesquioxane polymer solution containing polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 μm may be obtained. The hydrolysis and condensation reaction may be performed at room temperature for about 1 to about 24 hours, and may be performed at about 60 to about 100 ° C. for about 1 to about 8 hours to promote the reaction, but is not limited thereto. The solvent in the hydrolysis and condensation reaction is not particularly limited. For example, water, methanol, ethanol, propanol, isopropanol, n-butanol, tert-butanol, methoxypropanol and the like may be used alone or in combination of two or more thereof.

구체예에서, 상기 폴리오가노실세스퀴옥산 중합액(현탁액)은 스티렌계 단량체의 중합을 용이하게 하기 위하여, 물을 추가하여 사용할 수 있다. 이 경우, 폴리오가노실세스퀴옥산 입자 및 물의 중량비는 약 0.02 : 약 1 내지 약 0.9 : 약 1일 수 있으나, 이에 제한되지 않는다.In an embodiment, the polyorganosilsesquioxane polymer solution (suspension) may be used by adding water to facilitate polymerization of the styrene monomer. In this case, the weight ratio of the polyorganosilsesquioxane particles and water may be about 0.02: about 1 to about 0.9: about 1, but is not limited thereto.

다음으로, 상기 폴리오가노실세스퀴옥산 중합액(현탁액)을 상기 스티렌계 단량체와 혼합한 후, 스티렌계 단량체를 중합하여 폴리스티렌계 수지에 폴리오가노실세스퀴옥산이 분산된 형태의 광확산 파우더를 제조할 수 있다. 이와 같이, 폴리오가노실세스퀴옥산 현탁액을 분체화하지 않고, 스티렌계 단량체와 중합하는 경우, 종래 분체화된 폴리오가노실세스퀴옥산 입자를 폴리스티렌계 수지와 마스터 배치 조성물로 제조하는 공정을 생략할 수 있으므로 공정성을 향상시킬 수 있으며, 분체화에 따라 손실되는 약 0.5 ㎛ 이하의 폴리오가노실세스퀴옥산 미립자 역시 광확산 효과에 기여할 수 있으므로 우수한 경제성 및 광확산성을 확보할 수 있다.Next, the polyorganosilsesquioxane polymerization liquid (suspension) is mixed with the styrene monomer, and then the styrene monomer is polymerized to form a light diffusion powder having a polyorgano silsesquioxane dispersed in a polystyrene resin. It can manufacture. As described above, in the case where the polyorganosilsesquioxane suspension is polymerized without pulverizing, the step of preparing the conventionally powdered polyorganosilsesquioxane particles from the polystyrene resin and the master batch composition can be omitted. Therefore, the processability can be improved, and the polyorganosilsesquioxane fine particles of about 0.5 μm or less lost due to powdering can also contribute to the light diffusion effect, thereby ensuring excellent economic efficiency and light diffusion.

상기 스티렌계 단량체의 중합반응은 당업자에게 통상적으로 알려져 있다. 예를 들면, 공지의 현탁중합 방법을 사용할 수 있다. 구체적으로 스티렌계 단량체와 필요 시, 중합개시제, 연쇄이동제 등을 투입하고, 이를 분산안정제 등이 용해된 수용액에 투입하여 현탁중합을 수행할 수 있다. 본 발명에서는 상기 폴리오가노실세스퀴옥산 현탁액에 스티렌계 단량체 등을 투입 및 혼합하고, 현탁중합을 수행할 수 있다. 상기 현탁중합 시, 중합 온도와 중합 시간은 적절하게 조절할 수 있다. 예를 들면, 약 65 내지 약 125℃, 구체적으로 약 70 내지 약 120℃의 중합 온도에서 약 1 내지 약 8 시간 동안 반응시킬 수 있으나, 이에 제한되지 않는다.Polymerization of the styrene monomers is commonly known to those skilled in the art. For example, a known suspension polymerization method can be used. Specifically, a styrene-based monomer and, if necessary, a polymerization initiator, a chain transfer agent, etc. may be added, and this may be added to an aqueous solution in which a dispersion stabilizer or the like is dissolved to perform suspension polymerization. In the present invention, a styrene-based monomer or the like may be added to the polyorganosilsesquioxane suspension and mixed, and suspension polymerization may be performed. In the suspension polymerization, the polymerization temperature and the polymerization time can be appropriately adjusted. For example, the reaction may be performed at a polymerization temperature of about 65 to about 125 ° C, specifically about 70 to about 120 ° C for about 1 to about 8 hours, but is not limited thereto.

구체예에서, 상기 중합개시제로는 중합 분야에서 알려진 통상의 라디칼 중합 개시제를 사용할 수 있으며, 예를 들면, 포타슘 퍼설페이트, 옥탄오일 퍼옥사이드, 데칸오일 퍼옥사이드, 라우로일 퍼옥사이드, 벤조일 퍼옥사이드, 모노클로로벤조일 퍼옥사이드, 디클로로벤조일 퍼옥사이드, p-메틸벤조일 퍼옥사이드, tert-부틸 퍼벤조에이트, 아조비스이소부티로니트릴 및 아조비스-(2,4-디메틸)-발레로니트릴 등을 사용할 수 있으나, 이에 제한되는 것은 아니다. 상기 중합개시제는 단독 또는 2종 이상 혼합하여 적용될 수 있다. 상기 중합개시제는 상기 스티렌계 중합체 약 100 중량부에 대하여, 약 0.01 내지 약 10 중량부, 예를 들면 약 0.03 내지 약 5 중량부로 포함될 수 있으나, 이에 제한되지 않는다.In embodiments, the polymerization initiator may be used a conventional radical polymerization initiator known in the polymerization art, for example, potassium persulfate, octanoyl peroxide, decanyl peroxide, lauroyl peroxide, benzoyl peroxide Monochlorobenzoyl peroxide, dichlorobenzoyl peroxide, p-methylbenzoyl peroxide, tert-butyl perbenzoate, azobisisobutyronitrile and azobis- (2,4-dimethyl) -valeronitrile and the like can be used. May be, but is not limited thereto. The polymerization initiator may be applied alone or by mixing two or more kinds. The polymerization initiator may include about 0.01 to about 10 parts by weight, for example about 0.03 to about 5 parts by weight, based on about 100 parts by weight of the styrene-based polymer, but is not limited thereto.

일 구체예에서, 상기 폴리오가노실세스퀴옥산 현탁액과 스티렌계 단량체를 혼합 시 상술한 광안정제를 더 첨가할 수 있다. 이 경우, 스티렌계 단량체로부터 제조된 폴리스티렌계 수지(연속상, 매트릭스)에 상기 폴리오가노실세스퀴옥산 입자(분산상) 및 광안정제(분산상)가 분산된 광확산 파우더를 얻을 수 있다.In one embodiment, the above-described light stabilizer may be further added when the polyorganosilsesquioxane suspension and the styrene monomer are mixed. In this case, a light-diffusion powder in which the polyorganosilsesquioxane particles (dispersed phase) and the light stabilizer (dispersed phase) are dispersed in a polystyrene resin (continuous phase, matrix) prepared from a styrene monomer can be obtained.

일 구체예에서, 분체화된 광확산 파우더를 수득하기 위하여, 상기 광확산 파우더의 탈수 공정이 수행될 수 있다. 상기 탈수 공정은 원심분리기, 필터프레스, 바이브레이팅 스크린(vibrating screen) 등을 이용하여 1차 탈수된 슬러지를 수세 공정을 거쳐 정제한 후, 약 60 내지 약 200℃, 예를 들면 약 70 내지 약 90℃ 범위 내에서 유동층 건조기, 스핀 플러쉬 드라이어(spin flash dryer), 진공건조기, 대류식 오븐(convection oven) 등을 이용하여 건조시킴으로써, 백색의 파우더 형태의 광확산 파우더를 제조할 수 있다. 상기 분체화된 광확산 파우더는 수분 함량이 약 5 중량% 이하, 예를 들면 약 3 내지 약 5 중량%일 수 있다.In one embodiment, to obtain the powdered light diffusing powder, a dehydration process of the light diffusing powder may be performed. The dewatering process is purified by the centrifugal separator, filter press, vibrating screen (vibrating screen), etc. after the first dewatered sludge after washing with water, about 60 to about 200 ℃, for example about 70 to about 90 The light-diffusing powder in the form of a white powder may be prepared by drying using a fluidized bed dryer, a spin flash dryer, a vacuum dryer, a convection oven, or the like within a range of ° C. The powdered light diffusing powder may have a water content of about 5% by weight or less, for example, about 3 to about 5% by weight.

본 발명에 따른 광확산판은 상기 광확산 파우더를 이용하여 제조된 것이다. 본 발명의 광확산 파우더를 광확산판 제조에 적용될 경우, 우수한 휘도 및 광확산성을 구현할 수 있으며, 상기 광확산판은 LCD-TV 등에 사용되는 확산판으로서 특히 유용하다.The light diffusing plate according to the present invention is prepared using the light diffusing powder. When the light diffusion powder of the present invention is applied to the light diffusion plate production, it is possible to implement excellent brightness and light diffusion, the light diffusion plate is particularly useful as a diffusion plate used in LCD-TV.

구체예에서, 상기 광확산판은 열가소성 수지 약 100 중량부 및 상기 광확산 파우더 약 0.1 내지 약 10 중량부, 예를 들면 약 0.5 내지 약 8 중량부를 포함할 수 있다. 상기 범위에서 열가소성 수지의 투과율을 떨어트려 확산판으로서 적합할 수 있고, 휘도, 광확산성, 내광특성 등이 우수할 수 있다.In some embodiments, the light diffusion plate may include about 100 parts by weight of the thermoplastic resin and about 0.1 to about 10 parts by weight of the light diffusion powder, for example, about 0.5 to about 8 parts by weight. In the above range, the transmittance of the thermoplastic resin may be reduced to be suitable as the diffusion plate, and the luminance, light diffusing property, and light resistance may be excellent.

구체예에서, 상기 열가소성 수지로는 통상의 확산판에 사용되는 염화비닐계 수지, 폴리스티렌계 수지, 스티렌-아크릴로니트릴계 수지, 폴리아크릴계 수지, 아크릴-스티렌계 수지, 폴리에스테르계 수지, ABS계 수지 또는 폴리카보네이트 수지 등을 제한 없이 사용할 수 있다.In an embodiment, the thermoplastic resin may be a vinyl chloride resin, a polystyrene resin, a styrene-acrylonitrile resin, a polyacrylic resin, an acrylic-styrene resin, a polyester resin, or an ABS resin, which is used in a conventional diffusion plate. Resin or polycarbonate resin can be used without limitation.

이러한 광확산판의 제조방법은 본 발명이 속하는 분야의 통상의 지식을 가진 자에 의해 용이하게 실시될 수 있다. 예를 들면, 상기 열가소성 수지 및 광확산 파우더와 필요에 따라 기타 첨가제들을 혼합한 후에, 압출기 내에서 용융 압출하여 펠렛 형태로 제조하고, 이를 사출성형, 압출성형, 진공성형, 캐스팅성형 등의 다양한 성형방법을 통해 다양한 광확산판(성형품)으로 제조될 수 있다.The method of manufacturing such a light diffusion plate can be easily carried out by those skilled in the art. For example, after mixing the thermoplastic resin and the light diffusing powder and other additives as necessary, melt extrusion in the extruder to produce a pellet form, and various molding such as injection molding, extrusion molding, vacuum molding, casting molding Through the method, it can be manufactured into various light diffusing plates (molded articles).

이하, 본 발명의 바람직한 실시예를 통해 본 발명의 구성 및 작용을 더욱 상세히 설명하기로 한다. 다만, 하기 실시예는 본 발명의 이해를 돕기 위한 것으로, 본 발명의 범위가 하기 실시예에 한정되지는 않는다. 여기에 기재되지 않은 내용은 이 기술 분야에서 숙련된 자이면 충분히 기술적으로 유추할 수 있는 것이므로 그 설명을 생략하기로 한다.Hereinafter, the configuration and operation of the present invention through the preferred embodiment of the present invention will be described in more detail. However, the following examples are provided to help the understanding of the present invention, and the scope of the present invention is not limited to the following examples. Details that are not described herein will be omitted since those skilled in the art can sufficiently infer technically.

실시예Example

제조예Production Example 1:  One: 광확산Light diffusion 파우더의 제조 Preparation of Powder

메틸트리메톡시실란에 240 g을 이온교환수 1,760 g에 넣고 30분 동안 교반한 다음, 암모니아수를 첨가하여 pH를 9.6으로 조정하고 4시간 동안 정치하여 폴리메틸실세스퀴옥산 중합액(현탁액)을 제조하였다. 여기서, 레이저 스캐터링(laser scattering) 입도 분석법으로 측정한 상기 폴리메틸실세스퀴옥산 중합액 중 폴리메틸실세스퀴옥산 입자의 평균 입경(D50)은 0.3 ㎛이었으며, 0.5 ㎛ 이하 미립자의 함량은 99%이었다. 제조된 폴리메틸실세스퀴옥산 중합액 50 중량부와 이온교환수 50 중량부를 혼합한 후, 스티렌 단량체 10 중량부 및 중합개시제(포타슘 설페이트) 0.1 중량부와 광안정제로 Ciba사 Tinuvin-770 및 Tinuvin-P를 각각 3 중량부 첨가하고 30분간 교반하여 혼합 액적(droplet)을 제조하였다. 필요 시, 이온교환수 2.5 중량부에 용해시킨 트리칼슘포스페이트(tricalcium phosphate) 0.025 중량부를 첨가한 후, 온도를 75 내지 95℃에서 5시간 정도 유지하여 반응을 완료하였다. 얻어진 광확산 파우더(중합물)를 분체화하기 위하여 탈수 공정을 수행한 후 80℃에서 12시간 건조하여 분체화된 광확산 파우더를 수득하였다(수율: 98% 이상). 제조된 광확산 파우더는 폴리스티렌계 수지 및 폴리메틸실세스퀴옥산 입자의 중량비(PS:PMSQ)가 100 : 3.36이고, 레이저 스캐터링(laser scattering) 입도 분석법으로 측정한 입경이 0.1 내지 2 mm인 구형 및 장경이 0.5 내지 5 mm인 그래뉼 형상이 혼합된 형태였다.240 g of methyltrimethoxysilane was added to 1,760 g of ion-exchanged water, stirred for 30 minutes, pH was adjusted to 9.6 by addition of ammonia water, and left to stand for 4 hours to prepare a polymethylsilsesquioxane polymer solution (suspension). Prepared. Here, the average particle diameter (D50) of the polymethylsilsesquioxane particles in the polymethylsilsesquioxane polymer solution measured by laser scattering particle size analysis was 0.3 μm, and the content of the fine particles below 0.5 μm was 99 μm. It was%. After mixing 50 parts by weight of the prepared polymethylsilsesquioxane polymerization solution and 50 parts by weight of ion-exchanged water, 10 parts by weight of the styrene monomer, 0.1 parts by weight of the polymerization initiator (potassium sulfate) and light stabilizer, Ciba's Tinuvin-770 and Tinuvin 3 parts by weight of -P were each added and stirred for 30 minutes to prepare a mixed droplet. If necessary, after adding 0.025 parts by weight of tricalcium phosphate dissolved in 2.5 parts by weight of ion-exchanged water, the temperature was maintained at 75 to 95 ° C. for about 5 hours to complete the reaction. In order to powder the obtained light-diffusion powder (polymer), a dehydration process was performed and then dried at 80 ° C. for 12 hours to obtain powdered light-diffusion powder (yield: 98% or more). The prepared light-diffusion powder has a weight ratio (PS: PMSQ) of 100: 3.36 of polystyrene resin and polymethylsilsesquioxane particles, and has a spherical particle diameter of 0.1 to 2 mm measured by laser scattering particle size analysis. And a granule shape having a long diameter of 0.5 to 5 mm.

실시예Example 1 One

폴리스티렌 수지(중량평균분자량: 340,000 g/mol) 100 중량부 및 상기 제조예 1의 광확산 파우더 24.5 중량부를 Φ=45 mm인 이축 압출기에서 혼합 및 압출하여 펠렛을 제조하고, 10 oz 사출기를 사용하여, 성형온도 240℃에서 두께 1.5 mm의 평판 시편을 제조하였으며, 하기 물성 측정 방법에 따라, 투과율(전광선 투과율, TT) 및 헤이즈(haze)를 측정 후 그 결과를 하기 표 1에 나타내었다.100 parts by weight of polystyrene resin (weight average molecular weight: 340,000 g / mol) and 24.5 parts by weight of the light-diffusion powder of Preparation Example 1 were mixed and extruded in a twin screw extruder having Φ = 45 mm to prepare pellets, and using a 10 oz injection machine. , 1.5 mm thick plate specimens were manufactured at a molding temperature of 240 ° C., and the transmittance (transmittance of light, TT) and haze were measured according to the following physical property measurement method, and the results are shown in Table 1 below.

실시예Example 2 2

상기 제조예 1의 광확산 파우더를 30 중량부 사용한 것을 제외하고는 상기 실시예 1과 동일한 방법으로 평판 시편을 제조하였으며, 투과율 및 헤이즈를 측정하고, 그 결과를 하기 표 1에 나타내었다.A flat plate specimen was manufactured in the same manner as in Example 1, except that 30 parts by weight of the light diffusing powder of Preparation Example 1 was used. The transmittance and the haze were measured, and the results are shown in Table 1 below.

실시예Example 3 3

상기 제조예 1의 광확산 파우더를 40 중량부 사용한 것을 제외하고는 상기 실시예 1과 동일한 방법으로 평판 시편을 제조하였으며, 투과율 및 헤이즈를 측정하고, 그 결과를 하기 표 1에 나타내었다.A flat plate specimen was manufactured in the same manner as in Example 1, except that 40 parts by weight of the light diffusing powder of Preparation Example 1 was used. The transmittance and the haze were measured, and the results are shown in Table 1 below.

비교예Comparative example 1 One

폴리스티렌 수지(중량평균분자량: 340,000 g/mol) 100 중량부, 폴리메틸실세스퀴옥산 입자(제조사: Samsung SDI, 제품명: SL-100M, 평균 입경(D50): 1 ㎛, 평균 입경(D50) 0.5 ㎛ 이하 미립자의 함량: 50%) 15 중량부 및 광안정제로 Ciba사 Tinuvin-770 및 Tinuvin-P(중량비 1:1) 각각 5 중량부를 혼합하여, 마스터 배치 조성물을 형성하였다. 다음으로, 폴리스티렌 수지(중량평균분자량: 340,000 g/mol) 100 중량부 및 상기 마스터 배치 조성물 15 중량부를 Φ=45 mm인 이축 압출기에서 혼합 및 압출하여 펠렛을 제조하고, 10 oz 사출기를 사용하여, 성형온도 240℃에서 두께 1.5 mm의 평판 시편을 제조하였으며, 하기 물성 측정 방법에 따라, 투과율(전광선 투과율, T.T) 및 헤이즈(haze)를 측정 후 그 결과를 하기 표 1에 나타내었다.100 parts by weight of polystyrene resin (weight average molecular weight: 340,000 g / mol), polymethylsilsesquioxane particles (manufacturer: Samsung SDI, product name: SL-100M, average particle diameter (D50): 1 μm, average particle diameter (D50) 0.5 15 parts by weight of the microparticles and the like or less and 50 parts by weight and 5 parts by weight of Ciba Tinuvin-770 and Tinuvin-P (weight ratio 1: 1) were respectively mixed with a light stabilizer to form a master batch composition. Next, 100 parts by weight of polystyrene resin (weight average molecular weight: 340,000 g / mol) and 15 parts by weight of the master batch composition were mixed and extruded in a twin screw extruder having Φ = 45 mm to prepare pellets, and using a 10 oz injection machine, A flat plate specimen having a thickness of 1.5 mm was prepared at a molding temperature of 240 ° C., and the transmittance (transmittance of light, TT) and haze were measured according to the following physical property measurement method, and the results are shown in Table 1 below.

비교예Comparative example 2 2

상기 마스터 배치 조성물을 20 중량부 사용한 것을 제외하고는 상기 비교예 1과 동일한 방법으로 평판 시편을 제조하였으며, 투과율 및 헤이즈를 측정하고, 그 결과를 하기 표 1에 나타내었다.Except that 20 parts by weight of the master batch composition was used to prepare a flat plate specimen in the same manner as in Comparative Example 1, transmittance and haze were measured, and the results are shown in Table 1 below.

물성 평가 방법Property evaluation method

(1) 투과율(TT)(단위: %): 헤이즈미터(NDH 5000W, 日本電色工業株式會社)를 사용하여 측정하였다.(1) Transmittance (TT) (unit:%): It measured using the haze meter (NDH 5000W, Nippon Denshi Kogyo Co., Ltd.).

(2) 헤이즈(Haze)(단위: %): 헤이즈미터(NDH 5000W, 日本電色工業株式會社)를 사용하여 측정하였다.(2) Haze (unit:%): It measured using the haze meter (NDH 5000W, Nippon Denshi Kogyo Co., Ltd.).

실시예 1Example 1 실시예 2Example 2 실시예 3Example 3 비교예 1Comparative Example 1 비교예 2Comparative Example 2 폴리스티렌 수지Polystyrene resin 100100 100100 100100 100100 100100 광확산 파우더Light Diffusion Powder 24.524.5 3030 4040 -- -- 마스터 배치 조성물Masterbatch composition -- -- -- 1515 2020 PMSQ 입자 평균 입경 (D50)PMSQ Particle Average Particle Size (D50) 0.3 ㎛0.3 μm 0.3 ㎛0.3 μm 0.3 ㎛0.3 μm 1 ㎛1 μm 1 ㎛1 μm 시편 중 PMSQ 입자 함량 (중량%)PMSQ Particle Content in Specimens (wt%) 0.7960.796 0.9750.975 1.31.3 1.51.5 2.02.0 투과율(%)Transmittance (%) 61.161.1 62.162.1 61.161.1 64.5764.57 60.160.1 헤이즈(%)Haze (%) 92.192.1 92.892.8 91.891.8 91.291.2 86.486.4

(단위: 중량부)(Unit: parts by weight)

상기 표 1의 결과로부터, 본 발명의 광확산 파우더를 사용한 시편은 평균입경이 0.3 ㎛인 폴리메틸실세스퀴옥산 입자를 포함하여, 1.3 중량%의 적은 함량을 포함하여도, 확산 성능이 우수함을 알 수 있다.From the results of Table 1, the specimen using the light-diffusion powder of the present invention, including the polymethylsilsesquioxane particles having an average particle diameter of 0.3 ㎛, even if containing a small amount of 1.3% by weight, the diffusion performance is excellent Able to know.

반면, 평균입경(D50)이 1.0 ㎛인 폴리오가노실세스퀴옥산 입자를 사용한 비교예 1 및 2의 경우, 실시예에 비해 과량을 사용하여도, 투과율이 높거나 헤이즈가 낮아 확산 성능이 떨어짐을 알 수 있다.On the other hand, Comparative Examples 1 and 2 using polyorganosilsesquioxane particles having an average particle diameter (D50) of 1.0 μm exhibited low diffusion performance due to high transmittance or low haze, even when an excessive amount was used. Able to know.

본 발명의 단순한 변형 내지 변경은 이 분야의 통상의 지식을 가진 자에 의하여 용이하게 실시될 수 있으며, 이러한 변형이나 변경은 모두 본 발명의 영역에 포함되는 것으로 볼 수 있다.Simple modifications or changes of the present invention can be easily carried out by those skilled in the art, and all such modifications or changes can be seen to be included in the scope of the present invention.

Claims (14)

폴리스티렌계 수지; 및Polystyrene resin; And 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛인 폴리오가노실세스퀴옥산 입자를 포함하는 것을 특징으로 하는 광확산 파우더.Light-diffusion powder, characterized in that it comprises polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 μm. 제1항에 있어서, 상기 폴리오가노실세스퀴옥산 입자는 상기 폴리스티렌계 수지 약 100 중량부에 대하여 약 0.1 내지 약 45 중량부로 포함되는 것을 특징으로 하는 광확산 파우더.The light diffusing powder of claim 1, wherein the polyorganosilsesquioxane particles are included in an amount of about 0.1 to about 45 parts by weight based on about 100 parts by weight of the polystyrene-based resin. 제1항에 있어서, 상기 폴리스티렌계 수지는 연속상이고, 상기 폴리오가노실세스퀴옥산 입자는 분산상인 것을 특징으로 하는 광확산 파우더.The light diffusing powder of claim 1, wherein the polystyrene-based resin is a continuous phase and the polyorganosilsesquioxane particles are a dispersed phase. 제1항에 있어서, 상기 폴리오가노실세스퀴옥산 입자는 입경이 약 0.05 내지 약 0.5 ㎛인 미립자를 전체 폴리오가노실세스퀴옥산 입자 100 중량% 중 약 30 내지 약 99.9 중량%로 포함하는 것을 특징으로 하는 광확산 파우더.The polyorganosilsesquioxane particles according to claim 1, wherein the polyorganosilsesquioxane particles comprise fine particles having a particle diameter of about 0.05 to about 0.5 μm in about 30 to about 99.9 wt% of 100 wt% of the total polyorganosilsesquioxane particles. Light Diffusion Powder. 제1항에 있어서, 상기 광확산 파우더는 입경이 약 0.01 내지 약 10 mm인 구형이거나, 장경이 약 0.01 내지 약 10 mm인 그래뉼 형상인 것을 특징으로 하는 광확산 파우더.The light diffusing powder of claim 1, wherein the light diffusing powder has a spherical particle size of about 0.01 to about 10 mm, or a granule shape having a long diameter of about 0.01 to about 10 mm. 제1항에 있어서, 상기 광확산 파우더는 광안정제를 더 포함하는 것을 특징으로 하는 광확산 파우더.The light diffusing powder of claim 1, wherein the light diffusing powder further comprises a light stabilizer. 제6항에 있어서, 상기 광안정제는 벤조트리아졸계 화합물 및 트리아진계 화합물 중 1종 이상을 포함하는 것을 특징으로 하는 광확산 파우더.The light diffusing powder according to claim 6, wherein the light stabilizer comprises at least one of a benzotriazole compound and a triazine compound. 제6항에 있어서, 상기 광안정제는 분산상이고, 상기 폴리스티렌계 수지 약 100 중량부에 대하여 약 0.1 내지 약 45 중량부로 포함되는 것을 특징으로 하는 광확산 파우더.The light diffusing powder of claim 6, wherein the light stabilizer is in a dispersed phase and is included in an amount of about 0.1 to about 45 parts by weight based on about 100 parts by weight of the polystyrene resin. 평균입경(D50)이 약 0.1 내지 약 0.9 ㎛인 폴리오가노실세스퀴옥산 입자를 포함하는 중합액(현탁액)과 스티렌계 단량체를 혼합하고; 그리고Mixing a styrene monomer with a polymerization solution (suspension) containing polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 to about 0.9 μm; And 상기 스티렌계 단량체를 중합하여 광확산 파우더를 제조하는 단계;를 포함하며,And polymerizing the styrene-based monomers to prepare a light diffusion powder. 상기 광확산 파우더는 상기 폴리오가노실세스퀴옥산 입자 및 폴리스티렌계 수지를 포함하는 것을 특징으로 하는 광확산 파우더의 제조방법.The light diffusion powder is a method for producing a light diffusion powder, characterized in that containing the polyorganosilsesquioxane particles and polystyrene resin. 제9항에 있어서, 상기 폴리오가노실세스퀴옥산 중합액은 오가노 알콕시 실란을 졸-겔 공정을 통해 가수분해 및 축합반응시켜 제조하는 것을 특징으로 하는 광확산 파우더의 제조방법.The method of claim 9, wherein the polyorganosilsesquioxane polymer is prepared by hydrolyzing and condensing an organoalkoxy silane through a sol-gel process. 제9항에 있어서, 상기 폴리오가노실세스퀴옥산 중합액과 스티렌계 단량체를 혼합 시 광안정제를 더 첨가하는 것을 특징으로 하는 광확산 파우더의 제조방법.10. The method of claim 9, wherein a light stabilizer is further added when the polyorganosilsesquioxane polymer solution and a styrene monomer are mixed. 제9항에 있어서, 상기 광확산 파우더를 탈수하는 단계; 및 상기 탈수된 광확산 파우더를 건조하는 단계를 더 포함하는 것을 특징으로 하는 광확산 파우더의 제조방법.10. The method of claim 9, further comprising: dehydrating the light diffusing powder; And drying the dehydrated light-diffusing powder. 제12항에 있어서, 상기 광확산 파우더는 탈수 후, 수분 함량이 약 5 중량% 이하인 것을 특징으로 하는 광확산 파우더의 제조방법.The method of claim 12, wherein the light diffusing powder has a water content of about 5% by weight or less after dehydration. 제1항 내지 제8항 중 어느 한 항에 따른 광확산 파우더를 이용하여 제조된 광확산판.A light diffusing plate manufactured using the light diffusing powder according to any one of claims 1 to 8.
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