KR20220079035A - Inorganic particle dispersion composition for display and manufacturing method thereof - Google Patents

Abstract

The present invention relates to an inorganic particle dispersion composition for a display and a method for preparing the same, and an aspect of the present invention includes: metal oxide particles; acrylate-based monomers; epoxy-based monomers; or two; a monomer comprising; silane-based coupling agent; and a dispersing agent, wherein the silane-based coupling agent is pretreated by a hydrolysis process, and provides an inorganic particle dispersion composition for a display.

Description

Inorganic particle dispersion composition for display and manufacturing method thereof

The present invention relates to an inorganic particle dispersion composition for a display and a method for preparing the same.

Optically transparent polymer materials are widely used as optical coatings and optoelectronic materials due to their low cost, good processability, and high transmittance in the visible region. Studies of mixing and dispersing in

In transparent materials for displays, organic/inorganic hybrid materials with inorganic materials of high refractive index have been used to improve the quality of displays such as high brightness, high contrast, and low power, and this is expected to be applied more extensively in the future.

However, the organic/inorganic hybrid material introduced with the high refractive inorganic material has an improved refractive index due to the inorganic material, while optical properties such as transmittance, haze, and yellow index are lowered, making it difficult to use as a display material. This follows.

In order to solve this problem, techniques for improving transparency while maintaining physical properties such as refractive index and viscosity have been studied. By doing so, there is a problem that affects other physical properties.

Therefore, there is a need for a technique for preparing an inorganic particle dispersion capable of improving the transparency of an organic-inorganic hybrid material to which a high refractive inorganic material is introduced without affecting other physical properties.

The above-mentioned background art is possessed or acquired by the inventor in the process of deriving the disclosure of the present application, and it cannot necessarily be said to be a known technology disclosed to the general public prior to the present application.

The present invention is to solve the above problems, and an object of the present invention is to provide an inorganic particle dispersion composition for a display with improved transparency while having high refractive index and a method for preparing the same.

However, the problems to be solved by the present invention are not limited to those mentioned above, and other problems not mentioned will be clearly understood by those skilled in the art from the following description.

One aspect of the present invention, metal oxide particles; acrylate-based monomers; epoxy-based monomers; or two; a monomer comprising; silane-based coupling agent; and a dispersing agent, wherein the silane-based coupling agent is pretreated by a hydrolysis process, and provides an inorganic particle dispersion composition for a display.

According to an embodiment, the metal oxide particles are ZrO ₂ , SiO ₂ , TiO ₂ , SrTiO ₂ , MgO, Ta ₂ O ₅ , ZrO ₂ -TiO ₂ and SiO ₂ -Fe ₂ O ₃ Selected from the group consisting of It may include one or more.

According to one embodiment, the metal oxide particles may have a diameter of 1 nm to 20 nm.

According to an embodiment, the content of the metal oxide particles may be 30 wt% to 70 wt%.

According to an embodiment, the acrylate-based monomer is methyl acrylate, ethyl acrylate, propyl acrylate, isopropyl acrylate, butyl acrylate, isobutyl acrylate, t-butyl acrylate, pentyl acrylate, iso Pentyl acrylate, 2-ethylhexyl acrylate, isooctyl acrylate, nonyl acrylate, isononyl acrylate, dodecyl acrylate, stearyl acrylate, methyl methacrylate, ethyl methacrylate, propyl methacrylate, Isopropyl methacrylate, butyl methacrylate, isobutyl methacrylate, t-butyl methacrylate, pentyl methacrylate, isopentyl methacrylate, 2-ethylhexyl methacrylate, isooctyl methacrylate, nonyl Methacrylate, isononyl methacrylate, dodecyl methacrylate, stearyl methacrylate, 2-ethoxyethoxyethyl acrylate, 2-ethoxyethoxyethyl methacrylate, methoxyethyl acrylate, methacrylate Toxyethyl methacrylate, 2-phenoxyethyl acrylate, ethoxylate phenoxy acrylate, 3,3,5-trimethylcyclohexane acrylate, cyclic triethylpropane formal acrylate, benzyl acrylate, isobornyl acrylate Late, cyclohexyl acrylate, biphenylmethyl acrylate, o-phenylphenol EO Acrylate (OPPEA), phenol acrylate (Phenol (EO) Acrylate; PHEA) and 3-(phenoxyphenyl) Methylpropyl-2-enoate (3-(phenoxyphenyl)methyl prop-2-enoate; PBA) may include one or more selected from the group consisting of.

According to one embodiment, the epoxy-based monomer, 4,5-epoxy tetrahydrophthalic acid diglycidyl ester (4,5-epoxy tetrahydrophthalic acid diglycidyl ester), 1,3-bis (N, N- diglycidyl ester) dilaminomethyl)cyclohexane) (1,3-bis(N,N-diglycidyl aminomethyl)cyclohexane), tetraglycidyl-m-xylenediamine, 1,2-ethoxy-methyl Propane (1,2-Epoxy-2-methylpropane), 1,2-epoxy-3-phenoxypropane (1,2-Epoxy-3-phenoxypropane), 1,2-ethoxy-5-hexene (1,2 -Epoxy-5-hexene), 1,2-epoxy-9-decene (1,2-Epoxy-9-decene), 2,3-epoxy-1-butene (3,4-Epoxy-1-butene), 3,4-Epoxy-1-cyclohexene, 2-Ethylhexyl glycidyl ether, Allyl glycidyl ether, glycidyl ether Glycidyl 2-methylphenyl ether, glycidyl 4-methoxyphenyl ether, glycidyl hexadecyl ether, glycidyl isopropyl ether ( Glycidyl isopropyl ether, Glycidyl methacrylate, 2-biphenylyl glycidyl ether, 4-Chlorophenyl glycidyl ether, Butyl It may include one or more selected from the group consisting of glycidyl ether (Butyl glycidyl ether) and ethyl glycidyl ether (Ethyl glycidyl ether).

According to an embodiment, the silane-based coupling agent is 4-aminobutylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyldiethylisopropoxysilane, ( Mercaptomethyl)dimethylethoxysilane, di-4-mercaptobutyldimethoxysilane, 3-mercaptopropyltriisopropoxysilane, 3-methacryloxypropyldimethylethoxysilane, 3-acryloxypropyltrimethoxy Silane, (3-glycidoxypropyl)methyldimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutylmethyldibutoxysilane , 5-iodohexyldiethylmethoxysilane, 3-isocyanatepropyltrimethoxysilane, 3-isothiocyanatepropylmethyldimethoxysilane, 3-hydroxybutylisopropyldimethoxysilane, bis(2-hydroxyl Ethyl)-3-aminopropyltriethoxysilane, bromophenyltrimethoxysilane, (2-(iodophenyl)ethyl)ethyldimethoxysilane, bis(chloromethylphenyl)dimethoxysilane, bromomethylphenyldimethylisopro Poxysilane, bis(propyltrimethoxysilane)carbodiimide, N-ethyl-N-(propylethoxydimethoxysilane)-carbodiimide, 3-(trimethoxysilyl)propyl methacrylate, 3- (trimethoxysilyl)propanol, (3,5-hexadione)triethoxysilane, 3-(trimethoxysilyl)propylacetoacetate, 3-(trimethoxysilyl)propylmethacrylate silane, 3-amino Propyltrimethoxysilane, 2-aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropylmethyldimethoxysilane , 3-ureidepropyltrimethoxysilane, N-ethoxycarbonyl-3-aminopropyltrimethoxysilane, N-triethoxysilylpropyltriethylenetriamine, N-trimethoxysilylpropyltriethylenetriamine , 10-trimethoxysilyl-1,4,7-triazodecane, 10-triethoxysilyl-1,4,7-triazodecane, 9-trimethoxysilyl-3,6-azononyl acetate, 3-(triethoxysilyl)propylsuccinic anhydride, N-benzyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-bis-oxyethylene-3-aminopropyltri Methoxysilane and (methacryloxy)propyltrimethoxy It may include one or more selected from the group consisting of sisilane.

According to one embodiment, the content of the silane-based coupling agent may be 1 wt% to 10 wt%.

According to one embodiment, the dispersing agent, a fatty acid-based dispersing agent; Phosphate ester-based dispersant; or both; may be included.

According to one embodiment, the fatty acid-based dispersing agent, the fatty acid-based dispersing agent, ω6 fatty acids including oleic acid, palmitic acid, linoleic acid (LA), γ-linolenic acid (GLA), α- linolenic acid (ALA), stearidonic acid (SDA), docosapentaenoic acid (DPA), docosahexaenoic acid (DHA), polyunsaturated fatty acid (EPA), butyric acid, caproic acid, caprylic acid, capric acid, lauric acid, myristic acid One selected from the group consisting of , stearic acid, myristoleic acid, palmitoleic acid, sapienic acid, elaidic acid, baxenoic acid, linoelaidic acid, arachidonic acid, erucic acid and eicosatetraenoic acid (ETA) Including the above, wherein the phosphate ester-based dispersant is, isopropyl acid phosphate, diisopropyl acid phosphate, triisopropyl acid phosphate, butyric acid phosphate, dibutyl acid phosphate, tributylic acid phosphate, octylic acid phosphate, dioctyl acid phosphate , trioctylic acid phosphate, isodecylic acid phosphate, diisodecylic acid phosphate, triisodecylic acid phosphate, tridecanolic acid phosphate, bis(tridecanolic acid) phosphate, dimethyl acid phosphate, trimethyl acid phosphate, diethyl acid phosphate, tri Ethyl acid phosphate, dipropyl acid ester, tripropyl acid ester, methyl acid phosphate, ethyl acid phosphate, propyl acid phosphate, benzylic acid phosphate, dibenzyl acid phosphate, tribenzyl acid phosphate, polyoxyethylene nonyl phenol ether phosphate, tripoly Oxyethylene nonyl phenol ether phosphate, bis(tridecanolic acid) phosphate, ethylene glycol monoethyl phosphate, diethylene glycol monoethyl phosphate, triethylene glycol monoethyl phosphate, diethylene glycol monobutyl diphosphate, diethylene glycol monobutyl phosphate , may include one or more selected from the group consisting of isopropylene glycol monoethyl phosphate, diisopropylene glycol monoethyl phosphate and triisopropylene glycol monoethyl phosphate.

According to one embodiment, the content of the dispersant may be 1 wt% to 10 wt%.

According to an embodiment, the hydrolysis process is performed by mixing deionized water and alcohol with the silane-based coupling agent, and the content ratio of the silane-based coupling agent to the deionized water is 1:0.5 to 1:3.0 may be

According to one embodiment, the refractive index of the liquid phase may be 1.5 or more.

According to an embodiment, the haze value may be 20% or less.

According to one embodiment, based on 100 parts by weight of the metal oxide particles, the monomer may be 50 parts by weight to 100 parts by weight.

Another aspect of the present invention comprises the steps of: preparing a pre-treated silane-based coupling agent by hydrolyzing the silane-based coupling agent; preparing a mixed solution by adding the metal oxide particles and the pre-treated silane-based coupling agent to an organic solvent; preparing a metal oxide particle dispersion by adding beads to the mixed solution at twice the weight of the metal oxide particles and then dispersing; and adding a monomer and a dispersant to the metal oxide particle dispersion, and removing the organic solvent.

The inorganic particle dispersion composition for a display according to the present invention includes a pre-treated silane-based coupling agent, thereby having a high refractive index property and improved transparency.

In particular, since it has a feature of exhibiting a low haze value even when inorganic particles, ie, metal oxide particles, are included in a high content for realizing high refractive index, there is an effect of high utilization as a display material.

In the method for preparing the inorganic particle dispersion composition for display according to the present invention, even if the type and content combination of the metal oxide particles, monomer, silane-based coupling agent, and dispersant are changed, the silane-based coupling agent and the silane-based coupling agent are removed in the pretreatment process By controlling the ratio of ionized water (D.W), there is a feature that can effectively implement high transmittance and high transparency of the dispersion composition.

Hereinafter, embodiments will be described in detail. However, since various changes may be made to the embodiments, the scope of the patent application is not limited or limited by these embodiments. It should be understood that all modifications, equivalents and substitutes for the embodiments are included in the scope of the rights.

The terms used in the examples are used for the purpose of description only, and should not be construed as limiting. The singular expression includes the plural expression unless the context clearly dictates otherwise. In this specification, terms such as "comprise" or "have" are intended to designate that a feature, number, step, operation, component, part, or a combination thereof described in the specification exists, but one or more other features It should be understood that this does not preclude the existence or addition of numbers, steps, operations, components, parts, or combinations thereof.

Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which the embodiment belongs. Terms such as those defined in commonly used dictionaries should be interpreted as having a meaning consistent with the meaning in the context of the related art, and should not be interpreted in an ideal or excessively formal meaning unless explicitly defined in the present application. does not

In addition, in the description of the embodiment, if it is determined that the detailed description of the related known technology may unnecessarily obscure the gist of the embodiment, the detailed description thereof will be omitted.

In addition, in describing the components of the embodiment, terms such as first, second, A, B, (a), (b), etc. may be used. These terms are only for distinguishing the elements from other elements, and the essence, order, or order of the elements are not limited by the terms. When it is described that a component is "connected", "coupled" or "connected" to another component, the component may be directly connected or connected to the other component, but another component is between each component. It will be understood that may also be "connected", "coupled" or "connected".

Components included in one embodiment and components having a common function will be described using the same names in other embodiments. Unless otherwise stated, descriptions described in one embodiment may be applied to other embodiments as well, and detailed descriptions within the overlapping range will be omitted.

One aspect of the present invention, metal oxide particles; acrylate-based monomers; epoxy-based monomers; or two; a monomer comprising; silane-based coupling agent; and a dispersing agent, wherein the silane-based coupling agent is pretreated by a hydrolysis process, and provides an inorganic particle dispersion composition for a display.

The inorganic particle dispersion composition for display according to the present invention includes a silane-based coupling agent pretreated by a hydrolysis process, and thus has a high refractive index property and improved transparency.

The silane-based coupling agent is hydroxylated by a hydrolysis process, and the hydroxylated silane-based coupling agent can improve transparency by lowering the haze of the inorganic particle dispersion composition.

In particular, the inorganic particle dispersion composition for display according to the present invention has an advantage in that transparency can be improved by precisely controlling the hydroxylation degree of the silane-based coupling agent according to the combination of the metal oxide particles, the monomer, and the dispersing agent.

In the present invention, the inorganic particles may be metal oxide particles.

According to an embodiment, the metal oxide particles are ZrO ₂ , SiO ₂ , TiO ₂ , SrTiO ₂ , MgO, Ta ₂ O ₅ , ZrO ₂ -TiO ₂ and SiO ₂ -Fe ₂ O ₃ Selected from the group consisting of It may include one or more.

The metal oxide particles may improve the refractive index of the inorganic particle dispersion composition, thereby improving the high luminance, high contrast, and low power characteristics of a display when applied to a display material.

According to one embodiment, the metal oxide particles may have a diameter of 1 nm to 20 nm.

The diameter of the metal oxide particles may be the diameter of the primary metal oxide particles.

If the diameter of the metal oxide particles is less than the above range, dispersion may be difficult due to an increase in the surface energy of the nanoparticles. Problems such as defects and a decrease in refractive index may occur.

According to one embodiment, the content of the metal oxide particles, based on the total inorganic particle dispersion composition, may be 30% by weight to 70% by weight.

Preferably, the content of the metal oxide particles, based on the total inorganic particle dispersion composition, may be 40% by weight to 60% by weight.

If the content of the metal oxide particles is less than the above range, it may be difficult to implement a high refractive index, and if it exceeds the above range, transparency may be lowered, yellowness (Y.I) may be increased, and viscosity may increase .

The inorganic particle dispersion composition according to the present invention can improve transparency even when the metal oxide particles are contained in a high content, and thus has a feature that can effectively implement high refractive index and high transparency at the same time.

According to an embodiment, the acrylate-based monomer is methyl acrylate, ethyl acrylate, propyl acrylate, isopropyl acrylate, butyl acrylate, isobutyl acrylate, t-butyl acrylate, pentyl acrylate, iso Pentyl acrylate, 2-ethylhexyl acrylate, isooctyl acrylate, nonyl acrylate, isononyl acrylate, dodecyl acrylate, stearyl acrylate, methyl methacrylate, ethyl methacrylate, propyl methacrylate, Isopropyl methacrylate, butyl methacrylate, isobutyl methacrylate, t-butyl methacrylate, pentyl methacrylate, isopentyl methacrylate, 2-ethylhexyl methacrylate, isooctyl methacrylate, nonyl Methacrylate, isononyl methacrylate, dodecyl methacrylate, stearyl methacrylate, 2-ethoxyethoxyethyl acrylate, 2-ethoxyethoxyethyl methacrylate, methoxyethyl acrylate, methacrylate Toxyethyl methacrylate, 2-phenoxyethyl acrylate, ethoxylate phenoxy acrylate, 3,3,5-trimethylcyclohexane acrylate, cyclic triethylpropane formal acrylate, benzyl acrylate, isobornyl acrylate Late, cyclohexyl acrylate, biphenylmethyl acrylate, o-phenylphenol EO Acrylate (OPPEA), phenol acrylate (Phenol (EO) Acrylate; PHEA) and 3-(phenoxyphenyl) Methylpropyl-2-enoate (3-(phenoxyphenyl)methyl prop-2-enoate; PBA) may include one or more selected from the group consisting of.

According to one embodiment, the epoxy-based monomer, 4,5-epoxy tetrahydrophthalic acid diglycidyl ester (4,5-epoxy tetrahydrophthalic acid diglycidyl ester), 1,3-bis (N, N- diglycidyl ester) dilaminomethyl)cyclohexane) (1,3-bis(N,N-diglycidyl aminomethyl)cyclohexane), tetraglycidyl-m-xylenediamine, 1,2-ethoxy-methyl Propane (1,2-Epoxy-2-methylpropane), 1,2-epoxy-3-phenoxypropane (1,2-Epoxy-3-phenoxypropane), 1,2-ethoxy-5-hexene (1,2 -Epoxy-5-hexene), 1,2-epoxy-9-decene (1,2-Epoxy-9-decene), 2,3-epoxy-1-butene (3,4-Epoxy-1-butene), 3,4-Epoxy-1-cyclohexene, 2-Ethylhexyl glycidyl ether, Allyl glycidyl ether, glycidyl ether Glycidyl 2-methylphenyl ether, glycidyl 4-methoxyphenyl ether, glycidyl hexadecyl ether, glycidyl isopropyl ether ( Glycidyl isopropyl ether, Glycidyl methacrylate, 2-biphenylyl glycidyl ether, 4-Chlorophenyl glycidyl ether, Butyl It may include one or more selected from the group consisting of glycidyl ether (Butyl glycidyl ether) and ethyl glycidyl ether (Ethyl glycidyl ether).

The acrylate-based monomer and the epoxy-based monomer have high transmittance and low haze, and have corrosion resistance to ITO.

According to one embodiment, the content of the monomer may be 10 wt% to 50 wt%, based on the total inorganic particle dispersion composition.

Preferably, the content of the monomer may be 20 wt% to 50 wt%, more preferably, 30 wt% to 50 wt%, based on the total inorganic particle dispersion composition.

If the content of the monomer is less than the above range, the viscosity may increase or processability may decrease due to lack of functional groups.

On the other hand, when the content of the monomer exceeds the above range, the refractive index may be lowered or transparency may be lowered as the content of the metal oxide particles is relatively increased to reach the target refractive index.

According to an embodiment, the silane-based coupling agent is 4-aminobutylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyldiethylisopropoxysilane, ( Mercaptomethyl)dimethylethoxysilane, di-4-mercaptobutyldimethoxysilane, 3-mercaptopropyltriisopropoxysilane, 3-methacryloxypropyldimethylethoxysilane, 3-acryloxypropyltrimethoxy Silane, (3-glycidoxypropyl)methyldimethoxysilane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutylmethyldibutoxysilane , 5-iodohexyldiethylmethoxysilane, 3-isocyanatepropyltrimethoxysilane, 3-isothiocyanatepropylmethyldimethoxysilane, 3-hydroxybutylisopropyldimethoxysilane, bis(2-hydroxyl Ethyl)-3-aminopropyltriethoxysilane, bromophenyltrimethoxysilane, (2-(iodophenyl)ethyl)ethyldimethoxysilane, bis(chloromethylphenyl)dimethoxysilane, bromomethylphenyldimethylisopro Poxysilane, bis(propyltrimethoxysilane)carbodiimide, N-ethyl-N-(propylethoxydimethoxysilane)-carbodiimide, 3-(trimethoxysilyl)propyl methacrylate, 3- (trimethoxysilyl)propanol, (3,5-hexadione)triethoxysilane, 3-(trimethoxysilyl)propylacetoacetate, 3-(trimethoxysilyl)propylmethacrylate silane, 3-amino Propyltrimethoxysilane, 2-aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropylmethyldimethoxysilane , 3-ureidepropyltrimethoxysilane, N-ethoxycarbonyl-3-aminopropyltrimethoxysilane, N-triethoxysilylpropyltriethylenetriamine, N-trimethoxysilylpropyltriethylenetriamine , 10-trimethoxysilyl-1,4,7-triazodecane, 10-triethoxysilyl-1,4,7-triazodecane, 9-trimethoxysilyl-3,6-azononyl acetate, 3-(triethoxysilyl)propylsuccinic anhydride, N-benzyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-bis-oxyethylene-3-aminopropyltri Methoxysilane and (methacryloxy)propyltrimethoxy It may include one or more selected from the group consisting of sisilane.

The silane-based coupling agent may perform a function of dispersing the metal oxide particles in a solvent while maintaining high transparency and high refractive index.

According to one embodiment, the content of the silane-based coupling agent may be 1 wt% to 10 wt%.

Preferably, the content of the silane-based coupling agent may be 2 wt% to 8 wt%, and more preferably, 3 wt% to 7 wt%.

If the content of the silane-based coupling agent is less than the above range, the dispersibility of the metal oxide particles may be lowered and cloudiness may occur. can increase the viscosity of the dispersion.

According to one embodiment, the dispersing agent, a fatty acid-based dispersing agent; Phosphate ester-based dispersant; or both; may be included.

According to one embodiment, the fatty acid-based dispersant is oleic acid, palmitic acid, linoleic acid (LA), ω6 fatty acids including γ-linolenic acid (GLA), α-linolenic acid (ALA), stearidonic acid (SDA), docosa Pentaenoic acid (DPA), docosahexaenoic acid (DHA), polyunsaturated fatty acid (EPA), butyric acid, caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, stearic acid, myristic acid It may include at least one selected from the group consisting of oleic acid, palmituleic acid, sapienic acid, elaidic acid, baxenoic acid, linoelideic acid, arachidonic acid, erucic acid, and eicosatetraenoic acid (ETA). .

According to one embodiment, the phosphate ester-based dispersant is, isopropyl acid phosphate, diisopropyl acid phosphate, triisopropyl acid phosphate, butyric acid phosphate, dibutyl acid phosphate, tributyl acid phosphate, octylic acid phosphate, dioctyl acid Phosphate, trioctylic acid phosphate, isodecylic acid phosphate, diisodecylic acid phosphate, triisodecylic acid phosphate, tridecanolic acid phosphate, bis(tridecanolic acid) phosphate, dimethyl acid phosphate, trimethyl acid phosphate, diethyl acid phosphate, Triethyl acid phosphate, dipropyl acid ester, tripropyl acid ester, methyl acid phosphate, ethyl acid phosphate, propyl acid phosphate, benzylic acid phosphate, dibenzyl acid phosphate, tribenzyl acid phosphate, polyoxyethylene nonyl phenol ether phosphate, tri Polyoxyethylene nonyl phenol ether phosphate phosphate, bis(tridecanolic acid) phosphate, ethylene glycol monoethyl phosphate, diethylene glycol monoethyl phosphate, triethylene glycol monoethyl phosphate, diethylene glycol monobutyl diphosphate, diethylene glycol monobutyl It may include one or more selected from the group consisting of phosphate, isopropylene glycol monoethyl phosphate, diisopropylene glycol monoethyl phosphate, and triisopropylene glycol monoethyl phosphate.

According to one embodiment, the dispersant, the fatty acid-based dispersant: the content ratio of the phosphate ester-based dispersant, 5: 95 to 95: 5 may be one.

The dispersant, by including the fatty acid-based dispersant and the phosphate ester-based dispersant in the above content ratio, can effectively implement a low viscosity of the inorganic particle dispersion composition, and has the effect of securing transparency.

According to one embodiment, the content of the dispersant may be 1 wt% to 10 wt%.

Preferably, the content of the dispersant may be 1 wt% to 5 wt%.

If the content of the dispersant is less than the above range, the dispersibility of the metal oxide particles may be lowered to cause cloudiness or yellowing, which may cause problems in curing and visibility of the coating layer. On the other hand, when the content of the dispersant exceeds the above range, the viscosity of the dispersion composition may increase.

According to an embodiment, the hydrolysis process is performed by mixing deionized water and alcohol with the silane-based coupling agent, and the content ratio of the silane-based coupling agent to the deionized water is 1:0.5 to 1:3.0 may be

Preferably, the content ratio of the silane-based coupling agent to the deionized water may be 1:0.5 to 1:2.0, and more preferably, 1:1 to 1:2.

The content ratio of the silane-based coupling agent and the deionized water may play a key role in lowering the haze of the inorganic particle dispersion composition. phenomenon may occur.

That is, by controlling the content ratio of the silane-based coupling agent and the deionized water, it is possible to prevent gelation of the inorganic particle dispersion composition and improve transparency.

According to one embodiment, the refractive index of the liquid phase may be 1.5 or more.

According to an embodiment, the haze value may be 20% or less.

The inorganic particle dispersion composition according to the present invention is characterized in that it has a high refractive index of 1.5 or more and a haze value of 20% or less.

That is, the inorganic particle dispersion composition according to the present invention has the effect of simultaneously implementing high refractive index and high transparency.

Therefore, it can be used in a variety of mixtures such as resins, pressure-sensitive adhesives (PSA), etc. requiring high refractive properties.

According to an embodiment, the inorganic particle dispersion composition may have a liquid refractive index of 1.6 or more and a haze value of 19% or less.

According to an embodiment, the inorganic particle dispersion composition may have a viscosity of 225 cP or less.

According to one embodiment, based on 100 parts by weight of the metal oxide particles, the monomer may be 50 parts by weight to 100 parts by weight.

Preferably, based on 100 parts by weight of the metal oxide particles, the monomer may be in an amount of 60 parts by weight to 100 parts by weight, more preferably, based on 100 parts by weight of the metal oxide particles, the monomer is in an amount of 80 parts by weight to 100 parts by weight It may be 100 parts by weight.

If, based on the content of the metal oxide particles, if the content of the monomer is less than the above range, the viscosity may increase or processability may decrease, and if it exceeds the above range, the refractive index may decrease or the transparency of the dispersion may decrease. have.

According to one embodiment, the inorganic particle dispersion composition for display may be a solvent-free inorganic particle dispersion composition for display.

Another aspect of the present invention comprises the steps of: preparing a pre-treated silane-based coupling agent by hydrolyzing the silane-based coupling agent; preparing a mixed solution by adding the metal oxide particles and the pre-treated silane-based coupling agent to an organic solvent; preparing a metal oxide particle dispersion by adding beads to the mixed solution at twice the weight of the metal oxide particles and then dispersing; and adding a monomer and a dispersant to the metal oxide particle dispersion, and removing the organic solvent.

According to an embodiment, the hydrolysis is performed by mixing deionized water and alcohol with the silane coupling agent, and the content ratio of the silane coupling agent to the deionized water is 1: 0.5 to 1:3.0. have.

In the hydrolysis, deionized water may be mixed with the silane coupling agent, and alcohol may be mixed until transparent.

According to one embodiment, the hydrolysis may be performed for 1 hour to 72 hours.

If the duration of the hydrolysis is less than the above range, the haze reducing effect of the dispersion may be reduced, and if it exceeds the above range, the dispersion may be gelled.

According to one embodiment, after the hydrolysis, the deionized water and the alcohol may be removed through reduced pressure.

In the method for preparing the inorganic particle dispersion composition for display according to the present invention, even if the type and content combination of the metal oxide particles, the monomer, the silane-based coupling agent, and the dispersant are changed, in the pretreatment process of the silane-based coupling agent, the silane-based coupling agent By controlling the ratio of the coupling agent and deionized water (D.W), there is a feature that high transmittance and high transparency of the dispersion composition can be simultaneously implemented.

According to an embodiment, the organic solvent is tetrahydrofuran, isopropyl alcohol, n-butanol, ethylene glycol, propylene glycol, methyl ethyl ketone, diethyl ketone, methyl isobutyl ketone, CHN, ethyl acetate, butyl acetate, Propylene glycol monomethyl ether, propylene glycol monomethyl ether acetate, n-hexane, toluene, xylene, styrene, o-methyl styrene, m-methyl styrene, p-methyl styrene, vinyl toluene, p-methoxy styrene, benzyl acrylic Late, benzyl methacrylate, phenyl acrylate, diphenyl acrylate, biphenyl acrylate, 2-biphenylyl acrylate, 2-([1,1'-biphenyl] -2-yloxy) ethyl acrylate , Phenoxybenzylacrylate, 3-phenoxybenzyl-3-(1-naphthyl)acrylate, ethyl (2E)-3-hydroxy-2-(3-phenoxybenzyl)acrylate, phenyl methacrylate , Biphenyl methacrylate, 2-nitrophenyl acrylate, 4-nitrophenyl acrylate, 2-nitrophenyl methacrylate, 4-nitrophenyl methacrylate, 2-nitrobenzyl methacrylate, 4-nitrobenzyl methacrylate acrylate, 2-chlorophenyl acrylate, 4-chlorophenyl acrylate, 2-chlorophenyl methacrylate, 4-chlorophenyl methacrylate, ortho-phenylphenol ethyl acrylate, bisphenol diacrylate, urethane (meth) Acrylate, 2-ethylhexyl (meth) acrylate, isobornyl (meth) acrylate, dimethylaminoethyl (meth) acrylate, 2-hydroxyethyl acrylate, 2-hydroxypropyl acrylate, 2-hydroxy Butyl acrylate, methyl ethylene glycol mono (meth) acrylate, methyl triethylene diglycol (meth) acrylate, 1,4-butanediol di (meth) acrylate, neopentyl glycol di (meth) acrylate, hydroxyl Cypivalate neopentyl glycol di(meth)acrylate, dicyclopentanyl di(meth)acrylate, caprolactone-modified dicyclopentanyl di(meth)acrylate, ethylene oxide-modified phosphate di(meth)acrylate, arylated cyclo Hexyldi(meth)acrylate, ethylene glycol di(meth)acrylate, 1,6-hexadiol diacrylate, trimethylolpropane tri(meth)acrylate, pentaerythritol tri(meth)acrylate Other) A group consisting of acrylate, dipentaerythritol penta (meth) acrylate, dipentaerythritol hexa (meth) acrylate, polyol poly (meth) acrylate, urethane (meth) acrylate and glycerin trimethacrylate It may be to include one or more selected from.

According to one embodiment, the bead, zirconia, yttria, yttria stabilized zirconia, alumina, titanium dioxide, magnesia, silicon carbide, tungsten carbide, titanium carbide and silicon nitride comprising at least one selected from the group consisting of it could be

According to one embodiment, after the beads are added to the mixed solution, the metal oxide particles may be dispersed for 2 to 4 hours using a paint shaker.

In the inorganic particle dispersion composition for display prepared according to the present invention, the organic solvent is removed by vacuum and reduced pressure in the final step, whereby a solvent-free dispersion composition for display can be prepared.

Another aspect of the present invention, the inorganic particle dispersion composition for the display; UV photoinitiators; and a monomer for UV curing; it provides a film composition for a display, including.

Another aspect of the present invention provides an optical film for a display, prepared by UV curing the film composition for a display.

Hereinafter, the present invention will be described in more detail by way of Examples and Comparative Examples.

However, the following examples are only for illustrating the present invention, and the content of the present invention is not limited to the following examples.

<Example 1>

Preparation of pretreated silane-based coupling agent

After mixing 100 mmol of 3-(trimethoxysilyl)propyl methacrylate and 150 mmol of deionized water, ethanol was added while stirring until transparent.

After stirring at room temperature for 24 hours, alcohol and deionized water were removed under reduced pressure.

Preparation of inorganic particle dispersion composition

40 parts by weight of zirconia powder having a primary particle size of 10 nm and 5 parts by weight of a pre-treated silane-based coupling agent were added to tetrahydrofuran (THF), followed by stirring to prepare a mixture.

After sufficient stirring, 0.05 mm zirconia beads were added as much as twice the weight of the mixture, and then dispersed with a paint shaker to obtain a dispersion having a zirconia content of 40%.

An acrylate-based monomer and a dispersant (a phosphate ester-based and fatty acid-based mixture) were added thereto, filtered through a 1 μm filter, and then THF was removed under reduced pressure to obtain a final inorganic particle dispersion composition.

<Example 2>

An inorganic particle dispersion composition was prepared in the same manner as in Example 1, except that 50 mmol of deionized water was added during the preparation of the pretreated silane-based coupling agent.

<Example 3>

An inorganic particle dispersion composition was prepared in the same manner as in Example 1, except that 100 mmol of deionized water was added when preparing the pretreated silane-based coupling agent.

<1 in comparison>

An inorganic particle dispersion composition was prepared in the same manner as in Example 1, except that 200 mmol of deionized water was added during the preparation of the pretreated silane-based coupling agent.

<Comparative Example 2>

An inorganic particle dispersion composition was prepared in the same manner as in Example 1, except that 300 mmol of deionized water was added during the preparation of the pretreated silane-based coupling agent.

<Comparative Example 3>

An inorganic particle dispersion composition was prepared in the same manner as in Example 1, except that an untreated silane-based coupling agent was used.

Table 1 shows the final composition of the inorganic particle dispersion composition prepared in Examples 1 to 3 and Comparative Examples 1 to 3 and the content ratio of the silane coupling agent to the deionized water during hydrolysis of the silane coupling agent.

Ingredients (%) Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 metal oxide particles 50 50 50 50 50 50 monomer 42 42 42 42 42 42 Silane-based coupling agent 6 6 6 6 6 6 dispersant 2 2 2 2 2 2 total 100 100 100 100 100 100 DW/SCA
(when SCA hydrolysis)
1.5 0.5 1.0 2.0 3.0 -

<Experimental Example> Measurement of optical properties of inorganic particle dispersion composition

The liquid refractive index, haze, and viscosity of the inorganic particle dispersion composition prepared in Examples and Comparative Examples were measured using a refractometer (ATAGO, RX-9000α), a haze meter (Nippon Denshoku, NDH7000), and a viscometer (Brookfield, DV3T), respectively. measured. was measured through

The measurement results are shown in Table 2.

Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 refractive index 1.67 1.67 1.67 1.67 1.67 1.67 HAZE (%) 13.7 18.5 16.5 13.3 Gel 20.9 Viscosity (cP) 220 223 216 310 Gel 230

Referring to Table 2, it can be seen that the inorganic particle dispersion composition of Example exhibits a high refractive index of 1.67, a haze of 20% or less, and a viscosity of 225 cP or less.

In the case of Comparative Example 1, the haze characteristic was the lowest at 13.3%, but there was a problem in that the viscosity of the inorganic particle dispersion was increased, so it was judged as an unsuitable input amount.

Through this, it can be seen that the inorganic particle dispersion composition according to the present invention has high refractive index properties and improved transparency.

Although the embodiments have been described above, a person skilled in the art may apply various technical modifications and variations based on the above. For example, the described techniques are performed in an order different from the described method, and/or the described components of the system, structure, apparatus, circuit, etc. are combined or combined in a different form than the described method, or other components Or substituted or substituted by equivalents may achieve an appropriate result.

Therefore, other implementations, other embodiments, and equivalents to the claims are also within the scope of the following claims.

Claims (16)

metal oxide particles;
acrylate-based monomers; epoxy-based monomers; or two; a monomer comprising;
silane-based coupling agent; and
dispersing agent; including,
The silane-based coupling agent is pre-treated by a hydrolysis process,
Inorganic particle dispersion composition for display.
According to claim 1,
The metal oxide particles,
ZrO ₂ , SiO ₂ , TiO ₂ , SrTiO ₂ , MgO, Ta ₂ O ₅ , ZrO ₂ -TiO ₂ and SiO ₂ -Fe ₂ O ₃ Will include one or more selected from the group consisting of,
Inorganic particle dispersion composition for display.
According to claim 1,
The diameter of the metal oxide particles is,
1 nm to 20 nm,
Inorganic particle dispersion composition for display.
According to claim 1,
The content of the metal oxide particles is,
30% to 70% by weight,
Inorganic particle dispersion composition for display.
According to claim 1,
The acrylate-based monomer,
Methyl acrylate, ethyl acrylate, propyl acrylate, isopropyl acrylate, butyl acrylate, isobutyl acrylate, t-butyl acrylate, pentyl acrylate, isopentyl acrylate, 2-ethylhexyl acrylate, isooctyl Acrylate, nonyl acrylate, isononyl acrylate, dodecyl acrylate, stearyl acrylate, methyl methacrylate, ethyl methacrylate, propyl methacrylate, isopropyl methacrylate, butyl methacrylate, isobutyl Methacrylate, t-butyl methacrylate, pentyl methacrylate, isopentyl methacrylate, 2-ethylhexyl methacrylate, isooctyl methacrylate, nonyl methacrylate, isononyl methacrylate, dodecyl methacrylate Krylate, stearyl methacrylate, 2-ethoxyethoxyethyl acrylate, 2-ethoxyethoxyethyl methacrylate, methoxyethyl acrylate, methoxyethyl methacrylate, 2-phenoxyethyl acrylate , ethoxylate phenoxy acrylate, 3,3,5-trimethylcyclohexane acrylate, cyclic triethyl propane formal acrylate, benzyl acrylate, isobornyl acrylate, cyclohexyl acrylate, biphenylmethyl acrylate, o-phenylphenol EO Acrylate (OPPEA), phenol acrylate (Phenol(EO) Acrylate; PHEA) and 3-(phenoxyphenyl)methylpropyl-2-enoate (3-(phenoxyphenyl) ) which comprises at least one selected from the group consisting of methyl prop-2-enoate; PBA),
Inorganic particle dispersion composition for display.
According to claim 1,
The epoxy-based monomer,
4,5-epoxy tetrahydrophthalic acid diglycidyl ester, 1,3-bis(N,N-diglycidylaminomethyl)cyclohexane) (1,3- bis(N,N-diglycidyl aminomethyl)cyclohexane), tetraglycidyl-m-xylenediamine, 1,2-ethoxy-methylpropane (1,2-Epoxy-2-methylpropane) , 1,2-Epoxy-3-phenoxypropane (1,2-Epoxy-3-phenoxypropane), 1,2-ethoxy-5-hexene (1,2-Epoxy-5-hexene), 1,2- Epoxy-9-decene (1,2-Epoxy-9-decene), 2,3-epoxy-1-butene (3,4-Epoxy-1-butene), 3,4-epoxy-1-cyclohexene (3 ,4-Epoxy-1-cyclohexene), 2-ethylhexyl glycidyl ether (2-Ethylhexyl glycidyl ether), allyl glycidyl ether (Allyl glycidyl ether), glycidyl 2-methylphenyl ether ), glycidyl 4-methoxyphenyl ether, glycidyl hexadecyl ether, glycidyl isopropyl ether, glycidyl methacrylate ( Glycidyl methacrylate, 2-biphenylyl glycidyl ether, 4-chlorophenyl glycidyl ether, butyl glycidyl ether, and ethyl glycidyl ether Which comprises at least one selected from the group consisting of cydyl ether (Ethyl glycidyl ether),
Inorganic particle dispersion composition for display.
According to claim 1,
The silane-based coupling agent,
4-Aminobutylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, N-2-aminoethyl-3-aminopropyldiethylisopropoxysilane, (mercaptomethyl)dimethylethoxysilane, di-4- Mercaptobutyldimethoxysilane, 3-mercaptopropyltriisopropoxysilane, 3-methacryloxypropyldimethylethoxysilane, 3-acryloxypropyltrimethoxysilane, (3-glycidoxypropyl)methyldimethoxy Silane, 2-(3,4-epoxycyclohexyl)ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 4-bromobutylmethyldibutoxysilane, 5-iodohexyldiethylmethoxysilane, 3 -isocyanatepropyltrimethoxysilane, 3-isothiocyanatepropylmethyldimethoxysilane, 3-hydroxybutylisopropyldimethoxysilane, bis(2-hydroxyethyl)-3-aminopropyltriethoxysilane, bro Mophenyltrimethoxysilane, (2-(iodophenyl)ethyl)ethyldimethoxysilane, bis(chloromethylphenyl)dimethoxysilane, bromomethylphenyldimethylisopropoxysilane, bis(propyltrimethoxysilane)carbodiy Mead, N-ethyl-N-(propylethoxydimethoxysilane)-carbodiimide, 3-(trimethoxysilyl)propyl methacrylate, 3-(trimethoxysilyl)propanol, (3,5- Hexadione)triethoxysilane, 3-(trimethoxysilyl)propylacetoacetate, 3-(trimethoxysilyl)propylmethacrylate silane, 3-aminopropyltrimethoxysilane, 2-aminopropyltrimethoxy Silane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropylmethyldimethoxysilane, 3-ureidepropyltrimethoxysilane, N- Ethoxycarbonyl-3-aminopropyltrimethoxysilane, N-triethoxysilylpropyltriethylenetriamine, N-trimethoxysilylpropyltriethylenetriamine, 10-trimethoxysilyl-1,4,7 -Triazodecane, 10-triethoxysilyl-1,4,7-triazodecane, 9-trimethoxysilyl-3,6-azononylacetate, 3-(triethoxysilyl)propylsuccinic anhydride, N -benzyl-3-aminopropyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane, N-bis-oxyethylene-3-aminopropyltrimethoxysilane and (methacryloxy)propyltrimethoxy at least one selected from the group consisting of silanes which includes,
Inorganic particle dispersion composition for display.
According to claim 1,
The content of the silane-based coupling agent is,
1% to 10% by weight,
Inorganic particle dispersion composition for display.
According to claim 1,
The dispersant is
fatty acid-based dispersants; Phosphate ester-based dispersant; or the two;
Inorganic particle dispersion composition for display.
10. The method of claim 9,
The fatty acid-based dispersant is oleic acid, palmitic acid, linoleic acid (LA), ω6 fatty acid including γ-linolenic acid (GLA), α-linolenic acid (ALA), stearidonic acid (SDA), docosapentaenoic acid (DPA) , Docosahexaenoic acid (DHA), polyunsaturated fatty acid (EPA), butyric acid, caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, stearic acid, myristoleic acid, palmitoleic acid, It contains at least one selected from the group consisting of sapienic acid, elaidic acid, baxenic acid, linoelaidic acid, arachidonic acid, erucic acid, and eicosatetraenoic acid (ETA),
The phosphate ester-based dispersant is, isopropyl acid phosphate, diisopropyl acid phosphate, triisopropyl acid phosphate, butyric acid phosphate, dibutyl acid phosphate, tributylic acid phosphate, octylic acid phosphate, dioctyl acid phosphate, trioctylic acid phosphate , isodecylic acid phosphate, diisodecylic acid phosphate, triisodecylic acid phosphate, tridecanolic acid phosphate, bis(tridecanolic acid) phosphate, dimethyl acid phosphate, trimethyl acid phosphate, diethyl acid phosphate, triethyl acid phosphate, diethyl acid phosphate Propyl acid ester, tripropyl acid ester, methyl acid phosphate, ethyl acid phosphate, propyl acid phosphate, benzylic acid phosphate, dibenzylic acid phosphate, tribenzyl acid phosphate, polyoxyethylene nonyl phenol ether phosphate, tripolyoxyethylene nonyl phenol ether Phosphate phosphate, bis(tridecanolic acid) phosphate, ethylene glycol monoethyl phosphate, diethylene glycol monoethyl phosphate, triethylene glycol monoethyl phosphate, diethylene glycol monobutyl diphosphate, diethylene glycol monobutyl phosphate, isopropylene glycol mono Which comprises at least one selected from the group consisting of ethyl phosphate, diisopropylene glycol monoethyl phosphate and triisopropylene glycol monoethyl phosphate,
Inorganic particle dispersion composition for display.
According to claim 1,
The content of the dispersant is,
1% to 10% by weight,
Inorganic particle dispersion composition for display.
According to claim 1,
The hydrolysis process is
It is performed by mixing deionized water and alcohol with the silane-based coupling agent,
The silane-based coupling agent: the content ratio of the deionized water will be 1: 0.5 to 1: 3.0,
Inorganic particle dispersion composition for display.
According to claim 1,
The liquidus refractive index is 1.5 or more,
Inorganic particle dispersion composition for display.
According to claim 1,
That the haze (Haze) value is 20% or less,
Inorganic particle dispersion composition for display.
According to claim 1,
Based on 100 parts by weight of the metal oxide particles, the monomer is 50 parts by weight to 100 parts by weight,
Inorganic particle dispersion composition for display.
preparing a pre-treated silane-based coupling agent by hydrolyzing the silane-based coupling agent;
preparing a mixed solution by adding the metal oxide particles and the pre-treated silane-based coupling agent to an organic solvent;
preparing a metal oxide particle dispersion by adding beads to the mixed solution at twice the weight of the metal oxide particles and then dispersing; and
Including; adding a monomer and a dispersing agent to the metal oxide particle dispersion, and removing the organic solvent;
A method for preparing an inorganic particle dispersion composition for a display.