WO2021193683A1 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- WO2021193683A1 WO2021193683A1 PCT/JP2021/012120 JP2021012120W WO2021193683A1 WO 2021193683 A1 WO2021193683 A1 WO 2021193683A1 JP 2021012120 W JP2021012120 W JP 2021012120W WO 2021193683 A1 WO2021193683 A1 WO 2021193683A1
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- Prior art keywords
- coating film
- parts
- hydroxyl group
- mass
- colored
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Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08L—COMPOSITIONS OF MACROMOLECULAR 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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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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
- C09D201/02—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups
- C09D201/06—Coating compositions based on unspecified macromolecular compounds characterised by the presence of specified groups, e.g. terminal or pendant functional groups containing oxygen atoms
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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
- 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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- 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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2202/00—Metallic substrate
- B05D2202/10—Metallic substrate based on Fe
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
- B05D2401/20—Aqueous dispersion or solution
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2502/00—Acrylic polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2601/00—Inorganic fillers
- B05D2601/02—Inorganic fillers used for pigmentation effect, e.g. metallic effect
- B05D2601/08—Aluminium flakes or platelets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
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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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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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
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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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
- C08K7/00—Use of ingredients characterised by shape
Definitions
- the present invention relates to a method for forming a multi-layer coating film.
- the purpose of painting the paint is mainly to protect the material and give it an aesthetic appearance.
- aesthetics especially "color and texture” are important from the viewpoint of enhancing the product power.
- the textures of industrial products demanded by consumers are diverse, but in recent years, in the fields of automobile outer panels, automobile parts, home appliances, etc., bright colors with a glossy feel like metal are required (hereinafter referred to as “)”.
- Metallic luster is referred to as "metallic luster").
- the metallic luster is a texture characterized in that the vicinity of the specularly reflected light (highlight) of the coated plate looks brilliant and the oblique direction (shade) looks dark, that is, the brightness difference between the highlight region and the shade region is large. ..
- Patent Document 1 has a multi-layer coating having a metallic base coating film formed of a metallic base coating film containing a coloring pigment and a brilliant pigment, and a coloring base coating film formed of a coloring base coating film containing a coloring pigment.
- a film forming method in which a transparent clear coating film formed by a transparent clear coating film is formed on at least the uppermost layer, the brightness L * value of the metallic base coating film is set to 60 or less, and the wavelength of the coloring base coating film is 400 nm.
- a method for forming a multi-layer coating film is disclosed, which comprises setting the light transmittance of 700 nm or less to 30% or more and 50% or less.
- Patent Document 1 The coating film obtained in Patent Document 1 lacks vividness and metallic luster. Further, in painting, it is required to protect the material as well as to give an aesthetic appearance, and excellent coating film performance such as high water resistance is required.
- the present invention includes the subjects described in the following sections.
- Step (1) A step of coating a colored paint (W) containing a hydroxyl group-containing resin (w1) and a colored pigment (w2) on an object to be coated to form a colored coating film.
- Step (2) A bright pigment dispersion (X) containing a hydroxyl group-containing resin (x1) and a bright pigment (x2) on the colored coating film obtained in the step (1).
- the content of the bright pigment (x2) in the dispersion (X) is in the range of 15 to 80 parts by mass based on 100 parts by mass of the total solid content in the bright pigment dispersion (X).
- a step of coating the bright pigment dispersion (X) to form a bright first base coating film Step (3): A transparent colored second base paint (Y) containing a hydroxyl group-containing resin (y1) and a coloring pigment (y2) is coated on the brilliant first base coating film obtained in the step (2). , The process of forming a transparent colored second base coating film, Step (4): The transparent colored second base coating film obtained in step (3) contains a hydroxyl group-containing acrylic resin (z1) and a polyisocyanate compound (z2), and at least the polyisocyanate compound (z2) is contained.
- a step of applying a clear coating material (Z) containing an aliphatic triisocyanate compound (z2-1) having a molecular weight in the range of 200 to 350 to form a clear coating film and Step (5): By heating the multi-layer coating film including the brilliant first base coating film, the transparent colored second base coating film, and the clear coating film formed in the steps (2) to (4).
- a method for forming a multi-layer coating film which comprises a step of simultaneously curing the multi-layer coating film.
- Item 2 The method for forming a multi-layer coating film according to Item 1, wherein the colored paint (W) is a water-based paint.
- Item 3 The method for forming a multi-layer coating film according to Item 1 or 2, wherein the colored coating material (W) further contains a melamine resin and / or a blocked polyisocyanate compound.
- Item 4. The method for forming a multilayer coating film according to any one of Items 1 to 3, wherein the bright pigment dispersion (X) is a water-based paint.
- Item 5 The method for forming a multilayer coating film according to Item 4, wherein in the bright pigment dispersion (X), the hydroxyl group-containing resin (x1) contains a water-dispersible hydroxyl group-containing acrylic resin (x111).
- the glitter pigment (x2) contains a vapor-deposited aluminum flake pigment, and the content of the vapor-deposited aluminum flake pigment is 15 to 55 based on 100 parts by mass of the total solid content in the glitter pigment dispersion (X).
- Item 8. The method for forming a multilayer coating film according to any one of Items 1 to 5, which is within the range of parts by mass.
- the glitter pigment (x2) contains an aluminum flake pigment, and the content of the aluminum flake pigment is 45 to 80 parts by mass based on 100 parts by mass of the total solid content in the glitter pigment dispersion (X).
- Item 4. The method for forming a multi-layer coating film according to any one of Items 1 to 5, which is within the range of.
- Item 8 The method for forming a multilayer coating film according to any one of Items 1 to 7, wherein the transparent colored second base coating material (Y) is a water-based coating material.
- Item 9 The method for forming a multilayer coating film according to any one of Items 1 to 8, wherein the transparent colored second base coating material (Y) further contains a melamine resin and / or a blocked polyisocyanate compound.
- Item 10 In the clear paint (Z), the equivalent ratio (NCO / OH) of the total mol of the isocyanate groups of the polyisocyanate compound (z2) to the total mol of the hydroxyl groups of the hydroxyl group-containing acrylic resin (z1) is 1.1 to 2. Item 5. The method for forming a multilayer coating film according to any one of Items 1 to 9, which is within the range of 5.
- Item 11 The method for forming a multi-layer coating film according to any one of Items 1 to 10, wherein the film thickness of the brilliant first base coating film is in the range of 0.02 to 7 ⁇ m.
- Item 12. The method for forming a multi-layer coating film according to any one of Items 1 to 11, wherein the film thickness of the transparent colored second base coating film is within the range of 3 to 30 ⁇ m.
- Item 13 The method for forming a multilayer coating film according to any one of Items 1 to 12, wherein in the step (2), the bright pigment dispersion (X) is coated on the colored coating film that has been heat-cured.
- the bright pigment dispersion (X) is coated on the uncured colored coating film, and in the step (5), the coloring formed in the steps (1) to (4) is performed. Items 1 to 12 that cure the multi-layer coating film containing these four coating films at once by simultaneously heating the coating film, the brilliant first base coating film, the transparent colored second base coating film, and the clear coating film. The method for forming a multi-layer coating film according to any one of the above items.
- the method for forming a multi-layer coating film of the present invention it is possible to form a multi-layer coating film which is vivid, has a metallic luster, and exhibits excellent coating film performance such as water resistance.
- the method for forming a multi-layer coating film of the present invention includes the following steps (1) to (5): Step (1): A step of coating a colored paint (W) containing a hydroxyl group-containing resin (w1) and a colored pigment (w2) on an object to be coated to form a colored coating film. Step (2): A bright pigment dispersion (X) containing a hydroxyl group-containing resin (x1) and a bright pigment (x2) on the colored coating film obtained in the step (1).
- the content of the bright pigment (x2) in the dispersion (X) is in the range of 15 to 80 parts by mass based on 100 parts by mass of the total solid content in the bright pigment dispersion (X).
- a step of coating the bright pigment dispersion (X) to form a bright first base coating film Step (3): A transparent colored second base paint (Y) containing a hydroxyl group-containing resin (y1) and a coloring pigment (y2) is coated on the brilliant first base coating film obtained in the step (2). , The process of forming a transparent colored second base coating film, Step (4): The transparent colored second base coating film obtained in step (3) contains a hydroxyl group-containing acrylic resin (z1) and a polyisocyanate compound (z2), and at least the polyisocyanate compound (z2) is contained.
- a step of applying a clear coating material (Z) containing an aliphatic triisocyanate compound (z2-1) having a molecular weight in the range of 200 to 350 to form a clear coating film and Step (5): By heating the multi-layer coating film including the brilliant first base coating film, the transparent colored second base coating film, and the clear coating film formed in the steps (2) to (4).
- This is a method for forming a multi-layer coating film which comprises a step of simultaneously curing the multi-layer coating film.
- a colored coating film (W) containing a hydroxyl group-containing resin (w1) and a coloring pigment (w2) is coated on an object to be coated to form a colored coating film. Will be done.
- the object to be coated to which the colored paint (W) to be coated is applied is not particularly limited.
- the object to be coated include an outer panel portion of an automobile body such as a passenger car, a truck, a motorcycle, and a bus; an automobile part such as a bumper; an outer panel portion of a household electric product such as a mobile phone or an audio device. can. Of these, the outer panel portion of the automobile body and the automobile parts are preferable.
- the material of these objects to be coated is not particularly limited.
- metal materials such as iron, aluminum, brass, copper, tin, stainless steel, zinc-plated steel, zinc alloy (Zn-Al, Zn-Ni, Zn-Fe, etc.) plated steel; polyethylene resin, polypropylene resin, acrylonitrile- Resins such as butadiene-styrene (ABS) resin, polyamide resin, acrylic resin, vinylidene chloride resin, polycarbonate resin, polyurethane resin, epoxy resin, mixtures of these resins, plastic materials such as various fiber reinforced plastics (FRP); glass , Inorganic materials such as cement and concrete; wood; textile materials such as paper and cloth. Of these, metal materials and plastic materials are preferable.
- the object to be coated may be a combination of the above metal material and a plastic material.
- the object to be coated may be a metal surface such as the metal material or a vehicle body formed from the metal material, which may be subjected to surface treatment such as phosphate treatment, chromate treatment, composite oxide treatment, and the like.
- a coating film may be formed on the coating film.
- Examples of the object to be coated with the coating film formed include a substrate to which a surface treatment is applied as necessary and an undercoat coating film is formed on the base material.
- the undercoat coating film is usually formed for the purpose of imparting corrosion resistance, adhesion to a base material, concealment of irregularities on the surface of the base material (sometimes referred to as "base concealment"), and the like.
- NS As the undercoat coating material used for forming the undercoat coating film, a coating material known per se can be used.
- the multi-layer coating film to be formed is anticorrosive. From the viewpoint of properties and the like, it is preferable to use a cationic electrodeposition paint or an anionic electrodeposition paint, and from the viewpoint of chipping resistance and adhesion, it is preferable to use a cationic electrodeposition paint.
- the undercoat paint may be cured by means such as heating and blowing air, or may be dried to the extent that it does not cure.
- a cationic electrodeposition paint or an anionic electrodeposition paint is used as the undercoat paint, a multi-layer coating film having an excellent appearance can be obtained by preventing a mixture between the undercoat coating film and the coating film subsequently formed on the undercoat coating film.
- the coloring paint (W) contains a hydroxyl group-containing resin (w1) and a coloring pigment (w2).
- the form of the colored paint (W) is not particularly limited, and may be any of a water-based paint, an organic solvent type paint, and a solvent-free type paint.
- the water-based paint is a term to be contrasted with the organic solvent-type paint, and generally, water or a medium containing water as a main component (water-based medium), a coating-forming resin, a pigment, or the like is used. Means a paint in which is dispersed and / or dissolved.
- the content of water in the colored paint (W) is preferably 10 to 90% by mass, more preferably 20 to 80% by mass, and further preferably 30 to 70% by mass. It is in the range of%.
- the organic solvent type paint is a paint that does not substantially contain water as a solvent or that all or most of the solvent is an organic solvent.
- the colored paint (W) is preferably a water-based paint from the viewpoint of reducing the environmental load.
- the hydroxyl group-containing resin (w1) is a resin having at least one hydroxyl group in one molecule.
- the hydroxyl group-containing resin (w1) include resins having a hydroxyl group, such as acrylic resin, polyester resin, polyurethane resin, polyolefin resin, polyether resin, polycarbonate resin, epoxy resin, and alkyd resin. These can be used alone or in combination of two or more.
- the hydroxyl group-containing resin (w1) includes a hydroxyl group-containing acrylic resin (w11), a hydroxyl group-containing polyester resin (w12), and a hydroxyl group-containing resin from the viewpoints of water resistance, chipping resistance, finished appearance, and the like of the formed multi-layer coating film.
- Polyurethane resin (w13) can be preferably used.
- the hydroxyl group-containing resin (w1) is a hydroxyl group-containing polyolefin resin (w1) from the viewpoints of water resistance, chipping resistance, finished appearance, etc. of the formed multilayer coating film.
- w14) can be preferably used.
- the content of the hydroxyl group-containing resin (w1) in the colored paint (W) is preferably 1 to 100% by mass, more preferably 10 to 90% by mass, based on the total amount of resin solids in the colored paint (W). %, More preferably in the range of 20 to 80% by mass.
- the colored coating material (W) contains a cross-linking agent having reactivity with the hydroxyl group of the hydroxyl group-containing resin (w1) from the viewpoints of water resistance, chipping resistance, finished appearance, etc. of the formed multi-layer coating film. Is preferable.
- an amino resin, a polyisocyanate compound, a blocked polyisocyanate compound, or the like can be preferably used from the viewpoint of water resistance and adhesiveness of the obtained multilayer coating film.
- the cross-linking agent preferably contains an amino resin and / or a blocked polyisocyanate compound from the viewpoint of storage stability of the obtained colored coating film (W) and water resistance and adhesion of the obtained multi-layer coating film.
- Amino resin is more preferable, and melamine resin described later is particularly preferable.
- amino resin a partially methylolated amino resin or a completely methylolated amino resin obtained by reacting an amino component with an aldehyde component
- amino component examples include melamine, urea, benzoguanamine, acetoguanamine, steroguanamine, spiroguanamine, dicyandiamide and the like.
- aldehyde component examples include formaldehyde, paraformaldehyde, acetaldehyde, benzaldehyde and the like.
- a methylol group of the above methylolated amino resin partially or completely etherified with an appropriate alcohol can also be used.
- alcohols that can be used for etherification include methyl alcohol, ethyl alcohol, n-propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutyl alcohol, 2-ethyl-1-butanol, 2-ethyl-1-hexanol and the like. Can be mentioned.
- the melamine resin is preferable as the amino resin.
- a methyl-butyl mixed etherified melamine resin obtained by partially or completely etherifying the methylol group of a butyl etherified melamine resin or a partially or completely methylolated melamine resin with methyl alcohol and butyl alcohol is preferable.
- the etherified melamine resin is more preferable.
- the total content of the aliphatic polybasic acid and the alicyclic polybasic acid in the acid component of the raw material as the hydroxyl group-containing resin (w1) is high.
- a coating composition using at least one alkyl etherified melamine resin selected from the above-mentioned methyl etherified melamine resin, butyl etherified melamine resin and methyl-butyl mixed etherified melamine resin is particularly preferable as a cross-linking agent. be.
- the weight average molecular weight of the melamine resin is preferably in the range of 400 to 6000, more preferably 700 to 4000, and even more preferably 1000 to 3000.
- melamine resin Commercially available products can be used as the melamine resin, and specifically, for example, "Symel 202", “Symel 203", “Symel 204", “Symel 211", “Symel 238”, “Symel 250”, “Symel 251".
- sulfonic acids such as paratoluene sulfonic acid, dodecylbenzene sulfonic acid, and dinonylnaphthalene sulfonic acid; monobutyl phosphate, dibutyl phosphate, mono 2-ethylhexyl phosphate, and di2-ethylhexyl phosphorus.
- Alkyl phosphate esters such as acids; salts of these acids and amines and the like can be used as catalysts.
- the polyisocyanate compound is a compound having at least two isocyanate groups in one molecule, and is, for example, an aliphatic polyisocyanate, an alicyclic polyisocyanate, an aromatic aliphatic polyisocyanate, an aromatic polyisocyanate, or the polyisocyanate. Derivatives and the like are included.
- aliphatic polyisocyanate examples include trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1,2-propylene diisocyanate, 1,2-butylene diisocyanate, 2,3-butylene diisocyanate, and 1,3.
- -Adiocyanate diisocyanates such as butylene diisocyanate, 2,4,4- or 2,2,4-trimethylhexamethylene diisocyanate, diisocyanate dimerate, methyl 2,6-diisocyanatohexanate (common name: lysine diisocyanate); 2 , 6-Diisocyanatohexanoic acid 2-isocyanatoethyl, 1,6-diisocyanato-3-isocyanatomethylhexane, 1,4,8-triisocyanatooctane, 1,6,11-triisocyanatoundecane, 1, , 8-Diisocyanato-4-isocyanatomethyloctane, 1,3,6-triisocyanatohexane, 2,5,7-trimethyl-1,8-diisocyanato-5-isocyanatomethyloctane and other aliphatic triisocyanates, etc.
- alicyclic polyisocyanate examples include 1,3-cyclopentenediisocyanate, 1,4-cyclohexanediisocyanate, 1,3-cyclohexanediisocyanate, and 3-isocyanatomethyl-3,5,5-trimethylcyclohexylisocyanate (common name).
- Isophorone diisocyanate methyl-2,4-cyclohexanediisocyanate, methyl-2,6-cyclohexanediisocyanate, 1,3- or 1,4-bis (isocyanatomethyl) cyclohexane (common name: hydrogenated xylylene diisocyanate) or The mixture, alicyclic diisocyanates such as norbornenan diisocyanate; 1,3,5-triisocyanatocyclohexane, 1,3,5-trimethylisocyanatocyclohexane, 2- (3-isocyanatopropyl) -2,5-di ( Isocyanatomethyl) -bicyclo (2.2.1) heptane, 2- (3-isocyanatopropyl) -2,6-di (isocyanatomethyl) -bicyclo (2.2.1) heptane, 3- (3) -Isocyanatopropyl) -2,5
- aromatic aliphatic polyisocyanate examples include 1,3- or 1,4-xylylene diisocyanate or a mixture thereof, ⁇ , ⁇ '-diisocyanato-1,4-diethylbenzene, 1,3- or 1,4-bis.
- Arophilic aliphatic diisocyanate such as (1-isocyanato-1-methylethyl) benzene (common name: tetramethylxylylene diisocyanate) or a mixture thereof; aromatic aliphatic triisocyanate such as 1,3,5-triisocyanatomethylbenzene, etc. Can be mentioned.
- aromatic polyisocyanate examples include m-phenylene diisocyanate, p-phenylenedi isocyanate, 4,4'-diphenyldiisocyanate, 1,5-naphthalenediisocyanate, 2,4'-or 4,4'-diphenylmethane diisocyanate or the like.
- Aromatic diisocyanates such as mixtures, 2,4- or 2,6-tolylene diisocyanates or mixtures thereof, 4,4'-toluidine diisocyanates, 4,4'-diphenyl ether diisocyanates; triphenylmethane-4,4', 4'.
- Aromatic triisocyanates such as'-triisocyanate, 1,3,5-triisocyanatobenzene, 2,4,6-triisocyanatotoluene; 4,4'-diphenylmethane-2,2', 5,5'- Aromatic tetraisocyanates such as tetraisocyanates can be mentioned.
- the polyisocyanate and its derivatives may be used alone or in combination of two or more.
- these polyisocyanates it is preferable to use aliphatic diisocyanates, alicyclic diisocyanates and derivatives thereof individually or in combination of two or more.
- polyisocyanate compound a prepolymer obtained by urethanizing the polyisocyanate and its derivative with a polyhydric alcohol, a low molecular weight polyester resin or water under the condition of excess isocyanate group can also be used.
- the polyisocyanate compound usually has an equivalent ratio (NCO / OH) of an isocyanate group in the polyisocyanate compound to a hydroxyl group in the hydroxyl group-containing resin (w1) of 0.5 to. It is preferably used at a ratio of 2.0, particularly in the range of 0.8 to 1.5.
- the blocked polyisocyanate compound is a compound in which the isocyanate group of the polyisocyanate compound is blocked with a blocking agent.
- the blocking agent examples include phenol-based agents such as phenol, cresol, xylenol, nitrophenol, ethylphenol, hydroxydiphenyl, butylphenol, isopropylphenol, nonylphenol, octylphenol, and methyl hydroxybenzoate; Lactams such as ⁇ -butyrolactam and ⁇ -propiolactam; ethers such as ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, propylene glycol monomethyl ether and methoxymethanol.
- phenol-based agents such as phenol, cresol, xylenol, nitrophenol, ethylphenol, hydroxydiphenyl, butylphenol, isopropylphenol, nonylphenol, octylphenol, and methyl hydroxybenzoate
- azole compound examples include pyrazole, 3,5-dimethylpyrazole, 3-methylpyrazole, 4-benzyl-3,5-dimethylpyrazole, 4-nitro-3,5-dimethylpyrazole, 4-bromo-3, Pyrazole or pyrazole derivatives such as 5-dimethylpyrazole, 3-methyl-5-phenylpyrazole; imidazole or imidazole derivatives such as imidazole, benzimidazole, 2-methylimidazole, 2-ethylimidazole, 2-phenylimidazole; 2-methylimidazoline , 2-Pyrazole imidazoline and other imidazoline derivatives.
- an oxime-based blocking agent an active methylene-based blocking agent, pyrazole or a pyrazole derivative is particularly preferable.
- a hydroxycarboxylic acid having one or more hydroxyl groups and one or more carboxyl groups for example, hydroxypivalic acid, dimethylolpropionic acid and the like can also be used.
- the coloring paint (W) is a water-based paint
- a blocked polyisocyanate compound obtained by blocking the isocyanate group with the hydroxycarboxylic acid and then neutralizing the carboxyl group of the hydroxycarboxylic acid to impart water dispersibility is preferable. Can be used for.
- the content of the cross-linking agent is preferably 1 to 50% by mass, more preferably 5 based on the total amount of resin solids in the colored paint (W). It is in the range of ⁇ 45% by mass, more preferably 10 to 40% by mass.
- the content ratio of the hydroxyl group-containing resin (w1) and the cross-linking agent is the water resistance and chipping resistance of the formed multilayer coating film.
- the hydroxyl group-containing resin (w1) is preferably 30 to 99% by mass, more preferably 50 to 95% by mass, based on the total solid content of the hydroxyl group-containing resin (w1) and the cross-linking agent. It is more preferably 55 to 90% by mass, and the cross-linking agent is preferably in the range of 1 to 70% by mass, more preferably 5 to 50% by mass, still more preferably 10 to 45% by mass.
- the coloring paint (W) contains a coloring pigment (w2).
- coloring pigment (w2) examples include titanium oxide, zinc oxide, carbon black, molybdenum red, Prussian blue, cobalt blue, azo pigment, phthalocyanine pigment, quinacridone pigment, isoindolin pigment, and slen pigment.
- examples thereof include perylene-based pigments, dioxazine-based pigments, and diketopyrrolopyrrole-based pigments.
- titanium oxide and carbon black can be preferably used from the viewpoint of hiding the base of the multi-layer coating film to be formed. can.
- the blending amount of the colored pigment (w2) is preferably 1 to 1 to 100 parts by mass based on 100 parts by mass of the resin solid content in the colored paint (W) from the viewpoint of hiding the base of the multi-layer coating film to be formed. It is in the range of 180 parts by mass, more preferably 5 to 160 parts by mass, and even more preferably 15 to 150 parts by mass.
- the colored paint (W) preferably further contains an extender pigment from the viewpoint of chipping resistance and the like of the formed multi-layer coating film.
- extender pigment examples include barium sulfate, talc, clay, kaolin, barium carbonate, calcium carbonate, silica, alumina white and the like, and among them, barium sulfate and / or talc is preferably used.
- the blending amount of the extender pigment is the resin solid content in the colored paint (W) from the viewpoint of chipping resistance and the like of the formed multi-layer coating film. Based on 100 parts by mass, it is preferably in the range of 1 to 180 parts by mass, more preferably 5 to 140 parts by mass, and further preferably 10 to 120 parts by mass.
- the colored paint (W) may further appropriately contain a hydroxyl group-free resin, a bright pigment, an ultraviolet absorber, a light stabilizer, a defoaming agent, a thickener, a surface conditioner, and the like.
- the colored paint (W) can be applied according to a usual method, and examples thereof include air spray coating, airless spray coating, and rotary atomization coating.
- electrostatic coating may be applied as needed.
- electrostatic coating of the rotary atomization method and electrostatic coating of the air spray method are preferable, and the rotary atomization method is used. Electrostatic coating is particularly preferred.
- the colored paint (W) is appropriately added with water and / or an organic solvent and, if necessary, a viscosity modifier, a defoaming agent and the like. It is preferable to contain an agent and adjust the solid content and viscosity suitable for coating.
- the solid content of the colored paint (W) is preferably in the range of 10 to 60% by mass, more preferably 15 to 55% by mass, and further preferably 20 to 50% by mass. Further, the viscosity of the colored paint (W) should be in a range suitable for painting, usually in the range of 500 to 5000 mPa ⁇ s when measured at 20 ° C. and a rotation speed of 6 rpm using a B-type viscometer. It is preferable to appropriately adjust the mixture with water and / or an organic solvent.
- the cured film thickness of the colored coating film is preferably about 5.0 to 40 ⁇ m, more preferably 8.0 to 35 ⁇ m, and even more preferably 10 from the viewpoint of hiding the base of the multi-layer coating film to be formed. It is about 30 ⁇ m.
- the colored coating film may be left uncured and used for forming the glittering first base coating film in the next step (2), or may be heated before coating the glittering pigment dispersion (X). It may be cured.
- the colored coating film is used in the step (2) as it is uncured, the brilliant first base coating film and the transparent colored second base formed in the steps (2) to (4) in the step (5) described later. Since it can be heat-cured together with the coating film and the clear coating film, it is advantageous in terms of energy saving. Further, when the colored coating film is heat-cured before the coating of the bright pigment dispersion (X), the smoothness of the coating film is further improved by polishing the surface of the cured colored coating film by means such as water grinding. be able to.
- the heating means in the case of heat curing, for example, hot air heating, infrared heating, high frequency heating and the like can be used.
- the heating temperature is preferably 80 to 180 ° C, more preferably 100 to 160 ° C.
- the heating time is preferably 10 to 60 minutes, more preferably 15 to 40 minutes. If necessary, before the heat curing is performed, it is directly or indirectly heated at a temperature of about 50 to about 110 ° C., preferably about 60 to about 90 ° C. for about 1 to 60 minutes by preheating, air blowing, or the like. May be done.
- the content of the bright pigment (x2) in the bright pigment dispersion (X) is based on 100 parts by mass of the total solid content in the bright pigment dispersion (X).
- the brilliant pigment dispersion (X) in the range of 15 to 80 parts by mass is coated to form a brilliant first base coating film.
- the form of the glitter pigment dispersion (X) is preferably a water-based paint from the viewpoint of obtaining a multi-layer coating film exhibiting an excellent metallic luster.
- the hydroxyl group-containing resin (x1) is a resin having at least one hydroxyl group in one molecule.
- the hydroxyl group-containing resin (x1) include resins having a hydroxyl group, such as acrylic resin, polyester resin, polyurethane resin, polyolefin resin, polyether resin, polycarbonate resin, epoxy resin, and alkyd resin. These can be used alone or in combination of two or more.
- hydroxyl group-containing resin (x1) it is preferable to use a hydroxyl group-containing acrylic resin (x11) from the viewpoint of water resistance of the formed multilayer coating film.
- hydroxyl group-containing acrylic resin (x11) for example, a hydroxyl group-containing polymerizable unsaturated monomer (a) and another polymerizable unsaturated monomer (b) copolymerizable with the hydroxyl group-containing polymerizable unsaturated monomer are known per se. It can be produced by copolymerizing by the method of the above, for example, a solution polymerization method in an organic solvent, an emulsion polymerization method in water, or the like.
- the hydroxyl group-containing polymerizable unsaturated monomer (a) is a compound having one or more hydroxyl groups and one or more polymerizable unsaturated bonds in one molecule.
- Examples of the hydroxyl group-containing polymerizable unsaturated monomer include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, and 4-hydroxybutyl (meth) acrylate.
- the monomer corresponding to the (xvii) polymerizable unsaturated monomer having an ultraviolet absorbing functional group is another polymerizable monomer copolymerizable with the hydroxyl group-containing polymerizable unsaturated monomer (a). It should be defined as the unsaturated monomer (b) and is excluded from the hydroxyl group-containing polymerizable unsaturated monomer (a).
- the hydroxyl group-containing polymerizable unsaturated monomer (a) can be used alone or in combination of two or more.
- the other polymerizable unsaturated monomer (b) copolymerizable with the hydroxyl group-containing polymerizable unsaturated monomer for example, the following monomers (i) to (xx) can be used. These polymerizable unsaturated monomers can be used alone or in combination of two or more.
- Alkyl or cycloalkyl (meth) acrylate For example, methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl ( Meta) acrylate, tert-butyl (meth) acrylate, n-hexyl (meth) acrylate, n-octyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, nonyl (meth) acrylate, tridecyl (meth) acrylate, lauryl (meth) Meta) acrylate, stearyl (meth) acrylate, isostearyl (meth) acrylate, cyclohexyl (meth) acrylate, methylcyclohexyl (meth) acrylate
- (Vii) Polymerizable unsaturated monomer having an alkyl fluorinated group: perfluoroalkyl (meth) acrylate such as perfluorobutylethyl (meth) acrylate and perfluorooctylethyl (meth) acrylate; fluoroolefin and the like.
- (Viii) A polymerizable unsaturated monomer having a photopolymerizable functional group such as a maleimide group.
- (Ix) Vinyl compound: N-vinylpyrrolidone, ethylene, butadiene, chloroprene, vinyl propionate, vinyl acetate and the like.
- (Xii) Polymerizable unsaturated monomer having two or more polymerizable unsaturated groups in one molecule: allyl (meth) acrylate, ethylene glycol di (meth) acrylate, 1,4-butanediol di (meth) acrylate, neo Pentyl glycol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate and the like.
- Epoxy group-containing polymerizable unsaturated monomer glycidyl (meth) acrylate, ⁇ -methylglycidyl (meth) acrylate, 3,4-epoxycyclohexylmethyl (meth) acrylate, 3,4-epoxycyclohexylethyl (meth) acrylate , 3,4-Epoxycyclohexylpropyl (meth) acrylate, allylglycidyl ether, etc.
- (Xv) Polymerizable unsaturated monomer having a sulfonic acid group: 2-acrylamide-2-methylpropanesulfonic acid, 2-sulfoethyl (meth) acrylate, allylsulfonic acid, 4-styrenesulfonic acid, etc .; sodium salts of these sulfonic acids And ammonium salts, etc.
- (XVii) Polymerizable unsaturated monomer having UV-absorbing functional group: 2-hydroxy-4 (3-methacryloyloxy-2-hydroxypropoxy) benzophenone, 2-hydroxy-4- (3-acryloyloxy-2-hydroxypropoxy) ) Benzophenone, 2,2'-dihydroxy-4- (3-methacryloyloxy-2-hydroxypropoxy) benzophenone, 2,2'-dihydroxy-4- (3-acryloyloxy-2-hydroxypropoxy) benzophenone, 2-[ 2-Hydroxy-5- [2- (methacryloyloxy) ethyl] phenyl] -2H-benzotriazole and the like.
- (Xix) Polymerizable unsaturated monomer having a carbonyl group: acrolein, diacetone acrylamide, diacetone methacrylamide, acetoacetoxyethyl methacrylate, formyl styrene, vinyl alkyl ketone having 4 to 7 carbon atoms (eg, vinyl methyl ketone) , Vinyl ethyl ketone, vinyl butyl ketone), etc.
- (Xx) Polymerizable unsaturated monomer having an acid anhydride group: maleic anhydride, itaconic anhydride, citraconic anhydride and the like.
- the polymerizable unsaturated group means an unsaturated group capable of radical polymerization.
- examples of such polymerizable unsaturated groups include vinyl groups, (meth) acryloyl groups and the like.
- (meth) acrylate means acrylate or methacrylate.
- (Meta) acrylic acid means acrylic acid or methacrylic acid.
- (meth) acryloyl means acryloyl or methacryloyl.
- (meth) acrylamide means acrylamide or methacrylamide.
- the proportion of the hydroxyl group-containing polymerizable unsaturated monomer (a) used in producing the hydroxyl group-containing acrylic resin (x11) is preferably 1 to 45% by mass, preferably 2 to 35% by mass, based on the total amount of the monomer components. % Is more preferable, and 3 to 25% by mass is further preferable.
- the hydroxyl group-containing acrylic resin (x11) contains a water-dispersible hydroxyl group from the viewpoint of water resistance and adhesion of the formed multilayer coating film. It is preferable to contain an acrylic resin (x111).
- the above-mentioned hydroxyl group-containing acrylic resin (x11) is a polymerizable unsaturated monomer having at least two polymerizable unsaturated groups in one molecule.
- (C) and a polymerizable unsaturated monomer having one polymerizable unsaturated group in one molecule is a polymerizable unsaturated monomer having at least two polymerizable unsaturated groups in one molecule based on the total mass.
- (C) A copolymer obtained by copolymerizing 0.1 to 30% by mass and 70 to 99.9% by mass of a polymerizable unsaturated monomer (d) having one polymerizable unsaturated group in one molecule.
- the hydroxyl group-containing polymerizable unsaturated monomer (a) is 1 to 35% by mass
- the hydrophobic polymerizable unsaturated monomer (e) is 5 to 60% by mass.
- Examples of the polymerizable unsaturated monomer (c) having at least two polymerizable unsaturated groups constituting the core in one molecule include allyl (meth) acrylate, ethylene glycoldi (meth) acrylate, and the like.
- the polymerizable unsaturated monomer (c) having at least two polymerizable unsaturated groups in one molecule is preferably 0.1 to 30% by mass based on the total mass of the monomer (c) and the monomer (d). It can be more preferably used in the range of 0.5 to 10% by mass, more preferably 1 to 5% by mass.
- the polymerizable unsaturated monomer (d) having one polymerizable unsaturated group in one molecule constituting the core is a polymerizable unsaturated monomer (c) having at least two polymerizable unsaturated groups in one molecule.
- a polymerizable unsaturated monomer which is a polymerizable unsaturated monomer, and includes a compound containing one polymerizable unsaturated group in one molecule, for example, a vinyl group, a (meth) acryloyl group, an allyl group and the like.
- polymerizable unsaturated monomer (d) having one polymerizable unsaturated group in one molecule examples include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, and isopropyl.
- Polymerizable unsaturated monomer polymerizable unsaturated monomer having an adamantyl group such as adamantyl (meth) acrylate; vinyl aromatic compound such as styrene, ⁇ -methylstyrene, vinyltoluene; 2-hydroxyethyl (meth) acrylicate, Monoesteride of (meth) acrylic acid such as 2-hydroxypropyl (meth) acrylicate, 3-hydroxypropyl (meth) acrylate, 4-hydroxybutyl (meth) acrylate and divalent alcohol having 2 to 8 carbon atoms.
- adamantyl group such as adamantyl (meth) acrylate
- vinyl aromatic compound such as styrene, ⁇ -methylstyrene, vinyltoluene
- 2-hydroxyethyl (meth) acrylicate Monoesteride of (meth) acrylic acid such as 2-hydroxypropyl (meth) acrylicate, 3-hydroxypropyl (meth) acrylate,
- Hydroxyl group-containing polymerizable unsaturated monomer (meth) acrylic acid, maleic acid, crotonic acid, ⁇ -carboxyethyl acrylate and other carboxyl group-containing polymerizable unsaturated monomer; (meth) acrylonitrile, (meth) acrylamide, dimethylaminopropyl Examples thereof include nitrogen-containing polymerizable unsaturated monomers such as (meth) acrylamide, dimethylaminoethyl (meth) acrylate, and adducts of glycidyl (meth) acrylate and amines, which are used alone or in combination of two or more. Can be used.
- the polymerizable unsaturated monomer (d) having one polymerizable unsaturated group in one molecule is preferably 90 to 99.9% by mass, based on the total mass of the monomer (c) and the monomer (d). It can be preferably used in the range of 90 to 99.5% by mass, more preferably 95 to 99% by mass.
- hydroxyl group-containing polymerizable unsaturated monomer (a) constituting the shell for example, 2-hydroxyethyl (meth) acrylicate, 2-hydroxypropyl (meth) acrylicate, 3- Monoesteride of (meth) acrylic acid such as hydroxypropyl (meth) acrylate and 4-hydroxybutyl (meth) acrylate with a dihydric alcohol having 2 to 8 carbon atoms; (meth) acrylic acid and 2 to 8 carbon atoms.
- ⁇ -caprolactone modified product of monoesterified product with dihydric alcohol allylalcohol
- the hydroxyl group-containing polymerizable unsaturated monomer (a) is preferably 1 to 35% by mass, more preferably 5 to 25% by mass, based on the total mass of the monomer (a), the monomer (e) and the monomer (f). More preferably, it can be used in the range of 8 to 20% by mass.
- the hydrophobic polymerizable unsaturated monomer (e) constituting the shell is a polymerizable unsaturated monomer containing a linear, branched or cyclic saturated or unsaturated hydrocarbon group having 6 or more carbon atoms.
- the hydrophobic polymerizable unsaturated monomer (e) is generally 5 to 60% by mass, particularly 8 to 40% by mass, and more particularly 11 based on the total amount of the monomer (a), the monomer (e) and the monomer (f). It is preferably used in the range of ⁇ 25% by mass.
- Examples of the polymerizable unsaturated monomer (f) other than the hydroxyl group-containing polymerizable unsaturated monomer (a) and the hydrophobic polymerizable unsaturated monomer (e) constituting the shell include methyl (meth) acrylate and ethyl ().
- Alkyl (meth) acrylates such as meta) acrylate, n-propyl (meth) acrylate, isopropyl (meth) acrylate, n-butyl (meth) acrylate, isobutyl (meth) acrylate, and tert-butyl (meth) acrylate; (meth) Examples thereof include carboxyl group-containing polymerizable unsaturated monomers such as acrylic acid, maleic acid, crotonic acid, and ⁇ -carboxyethyl acrylate, and these can be used alone or in combination of two or more.
- the polymerizable unsaturated monomer (f) other than the hydroxyl group-containing polymerizable unsaturated monomer (a) and the hydrophobic polymerizable unsaturated monomer (e) is at least one of the components thereof from the viewpoint of ensuring the smoothness of the formed coating film. As a part, it is preferable to contain a carboxyl group-containing polymerizable unsaturated monomer (g).
- Examples of the carboxyl group-containing polymerizable unsaturated monomer (g) include (meth) acrylic acid, maleic acid, crotonic acid, ⁇ -carboxyethyl acrylate, and the like, and among them, (meth) acrylic acid is preferable. Is.
- the carboxyl group-containing polymerizable unsaturated monomer (g) is the monomer (a) from the viewpoint of the stability of the water-dispersible hydroxyl group-containing acrylic resin (x111') in an aqueous medium and the smoothness and water resistance of the formed coating film. , It is generally preferable to use in the range of 1 to 40% by mass, particularly 6 to 25% by mass, and more particularly 11 to 19% by mass based on the total mass of the monomer (e) and the monomer (f).
- the water-dispersible hydroxyl group-containing acrylic resin (x111') is generally 1 to 200 mgKOH / g, particularly 5 to 180 mgKOH / g, and more particularly 7 to 130 mgKOH from the viewpoint of water resistance and adhesion of the formed multi-layer coating film. It is preferable to have a hydroxyl value in the range of / g.
- the water-dispersible hydroxyl group-containing acrylic resin (x111') is generally 1 to 130 mgKOH / g, particularly 5 to 100 mgKOH / g, from the viewpoints of storage stability, water resistance and adhesion of the formed multi-layer coating film. Further, it is particularly preferable to have an acid value in the range of 7 to 70 mgKOH / g. Further, from the viewpoint of water resistance and adhesiveness of the formed multilayer coating, only one polymerizable unsaturated group is contained in one molecule as the monomer (a), the monomer (e) and the monomer (f). It is preferable to use a polymerizable unsaturated monomer and to make the shell of the water-dispersible hydroxyl group-containing acrylic resin (x111') uncrosslinked.
- the water-dispersible hydroxyl group-containing acrylic resin (x111') contains, for example, a polymerizable unsaturated monomer (c) having at least two polymerizable unsaturated groups in one molecule and one polymerizable unsaturated group in one molecule. Based on the total mass of the polymerizable unsaturated monomer (d) having, the polymerizable unsaturated monomer (c) having at least two polymerizable unsaturated groups in one molecule is 0.1 to 30% by mass and the polymerizable unsaturated group.
- hydroxyl group-containing polymerizable unsaturated monomer (a) 1 to 35% by mass, hydrophobic polymerizable unsaturated monomer (e) 5 to 60% by mass, and polymerizable unsaturated monomer other than the above-mentioned monomers (a) and monomer (d). It can be obtained by adding a monomer mixture (II) containing 5 to 94% by mass of the monomer (f) and further polymerizing it.
- the emulsion polymerization of the monomer mixture can be carried out by a method known per se, for example, using a polymerization initiator in the presence of an emulsifier.
- an anionic emulsifier or a nonionic emulsifier is suitable.
- the anionic emulsifier include sodium salts and ammonium salts of organic acids such as alkylsulfonic acid, alkylbenzenesulfonic acid and alkylphosphate, and examples of the nonionic emulsifier include polyoxyethylene oleyl ether.
- Polyoxyethylene stearyl ether Polyoxyethylene lauryl ether, polyoxyethylene tridecyl ether, polyoxyethylene phenyl ether, polyoxyethylene nonylphenyl ether, polyoxyethylene octylphenyl ether, polyoxyethylene monolaurate, polyoxyethylene Examples thereof include monostearate, polyoxyethylene monooleate, sorbitan monolaurate, sorbitan monostearate, sorbitan monostearate, sorbitan triolate, and polyoxyethylene sorbitan monolaurate.
- a reactive anionic emulsifier having the above may be used, and among them, it is preferable to use a reactive anionic emulsifier.
- Examples of the reactive anionic emulsifier include sodium salts and ammonium salts of sulfonic acid compounds having radically polymerizable unsaturated groups such as (meth) allyl group, (meth) acryloyl group, propenyl group and butenyl group. .. Of these, an ammonium salt of a sulfonic acid compound having a radically polymerizable unsaturated group is preferable because the formed coating film has excellent water resistance. Examples of the ammonium salt of the sulfonic acid compound include commercially available products such as "Latemuru S-180A" (trade name, manufactured by Kao Corporation).
- ammonium salts of the sulfonic acid compound having a radically polymerizable unsaturated group the ammonium salt of the sulfonic acid compound having a radically polymerizable unsaturated group and a polyoxyalkylene group is more preferable.
- the ammonium salt of the sulfonic acid compound having a radically polymerizable unsaturated group and a polyoxyalkylene group include "Aqualon KH-10" (trade name, manufactured by Daiichi Kogyo Seiyaku Co., Ltd.) and "SR-1025A" (commodity). Name, commercially available products such as Asahi Denka Kogyo Co., Ltd.) can be mentioned.
- the emulsifier is preferably in the range of 0.1 to 15% by mass, more preferably 0.5 to 10% by mass, still more preferably 1 to 5% by mass, based on the total amount of all the monomers used. Can be used.
- the polymerization initiator may be of any type, oil-soluble or water-soluble, and for example, benzoyl peroxide, octanoyl peroxide, lauroyl peroxide, stearoyl peroxide, cumene hydroperoxide, tert-.
- Organic peroxides such as butyl peroxide, tert-butyl peroxylaurate, tert-butyl peroxyisopropyl carbonate, tert-butyl peroxy acetate, diisopropylbenzene hydroperoxide; azobisisobutyronitrile, azobis (2, 4-Dimethylvaleronitrile), azobis (2-methylpropionnitrile), azobis (2-methylbutyronitrile), 4,4'-azobis (4-cyanobutanoic acid), dimethylazobis (2-methylpropionate) , Azobis [2-methyl-N- (2-hydroxyethyl) -propionamide], azobis ⁇ 2-methyl-N- [2- (1-hydroxybutyl)]-propionamide ⁇ and other azo compounds; , Azobisisobutyric salt such as ammonium persulfate and sodium persulfate. These can be used alone or in combination of two or more.
- a reducing agent such as sugar, sodium formaldehyde sulfoxylate, or iron complex may be used in combination with the above-mentioned polymerization initiator to form a redox polymerization system.
- the above-mentioned polymerization initiator is preferably used in the range of 0.1 to 5% by mass, particularly preferably 0.2 to 3% by mass, based on the total mass of all the monomers used.
- the method of adding the polymerization initiator is not particularly limited, and can be appropriately selected depending on the type and amount thereof.
- the polymerization initiator may be contained in a monomer mixture or an aqueous medium in advance, or may be added all at once at the time of polymerization, or may be added dropwise.
- the water-dispersible hydroxyl group-containing acrylic resin (x111') is obtained by adding the hydroxyl group-containing polymerizable unsaturated monomer (a), the hydrophobic polymerizable unsaturated monomer (e), and the above-mentioned monomer (a) to the emulsion obtained as described above. ) And a monomer mixture (II) containing a polymerizable unsaturated monomer (f) other than the monomer (e), and further polymerizing the mixture.
- the monomer mixture (II) can appropriately contain components such as a polymerization initiator, a chain transfer agent, a reducing agent, and an emulsifier as listed above, if necessary.
- the monomer mixture (II) can be dropped as it is, it is desirable to disperse the monomer mixture (II) in an aqueous medium and drop it as a monomer emulsion.
- the particle size of the monomer emulsion in this case is not particularly limited.
- the polymerization of the monomer mixture (II) can be carried out, for example, by adding the monomer mixture (II) which may be emulsified to the above emulsion in a batch or by dropping, and heating to an appropriate temperature with stirring.
- the water-dispersible hydroxyl group-containing acrylic resin (x111') obtained as described above contains a polymerizable unsaturated monomer (c) having at least two polymerizable unsaturated groups in one molecule and one polymerizable unsaturated group.
- the copolymer (I-1) formed from the monomer mixture (I) containing one polymerizable unsaturated monomer (d) in the molecule is used as the core, and the hydroxyl group-containing polymerizable unsaturated monomer (a) is hydrophobic.
- the water-dispersible hydroxyl group-containing acrylic resin (x111') is polymerized to form another resin layer between the step of obtaining the copolymer (I-1) and the step of obtaining the copolymer (II-1).
- a resin particle composed of three or more layers may be obtained by adding a step of supplying a sex unsaturated monomer (one or a mixture of two or more kinds) to carry out emulsion polymerization.
- the "shell” of the water-dispersible hydroxyl group-containing acrylic resin (x111') means the polymer layer existing in the outermost layer of the resin particles, and the “core” is the inner layer of the resin particles excluding the shell portion. It means a polymer layer, and "core / shell type structure” means a structure having the above-mentioned core and shell.
- the core / shell type structure usually has a layered structure in which the core is completely covered with a shell, but depending on the mass ratio of the core and the shell, the amount of the monomer in the shell forms the layered structure. It may be inadequate.
- a structure in which a part of the core is covered with a shell may be used, or a part of the core may be a polymerizable component of the shell. It may have a structure in which unsaturated monomers are graft-polymerized. Further, the concept of the multilayer structure in the core / shell type structure is similarly applied to the case where the multilayer structure is formed in the core in the water-dispersible hydroxyl group-containing acrylic resin (x111').
- the ratio of the copolymer (I-1) to the copolymer (II-1) in the water-dispersible hydroxyl group-containing acrylic resin (x111') having a core / shell type relayer structure is determined by the multi-layer coating film to be formed.
- the solid content mass ratio of the copolymer (I-1) / copolymer (II-1) is preferably 10/90 to 90/10, more preferably 50/50. It is in the range of ⁇ 85/15, more preferably 65/35 to 80/20.
- the water-dispersible hydroxyl group-containing acrylic resin (x111') obtained as described above can generally have an average particle size in the range of 10 to 1000 nm, particularly 20 to 500 nm.
- the average particle size of the hydroxyl group-containing acrylic resin is a value measured by the Coulter counter method at a measurement temperature of 20 ° C. This measurement can be performed using, for example, "COOLTER N4 type" (trade name, manufactured by Beckman Coulter).
- an acidic group such as a carboxyl group of the water-dispersible hydroxyl group-containing acrylic resin (x111') is used. It is desirable to neutralize with a Japanese agent.
- the neutralizing agent can be used without particular limitation as long as it can neutralize an acidic group. For example, sodium hydroxide, potassium hydroxide, trimethylamine, 2- (dimethylamino) ethanol, etc.
- Examples thereof include 2-amino-2-methyl-1-propanol, triethylamine, aqueous ammonia, etc., and these neutralizing agents have a pH of an aqueous dispersion of an aqueous dispersible hydroxyl group-containing acrylic resin (x111') after neutralization. It is desirable to use it in an amount such that it is about 6.5 to about 9.0.
- the hydroxyl group-containing acrylic resin (x11) preferably has a hydroxyl value of 1 to 200 mgKOH / g, and more preferably 5 to 180 mgKOH / g, from the viewpoint of water resistance of the formed multi-layer coating film. It is preferably 7 to 130 mgKOH / g, more preferably 7 to 130 mgKOH / g.
- the hydroxyl group-containing acrylic resin (x11) preferably has an acid value of 1 to 130 mgKOH / g, preferably 5 to 100 mgKOH / g, from the viewpoint of water resistance of the formed multi-layer coating film. Is more preferable, and 7 to 70 mgKOH / g is even more preferable.
- the content of the hydroxyl group-containing acrylic resin (x11) is 100 parts by mass of the total solid content of the bright base coating material (X) from the viewpoint of obtaining a design exhibiting water resistance and metallic luster of the formed multi-layer coating film. It is preferably in the range of 0.5 to 40 parts by mass, more preferably 2.5 to 35 parts by mass, and further preferably 5 to 30 parts by mass.
- the solid content means a non-volatile content, and means a residue obtained by removing volatile components such as water and an organic solvent from a sample.
- the solid content can be calculated by multiplying the mass of the sample by the solid content concentration.
- the solid content concentration can be measured by dividing the mass of the residue obtained by drying 3 grams of the sample at 105 ° C. for 3 hours by the mass before drying.
- Bright pigment (x2) The bright pigment dispersion (X) contains a bright pigment (x2).
- Examples of the brilliant pigment (x2) include a vapor-deposited metal flake pigment, an aluminum flake pigment, a photointerfering pigment and the like. Among them, from the viewpoint of obtaining a multi-layer coating film exhibiting excellent metallic luster, it is preferable to use a vapor-deposited metal flake pigment, aluminum flake pigment, or both, and it is more preferable to use a vapor-deposited metal flake pigment. It is more preferable to use a vapor-deposited aluminum flake pigment described later. One or two or more of these pigments can be appropriately selected and used depending on the texture required for the obtained coating film.
- the vapor-filmed metal flake pigment is obtained by depositing a metal film on a base base material, peeling off the base base material, and then crushing the vapor-deposited metal film.
- the base material include a film and the like.
- the material of the metal is not particularly limited, and examples thereof include aluminum, gold, silver, copper, brass, titanium, chrome, nickel, nickel chrome, and stainless steel. Of these, aluminum or chromium is particularly preferable from the viewpoint of availability and handling.
- the vapor-deposited metal flake pigment obtained by depositing aluminum is referred to as "deposited aluminum flake pigment”
- the vapor-deposited metal flake pigment obtained by depositing chromium is referred to as "deposited chrome flake pigment”.
- the thin-film metal flake pigment one formed from one layer of the thin-film metal film can be used, but a multi-layer type in which another metal or metal oxide is further formed on the thin-film metal film is used. You may.
- the surface of the vapor-deposited aluminum flake pigment is preferably treated with silica from the viewpoint of storage stability and obtaining a coating film having excellent metallic luster.
- Examples of commercially available products that can be used as the above-mentioned vapor-filmed aluminum flake pigments include the "METALURE” series (trade name, manufactured by Ekart), the “Hydrosine WS” series (trade name, manufactured by Ekart), and the “Decomet” series (trade name, manufactured by Schlenk). (Manufactured by BASF), "Metaseen” series (trade name, manufactured by BASF) and the like can be mentioned.
- vapor-deposited chrome flake pigment examples include the "Metalure Liquid Black” series (trade name, manufactured by Ecult Co., Ltd.) and the like.
- the average thickness of the vapor-filmed metal flake pigment is preferably 0.01 to 1.0 ⁇ m, more preferably 0.015 to 0.1 ⁇ m.
- the average particle size of the vapor-deposited metal flake pigment is preferably 1 to 50 ⁇ m, more preferably 5 to 20 ⁇ m.
- the aluminum flake pigment is generally produced by pulverizing and grinding aluminum in a ball mill or an attritor mill in the presence of a pulverizing medium solution using a pulverizing aid.
- a pulverizing aid in the manufacturing process of the aluminum flake pigment include higher fatty acids such as oleic acid, stearic acid, isostearic acid, lauric acid, palmitic acid and myristic acid, as well as aliphatic amines, aliphatic amides and fatty alcohols. used.
- Aliphatic hydrocarbons such as mineral spirits are used as the pulverized medium.
- a colored aluminum pigment such as one in which the surface of the aluminum flake pigment is coated with a coloring pigment and further coated with a resin, or one in which the surface of the aluminum flake pigment is coated with a metal oxide such as iron oxide is used. You may.
- the aluminum flake pigment preferably has an average particle size in the range of 1 to 100 ⁇ m, more preferably in the range of 5 to 50 ⁇ m, and particularly preferably in the range of 7 to 30 ⁇ m. Is.
- the thickness is preferably in the range of 0.01 to 2.0 ⁇ m, and particularly preferably in the range of 0.02 to 1.0 ⁇ m.
- the photointerfering pigment examples include natural mica, artificial mica, glass, silica, iron oxide, aluminum oxide, and other transparent to translucent scaly substrates on the surface of the substrate. Examples thereof include bright pigments coated with metal oxides having different refractive coefficients.
- the photocoherent pigment can be used alone or in combination of two or more.
- Natural mica is a scaly base material obtained by crushing ore mica (mica). Artificial mica is synthesized by heating industrial raw materials such as SiO 2 , MgO, Al 2 O 3 , K 2 SiF 6 , and Na 2 SiF 6 , melting them at a high temperature of about 1500 ° C, cooling them, and crystallizing them. It has few impurities and is uniform in size and thickness when compared with natural mica.
- fluorine gold mica KMg 3 AlSi 3 O 10 F 2
- potassium tetrasilicon mica KMg 2.5 AlSi 4 O 10 F 2
- sodium tetrasilicon mica NaMg 2.5 AlSi 4) O 10 F 2
- Na teniolite NaMg 2 LiSi 4 O 10 F 2
- LiNa teniolite LiMg 2 LiSi 4 O 10 F 2
- the like can be mentioned.
- Examples of the metal oxide that coats the base material include titanium oxide and iron oxide, and the photocoherent pigment can exhibit various different interference colors depending on the difference in the thickness of the metal oxide. ..
- photo-interfering pigment examples include the following metal oxide-coated mica pigments, metal oxide-coated alumina flake pigments, metal oxide-coated glass flake pigments, and metal oxide-coated silica flake pigments. ..
- the metal oxide-coated mica pigment is a pigment in which natural mica or artificial mica is used as a base material and the surface of the base material is coated with a metal oxide.
- the metal oxide-coated alumina flake pigment is a pigment in which alumina flakes are used as a base material and the surface of the base material is coated with a metal oxide.
- Alumina flakes mean scaly (flaky) aluminum oxide, which is colorless and transparent. The alumina flakes do not have to be a single component of aluminum oxide and may contain oxides of other metals.
- a metal oxide-coated glass flake pigment is a pigment in which scaly glass is used as a base material and the surface of the base material is coated with a metal oxide. Since the surface of the base material of the metal oxide-coated glass flake pigment is smooth, strong light reflection occurs.
- the metal oxide-coated silica flake pigment is a pigment in which a metal oxide coats scaly silica, which is a base material having a smooth surface and a uniform thickness.
- the content of the brilliant pigment (x2) is in the range of 15 to 80 parts by mass based on 100 parts by mass of the total solid content in the brilliant pigment dispersion (X).
- the content of the brilliant pigment (x2) is 15 parts by mass or more based on 100 parts by mass of the total solid content in the brilliant pigment dispersion (X), an excellent metallic luster is exhibited.
- a layered coating film can be obtained, and when the amount is 80 parts by mass or less, a multi-layered coating film having excellent water resistance can be obtained.
- the content of the bright pigment (x2) is the total in the bright pigment dispersion (X).
- the solid content is preferably in the range of 17 to 75 parts by mass, more preferably in the range of 20 to 70 parts by mass, based on 100 parts by mass of the solid content.
- the brilliant pigment (x2) is used from the viewpoint of obtaining a multi-layer coating film having excellent water resistance and excellent metallic luster.
- the content of is preferably in the range of 15 to 55 parts by mass, preferably in the range of 20 to 45 parts by mass, based on 100 parts by mass of the total solid content in the bright pigment dispersion (X). Is even more preferable.
- the brilliant pigment (x2) is used from the viewpoint of obtaining a multi-layer coating film having excellent water resistance and excellent metallic luster.
- the content is preferably in the range of 45 to 80 parts by mass, preferably in the range of 55 to 75 parts by mass, based on 100 parts by mass of the total solid content in the bright pigment dispersion (X). Is even more preferable.
- the glitter pigment dispersion (X) further contains water as a main solvent, and also contains a surface conditioner and a viscosity conditioner.
- the surface conditioner is used to support the uniform orientation of the photo-interfering pigment dispersed in water on the object when the bright pigment dispersion (X) is coated.
- a known surface conditioner can be used.
- the surface adjusting agent examples include surface adjusting agents such as silicone-based surface adjusting agents, acrylic-based surface adjusting agents, vinyl-based surface adjusting agents, fluorine-based surface adjusting agents, and acetylenediol-based surface adjusting agents. From the viewpoint of the orientation of the bright pigment (x2), an acetylene diol-based surface conditioner is preferable.
- the above surface conditioners can be used alone or in combination of two or more as appropriate.
- surface conditioners include, for example, Evonik Industries' Dynal series, Surfinol series, Tego series, Big Chemie's BYK series, Kyoei's Chemical's Granol series, Polyflow series, and Kusumoto Kasei's Dispa.
- the Ron series and the like can be mentioned.
- the content of the surface conditioner is a glitter pigment dispersion (from the viewpoint of obtaining a multi-layer coating film exhibiting excellent metallic luster, etc. Based on 100 parts by mass of the total solid content in X), it is preferably in the range of 2.5 to 35 parts by mass, and more preferably in the range of 5 to 25 parts by mass.
- viscosity adjusting agent known ones can be used, for example, silica-based fine powder, mineral-based viscosity adjusting agent, barium sulfate atomized powder, polyamide-based viscosity adjusting agent, organic resin fine particle viscosity adjusting agent, diurea-based viscosity adjusting agent.
- examples thereof include agents, urethane-associated viscosity modifiers, acrylic swelling polyacrylic acid viscosity modifiers, and cellulose viscosity modifiers.
- a mineral-based viscosity modifier a polyacrylic acid-based viscosity modifier, and a cellulosic viscosity adjuster from the viewpoint of obtaining a multi-layer coating having an excellent metallic luster, and in particular, a cellulosic viscosity adjuster. It is preferable to use a modifier.
- These viscosity modifiers can be used alone or in combination of two or more as appropriate.
- Examples of the mineral viscosity modifier include a swellable layered silicate having a 2: 1 type structure in its crystal structure.
- smectite clay minerals such as natural or synthetic montmorillonite, saponite, hectorite, stivensite, biderite, nontronite, bentonite, and laponite Na-type tetrasilicic fluorine mica, Li-type tetrasilicic fluorine mica, Na.
- Swellable mica clay minerals such as salt-type fluorine teniolite and Li-type fluorine teniolite; vermiculite; substitutions or derivatives thereof; and mixtures thereof.
- polyacrylic acid-based viscosity regulator examples include sodium polyacrylate and a polyacrylic acid- (meth) acrylic acid ester copolymer.
- polyacrylic acid-based viscosity modifiers include, for example, Dow Chemical's "Primal ASE-60”, “Primal TT615", “Primal RM5" (above, trade name), and San Nopco's "SN Thickener 613". , “SN Thickener 618”, “SN Thickener 630”, “SN Thickener 634", “SN Thickener 636” (above, trade name) and the like.
- the solid acid value of the polyacrylic acid-based viscosity modifier is preferably in the range of 30 to 300 mgKOH / g, more preferably 80 to 280 mgKOH / g.
- Examples of the cellulosic viscosity modifier include carboxymethyl cellulose, methyl cellulose, hydroxyethyl cellulose, hydroxyethyl methyl cellulose, hydroxypropyl methyl cellulose, nanocellulose crystal, cellulose nanofiber and the like, and among them, excellent metallic luster is exhibited. From the viewpoint of obtaining a multi-layer coating film, it is preferable to use cellulose nanofibers and / or cellulose nanocrystals, and it is more preferable to use cellulose nanofibers.
- cellulose nanofibers may be referred to as cellulose nanofibrils or fibrated celluloses.
- cellulose nanocrystals are sometimes referred to as nanocellulose crystals.
- the cellulose nanofibers have a number average fiber diameter of preferably 2 to 500 nm, more preferably 2 to 250 nm, still more preferably 2 to 150 nm, from the viewpoint of obtaining a multi-layer coating film exhibiting excellent metallic luster.
- the number average fiber length is preferably in the range of 0.1 to 20 ⁇ m, more preferably 0.1 to 15 ⁇ m, and even more preferably 0.1 to 10 ⁇ m.
- a sample obtained by diluting cellulose nanofibers with water is dispersed and cast on a carbon film-coated grid that has been hydrophilized, and this is cast on a transmission electron microscope (transmission electron microscope). It is measured and calculated from the image observed by TEM).
- the cellulose nanofibers those obtained by defibrating the cellulose raw material and stabilizing it in water can be used.
- the cellulose raw material means various forms of materials mainly composed of cellulose, and specifically, for example, pulp (wood pulp, jute, Manila hemp, herbaceous pulp such as Kenaf, etc.); produced by microorganisms.
- Natural cellulose such as cellulose; regenerated cellulose spun after dissolving cellulose in some solvent such as copper ammonia solution or morpholin derivative; and the above cellulose raw materials such as hydrolysis, alkali hydrolysis, enzymatic decomposition, blasting, vibration ball mill, etc. Examples thereof include fine cellulose obtained by depolymerizing cellulose by mechanical treatment or the like.
- anion-modified cellulose nanofibers can also be used.
- anion-modified cellulose nanofibers include carboxylated cellulose nanofibers, carboxylmethylated cellulose nanofibers, sulfonic acid group-containing cellulose nanofibers, and phosphoric acid group-containing cellulose nanofibers.
- a functional group such as a carboxyl group or a carboxylmethyl group is introduced into a cellulose raw material by a known method, and the obtained modified cellulose is washed to prepare a dispersion liquid of the modified cellulose. This dispersion can be obtained by defibrating.
- the carboxylated cellulose is also called oxidized cellulose.
- the above-mentioned cellulose oxide is obtained, for example, by oxidizing the cellulose raw material in water with an oxidizing agent in the presence of a compound selected from the group consisting of N-oxyl compounds, bromides, and iodides or mixtures thereof. be able to.
- Examples of commercially available products of the cellulose nanofibers include Leocrysta (registered trademark) manufactured by Dai-ichi Kogyo Seiyaku Co., Ltd. and Auro Visco (registered trademark) manufactured by Oji Holdings Co., Ltd. Further, as a commercially available product of the cellulose nanocrystal, for example, "Cellulose NCC” manufactured by Celluforce Co., Ltd. and the like can be mentioned.
- the content of the viscosity modifier is such that a multi-layer coating film exhibiting excellent metallic luster can be obtained. Based on 100 parts by mass of the total solid content in X), it is preferably in the range of 5 to 40 parts by mass, and more preferably in the range of 10 to 25 parts by mass.
- the bright pigment dispersion (X) further comprises a hydroxyl group-free resin, a coloring pigment, an extender pigment, an organic solvent, a pigment dispersant, a pigment derivative, an anti-precipitation agent, an antifoaming agent, an ultraviolet absorber, and the like.
- a light stabilizer or the like may be appropriately contained.
- the coloring pigment is not particularly limited, but specifically, for example, benzimidazolone pigment, pyrazolone pigment, azo pigment, quinacridone pigment, diketopyrrolopyrrole pigment, perylene pigment, perinone.
- Organic pigments such as system pigments, isoindolin type pigments, isoindolinone type pigments, metal chelate azo type pigments, phthalocyanine type pigments, indanslon type pigments, dioxazine type pigments, slene type pigments, indigo type pigments, composite oxide type inorganic Examples include pigments and carbon black pigments. These can be used alone or in combination of two or more.
- the content thereof is preferably 30 parts by mass or less with respect to 100 parts by mass of the total solid content in the bright pigment dispersion (X). More preferably, it is in the range of 0.1 to 20 parts by mass.
- extender pigments examples include talc, silica, calcium carbonate, barium sulfate, zinc oxide and the like.
- the content thereof is preferably 30 parts by mass or less with respect to 100 parts by mass of the total solid content in the bright pigment dispersion (X). More preferably, it is in the range of 0.1 to 20 parts by mass.
- the glitter pigment dispersion (X) can be coated according to a usual method, and examples thereof include air spray coating, airless spray coating, and rotary atomization coating.
- electrostatic coating may be applied as needed.
- electrostatic coating of the rotary atomization method and electrostatic coating of the air spray method are preferable, and rotation is preferable.
- Atomization type electrostatic coating is particularly preferable.
- the glitter pigment dispersion (X) is appropriately prepared with water and / or an organic solvent and, if necessary, an additive such as an antifoaming agent. It is preferable to adjust the solid content and viscosity to be suitable for coating.
- the solid content of the bright pigment dispersion (X) at the time of coating is preferably 0.1 to 10% by mass, more preferably 0, from the viewpoint of obtaining a multi-layer coating film exhibiting excellent metallic luster. It is in the range of .5 to 9% by mass, more preferably 1 to 8% by mass.
- the viscosity of the bright pigment dispersion (X) is the viscosity after 1 minute at 60 rpm measured with a B-type viscometer at a temperature of 20 ° C. from the viewpoint of obtaining a multi-layer coating film exhibiting excellent metallic luster. (In this specification, it may be referred to as "B60 value”) is preferably 50 to 900 mPa ⁇ s, and more preferably 100 to 800 mPa ⁇ s.
- the viscometer used is a digital bismetron viscometer VDA type (manufactured by Shibaura System Co., Ltd., B type viscometer).
- the cured film thickness of the brilliant first base coating film is preferably about 0.02 to 7 ⁇ m, more preferably 0.1 to 4 ⁇ m, from the viewpoint of obtaining a multi-layer coating film exhibiting excellent metallic luster. , More preferably about 0.15 to 3 ⁇ m.
- Process (3) According to the method for forming a multi-layer coating film of the present invention, next, a transparent coloring containing a hydroxyl group-containing resin (y1) and a coloring pigment (y2) is performed on the brilliant first base coating film obtained in the step (2).
- the second base paint (Y) is applied to form a transparent colored second base coating film.
- the form of the transparent colored second base paint (Y) is not particularly limited, and may be any of a water-based paint, an organic solvent type paint, and a solvent-free type paint.
- the transparent colored second base paint (Y) is preferably a water-based paint from the viewpoint of reducing the environmental load.
- the transparent colored second base paint (Y) is a colored and transparent paint.
- the transparent colored second base coating film obtained by applying the transparent colored second base paint (Y) is a coating film that is colored and does not hide the base layer.
- transparent coloring is defined by the haze value of the coating film.
- the transparent colored second base paint (Y) used in the present invention has a haze value of 30% or less of a dry film having a film thickness of 10 ⁇ m obtained by coating the transparent colored second base paint (Y).
- the haze value is determined by coating a smooth polytetrafluoroethylene (PTFE) plate with a cured and peeled coating film of "turbidity meter COH-300A" (trade name, manufactured by Nippon Denshoku Kogyo Co., Ltd.). ), It shall be defined as a numerical value calculated by the following formula from the diffused light transmittance (DF) and the parallel light transmittance (PT).
- the hydroxyl group-containing resin (y1) is a resin having at least one hydroxyl group in one molecule.
- the hydroxyl group-containing resin (y1) include resins having a hydroxyl group, such as acrylic resin, polyester resin, polyurethane resin, polyolefin resin, polyether resin, polycarbonate resin, epoxy resin, and alkyd resin. These can be used alone or in combination of two or more.
- the hydroxyl group-containing resin (y1) includes a hydroxyl group-containing acrylic resin (y11), a hydroxyl group-containing polyester resin (y12), and a hydroxyl group-containing resin from the viewpoints of water resistance, chipping resistance, finished appearance, and the like of the formed multi-layer coating film.
- Polyurethane resin (y13) can be preferably used.
- the content of the hydroxyl group-containing resin (y1) in the transparent colored second base paint (Y) is preferably 1 to 100% by mass based on the total amount of resin solids in the transparent colored second base paint (Y). , More preferably in the range of 10 to 90% by mass, still more preferably in the range of 20 to 80% by mass.
- the transparent colored second base coating material (Y) is a crosslink having reactivity with the hydroxyl group of the hydroxyl group-containing resin (y1) from the viewpoints of water resistance, chipping resistance, finished appearance, etc. of the formed multi-layer coating film. It is preferable to contain an agent.
- an amino resin, a polyisocyanate compound, a blocked polyisocyanate compound, or the like can be preferably used from the viewpoint of water resistance and adhesiveness of the obtained multilayer coating film.
- the above-mentioned cross-linking agent is an amino resin and / or a blocked polyisocyanate compound from the viewpoint of the storage stability of the obtained transparent colored second base coating material (Y) and the water resistance and adhesiveness of the obtained multi-layer coating film. It is preferably contained, more preferably an amino resin is contained, and particularly preferably a melamine resin is contained.
- amino resin melamine resin, polyisocyanate compound and blocked polyisocyanate compound, those described in the explanation column of the colored paint (W) can be used.
- the melamine resin examples include a methyl etherified melamine resin in which the methylol group of the partially or completely methylated melamine resin is partially or completely etherified with methyl alcohol, and the methylol group of the partially or completely methylated melamine resin is partially etherified with butyl alcohol.
- a methyl-butyl mixed etherified melamine resin in which the methylol group of a partially or completely etherified butyl etherified melamine resin is partially or completely etherified with methyl alcohol and butyl alcohol is preferable.
- a methyl-butyl mixed etherified melamine resin is more preferable.
- the weight average molecular weight of the melamine resin is preferably in the range of 400 to 6000, more preferably 700 to 4000, and even more preferably 1000 to 3000.
- the content of the cross-linking agent is preferably 1 to 1 based on the total amount of resin solids in the transparent colored second base paint (Y). It is in the range of 50% by mass, more preferably 5 to 45% by mass, and even more preferably 10 to 40% by mass.
- the content ratio of the hydroxyl group-containing resin (y1) and the cross-linking agent is the water resistance of the formed multilayer coating film.
- the hydroxyl group-containing resin (y1) is preferably 30 to 99% by mass, more preferably 50 to 50, based on the total solid content of the hydroxyl group-containing resin (y1) and the cross-linking agent.
- the cross-linking agent is preferably in the range of 1 to 70% by mass, more preferably 5 to 50% by mass, still more preferably 10 to 45% by mass. ing.
- Color pigment (y2) The transparent colored second base paint (Y) contains a colored pigment (y2).
- the coloring pigment (y2) may contain one selected from the group consisting of red pigments, yellow pigments, green pigments, and blue pigments from the viewpoint of obtaining a multi-layer coating film having a vivid metallic luster. preferable.
- red pigment examples include azo pigments such as iron oxide pigments, azo lake pigments, insoluble azo pigments, and condensed azo pigments, anthrone pigments, anthracinone pigments, perylene maroon pigments, and quinacridone pigments.
- azo pigments such as iron oxide pigments, azo lake pigments, insoluble azo pigments, and condensed azo pigments, anthrone pigments, anthracinone pigments, perylene maroon pigments, and quinacridone pigments.
- examples thereof include diketopyrrolopyrrole pigments and dioxazine pigments.
- yellow pigment examples include bismuth vanadate, yellow lead, chromium yellow, monoazo pigment, disazo pigment, benzoimidazolone pigment, isoindolinone pigment, isoindoline pigment, quinophthalone pigment, and azomethine pigment. , Antron pigments and the like.
- green pigment examples include phthalocyanine pigments and azomethine pigments.
- blue pigment examples include phthalocyanine pigments, slene pigments, indigoid pigments, Prussian blue pigments, cobalt blue pigments and the like.
- the coloring pigment (y2) can be used alone or in combination of two or more.
- the content of the coloring pigment (y2) is based on 100 parts by mass of the resin solid content in the transparent coloring second base coating material (Y) from the viewpoint of obtaining a multi-layer coating film having a vivid and metallic luster. It is preferably in the range of 1 to 10 parts by mass, and more preferably in the range of 2 to 8 parts by mass.
- the transparent coloring second base paint (Y) further comprises a hydroxyl group-free resin, an extender pigment, a bright pigment, an organic solvent, a pigment dispersant, a pigment derivative, an anti-precipitation agent, an antifoaming agent, and an ultraviolet absorber, if necessary. Agents, light stabilizers and the like may be appropriately contained.
- extender pigment examples include talc, silica, calcium carbonate, barium sulfate, zinc oxide and the like.
- the content thereof may be 30 parts by mass or less with respect to 100 parts by mass of the resin solid content in the transparent colored second base paint (Y). It is preferably in the range of 0.1 to 20 parts by mass.
- the brilliant pigment examples include aluminum (including vapor-deposited aluminum), copper, zinc, brass, nickel, glass flakes, aluminum oxide, mica, titanium oxide and / or iron oxide-coated aluminum oxide, titanium oxide and the like. / Or an iron oxide-coated mica or the like.
- the content thereof shall be 30 parts by mass or less with respect to 100 parts by mass of the resin solid content in the transparent colored second base paint (Y). Is preferable, and more preferably it is in the range of 0.1 to 20 parts by mass.
- the transparent colored second base paint (Y) can be coated according to a usual method, and examples thereof include air spray coating, airless spray coating, and rotary atomization coating.
- electrostatic coating may be applied as needed.
- electrostatic coating of the rotary atomization method and electrostatic coating of the air spray method are preferable.
- the rotary atomization type electrostatic coating is particularly preferable.
- the transparent colored second base coating material (Y) is appropriately prepared with water and / or an organic solvent, and if necessary, a viscosity modifier and a defoaming agent. It is preferable to add an additive such as an agent to adjust the solid content and viscosity suitable for coating.
- the solid content of the transparent colored second base paint (Y) is preferably in the range of 10 to 60% by mass, more preferably 15 to 55% by mass, and further preferably 20 to 50% by mass. Further, the viscosity of the transparent colored second base paint (Y) is in a range suitable for painting, usually in the range of 500 to 5000 mPa ⁇ s when measured at 20 ° C. and a rotation speed of 6 rpm using a B-type viscometer. It is preferable to appropriately adjust the content so that it is inside, using water and / or an organic solvent.
- the cured film thickness of the transparent colored second base coating film is preferably about 3.0 to 30 ⁇ m from the viewpoint of obtaining a multi-layer coating film which is vivid, exhibits metallic luster, and has excellent water resistance. , More preferably 4.0 to 25 ⁇ m, still more preferably about 5 to 20 ⁇ m.
- the hydroxyl group-containing acrylic resin (z1) and the polyisocyanate compound (z2) are contained on the transparent colored second base coating film obtained in the step (3).
- a clear paint (Z) containing an aliphatic triisocyanate compound (z2-1) having a molecular weight in the range of 200 to 350 is coated with the polyisocyanate compound (z2) as at least one of them.
- a film is formed.
- the hydroxyl group-containing acrylic resin (z1) is an acrylic resin having at least one hydroxyl group in one molecule.
- the hydroxyl group-containing acrylic resin (z1) can be obtained from, for example, a method known per se, for example, a hydroxyl group-containing polymerizable unsaturated monomer and another polymerizable unsaturated monomer copolymerizable with the hydroxyl group-containing polymerizable unsaturated monomer. It can be produced by copolymerizing by a method such as a solution polymerization method in an organic solvent or an emulsion polymerization method in water. Of these, it is preferably produced by a solution polymerization method in an organic solvent.
- Examples of the hydroxyl group-containing polymerizable unsaturated monomer and other polymerizable unsaturated monomer copolymerizable with the hydroxyl group-containing polymerizable unsaturated monomer include the polymerizable property described in the explanation column of the hydroxyl group-containing acrylic resin (x11). Unsaturated monomers can be used.
- the amount of the hydroxyl group-containing polymerizable unsaturated monomer used is a copolymerized monomer component from the viewpoints of water resistance, chipping resistance, finished appearance, etc. of the formed multilayer coating film. It is preferably in the range of 15 to 50% by mass, more preferably 20 to 40% by mass, based on the total amount of the above.
- the hydroxyl value of the hydroxyl group-containing acrylic resin (z1) is preferably 50 to 210 mgKOH / g, more preferably 80 to 200 mgKOH / g, from the viewpoints of water resistance, chipping resistance, finished appearance, etc. of the formed multilayer coating film. , More preferably in the range of 100 to 170 mgKOH / g.
- the weight average molecular weight of the hydroxyl group-containing acrylic resin (z1) is preferably 2000 to 50,000, more preferably 3000 to 30000, from the viewpoints of water resistance, chipping resistance, finished appearance, etc. of the formed multi-layer coating film. , More preferably in the range of 4000 to 10000.
- the acid value of the hydroxyl group-containing acrylic resin (z1) is preferably 30 mgKOH / g or less from the viewpoints of the finished appearance of the formed multi-layer coating film, water resistance, pot life of the clear paint (Z), and the like. Is in the range of 1 to 20 mgKOH / g.
- the glass transition temperature of the hydroxyl group-containing acrylic resin (z1) is preferably ⁇ 50 to 60 ° C., more preferably 10 to 0, from the viewpoints of water resistance, chipping resistance, finished appearance, etc. of the formed multi-layer coating film. It is in the range of 50 ° C., more preferably 20 to 45 ° C.
- the glass transition temperature (° C.) of the acrylic resin was calculated by the following formula.
- Tg (K) (W1 / T1) + (W2 / T2) + ... (1)
- Tg (° C.) Tg (K) -273 (2)
- W1, W2, ... represent the mass fraction of each of the monomers used in the copolymerization
- T1, T2, ... represent the Tg (K) of the homopolymer of each monomer. Note that T1, T2, ... Are values according to Polymer Hand Book (Edited by Second Edition, J. Brandup, E. H. Immunogut), pp. III-139 to 179.
- the glass transition temperature (° C.) is set to the static glass transition temperature, and for example, a differential scanning calorimeter "DSC-220U" (manufactured by Seiko Instruments) is used.
- DSC-220U differential scanning calorimeter
- the sample is placed in a measuring cup, vacuum sucked to completely remove the solvent, and then the calorific value change is measured in the range of -20 ° C to + 200 ° C at a temperature rise rate of 3 ° C / min, and the temperature of the first baseline on the low temperature side is measured.
- the change point was defined as the static glass transition temperature.
- a solution polymerization method in which polymerization is carried out in an organic solvent in the presence of a polymerization initiator can be preferably used.
- organic solvent used in the above solution polymerization method examples include aromatic solvents such as toluene, xylene, and "Swazole 1000" (manufactured by Cosmo Petroleum Co., Ltd., trade name, high boiling petroleum solvent); ethyl acetate, butyl acetate.
- ketone solvents such as methyl ethyl ketone, methyl isobutyl ketone and methyl amyl ketone
- alcohol solvents such as isopropanol, n-butanol, isobutanol and 2-ethylhexanol.
- organic solvents can be used alone or in combination of two or more, but it is preferable to use an ester solvent or a ketone solvent from the viewpoint of solubility of the acrylic resin. Further, it is also possible to use an aromatic solvent in a suitable combination.
- Examples of the polymerization initiator that can be used in the copolymerization of the hydroxyl group-containing acrylic resin (z1) include 2,2'-azobisisobutyronitrile, benzoyl peroxide, di-t-butyl peroxide, and di-t-amyl.
- Known radical polymerization initiators such as peroxide, t-butylperoctate, 2,2'-azobis (2-methylbutyronitrile), 2,2'-azobis (2,4-dimethylvaleronitrile), etc. be able to.
- the hydroxyl group-containing acrylic resin (z1) can be used alone or in combination of two or more.
- Polyisocyanate compound (z2) The clear coating material (Z) according to the present invention contains an aliphatic triisocyanate compound (z2), and the polyisocyanate compound (z2) is at least one of them and has a molecular weight in the range of 200 to 350. Contains compound (z2-1).
- Aliphatic triisocyanate compound (z2-1) is an aliphatic polyisocyanate compound having a molecular weight in the range of 200 to 350 and having three isocyanate groups. Among them, the molecular weight is preferably in the range of 200 to 300, and more preferably in the range of 230 to 280, from the viewpoint of water resistance and the like of the multi-layer coating film to be formed.
- aliphatic triisocyanate compound (z2-1) examples include 1,8-diisocyanato-4-isocyanatomethyloctane and (2S) -2,6-diisocyanatohexanoate 2-isocyanatoethyl.
- (2S) -2,6-diisocyanatohexanoate 2-isocyanatoethyl.
- (Common name: lysocyanate triisocyanate) 2,6-diisocyanatohexanoate 2-isocyanatoethyl, 1,6,11-triisocyanatoundecane and the like can be mentioned, and these may be used alone or in combination of two or more. Can be used.
- the aliphatic triisocyanate compound (z2-1) includes 1,8-diisocyanato-4-isocyanatomethyloctane, (2S) -2 from the viewpoint of water resistance of the formed multi-layer coating film.
- the aliphatic triisocyanate compound (z2-1) preferably has a viscosity at 23 ° C. of 1 to 50 mPa ⁇ s, more preferably 1 to 30 mPa ⁇ s, from the viewpoint of water resistance of the formed multilayer coating film. It is within the range of s.
- the clear paint (Z) further comprises, as the polyisocyanate compound (z2), a polyisocyanate compound other than the aliphatic triisocyanate compound (z2-1) having a molecular weight in the range of 200 to 350. Can be contained.
- Polyisocyanate compounds other than the aliphatic triisocyanate compound (z2-1) examples include aliphatic groups other than the aliphatic triisocyanate compound (z2-1). Examples thereof include a polyisocyanate compound, an alicyclic polyisocyanate compound, an aromatic aliphatic polyisocyanate compound, an aromatic polyisocyanate compound, and a derivative of the polyisocyanate compound.
- Examples of the aliphatic polyisocyanate compound other than the aliphatic triisocyanate compound (z2-1) include trimethylene diisocyanate, tetramethylene diisocyanate, hexamethylene diisocyanate, pentamethylene diisocyanate, 1,2-propylene diisocyanate, 1,2-.
- Examples of the alicyclic polyisocyanate compound include 1,3-cyclopentenediisocyanate, 1,4-cyclohexanediisocyanate, 1,3-cyclohexanediisocyanate, and 3-isocyanatomethyl-3,5,5-trimethylcyclohexylisocyanate (conventional use).
- Cyclohexane (common name: hydrogenated xylylene diisocyanate) or a mixture thereof, alicyclic diisocyanate such as norbornenan diisocyanate, for example, 1,3,5-triisocyanatocyclohexane, 1,3,5-trimethylisocyanatocyclohexane, 2- (3-Isocyanatopropyl) -2,5-di (isocyanatomethyl) -bicyclo (2.2.1) heptane, 2- (3-isocyanatopropyl) -2,6-di (isocyanatomethyl)- Bicyclo (2.2.1) h
- aromatic aliphatic polyisocyanate compound examples include 1,3- or 1,4-xylylene diisocyanate or a mixture thereof, ⁇ , ⁇ '-diisocyanato-1,4-diethylbenzene, 1,3- or 1,4-.
- Arophilic aliphatic diisocyanates such as bis (1-isocyanato-1-methylethyl) benzene (common name: tetramethylxylylene diisocyanate) or a mixture thereof, for example, aromatic aliphatic diisocyanates such as 1,3,5-triisocyanatomethylbenzene. Examples thereof include triisocyanate.
- aromatic polyisocyanate compound examples include m-phenylene diisocyanate, p-phenylenedi isocyanate, 4,4'-diphenyldiisocyanate, 1,5-naphthalenediisocyanate, 2,4'-or 4,4'-diphenylmethane diisocyanate or The mixture, 2,4- or 2,6-tolylene diisocyanate or a mixture thereof, aromatic diisocyanates such as 4,4'-toluidine diisocyanate, 4,4'-diphenyl ether diisocyanate, for example, triphenylmethane-4,4'.
- Examples of the derivative of the polyisocyanate compound include dimer, trimmer, biuret, allophanate, carbodiimide, uretdione, uretoimine, isocyanurate, oxadiazine trione, and polymethylene polyphenyl polyisocyanate (crude MDI,) of the polyisocyanate compound.
- Polymeric MDI) and crude TDI can be mentioned.
- the equivalent ratio (NCO / OH) of the total mol number of isocyanate groups in the polyisocyanate compound (z2) and the total mol number of hydroxyl groups in the hydroxyl group-containing acrylic resin (z1) is formed. From the viewpoint of water resistance and the like of the multi-layer coating film, it is preferably in the range of 1.1 to 2.5, more preferably 1.3 to 2.3, and further preferably 1.5 to 2.0. ..
- the content ratio of the aliphatic triisocyanate compound (z2-1) in the polyisocyanate compound (z2) is the same as that of the polyisocyanate compound (z2) from the viewpoint of water resistance of the multi-layer coating film to be formed. Based on the total solid content, it is preferably in the range of 30 to 100% by mass, more preferably 50 to 100% by mass, and further preferably 70 to 100% by mass.
- a solvent such as water or an organic solvent, a resin other than the hydroxyl group-containing acrylic resin (z1), a curing catalyst, a defoaming agent, an ultraviolet absorber, a rheology control agent, and a settling inhibitor.
- Additives for paints such as, etc. can be appropriately blended.
- a coloring pigment can be appropriately used as long as the transparency of the coating film is not impaired.
- the coloring pigment pigments known per se for inks or paints can be used alone or in combination of two or more.
- the blending amount varies depending on the type of coloring pigment used and the like, but is preferably 30% by mass or less, more preferably 0.05 to 20% by mass, and further, based on the total solid content of the resin component in the clear paint. It can be preferably in the range of 0.1 to 10% by mass.
- the clear coating film (Z) can be applied by a method such as electrostatic coating, air spray, or airless spray, and the film thickness of the clear coating film is preferably about 10 to 60 ⁇ m, more preferably about 10 to 60 ⁇ m, based on the cured coating film. It is about 15 to 50 ⁇ m, more preferably about 20 to 40 ⁇ m.
- the solid content of the clear paint (Z) is preferably in the range of 10 to 65% by mass, preferably 15 to 55% by mass, and more preferably 20 to 50% by mass. Further, the viscosity of the clear paint (Z) is set in a range suitable for painting, usually, Ford Cup No. 4 It is preferable to appropriately adjust the viscometer with water and / or an organic solvent so that the temperature is within the range of about 15 to 60 seconds, particularly about 20 to 50 seconds at 20 ° C.
- the colored coating film when the colored coating film is not heat-cured after the coating of the colored paint (W), the colored coating formed in the steps (1) to (4) in the main step (5).
- the multi-layer coating film containing these four coating films can be cured at once. In this case, since heat curing can be omitted once, energy saving can be further improved.
- the heating means can be, for example, hot air heating, infrared heating, high frequency heating, or the like.
- the heating temperature is preferably 80 to 160 ° C, more preferably 100 to 140 ° C.
- the heating time is preferably 10 to 60 minutes, more preferably 15 to 40 minutes. If necessary, before the heat curing, direct or indirect by preheating, air blowing, etc., at a temperature of preferably about 50 to about 110 ° C., more preferably about 60 to about 90 ° C. for about 1 to 60 minutes. You may heat it.
- the present invention may include the following aspects.
- Step (1) A step of coating a colored paint (W) containing a hydroxyl group-containing resin (w1) and a colored pigment (w2) on an object to be coated to form a colored coating film.
- Step (2) A bright pigment dispersion (X) containing a hydroxyl group-containing resin (x1) and a bright pigment (x2) on the colored coating film obtained in the step (1).
- the content of the bright pigment (x2) in the dispersion (X) is in the range of 15 to 80 parts by mass based on 100 parts by mass of the total solid content in the bright pigment dispersion (X).
- a step of coating the bright pigment dispersion (X) to form a bright first base coating film Step (3): A transparent colored second base paint (Y) containing a hydroxyl group-containing resin (y1) and a coloring pigment (y2) is coated on the brilliant first base coating film obtained in the step (2). , The process of forming a transparent colored second base coating film, Step (4): The transparent colored second base coating film obtained in step (3) contains a hydroxyl group-containing acrylic resin (z1) and a polyisocyanate compound (z2), and at least the polyisocyanate compound (z2) is contained.
- a step of applying a clear coating material (Z) containing an aliphatic triisocyanate compound (z2-1) having a molecular weight in the range of 200 to 350 to form a clear coating film and Step (5): By heating the multi-layer coating film including the brilliant first base coating film, the transparent colored second base coating film, and the clear coating film formed in the steps (2) to (4).
- a method for forming a multi-layer coating film which comprises a step of simultaneously curing the multi-layer coating film.
- Item 2 The method for forming a multi-layer coating film according to Item 1, wherein the colored paint (W) is a water-based paint.
- Item 3 The method for forming a multi-layer coating film according to Item 1 or 2, wherein the colored coating material (W) further contains a melamine resin and / or a blocked polyisocyanate compound.
- Item 4. The method for forming a multilayer coating film according to any one of Items 1 to 3, wherein the bright pigment dispersion (X) is a water-based paint.
- Item 5 The method for forming a multilayer coating film according to Item 4, wherein the hydroxyl group-containing resin (x1) contains a hydroxyl group-containing acrylic resin (x11) in the bright pigment dispersion (X).
- Item 6 The method for forming a multilayer coating film according to Item 4, wherein in the bright pigment dispersion (X), the hydroxyl group-containing resin (x1) contains a water-dispersible hydroxyl group-containing acrylic resin (x111).
- Item 7 The multilayer coating according to Item 4, wherein in the bright pigment dispersion (X), the hydroxyl group-containing resin (x1) contains a water-dispersible hydroxyl group-containing acrylic resin (x111') having a core / shell type multilayer structure. Membrane formation method.
- the glitter pigment (x2) contains a vapor-deposited aluminum flake pigment, and the content of the vapor-deposited aluminum flake pigment is 15 to 55 based on 100 parts by mass of the total solid content in the glitter pigment dispersion (X).
- Item 8. The method for forming a multilayer coating film according to any one of Items 1 to 7, which is within the range of parts by mass.
- the glitter pigment (x2) contains an aluminum flake pigment, and the content of the aluminum flake pigment is 45 to 80 parts by mass based on 100 parts by mass of the total solid content in the glitter pigment dispersion (X).
- Item 4. The method for forming a multi-layer coating film according to any one of Items 1 to 7, which is within the range of.
- Item 10 The method for forming a multi-layer coating film according to any one of Items 1 to 9, wherein the transparent colored second base coating material (Y) is a water-based coating material.
- Item 11 The method for forming a multilayer coating film according to any one of Items 1 to 10, wherein the transparent colored second base coating material (Y) further contains a melamine resin and / or a blocked polyisocyanate compound.
- the equivalent ratio (NCO / OH) of the total mol of the isocyanate groups of the polyisocyanate compound (z2) to the total mol of the hydroxyl groups of the hydroxyl group-containing acrylic resin (z1) is 1.1 to 2.
- Item 13 The method for forming a multi-layer coating film according to any one of Items 1 to 12, wherein the cured film thickness of the colored coating film is 5.0 to 40 ⁇ m.
- Item 14 The method for forming a multi-layer coating film according to any one of Items 1 to 13, wherein the film thickness of the brilliant first base coating film is in the range of 0.02 to 7 ⁇ m.
- Item 15 The method for forming a multi-layer coating film according to any one of Items 1 to 14, wherein the film thickness of the transparent colored second base coating film is within the range of 3 to 30 ⁇ m.
- Item 16 The method for forming a multi-layer coating film according to any one of Items 1 to 15, wherein the thickness of the clear coating film is 10 to 60 ⁇ m.
- Item 17 The method for forming a multilayer coating film according to any one of Items 1 to 16, wherein in the step (2), the bright pigment dispersion (X) is coated on the colored coating film that has been heat-cured.
- the bright pigment dispersion (X) is coated on the uncured colored coating film, and in the step (5), the coloring formed in the steps (1) to (4) is performed. Items 1 to 16 that cure the multi-layer coating film including these four coating films at once by simultaneously heating the coating film, the brilliant first base coating film, the transparent colored second base coating film, and the clear coating film. The method for forming a multi-layer coating film according to any one of the above items.
- Item 19 The method for forming a multi-layer coating film according to any one of Items 1 to 18, wherein the saturation C * (15 °) in the L * C * h color system is 90 or more.
- Item 20 The method for forming a multi-layer coating film according to any one of Items 1 to 19, wherein the FF68 obtained by the following formula is 1.59 or more.
- Item 22 The method for forming a multi-layer coating film according to any one of Items 1 to 21, wherein the object to be coated is an outer panel portion of an automobile body or an automobile part.
- a cationic resin using a block polyisocyanate compound as a curing agent is electrodeposited based on a cured coating film so that the film thickness is 20 ⁇ m, heated at 170 ° C. for 20 minutes to be crosslinked and cured, and then electrodeposited. By forming a film, it was made into an object to be coated.
- Monomer emulsion 50 parts of deionized water, 10 parts of styrene, 40 parts of methyl methacrylate, 35 parts of ethyl acrylate, 3.5 parts of n-butyl methacrylate, 10 parts of 2-hydroxyethyl methacrylate, 1.5 parts of acrylic acid, "Aqualon" 1.0 part of KH-10 and 0.03 part of ammonium persulfate were mixed and stirred to obtain a monomer emulsion.
- hydroxyl group-containing polyester resin solution (w12-1) having a solid content concentration of 45%.
- the obtained hydroxyl group-containing polyester resin had a hydroxyl value of 128 mgKOH / g, an acid value of 35 mgKOH / g, and a weight average molecular weight of 13000.
- Pigment Dispersion Liquid Production Example 3 56 parts (solid content 25 parts) of the hydroxyl group-containing polyester resin solution (w12-1) obtained in Production Example 2, 70 parts of "Typake UT-771” (trade name, rutile-type titanium dioxide pigment, manufactured by Ishihara Sangyo Co., Ltd.), " 0.5 part of "Carbon MA-100” (trade name, carbon black pigment, manufactured by Mitsubishi Chemical Co., Ltd.) and 5 parts of deionized water were mixed and adjusted to pH 8.0 with 2- (dimethylamino) ethanol.
- “Typake UT-771” trade name, rutile-type titanium dioxide pigment, manufactured by Ishihara Sangyo Co., Ltd.
- Carbon MA-100 trade name, carbon black pigment, manufactured by Mitsubishi Chemical Co., Ltd.
- the obtained mixed solution was placed in a wide-mouthed glass bottle, glass beads having a diameter of about 1.3 mm ⁇ were added as a dispersion medium, sealed, and dispersed with a paint shaker for 30 minutes to obtain a pigment dispersion (P-1). Obtained.
- the remaining monomer emulsion (1) was added dropwise to the reaction vessel kept at the same temperature over 3 hours, and aging was carried out for 1 hour after the completion of the addition.
- the following monomer emulsion (2) was added dropwise over 1 hour, and after aging for 1 hour, 40 parts of a 5% dimethylethanolamine aqueous solution was gradually added to the reaction vessel and cooled to 30 ° C., and 100 mesh nylon was used.
- the mixture was discharged while being filtered with a cloth to obtain an aqueous dispersible hydroxyl group-containing acrylic resin (x111'-1) having a core / shell type multilayer structure having a solid content concentration of 28%.
- the obtained water-dispersible hydroxyl group-containing acrylic resin (x111'-1) having a core / shell type multilayer structure had a hydroxyl value of 25 mgKOH / g and an acid value of 33 mgKOH / g.
- Monomer emulsion (1) 47 parts of deionized water, 0.72 parts of "Aqualon KH-10", 2.1 parts of methylenebisacrylamide, 2.8 parts of styrene, 16.1 parts of methyl methacrylate, 28 parts of ethyl acrylate and 21 parts of n-butyl acrylate was mixed and stirred to obtain a monomer emulsion (1).
- Monomer emulsion (2) 23 parts of deionized water, 0.31 part of "Aqualon KH-10", 0.03 part of ammonium persulfate, 5.1 part of methacrylic acid, 5.1 part of 2-hydroxyethyl acrylate, 3 parts of styrene.
- a monomer emulsion (2) was obtained by mixing and stirring 6 parts of methyl methacrylate, 1.8 parts of ethyl acrylate and 9 parts of n-butyl acrylate.
- hydroxyl group-containing acrylic resin solution (y11-1) having a solid content of 55%.
- the obtained hydroxyl group-containing acrylic resin had an acid value of 47 mgKOH / g, a hydroxyl value of 72 mgKOH / g, and a weight average molecular weight of 58,000.
- Production of Hydroxy Group-Containing Polyester Resin Solution (y12-1) Production example 16 109 parts of trimethylol propane, 141 parts of 1,6-hexanediol, 126 parts of 1,2-cyclohexanedicarboxylic acid anhydride and adipic acid in a reaction vessel equipped with a thermometer, thermostat, stirrer, reflux condenser and water separator. 120 parts of acid was charged, the temperature was raised from 160 ° C. to 230 ° C. over 3 hours, and then the condensation reaction was carried out at 230 ° C. for 4 hours.
- a hydroxyl group-containing polyester resin solution (y12-1) having a solid content of 70% was obtained.
- the obtained hydroxyl group-containing polyester resin had an acid value of 46 mgKOH / g, a hydroxyl value of 150 mgKOH / g, and a number average molecular weight of 1400.
- Pigment Dispersion Liquids Production of Pigment Dispersion Liquids (P-2) to (P-5) Production Example 17 327 parts (solid content 180 parts) of the hydroxyl group-containing acrylic resin solution (y11-1) obtained in Production Example 15, 360 parts of deionized water, "Surfinol 104A” (trade name, defoaming agent manufactured by Air Products Co., Ltd., solid content) 50%) 6 parts (solid content 3 parts) and "Varifine BF-20” (trade name, manufactured by Sakai Chemical Industry Co., Ltd., barium sulfate powder, average particle size 0.03 ⁇ m) 250 parts (solid content 250 parts) , A glass bead medium was added, and the mixture was mixed and dispersed at room temperature for 1 hour to obtain a pigment dispersion liquid (P-2) having a solid content of 44%.
- Production Example 18 182 parts (solid content 100 parts) of the hydroxyl group-containing acrylic resin solution (y11-1) obtained in Production Example 15, 100 parts (solid) of "CHROMOFINE BLUE 5206M" (trade name, manufactured by Dainichiseika Kogyo Co., Ltd., phthalocyanine blue pigment) 100 parts) and 450 parts of deionized water were mixed, adjusted to pH 7.5 with 2-amino-2-methyl-1-propanol, and then dispersed with a paint shaker for 2 hours to obtain a pigment dispersion having a solid content of 27%. (P-3) was obtained.
- Production example 19 182 parts (solid content 100 parts) of the hydroxyl group-containing acrylic resin solution (y11-1) obtained in Production Example 15, 150 parts (solid) of "MAROON 179 229-6438" (trade name, manufactured by SUN CHEMICAL CORPORATION, organic perylene pigment). (150 parts per minute) and 479 parts of deionized water were mixed, adjusted to pH 7.5 with 2-amino-2-methyl-1-propanol, and then dispersed with a paint shaker for 2 hours to obtain a pigment dispersion having a solid content of 31%. (P-4) was obtained.
- Production example 20 182 parts (solid content 100 parts) of the hydroxyl group-containing acrylic resin solution (y11-1) obtained in Production Example 15, 150 parts (solid content) of "Irgazin DPP Red BO" (trade name, manufactured by BASF, diketopyrrolopyrrole pigment) 150 parts) and 479 parts of deionized water were mixed, adjusted to pH 7.5 with 2-amino-2-methyl-1-propanol, and then dispersed with a paint shaker for 2 hours to obtain a pigment dispersion having a solid content of 31% (15 parts). P-5) was obtained.
- the stirring and mixing container contains 31.8 parts (14 parts of solid content) of the pigment dispersion liquid (P-2) obtained in Production Example 17 and an aqueous dispersible hydroxyl group having a core / shell type multilayer structure obtained in Production Example 5.
- the transparent second base paint (V-1) obtained in Production Example 21 was placed in a stirring and mixing container, and "CHROMOFINE BLUE 5206M" (trade name, manufactured by Dainichiseika Kogyo Co., Ltd., phthalocyanine) was added to 100 parts by mass of the resin solid content.
- the pigment dispersion (P-3) obtained in Production Example 18 was added so that the amount of the blue pigment (based blue pigment) was 5 parts by mass, and the mixture was stirred and mixed to prepare a transparent blue second base paint (Y-1).
- Production Example 23 The transparent second base paint (V-1) obtained in Production Example 21 was placed in a stirring and mixing container, and "MAROON 179 229-6438" (trade name, manufactured by SUN CHEMICAL CORPORATION) was added to 100 parts by mass of the resin solid content.
- the pigment dispersion liquid (P-4) obtained in Production Example 19 was added so that the amount of the organic perylene pigment) was 5 parts by mass, and the mixture was stirred and mixed to prepare a transparent red second base paint (Y-2).
- the cured coating film was coated to a film thickness of 10 ⁇ m, left at room temperature for 3 minutes, and 140 ° C. in a hot air circulation type drying furnace. After heating for 30 minutes in, it was obtained by peeling from the PTFE plate.
- the colored second base paint (V-2) does not correspond to the transparent colored second base paint according to the present invention because the haze value of the obtained coating film exceeds 30%.
- the obtained hydroxyl group-containing acrylic resin (z1-1) had a hydroxyl value of 139 mgKOH / g, an acid value of 5.5 mgKOH / g, a weight average molecular weight of 5,500, and a glass transition temperature of 38 ° C.
- test plate Example 1 (Painting of colored paint (W)) Above 1. On the base material prepared in 2. above. Using a mini-bell type rotary electrostatic coating machine, the colored paint (W-1) produced in the above was coated with a booth temperature of 23 ° C. and a humidity of 68% so as to have a film thickness of 25 ⁇ m as a cured coating film. The mixture was left at room temperature for 15 minutes to obtain an uncured colored coating film.
- Example 2 to 15 Comparative Examples 1 to 10 A test plate was obtained in the same manner as in Example 1 except that the paints and film thicknesses shown in Table 4 were used.
- L * C * h color system refers to the L * a * b * color system specified by the International Commission on Illumination in 1976 and also adopted in JIS Z 8781-4 (2013).
- the L * value represents the brightness
- the C * value represents the saturation as the distance from the origin
- the h value is the L * a * b * a * red direction in the color system.
- the axis is 0 °, and the hue angle moved from here with respect to the hue in the counterclockwise direction is represented.
- Saturation C * (15 °) refers to the light received at an angle of 15 ° in the direction of the measurement light from the specular reflection angle by irradiating the measurement light from an angle of 45 ° with respect to the axis perpendicular to the measurement target surface. Represents the measured saturation C *.
- IV68 was measured using "MA-68II" (trade name, manufactured by x-rite). The larger the value, the better the sense of brightness.
- the IV68 irradiates the measurement light from an angle of 45 ° with respect to the axis perpendicular to the measurement target surface, and measures the light received at an angle of 15 ° from the normal reflection angle in the direction of the measurement light. It represents the brightness Y value in the XYZ color system based on the rate.
- SV68 was measured using "MA-68II” (trade name, manufactured by x-rite). The smaller the value, the better the orientation of the bright material.
- the SV68 irradiates the measurement light from an angle of 45 ° with respect to the axis perpendicular to the measurement target surface, and measures the light received at an angle of 45 ° from the normal reflection angle in the direction of the measurement light. It represents the brightness Y value in the XYZ color system based on the rate.
- A 100 Goban-grain coating films remain, and there is no small edge chipping of the coating film at the cut edge of the cutter.
- B 100 Goban-grain coating films remain, but small edge chipping of the coating film occurs at the cut edge of the cutter, and less than 10 residual coating films have chipped edges.
- C 100 Goban-grain coating films remain, but small edge chipping of the coating film occurs at the cut edge of the cutter, and 10 or more residual coating films have chipped edges.
- D 90 to 99 Goban-grain coating films remain, E: The number of remaining Goban-grain coating films is 89 or less.
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Abstract
Description
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15~80質量部の範囲内である光輝性顔料分散体(X)を塗装して光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200~350の範囲内である脂肪族トリイソシアネート化合物(z2-1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)~(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法。
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15~80質量部の範囲内である光輝性顔料分散体(X)を塗装して光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200~350の範囲内である脂肪族トリイソシアネート化合物(z2-1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)~(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法である。
本発明の複層塗膜形成方法によれば、まず、被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)が塗装され、着色塗膜が形成される。
着色塗料(W)を適用する被塗物は、特に限定されない。該被塗物としては、例えば、乗用車、トラック、オートバイ、バス等の自動車車体の外板部;バンパー等の自動車部品;携帯電話、オーディオ機器等の家庭電気製品の外板部等を挙げることができる。これらのうち、自動車車体の外板部及び自動車部品が好ましい。
着色塗料(W)は、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する。
水酸基含有樹脂(w1)は、1分子中に少なくとも1個の水酸基を有する樹脂である。該水酸基含有樹脂(w1)としては、例えば、水酸基を有する、アクリル樹脂、ポリエステル樹脂、ポリウレタン樹脂、ポリオレフィン樹脂、ポリエーテル樹脂、ポリカーボネート樹脂、エポキシ樹脂、アルキド樹脂等の樹脂が挙げられる。これらはそれぞれ単独でもしくは2種以上組み合わせて使用することができる。
着色塗料(W)は、着色顔料(w2)を含有する。
本発明の複層塗膜形成方法によれば、次に、工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15~80質量部の範囲内である光輝性顔料分散体(X)が塗装され、光輝性第1ベース塗膜が形成される。
水酸基含有樹脂(x1)は、1分子中に少なくとも1個の水酸基を有する樹脂である。該水酸基含有樹脂(x1)としては、例えば、水酸基を有する、アクリル樹脂、ポリエステル樹脂、ポリウレタン樹脂、ポリオレフィン樹脂、ポリエーテル樹脂、ポリカーボネート樹脂、エポキシ樹脂、アルキド樹脂等の樹脂が挙げられる。これらはそれぞれ単独でもしくは2種以上組み合わせて使用することができる。
水酸基含有アクリル樹脂(x11)は、例えば、水酸基含有重合性不飽和モノマー(a)及び該水酸基含有重合性不飽和モノマーと共重合可能な他の重合性不飽和モノマー(b)を、それ自体既知の方法、例えば、有機溶媒中での溶液重合法、水中でのエマルション重合法等の方法により共重合せしめることによって製造することができる。
(i) アルキル又はシクロアルキル(メタ)アクリレート:例えば、メチル(メタ)アクリレート、エチル(メタ)アクリレート、n-プロピル(メタ)アクリレート、イソプロピル(メタ)アクリレート、n-ブチル(メタ)アクリレート、イソブチル(メタ)アクリレート、tert-ブチル(メタ)アクリレート、n-ヘキシル(メタ)アクリレート、n-オクチル(メタ)アクリレート、2-エチルヘキシル(メタ)アクリレート、ノニル(メタ)アクリレート、トリデシル(メタ)アクリレート、ラウリル(メタ)アクリレート、ステアリル(メタ)アクリレート、イソステアリル(メタ)アクリレート、シクロヘキシル(メタ)アクリレート、メチルシクロヘキシル(メタ)アクリレート、t-ブチルシクロヘキシル(メタ)アクリレート、シクロドデシル(メタ)アクリレート、トリシクロデカニル(メタ)アクリレート等。
(ii) イソボルニル基を有する重合性不飽和モノマー:イソボルニル(メタ)アクリレート等。
(iii) アダマンチル基を有する重合性不飽和モノマー:アダマンチル(メタ)アクリレート等。
(iv) トリシクロデセニル基を有する重合性不飽和モノマー:トリシクロデセニル(メタ)アクリレート等。
(v) 芳香環含有重合性不飽和モノマー:ベンジル(メタ)アクリレート、スチレン、α-メチルスチレン、ビニルトルエン等。
(vi) アルコキシシリル基を有する重合性不飽和モノマー:ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリス(2-メトキシエトキシ)シラン、γ-(メタ)アクリロイルオキシプロピルトリメトキシシラン、γ-(メタ)アクリロイルオキシプロピルトリエトキシシラン等。
(vii) フッ素化アルキル基を有する重合性不飽和モノマー:パーフルオロブチルエチル(メタ)アクリレート、パーフルオロオクチルエチル(メタ)アクリレート等のパーフルオロアルキル(メタ)アクリレート;フルオロオレフィン等。
(viii) マレイミド基等の光重合性官能基を有する重合性不飽和モノマー。
(ix) ビニル化合物:N-ビニルピロリドン、エチレン、ブタジエン、クロロプレン、プロピオン酸ビニル、酢酸ビニル等。
(x) カルボキシル基含有重合性不飽和モノマー:(メタ)アクリル酸、マレイン酸、クロトン酸、β-カルボキシエチル(メタ)アクリレート等。
(xi) 含窒素重合性不飽和モノマー:(メタ)アクリロニトリル、(メタ)アクリルアミド、N,N-ジメチルアミノエチル(メタ)アクリレート、N,N-ジエチルアミノエチル(メタ)アクリレート、N,N-ジメチルアミノプロピル(メタ)アクリルアミド、メチレンビス(メタ)アクリルアミド、エチレンビス(メタ)アクリルアミド、グリシジル(メタ)アクリレートとアミン化合物との付加物等。
(xii) 重合性不飽和基を1分子中に2個以上有する重合性不飽和モノマー:アリル(メタ)アクリレート、エチレングリコールジ(メタ)アクリレート、1,4-ブタンジオールジ(メタ)アクリレート、ネオペンチルグリコールジ(メタ)アクリレート、1,6-ヘキサンジオールジ(メタ)アクリレート等。
(xiii) エポキシ基含有重合性不飽和モノマー:グリシジル(メタ)アクリレート、β-メチルグリシジル(メタ)アクリレート、3,4-エポキシシクロヘキシルメチル(メタ)アクリレート、3,4-エポキシシクロヘキシルエチル(メタ)アクリレート、3,4-エポキシシクロヘキシルプロピル(メタ)アクリレート、アリルグリシジルエーテル等。
(xiv) 分子末端がアルコキシ基であるポリオキシエチレン鎖を有する(メタ)アクリレート。
(xv) スルホン酸基を有する重合性不飽和モノマー:2-アクリルアミド-2-メチルプロパンスルホン酸、2-スルホエチル(メタ)アクリレート、アリルスルホン酸、4-スチレンスルホン酸等;これらスルホン酸のナトリウム塩及びアンモニウム塩等。
(xvi) リン酸基を有する重合性不飽和モノマー:アシッドホスホオキシエチル(メタ)アクリレート、アシッドホスホオキシプロピル(メタ)アクリレート、アシッドホスホオキシポリ(オキシエチレン)グリコール(メタ)アクリレート、アシッドホスホオキシポリ(オキシプロピレン)グリコール(メタ)アクリレート等。
(xvii) 紫外線吸収性官能基を有する重合性不飽和モノマー:2-ヒドロキシ-4(3-メタクリロイルオキシ-2-ヒドロキシプロポキシ)ベンゾフェノン、2-ヒドロキシ-4-(3-アクリロイルオキシ-2-ヒドロキシプロポキシ)ベンゾフェノン、2,2’-ジヒドロキシ-4-(3-メタクリロイルオキシ-2-ヒドロキシプロポキシ)ベンゾフェノン、2,2’-ジヒドロキシ-4-(3-アクリロイルオキシ-2-ヒドロキシプロポキシ)ベンゾフェノン、2-[2-ヒドロキシ-5-[2-(メタクリロイルオキシ)エチル]フェニル]-2H-ベンゾトリアゾール等。
(xviii) 光安定性重合性不飽和モノマー:4-(メタ)アクリロイルオキシ1,2,2,6,6-ペンタメチルピペリジン、4-(メタ)アクリロイルオキシ-2,2,6,6-テトラメチルピペリジン、4-シアノ-4-(メタ)アクリロイルアミノ-2,2,6,6-テトラメチルピペリジン、1-(メタ)アクリロイル-4-(メタ)アクリロイルアミノ-2,2,6,6-テトラメチルピペリジン、1-(メタ)アクリロイル-4-シアノ-4-(メタ)アクリロイルアミノ-2,2,6,6-テトラメチルピペリジン、4-クロトノイルオキシ-2,2,6,6-テトラメチルピペリジン、4-クロトノイルアミノ-2,2,6,6-テトラメチルピペリジン、1-クロトノイル-4-クロトノイルオキシ-2,2,6,6-テトラメチルピペリジン等。
(xix) カルボニル基を有する重合性不飽和モノマー:アクロレイン、ダイアセトンアクリルアミド、ダイアセトンメタクリルアミド、アセトアセトキシエチルメタクリレート、ホルミルスチロール、4~7個の炭素原子を有するビニルアルキルケトン(例えば、ビニルメチルケトン、ビニルエチルケトン、ビニルブチルケトン)等。
(xx) 酸無水物基を有する重合性不飽和モノマー:無水マレイン酸、無水イタコン酸、無水シトラコン酸等。
光輝性顔料分散体(X)は、光輝性顔料(x2)を含有する。
本発明の複層塗膜形成方法によれば、次に、工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)が塗装され、透明着色第2ベース塗膜が形成される。
式:ヘイズ値=100*DF/(DF+PT)
水酸基含有樹脂(y1)
水酸基含有樹脂(y1)は、1分子中に少なくとも1個の水酸基を有する樹脂である。該水酸基含有樹脂(y1)としては、例えば、水酸基を有する、アクリル樹脂、ポリエステル樹脂、ポリウレタン樹脂、ポリオレフィン樹脂、ポリエーテル樹脂、ポリカーボネート樹脂、エポキシ樹脂、アルキド樹脂等の樹脂が挙げられる。これらはそれぞれ単独でもしくは2種以上組み合わせて使用することができる。
透明着色第2ベース塗料(Y)は、着色顔料(y2)を含有する。
本発明の複層塗膜形成方法によれば、次に、工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200~350の範囲内である脂肪族トリイソシアネート化合物(z2-1)を含有するクリヤ塗料(Z)が塗装され、クリヤ塗膜が形成される。
水酸基含有アクリル樹脂(z1)は、1分子中に少なくとも1個の水酸基を有するアクリル樹脂である。
Tg(℃)=Tg(K)-273 (2)
各式中、W1、W2、・・は共重合に使用されたモノマーのそれぞれの質量分率、T1、T2、・・はそれぞれの単量体のホモポリマ-のTg(K)を表わす。なお、T1、T2、・・は、Polymer Hand Book(Second Edition,J.Brandup・E.H.Immergut 編)III-139~179頁による値である。また、モノマーのホモポリマーのTgが明確でない場合のガラス転移温度(℃)は、静的ガラス転移温度とし、例えば示差走査熱量計「DSC-220U」(セイコーインスツルメント社製)を用いて、試料を測定カップにとり、真空吸引して完全に溶剤を除去した後、3℃/分の昇温速度で-20℃~+200℃の範囲で熱量変化を測定し、低温側の最初のベースラインの変化点を静的ガラス転移温度とした。
本発明に係るクリヤ塗料(Z)は、ポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200~350の範囲内である脂肪族トリイソシアネート化合物(z2-1)を含有する。
脂肪族トリイソシアネート化合物(z2-1)は、分子量が200~350の範囲内であり、イソシアネート基を3個有する脂肪族ポリイソシアネート化合物である。なかでも、形成される複層塗膜の耐水性等の観点から、分子量が200~300の範囲内であることが好ましく、230~280の範囲内であることがより好ましい。
脂肪族トリイソシアネート化合物(z2-1)以外のポリイソシアネート化合物としては、例えば、前記脂肪族トリイソシアネート化合物(z2-1)以外の脂肪族ポリイソシアネート化合物、脂環族ポリイソシアネート化合物、芳香脂肪族ポリイソシアネート化合物、芳香族ポリイソシアネート化合物、該ポリイソシアネート化合物の誘導体等を挙げることができる。
本発明の複層塗膜形成方法によれば、次に、前記工程(2)~(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる。
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15~80質量部の範囲内である光輝性顔料分散体(X)を塗装して光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200~350の範囲内である脂肪族トリイソシアネート化合物(z2-1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)~(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法。
項21.被塗物には、カチオン電着塗料又はアニオン電着塗料である下塗り塗料が施されている項1~20のいずれか1項に記載の複層塗膜形成方法。
1.基材の作製
脱脂及びりん酸亜鉛処理した鋼板(JISG3141、大きさ400mm×300mm×0.8mm)にカチオン電着塗料「エレクロンGT-10」(商品名:関西ペイント株式会社製、エポキシ樹脂ポリアミン系カチオン樹脂に硬化剤としてブロックポリイソシアネート化合物を使用したもの)を硬化塗膜に基づいて膜厚が20μmになるように電着塗装し、170℃で20分加熱して架橋硬化させ、電着塗膜を形成せしめることにより、被塗物とした。
水酸基含有樹脂(w1)の製造
水分散性水酸基含有アクリル樹脂(w11-1)の製造
製造例1
温度計、サーモスタット、撹拌装置、還流冷却器及び滴下装置を備えた反応容器に、脱イオン水70.7部及び「アクアロンKH-10」(商品名、第一工業製薬社製、乳化剤、有効成分97%)0.52部を仕込み、窒素気流中で撹拌混合し、80℃に昇温した。次いで、下記のモノマー乳化物のうちの全量の1%量及び6%過硫酸アンモニウム水溶液5部を反応容器内に導入し80℃で15分間保持した。その後、残りのモノマー乳化物を3時間かけて、同温度に保持した反応容器内に滴下し、滴下終了後1時間熟成した後、5%2-(ジメチルアミノ)エタノール水溶液40部を反応容器に徐々に加えながら30℃まで冷却し、100メッシュのナイロンクロスで濾過しながら排出し、固形分濃度45%の水分散性水酸基含有アクリル樹脂(w11-1)を得た。得られた水分散性水酸基含有アクリル樹脂の水酸基価は43mgKOH/g、酸価は12mgKOH/gであった。
製造例2
温度計、サーモスタット、攪拌装置、還流冷却器及び水分離器を備えた反応容器に、トリメチロールプロパン174部、ネオペンチルグリコール327部、アジピン酸352部、イソフタル酸109部及び1,2-シクロヘキサンジカルボン酸無水物101部を仕込み、160℃から230℃まで3時間かけて昇温させた後、生成した縮合水を水分離器により留去させながら230℃で保持し、酸価が3mgKOH/g以下となるまで反応させた。この反応生成物に、無水トリメリット酸59部を添加し、170℃で30分間付加反応を行った後、50℃以下に冷却し、2-(ジメチルアミノ)エタノールを酸基に対して当量添加し中和してから、脱イオン水を徐々に添加することにより、固形分濃度45%の水酸基含有ポリエステル樹脂溶液(w12-1)を得た。得られた水酸基含有ポリエステル樹脂は、水酸基価が128mgKOH/g、酸価が35mgKOH/g、重量平均分子量が13000であった。
製造例3
製造例2で得た水酸基含有ポリエステル樹脂溶液(w12-1)56部(固形分25部)、「タイペーク UT-771」(商品名、ルチル型二酸化チタン顔料、石原産業社製)70部、「カーボン MA-100」(商品名、カーボンブラック顔料、三菱ケミカル社製)0.5部及び脱イオン水5部を混合し、2-(ジメチルアミノ)エタノールでpH8.0に調整した。次いで、得られた混合液を広口ガラスビン中に入れ、分散メジアとして直径約1.3mmφのガラスビーズを加えて密封し、ペイントシェイカーにて30分間分散して、顔料分散液(P-1)を得た。
製造例4
製造例3で得た顔料分散ペースト(P-1)131.5部、製造例1で得た水分散性水酸基含有アクリル樹脂(w11-1)44.4部(固形分20部)、「ユーコートUX-8100」(商品名、ウレタンエマルション、三洋化成工業社製、固形分35%)71.4部(固形分25部)及び「サイメル325」(商品名、メラミン樹脂、オルネクスジャパン社製、固形分80%)37.5部(固形分30部)を均一に混合した。次いで、得られた混合物に、「UH-752」(商品名、ADEKA社製、増粘剤)、2-(ジメチルアミノ)エタノール及び脱イオン水を添加し、pH8.0、塗料固形分25%、B型粘度計を用いて20℃において回転数6rpmで測定したときの粘度が3000mPa・sの着色塗料(W-1)を得た。
コア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’-1)の製造
製造例5
温度計、サーモスタット、撹拌器、還流冷却器及び滴下装置を備えた反応容器に、脱イオン水145部及び「アクアロンKH-10」0.52部を仕込み、窒素気流中で撹拌混合し、80℃に昇温した。次いで下記のモノマー乳化物(1)のうちの全量の1%量及び6%過硫酸アンモニウム水溶液5.3部を反応容器内に導入し80℃で15分間保持した。その後、残りのモノマー乳化物(1)を3時間かけて、同温度に保持した反応容器内に滴下し、滴下終了後1時間熟成を行なった。その後、下記のモノマー乳化物(2)を1時間かけて滴下し、1時間熟成した後、5%ジメチルエタノールアミン水溶液40部を反応容器に徐々に加えながら30℃まで冷却し、100メッシュのナイロンクロスで濾過しながら排出し、固形分濃度28%のコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’-1)を得た。得られたコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’-1)は、水酸基価が25mgKOH/g、酸価が33mgKOH/gであった。
製造例6
攪拌混合容器に、蒸留水50.1部、「レオクリスタ」(商品名、第一工業製薬社製、セルロースナノファイバー、固形分2%)25.5部(固形分0.5部)、「Dynol-604」(商品名、エボニックインダストリーズ社製、アセチレンジオール系表面調整剤、固形分100%)0.3部(固形分0.3部)、「Hydroshine WS-3001」(商品名、水性用蒸着アルミニウムフレーク顔料、Eckart社製、固形分:10%、内部溶剤:イソプロパノール、平均粒子径D50:13μm、厚さ:0.05μm、表面がシリカ処理されている)12.1部(固形分1.2部)、製造例5で得たコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’-1)2.5部(固形分0.7部)、「TINUVIN 479-DW(N)」(商品名、BASF社製、紫外線吸収剤、固形分40%)0.3部(固形分0.1部)、「TINUVIN 123-DW(N)」(商品名、BASF社製、光安定剤、固形分50%)0.2部(固形分0.1部)、2-エチルヘキサノール0.5部、イソプロピルアルコール8.5部を添加して攪拌混合し、光輝性顔料分散体(X-1)を調整した。
表1に記載の配合とする以外は全て製造例6と同様にして光輝性顔料分散体(X-2)~(X-8)を得た。
「WBC-713T エナメルクリヤ」(商品名、関西ペイント社製、水性ベースコート塗料、透明色)に「GX-3100」(商品名、旭化成社製、アルミニウムフレーク、固形分74%、平均粒子径10μm)を添加し、合計固形分100質量部を基準として、「GX-3100」の含有量が8質量部となるように調整し、撹拌して、光輝性顔料分散体(X-9)とした。
水酸基含有アクリル樹脂溶液(y11-1)の製造
製造例15
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器にプロピレングリコールモノプロピルエーテル35部を仕込み85℃に昇温後、メチルメタクリレート30部、2-エチルヘキシルアクリレート20部、n-ブチルアクリレート29部、2-ヒドロキシエチルアクリレート15部、アクリル酸6部、プロピレングリコールモノプロピルエーテル15部及び2,2’-アゾビス(2,4-ジメチルバレロニトリル)2.3部の混合物を4時間かけて滴下し、滴下終了後1時間熟成した。その後さらにプロピレングリコールモノプロピルエーテル10部及び2,2’-アゾビス(2,4-ジメチルバレロニトリル)1部の混合物を1時間かけて滴下し、滴下終了後1時間熟成した。さらにジエタノールアミン7.4部を加え、固形分55%の水酸基含有アクリル樹脂溶液(y11-1)を得た。得られた水酸基含有アクリル樹脂は酸価が47mgKOH/g、水酸基価が72mgKOH/g、重量平均分子量が58000であった。
製造例16
温度計、サーモスタット、攪拌装置、還流冷却器及び水分離器を備えた反応容器に、トリメチロールプロパン109部、1,6-ヘキサンジオール141部、1,2-シクロヘキサンジカルボン酸無水物126部及びアジピン酸120部を仕込み、160℃から230℃迄3時間かけて昇温させた後、230℃で4時間縮合反応させた。次いで、得られた縮合反応生成物に、カルボキシル基を導入するために、無水トリメリット酸38.3部を加えて、170℃で30分間反応させた後、2-エチル-1-ヘキサノールで希釈し、固形分70%の水酸基含有ポリエステル樹脂溶液(y12-1)を得た。得られた水酸基含有ポリエステル樹脂は、酸価が46mgKOH/g、水酸基価が150mgKOH/g、数平均分子量が1400であった。
製造例17
製造例15で得た水酸基含有アクリル樹脂溶液(y11-1)327部(固形分180部)、脱イオン水360部、「サーフィノール104A」(商品名、エアープロダクツ社製消泡剤、固形分50%)6部(固形分3部)、及び「バリファインBF-20」(商品名、堺化学工業社製、硫酸バリウム粉末、平均粒子径0.03μm)250部(固形分250部)を、ペイントコンディショナー中に入れ、ガラスビーズ媒体を加えて、室温で1時間混合分散し、固形分44%の顔料分散液(P-2)を得た。
製造例15で得た水酸基含有アクリル樹脂溶液(y11-1)182部(固形分100部)、「CHROMOFINE BLUE 5206M」(商品名、大日精化工業社製、フタロシアニン系青色顔料)100部(固形分100部)及び脱イオン水450部を混合し、2-アミノ-2-メチル-1-プロパノールでpH7.5に調整した後、ペイントシェーカーで2時間分散して固形分27%の顔料分散液(P-3)を得た。
製造例15で得た水酸基含有アクリル樹脂溶液(y11-1)182部(固形分100部)、「MAROON 179 229-6438」(商品名、SUN CHEMICAL CORPORATION社製、有機ペリレン顔料)150部(固形分150部)及び脱イオン水479部を混合し、2-アミノ-2-メチル-1-プロパノールでpH7.5に調整した後、ペイントシェーカーで2時間分散して固形分31%の顔料分散液(P-4)を得た。
製造例15で得た水酸基含有アクリル樹脂溶液(y11-1)182部(固形分100部)、「Irgazin DPP Red BO」(商品名、BASF社製、ジケトピロロピロール顔料)150部(固形分150部)及び脱イオン水479部を混合し、2-アミノ-2-メチル-1-プロパノールでpH7.5に調整した後、ペイントシェーカーで2時間分散して固形分31%の顔料分散液(P-5)を得た。
製造例21
攪拌混合容器に、製造例17で得た顔料分散液(P-2)31.8部(固形分14部)、製造例5で得たコア/シェル型複層構造を有する水分散性水酸基含有アクリル樹脂(x111’-1)107.1部(固形分30部)、製造例16で得た水酸基含有ポリエステル樹脂溶液(y12-1)32.9部(固形分23部)、「ユーコートUX-310」(商品名、三洋化成社製、ウレタン樹脂水分散体、固形分含有率40%)32.5部(固形分13部)、及び「サイメル251」(商品名、オルネクスジャパン社製、メラミン樹脂、固形分含有率80%)37.5部(固形分30部)となるように添加して攪拌混合し、透明第2ベース塗料(V-1)を調製した。
製造例22
攪拌混合容器に、製造例21で得た透明第2ベース塗料(V-1)を入れ、樹脂固形分100質量部に対して「CHROMOFINE BLUE 5206M」(商品名、大日精化工業社製、フタロシアニン系青色顔料)が5質量部となるように製造例18で得た顔料分散液(P-3)を添加して、攪拌混合し、透明青色第2ベース塗料(Y-1)を調製した。
攪拌混合容器に、製造例21で得た透明第2ベース塗料(V-1)を入れ、樹脂固形分100質量部に対して「MAROON 179 229-6438」(商品名、SUN CHEMICAL CORPORATION社製、有機ペリレン顔料)が5質量部となるように製造例19で得た顔料分散液(P-4)を添加して、攪拌混合し、透明赤色第2ベース塗料(Y-2)を調製した。
製造例24
攪拌混合容器に、製造例21で得た透明第2ベース塗料(V-1)を入れ、樹脂固形分100質量部に対して「Irgazin DPP Red BO」(商品名、BASF社製、ジケトピロロピロール顔料)が5質量部となるように製造例20で得た顔料分散液(P-5)を添加して、攪拌混合し、着色赤色第2ベース塗料(V-2)を調製した。
上記で得られた透明着色第2ベース塗料(Y-1)、(Y-2)及び着色第2ベース塗料(V-2)を用い、塗膜のヘイズ値を、「濁度計COH-300A」(商品名、日本電色工業社製)にて測定した拡散光線透過率(DF)及び平行光線透過率(PT)から、次式によって計算し、評価した。
式:ヘイズ値=100*DF/(DF+PT)
塗膜は、平滑なPTFE板上に、透明着色第2ベース塗料(Y-1)、(Y-2)及び着色第2ベース塗料(V-2)のいずれかをミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として10μmの膜厚となるように塗装し、室温にて3分間放置し、熱風循環式乾燥炉内にて140℃で30分間加熱した後、PTFE板から剥離することにより得た。上記着色第2ベース塗料(V-2)は、得られた塗膜のヘイズ値が30%を超えており、本発明に係る透明着色第2ベース塗料に該当しない。
水酸基含有アクリル樹脂(z1-1)の製造
製造例25
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管及び滴下装置を備えた反応容器に、「スワゾール1000」(商品名、コスモ石油社製、芳香族系有機溶剤)27部及びプロピレングリコールモノメチルエーテルアセテート5部を仕込み、窒素ガスを吹き込みながら150℃で攪拌し、この中にスチレン20部、2-ヒドロキシプロピルアクリレート32.5部、イソブチルメタクリレート46.8部、アクリル酸0.7部及びジターシャリアミルパーオキサイド(重合開始剤)6.0部からなるモノマー混合物を4時間かけて均一速度で滴下した。その後、150℃で1時間熟成させた後冷却し、さらに酢酸イソブチルを21部加えて希釈し、固形分濃度65質量%の水酸基含有アクリル樹脂(z1-1)溶液を得た。得られた水酸基含有アクリル樹脂(z1-1)の水酸基価は139mgKOH/g、酸価は5.5mgKOH/g、重量平均分子量は5,500、ガラス転移温度38℃であった。
製造例26
製造例25で得た水酸基含有アクリル樹脂(z1-1)溶液108.6部(固形分70.6部)、「BYK-300」(商品名、ビックケミー社製、表面調整剤、有効成分52%)0.4部(固形分0.2部)を均一に混合した主剤と、
硬化剤として、1,8-ジイソシアナト-4-イソシアナトメチルオクタン(固形分100%、NCO含有率50%、分子量251、粘度は23℃において8mPa・s)29.4部(固形分29.4部)とを塗装直前に均一に混合し、さらに、酢酸ブチルを加えて、20℃におけるフォードカップNo.4による粘度が30秒となるように調整してクリヤ塗料(Z-1)を得た。
表3に記載の配合とする以外は全て製造例26と同様にしてクリヤ塗料(Z-2)~(Z-7)を得た。
(注3)「スミジュールN3300」:商品名、住化コベストロウレタン社製、ヘキサメチレンジイソシアネートのイソシアヌレート体、固形分100%、NCO含有率21.8%、
(注4)「スミジュールN3400」:商品名、住化コベストロウレタン社製、ヘキサメチレンジイソシアネートのウレトジオン体、固形分100%、NCO含有率21.8%。
試験板の作成
実施例1
(着色塗料(W)の塗装)
上記1.で作製した基材上に、上記2.で製造した着色塗料(W-1)をミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として25μmの膜厚となるように塗装し、室温にて15分間放置し、未硬化の着色塗膜を得た。
上記未硬化の着色塗膜上に、上記2.で製造した光輝性顔料分散体(X-1)をミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として1μmの膜厚となるように塗装し、室温にて2分間放置し、未硬化の光輝性第1ベース塗膜を得た。
上記未硬化の光輝性第1ベース塗膜上に、上記2.で製造した透明着色第2ベース塗料(Y-1)をミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として10μmの膜厚となるように塗装し、室温にて3分間放置した後、80℃で3分間プレヒートを行い、未硬化の透明着色第2ベース塗膜を得た。
上記未硬化の透明着色第2ベース塗膜上に、上記2.で製造したクリヤ塗料(Z-1)を、ミニベル型回転式静電塗装機を用いて、ブース温度23℃、湿度68%の条件で、硬化塗膜として35μmとなるように塗装し、室温にて7分間放置した後、熱風循環式乾燥炉内にて140℃で30分間加熱し、着色塗膜、光輝性第1ベース塗膜、透明着色第2ベース塗膜及びクリヤ塗膜からなる複層塗膜を同時に乾燥硬化せしめて試験板を作製した。
x=sc/sg/S*10000
x:膜厚[μm]
sc:塗着固形分[g]
sg:塗膜比重[g/cm3]
S:塗着固形分の評価面積[cm2]
表4に記載の塗料、膜厚とする以外は全て実施例1と同様にして試験板を得た。
上記のようにして得られた各試験板について、以下の方法で塗膜を評価し、表4にその結果を示した。
(1)L*C*h表色系における彩度C*(15°)
各試験板について、「MA-68II」(商品名、x-rite社製)を使用して、L*C*h表色系における彩度C*(15°)を測定した。値が大きいほど彩度が高いことを示す。
各試験板について、「MA-68II」(商品名、x-rite社製)を使用して、IV68を測定した。値が大きいほど、輝度感が良好であることを示す。
各試験板について、「MA-68II」(商品名、x-rite社製)を使用して、SV68を測定した。値が小さいほど、光輝材の配向が良好であることを示す。
上記IV68及びSV68から下記計算式によって求められる値であり、値が大きいほどフリップフロップ性が高いことを表す。
試験板を40℃の温水に240時間浸漬し、引き上げ、布で水滴・汚れをふきとり、室温23℃で10分以内に、試験板の複層塗膜を素地に達するようにカッターで格子状に切り込み、大きさ2mm×2mmのゴバン目を100個作る。続いて、その表面に粘着セロハンテープを貼着し、そのテープを急激に剥離した後のゴバン目塗膜の残存状態を調べ、下記基準で耐水性を評価した。A及びBが合格である。
A:ゴバン目塗膜が100個残存し、カッターの切り込みの縁において塗膜の小さな縁欠けが生じていない、
B:ゴバン目塗膜が100個残存するが、カッターの切り込みの縁において塗膜の小さな縁欠けが生じており、縁欠けした残存塗膜が10個未満である、
C:ゴバン目塗膜が100個残存するが、カッターの切り込みの縁において塗膜の小さな縁欠けが生じており、縁欠けした残存塗膜が10個以上である、
D:ゴバン目塗膜が90~99個残存する、
E:ゴバン目塗膜の残存数が89個以下である。
促進耐候性試験には、JIS B 7754に規定されたスーパーキセノンウェザオメーター(商品名、スガ試験機社製)を使用し、1時間42分間のキセノンアークランプの照射と18分間の降雨条件における同ランプの照射による2時間を1サイクルとして、4000時間経過後に、上記耐水付着性試験と同様の操作を行った。A、B及びCが合格である。
Claims (14)
- 下記の工程(1)~(5):
工程(1):被塗物上に、水酸基含有樹脂(w1)及び着色顔料(w2)を含有する着色塗料(W)を塗装して、着色塗膜を形成する工程、
工程(2):工程(1)で得られる着色塗膜上に、水酸基含有樹脂(x1)及び光輝性顔料(x2)を含有する光輝性顔料分散体(X)であって、該光輝性顔料分散体(X)中の上記光輝性顔料(x2)の含有量が、該光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15~80質量部の範囲内である光輝性顔料分散体(X)を塗装して光輝性第1ベース塗膜を形成する工程、
工程(3):工程(2)で得られる光輝性第1ベース塗膜上に、水酸基含有樹脂(y1)及び着色顔料(y2)を含有する透明着色第2ベース塗料(Y)を塗装して、透明着色第2ベース塗膜を形成する工程、
工程(4):工程(3)で得られる透明着色第2ベース塗膜上に、水酸基含有アクリル樹脂(z1)及びポリイソシアネート化合物(z2)を含有し、かつ該ポリイソシアネート化合物(z2)が少なくともその1種として、分子量が200~350の範囲内である脂肪族トリイソシアネート化合物(z2-1)を含有するクリヤ塗料(Z)を塗装してクリヤ塗膜を形成する工程、ならびに、
工程(5):前記工程(2)~(4)で形成される光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を含む複層塗膜を加熱することによって、前記複層塗膜を同時に硬化させる工程、を含む複層塗膜形成方法。 - 前記着色塗料(W)が、水性塗料である請求項1に記載の複層塗膜形成方法。
- 前記着色塗料(W)が、さらにメラミン樹脂及び/又はブロック化ポリイソシアネート化合物を含有する請求項1又は2に記載の複層塗膜形成方法。
- 前記光輝性顔料分散体(X)が、水性塗料である請求項1~3のいずれか1項に記載の複層塗膜形成方法。
- 前記光輝性顔料分散体(X)において、前記水酸基含有樹脂(x1)が、水分散性水酸基含有アクリル樹脂(x111)を含む請求項4に記載の複層塗膜形成方法。
- 前記光輝性顔料(x2)が、蒸着アルミニウムフレーク顔料を含み、該蒸着アルミニウムフレーク顔料の含有量が、前記光輝性顔料分散体(X)中の合計固形分100質量部を基準として、15~55質量部の範囲内である請求項1~5のいずれか1項に記載の複層塗膜形成方法。
- 前記光輝性顔料(x2)が、アルミニウムフレーク顔料を含み、該アルミニウムフレーク顔料の含有量が、前記光輝性顔料分散体(X)中の合計固形分100質量部を基準として、45~80質量部の範囲内である請求項1~5のいずれか1項に記載の複層塗膜形成方法。
- 前記透明着色第2ベース塗料(Y)が、水性塗料である請求項1~7のいずれか1項に記載の複層塗膜形成方法。
- 前記透明着色第2ベース塗料(Y)が、さらにメラミン樹脂及び/又はブロック化ポリイソシアネート化合物を含有する請求項1~8のいずれか1項に記載の複層塗膜形成方法。
- 前記クリヤ塗料(Z)において、ポリイソシアネート化合物(z2)のイソシアネート基の合計molと、水酸基含有アクリル樹脂(z1)の水酸基の合計molとの当量比(NCO/OH)が、1.1~2.5の範囲内である請求項1~9のいずれか1項に記載の複層塗膜形成方法。
- 前記光輝性第1ベース塗膜の膜厚が、0.02~7μmの範囲内である請求項1~10のいずれか1項に記載の複層塗膜形成方法。
- 前記透明着色第2ベース塗膜の膜厚が、3~30μmの範囲内である請求項1~11のいずれか1項に記載の複層塗膜形成方法。
- 前記工程(2)において、加熱硬化させた前記着色塗膜上に、光輝性顔料分散体(X)を塗装する、請求項1~12のいずれか1項に記載の複層塗膜形成方法。
- 前記工程(2)において、未硬化の前記着色塗膜上に、光輝性顔料分散体(X)を塗装し、
前記工程(5)において、前記工程(1)~(4)で形成される着色塗膜、光輝性第1ベース塗膜、透明着色第2ベース塗膜、及びクリヤ塗膜を同時に加熱することによって、これら4つの塗膜を含む複層塗膜を一度に硬化させる請求項1~12のいずれか1項に記載の複層塗膜形成方法。
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