CN107667142B - Light diffusing powder and method of making same - Google Patents
Light diffusing powder and method of making same Download PDFInfo
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- CN107667142B CN107667142B CN201680031294.1A CN201680031294A CN107667142B CN 107667142 B CN107667142 B CN 107667142B CN 201680031294 A CN201680031294 A CN 201680031294A CN 107667142 B CN107667142 B CN 107667142B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L25/00—Compositions 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
- C08L25/02—Homopolymers or copolymers of hydrocarbons
- C08L25/04—Homopolymers or copolymers of styrene
- C08L25/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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
- C08L83/04—Polysiloxanes
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/02—Diffusing elements; Afocal elements
Abstract
The light diffusing powder of the present invention comprises: a polystyrene-based resin; and polyorganosilsesquioxane particles having an average diameter (D50) of about 0.1 to 0.9 μm. The light diffusion powder has excellent light diffusion properties and brightness, and the preparation method thereof reduces the loss of polyorganosilsesquioxane fine particles of about 0.5 μm or less and has excellent economic efficiency and processability.
Description
Technical Field
The present invention relates to a light diffusing powder and a method of making the same. More particularly, the present invention relates to a light diffusion powder used in a light diffusion plate.
Background
Silicone particles such as silica or polyorganosilsesquioxane generally have good compatibility with various polymer resins and organic materials, and are widely used as additives for paints, plastics, rubbers, paper or coating liquids and active agents for improving the running stability of high quality video tapes.
In particular, polyorganosilsesquioxane particles have a three-dimensional network molecular structure and good flowability as well as good compatibility with resins and a low refractive index, and are attracting attention as (light) diffusing agents for lamp covers, signboards, and backlight units for liquid crystal displays, and as additives for light guide plates.
Such polyorganosilsesquioxane particles are prepared by a sol-gel method using a hydrolysis and condensation mechanism of methyltrialkoxysilane monomers, as disclosed in, for example, Japanese patent application laid-open No. 2000-186148.
In a typical method, in order to use polyorganosilsesquioxane particles as a diffusing agent of a light diffusion plate, fine polyorganosilsesquioxane particles are mixed with a thermoplastic resin such as a styrene resin to prepare a master batch, and then the master batch is mixed with another thermoplastic resin, and the mixture is extruded to manufacture a light diffusion plate. Then, this method has a problem in that fine particles having a particle diameter of about 0.5 μm or less are likely to be lost during pulverization (e.g., dehydration) of polyorganosilsesquioxane particles, and it is necessary to pulverize a diffusing agent at a high concentration and prepare a master batch containing the diffusing agent, thereby causing a complication of the process.
The inventors have developed a light diffusion powder which can minimize the loss of fine polyorganosilsesquioxane particles having a particle size of about 0.5 μm or less, thereby achieving good light diffusion and brightness, and which can simplify the manufacturing process, thereby improving processability.
Disclosure of Invention
Technical problem
An object of the present invention is to provide a light-diffusing powder capable of achieving good light diffusion and brightness.
It is another object of the present invention to provide a method of preparing a light diffusing powder that minimizes the loss of fine polyorganosilsesquioxane particles having a particle size of about 0.5 μm or less.
It is still another object of the present invention to provide a method for preparing a light-diffusing powder, which can ensure good economic feasibility and processability.
It is still another object of the present invention to provide a light diffusion plate using the light diffusion powder as above.
The above and other objects of the present invention can be accomplished by the present invention described hereinafter.
Technical scheme
One aspect of the present invention relates to a light diffusing powder. The light diffusing powder includes: a polystyrene resin; and polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 μm to about 0.9 μm.
In exemplary embodiments, the polyorganosilsesquioxane particles may be present in an amount of about 0.1 parts by weight to about 45 parts by weight, relative to 100 parts by weight of the polystyrene resin.
In exemplary embodiments, the polystyrene resin may be present in a continuous phase and the polyorganosilsesquioxane particles may be present in a dispersed phase.
In exemplary embodiments, the polyorganosilsesquioxane particles may include about 30 wt% to about 99.9 wt% of fine particles having a particle size of about 0.05 μm to about 0.5 μm, based on 100 wt% of the total weight of the polyorganosilsesquioxane particles.
In exemplary embodiments, the light diffusion powder may be in the shape of a sphere having a particle size of about 0.01mm to about 10mm, or may be in the shape of a particle having a major diameter of about 0.01mm to about 10 mm.
In an exemplary embodiment, the light diffusing powder may further include a light stabilizer.
In exemplary embodiments, the light stabilizer may include at least one of a benzotriazole compound and a triazine compound.
In exemplary embodiments, the light stabilizer may have a dispersed phase and may be present in an amount of about 0.1 parts by weight to about 45 parts by weight, relative to about 100 parts by weight of the polystyrene resin.
Another aspect of the invention relates to a method of making a light diffusing powder. The method comprises the following steps: mixing styrene monomer with a polymer solution (suspension) containing polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 μm to about 0.9 μm; and preparing a light diffusion powder by polymerization of styrene monomers, wherein the light diffusion powder includes polyorganosilsesquioxane particles and a polystyrene resin.
In exemplary embodiments, the polyorganosilsesquioxane polymer solution may be prepared by hydrolyzing and condensing organoalkoxysilane by a sol-gel method.
In exemplary embodiments, mixing the styrene monomer with the polyorganosilsesquioxane polymer solution may include further adding a light stabilizer.
In an exemplary embodiment, the method may further include: dehydrating the light diffusing powder; and drying the dehydrated light diffusing powder.
In an exemplary embodiment, the light diffusing powder may have a water content of about 5 wt% measured after dehydration.
Still another aspect of the present invention relates to a light diffusion plate manufactured using the above light diffusion powder.
Advantageous effects
The present invention provides: a light-diffusing powder capable of achieving good light diffusion and brightness; a method of preparing a light diffusion powder capable of minimizing loss of fine polyorganosilsesquioxane particles having a particle size of about 0.5 μm or less and ensuring good economic feasibility and processability; and a light diffusion plate using the light diffusion powder.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail.
According to one aspect of the present invention, a light diffusing powder includes: a polystyrene resin; and polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 μm to about 0.9 μm.
The polystyrene resin may include any typical polystyrene resin used in a light diffusion plate and may be obtained by polymerizing styrene monomers by a known polymerization method.
In some embodiments, the styrene monomer may include styrene, alpha-methylstyrene, beta-methylstyrene, p-tert-butylstyrene, ethylstyrene, vinylxylene, monochlorostyrene, dichlorostyrene, dibromostyrene, and vinylnaphthalene, but is not limited thereto. These may be used alone or as a mixture thereof.
In some embodiments, the polystyrene resin may form the continuous phase (matrix) of the light diffusing powder. For example, a polyorganosilsesquioxane suspension containing polyorganosilsesquioxane particles as described below may be mixed with a styrene monomer, followed by polymerization of the styrene monomer, thereby obtaining a polystyrene resin (continuous phase) in which the polyorganosilsesquioxane particles (dispersed phase) are dispersed.
In some embodiments, the polystyrene resin can have a weight average molecular weight of about 5,000g/mol to about 50,000g/mol, for example about 5,000g/mol to about 30,000g/mol, as measured by Gel Permeation Chromatography (GPC). In this range, the polyorganosilsesquioxane particles (dispersed phase) can be uniformly dispersed in the polystyrene resin (continuous phase), and the light diffusion powder can be uniformly diffused and distributed in the matrix during the manufacture of the light diffusion plate by extrusion.
The polyorganosilsesquioxane particles act as a light diffuser and may have an average particle diameter (D50) of about 0.1 μm to about 0.9 μm, for example about 0.3 μm to about 0.6 μm, as measured by laser scattering particle size analysis. If the average particle diameter of the polyorganosilsesquioxane particles is less than about 0.1 μm, the particles are outside the rayleigh scattering region, resulting in an increase in light transmittance rather than diffusion performance, whereas if the average particle diameter of the polyorganosilsesquioxane particles exceeds about 0.9 μm, both light transmittance and brightness cannot be sufficiently improved, requiring the use of an excessive amount of a light diffusing agent.
In some embodiments, the polyorganosilsesquioxane particles may contain a repeating unit represented by formula 1.
< formula 1>
RSiO1.5-x(OH)x
In formula 1, R is C1To C6An alkyl group, an alkenyl group, or an aryl group, and x is in the range of 0 to 1.5. For example, R can be a methyl group, an ethyl group, a phenyl group, and the like. From the industrial viewpointIn view of this, a methyl group is preferable.
In some embodiments, the polyorganosilsesquioxane particles may be prepared by a sol-gel method (hydrolysis and condensation) using organoalkoxysilane as a monomer, but is not limited thereto.
In some embodiments, the polyorganosilsesquioxane particles may comprise about 30 wt% to about 99.9 wt% (e.g., about 40 wt% to about 99 wt%) of fine particles having a particle size of about 0.05 μm to about 0.5 μm, based on 100 wt% of the total weight of the polyorganosilsesquioxane particles. Within this range, the polyorganosilsesquioxane particles can have good light diffusion efficiency. Further, since the amount of the light diffusing agent (polyorganosilsesquioxane particles) used in the light diffusing plate can be reduced while maintaining the same light transmittance, deterioration or breakage of strength due to a poor compatibility between the light diffusing agent and the resin can be reduced, and the manufacturing cost can be reduced.
In some embodiments, the polyorganosilsesquioxane particles may be the dispersed phase of the light diffusing powder. For example, the polyorganosilsesquioxane suspension described below may be mixed with styrene monomer, followed by polymerization of the styrene monomer without pulverizing the polyorganosilsesquioxane suspension, and the polyorganosilsesquioxane particles may be dispersed (i.e., present as a dispersed phase) in the polystyrene resin (continuous phase).
In some embodiments, the polyorganosilsesquioxane particles may be present in an amount of about 0.1 parts by weight to about 45 parts by weight, for example about 3 parts by weight to about 10 parts by weight, relative to about 100 parts by weight of the polystyrene resin. In this range, the light diffusion powder can provide good light diffusion and brightness.
In one embodiment, the light diffusing powder may further include a light stabilizer.
In some embodiments, the photostabilizer can have an absorbance of about 0.25AU or greater, for example about 0.5AU to about 1.0AU, measured at a wavelength of about 380nm at a concentration of about 20mg/L in toluene. In this range, the light diffusion powder can sufficiently absorb light having a wavelength of about 380nm to about 390nm among external light, and has low light transmittance, thereby improving stability to external light of the display.
In some embodiments, the light stabilizer may include at least one of a benzotriazole compound and a triazine compound. Further, the light stabilizer may include any suitable commercially available light stabilizer. Specifically, the light stabilizer may include Tinuvin-770, Tinuvin-P, Tinuvin-477, and Tinuvin-326(Ciba-Geigy Corp.), but is not limited thereto.
In some embodiments, the light stabilizer may be dispersed (i.e., present as a dispersed phase) in the polystyrene resin (continuous phase, matrix). For example, a light stabilizer and a polyorganosilsesquioxane suspension described below may be mixed with a styrene monomer, followed by polymerization of the styrene monomer, thereby obtaining a light diffusing powder in which polyorganosilsesquioxane particles (dispersed phase) and a light stabilizer (dispersed phase) are dispersed in a polystyrene resin (continuous phase, matrix).
In some embodiments, the light stabilizer may be present in an amount of about 0.1 parts by weight to about 45 parts by weight, for example about 0.5 parts by weight to about 30 parts by weight, specifically about 1 part by weight to about 20 parts by weight, relative to 100 parts by weight of the polystyrene resin. In this range, stability to external light can be improved by securing light transmittance of about 1% or less at a wavelength of about 380nm to about 390nm, and light excessive stabilizer can be prevented from precipitating as white spots.
In some embodiments, the light diffusing powder may be in the shape of a sphere having a particle size of about 0.01mm to about 10mm, such as about 0.03mm to about 5mm, specifically about 0.03mm to about 1mm, or may be in the shape of a particle having a major diameter of about 0.01mm to about 10mm, such as about 0.1mm to about 5mm, specifically about 0.1mm to about 1 mm. When the light diffusion powder has a particle shape, the ratio of the large diameter to the small diameter (large diameter: small diameter) may be in the range of about 4:1 to about 1:1, for example about 2:1 to about 1.5: 1. In this range, the light diffusion powder can provide good light diffusion and brightness.
According to another aspect of the present invention, a method of preparing a light diffusing powder includes: mixing styrene monomer with a polymerization solution (suspension) comprising polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 μm to about 0.9 μm; the light diffusing powder is prepared by polymerization of styrene monomer.
Methods for preparing polyorganosilsesquioxane polymerization solutions (suspensions or latexes) are well known to those skilled in the art. For example, polyorganosilsesquioxane polymerization solutions can be prepared by a sol-gel method using organoalkoxysilanes as monomers. Specifically, the polyorganosilsesquioxane polymerization solution may be prepared by subjecting organotrialkoxysilane to hydrolysis and condensation in an aqueous phase in the presence of an acid or base catalyst.
In some embodiments, the organotrialkoxysilane may be represented by formula 2.
< formula 2>
RSi(OR1)3
In formula 2, R is as defined for formula 1, and R is1Is C1To C5An alkyl group. For example, R may be a methyl group, an ethyl group, or a phenyl group, and R1It may be a methyl group, an ethyl group, a propyl group or a butyl group. From an industrial point of view, R and R1Both are preferably methyl groups.
The sol-gel process (hydrolysis and condensation) is well known to those skilled in the art. Specifically, the hydrolysis and condensation may be performed by mixing the organoalkoxysilane-containing monomer with a predetermined solvent. Here, a catalyst may be added to control the reaction rate. The catalyst may include acid catalysts such as hydrochloric acid, acetic acid, hydrofluoric acid, nitric acid, sulfuric acid, chlorosulfonic acid, or iodic acid; and base catalysts such as ammonia, potassium hydroxide, sodium hydroxide, barium hydroxide and imidazole. More specifically, the hydrolysis and condensation may be carried out using a base catalyst at a pH of about 8.5 to about 13, for example about 10 to about 13. When hydrolysis and condensation are carried out at a pH within this range, a polyorganosilsesquioxane polymerization solution containing polyorganosilsesquioxane particles having an average particle diameter (D50) of about 0.1 μm to about 0.9 μm can be obtained. The hydrolysis and condensation may be performed at room temperature for about 1 to 24 hours, or may be performed at about 60 ℃ to about 100 ℃ for about 1 to 8 hours to facilitate the reaction, but is not limited thereto. The solvent used for the hydrolysis and condensation is not particularly limited and may include, for example, water, methanol, ethanol, propanol, isopropanol, n-butanol, t-butanol, and methoxypropanol. These solvents may be used alone or as a mixture thereof.
In some embodiments, water may be added to the polyorganosilsesquioxane polymerization solution (suspension) to facilitate polymerization of the styrene monomer. When water is added, the weight ratio of polyorganosilsesquioxane particles to water may range from about 0.02:1 to about 0.9:1, but is not limited thereto.
Then, the polyorganosilsesquioxane polymerization solution (suspension) may be mixed with a styrene monomer, followed by polymerization of the styrene monomer, thereby preparing a light diffusion powder in which polyorganosilsesquioxane particles are dispersed in a polystyrene resin. When the polyorganosilsesquioxane suspension is polymerized with the styrene monomer without being pulverized, a process of mixing polyorganosilsesquioxane powder with the polystyrene resin to prepare a master batch may be omitted, thereby improving processability. Furthermore, fine polyorganosilsesquioxane particles having an average particle size of about 0.5 μm, which would otherwise be lost during pulverization of the suspension, may also contribute to light diffusion, thereby ensuring economic feasibility and light diffusion efficiency.
The polymerization of styrene monomers is well known to those skilled in the art. For example, a known suspension polymerization method can be used. Specifically, suspension polymerization can be performed by introducing a styrene monomer and optionally a polymerization initiator, a chain transfer agent, and the like into an aqueous solution in which a dispersion stabilizer and the like are dissolved. According to the present invention, styrene monomer or the like may be mixed with the polyorganosilsesquioxane suspension, followed by suspension polymerization. Here, the suspension polymerization may be performed at a predetermined temperature for a predetermined time. For example, the suspension polymerization may be carried out at about 65 ℃ to about 125 ℃ (particularly at about 70 ℃ to about 120 ℃) for about 1 to 8 hours, but is not limited thereto.
In some embodiments, the polymerization initiator may include any typical free radical polymerization initiator known in the art. Examples of the radical polymerization initiator may include potassium persulfate, octanoyl peroxide, decanoyl peroxide, lauroyl peroxide, benzoyl peroxide, monochlorobenzoyl peroxide, dichlorobenzoyl peroxide, p-methylbenzoyl peroxide, tert-butyl perbenzoate, azobisisobutyronitrile, and azobis (2, 4-dimethyl) -valeronitrile, but are not limited thereto. These initiators may be used alone or as a mixture thereof. These polymerization initiators may be present in an amount of about 0.01 parts by weight to about 10 parts by weight, for example about 0.03 parts by weight to about 5 parts by weight, relative to about 100 parts by weight of the styrene polymer, but are not limited thereto.
In one embodiment, when the polyorganosilsesquioxane suspension is mixed with the styrene monomer, a light stabilizer may be further added. In this way, a light diffusing powder can be obtained in which polyorganosilsesquioxane particles (dispersed phase) and a light stabilizer (dispersed phase) are dispersed in a polystyrene resin (continuous phase, matrix) prepared from styrene monomers.
In one embodiment, to obtain the light diffusing powder, the light diffusing powder may be subjected to dehydration. In the dehydration, the sludge preliminarily dehydrated using a centrifugal separator, a filter press or a vibrating screen is purified by washing, and then dried at about 60 ℃ to about 200 ℃ (e.g., about 70 ℃ to about 90 ℃) using a fluidized bed dryer, a spin flash dryer, a vacuum dryer or a convection oven, thereby preparing the light diffusion powder in the form of white powder. The light diffusing powder may have a moisture content of less than about 5 wt%, for example from about 3 wt% to about 5 wt%.
According to a further aspect of the present invention, a light diffusion plate is manufactured using the above light diffusion powder. The light diffusion plate manufactured using the light diffusion powder according to the present invention can achieve good luminance and light diffusion. In particular, the light diffusion plate can be used as a diffusion plate for an LCD-TV or the like.
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 (e.g., about 0.5 to about 8 parts by weight) of the light diffusion powder. Within these ranges, the light diffusion plate is suitable as a diffusion plate due to low light transmittance of the thermoplastic resin, and can provide good performance in terms of luminance, light diffusion, and light resistance.
In some embodiments, the thermoplastic resin may include any typical thermoplastic resin used for a diffusion plate, such as a vinyl chloride resin, a polystyrene resin, a styrene-acrylonitrile resin, a polyacrylic resin, an acrylic-styrene resin, a polyester resin, an ABS resin, or a polycarbonate resin.
The method of manufacturing the light diffusion plate may be easily performed by one of ordinary skill in the art to which the present invention pertains. For example, pellets may be prepared by mixing a thermoplastic resin, a light diffusing powder, and optionally other additives, and then melt-extruding them in an extruder. The prepared pellets can be produced into various light diffusion plates (molded articles) by various molding methods such as injection molding, extrusion, vacuum forming and casting.
Modes for carrying out the invention
Next, the present invention will be described in more detail with reference to examples. It should be noted, however, that these examples are for illustration only and should not be construed as limiting the invention in any way. Moreover, the descriptions of details that are apparent to those of ordinary skill in the art have been omitted for the sake of clarity.
Examples
Preparation example 1: preparation of light-diffusing powders
240g of methyltrimethoxysilane was added to 1760g of deionized water, followed by stirring for 30 minutes, then aqueous ammonia was added to adjust the pH to 9.6, and the resulting mixture was allowed to stand for 4 hours, thereby preparing a polymethylsilsesquioxane polymerization solution (suspension). Here, the average particle diameter (D50) of polymethylsilsesquioxane particles in the polymethylsilsesquioxane polymerization solution was 0.3 μm, as measured by laser scattering particle size analysis, and fine particles having a particle diameter of 0.5 μm or less were present in the solution in an amount of 99%. After 50 parts by weight of the polymethylsilsesquioxane polymerization solution was mixed with 50 parts by weight of ion-exchanged water, 10 parts by weight of a styrene monomer, 0.1 part by weight of a polymerization initiator (potassium sulfate), and 3 parts by weight of each of Tinuvin-770 and Tinuvin-P (Ciba-Geigy Corp.) as a light stabilizer were added, followed by stirring for 30 minutes, thereby preparing mixed droplets. If necessary, tricalcium phosphate dissolved in 0.025 parts by weight of deionized water in 2.5 parts by weight was added, and the resulting mixture was left at 75 to 95 ℃ for about 5 hours, thereby completing the reaction. Then, dehydration was performed to powderize the obtained light diffusion powder (polymer), followed by drying at 80 ℃ for 12 hours, thereby obtaining a light diffusion powder (yield: 98% or more). In the obtained light diffusion powder, the weight ratio (PS: PMSQ) of the polystyrene resin to the polymethylsilsesquioxane particles was 100:3.36, and the obtained light diffusion powder contained both spherical-shaped particles having an average particle diameter of 0.1mm to 2mm and particle-shaped particles having a major diameter of 0.5mm to 5mm as measured by laser scattering particle size analysis.
Example 1
Pellets were prepared by mixing 100 parts by weight of a polystyrene resin (weight average molecular weight: 340,000g/mol) and 24.5 parts by weight of the light diffusion powder of preparation example 1 and extruding in a twin-screw extruder (phi-45 mm). Then, the pellets were subjected to injection molding using a 10 oz injection molding machine at a molding temperature of 240 ℃ to thereby produce flat plate specimens 1.5mm thick. The light transmittance (total light transmittance, TT) and haze of the fabricated test specimens were evaluated according to the following methods. The results are shown in Table 1.
Example 2
A flat plate sample was manufactured in the same manner as in example 1, except that the light diffusion powder of preparation example 1 was used in an amount of 30 parts by weight. The fabricated samples were evaluated for light transmittance and haze. The results are shown in Table 1.
Example 3
A flat plate sample was manufactured in the same manner as in example 1, except that the light diffusion powder of preparation example 1 was used in an amount of 40 parts by weight. The fabricated samples were evaluated for light transmittance and haze. The results are shown in Table 1.
Comparative example 1
A master batch was prepared by mixing 100 parts by weight of a polystyrene resin (weight average molecular weight: 340,000g/mol) with 15 parts by weight of polymethylsilsesquioxane particles (SL-100M, Samsung SDI, average particle diameter (D50):1 μ M, content of fine particles having an average particle diameter (D50) of 0.5 μ M or less: 50%) and 5 parts by weight each of Tinuvin-770 and Tinuvin-P (Ciba-Geigy Corp., weight ratio: 1:1) as a light stabilizer. Then, 100 parts by weight of a polystyrene resin (weight average molecular weight: 340,000g/mol) and 15 parts by weight of the master batch were mixed and extruded in a twin-screw extruder (phi-45 mm), thereby preparing pellets. Then, the pellets were injection-molded at a molding temperature of 240 ℃ using a 10 oz injection molding machine to prepare flat plate specimens having a thickness of 1.5 mm. The light transmittance (total light transmittance, TT) and haze of the fabricated test specimens were evaluated according to the following methods. The results are shown in Table 1.
Comparative example 2
A flat plate sample was produced in the same manner as in comparative example 1 except that the master batch was used in an amount of 20 parts by weight. The fabricated samples were evaluated for light transmittance and haze. The results are shown in Table 1.
Evaluation of Properties
(1) Light transmittance (TT) (unit:%): the light transmittance of each sample was measured using a haze meter (NDH 5000W, Nippon Denshoku Industries co., Ltd.).
(2) Haze (unit:%): the haze of each sample was measured using a haze meter (NDH 5000W, Nippon Denshoku Industries co., Ltd.).
[ Table 1]
(unit: parts by weight)
As can be seen from the results shown in table 1, the samples manufactured using the light diffusion powder according to the present invention (including polymethylsilsesquioxane particles having an average particle size of 0.3 μm) had good diffusion properties, although the amount of polymethylsilsesquioxane particles used was as low as 1.3 wt%.
In contrast, it can be seen that the samples of comparative examples 1 and 2 using polyorganosilsesquioxane particles having an average particle diameter (D50) of 1.0 μm have high light transmittance or low haze, and thus exhibit poor light diffusion properties, although a larger amount of polyorganosilsesquioxane particles is used than in the examples.
It is to be understood that various modifications, alterations, adaptations, and equivalent embodiments may be made by those skilled in the art without departing from the spirit and scope of the present invention.
Claims (10)
1. A light diffusing powder comprising:
a polystyrene resin; and
polyorganosilsesquioxane particles having an average particle diameter of 0.1 to 0.9 [ mu ] m,
wherein the polystyrene resin is present in a continuous phase and the polyorganosilsesquioxane particles are present in a dispersed phase,
wherein the polyorganosilsesquioxane particles comprise 30 to 99.9 wt% of fine particles having a particle diameter of 0.05 to 0.5 μm based on the total weight of the polyorganosilsesquioxane particles,
wherein the light diffusing powder is in the form of particles having a major diameter of 0.01mm to 10mm, and
wherein the polyorganosilsesquioxane particles are present in an amount of 0.1 part by weight to 45 parts by weight, relative to 100 parts by weight of the polystyrene resin.
2. The light diffusing powder of claim 1, further comprising: light stabilizers.
3. The light diffusing powder of claim 2, wherein the light stabilizer comprises at least one of a benzotriazole compound and a triazine compound.
4. The light diffusing powder of claim 2 wherein the light stabilizer is present in a dispersed phase and in an amount of 0.1 to 45 parts by weight relative to 100 parts by weight of the polystyrene resin.
5. A method of making a light diffusing powder comprising:
mixing styrene monomer with a polymerization solution containing polyorganosilsesquioxane particles having an average particle size of 0.1 to 0.9 μm; and
preparing a light diffusion powder by polymerization of the styrene monomer,
wherein the light diffusion powder comprises the polyorganosilsesquioxane particles and a polystyrene resin,
wherein the polystyrene resin is present in a continuous phase and the polyorganosilsesquioxane particles are present in a dispersed phase,
wherein the polyorganosilsesquioxane particles comprise 30 to 99.9 wt% of fine particles having a particle diameter of 0.05 to 0.5 μm based on the total weight of the polyorganosilsesquioxane particles,
wherein the light diffusing powder is in the form of particles having a major diameter of 0.01mm to 10mm, and
wherein the polyorganosilsesquioxane particles are present in an amount of 0.1 part by weight to 45 parts by weight, relative to 100 parts by weight of the polystyrene resin.
6. The method of preparing a light diffusing powder of claim 5 wherein the polymer solution of polyorganosilsesquioxane is prepared by hydrolyzing and condensing organoalkoxysilane through a sol-gel process.
7. The method of preparing a light diffusing powder of claim 5 wherein mixing the styrene monomer with the polymer solution of polyorganosilsesquioxane includes further adding a light stabilizer.
8. The method of making a light diffusing powder of claim 5, further comprising:
dehydrating the light diffusing powder; and
drying the dehydrated light diffusing powder.
9. The method of making a light diffusing powder of claim 8 wherein the light diffusing powder has a water content of 5 wt% measured after dehydration.
10. A light diffusion plate manufactured using the light diffusion powder according to any one of claims 1 to 4, wherein the light diffusion plate comprises 100 parts by weight of a thermoplastic resin and 0.1 to 10 parts by weight of the light diffusion powder.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020150074319A KR20160141078A (en) | 2015-05-27 | 2015-05-27 | Light diffusion powder and method for preparing the same |
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| PCT/KR2016/004602 WO2016190560A1 (en) | 2015-05-27 | 2016-05-02 | Light diffusing powder and preparation method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1942521A (en) * | 2004-04-14 | 2007-04-04 | 出光兴产株式会社 | Light-diffusing resin composition |
| KR20080012257A (en) * | 2005-05-20 | 2008-02-11 | 제너럴 일렉트릭 캄파니 | Light diffusing films, methods of making the same, and articles using the same |
| KR100837090B1 (en) * | 2007-03-20 | 2008-06-12 | 제일모직주식회사 | Light diffusing particle, method for preparing the same and light-diffusing plate using the same |
| CN103842423A (en) * | 2011-10-31 | 2014-06-04 | 道康宁印度私人有限公司 | Light diffusing thermoplastic resin compositions and light diffusing members |
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| KR100856718B1 (en) * | 2006-12-15 | 2008-09-04 | 제일모직주식회사 | Silicone Light-Diffusing Agent with Bimodal Size Distribution, Method for Preparing the Same, and Light-Diffusing Plate Using the Same |
| KR100859498B1 (en) * | 2006-12-20 | 2008-09-22 | 제일모직주식회사 | Silicon Bead with High Quality Luminance and Lightfastness, Method for Preparing the Same and Light-Diffusing Plate Using the Same |
| KR101400323B1 (en) * | 2007-12-21 | 2014-05-28 | 코오롱인더스트리 주식회사 | Polymer beads having core-shell structure and Preparation method of polymer beads by core-shell method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1942521A (en) * | 2004-04-14 | 2007-04-04 | 出光兴产株式会社 | Light-diffusing resin composition |
| KR20080012257A (en) * | 2005-05-20 | 2008-02-11 | 제너럴 일렉트릭 캄파니 | Light diffusing films, methods of making the same, and articles using the same |
| KR100837090B1 (en) * | 2007-03-20 | 2008-06-12 | 제일모직주식회사 | Light diffusing particle, method for preparing the same and light-diffusing plate using the same |
| CN103842423A (en) * | 2011-10-31 | 2014-06-04 | 道康宁印度私人有限公司 | Light diffusing thermoplastic resin compositions and light diffusing members |
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| KR20160141078A (en) | 2016-12-08 |
| CN107667142A (en) | 2018-02-06 |
| JP2018517017A (en) | 2018-06-28 |
| WO2016190560A1 (en) | 2016-12-01 |
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