WO2017163817A1 - ポリオレフィン系樹脂接着用表面処理金属板及びそれを用いた複合部材 - Google Patents
ポリオレフィン系樹脂接着用表面処理金属板及びそれを用いた複合部材 Download PDFInfo
- Publication number
- WO2017163817A1 WO2017163817A1 PCT/JP2017/008458 JP2017008458W WO2017163817A1 WO 2017163817 A1 WO2017163817 A1 WO 2017163817A1 JP 2017008458 W JP2017008458 W JP 2017008458W WO 2017163817 A1 WO2017163817 A1 WO 2017163817A1
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- WO
- WIPO (PCT)
- Prior art keywords
- acid
- resin
- chemical conversion
- polyolefin resin
- adhesive layer
- Prior art date
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C22/68—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous solutions with pH between 6 and 8
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- B32B2323/10—Polypropylene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2419/00—Buildings or parts thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2479/00—Furniture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2509/00—Household appliances
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/304—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being heat-activatable, i.e. not tacky at temperatures inferior to 30°C
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/10—Presence of inorganic materials
- C09J2400/16—Metal
- C09J2400/163—Metal in the substrate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2451/00—Presence of graft polymer
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2451/00—Presence of graft polymer
- C09J2451/003—Presence of graft polymer in the primer coating
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Definitions
- the present invention relates to a polyolefin-based resin-treated surface-treated metal plate excellent in adhesiveness and a composite member using the same.
- metal parts such as steel plates (metal plates) are used in automobiles, home appliances, office automation equipment, and the like. In many cases, such a metal part is used after a metal plate is press-molded and given a predetermined shape and then joined to another metal part or a plastic part by welding or screwing.
- the adhesion of plastic to the surface of the metal plate can be imparted, after the metal plate is press-molded, it is set in a plastic mold, poured into molten plastic, and solidified by cooling.
- a metal plate composite resin molded product (hereinafter referred to as a composite member) bonded to a resin molded product such as a plastic part can be formed, which leads to the efficiency of the member manufacturing process and the weight reduction of the member.
- the present applicant is a surface-treated steel sheet in which a metal substrate, a chemical conversion treatment film, and an adhesive layer are laminated in this order.
- a surface-treated steel sheet is proposed in which the treated film contains colloidal silica and a thermosetting resin.
- Patent Document 1 a resin molded product containing a polypropylene resin is used.
- the composite member obtained by bonding the surface-treated steel sheet of Patent Document 1 and a resin molded product containing polypropylene resin has a certain degree of adhesive strength between the metal substrate and the resin molded product (hereinafter, simply referred to as adhesive strength).
- adhesive strength the degree of adhesive strength between the metal substrate and the resin molded product.
- the resin contained in the chemical conversion film is a thermosetting resin, the chemical conversion film and the adhesive layer may be easily peeled off. That is, it may not be said that there is sufficient adhesion when used in applications where high adhesion is required, such as automobile structural parts.
- Patent Document 1 also proposes a surface-treated steel sheet in which a primer layer is provided between the chemical conversion film and the adhesive layer to increase the adhesive strength, but the surface treatment is performed by laminating three layers on the metal substrate. It is necessary to produce a steel plate, which increases the number of manufacturing steps and increases the manufacturing cost. In addition, it is desired to reduce the number of stacked layers from the viewpoint of weight reduction of members that are required in recent years.
- an object of the present invention is to provide a surface-treated metal sheet for bonding a polyolefin resin excellent in adhesiveness at a low cost.
- One aspect of the present invention is a polyolefin-based resin-bonded surface-treated metal plate in which an adhesive layer is laminated on at least one surface of a metal substrate via a chemical conversion treatment film, the coating forming the chemical conversion treatment film.
- the working solution contains an acid-modified polyolefin resin, colloidal silica, and a silane coupling agent, and the amount of the chemical conversion coating is 0.05 to 3 g / m 2 in terms of dry mass. It contains an acid-modified polyolefin resin, and the adhesive layer has a thickness of 5 to 100 ⁇ m.
- the adhesive bond layer is laminated
- the coating liquid for forming the chemical conversion film contains an acid-modified polyolefin resin, colloidal silica, and a silane coupling agent, and the amount of the chemical conversion film is 0.05 to 3 g / m 2 in terms of dry mass.
- the adhesive layer contains an acid-modified polyolefin resin, and the thickness of the adhesive layer is 5 to 100 ⁇ m.
- the surface treatment metal plate excellent in adhesiveness can be manufactured at low cost by using the chemical conversion treatment film containing acid-modified polyolefin resin and the adhesive bond layer containing acid-modified polyolefin resin.
- the surface-treated metal plate of the present invention can be used for casings and interior / exterior parts of automobiles and household electric products, and for outer plate materials such as steel furniture and building materials.
- the composite member of the present invention is useful for various applications such as automobile parts, home appliances, building materials, and OA equipment.
- an adhesive layer is laminated on at least one surface of the metal substrate only through the chemical conversion treatment film.
- Metal substrate (steel plate)
- a metal substrate used by this invention for example, in addition to steel plates, such as a non-plated cold rolled steel plate, a hot dip galvanized steel plate, an alloyed hot dip galvanized steel plate, an electrogalvanized steel plate, an aluminum plate and a titanium plate Etc.
- a hot dip galvanized steel plate, an electrogalvanized steel plate, an aluminum plate, and a titanium plate are preferable, and an alloyed hot dip galvanized steel plate is more preferable.
- the thickness of the metal substrate is not particularly limited, but is preferably about 0.3 to 3.2 mm for reducing the weight of the final product.
- various metal substrates can be used for this invention.
- the chemical conversion treatment film can be prepared using a coating solution for forming a chemical conversion treatment film containing an acid-modified polyolefin resin, colloidal silica, and a silane coupling agent.
- the coating liquid for forming a chemical conversion treatment film used in the present embodiment contains an acid-modified polyolefin resin, that is, the chemical conversion treatment film contains an acid-modified polyolefin resin.
- the acid-modified polyolefin resin preferably includes an acid-modified polypropylene resin.
- the acid-modified polyolefin resin used in the present embodiment is obtained by graft polymerization of at least one selected from the group consisting of unsaturated dicarboxylic acids, anhydrides thereof and ester derivatives onto the polyolefin resin.
- the polyolefin resin used as a raw material for the acid-modified polyolefin resin examples include polyethylene, polypropylene, polybutene, polymethylpentene, ⁇ -olefin and ethylene or propylene copolymer, ethylene-vinyl acetate copolymer, ethylene- Resin such as acrylic acid copolymer, ethylene-methacrylic acid copolymer, ethylene-maleic anhydride copolymer, propylene-maleic anhydride copolymer, etc., may be used alone or in combination of two or more. It may be used. From the viewpoint of suppressing peeling between the chemical conversion film and the adhesive layer, the polyolefin resin preferably includes a polypropylene resin, and more preferably a polypropylene resin.
- the polypropylene resin may be homopolypropylene (propylene homopolymer), which is a copolymer of propylene and one or more selected from the group consisting of ethylene, other ⁇ -olefins, and vinyl compounds. Also good.
- Other ⁇ -olefins are preferably ⁇ -olefins having 4 to 18 carbon atoms, such as 1-butene, isobutene, 1-pentene, 4methyl-1-pentene, 1-hexene, 1-octene, 1-decene, -Dodecene and the like.
- homopolypropylene is particularly preferable from the viewpoint of adhesion between the chemical conversion film and the adhesive layer.
- Examples of the unsaturated dicarboxylic acid include maleic acid, fumaric acid, citraconic acid, mesaconic acid, itaconic acid and the like.
- Examples of the unsaturated dicarboxylic acid anhydride include maleic anhydride, itaconic anhydride, citraconic anhydride, and the like.
- Examples of the ester derivative of unsaturated dicarboxylic acid include monomethyl maleate. Of these, unsaturated dicarboxylic acid anhydrides are preferred, and maleic anhydride is more preferred.
- the unsaturated dicarboxylic acid, anhydride or ester derivative thereof may be used alone or in combination of two or more.
- the acid-modified polyolefin resin is produced by graft polymerization of unsaturated dicarboxylic acid, its anhydride or ester derivative to the above-mentioned polyolefin resin according to a conventional method.
- a maleic anhydride-modified polyolefin resin can be synthesized as follows. Using xylene, 2,2,4-trimethyl-1,3-pentanediol diisobutyrate as a solvent, polypropylene resin, maleic anhydride, and organic peroxides (eg, t-butylperoxy-2-ethylhexyl carbonate) ) In any order or together, and maleic anhydride-modified polyolefin resin is obtained by graft polymerization of maleic anhydride onto the polyolefin resin under normal heating, for example, at about 130 to 150 ° C. I can do it.
- organic peroxides eg, t-butylperoxy-2-ethylhexyl carbonate
- the acid value of the acid-modified polyolefin resin in the chemical conversion film is preferably 3 to 100 mgKOH / g, more preferably 5 to 80 mgKOH / g, and still more preferably 5 to 60 mKOH / g.
- the acid value is less than 3 mgKOH / g, it is difficult to produce a water-based chemical conversion coating film-forming coating solution.
- the graft amount of maleic anhydride in the acid-modified polyolefin resin is preferably 0.1 to 10% by mass, more preferably 0.3 to 7% by mass, and 0.5 to 5% by mass. More preferably. If the graft amount is less than 0.1% by mass, the adhesive strength may be insufficient. On the other hand, when the graft amount exceeds 10% by mass, the compatibility with the unmodified polyolefin resin may be deteriorated.
- 2 or more types of unsaturated dicarboxylic acid, its anhydride, and ester derivative are used, let the sum of these content be graft amount.
- the chemical conversion film preferably does not contain any thermoplastic resin other than the acid-modified polyolefin resin, but other thermoplastic resins other than the acid-modified polyolefin resin may be used as long as the effects of the present invention are not impaired. May be included.
- thermoplastic resins include polystyrene resin, acrylonitrile-butadiene-styrene (ABS) copolymer, acrylonitrile-EPDM-styrene (AES) copolymer, acrylic resin, polybutadiene, polyacetal resin, polyether resin, Polyvinyl acetate, polyvinyl chloride, polyvinylidene chloride and the like can be mentioned, and these may be used alone or in combination of two or more.
- the content of the acid-modified polyolefin resin is preferably 80% by mass or more, more preferably 90% by mass or more, and 99.91% by mass or more. Is more preferably 99.95% by mass or more, and most preferably 100% by mass (the resin contained in the chemical conversion film is only an acid-modified polyolefin resin).
- the thermoplastic resin is preferably 30 to 60 parts by mass, more preferably 35 to 55 parts by mass, and more preferably 40 to 50 parts by mass in 100 parts by mass of the solid content of the coating solution for forming a chemical conversion film. More preferably. Further, the thermoplastic resin contained in the chemical conversion coating is preferably 30 to 60% by mass, more preferably 35 to 55% by mass, and further preferably 40 to 50% by mass.
- the coating liquid for forming a chemical conversion film preferably contains colloidal silica. That is, it is preferable that colloidal silica is contained in the chemical conversion treatment film of this embodiment. It is because it has the effect which improves corrosion resistance by including colloidal silica.
- colloidal silica “XS”, “SS”, “40”, “N”, “UP”, etc. of “Snowtex (registered trademark)” series (colloidal silica manufactured by Nissan Chemical Industries, Ltd.) are preferably used. .
- “Snowtex (registered trademark) 40” having a surface area average particle diameter of about 10 to 20 nm is preferably used.
- the amount of colloidal silica is preferably 30 to 60 parts by mass, more preferably 35 to 55 parts by mass, and more preferably 40 to 50 parts by mass, based on 100 parts by mass of the solid content of the chemical conversion film forming coating solution. More preferably. Further, the amount of colloidal silica contained in the chemical conversion coating is preferably 50 to 150 parts by mass and preferably 75 to 125 parts by mass with respect to 100 parts by mass of the thermoplastic resin contained in the chemical conversion coating. More preferred.
- the silane coupling agent is contained in the coating liquid for chemical conversion treatment film formation.
- the adhesion of the chemical conversion film to the metal substrate can be improved.
- the silane coupling agent include ⁇ -aminopropyltrimethoxysilane, ⁇ -aminopropyltriethoxysilane, N- ( ⁇ -aminoethyl) - ⁇ -aminopropyltrimethoxysilane, N- ( amino group-containing silane coupling agents such as ⁇ -aminoethyl) - ⁇ -aminopropylmethyldimethoxysilane; ⁇ -glycidoxypropyltrimethoxysilane, ⁇ -glycidoxypropylmethyldimethoxysilane, ⁇ -glycidoxypropyltri Glycidoxy group-containing silane coupling agents such as ethoxysilane and ⁇ -glycidoxy
- silane coupling agents may be used alone or in combination of two or more.
- an amino group-containing silane coupling agent and a glycidoxy group-containing silane coupling agent are preferable, and an amino group-containing silane coupling agent is more preferable.
- the amount of the silane coupling agent is preferably 1 to 30 parts by mass, more preferably 3 to 20 parts by mass, based on 100 parts by mass of the solid content of the chemical conversion film forming coating solution. More preferably, it is part by mass.
- silane coupling agent for example, Shin-Etsu Silicone KBM903 (3-aminopropyltrimethoxysilane), Toray Dow Corning Z-6011 (3-aminopropyltriethoxysilane).
- Z-6020 (3- (2-aminoethyl) aminopropyltrimethoxysilane) manufactured by Toray Dow Corning is preferably used.
- the adhesion amount of the chemical conversion coating is 0.05 to 3 g / m 2 , preferably 0.1 to 2.5 g / m 2 , more preferably 0.2 to 2 g / m 2 in terms of dry mass. .
- the adhesion amount of the chemical conversion coating is out of the above range, the adhesive strength with the resin molded product may be lowered.
- a chemical conversion coating film is formed by applying a coating solution for forming a chemical conversion coating containing an acid-modified polyolefin resin, colloidal silica, and a silane coupling agent to at least one surface of the metal substrate.
- a coating solution for forming a chemical conversion coating containing an acid-modified polyolefin resin, colloidal silica, and a silane coupling agent
- other known additives may be added to the coating solution.
- the method for forming the chemical conversion coating on the metal substrate is not particularly limited, and a conventionally known coating method can be employed.
- a coating liquid for chemical conversion coating can be applied by a roll coater method, a spray method, a curtain flow coater method, or the like. It can be used by applying to one or both surfaces of the surface of the metal substrate and drying by heating.
- the heating and drying temperature is not particularly limited, but since the coating liquid for forming the chemical conversion film is aqueous, it may be heated at around 100 ° C. where water evaporates for
- An adhesive layer made of an adhesive containing an acid-modified polyolefin-based resin is provided on the chemical conversion film to obtain a surface-treated steel sheet.
- the adhesive layer may be provided on the entire surface of the chemical conversion treatment film, or may be provided only on a part of the surface of the chemical conversion treatment film.
- the adhesive layer may be provided in some lines or dots. Also good.
- the adhesive layer those having excellent adhesiveness with a resin molded product to be described later combined with the surface-treated steel sheet are preferable.
- the adhesive contains an acid-modified polyolefin resin, preferably an acid-modified polypropylene resin, and more preferably an acid-modified polypropylene resin.
- the acid value of the acid-modified polyolefin resin in the adhesive layer is preferably 5 to 60 mgKOH / g, more preferably 10 to 50 mgKOH / g, and still more preferably 13 to 40 mgKOH / g. If the acid value of the acid-modified polyolefin resin is outside the above range, the adhesive strength may be lowered.
- the acid-modified polyolefin resin can be produced by the same method as the acid-modified polyolefin resin contained in the chemical conversion film.
- the acid-modified polyolefin resin contained in the adhesive layer may have the same or different acid value as the acid-modified polyolefin resin contained in the chemical conversion coating, but preferably has the same acid value. .
- the adhesive layer preferably contains no thermoplastic resin other than the acid-modified polyolefin resin, but other thermoplastic resins other than the acid-modified polyolefin resin may be used as long as the effects of the present invention are not impaired. May be included.
- thermoplastic resins include polystyrene resin, acrylonitrile-butadiene-styrene (ABS) copolymer, acrylonitrile-EPDM-styrene (AES) copolymer, acrylic resin, polybutadiene, polyacetal resin, polyether resin, Polyvinyl acetate, polyvinyl chloride, polyvinylidene chloride and the like can be mentioned, and these may be used alone or in combination of two or more.
- the content of the acid-modified polyolefin resin is preferably 80% by mass or more, more preferably 90% by mass or more, and 99.91% by mass or more. Is more preferably 99.95% by mass or more, and most preferably 100% by mass (the resin contained in the adhesive layer is only an acid-modified polyolefin resin).
- the thickness of the adhesive layer after drying is 5 to 100 ⁇ m, and preferably 10 to 90 ⁇ m. If the thickness of the adhesive layer is out of the above range, the adhesive strength may be lowered.
- a hot melt adhesive containing an acid-modified polyolefin-based resin is applied on the chemical conversion film to laminate an adhesive layer.
- the hot melt adhesive can be applied by a known method, and for example, can be applied to the surface of the chemical conversion treated steel sheet in a powder state. Moreover, you may apply
- the surface-treated steel sheet of this embodiment can be used in combination with a resin molded product (resin layer), that is, a composite member in which a resin layer is provided on an adhesive layer.
- a resin molded product that is, a composite member in which a resin layer is provided on an adhesive layer.
- an adhesive layer may be provided after press-forming the chemical conversion treated steel plate into a target shape, and a target shape of the surface treated steel plate provided with the adhesive layer on the chemical conversion treated steel plate You may press-mold. Then, the surface-treated steel sheet is inserted into a mold of an injection molding machine, clamped, and the molten resin is injected into the mold. When the resin is cooled and solidified, a composite member is obtained.
- the surface-treated steel sheet of the present embodiment may be combined with the resin layer by a press molding method, but it is preferable to adopt the injection molding method in order to take advantage of the short time and high efficiency of the injection molding.
- the injection molding conditions may be appropriately changed according to the type of resin constituting the molded product.
- the resin molded product is a polypropylene resin
- the cylinder temperature is 230 to 250 ° C. and the mold temperature is The temperature can be 45 to 55 ° C.
- the injection holding time can be 5 to 8 seconds
- the cooling time can be about 20 to 30 seconds.
- the resin layer includes a polyolefin resin.
- polyolefin resins include polyethylene, polypropylene, polybutene, polymethylpentene, copolymers of ⁇ -olefin and ethylene or propylene, ethylene-vinyl acetate copolymer, ethylene-acrylic acid copolymer, ethylene-methacrylic acid. Examples thereof include resins such as acid copolymers, ethylene-maleic anhydride copolymers, and propylene-maleic anhydride copolymers, which may be used alone or in combination of two or more.
- the polyolefin-based resin preferably includes a polypropylene resin, and more preferably includes only a polypropylene resin.
- the resin layer may contain about 5 to 60% by mass of reinforcing fibers such as glass fibers and carbon fibers.
- reinforcing fibers such as glass fibers and carbon fibers.
- the adhesive strength of the composite member is preferably 12 MPa or more, more preferably 12.5 MPa or more, further preferably 13 MPa or more, and particularly preferably 14 MPa or more.
- the adhesive strength of the composite member can be sufficiently increased even in the case of a surface-treated steel sheet having only two layers of a chemical conversion film and an adhesive layer on a metal substrate. A method for measuring the adhesive strength will be described later.
- the present invention is a polyolefin-based resin-bonded surface-treated metal plate in which an adhesive layer is laminated on at least one surface of a metal substrate via a chemical conversion coating, and the coating liquid for forming the chemical conversion coating is ,
- An acid-modified polyolefin resin, colloidal silica, and a silane coupling agent, and the amount of the chemical conversion film is 0.05 to 3 g / m 2 in dry mass
- the adhesive layer is an acid-modified polyolefin.
- a thickness of the adhesive layer is 5 to 100 ⁇ m.
- the acid value of the acid-modified polyolefin resin in the chemical conversion coating is preferably 3 to 100 mgKOH / g, and the acid-modified polyolefin resin in the chemical conversion coating is It is preferable to include an acid-modified polypropylene resin.
- the acid value of the acid-modified polyolefin resin in the adhesive layer is preferably 5 to 60 mgKOH / g, and the acid-modified polyolefin resin in the adhesive layer is It is preferable to include an acid-modified polypropylene resin.
- the metal substrate is preferably a steel plate.
- the present invention also includes a composite member in which a resin layer containing a polyolefin resin is provided on the adhesive layer in the surface-treated metal plate, and the polyolefin resin preferably contains a polypropylene resin. .
- the present invention also includes a method for producing the surface-treated metal plate for bonding a polyolefin-based resin, which includes a chemical conversion treatment containing an acid-modified polyolefin-based resin, colloidal silica, and a silane coupling agent.
- a step of laminating an adhesive layer is also includes a method for producing the surface-treated metal plate for bonding a polyolefin-based resin, which includes a chemical conversion treatment containing an acid-modified polyolefin-based resin, colloidal silica, and a silane coupling agent.
- the longitudinal end portion of the surface-treated steel plate and the longitudinal end portion of the resin layer are gripped with a chuck of a tensile tester in an atmosphere at 25 ° C., and the tensile strength is 10 mm / min.
- the tensile strength was measured when the resin layer was peeled off from the surface-treated steel sheet, and the value was taken as the adhesive strength.
- the longitudinal end of the surface-treated steel sheet is the end that is not covered with the resin layer
- the longitudinal end of the resin layer is the end of the surface-treated steel sheet that is not bonded. It is a part.
- Example 1 [Preparation of maleic anhydride grafted polypropylene resin]
- 400 ml of xylene and 60 g of granular homopolypropylene (melt flow rate: 4 g / 10 min) were placed, and the mixture was heated and stirred at 140 ° C. in a nitrogen stream.
- 40 ml of xylene in which 11 g of maleic anhydride and 4 g of t-butylperoxy 2-ethylhexyl carbonate were dissolved was dropped into the stirred solution over 1 hour, and then the reaction was performed for 1 hour.
- maleic anhydride grafted polypropylene resin The graft amount of maleic anhydride in the obtained maleic anhydride grafted polypropylene resin was 3.0% by mass, and the acid value of the obtained maleic anhydride grafted polypropylene resin was 25 mgKOH / g.
- a stainless steel pressure vessel was charged with 10 g of the maleic anhydride grafted polypropylene resin, 1 g of triethylamine, 10 g of butanol and 30 g of distilled water, and stirred at 170 ° C. for 1 hour at 100 rpm. Thereafter, the mixture was cooled to obtain a maleic anhydride-grafted polypropylene resin aqueous dispersion.
- Snowtex (registered trademark) 40 surface area average particle size: 10 to 20 nm) manufactured by Nissan Chemical Industries, Ltd. was used as colloidal silica
- KBM903 ⁇ -aminopropyltrimethoxysilane manufactured by Shin-Etsu Chemical Co., Ltd. was used as a silane coupling agent.
- [Chemical conversion steel sheet] A coating solution for forming a chemical conversion film is applied to the surface of a galvannealed steel sheet having a thickness of 1.0 mm so as to have a dry mass of 0.2 g / m 2, and heated at 100 ° C. for 1 minute. The chemical conversion treatment steel plate provided with the processing film was obtained.
- the surface of the surface-treated steel sheet is not adhered so as to be completely covered with the resin layer, and the resin layer and the surface-treated steel sheet overlap each other with a length of 12.5 mm ⁇ 25 mm (only part of the surface of the surface-treated steel sheet). Are covered with a resin layer) to obtain a composite member.
- the injection conditions are shown in Table 2. Further, the adhesive strength of the composite member was measured by the above-described measuring method, and the results are shown in Table 1.
- Example 2 and 3 Comparative Examples 1 and 2
- a composite member was obtained in the same manner as in Example 1 except that the adhesion amount of the chemical conversion coating was changed to the amount shown in Table 1.
- the adhesive strength of the composite member is shown in Table 1.
- Example 4 Comparative Examples 3 to 4
- Example 4 A composite member was obtained in the same manner as in Example 1 except that the thickness of the adhesive layer was as shown in Table 1.
- the adhesive strength of the composite member is shown in Table 1.
- Example 6 to 10 Comparative Examples 5 to 6
- a composite member was obtained in the same manner as in Example 1 except that the maleic anhydride grafted polypropylene resin of the chemical conversion coating was changed to the acid values shown in Table 1.
- the adhesive strength of the composite member is shown in Table 1.
- the acid value of the resin was adjusted by adjusting the charging ratio of homopolypropylene and maleic anhydride.
- Example 11 to 12 Comparative Examples 7 to 8
- a composite member was obtained in the same manner as in Example 1 except that the maleic anhydride grafted polypropylene resin of the adhesive layer was changed to the acid values shown in Table 1.
- the adhesive strength of the composite member is shown in Table 1.
- the acid value of the resin was adjusted by adjusting the charging ratio of homopolypropylene and maleic anhydride.
- the composite members provided with the surface-treated steel sheets of Examples 1 to 12 that satisfy the constituent requirements of the present invention were excellent in adhesive strength.
- Comparative Example 3 since the adhesive layer was too thin, the composite member provided with the surface-treated steel sheet of Comparative Example 3 was inferior in adhesive strength. In Comparative Example 4, since the adhesive layer was too thick, the composite member provided with the surface-treated steel sheet of Comparative Example 4 was inferior in adhesive strength.
- Comparative Example 5 since the acid value of the acid-modified polypropylene resin in the chemical conversion film was very small, it was not possible to produce a water-based chemical conversion film forming coating solution. In Comparative Example 6, an attempt was made to produce a resin having a very large acid value of the acid-modified polypropylene resin in the chemical conversion coating, but no acid-modified olefin resin could be produced.
- Comparative Example 7 since the acid value of the acid-modified polyolefin resin in the adhesive layer was too low, the composite member provided with the surface-treated steel sheet of Comparative Example 7 was inferior in adhesive strength. In Comparative Example 8, since the acid value of the acid-modified polyolefin resin in the adhesive layer was too high, the composite member provided with the surface-treated steel sheet of Comparative Example 8 was inferior in adhesive strength. This is presumably because the adhesive force between the resin layer and the adhesive layer was weak.
- the surface-treated steel sheets of Comparative Examples 9 to 10 have a chemical conversion film that does not contain an acid-modified polyolefin resin. Therefore, the composite members provided with the surface-treated steel sheets of Comparative Examples 9 to 10 were inferior in adhesive strength.
- the present invention has wide industrial applicability in the technical field related to the surface-treated metal sheet.
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Abstract
Description
本発明で用いられる金属基板としては、特に限定されないが、例えば、非めっき冷延鋼板、溶融亜鉛めっき鋼板、合金化溶融亜鉛めっき鋼板、電気亜鉛めっき鋼板等の鋼板の他、アルミニウム板およびチタン板等を挙げることができる。これらの中でも、溶融亜鉛めっき鋼板、電気亜鉛めっき鋼板、アルミニウム板、およびチタン板が好ましく、合金化溶融亜鉛めっき鋼板がより好ましい。金属基板の厚みは特に限定されないが、最終製品の軽量化のためには、0.3~3.2mm程度が好ましい。以下では、金属基板の好ましい例である鋼板を用いた実施形態について説明するが、本発明には各種の金属基板を用いることができる。
化成処理皮膜は、酸変性ポリオレフィン系樹脂、コロイダルシリカ、及びシランカップリング剤が含まれた化成処理皮膜形成用塗工液を用いて作製することができる。
本実施形態で用いられる化成処理皮膜形成用塗工液には、酸変性ポリオレフィン系樹脂が含まれており、すなわち、化成処理皮膜には、酸変性ポリオレフィン系樹脂が含まれる。酸変性ポリオレフィン系樹脂を含むことによって、化成処理皮膜と接着剤層との剥離を抑制することができる。酸変性ポリオレフィン系樹脂は酸変性ポリプロピレン樹脂を含むことが好ましい。
化成処理皮膜形成用塗工液にはコロイダルシリカが含まれていることが好ましい。すなわち、本実施形態の化成処理皮膜には、コロイダルシリカが含まれることが好ましい。コロイダルシリカを含むことによって、耐食性を高める効果を有するからである。コロイダルシリカとしては、「スノーテックス(登録商標)」シリーズ(日産化学工業社製のコロイダルシリカ)の「XS」、「SS」、「40」、「N」、「UP」等が好適に用いられる。特に、表面積平均粒子径が10~20nm程度の「スノーテックス(登録商標)40」が好適に用いられる。コロイダルシリカの量は、化成処理皮膜形成用塗工液の固形分100質量部中、30~60質量部であることが好ましく、35~55質量部であることがより好ましく、40~50質量部であることがさらに好ましい。また、化成処理皮膜に含まれるコロイダルシリカの量は、化成処理皮膜に含まれる熱可塑性樹脂100質量部に対して、50~150質量部であることが好ましく、75~125質量部であることがより好ましい。
化成処理皮膜形成用塗工液にはシランカップリング剤が含まれていることが好ましい。シランカップリング剤を含むことによって、金属基板に対する化成処理皮膜の密着性を向上させることができる。シランカップリング剤としては、具体的には、例えば、γ-アミノプロピルトリメトキシシラン、γ-アミノプロピルトリエトキシシラン、N-(β-アミノエチル)-γ-アミノプロピルトリメトキシシラン、N-(β-アミノエチル)-γ-アミノプロピルメチルジメトキシシランなどのアミノ基含有シランカップリング剤;γ-グリシドキシプロピルトリメトキシシラン、γ-グリシドキシプロピルメチルジメトキシシラン、γ-グリシドキシプロピルトリエトキシシラン、γ-グリシドキシメチルジメトキシシランなどのグリシドキシ基含有シランカップリング剤;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(β-メトキシエトキシ)シランなどのビニル基含有シランカップリング剤;γ-メタクリロキシプロピルトリメトキシシランなどのメタクリロキシ基含有シランカップリング剤;γ-メルカプトプロピルトリメトキシシラン、γ-メルカプトプロピルメチルジメトキシシランなどのメルカプト基含有シランカップリング剤;γ-クロロプロピルメトキシシラン、γ-クロロプロピルトリメトキシシランなどのハロゲン基含有シランカップリング剤などが挙げられ、中でもアミノ基含有シランカップリング剤であることが好ましい。これらのシランカップリング剤は、単独で用いてもよいし、2種以上を併用してもよい。これらの中では、接着性が良好になる観点から、アミノ基含有シランカップリング剤やグリシドキシ基含有シランカップリング剤が好ましく、アミノ基含有シランカップリング剤がより好ましい。シランカップリング剤の量は、化成処理皮膜形成用塗工液の固形分100質量部中、1~30質量部であることが好ましく、3~20質量部であることがより好ましく、5~15質量部であることがさらに好ましい。
化成処理皮膜の付着量は、乾燥質量で0.05~3g/m2であり、好ましくは0.1~2.5g/m2であり、より好ましくは0.2~2g/m2である。化成処理皮膜の付着量が上記範囲外であると、樹脂成形品との接着強度が低くなるおそれがある。
酸変性ポリオレフィン系樹脂、コロイダルシリカ、及びシランカップリング剤を含有する化成処理皮膜形成用塗工液を金属基板の少なくとも一方の面に塗布して化成処理皮膜を形成している。化成処理皮膜形成時には、塗工液中にその他の公知の添加剤を加えてもよい。金属基板上に化成処理皮膜を形成する方法は特に限定されず、従来公知の塗布方法が採用でき、例えば、化成処理皮膜用塗工液を、ロールコーター法、スプレー法、カーテンフローコーター法等を用いて、金属基板表面の片面もしくは両面に塗布して、加熱乾燥すればよい。加熱乾燥温度は特に限定されないが、化成処理皮膜形成用の塗工液は水性であるため、水が蒸発する100℃前後で数十秒~数分程度加熱するとよい。
上記化成処理皮膜の上に酸変性ポリオレフィン系樹脂を含む接着剤からなる接着剤層を設けて、表面処理鋼板とする。接着剤層は、化成処理皮膜表面の全面に設けてもよいし、化成処理皮膜表面の一部の必要な場所だけに設けてもよく、例えば何本かのライン状や、ドット状に設けてもよい。接着剤層としては、表面処理鋼板と複合する後述の樹脂成形品との接着性に優れたものが好ましい。
接着剤は、酸変性ポリオレフィン系樹脂を含んでおり、酸変性ポリプロピレン樹脂を含むことが好ましく、酸変性ポリプロピレン樹脂からなることがより好ましい。
本実施形態では、化成処理皮膜上に、酸変性ポリオレフィン系樹脂を含有するホットメルト接着剤を塗布して接着剤層を積層している。ホットメルト接着剤は公知の方法で塗工でき、例えば、粉末の状態で化成処理鋼板の表面に塗布することができる。また、接着剤を有機溶剤に溶解させた溶液や、水に分散させた水分散液を、化成処理鋼板に塗布してもよい。接着剤塗布後は、接着剤の種類に適した温度(例えば、180~230℃程度)で、1~3分程度加熱する。
本実施形態の表面処理鋼板は、樹脂成形品(樹脂層)と複合して用いる、すなわち接着剤層の上に、樹脂層が設けられた複合部材とすることができる。このとき、加工が必要な場合は、化成処理鋼板を目的とする形状にプレス成形した後に接着剤層を設けてもよく、化成処理鋼板に接着剤層を設けた表面処理鋼板を目的とする形状にプレス成形してもよい。そして、表面処理鋼板を、射出成形機の金型の中に装入し、型締めして、溶融樹脂を型内に射出し、樹脂が冷却固化すれば、複合部材が得られる。もちろん、本実施形態の表面処理鋼板は、プレス成形法で樹脂層と複合してもよいが、射出成形の短時間・高効率というメリットを生かすには、射出成形法を採用することが好ましい。
樹脂層はポリオレフィン系樹脂を含む。ポリオレフィン系樹脂としては、例えば、ポリエチレン、ポリプロピレン、ポリブテン、ポリメチルペンテン、α-オレフィンとエチレンもしくはプロピレンとの共重合体、エチレン-酢酸ビニル共重合体、エチレン-アクリル酸共重合体、エチレン-メタクリル酸共重合体、エチレン-無水マレイン酸共重合体、プロピレン-無水マレイン酸共重合体などの樹脂が挙げられ、単独で用いても、2種以上を組み合わせて用いてもよい。ポリオレフィン系樹脂は、ポリプロピレン樹脂を含むことが好ましく、ポリプロピレン樹脂のみからなることがより好ましい。
(接着性)
複合部材の接着強度は12MPa以上であることが好ましく、12.5MPa以上であることがより好ましく、13MPa以上であることがさらに好ましく、14MPa以上であることが特に好ましい。本実施形態の表面処理鋼板を用いることによって、化成処理皮膜及び接着剤層の2層のみを金属基板に備えた表面処理鋼板であっても複合部材の接着強度を十分に高めることができる。接着強度の測定方法については後述する。
後述の製造方法で得られる複合部材において、表面処理鋼板の長手方向端部と樹脂層の長手方向端部とを、25℃の雰囲気下で、引張試験機のチャックで掴み、10mm/分の引張速度で引張り、樹脂層が表面処理鋼板から剥離した時の引張強度を測定し、その値を接着強度とした。ただし、表面処理鋼板の長手方向端部とは、樹脂層で覆われていない方の端部のことであり、樹脂層の長手方向端部とは、表面処理鋼板が接着されていない方の端部のことである。
[無水マレイン酸グラフトポリプロピレン樹脂の調製]
冷却管を備えたフラスコに溶媒としてキシレン400mlと、粒状のホモポリプロピレン(メルトフローレート:4g/10min)60gとを入れ、窒素気流下、140℃に加熱攪拌した。その後、攪拌した溶液に無水マレイン酸11gとt-ブチルパーオキシ2-エチルヘキシルカーボネート4gとを溶かしたキシレン40mlを1時間かけて滴下し、その後1時間反応を行った。続いて、内容物を室温まで下げ、大量のメチルエチルケトンに投入した。最後にろ過を行い、無水マレイン酸グラフトポリプロピレン樹脂を得た。得られた無水マレイン酸グラフトポリプロピレン樹脂における無水マレイン酸のグラフト量は3.0質量%であり、得られた無水マレイン酸グラフトポリプロピレン樹脂の酸価は25mgKOH/gであった。
ステンレス製耐圧容器に、上記無水マレイン酸グラフトポリプロピレン樹脂10g、トリエチルアミン1g、ブタノール10g、蒸留水30gを仕込み、170℃で1時間100rpmで攪拌した。その後、冷却して、無水マレイン酸グラフトポリプロピレン樹脂水分散体を得た。次に100mlオートクレーブに、上記の製法で作製した無水マレイン酸グラフトポリプロピレン樹脂水分散体、コロイダルシリカ、及びシランカップリング剤を質量比(固形分)で無水マレイン酸グラフトポリプロピレン樹脂:コロイダルシリカ:シランカップリング剤=50:50:10となるように添加し、温度140℃、攪拌速度500rpmで2時間攪拌し、化成処理皮膜形成用塗工液を得た。コロイダルシリカとして日産化学工業社製スノーテックス(登録商標)40(表面積平均粒径10~20nm)を、シランカップリング剤として信越化学工業社製KBM903(γ-アミノプロピルトリメトキシシラン)を用いた。
厚さ1.0mmの合金化溶融亜鉛めっき鋼板の表面に、化成処理皮膜形成用塗工液を乾燥質量で0.2g/m2となるように塗布し、100℃で1分間加熱し、化成処理皮膜を備えた化成処理鋼板を得た。
上記化成処理鋼板の化成処理皮膜上に、25mgKOH/gである上記無水マレイン酸グラフトポリプロピレン樹脂をバーコーターで厚さ20μmとなるように塗布した後、220℃で2分間加熱し、化成処理皮膜及び接着剤層を備えた表面処理鋼板を得た。
次に、射出成形機(日精樹脂工業社製PNX60)を用いて射出成形を行った。まず、上記表面処理鋼板を100mm×25mmにカットし、金型に入れた。その後、ガラス繊維が20質量%含まれたポリプロピレン樹脂であるプライムポリマー社製プライムポリプロ(登録商標)V7000を溶融させて、100mm長さ×25mm幅×3mm厚である樹脂層を備えた複合部材を得た。ただし、表面処理鋼板の表面を樹脂層で完全に覆うように接着させてはおらず、樹脂層と表面処理鋼板とは12.5mm長さ×25mm幅で重なる(表面処理鋼板の表面の一部だけを樹脂層で覆う)ように接着させて複合部材を得た。射出条件は、表2に示した。また、複合部材の接着強度を上述の測定方法で測定し、その結果を表1に示した。
化成処理皮膜の付着量を表1に記載の量とした以外は、実施例1と同様にして複合部材を得た。複合部材の接着強度を表1に示した。
接着剤層を表1に記載の厚さとした以外は、実施例1と同様にして複合部材を得た。複合部材の接着強度を表1に示した。
化成処理皮膜の無水マレイン酸グラフトポリプロピレン樹脂を表1に記載の酸価とした以外は、実施例1と同様にして複合部材を得た。複合部材の接着強度を表1に示した。なお、上述した無水マレイン酸グラフトポリプロピレン樹脂の調製において、ホモポリプロピレン及び無水マレイン酸の仕込み比率を調整することによって樹脂の酸価を調整した。
接着剤層の無水マレイン酸グラフトポリプロピレン樹脂を表1に記載の酸価とした以外は、実施例1と同様にして複合部材を得た。複合部材の接着強度を表1に示した。なお、上述した無水マレイン酸グラフトポリプロピレン樹脂の調製において、ホモポリプロピレン及び無水マレイン酸の仕込み比率を調整することによって樹脂の酸価を調整した。
化成処理皮膜の樹脂を無水マレイン酸グラフトポリプロピレン樹脂に代えて表1に記載の樹脂を用いた以外は、実施例1と同様にして複合部材を得た。複合部材の接着強度を表1に示した。
Claims (9)
- 金属基板の少なくとも一方の面に、化成処理皮膜を介して接着剤層が積層されたポリオレフィン系樹脂接着用表面処理金属板であって、
上記化成処理皮膜は、酸変性ポリオレフィン系樹脂、コロイダルシリカ、及びシランカップリング剤を含有する塗工液を前記金属基板に塗布して得られた皮膜であり、上記化成処理皮膜の付着量は、乾燥質量で0.05~3g/m2であり、
上記接着剤層は酸変性ポリオレフィン系樹脂を含有し、上記接着剤層の厚さは5~100μmである
ことを特徴とするポリオレフィン系樹脂接着用表面処理金属板。 - 上記化成処理皮膜における酸変性ポリオレフィン系樹脂の酸価は3~100mgKOH/gである請求項1に記載のポリオレフィン系樹脂接着用表面処理金属板。
- 上記化成処理皮膜における酸変性ポリオレフィン系樹脂は酸変性ポリプロピレン樹脂を含む請求項1に記載のポリオレフィン系樹脂接着用表面処理金属板。
- 上記接着剤層における酸変性ポリオレフィン系樹脂の酸価は5~60mgKOH/gである請求項1に記載のポリオレフィン系樹脂接着用表面処理金属板。
- 上記接着剤層における酸変性ポリオレフィン系樹脂は酸変性ポリプロピレン樹脂を含む請求項1に記載のポリオレフィン系樹脂接着用表面処理金属板。
- 上記金属基板は鋼板である、請求項1に記載のポリオレフィン系樹脂接着用表面処理金属板。
- 請求項1~5のいずれか1項に記載の表面処理金属板における接着剤層の上に、ポリオレフィン系樹脂を含む樹脂層が設けられていることを特徴とする複合部材。
- 上記ポリオレフィン系樹脂はポリプロピレン樹脂を含む請求項7に記載の複合部材。
- 請求項1~5のいずれか1項に記載のポリオレフィン系樹脂接着用表面処理金属板の製造方法であって、
酸変性ポリオレフィン系樹脂、コロイダルシリカ、及びシランカップリング剤を含有する化成処理皮膜形成用塗工液を金属基板の少なくとも一方の面に塗布して化成処理皮膜を形成する工程と、
上記化成処理皮膜上に、酸変性ポリオレフィン系樹脂を含有するホットメルト接着剤を塗布して接着剤層を積層する工程とを有する
ことを特徴とするポリオレフィン系樹脂接着用表面処理金属板の製造方法。
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US11642871B2 (en) | 2017-03-29 | 2023-05-09 | Kobe Steel, Ltd. | Surface-treated metal plate for polyolefin bonding, composite member, and method for manufacturing composite member |
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CN116802045A (zh) * | 2021-01-07 | 2023-09-22 | 日本制铁株式会社 | 复合构件和设备 |
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CN108778716A (zh) | 2018-11-09 |
EP3434470A1 (en) | 2019-01-30 |
KR20180124964A (ko) | 2018-11-21 |
JP2017170828A (ja) | 2017-09-28 |
US20200316912A1 (en) | 2020-10-08 |
JP6621694B2 (ja) | 2019-12-18 |
EP3434470A4 (en) | 2019-11-20 |
KR102142843B1 (ko) | 2020-08-10 |
TWI630104B (zh) | 2018-07-21 |
US11897230B2 (en) | 2024-02-13 |
TW201805165A (zh) | 2018-02-16 |
CN108778716B (zh) | 2021-05-11 |
EP3434470B1 (en) | 2023-12-20 |
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