WO2016009979A1 - Dispersion de particules d'oxyde métallique, composition contenant des particules d'oxyde métallique, film de revêtement et dispositif d'affichage - Google Patents

Dispersion de particules d'oxyde métallique, composition contenant des particules d'oxyde métallique, film de revêtement et dispositif d'affichage Download PDF

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WO2016009979A1
WO2016009979A1 PCT/JP2015/069987 JP2015069987W WO2016009979A1 WO 2016009979 A1 WO2016009979 A1 WO 2016009979A1 JP 2015069987 W JP2015069987 W JP 2015069987W WO 2016009979 A1 WO2016009979 A1 WO 2016009979A1
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Prior art keywords
metal oxide
oxide particle
mass
particle dispersion
oxide particles
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PCT/JP2015/069987
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English (en)
Japanese (ja)
Inventor
哲朗 板垣
鈴木　一也
有紀 釘本
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住友大阪セメント株式会社
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Priority to CN201580038123.7A priority Critical patent/CN106661362A/zh
Priority to KR1020177001440A priority patent/KR20170030532A/ko
Publication of WO2016009979A1 publication Critical patent/WO2016009979A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
    • C09D17/007—Metal oxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00—Compounds of zirconium
    • C01G25/02—Oxides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D17/00—Pigment pastes, e.g. for mixing in paints
    • C09D17/002—Pigment pastes, e.g. for mixing in paints in organic medium
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D201/00—Coating compositions based on unspecified macromolecular compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives

Definitions

  • the present invention relates to a metal oxide particle dispersion, a metal oxide particle-containing composition, a coating film, and a display device.
  • Metal oxide particles are used for the purpose of adjusting the refractive index, imparting functionality such as conductivity, antistatic properties, ultraviolet shielding properties, heat ray shielding properties, electromagnetic wave shielding properties, and improving mechanical strength. It is used by being dispersed in a substrate or the like.
  • a functional film of a plastic substrate used in a display device such as a liquid crystal display (LCD), a plasma display (PDP), or an electroluminescence display (EL) requires transparency, refractive index, mechanical properties, and the like. . Therefore, a functional film is formed by applying a composition obtained by mixing a resin substrate with inorganic oxide particles such as zirconia having a high refractive index and a resin on a plastic substrate (see, for example, Patent Document 1). ).
  • metal oxide particles antimony-doped tin oxide (ATO) or tin-doped indium oxide (ITO) particles provide a heat ray shielding coating solution and a heat ray shielding film excellent in visible light transmittance and heat ray shielding properties.
  • ATO antimony-doped tin oxide
  • ITO tin-doped indium oxide
  • metal oxide particles zinc oxide particles are used to obtain a highly transparent gas barrier laminate (see, for example, Patent Document 3).
  • the metal oxide particles are used in a state of a metal oxide particle dispersion liquid previously dispersed in a solvent and mixed in a paint or a resin monomer.
  • the step of drying the coating film, the step of removing the solvent, and the like the target paint, coating film, base material, etc. are required to exhibit excellent dispersibility.
  • the refractive index of the metal oxide particles is 1.9 or more, the optical characteristics (transparency, etc.) of the paint, coating film, base material, etc.
  • the product particle dispersion is required to have high dispersibility and stability.
  • a method for dispersing metal oxide particles in a solvent a method is known in which the surface of metal oxide particles is treated with an organosilicon compound having a group that generates a silanol group by hydrolysis of a silane coupling agent or the like. (For example, see Patent Documents 4 to 6).
  • the metal oxide particles are made of epoxy resin (10.9), acrylic resin (9.5), polystyrene (8.5 to 10.3), urethane resin (10 to 11), phenol resin (11.5), cellulose.
  • a medium polarity resin such as resin (10-12), polyester resin (10-11), epoxy resin (10-11), etc. Is designed so that the SP value of the dispersion medium in the dispersion is adjusted to the same level as the SP value of the resin so that the surface-treated metal oxide particles have a good affinity for both the dispersion medium and the resin. There was a need to do.
  • the present invention has been made in view of the above circumstances, and provides a metal oxide particle dispersion, a metal oxide particle-containing composition, a coating film, and a display device that have high transparency and excellent stability over time. For the purpose.
  • the present inventors have a silanol group when an amine having 2 or more carbon atoms is used as a reaction catalyst in a medium-polar organic solvent, Alternatively, the surface treatment reaction of metal oxide particles by an organosilicon compound having a group that generates a silanol group by hydrolysis proceeds with a small amount of water (water content), so transparency is high and stability over time is improved.
  • the inventors have found that an excellent metal oxide particle dispersion can be obtained, and have completed the present invention.
  • the present invention provides a metal oxide particle dispersion liquid in which metal oxide particles surface-treated with a silicon compound represented by the following general formula (1) are dispersed in a solvent.
  • the metal oxide particle dispersion further contains an amine having 2 or more carbon atoms, The average primary particle diameter of the metal oxide particles is 3 nm or more and 20 nm or less, the refractive index is 1.9 or more,
  • the solvent contains 70% by mass or more of an organic solvent,
  • the solubility parameter of the organic solvent is 8.0 or more and 12 or less, the solubility in water is 1.5 g / 100 ml or more,
  • a metal oxide particle dispersion is provided, wherein the water content is 3% by mass or less of the content of the metal oxide particles.
  • the present invention provides a metal oxide particle-containing composition comprising the metal oxide particle dispersion of the present invention and a binder component.
  • the present invention provides a coating film characterized by being formed using the metal oxide particle-containing composition of the present invention.
  • the present invention provides a display device comprising the coating film of the present invention.
  • the metal oxide particle dispersion of the present invention has high transparency, excellent dispersion stability of the metal oxide particles, and excellent stability of the dispersion for long-term storage.
  • the metal oxide particle-containing composition of the present invention contains the metal oxide particle dispersion of the present invention that is highly transparent and excellent in dispersion stability of the metal oxide particles. For this reason, it is excellent in the dispersion stability of a metal oxide particle, and is excellent in the stability of long-term storage of a composition.
  • the coating film of the present invention is formed using the metal oxide particle-containing composition of the present invention. For this reason, the coating film excellent in transparency can be obtained.
  • the display device of the present invention includes the coating film of the present invention that is excellent in transparency. For this reason, it is excellent in visibility.
  • the metal oxide particle dispersion of the present embodiment is surface-treated with a silicon compound represented by the following general formula (1), the average primary particle diameter is 3 nm or more and 20 nm or less, and the refractive index is 1.9 or more.
  • This is a product particle dispersion, which contains an amine having 2 or more carbon atoms, and the water content is 3% by mass or less of the content of the metal oxide particles.
  • Metal oxide particles The metal oxide particles in the present embodiment are not particularly limited as long as the refractive index is a metal oxide particle having a refractive index of 1.9 or more.
  • the refractive index is a metal oxide particle having a refractive index of 1.9 or more.
  • Metal oxide particles containing one or more metal elements selected from the group of niobium, tungsten, europium and hafnium are preferably used.
  • Examples of the metal oxide particles composed of one kind of metal element include: Zirconium (IV) oxide (ZrO 2 : refractive index 2.05 to 2.4), Zinc (II) oxide (ZnO: refractive index 2.01 to 2.1), Iron (III) oxide (Fe 2 O 3 : refractive index 3.01), Copper (I) oxide (Cu 2 O: refractive index 2.71), Titanium (IV) oxide (TiO 2 : refractive index 2.3 to 2.7), Tin oxide (IV) (SnO 2 : refractive index 2.00), Cerium (IV) oxide (CeO 2 : refractive index 2.1), Tantalum oxide (V) (Ta 2 O 5 : refractive index 2.2), Niobium oxide (V) (Nb 2 O 5 : refractive index 2.4), Tungsten oxide (VI) (WO 3 : refractive index 2.2), Europium (III) oxide (Eu 2 O 3 : refractive index 1.98), Hafnium (IV) oxide
  • metal oxide particles composed of two kinds of metal elements include: Potassium titanate (K 2 Ti 6 O 13 : refractive index 2.68), Barium titanate (BaTiO 3 : refractive index 2.3 to 2.5), Strontium titanate (SrTiO 3 : refractive index 2.37), Potassium niobate (KNbO 3 : refractive index 2.17), Lithium niobate (LiNbO 3 : refractive index 2.35), Calcium tungstate (CaWO 4 : refractive index 1.91), Antimony-added tin oxide (ATO; Sb solid solution SnO 2 : refractive index 1.95 to 2.05), indium added tin oxide (ITO; In solid solution SnO 2 : refractive index 1.95 to 2.05), etc. are suitable Used for.
  • K 2 Ti 6 O 13 refractive index 2.68
  • Barium titanate BaTiO 3 : refractive index 2.3 to 2.5
  • zirconium oxide (IV), zinc oxide (II), titanium oxide (IV), antimony-added tin oxide, and indium-added tin oxide are more preferably used from the viewpoint of raw material costs and manufacturing costs.
  • Zirconium (IV) oxide is more preferably used because it is less likely to be colored by absorption / scattering around 400 nm.
  • the average primary particle diameter of the metal oxide particles is 3 nm or more and 20 nm or less, preferably 8 nm or more and 20 nm or less, more preferably 10 nm or more and 15 nm or less. If the average primary particle diameter of the metal oxide particles is less than 3 nm, the crystallinity of the metal oxide particles is low, and the target refractive index may not be obtained. In addition, when the metal oxide particles are dispersed in a solvent, the metal oxide particles are likely to aggregate, and thus a highly transparent dispersion may not be obtained.
  • the specific surface area of the metal oxide particles becomes large, the amount of silicon compound necessary for obtaining a dispersion increases, and there is a possibility that a sufficient refractive index as the surface-treated metal oxide particles cannot be obtained.
  • the average primary particle diameter exceeds 20 nm, the dispersed particle diameter when the metal oxide particles are dispersed in the solvent is increased, and a highly transparent dispersion liquid may not be obtained.
  • the “average primary particle size” means the particle size of each individual particle.
  • the major axis of each metal oxide particle for example, each of 100 or more metal oxide particles.
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • a method of measuring the major axis, preferably the major axis of each of the 500 metal oxide particles, and calculating the arithmetic average value thereof can be mentioned.
  • the specific surface area of the metal oxide particles is preferably 70m 2 / g or more and is 95 m 2 / g or less.
  • the larger the specific surface area of the metal oxide particles the greater the amount of silicon compound and the amount of water necessary for the surface treatment.
  • the silicon compound in this embodiment is represented by the general formula (1). That is, the silicon compound in the present embodiment is an organosilicon compound having a silanol group or a group that generates a silanol group by hydrolysis.
  • R in the general formula (1) is preferably a hydrogen atom or an alkyl group having 1 to 22 carbon atoms.
  • the alkyl group may be linear, branched or cyclic. When the alkyl group is cyclic, it may be monocyclic or polycyclic.
  • the alkyl group preferably has 1 to 22 carbon atoms. However, in order to obtain a compound having higher affinity for the solvent described later, the alkyl group must have 1 to 6 carbon atoms. More preferred.
  • the linear or branched alkyl group preferably has 1 to 22 carbon atoms.
  • alkyl group include a methyl group, an ethyl group, an n-propyl group, an isopropyl group, n -Butyl group, isobutyl group, sec-butyl group, tert-butyl group, n-pentyl group, isopentyl group, neopentyl group, tert-pentyl group, 1-methylbutyl group, n-hexyl group, 2-methylpentyl group, 3 -Methylpentyl group, 2,2-dimethylbutyl group, 2,3-dimethylbutyl group, n-heptyl group, 2-methylhexyl group, 3-methylhexyl group, 2,2-dimethylpentyl group, 2,3- Dimethylpentyl group, 2,4-dimethylpentyl group, 3,3-dimethylpentyl group
  • the cyclic alkyl group preferably has 1 to 22 carbon atoms, and preferably 3 to 10 carbon atoms.
  • Examples of such a cyclic alkyl group include a cyclopropyl group, a cyclobutyl group, a cyclopentyl group, a cyclohexyl group, a cycloheptyl group, a cyclooctyl group, a cyclononyl group, a cyclodecyl group, a norbornyl group, an isobornyl group, a 1-adamantyl group, And 2-adamantyl group.
  • examples of the alkyl group include those in which one or more hydrogen atoms of these cyclic alkyl groups are substituted with a linear, branched or cyclic alkyl group.
  • the cyclic alkyl group further preferably has 3 or more and 6 or less carbon atoms from the viewpoint of affinity for the solvent described later.
  • one or two or more hydrogen atoms in the alkyl group may be optionally substituted with a halogen atom.
  • halogen atom substituted for the hydrogen atom include a fluorine atom, a chlorine atom, a bromine atom, and an iodine atom.
  • R ′ in the general formula (1) is an organic group. What is necessary is just to select suitably in consideration of affinity with the solvent mentioned later. Examples include acryloyl group, methacryloyl group, vinyl group, propyl group, butadienyl group, styryl group, ethynyl group, cinnamoyl group, maleate group, acrylamide group, amino group, allyl group, epoxy group, glycidoxy group and the like.
  • the organic group is preferably a functional group having a polymerizable unsaturated group.
  • the polymerizable unsaturated group is not particularly limited, and examples thereof include acryloyl group, methacryloyl group, vinyl group, propenyl group, butadienyl group, styryl group, ethynyl group, cinnamoyl group, maleate group, and acrylamide group. These polymerizable unsaturated groups are structural units that undergo addition polymerization with active radical species.
  • Examples of the silicon compound represented by the general formula (1) include compounds in which an alkoxy group such as a methoxy group, an ethoxy group, and an isopropoxy group, an aryloxy group, an acetoxy group, an amino group, or a halogen atom is bonded to a silicon atom. Is mentioned. Among these, a compound in which an alkoxy group is bonded to a silicon atom, that is, an organoalkoxysilane is particularly preferable.
  • silicon compound represented by the general formula (1) examples include vinyltrimethoxysilane, vinyltriethoxysilane, 2- (3,4-epoxycyclohexyl) ethyltrimethoxysilane, and 3-glycidoxypropyl.
  • the silicon compound represented by the general formula (1) has a polymerizable unsaturated group such as acryloyl group, methacryloyl group, vinyl group, propenyl group, butadienyl group, styryl group, ethynyl group, cinnamoyl group, maleate group, and acrylamide group. It is preferable that the functional group which has is included. In this case, since it can be combined with a resin or the like, when the metal oxide particle dispersion of this embodiment is blended in a paint or the like and a coating film is produced, the metal oxide particles are unlikely to aggregate.
  • the surface treatment of the metal oxide particles with the silicon compound may be performed as long as the silicon compound and the metal oxide particles interact with each other and are bonded to each other. They may be bound by a covalent bond, or may be bound by a non-covalent bond such as physical adsorption. Moreover, after pre-hydrolyzing metal oxide particles and allowing some or all of the hydrolysis to proceed, the metal oxide particles may be surface-treated with a silicon compound.
  • Organic solvent contains 70% by mass or more and 80% by mass of an organic solvent having a solubility parameter (SP value) of 8.0 or more and 12 or less and a solubility in water of 1.5 g / 100 ml or more. It is preferable to contain above, and it is more preferable to contain 90 mass% or more.
  • SP value solubility parameter
  • the content of the organic solvent is less than 70% by mass, when forming a coating film using the metal oxide particle dispersion of this embodiment, or when removing the solvent from the metal oxide particle dispersion of this embodiment.
  • the metal oxide particles may aggregate or gel.
  • water necessary for hydrolysis of the silicon compound cannot be dissolved.
  • the volatilization rate is increased when a coating film is formed using the paint or when the solvent is removed from the paint. There is a risk of segregation of product particles.
  • the metal oxide particle dispersion of the present embodiment is converted into an epoxy resin (SP value: 10.9), an acrylic resin (SP value: 9.5), polystyrene (SP). Value: 8.5 to 10.3), urethane resin (SP value: 10 to 11), phenol resin (SP value: 11.5), cellulose resin (SP value: 10 to 12), polyester resin (SP value: 10 to 11) and epoxy resins (SP value: 10 to 11), and can be suitably blended with resins having a medium polarity (SP value: 8.5 to 12).
  • the solubility parameter of the organic solvent when the solubility parameter of the organic solvent is not in the above range, the difference in polarity between the metal oxide particle dispersion of the present embodiment and the above resin may increase, and it may be difficult to obtain a transparent paint. is there. Further, when forming a coating film using a paint containing the metal oxide particle dispersion of this embodiment, or when removing the solvent from the paint, the metal oxide particles may agglomerate or gel. is there.
  • Examples of the organic solvent in the present embodiment include methyl isobutyl ketone (SP value: 8.4), butyl acetate (SP value: 8.5), ethyl acrylate (SP value: 8.6), diacetone alcohol ( SP value: 9.2), methyl ethyl ketone (SP value: 9.3), cyclohexanone (SP value: 9.9), 1-methoxy-2-propanol (SP value: 9.5), dodecanol (SP value: 9) 8-10.3), cyclopentanone (SP value: 10.4), 2,3-butanediol (SP value: 11.1), 1-propanol (SP value: 11.9), and the like. .
  • the solubility parameter ((cal / cm) 1/2 ) is, for example, J. It can be calculated by the method described in VII 675 to 713 of “Polymer Handbook fourth edition” by Brandrup et al. (Especially formulas B3 and B8). In addition, the values in Table 1 (VII 711), Table 7 (VII 688-694), and Table 8 (VII 694-697) in the above document can be used.
  • the boiling point of the organic solvent is preferably 80 ° C. or higher. If the boiling point of the organic solvent is 80 ° C. or higher, the metal oxide particle dispersion of this embodiment is blended into the paint, and then the solvent is removed from the paint when forming a coating film using the paint. In this case, an appropriate volatilization rate is obtained and segregation of the metal oxide particles can be suppressed.
  • Examples of the organic solvent having a solubility parameter of 8.0 or more and 12 or less and a solubility in water of 1.5 g / 100 ml or more include methyl isobutyl ketone (MIBK), cyclohexanone, diacetone alcohol, 1-methoxy- Examples include 2-propanol (PGM), isopropanol, methyl ethyl ketone (MEK), and ethyl acetate.
  • a solvent having a solubility parameter of 8.0 or more and 12 or less and a solubility in water of 1.5 g / 100 ml or more may be used alone, or a mixed solvent in which two or more kinds are mixed. May be.
  • the solvent in the present embodiment removes the solvent from the coating speed and the drying speed when forming a coating film using a paint containing the metal oxide particle dispersion liquid of the present embodiment in addition to the organic solvent described above.
  • a high boiling point solvent, a dispersing agent or the like may be included.
  • This high boiling point solvent is also preferably a solvent having a solubility parameter of 8.0 or more and 12 or less and a solubility in water of 1.5 g / 100 ml or more.
  • the organic solvent contained in the metal oxide particle dispersion is preferably a solvent having a solubility parameter of 8.0 or more and 12 or less and a solubility in water of 1.5 g / 100 ml or more.
  • the solubility parameter is 8.0 or more and 12 or less
  • the organic solvent other than the organic solvent whose solubility in water is 1.5 g / 100 ml or more
  • the organic solvent may be contained.
  • the amine having 2 or more carbon atoms in the present embodiment plays a role as a catalyst in the surface treatment of the metal oxide particles by the silicon compound.
  • the amine having 2 or more carbon atoms in the present embodiment also serves as a dispersant for the metal oxide particles, and suppresses the progress of the surface treatment reaction in a state where the metal oxide particles are aggregated.
  • amines with 2 or more carbon atoms have their substituents interacting with the metal oxide particles, so the hydrolysis reaction proceeds on the surface of the metal oxide particles and the progress of condensation between silicon compounds is suppressed. And it plays the role of facilitating the surface treatment reaction of the metal oxide particles by the silicon compound. Therefore, the amine in this embodiment preferably has 6 or more carbon atoms, and more preferably has 10 or more carbon atoms.
  • Examples of the amine having 2 or more carbon atoms in the present embodiment include alkanolamines such as monoethanolamine, diethanolamine, triethanolamine, monoisopropanolamine, diisopropanolamine, and triisopropanolamine; monoethylamine, diethylamine, Aliphatic polyamines such as triethylamine, ethylenediamine, isopropylamine, diethylenetriamine, 2-ethylhexylamine, triethylenetetramine, and tetraethylenepentamine; aniline, o-toluidine, methylene orthochloramine, 4,4'-diphenylmethanediamine, 2, Aromatic polyamines such as 4'-tolylenediamine, 2,6'-tolylenediamine, and 4-aminobenzoic acid; polyaminoamides, polyamides And the like; key role polyaminoamide, polyoxyethylene alkyl amines, polyester polyamines, and polymers having an amino
  • polymers having amino groups such as polyaminoamide and polyalkylolaminoamide that also have a function as a dispersibility / dispersion aid of the metal oxide particles are preferable. .
  • the product of the amine value of an amine having 2 or more carbon atoms and the content of the amine having 2 or more carbon atoms that is, (amine value of an amine having 2 or more carbon atoms) ⁇ (metal of this embodiment)
  • the content (mass%) of the amine having 2 or more carbon atoms with respect to the whole oxide particle dispersion is preferably 10 or more and 45 or less, and more preferably 25 or more and 42 or less. If the product of the amine value of an amine having 2 or more carbon atoms and the content of an amine having 2 or more carbon atoms is less than 10, the amount of amine as a reaction catalyst is small, so the hydrolysis reaction of the silicon compound May not progress sufficiently.
  • the content of water in the metal oxide particle dispersion of this embodiment is 3% by mass or less of the content of metal oxide particles. That is, when the content of the metal oxide particles in the metal oxide particle dispersion is 100% by mass, the content of water in the metal oxide particle dispersion is 3% by mass of the content of the metal oxide particles. It is as follows. If the water content exceeds 3% by mass of the metal oxide particle content, the temporal stability in the metal oxide particle dispersion may be impaired.
  • the metal oxide particle dispersion of this embodiment is blended with a paint containing a resin with a medium polarity (SP value: 8.5 to 12), and a coating film is formed using the paint.
  • the solubility parameter of water is as high as 23.4
  • the polarity in the coating becomes higher as the solvent evaporates from the coating film.
  • metal oxide particles may aggregate or segregate.
  • the stability over time of the metal oxide particle dispersion of the present embodiment means that the metal oxide particles are less likely to aggregate over time, and the metal oxide particles are stably dispersed in the solvent over a long period of time. It is the performance to do.
  • the metal oxide particle dispersion liquid of this embodiment contains an amount of water necessary for the hydrolysis of the silicon compound
  • the water content is preferably as small as possible.
  • the content of water in the metal oxide particle dispersion is preferably 1.2% by mass or less based on the entire metal oxide particle dispersion.
  • the temporal stability of the metal oxide particle dispersion can be further improved.
  • the content of water necessary for the hydrolysis of the silicon compound is an amount by which hydrolysis necessary for the surface treatment of the metal oxide particles with the silicon compound proceeds, and all the hydrolysis proceeds (hydrolysis).
  • the water content may be less than that required for a rate of 100%).
  • attached water of metal oxide particles and bound water can be used for the surface treatment reaction.
  • the content of the metal oxide particles in the metal oxide particle dispersion of the present embodiment is preferably 10% by mass or more and 60% by mass or less with respect to the entire metal oxide particle dispersion of the present embodiment. 20 mass% or more and 50 mass% or less is more preferable, and 30 mass% or more and 50 mass% or less is further more preferable. If the content of the metal oxide particles in the metal oxide particle dispersion is 10% by mass or more, the amount of the solvent in the paint is an appropriate amount when the metal oxide particle dispersion is used in a paint or the like. Therefore, the cost of the solvent can be suppressed. Moreover, the cost at the time of removing a solvent from the coating film formed using the coating material can also be suppressed.
  • the content of the metal oxide particles is 60% by mass or less, an appropriate interaction between the metal oxide particles can be obtained.
  • inconveniences such as increase in the viscosity of the metal oxide particle dispersion or gelation of the metal oxide particle dispersion are unlikely to occur, and the excellent temporal stability of the metal oxide particle dispersion can be maintained.
  • ⁇ ⁇ 1 (generally ⁇ ⁇ 0.4) in the following formula (2)
  • the light scattering by the metal oxide particles is Rayleigh scattering.
  • the dispersed particle diameter of the metal oxide particles in the metal oxide particle dispersion is larger than the wavelength of light, light scattering by the metal oxide particles is Mie scattering.
  • ⁇ ⁇ ⁇ D / ⁇ (2)
  • ⁇ is a particle size parameter
  • D is a dispersed particle size of metal oxide particles
  • ⁇ is a wavelength of light.
  • the dispersed particle diameter of the metal oxide particles exceeds about 50 nm, Mie scattering with higher scattering intensity is performed instead of Rayleigh scattering. Since the scattering intensity depends not only on the dispersed particle diameter of the metal oxide particles but also on the refractive index of the metal oxide particles, in particular, the metal oxide particle dispersion including metal oxide particles having a refractive index of 1.9 or more. In order to increase the transparency of the liquid, it is important to maintain the dispersed particle size of the metal oxide particles at about 50 nm or less.
  • the particle size (D90) when the cumulative volume percentage of the particle size distribution of the metal oxide particle dispersion of this embodiment is 90% is preferably 60 nm or less, and preferably 50 nm or less. More preferred. If the particle size (D90) when the cumulative volume percentage of the particle size distribution of the metal oxide particle dispersion is 90% is 60 nm or less, the transparency of the metal oxide particle dispersion can be further increased.
  • the particle size distribution (D90) when the cumulative volume percentage of the particle size distribution is 90% is used in the metal oxide particle dispersion of this embodiment.
  • the value divided by the particle size (D50) when the cumulative volume percentage is 50% is preferably 3 or less, and more preferably 2 or less.
  • the metal oxide containing metal oxide particles having an average primary particle diameter of 10 nm or more and 20 nm or more.
  • D90 / D50 is 3 or less.
  • the lower limit of D90 / D50 is 1 or more.
  • the metal oxide particle dispersion of the present embodiment has a liquid haze value of preferably 35% or less, more preferably 27% or less, and preferably 22% or less when measured on the basis of air. Further preferred. If the liquid haze value of the metal oxide particle dispersion is 35% or less, the coating film formed using the paint by mixing the metal oxide particle dispersion in the paint has an appropriate light scattering, The coating is suitable for specifications in optical applications. Moreover, when it is used as a protective layer or the like, there is no risk of impairing the design of the underlayer.
  • the metal oxide particle dispersion of this embodiment preferably has a liquid haze value of 35% or less when the content of metal oxide particles is 30% by mass and the optical path length is 2 mm. % Or less is more preferable, and 22% or less is more preferable.
  • the metal oxide particle content is 30% by mass and the optical path length is 2 mm
  • the liquid haze value of the metal oxide particle dispersion is 35% or less, the metal oxide particle dispersion is applied to the paint.
  • the coating film formed by blending and using the coating material has moderate scattering of light, and the coating film is suitable for specifications in optical applications. Further, when used as a protective layer or the like, there is no risk of impairing the design of the underlayer.
  • the liquid haze value is preferably 25% or less when the content of the metal oxide particles is 10% by mass and the optical path length is 2 mm. % Or less is more preferable, and 15% or less is still more preferable.
  • the metal oxide particle content is 10% by mass and the optical path length is 2 mm
  • the liquid haze value of the metal oxide particle dispersion is 25% or less, the metal oxide particle dispersion is added to the paint.
  • the coating film formed using the coating material has moderate light scattering, and the coating film is suitable for the specifications for optical applications. Further, when used as a protective layer or the like, there is no risk of impairing the design of the underlayer.
  • the “haze value” is a ratio (%) of diffuse transmitted light to total light transmitted light.
  • the “liquid haze value” is a haze value of the metal oxide particle dispersion measured with a haze meter (trade name: HAZE METER TC-H3DP, manufactured by Tokyo Denshoku Co., Ltd.) using a 2 mm cuvette.
  • the metal oxide particle dispersion of the present embodiment may contain other components such as a dispersant, a photosensitizer, and a resin.
  • a bead mill, a ball mill, a homogenizer, a disper, a stirrer and the like using the above media are preferably used.
  • amine or water may be added to the suspension, or may be added during the surface treatment reaction of the metal oxide particles.
  • amine or water can be added stepwise or continuously in order to adjust the reaction rate of the surface treatment reaction of the metal oxide particles.
  • a bead mill, a ball mill, a homogenizer, a disper, a stirrer, or the like using media such as zirconia beads is preferably used.
  • amine or water can be added stepwise or continuously in order to adjust the reaction rate of the surface treatment reaction of the metal oxide particles.
  • an amine having 2 or more carbon atoms is used as a reaction catalyst in a medium polarity organic solvent without using a binder.
  • the metal oxide particles can be surface-treated with the silicon compound by an interaction such as a covalent bond between the silicon compound represented by (II) and the metal oxide particles.
  • a metal oxide particle dispersion having high transparency, excellent dispersion stability of the metal oxide particles, and excellent long-term storage stability of the dispersion can be obtained.
  • the metal oxide particle-containing composition of the present embodiment comprises the metal oxide particle dispersion liquid of the present embodiment and a binder component.
  • Binder component Although a binder component is not specifically limited, for example, a resin monomer, a resin oligomer, a resin polymer, an organosilicon compound, its polymer, etc. can be used conveniently.
  • the binder component in applications such as a display device is not particularly limited as long as it is a monomer, oligomer, or polymer of a curable resin used for a general hard coat film.
  • a polymer may be used and a monomer or oligomer of a thermosetting resin may be used.
  • the monomer of the photocurable resin include radical polymerization monomers such as monofunctional acrylate, bifunctional acrylate, trifunctional acrylate, and 4-6 functional acrylate, alicyclic epoxy resin, glycidyl ether epoxy resin, urethane vinyl ether, And cationic polymerization monomers such as polyester vinyl ether.
  • photocurable resin oligomers and polymers examples include, for example, epoxy acrylate, urethane acrylate, polyester acrylate, copolymer acrylate, polybutadiene acrylate, silicon acrylate, amino resin acrylate, and other radical polymerization oligomers, polymers, and alicyclic epoxies.
  • examples thereof include cationic polymerization oligomers and polymers such as resins, glycidyl ether epoxy resins, urethane vinyl ethers, and polyester vinyl ethers.
  • radically polymerizable monomers, oligomers, and polymers that can be easily blended with a plurality of components and can suppress a curing failure by using a photoinitiator and a light stabilizer are preferably used.
  • a radical polymerization polyfunctional monomer such as dipentaristol hexaacrylate is preferably used.
  • radical polymerization oligomers and polymers such as urethane acrylate are preferably used.
  • the monomers, oligomers and polymers of these photopolymerizable resins can be used alone, or two or more kinds can be mixed and used in accordance with the required function.
  • Examples of the functional group other than the acryloyl group and methacryloyl group of the polyfunctional monomer include a vinyl group, an allyl group, an allyl ether group, a styryl group, and a hydroxyl group.
  • polyfunctional acrylate examples include, for example, (meth) trimethylolpropane triacrylate, (meth) ditrimethylolpropane tetraacrylate, (meth) pentaerythritol triacrylate, (meth) pentaerythritol tetraacrylate, (meth) dipenta
  • polyol polyacrylates such as erythritol hexaacrylate, epoxy (meth) acrylates, polyester (meth) acrylates, urethane acrylates, and polysiloxane acrylates. These polyfunctional acrylates may be used alone or in combination of two or more.
  • the functional group has one or two functional groups as long as the effects of the invention are not inhibited, and monomers, oligomers, dispersants not included in the above-mentioned monomers, Polymerization initiator, antistatic agent, refractive index regulator, antioxidant, ultraviolet absorber, light stabilizer, leveling agent, antifoaming agent, inorganic filler, coupling agent, preservative, plasticizer, flow regulator
  • various general additives such as a thickener, a pH adjuster, and a polymerization initiator may be appropriately contained.
  • dispersant examples include anionic surfactants such as sulfate esters, carboxylic acids, and polycarboxylic acids, cationic surfactants such as quaternary salts of higher aliphatic amines, higher fatty acid polyethylene glycol esters, and the like.
  • anionic surfactants such as sulfate esters, carboxylic acids, and polycarboxylic acids
  • cationic surfactants such as quaternary salts of higher aliphatic amines, higher fatty acid polyethylene glycol esters, and the like.
  • Nonionic surfactants silicon surfactants, fluorine surfactants, polymer surfactants having an amide ester bond, and the like.
  • the polymerization initiator is appropriately selected according to the type of monomer used.
  • a photopolymerization initiator is used.
  • the kind and amount of the photopolymerization initiator are appropriately selected according to the monomer of the photocurable resin to be used.
  • the photopolymerization initiator for example, benzophenone, diketone, acetophenone, benzoin, thioxanthone, quinone, benzyldimethyl ketal, alkylphenone, acylphosphine oxide, phenylphosphine oxide, and the like are known. The photoinitiator of this is mentioned.
  • the viscosity is 0.2 mPa ⁇ s or more and 500 mPa ⁇ s in order to facilitate coating. or less, more preferably 0.5 mPa ⁇ s or more and 200 mPa ⁇ s or less. If the viscosity of the metal oxide particle-containing composition is 0.2 mPa ⁇ s or more, it is preferable because the film thickness when formed into a coating film does not become too thin and the film thickness can be easily controlled.
  • the viscosity of the metal oxide particle-containing composition is 500 mPa ⁇ s or less, the viscosity is not too high, and the metal oxide particle-containing composition at the time of coating becomes easy to handle, which is preferable.
  • the viscosity of the metal oxide particle-containing composition is preferably adjusted to the above range by appropriately adding an organic solvent to the metal oxide particle-containing composition.
  • the organic solvent is not particularly limited as long as it is compatible with the metal oxide particle-containing composition.
  • aliphatic hydrocarbons such as hexane, heptane and cyclohexane, aromatic hydrocarbons such as toluene and xylene, alcohols such as methanol, ethanol and propanol, halogenated carbonization such as methylene chloride and ethylene chloride Hydrogens, acetone, methyl ethyl ketone, methyl isobutyl ketone, ketones such as 2-pentanone and isophorone, esters such as ethyl acetate and butyl acetate, cellosolves such as ethyl cellosolve, propylene glycol monomethyl ether, and propylene glycol monoethyl Examples include ethers such as ether
  • the metal oxide particle-containing composition of the present embodiment contains the metal oxide particle dispersion of the present invention that is highly transparent and excellent in dispersion stability of the metal oxide particles. For this reason, it is excellent in the dispersion stability of a metal oxide particle, and is excellent also in the stability of long-term storage of a composition.
  • Method for producing metal oxide particle-containing composition As a manufacturing method of the metal oxide particle containing composition of this embodiment, the method of mixing each material mentioned above as a component of a metal oxide particle containing composition mechanically is mentioned.
  • the mixing device include a stirrer, a self-revolving mixer, a homogenizer, and an ultrasonic homogenizer.
  • the coating film of this embodiment is formed using the metal oxide particle containing composition of this embodiment.
  • the film thickness of this coating film is appropriately adjusted depending on the application, but is usually preferably 0.01 ⁇ m or more and 20 ⁇ m or less, more preferably 0.5 ⁇ m or more and 10 ⁇ m or less, and more preferably 0.5 ⁇ m or more. And it is more preferable that it is 2 micrometers or less.
  • the manufacturing method of the coating film of this embodiment has the process of forming a coating film by apply
  • the coating method for forming a coating film include a bar coating method, a flow coating method, a dip coating method, a spin coating method, a roll coating method, a spray coating method, a meniscus coating method, a gravure coating method, a suction coating method, A normal wet coating method such as a brush coating method is used.
  • a method of appropriately selecting according to the kind of the binder component and performing thermal curing or photocuring is used.
  • the energy ray used for photocuring is not particularly limited as long as the coating is cured.
  • energy rays such as ultraviolet rays, far infrared rays, near ultraviolet rays, infrared rays, X-rays, ⁇ rays, electron beams, proton rays, and neutron rays are used.
  • ultraviolet rays such as ultraviolet rays, far infrared rays, near ultraviolet rays, infrared rays, X-rays, ⁇ rays, electron beams, proton rays, and neutron rays are used.
  • ultraviolet rays it is preferable to use ultraviolet rays because the curing speed is fast and the device is easily available and handled.
  • ultraviolet rays are emitted at an energy of 100 to 3,000 mJ / cm 2 using a high-pressure mercury lamp, metal halide lamp, xenon lamp, chemical lamp, etc. that generates ultraviolet rays in a wavelength band of 200 nm to 500 nm.
  • a high-pressure mercury lamp, metal halide lamp, xenon lamp, chemical lamp, etc. that generates ultraviolet rays in a wavelength band of 200 nm to 500 nm.
  • the method of irradiating etc. is mentioned.
  • the coating film of this embodiment is formed using the metal oxide particle-containing composition.
  • the metal oxide particles contained in the metal oxide particle-containing composition have a sharp particle size distribution, in other words, the size of the metal oxide particles is almost uniform. For this reason, the metal oxide particles are easily uniformly filled in the coating film without any gaps.
  • the resulting coating film is excellent in film formability, and the performance at all locations in the film surface is uniform. Therefore, for example, since the refractive index in the film surface becomes almost uniform, the occurrence of uneven color in the coating film is suppressed. When applied to a display device or the like, visibility can be improved.
  • the metal oxide particles having a sharp particle size distribution are used in the coating film of this embodiment, the metal oxide particles are uniformly filled in the film, and there are few voids in the film. Therefore, for example, when it is desired to improve the refractive index using metal oxide particles having a refractive index of 1.9 or more, it is possible to reduce the amount of metal oxide particles necessary to improve the refractive index than before. it can. Accordingly, even in a thin film of 10 nm to 200 nm, the entire coating film is uniformly filled with metal oxide particles, and the voids in the film can be reduced uniformly, thereby improving the refractive index of the coating film. be able to.
  • the coating film of this embodiment since the performance in all the places in a film surface becomes uniform, generation
  • the silicon compound has a polymerizable unsaturated group-containing functional group
  • the metal oxide particles are bonded to the resin at the time of curing, so that they aggregate in the film at the time of curing or the particle distribution differs between the surface and the inside of the film. It is suitable because it is suppressed.
  • the coating film of this embodiment may be a thin film for adjusting the refractive index.
  • the thick film which can adjust a refractive index and also has hard-coat property may be sufficient.
  • the coating film of this embodiment can be used for various uses.
  • the coating film of the present embodiment since it is formed using the metal oxide particle-containing composition of the present embodiment, a coating film excellent in transparency and film formability can be obtained.
  • the plastic substrate with a coating film of this embodiment has a base body (plastic base material) formed using a resin material and a coating film of this embodiment provided on at least one surface of the base body.
  • the plastic substrate with a coating film is formed by coating the metal oxide particle-containing composition of the present embodiment on a substrate body using a known coating method, and curing the coating film. Is obtained.
  • the substrate body is not particularly limited as long as it is a plastic substrate.
  • plastic substrate those formed from plastics such as polyethylene terephthalate, triacetyl cellulose, acrylic, acryl-styryl copolymer, acrylonitrile-butadiene-styrene copolymer, polystyrene, polyethylene, polypropylene, polycarbonate, vinyl chloride and the like are used.
  • plastic substrate having optical transparency as the substrate body.
  • the substrate body may be in the form of a sheet or film, but is preferably in the form of a film.
  • the plastic substrate with a coating film of the present embodiment has a haze value of preferably 1.4% or less, more preferably 1.0% or less, when measured on the basis of air.
  • the “haze value” is a ratio (%) of diffuse transmitted light to total light transmitted light, and a haze meter NDH-2000 (manufactured by Nippon Denshoku Co., Ltd.) is used on the basis of air. It means a value measured based on the standard JIS-K-7136.
  • the plastic substrate with a coating film of this embodiment may be provided with a hard coat film between the plastic substrate and the coating film. You may laminate
  • the coating film of the present embodiment since the coating film of the present embodiment is formed, a plastic substrate with a coating film having excellent transparency and film forming property can be obtained.
  • the display device of this embodiment includes one or both of the coating film of this embodiment and the plastic substrate with a coating film of this embodiment.
  • the display device is not particularly limited, but in this embodiment, a liquid crystal display device for a touch panel will be described.
  • the refractive index of a transparent base material and an ITO electrode is provided by providing the coating film of this embodiment which selected the metal oxide particle with a refractive index of 1.9 or more as a layer between a transparent base material and an ITO electrode. The difference can be relaxed and the bone appearance phenomenon can be suppressed.
  • the method of providing either one or both of the coating film of this embodiment and the plastic substrate with a coating film of this embodiment on the touch panel is not particularly limited.
  • the display device of this embodiment includes either one or both of the coating film of this embodiment and the plastic substrate with a coating film of this embodiment, which are excellent in transparency and film forming property. Since there is almost no variation in the optical characteristics within the surface of the coating film, the display device is excellent in visibility.
  • Example 1 "Metal oxide particle dispersion" Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.1% After mixing mass%, water 0.6 mass%, and methyl isobutyl ketone (MIBK) 64.7 mass%, a bead mill was used for dispersion treatment to obtain a metal oxide particle dispersion of Example 1. It was.
  • MIBK methyl isobutyl ketone
  • the temporal stability of the obtained metal oxide particle dispersion was evaluated by particle size distribution after being stored in a refrigerator at 5 ° C. for 90 days and in a thermostat at 25 ° C. for 60 days.
  • the case where the change in D50 was 5 nm or less and the change in D90 was 10 nm or less was rated as ⁇ , and the case where the change in D50 exceeded 5 nm, or the change in D10 exceeded 10 nm was rated as x.
  • Tables 1 and 2 The results are shown in Tables 1 and 2.
  • Example 2 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.2 After mixing mass%, water 0.6 mass% and methyl ethyl ketone (MEK) 64.7 mass%, a bead mill was used for dispersion treatment to obtain a metal oxide particle dispersion of Example 2. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 3 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.3% After mixing mass%, water 0.6 mass%, and methyl ethyl ketone (MEK) 64.6 mass%, the dispersion process was performed using the bead mill, and the metal oxide particle dispersion liquid of Example 3 was obtained. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 4 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.2
  • the metal oxide particles of Example 4 were mixed with a mass%, 0.6 mass% water, and 64.7 mass% 1-methoxy-2-propanol (PGM), and then dispersed using a bead mill. A dispersion was obtained. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 5 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.1% After mixing mass%, water 0.6 mass%, and methyl ethyl ketone (MEK) 64.8 mass%, a dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 5. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 6 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 3.0% by mass, alkyldimethylamine (amine value 140) 0.2 After mixing 6% by mass of 0.6% by mass of water, 0.6% by mass of water and 66.2% by mass of methyl isobutyl ketone (MIBK), dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 6. It was. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 7 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 4.5% by mass, polyester acid amide amine salt (amine value 40) 0
  • dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 7. It was. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 8 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) is 30% by mass, 3-acryloxypropyltrimethoxysilane is 6.0% by mass, and alkyldimethylamine (amine value 140) is 0.3%.
  • the metal oxide particles of Example 8 were mixed with 6 wt% of water, 0.6 wt% of water and 63.1 wt% of 1-methoxy-2-propanol (PGM), and then dispersed using a bead mill. A dispersion was obtained. The moisture content, particle size distribution, liquid haze value, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 9 10% by mass of zirconium (IV) oxide (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement), 1.5% by mass of 3-acryloxypropyltrimethoxysilane, 0.1% of alkyldimethylamine (amine value 140) After mixing 8% by mass of 0.2% by mass of water, 0.2% by mass of water, and 88.2% by mass of methyl isobutyl ketone (MIBK), dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 9. It was. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Tables 1 and 2.
  • Example 10 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 40% by mass, 3-acryloxypropyltrimethoxysilane 6.0% by mass, alkyldimethylamine (amine value 140) 0.3% After mixing 5% by mass, 0.8% by mass of water and 52.9% by mass of methyl isobutyl ketone (MIBK), a dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 10. It was. The moisture content, particle size distribution, liquid haze value, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 11 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 40% by mass, 3-acryloxypropyltrimethoxysilane 6.0% by mass, alkyldimethylamine (amine value 140) 0.3% After mixing 52% by mass of 0.92% by mass of water, 0.92% by mass of water and 52.78% by mass of methyl isobutyl ketone (MIBK), dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 11. It was. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 12 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 40% by mass, 3-acryloxypropyltrimethoxysilane 6.0% by mass, alkyldimethylamine (amine value 140) 0.3% After mixing 50% by mass, 0.95% by mass of water, and 52.75% by mass of methyl isobutyl ketone (MIBK), dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 12. It was. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 13 Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 40% by mass, 3-acryloxypropyltrimethoxysilane 6.0% by mass, alkyldimethylamine (amine value 140) 0.3% After mixing 5% by mass, 1.8% by mass of water and 51.9% by mass of methyl isobutyl ketone (MIBK), a dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 13. It was. The moisture content, particle size distribution, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 14 Zirconium (IV) oxide (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-acryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.23 After mixing 64% by mass of 0.6% by mass of water, 0.6% by mass of water and methyl isobutyl ketone (MIBK), dispersion treatment was performed using a bead mill to obtain a metal oxide particle dispersion of Example 14. It was. The moisture content, particle size distribution, liquid haze value, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 15 Zirconium (IV) oxide (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-acryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.23 After mixing with water, 0.6% by weight of water, 45.07% by weight of methyl isobutyl ketone (MIBK) and 19.6% by weight of toluene (solubility in water 0.035), and then using a bead mill. The metal oxide particle dispersion liquid of Example 15 was obtained by processing. The moisture content, particle size distribution, liquid haze value, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 16 Zirconium (IV) oxide (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-acryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.23 1% by mass, 0.6% by mass of water, 58.17% by mass of methyl isobutyl ketone (MIBK), and 6.5% by mass of toluene (solubility in water 0.035) are dispersed using a bead mill.
  • the metal oxide particle dispersion liquid of Example 16 was obtained by processing.
  • the moisture content, particle size distribution, liquid haze value, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 17 Zirconium (IV) oxide (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-acryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.23 After mixing 1% by mass of mass%, 0.6% by mass of water, 45.07% by mass of methyl isobutyl ketone (MIBK) and 19.6% by mass of methanol (SP value: 14.8, boiling point 65 ° C.), a bead mill is used. Then, a dispersion treatment was performed to obtain a metal oxide particle dispersion of Example 17. The moisture content, particle size distribution, liquid haze value, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Example 18 Zirconium (IV) oxide (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-acryloxypropyltrimethoxysilane 4.5% by mass, alkyldimethylamine (amine value 140) 0.23 After mixing mass%, water 0.6 mass%, methyl isobutyl ketone (MIBK) 58.17 mass% and methanol (SP value: 14.8, boiling point 65 ° C.) 6.5 mass%, a bead mill was used. Then, a dispersion treatment was performed to obtain a metal oxide particle dispersion of Example 18. The moisture content, particle size distribution, liquid haze value, and temporal stability of the obtained metal oxide particle dispersion were measured in the same manner as in Example 1. The results are shown in Table 3 and Table 4.
  • Zirconium oxide (IV) (average primary particle size 12 nm, manufactured by Sumitomo Osaka Cement Co., Ltd.) 30% by mass, 3-methacryloxypropyltrimethoxysilane 4.5% by mass, 1% acetic acid 3.0% by mass, water 0.6% by mass and 11.9% by mass of 1-methoxy-2-propanol (PGM) were mixed and then dispersed using a bead mill. However, the particles settled and the metal oxide particle dispersion was mayben't get.
  • PGM 1-methoxy-2-propanol
  • Example 19 Metal oxide particle-containing composition 62% by mass of the zirconia dispersion of Example 10, urethane acrylate (weight average molecular weight (MW) 20,000 to 40,000) 10.6% by mass, polymerization initiator 0.6% by mass, and polymerization accelerator 0.1% by mass, 6% by mass of isopropyl alcohol, and 20.7% by mass of methyl isobutyl ketone were mixed to obtain a metal oxide particle-containing composition of Example 19.
  • This composition had components other than the solvent, that is, a solid content of 40% by mass, and the content of zirconia in the solid content of 100% by mass was 62% by mass.
  • the particle size distribution of the obtained composition was measured in the same manner as in Example 1. As a result, D50 was 11 nm, D90 was 16 nm, and D90 / D50 was 1.5.
  • the obtained metal oxide particle-containing composition was applied to a 50 ⁇ m thick polyethylene terephthalate film by a bar coating method so that the dry film thickness was 1 ⁇ m, and dried by heating at 90 ° C. for 1 minute. Formed. Next, using a high-pressure mercury lamp (120 W / cm), the coating film was exposed to ultraviolet light with an energy of 250 mJ / cm 2 , and the coating film was cured to obtain a plastic substrate with a coating film of Example 19. .
  • Total light transmittance, haze value The total light transmittance and haze value of the plastic substrate with a coating film were measured based on Japanese Industrial Standard JIS-K-7136 using a haze meter NDH-2000 (manufactured by Nippon Denshoku Co., Ltd.) on the basis of air.
  • a test piece of 100 mm ⁇ 100 mm was produced from the produced plastic substrate with a coating film, and the test piece was used. As a result, the total light transmittance was 89.3%, and the haze value was 0.73%.
  • Example 20 The zirconia dispersion of Example 10 was 71.3% by mass, dipentaerythritol hexaacrylate was 16.3% by mass, the polymerization initiator was 0.6% by mass, the polymerization accelerator was 0.1% by mass, and isopropyl alcohol was 5%.
  • the metal oxide particle-containing composition of Example 20 was obtained by mixing mass% and 6.7 mass% of methyl isobutyl ketone. This composition had components other than the solvent, that is, a solid content of 50% by mass, and the content of zirconia in the solid content of 100% by mass was 57% by mass.
  • the particle size distribution of the obtained composition was measured in the same manner as in Example 1. As a result, D50 was 11 nm, D90 was 16 nm, and D90 / D50 was 1.5.
  • Example 19 the scratch resistance of the plastic substrate with a coating film of Example 20 was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less.
  • Example 1 The day on which the metal oxide particle-containing composition of Example 19 was produced was defined as 0 storage days. The particle size distribution of the composition was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 2 After the metal oxide particle-containing composition of Example 19 was stored in a thermostatic bath at 5 ° C. for 30 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 3 After storing the metal oxide particle-containing composition of Example 19 in a thermostatic bath at 5 ° C. for 60 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 4 After the metal oxide particle-containing composition of Example 19 was stored in a thermostatic bath at 5 ° C. for 90 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 5 After storing the metal oxide particle-containing composition of Example 19 in a thermostatic bath at 25 ° C. for 30 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 6 After storing the metal oxide particle-containing composition of Example 19 in a thermostatic bath at 25 ° C. for 60 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 7 After the metal oxide particle-containing composition of Example 19 was stored in a thermostatic bath at 25 ° C. for 90 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 8 After the metal oxide particle-containing composition of Example 19 was stored in a constant temperature bath at 35 ° C. for 30 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 9 After storing the metal oxide particle-containing composition of Example 19 in a thermostatic bath at 35 ° C. for 60 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • Example 10 After the metal oxide particle-containing composition of Example 19 was stored in a thermostatic bath at 35 ° C. for 90 days, the particle size distribution was measured in the same manner as in Example 1. Moreover, the total light transmittance and haze value of the plastic substrate with a coating film produced in the same manner as in Example 19 were measured using this composition. Further, in the same manner as in Example 19, the scratch resistance of this coated plastic substrate was evaluated. As a result, when the number of scratches was counted visually, it was 10 or less. The results are shown in Table 7.
  • the metal oxide particle dispersion of the present invention can be applied to all industrial uses in which the metal oxide particle dispersion is conventionally used. For example, for optical film use, house exterior use, heat ray shielding use, etc. Can be applied.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

　L'invention concerne une dispersion de particules d'oxyde métallique ayant une grande transparence et une excellente stabilité dans le temps, une composition contenant des particules d'oxyde métallique, un film de revêtement, et un dispositif d'affichage. L'invention concerne une dispersion de particules d'oxyde métallique dans laquelle des particules d'oxyde métallique, traitées en surface avec un composé du silicium représenté par la formule générale (1), sont dispersées dans un solvant, la dispersion de particules d'oxyde métallique étant caractérisée en ce que la dispersion de particules d'oxyde métallique comprend en outre une amine ayant 2 atomes de carbone ou plus, la granulométrie primaire moyenne des particules d'oxyde métallique est de 3 nm à 20 nm, l'indice de réfraction est de 1,9 ou plus, le solvant contient 70 % en masse ou plus d'un solvant organique, le paramètre de solubilité du solvant organique est de 8,0 à 12, et sa solubilité dans l'eau est de 1,5 g/100 ml ou plus, et la teneur en eau est de 3 % en masse ou moins par rapport à la quantité des particules d'oxyde métallique. (1) : R'nSi(OR)m (Dans la formule, R représente un atome d'hydrogène ou un groupe alkyle, R' représente un groupe organique, n et m sont des entiers, n + m = 4, et 0 < n < 4.)
PCT/JP2015/069987 2014-07-14 2015-07-13 Dispersion de particules d'oxyde métallique, composition contenant des particules d'oxyde métallique, film de revêtement et dispositif d'affichage WO2016009979A1 (fr)

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KR1020177001440A KR20170030532A (ko) 2014-07-14 2015-07-13 금속 산화물 입자 분산액, 금속 산화물 입자 함유 조성물, 도막, 및 표시 장치

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CN114405304B (zh) * 2022-02-17 2023-08-08 河北科技大学 一种用于在有机溶剂中分散氧化镍的组合物及分散方法
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