WO2016047231A1 - 着色金属顔料 - Google Patents
着色金属顔料 Download PDFInfo
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- WO2016047231A1 WO2016047231A1 PCT/JP2015/069100 JP2015069100W WO2016047231A1 WO 2016047231 A1 WO2016047231 A1 WO 2016047231A1 JP 2015069100 W JP2015069100 W JP 2015069100W WO 2016047231 A1 WO2016047231 A1 WO 2016047231A1
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- metal
- layer
- pigment
- silicon oxide
- amorphous silicon
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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
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0078—Pigments consisting of flaky, non-metallic substrates, characterised by a surface-region containing free metal
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/0254—Platelets; Flakes
- A61K8/0258—Layered structure
- A61K8/0262—Characterized by the central layer
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0241—Containing particulates characterized by their shape and/or structure
- A61K8/0254—Platelets; Flakes
- A61K8/0258—Layered structure
- A61K8/0266—Characterized by the sequence of layers
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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- A61K8/25—Silicon; Compounds thereof
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
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- A61K8/26—Aluminium; Compounds thereof
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- A—HUMAN NECESSITIES
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
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- A61Q3/02—Nail coatings
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- A—HUMAN NECESSITIES
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- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/22—Oxides; Hydroxides of metals
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- C08K3/36—Silica
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K9/02—Ingredients treated with inorganic substances
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/62—Metallic pigments or fillers
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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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
- C09D201/00—Coating compositions based on unspecified macromolecular compounds
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/36—Pearl essence, e.g. coatings containing platelet-like pigments for pearl lustre
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- 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
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
- A61K2800/436—Interference pigments, e.g. Iridescent, Pearlescent
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/60—Particulates further characterized by their structure or composition
- A61K2800/65—Characterized by the composition of the particulate/core
- A61K2800/651—The particulate/core comprising inorganic material
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/10—Interference pigments characterized by the core material
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- C09C2200/1058—Interference pigments characterized by the core material the core consisting of a metal comprising a protective coating on the metallic layer
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/24—Interference pigments comprising a metallic reflector or absorber layer, which is not adjacent to the core
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- C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
- C09C2200/50—Interference pigments comprising a layer or a core consisting of or comprising discrete particles, e.g. nanometric or submicrometer-sized particles
- C09C2200/502—Metal particles
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- C09C2220/00—Methods of preparing the interference pigments
- C09C2220/10—Wet methods, e.g. co-precipitation
- C09C2220/103—Wet methods, e.g. co-precipitation comprising a drying or calcination step after applying each layer
Definitions
- the color pigment attached to the metal pigment includes diketopyrrolopyrrole, quinacridone, dioxazine, isoindolinone, condensed azo, selenium, perinone, perylene, phthalone, phthalocyanine.
- Organic pigments such as those or inorganic pigments such as iron oxide and carbon black are used.
- the colored metal pigment disclosed in International Publication No. 2007/094253 includes a metal pigment, an amorphous silicon oxide film layer formed on the surface of the metal pigment, and an amorphous silicon oxide film layer.
- the metal layer formed on the surface of the metal layer and the metal particles formed on the surface of the metal layer can be obtained, whereby a good design property can be obtained.
- the colored metal pigment disclosed in JP2012-031232A includes a metal pigment, an amorphous silicon oxide film layer formed on the surface of the metal pigment, and a metal other than silicon oxide. It has a configuration including a metal oxide layer made of an oxide and metal particles formed on the surface of the metal oxide layer, and it is possible to obtain a good design.
- the mechanism by which the colored metal pigments of Patent Document 1 and Patent Document 2 develop color is as follows. That is, an amorphous silicon oxide film layer and a layer made of metal oxide or metal are formed on the surface of the metal pigment that is the base material. Reflected on the surface of the colored metal pigment without being incident on these layers (first reflected light), on the other hand, other light is refracted in these layers and the surface of the metal pigment as the base material (or on each layer) Reflected at the interface) (second reflected light). Therefore, when light is incident on the surface of the colored metal pigment, the length of the optical path of these two reflected lights is different (optical path difference), and the phase difference of the wavelength of the light occurs due to the optical path difference. The light is emphasized and colored.
- the formation of the amorphous silicon oxide film layer provides an effect that an arbitrary refractive index is given and an interference color appears. Moreover, the change of a color tone becomes larger than before by setting it as the layer thickness exceeding 500 nm.
- a method for forming the amorphous silicon oxide film layer for example, a method of stirring or kneading a metal pigment and a solution containing an organosilicon compound in a slurry state or a paste state while maintaining a basic or acidic state can be adopted. Thereby, an amorphous silicon oxide film layer can be formed on the surface of the metal pigment or the surface of the metal pigment on which the underlayer is formed.
- organosilicon compound examples include methyltriethoxysilane, methyltrimethoxysilane, tetraethoxysilane, tetramethoxysilane, tetraisopropoxysilane and the like, and condensates thereof, ⁇ -aminopropyltriethoxysilane, N-2-amino.
- organosilicon compound examples include methyltriethoxysilane, methyltrimethoxysilane, tetraethoxysilane, tetramethoxysilane, tetraisopropoxysilane and the like, and condensates thereof, ⁇ -aminopropyltriethoxysilane, N-2-amino.
- the metal layer may be deposited uniformly or non-uniformly on the surface of the amorphous silicon oxide film layer (or a metal oxide layer described later). For example, even when the thickness of the metal layer is so thin that it cannot be observed by TEM, the metal particles can be densely and uniformly deposited when the metal layer is deposited.
- the adhesion of metal particles is stronger than in the prior art, Excellent color stability against mechanical, thermal and chemical attack. Further, by forming the metal oxide layer on the amorphous silicon oxide film layer, it is possible to obtain a color development different from that of the prior art.
- the thickness of the metal oxide layer is preferably 30 nm or less. In this case, good saturation and interference color are imparted by the resulting colored metal pigment.
- the thickness of the metal oxide layer is preferably further in the range of 0.1 to 10 nm. Note that the metal oxide layer may be deposited uniformly or non-uniformly on the surface of the amorphous silicon oxide film layer. When the metal oxide layer is too thick, the thickness of the resulting colored metal pigment is also increased, and the hiding power is reduced. On the other hand, if it is too thin, a sufficient effect cannot be obtained and the color tone is not stable.
- the thickness of the metal oxide layer can be measured by cross-sectional observation using a transmission electron microscope (TEM).
- Examples of the silane coupling agent include R A —Si (OR B ) 3 or R A —SiR B (OR B ) 2 (R A : C 2-18 alkyl group, aryl group or alkenyl group, R B : Preferred examples include alkyl groups having 1 to 3 carbon atoms. It is also preferred that R A in the above formula has a functional group. Examples of the functional group include an amino group, a ureido group, an epoxy group, a sulfide group, a vinyl group, a methacryloxy (methacrylic) group, an acryloxy (acrylic) group, a mercapto group, and a ketimino group.
- polymerizable monomers having a benzene nucleus examples include styrene, ⁇ -methylstyrene, vinyl toluene, divinyl benzene, phenyl vinyl ketone, phenyl vinyl ether, divinyl benzene monooxide phenoxyethyl acrylate, phenoxy-polyethylene glycol acrylate, 2-hydroxy- Examples include 3-phenoxypropyl acrylate.
- the following monomers may be used for copolymerization.
- performances such as moisture resistance, weather resistance and adhesion of the coating film using the colored metal pigment of the present invention can be further improved.
- the present invention also relates to a resin composition such as paint or ink, which contains at least the above-described colored metal pigment.
- the resin composition in the present invention includes, for example, a paint containing a colored metal pigment and a coating film thereof, a resin molded product or ink and a printed product thereof.
- the change in color tone is very large, for example, it can also be used for a resin composition applied to or formed on an article for authenticity determination.
- the paint and ink either an organic solvent type or an aqueous solution can be adopted.
- water, organic solvents, surfactants, curing agents, ultraviolet absorbers, static eliminating agents, thickeners, and the like can be appropriately blended with the resin composition of the present invention.
- the coating film When a coating film is formed using the resin composition of the present invention, the coating film may be formed on an undercoat layer or an intermediate coating layer by electrodeposition coating or the like, or a coating film by the resin composition of the present invention. A top coat layer may be further formed thereon.
- the present invention also relates to a coated product obtained by coating any of the above resin compositions on a substrate.
- the material of the substrate constituting such a coated material is not particularly limited, and examples thereof include metal, resin, wood, paper, leather and the like.
- ⁇ Others> Surfactant, moisturizer, polyhydric alcohol, water-soluble polymer, film-forming agent, water-insoluble polymer, polymer emulsion, powder, pigment, dye, lake, lower alcohol, UV absorber, vitamins, antioxidant Agent, antibacterial agent, fragrance, water.
- an amorphous silicon oxide film layer is formed on the base layer (amorphous silicon oxide film layer forming step).
- amorphous silicon oxide film layer forming step By hydrolyzing the organosilicon compound and precipitating amorphous silicon oxide on the metal pigment (underlayer) in a solvent mainly composed of a hydrophilic solvent in which the metal pigment forming the underlayer is dispersed, An amorphous silicon oxide film layer is formed on the surface of the metal pigment (underlayer).
- organosilicon compound examples include methyltriethoxysilane, methyltrimethoxysilane, tetraethoxysilane, tetramethoxysilane, tetraisopropoxysilane, and their condensates, ⁇ -aminopropyltriethoxysilane, N-2-aminoethyl, and the like.
- -3-Aminopropyltriethoxysilane, N-2-aminoethyl-3-aminopropylmethyldimethoxysilane, and the like can be used.
- the compound is adsorbed (or bonded) to the surface of the amorphous silicon oxide film layer being formed. Further, since the compound is present on the surface of the amorphous silicon oxide film layer being formed, the organosilicon compound is adsorbed starting from the compound, and the amorphous silicon oxide film layer is formed on the surface of the amorphous silicon oxide film layer being formed. A film is easily formed. The reason for this is not clear, but when the compound is further adsorbed or bonded to the surface of the amorphous silicon oxide film formed on the surface of the metal pigment, it becomes amorphous in the amorphous silicon oxide film layer forming step.
- organic compounds containing nitrogen include acid amides (urea, dimethylformamide, oleic acid amide, stearic acid amide, etc.), amino acids (2-aminobenzoic acid, N-methylglycine, cystine, phenylalanine, etc.), aliphatic amines ( 2-ethylhexylamine, laurylamine, stearylamine, etc.), alkanolamines (2-dimethylaminoethanol, monoethanolamine, diethanolamine, triethanolamine, etc.), nitro compounds (2-nitropropane, nitrocellulose, etc.), amino group-containing Coupling agents (aminophenylsilane, ⁇ -aminopropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, N- ⁇ - (aminoethyl) - ⁇ -aminopropyltrimethoxysilane, ⁇ -ureidopropyltrie Toxisilane,
- a metal particle supporting layer is formed on the surface of the metal pigment covered with the amorphous silicon oxide film layer by the above method. Below, it divides into a metal layer and a metal oxide layer, and demonstrates each.
- a water-soluble metal salt containing any of Al, Ti, Cr, Fe, Co, Ni, Cu, Zn, Ru, Rh, Pd, Ag, Sn, Pt, and Au can be used.
- nitrate, nitrite, sulfate, oxalate, carbonate, chloride, acetate, lactate, sulfamate, fluoride, iodide, cyanide and the like can be used.
- hypophosphorous acid formaldehyde, boron hydride, dimethylamine borane, trimethylamine borane, hydrazine, glucose, tartaric acid and alkali metal salts thereof can be used.
- a surface activation treatment with a solution containing Sn, Pt, Pd, Au or the like is performed on the metal particle supporting layer (that is, the metal layer or the metal oxide layer) as a pretreatment. Also good.
- a step of forming a weather resistant coating layer is included after the metal particle forming step.
- the weather-resistant coating layer contains aluminum and / or silicon, as described above, stirring or kneading the metal pigment having at least metal particles and the solution containing aluminum and / or silicon in a slurry state or a paste state
- a hydrated film can be formed by heating, and then a weatherable film layer comprising a single film or a mixed film of at least one of oxides, hydroxides and hydrates of aluminum and / or silicon can be formed by heating.
- a coupling treatment step is further combined.
- the coupling treatment is performed by stirring or pasting the metal pigment after the metal particles are formed and the solution containing aluminum and / or silicon in a slurry state or a paste state.
- the weather-resistant coating layer contains cerium after kneading
- the metal pigment after the formation of metal particles is added to the solution or dispersion of the cerium compound, and the basic atmosphere is added. It is carried out by a method of adding a coupling agent after stirring or kneading while maintaining the above.
- distribute the metal pigment after the weather-resistant film layer was formed to solvents, such as isopropyl alcohol, and make it a slurry, and add a coupling agent to this slurry, etc. may be employ
- a step (resin coating layer forming step) of forming a resin coating layer may be included after the metal particle forming step.
- the metal pigment having at least metal particles formed is dispersed in a nonpolar solvent such as mineral spirit, heptane, octane, isoparaffin, etc., and the monomer described above is further added, While stirring and mixing at 150 ° C., more preferably 70 to 100 ° C., a polymerization initiator such as benzoyl peroxide, lauroyl peroxide, azobisisobutyronitrile is added. Thereafter, stirring is continued until the monomer is sufficiently polymerized (1 to 20 hours, more preferably 3 to 10 hours). After completion of the reaction, the slurry is solid-liquid separated to obtain a paste-like composition. Can be formed.
- the slurry was subjected to solid-liquid separation using a filter, and an amorphous silicon oxide film layer was formed on the surface of the metal pigment (amorphous silicon oxide film layer forming step).
- the metal pigment in this state is referred to as “silica-coated aluminum pigment”.
- metal particle-carrying layer-covered aluminum pigment obtained above was dispersed in 800 g of electroless silver plating solution containing 3 g of silver nitrate, 2 g of formaldehyde, and 10 g of aqueous ammonia, and kept at 30 ° C. for 1 hour.
- Metal particles (silver particles) were formed on the surface of the metal particle support layer by electrolytic plating (metal particle forming step).
- the metal pigment in this state is referred to as “metal particle-attached aluminum pigment”.
- This metal particle-adhered aluminum pigment is one in which metal particles are uniformly formed on the metal particle support layer at a predetermined interval (that is, the metal particles are formed so as to directly cover a part of the metal particle support layer). ).
- the cross section of 50 colored aluminum pigments thus obtained was observed with a scanning electron microscope.
- the average thickness of the amorphous silicon oxide film layer was 627 nm.
- the thickness of the metal particle support layer (metal oxide layer) was 2 nm, and the average particle diameter of the metal particles was 5 nm. It was uniformly formed on the metal particle support layer (metal oxide layer) with an interval of 5 nm.
- a solution obtained by adding 0.3 g of metal molybdenum powder little by little to 3 g of hydrogen peroxide containing 30% by mass of hydrogen peroxide and reacting the solution was dissolved in 500 g of isopropyl alcohol (hereinafter abbreviated as IPA).
- IPA isopropyl alcohol
- As a commercially available aluminum pigment (flaky aluminum, trade name: “5422NS” (manufactured by Toyo Aluminum Co., Ltd.), solid content: 75% by mass, average particle size: 19 ⁇ m, average thickness: 1 ⁇ m) 30 g) and stirred and mixed at 75 ° C. for 1 hour to obtain a slurry. In this way, a metal pigment having molybdenum oxide formed on the surface as an underlayer was obtained.
- the slurry was subjected to solid-liquid separation using a filter, and an amorphous silicon oxide film layer was formed on the surface of the metal pigment (amorphous silicon oxide film layer forming step).
- the metal pigment in this state is referred to as “silica-coated aluminum pigment”.
- metal oxide layer-coated aluminum pigment obtained above was dispersed in 800 g of an electroless silver plating solution containing 3 g of silver nitrate, 2 g of formaldehyde, and 10 g of aqueous ammonia, and kept at 30 ° C. for 1 hour.
- Metal particles silver particles
- metal particle forming step Metal particles
- the metal pigment in this state is referred to as “metal particle-attached aluminum pigment”.
- This metal particle-attached aluminum pigment is one in which metal particles are uniformly formed on a metal oxide layer at regular intervals (that is, the metal particles are formed so as to directly cover a part of the metal oxide layer).
- the thus obtained metal particle-attached aluminum pigment was solid-liquid separated and dried to obtain a blue colored aluminum pigment.
- the colored aluminum pigment was visually observed, it exhibited an interference color that changed from blue-violet to dark brown depending on the viewing angle, and had a good metallic feeling.
- the cross section of 50 colored aluminum pigments thus obtained was observed with a scanning electron microscope.
- the average thickness of the amorphous silicon oxide film layer was 70 nm.
- the thickness of the metal oxide layer was 2 nm, the average particle diameter of the metal particles was 5 nm, and the metal particles were separated by an interval of 0.5 nm. And uniformly formed on the metal oxide layer.
- the paint was drawn down onto art paper using a 9 mil doctor blade to prepare a coated paper for colorimetry.
- a coated paper for colorimetry was prepared in the same manner.
- variable angle colorimetry system (trade name: “GCMS-4”) and a variable angle spectrophotometer system (trade name: “GSP-2”) (both manufactured by Murakami Color Research Laboratory) ) To measure the color of each of the coated papers.
- GSP-2 variable angle spectrophotometer system
- Example 1 As is clear, when comparing the results of Example 1 and Comparative Example 1, in the a * value in the case of acceptance angle 40 °, the a * value in the case of acceptance angle 80 °, Example 1 The change of the a * value is significantly larger than that of Comparative Example 1. For this reason, it can be seen that the change in color tone according to the viewing angle is larger in the first embodiment. This is presumably because the thickness of the amorphous silicon oxide film layer of Example 1 exceeds 500 nm.
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Abstract
Description
<着色金属顔料>
本発明の着色金属顔料は、金属顔料と、該金属顔料の表面に形成された非晶質酸化珪素膜層と、該非晶質酸化珪素膜層の表面に形成された金属粒子担持層と、該金属粒子担持層の表面に形成された金属粒子と、を少なくとも含み、該金属粒子担持層は、金属層および酸化珪素以外の金属酸化物からなる金属酸化物層のうちいずれか一方または両方であり、該金属粒子は、該金属粒子担持層の一部を直接被覆するように形成されており、該非晶質酸化珪素膜層は、その厚みが500nmを超えることを特徴とする。
本発明で使用される金属顔料としては、たとえばアルミニウム、銅、亜鉛、チタン、鉄、ニッケル、クロムおよびこれらの合金、あるいは金属被覆フレーク状ガラスその他の金属被覆無機顔料等が好ましく例示でき、このうちアルミニウムが意匠性の点で特に好ましく用いられる。アルミニウムを用いた場合、非晶質酸化珪素膜層を形成し、さらに金属粒子を重ねることによって、干渉色を呈する多彩な着色金属顔料が得られる点で有利である。
本発明の着色金属顔料においては、金属顔料の表面に層厚みが500nmを超える非晶質酸化珪素膜層(非晶質酸化珪素により構成される層)が形成されている。この非晶質酸化珪素膜層は、金属顔料の表面の全面に形成されることが好ましいが、金属顔料の表面の一部において非晶質酸化珪素膜層が形成されていない部分が含まれていても、本発明の効果を示す限り本発明の範囲を逸脱するものではない。このような非晶質酸化珪素膜層は金属顔料の表面に直接形成されても良いが、金属顔料と非晶質酸化珪素膜層との間に他の層を下地層として介在させることが好ましい。下地層としては、後述するような、モリブデン、リン、およびアルミニウムからなる群より選ばれる少なくとも1種の元素を含む酸化物、水酸化物、水和物の少なくともいずれかの単独膜または混合物膜からなる層が例示できるが、これに限定されない。また、該下地層は1層または2層以上とされることができ、2層以上の場合は組成の異なる層を積層しても良い。
本発明において、上記の非晶質酸化珪素膜層の表面には、金属粒子担持層が形成される。この金属粒子担持層は、非晶質酸化珪素膜層の表面の全面に形成されることが好ましいが、非晶質酸化珪素膜層の表面の一部において金属粒子担持層が形成されていない部分が含まれていても、本発明の効果を示す限り本発明の範囲を逸脱するものではない。
<金属層>
本発明における金属粒子が、水溶性金属塩を使用して無電解めっきにより形成される場合、金属層は、該無電解めっきの前処理として用いられる方法を用いて形成されることができる。無電解めっきの前処理としては、一般的にキャタリスト(キャタライジングとも称する)-アクセレータ(アクセレーティングとも称する)法と、センシタイジング-アクチベーティング法があり、どちらの方法を用いても良い。また、キャタリストのみまたはセンシタイジングのみを行なっても良い。
本発明においては、非晶質酸化珪素膜層の表面(金属層が先に形成される場合は、金属層の表面、以下において同じ)に、酸化珪素以外の金属酸化物からなる金属酸化物層が形成される。この金属酸化物層は、非晶質酸化珪素膜層の表面の全面に形成されることが好ましいが、非晶質酸化珪素膜層の表面の一部において金属酸化物層が形成されていない部分が含まれていても、本発明の効果を示す限り本発明の範囲を逸脱するものではない。このような金属酸化物層が形成されることにより、後述の金属粒子と金属酸化物層との良好な吸着状態により、金属粒子を一定の間隔を隔てて緻密かつ均一に析出させ、彩度の高い干渉色を発現させることができる。
本発明の着色金属顔料においては、金属粒子が金属粒子担持層の表面に形成される。そして、この金属粒子は、金属粒子担持層の表面の一部を直接被覆するように形成されることを特徴とする。
本発明においては、金属粒子の上に、下記に示すような耐候被膜層等が形成されていても良い。
酸化物、水酸化物、水和物の少なくともいずれかの単独膜または混合物膜からなる耐候被膜層がさらに形成されていることが好ましい。該耐候被膜層を形成することにより、本発明に係る着色金属顔料を配合した塗膜に変色防止効果が付与され、塗膜の耐候性を向上させることができる。特に金属粒子として銀や銅など、酸化反応や硫化反応を起こしやすい金属を使用した場合には、耐候被膜層を形成することにより耐候性が付与されるため有効である。特に、アルミニウム、珪素、セリウムから選ばれる少なくとも1種を含む酸化物、水酸化物、水和物を含む層が好ましい。
金属粒子または上記の耐候被膜層を形成する場合には該耐候被膜層が、カップリング剤、特に珪素および/またはチタンを含むカップリング剤でさらに処理されていることが好ましい。この場合、本発明の着色金属顔料と塗料樹脂等とを含有する樹脂組成物から塗膜を形成する際に着色金属顔料と塗料樹脂との親和性が向上すること等によって、塗膜の密着性の向上効果が得られる。カップリング剤としてはたとえばシランカップリング剤(珪素を含むカップリング剤)が好ましい。シランカップリング剤としては、RA-Si(ORB)3、またはRA-SiRB(ORB)2(RA:炭素数2~18のアルキル基またはアリール基またはアルケニル基、RB:炭素数1~3のアルキル基)等が好ましく例示できる。また上記式中のRAが官能基を有することも好ましい。該官能基としては、アミノ基、ウレイド基、エポキシ基、スルフィド基、ビニル基、メタクリロキシ(メタクリル)基、アクリロキシ(アクリル)基、メルカプト基、ケチミノ基等が挙げられる。
本発明の着色金属顔料に、最外層として樹脂被覆層を形成することにより、該着色金属顔料を配合した塗膜の耐薬品性、耐候性、耐水性、耐湿性等の性能を向上させることができる。これは、本発明の着色金属顔料と塗料樹脂とを配合した樹脂組成物を用いて塗膜を形成する際に、着色金属顔料と塗料樹脂との密着性が向上し、塗膜物性が良好になるためである。
本発明はまた、上記の着色金属顔料を少なくとも含有する、塗料またはインキなどの樹脂組成物に関する。なお、本発明における樹脂組成物には、たとえば着色金属顔料を含む塗料およびその塗膜、樹脂成形品あるいはインキおよびその印刷物が包含される。特に色調の変化が非常に大きいので、例えば、真贋判定を行なうために物品に塗布あるいは形成される樹脂組成物にも用いることができる。塗料およびインキとしては有機溶剤型、水性のいずれも採用可能である。
本発明は、上記の樹脂組成物のいずれかを基体に塗布した塗布物にも関する。このような塗布物を構成する基体の素材は、特に限定されず、例えば金属、樹脂、木材、紙、皮革等を挙げることができる。
本発明はまた、上記の着色金属顔料を少なくとも含有する化粧料に関する。
1)化粧料の種類としては以下のようなものが挙げられる。
メーキャップ化粧料(口紅、ファンデーション、頬紅、アイシャドウ、ネイルエナメルなど)、毛髪化粧料(ヘアージェル、ヘアワックス、ヘアトリートメント、シャンプー、ヘアマニキュアジェルなど)、基礎化粧料(下地クリーム)。
油脂(オリーブ油、ひまし油等)、ロウ類(ミツロウ、カルナバロウ、ラノリンなど)、炭化水素油(流動パラフィン、スクワラン、ポリブテンなど)、脂肪酸エステル(ミリスチン酸イソプロピル、2-エチルヘキサン酸セチル、アジピン酸ジイソプロピル、トリミリスチン酸グリセリルなど)、高級脂肪酸(オレイン酸、イソステアリン酸など)、高級アルコール(イソステアリルアルコール、オレイルアルコールなど)、シリコーン油(ジメチルポリシロキサン、メチルフェニルポリシロキサン、オクタメチルシクロテトラシロキサンなど)、フッ素化合物(パーフルオロポリエーテルなど)。
界面活性剤、保湿剤、多価アルコール、水溶性高分子、皮膜形成剤、非水溶性高分子、高分子エマルション、粉末、顔料、染料、レーキ、低級アルコール、紫外線吸収剤、ビタミン類、酸化防止剤、抗菌剤、香料、水。
化粧料中に着色金属顔料を0.1~99質量%、好ましくは1~80質量%配合する。
特に限定されず通常の化粧料の製造方法が適用できる。
<着色金属顔料の製造方法>
本発明の着色金属顔料は、たとえば以下の製造工程に従って製造され得る。すなわち、金属顔料を分散させた親水性溶剤を主成分とする溶剤中で、有機珪素化合物を加水分解して非晶質酸化珪素を金属顔料上に析出させることにより、金属顔料の表面に非晶質酸化珪素膜層を形成する工程(非晶質酸化珪素膜層形成工程)と、該非晶質酸化珪素膜層の表面に金属粒子担持層を析出させることにより金属粒子担持層を形成する工程(金属粒子担持層形成工程)と、無電解めっき法等により該金属粒子担持層の表面に金属粒子を形成する工程(金属粒子形成工程)とを含む、製造方法により製造することができる。
過酸化水素30質量%を含む過酸化水素水3gに金属モリブデン粉末0.3gを少しずつ加え、反応させて得られた溶液をイソプロピルアルコール(以下IPAと略す)500gに溶解し、さらに、金属顔料として市販のアルミニウム顔料(フレーク状アルミニウム、商品名:「5422NS」(東洋アルミニウム(株)製)、固形分:75質量%、平均粒径:19μm、平均厚み:1μm)を40g(すなわちアルミニウム分として30g)加え、75℃で1時間攪拌混合してスラリーを得た。このようにして、下地層としてモリブデン酸化物がその表面に形成された金属顔料を得た。
特開2012-031232号公報(特許文献2)の実施例1と全く同様の方法により着色金属顔料を作製した。
実施例1で得られた着色アルミニウム顔料をパウダー状にしたもの5gとニトロセルロースラッカー(商品名:「NCクリヤーTY」、斉藤塗料株式会社製)45gとを攪拌機(装置名:「MAZERUSTAR」、倉敷紡績株式会社製)を用いて混合し測色用の塗料を調製した。上記塗料を9milのドクターブレードを用いて、アート紙にドローダウンし測色用の塗紙を作製した。比較例1で得られた着色アルミニウム顔料についても同様にして測色用の塗紙を作製した。
Claims (7)
- 金属顔料と、
前記金属顔料の表面に形成された非晶質酸化珪素膜層と、
前記非晶質酸化珪素膜層の表面に形成された金属粒子担持層と、
前記金属粒子担持層の表面に形成された金属粒子と、を少なくとも含む着色金属顔料であって、
前記金属粒子担持層は、金属層および酸化珪素以外の金属酸化物からなる金属酸化物層のうちいずれか一方または両方からなり、
前記金属粒子は、前記金属粒子担持層の表面の一部を直接被覆するように形成されており、
前記非晶質酸化珪素膜層は、その厚みが500nmを超える、着色金属顔料。 - 前記非晶質酸化珪素膜層は、その厚みが500nmを超え、1000nm以下の範囲内であり、かつ、
前記金属粒子は、その平均粒径が50nm以下である、請求項1に記載の着色金属顔料。 - 前記金属層は、Sn、Pd、Pt、およびAuからなる群より選ばれる少なくとも1種を含み、
前記金属酸化物層は、Mg、Sn、Zn、Co、Ni、Fe、Zr、Ti、およびCeからなる群より選ばれる少なくとも1種の元素の酸化物を含む、請求項1または2に記載の着色金属顔料。 - 前記金属粒子は、Cu、Ni、およびAgからなる群より選ばれる少なくとも1種の元素を含む、請求項1~3のいずれかに記載の着色金属顔料。
- 請求項1~4のいずれかに記載の着色金属顔料を少なくとも含有する樹脂組成物。
- 請求項5に記載の樹脂組成物を基体に塗布した塗布物。
- 請求項1~4のいずれかに記載の着色金属顔料を少なくとも含有する化粧料。
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EP15845352.2A EP3199596B1 (en) | 2014-09-26 | 2015-07-02 | Colored metallic pigment |
US15/508,004 US10106685B2 (en) | 2014-09-26 | 2015-07-02 | Colored metallic pigment |
CN201580032202.7A CN106459613B (zh) | 2014-09-26 | 2015-07-02 | 着色金属颜料 |
KR1020167036118A KR20170005132A (ko) | 2014-09-26 | 2015-07-02 | 착색 금속 안료 |
KR1020187025749A KR101989766B1 (ko) | 2014-09-26 | 2015-07-02 | 착색 금속 안료 |
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JP2014197082A JP6367067B2 (ja) | 2014-09-26 | 2014-09-26 | 着色金属顔料 |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN108219540A (zh) * | 2016-12-21 | 2018-06-29 | 唯亚威解决方案股份有限公司 | 混杂着色金属颜料 |
US11891524B2 (en) | 2016-12-21 | 2024-02-06 | Viavi Solutions Inc. | Pigments having a vapor deposited colorant |
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EP3369784A1 (fr) | 2017-03-02 | 2018-09-05 | The Swatch Group Research and Development Ltd | Pigment interferenciel basé sur un coeur métallique choisi parmit l'au, ag, pd, rh, ru, pt, os, ir et leurs alliages |
JP7340173B2 (ja) * | 2019-03-05 | 2023-09-07 | 東洋アルミニウム株式会社 | 黒色アルミニウム顔料およびその製造方法 |
DE102019211509A1 (de) * | 2019-08-01 | 2021-02-04 | Henkel Ag & Co. Kgaa | Verfahren zur Behandlung von Keratinmaterial, umfassend die Anwendung eines organischen C1-C6-Alkoxy-silans und einer Aminosäure und/oder eines Aminosäurederivats |
DE102019211506A1 (de) * | 2019-08-01 | 2021-02-04 | Henkel Ag & Co. Kgaa | Verfahren zur Färbung von Keratinmaterial, umfassend die Anwendung eines organischen C1-C6-Alkoxy-silans und eines Alkalisierungsmittels |
JP2021038015A (ja) * | 2019-09-05 | 2021-03-11 | 東洋アルミニウム株式会社 | プレススルーパック材及びそれを用いたプレススルーパック |
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- 2015-07-02 CN CN201580032202.7A patent/CN106459613B/zh not_active Ceased
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CN108219540A (zh) * | 2016-12-21 | 2018-06-29 | 唯亚威解决方案股份有限公司 | 混杂着色金属颜料 |
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Also Published As
Publication number | Publication date |
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US20170306160A1 (en) | 2017-10-26 |
CN106459613B (zh) | 2019-03-15 |
KR20180102214A (ko) | 2018-09-14 |
EP3199596A4 (en) | 2018-05-16 |
EP3199596A1 (en) | 2017-08-02 |
JP6367067B2 (ja) | 2018-08-01 |
CN106459613A (zh) | 2017-02-22 |
EP3199596B1 (en) | 2019-05-29 |
KR101989766B1 (ko) | 2019-06-14 |
US10106685B2 (en) | 2018-10-23 |
JP2016069402A (ja) | 2016-05-09 |
KR20170005132A (ko) | 2017-01-11 |
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