KR20160144578A - Light diffusion particle and light diffusion sheet comprising the same - Google Patents
Light diffusion particle and light diffusion sheet comprising the same Download PDFInfo
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- KR20160144578A KR20160144578A KR1020150080851A KR20150080851A KR20160144578A KR 20160144578 A KR20160144578 A KR 20160144578A KR 1020150080851 A KR1020150080851 A KR 1020150080851A KR 20150080851 A KR20150080851 A KR 20150080851A KR 20160144578 A KR20160144578 A KR 20160144578A
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Abstract
Description
The present invention relates to a light diffusion particle and a light diffusion plate comprising the same.
Silicone fine particles such as silica and polyorganosiloxanequioxane are generally excellent in compatibility with various polymer resins and organic materials, and can be used as additives for paints, plastics, rubbers, paper, coating liquids, and activators for improving the running stability of high- And is widely used.
Particularly, the polyorganosiloxanesquioxane microparticles have a molecular structure of a three-dimensional network structure and are excellent in compatibility with resins, so that the resin composition containing the polyorganosilsesquioxane particles has excellent fluidity and exhibits properties such as optically low refractive index. Accordingly, molded articles containing such nioxylsquioxane microparticles as polio have been spotlighted as an illumination cover, a signboard, a liquid crystal display device backlight, a diffuser for a light diffusion plate (film), an additive for a light guide plate, and the like.
Such polylguanosilsesquioxane fine particles can be produced by a sol-gel method using a hydrolysis reaction and a condensation reaction mechanism using an organoalkoxysilane monomer such as methyltrialkoxysilane monomer as in the method disclosed in Japanese Patent Application Laid-Open No. 2000-186148 .
The silicon-based fine particles can realize a light diffusion effect by controlling the refractive index difference and the particle size with the matrix resin. For example, the silicone-based fine particles can be used as a light diffusing agent, Can be used.
In recent years, in order to further improve the light diffusion effect, studies have been made to lower the refractive index by reducing the particle size of soft type silicon-based fine particles (optical acid particles) such as polydimethylsiloxane. However, in the case of the soft type silicon-based fine particles, there are restrictions on the polymerization raw material, polymerization reactivity, morphology (implementation of spherical particles) and the like, in order to polymerize particles having a small particle diameter. There is a possibility of occurrence.
Therefore, there is a need to develop a light diffusion particle capable of reducing the influence of the particle diameter and morphology of the light diffusion particles at the time of using the soft silicon-based fine particles and exhibiting an excellent light diffusion effect.
Disclosure of the Invention The object of the present invention is to provide a light-diffusing particle having a lower refractive index than polystyrene sesquioxanequioxane particles having the same average particle size (D50) and a method for producing the same.
Another problem to be solved by the present invention is to provide a light diffusion particle having excellent light diffusibility capable of maintaining a spherical shape irrespective of the particle size and a method for manufacturing the same.
Another object to be solved by the present invention is to provide a light diffusion plate comprising the light diffusion particles.
One aspect of the invention relates to light diffusing particles. Wherein the light diffusing particles comprise a polyisocyanate-polydialkylsiloxane copolymer, wherein the polyol in the copolymer has a molar ratio of novolacsquioxane units (T units) and polydialkylsiloxane units (D units) T: D) is 1: 0.001 to 1: 0.5.
In an embodiment, the refractive index of the light-diffusing particles may be 1.43 or less.
In embodiments, the copolymer may be a copolymer of monomer mixtures comprising organotrialkoxysilanes and dialkyldialkoxysilanes.
In an embodiment, the organotrialkoxysilane comprises at least one of methyltrimethoxysilane (MTMS), methyltriethoxysilane and methyltripropoxysilane, the dialkyldialkoxysilane is selected from the group consisting of dimethyldimethoxysilane (DMDS), and dimethyldiethoxysilane.
In an embodiment, the light-diffusing particles may be spherical particles having an average particle diameter (D50) of 0.3 to 10 mu m.
Another aspect of the present invention relates to a method for producing the light-diffusing particles. The method comprises polymerizing a monomer mixture comprising an organotrialkoxysilane and a dialkyldialkoxysilane wherein the molar ratio of organotrialkoxysilane and dialkyldialkoxysilane in the monomer mixture is from 1: 0.001 to 1: 0.5.
In an embodiment, the polymerization can be carried out by a sol-gel method.
Another aspect of the present invention relates to a light diffusing plate. Wherein the optical diffusion plate comprises a thermoplastic resin and the light diffusion particles.
In an embodiment, the refractive index of the thermoplastic resin may be 1.47 to 1.60.
In an embodiment, the refractive index difference between the thermoplastic resin and the light-diffusing particle may be 0.04 to 0.17.
Disclosed is a light-diffusing particle having a low refractive index and excellent spherical shape regardless of the size of the particle, the light diffusing particle having an average particle size (D50) equal to that of the polystyrene-less novyesedquioxane particle, The light diffusing plate is provided with a light diffusion plate.
1 is a solid-state NMR spectrum of light diffusing particles prepared according to Example 2. Fig.
Hereinafter, the present invention will be described in detail.
The light diffusing particle according to the present invention comprises a polyorganosilsesquioxane-polydialkylsiloxane copolymer, wherein the polyorganosiloxane unit (T unit) and the polydialkylsiloxane unit (D unit) (T: D) of 1: 0.001 to 1: 0.5.
As used herein, the term "T unit" is formula (R 1 SiO 3/2) siloxane units, trifunctional means, which may be represented by, and the term "D unit" is represented by the formula (R 2 2 SiO 2/2) R 1 represents an alkyl group, a vinyl group or an aryl group having 1 to 6 carbon atoms, such as an alkyl group having 1 to 6 carbon atoms, specifically, a methyl group, an ethyl group or a propyl group, R 2 each independently represents an alkyl group having 1 to 6 carbon atoms, such as a methyl group, an ethyl group or a propyl group.
In a specific example, the polyisocyanurate unit (T unit) may be a random structure of the following formula (1), a ladder structure of the following formula (2), a cage structure of the following formula (3) 4 < / RTI > partial cage structure.
[Chemical Formula 1]
(2)
(3)
[Chemical Formula 4]
In the general formulas (1), (2), (3) and (4), R represents an alkyl group, a vinyl group or an aryl group having 1 to 6 carbon atoms, for example, an alkyl group having 1 to 6 carbon atoms, specifically a methyl group,
As a specific example, the polydialkylsiloxane unit (D unit) may include a repeating unit represented by the following formula (5).
[Chemical Formula 5]
In the formula (5), R 2 is independently an alkyl group having 1 to 6 carbon atoms, for example, a methyl group, an ethyl group, a propyl group and the like.
In embodiments, the polyorganosilsesquioxane-polydialkylsiloxane copolymer may have a crosslinked structure. In the present invention, the crosslinked structure means a structure in which a T unit is introduced into a linear structure derived from a D unit.
As a specific example, the polyorganosilsesquioxane-polydialkylsiloxane copolymer has a molar ratio (T: D) of polyorganosilsesquioxane units (T units) and polydialkylsiloxane units (D units) Can be from 1: 0.001 to 1: 0.5, for example, from 0.01 to 0.5, more specifically from 0.05 to 0.4. When the molar ratio (T: D) of the polyoxyalkylene silsesquioxane unit (T unit) to the polydialkylsiloxane unit (D unit) is less than 1: 0.001, the refractive index of the light diffusion particles is high, If the ratio is more than 1: 0.5, the light diffusion particles may not have a spherical shape or aggregation of individual particles may occur, and the light diffusion effect may be deteriorated.
In an embodiment, the light-diffusing particles may be spherical particles having an average particle size (D50) measured by a laser scattering particle size analysis of 0.3 to 10 mu m, for example, 0.5 to 5 mu m.
As used herein, the term "spherical particles" means "particles having a substantially spherical shape ", and may include, for example, an ellipse or an irregularly shaped spherical shape. The spherical particles may have a ratio of long diameter to short diameter (long diameter / short diameter) of 1.0 to 1.5.
In an embodiment, the light-diffusing particles may have a refractive index of 1.43 or less, for example 1.40 to 1.43. In the above range, scattering of light at the interface between the matrix resin (thermoplastic resin) of the light diffusion plate and the light diffusion particles can be increased and the light diffusion effect can be improved.
The light-diffusing particles according to one embodiment of the present invention can be prepared through a process comprising the step of polymerizing a monomer mixture comprising organotrialkoxysilane and dialkyldialkoxysilane.
In an embodiment, the organotrialkoxysilane may be represented by the following formula (6), and the dialkyl dialkoxysilane may be represented by the following formula (7).
[Chemical Formula 6]
In Formula 6, R 1 is or the like group having 1 to 6 carbon alkyl group, a vinyl group or an aryl group, for example an alkyl group having 1 to 6 carbon atoms, specifically a methyl group, an ethyl group, a propyl, R 10, R 11 and R 12 is And each independently represents an alkoxy group having 1 to 10 carbon atoms, for example, a methoxy group, an ethoxy group, a propoxy group, or the like.
(7)
In the above formula (7), R 2 is independently an alkyl group having 1 to 6 carbon atoms, such as a methyl group, an ethyl group or a propyl group, R 13 and R 14 each independently represent an alkoxy group having 1 to 10 carbon atoms, Ethoxy group, propoxy group, and the like.
In an embodiment, the organotrialkoxysilane may be, but is not limited to, methyltrimethoxysilane (MTMS), methyltriethoxysilane, methyltripropoxysilane, combinations thereof, and the like. The use of methyltrimethoxysilane (MTMS) may be advantageous in terms of flowability, degradability and economics in the process.
In an embodiment, the dialkyldialkoxysilane may be dimethyldimethoxysilane (DMDS), dimethyldiethoxysilane, combinations thereof, etc. However, it is not limited thereto. Use of dimethyldimethoxysilane (DMDS) Economical and reactive.
In embodiments, the molar ratio of organotrialkoxysilane and dialkyldialkoxysilane in the monomer mixture may be from 1: 0.001 to 1: 0.5, such as from 0.01 to 0.5, specifically from 0.05 to 0.4. When the molar ratio of the organotrialkoxysilane and the dialkyldialkoxysilane is less than 1: 0.001, the refractive index of the light diffusing particles may be high and the light diffusion effect may be deteriorated. The particles may not have a spherical shape or aggregation of individual particles may occur, and there is a fear that the light diffusion effect is lowered.
In an embodiment, the polymerization can be carried out by a sol-gel method. The sol-gel method (hydrolysis and condensation reaction) is generally known to those skilled in the art. Specifically, the hydrolysis and condensation reaction may be performed by mixing the monomer mixture with a predetermined solvent, and may further include a catalyst for controlling the reaction rate. The catalyst may be an acid catalyst such as hydrochloric acid, acetic acid, hydrogen fluoride, nitric acid, sulfuric acid, chlorosulfonic acid, or iodic acid; Basic catalysts such as ammonia, potassium hydroxide, sodium hydroxide, barium hydroxide and imidazole; Amberite IRA-400, IRA-67, and the like can be used. More specifically, using a base catalyst, at a pH of 10 to 14, for example, at a pH of 12 to 13. Within this range, light diffusing particles comprising a polyorganosilsesquioxane-polydialkylsiloxane copolymer can be obtained. The hydrolysis and condensation reaction may be performed at room temperature for 3 hours to 7 days, and may be carried out at 60 ° C to 100 ° C for 2 to 72 hours to promote the reaction, but the present invention is not limited thereto. In the hydrolysis and condensation reaction, the solvent is not particularly limited. For example, water, methanol, ethanol, propanol, isopropanol, n-butanol, tert-butanol and methoxypropanol may be used singly or in combination.
In one embodiment, a dehydration process of the light-diffusing particles may be performed to obtain the powdered light-diffusing particles. In the dewatering process, the primary dewatered sludge is purified through a washing process using a centrifugal separator, a filter press, a vibrating screen, and the like, and then the product is spin-dried in the range of 80 to 250 ° C. , A vacuum dryer or the like, thereby to prepare a light diffusing particle in the form of a white powder (spherical particle). The powdered light-diffusing particles may have a water content of 5 wt% or less, for example, 3 to 5 wt%.
In one embodiment, further drying (secondary drying or sintering) may be performed to further lower the moisture content of the powdered light diffusing particles. The drying or sintering may be performed at a temperature of 200 to 400 ° C, for example, 250 to 350 ° C for 30 minutes to 3 hours, for example, for 1 to 3 hours, but is not limited thereto.
The optical diffusing plate (film) according to the present invention comprises the above-mentioned light diffusing particles, and has a refractive index lower than that of the polystyrenesquioxane fine particles having the same average particle size (D50), and maintains a spherical shape regardless of the particle size It is possible to obtain excellent light diffusing properties and brightness. The light diffusing diffusion plate or film is used for a BLU of an LCD-TV.
In an embodiment, the light diffusing plate may vary depending on the transmittance degree of the light diffusing plate, but may include 100 parts by weight of the thermoplastic resin and 0.1 to 20 parts by weight, for example, 0.5 to 10 parts by weight of the light diffusing particles.
In a specific example, the thermoplastic resin may be a vinyl chloride resin, a polystyrene resin, a styrene-acrylonitrile resin, a polyacrylic resin, an acryl-styrene resin, a polyester resin, an ABS resin Resin or polycarbonate resin may be used without limitation.
In an embodiment, the refractive index of the thermoplastic resin may be 1.47 to 1.60, for example, 1.49 to 1.53, and the refractive index difference between the thermoplastic resin and the light-diffusing particle may be 0.04 to 0.17, for example, 0.05 to 0.16. It is possible to obtain a light diffusion plate having excellent luminance and light diffusibility in the above range.
The method of manufacturing such a light diffusing plate can be easily carried out by a person having ordinary skill in the art to which the present invention belongs. For example, after the thermoplastic resin and the light-diffusing particles are mixed with other additives as needed, they are melt-extruded in an extruder to produce pellets, which are then subjected to various molding processes such as injection molding, extrusion molding, vacuum molding, (Molded product) by various methods.
Hereinafter, the configuration and operation of the present invention will be described in more detail with reference to preferred embodiments of the present invention. However, the following examples are provided to aid understanding of the present invention, and the scope of the present invention is not limited to the following examples. The contents not described here are sufficiently technically inferior to those skilled in the art, and a description thereof will be omitted.
Example
Example 1: Preparation of light-diffusing particles
100 parts by weight of methyltrimethoxysilane (MTMS) and dimethyldimethoxysilane (DMDS) were dispersed in 570 parts by weight of distilled water and stirred for 1 hour according to the contents of the following Table 1, and the pH was adjusted to 10 by adding ammonia water (PMSQ) -polydimethylsiloxane (PDMS) in the form of a latex was added to the reaction mixture at a rate of 200 rpm for 0.5 to 2 hours and then allowed to stand at room temperature (about 25 ° C.) Was prepared. This was dehydrated and dried to prepare powdered light diffusing particles. The average particle diameter (D50) of the prepared light diffusing particles was measured, and the chemical structure and the copolymerization ratio of the light diffusing particles were measured through solid-state NMR spectroscopy. The theoretical refractive index of the optical particles was calculated and shown in Table 1 below.
Example 2: Preparation of light-diffusing particles
Light-diffusing particles were prepared in the same manner as in Example 1 except that the molar ratio of methyltrimethoxysilane (MTMS) and dimethyldimethoxysilane (DMDS) was changed according to the content of Table 1 below. The average particle size (D50) of the prepared light diffusing particles was measured and the chemical structure and the copolymerization ratio of the light diffusing particles were measured through a solid-state NMR spectrum. The solid nuclear magnetic resonance (solid-state NMR) spectrum is shown in Fig. The theoretical refractive index of the optical particles was calculated and shown in Table 1 below.
Comparative Example 1: Production of light-diffusing particles
Light-diffusing particles were prepared in the same manner as in Example 1 except that the molar ratio of methyltrimethoxysilane (MTMS) and dimethyldimethoxysilane (DMDS) was changed according to the content of Table 1 below. The average particle diameter (D50) of the prepared light diffusing particles was measured, and the chemical structure and the copolymerization ratio of the light diffusing particles were measured through solid-state NMR spectroscopy. The theoretical refractive index of the optical particles was calculated and shown in Table 1 below.
Comparative Example 2: Production of light-diffusing particles
Light-diffusing particles were prepared in the same manner as in Example 1 except that the molar ratio of methyltrimethoxysilane (MTMS) and dimethyldimethoxysilane (DMDS) was changed according to the content of Table 1 below. The average particle diameter (D50) of the prepared light diffusing particles was measured, and the chemical structure and the copolymerization ratio of the light diffusing particles were measured through solid-state NMR spectroscopy. The theoretical refractive index of the optical particles was calculated and shown in Table 1 below.
Comparative Example 3: Preparation of light-diffusing particles
Light-diffusing particles were prepared in the same manner as in Example 1 except that the molar ratio of methyltrimethoxysilane (MTMS) and dimethyldimethoxysilane (DMDS) was changed according to the content of Table 1 below. The average particle diameter (D50) of the prepared light diffusing particles was measured, and the chemical structure and the copolymerization ratio of the light diffusing particles were measured through solid-state NMR spectroscopy. The theoretical refractive index of the optical particles was calculated and shown in Table 1 below.
Property evaluation method
(1) Average particle size (D50) (unit: 占 퐉): Measured by laser scattering particle size analysis method.
(2) Refractive index: The theoretical refractive index was calculated from the following equation (1).
[Formula 1]
Theoretical refractive index = RM * AM + RD * AD
In the above formula 1, RM is the refractive index of methyltrimethoxysilane (MTMS), AM is the copolymerization ratio (mole ratio) of methyltrimethoxysilane, RD is the refractive index of dimethyldimethoxysilane (DMDS) And the copolymerization ratio (molar ratio) of trimethoxysilane.
(3) Copolymerization ratio: The ratio of D1 unit, D2 unit, T2 unit and T3 unit was measured using a solid-state NMR apparatus (AVANCE III 600 MHz WB, Bruker) (T: D) of a polymethylsilsesquioxane (PMSQ) unit (T unit) and a polydimethylsiloxane (PDMS) unit (D unit) was calculated.
[Formula 2]
T unit (PMSQ): D unit (PDMS) = (T2 + T3): (D1 + D2)
In the above Equation 2, D1, D2, T2, and T3 are as follows.
It can be seen from Table 1 that the light-diffusing particles of the present invention (Examples 1 and 2) have a low refractive index and are excellent in light diffusibility, and the polymethylsilsesquioxane fine particles having the same average particle size (D50) ), The refractive index is low. In the case of polydimethylsiloxane (Comparative Example 2), the particle size could not be measured due to the aggregation of particles, and the refractive index was low, but it did not have a spherical particle shape and did not exhibit particle effect. Also, in Comparative Example 3 in which the copolymerization ratio was out of the range of the present invention, pulverized spherical particles could not be obtained due to excessive polydimethylsiloxane.
It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
Wherein the molar ratio (T: D) of polystyrene sesquioxane units (T units) and polydialkylsiloxane units (D units) in the copolymer is 1: 0.001 to 1: 0.5.
Wherein the molar ratio of the organotrialkoxysilane and the dialkyl dialkoxysilane in the monomer mixture is from 1: 0.001 to 1: 0.5.
A light diffusing plate comprising the light-diffusing particles according to any one of claims 1 to 5.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111019316A (en) * | 2019-12-26 | 2020-04-17 | 陈志强 | Polycarbonate composition with light diffusion performance, preparation method and application |
| CN111286032A (en) * | 2020-03-19 | 2020-06-16 | 衢州市中通化工有限公司 | Preparation method of homopolymerized organic silicon resin microspheres |
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| JP3970449B2 (en) | 1998-12-21 | 2007-09-05 | モメンティブ・パフォーマンス・マテリアルズ・ジャパン合同会社 | Method for producing spherical polymethylsilsesquioxane fine particles |
| JP6181394B2 (en) | 2013-03-15 | 2017-08-16 | 帝人株式会社 | Thermoplastic resin composition and molded article thereof |
| JP6204839B2 (en) | 2013-10-04 | 2017-09-27 | 三菱ケミカル株式会社 | Light emitting device and wavelength conversion member |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111019316A (en) * | 2019-12-26 | 2020-04-17 | 陈志强 | Polycarbonate composition with light diffusion performance, preparation method and application |
| CN111286032A (en) * | 2020-03-19 | 2020-06-16 | 衢州市中通化工有限公司 | Preparation method of homopolymerized organic silicon resin microspheres |
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