JP6466977B2 - 複層塗膜形成方法 - Google Patents
複層塗膜形成方法 Download PDFInfo
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- JP6466977B2 JP6466977B2 JP2017026041A JP2017026041A JP6466977B2 JP 6466977 B2 JP6466977 B2 JP 6466977B2 JP 2017026041 A JP2017026041 A JP 2017026041A JP 2017026041 A JP2017026041 A JP 2017026041A JP 6466977 B2 JP6466977 B2 JP 6466977B2
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- QVTWBMUAJHVAIJ-UHFFFAOYSA-N hexane-1,4-diol Chemical compound CCC(O)CCCO QVTWBMUAJHVAIJ-UHFFFAOYSA-N 0.000 description 1
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- 125000002768 hydroxyalkyl group Chemical group 0.000 description 1
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- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000001034 iron oxide pigment Substances 0.000 description 1
- DCYOBGZUOMKFPA-UHFFFAOYSA-N iron(2+);iron(3+);octadecacyanide Chemical compound [Fe+2].[Fe+2].[Fe+2].[Fe+3].[Fe+3].[Fe+3].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] DCYOBGZUOMKFPA-UHFFFAOYSA-N 0.000 description 1
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- GWYFCOCPABKNJV-UHFFFAOYSA-M isovalerate Chemical compound CC(C)CC([O-])=O GWYFCOCPABKNJV-UHFFFAOYSA-M 0.000 description 1
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
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- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
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- 150000002739 metals Chemical class 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
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- AYLRODJJLADBOB-QMMMGPOBSA-N methyl (2s)-2,6-diisocyanatohexanoate Chemical compound COC(=O)[C@@H](N=C=O)CCCCN=C=O AYLRODJJLADBOB-QMMMGPOBSA-N 0.000 description 1
- AYLRODJJLADBOB-UHFFFAOYSA-N methyl 2,6-diisocyanatohexanoate Chemical compound COC(=O)C(N=C=O)CCCCN=C=O AYLRODJJLADBOB-UHFFFAOYSA-N 0.000 description 1
- JFZUABNDWZQLIJ-UHFFFAOYSA-N methyl 2-[(2-chloroacetyl)amino]benzoate Chemical compound COC(=O)C1=CC=CC=C1NC(=O)CCl JFZUABNDWZQLIJ-UHFFFAOYSA-N 0.000 description 1
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- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 description 1
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- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
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- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
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- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
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- OTLDLKLSNZMTTA-UHFFFAOYSA-N octahydro-1h-4,7-methanoindene-1,5-diyldimethanol Chemical compound C1C2C3C(CO)CCC3C1C(CO)C2 OTLDLKLSNZMTTA-UHFFFAOYSA-N 0.000 description 1
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
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- 238000005580 one pot reaction Methods 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- HXSACZWWBYWLIS-UHFFFAOYSA-N oxadiazine-4,5,6-trione Chemical compound O=C1ON=NC(=O)C1=O HXSACZWWBYWLIS-UHFFFAOYSA-N 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- QQWAKSKPSOFJFF-UHFFFAOYSA-N oxiran-2-ylmethyl 2,2-dimethyloctanoate Chemical compound CCCCCCC(C)(C)C(=O)OCC1CO1 QQWAKSKPSOFJFF-UHFFFAOYSA-N 0.000 description 1
- FIWHJQPAGLNURC-UHFFFAOYSA-N oxiran-2-ylmethyl 7,7-dimethyloctanoate Chemical compound CC(C)(C)CCCCCC(=O)OCC1CO1 FIWHJQPAGLNURC-UHFFFAOYSA-N 0.000 description 1
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
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- 230000036961 partial effect Effects 0.000 description 1
- WCVRQHFDJLLWFE-UHFFFAOYSA-N pentane-1,2-diol Chemical compound CCCC(O)CO WCVRQHFDJLLWFE-UHFFFAOYSA-N 0.000 description 1
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- GLOBUAZSRIOKLN-UHFFFAOYSA-N pentane-1,4-diol Chemical compound CC(O)CCCO GLOBUAZSRIOKLN-UHFFFAOYSA-N 0.000 description 1
- IDZAUPYMMSSVHP-UHFFFAOYSA-N pentyl 3-oxobutanoate Chemical compound CCCCCOC(=O)CC(C)=O IDZAUPYMMSSVHP-UHFFFAOYSA-N 0.000 description 1
- 125000005010 perfluoroalkyl group Chemical group 0.000 description 1
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- 125000000286 phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
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- 230000002265 prevention Effects 0.000 description 1
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- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
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- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical group CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- 229960003351 prussian blue Drugs 0.000 description 1
- 239000013225 prussian blue Substances 0.000 description 1
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- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 239000003813 safflower oil Substances 0.000 description 1
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- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- PYBOTXJDCXMILP-ICYLSCGJSA-M sodium;(z,12r)-12-hydroxy-2-sulfooctadec-9-enoate Chemical compound [Na+].CCCCCC[C@@H](O)C\C=C/CCCCCCC(C([O-])=O)S(O)(=O)=O PYBOTXJDCXMILP-ICYLSCGJSA-M 0.000 description 1
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 235000015096 spirit Nutrition 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 229940012831 stearyl alcohol Drugs 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- JKUYRAMKJLMYLO-UHFFFAOYSA-N tert-butyl 3-oxobutanoate Chemical compound CC(=O)CC(=O)OC(C)(C)C JKUYRAMKJLMYLO-UHFFFAOYSA-N 0.000 description 1
- BTHNEHUFXUBOQG-UHFFFAOYSA-N tert-butyl 4-methyl-3-oxopentanoate Chemical compound CC(C)C(=O)CC(=O)OC(C)(C)C BTHNEHUFXUBOQG-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 description 1
- UFDHBDMSHIXOKF-UHFFFAOYSA-N tetrahydrophthalic acid Natural products OC(=O)C1=C(C(O)=O)CCCC1 UFDHBDMSHIXOKF-UHFFFAOYSA-N 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229940117013 triethanolamine oleate Drugs 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- FOETTWZZVDEKIW-UHFFFAOYSA-N triisocyanatomethylbenzene Chemical compound O=C=NC(N=C=O)(N=C=O)C1=CC=CC=C1 FOETTWZZVDEKIW-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- AVWRKZWQTYIKIY-UHFFFAOYSA-N urea-1-carboxylic acid Chemical compound NC(=O)NC(O)=O AVWRKZWQTYIKIY-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- FUSUHKVFWTUUBE-UHFFFAOYSA-N vinyl methyl ketone Natural products CC(=O)C=C FUSUHKVFWTUUBE-UHFFFAOYSA-N 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 235000014692 zinc oxide Nutrition 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- IFNXAMCERSVZCV-UHFFFAOYSA-L zinc;2-ethylhexanoate Chemical compound [Zn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O IFNXAMCERSVZCV-UHFFFAOYSA-L 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 150000007934 α,β-unsaturated carboxylic acids Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
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Description
工程(1):電着塗膜上に、水性中塗り塗料(X)を塗装して中塗り塗膜を形成する工程
工程(2):予備加熱後、中塗り塗膜上に、水性ベース塗料(Y)を塗装してベース塗膜を形成する工程
工程(3):予備加熱後、ベース塗膜上に、塗料中の樹脂成分固形分100質量部を基準として、カルボキシル基含有化合物40〜60質量部及びポリエポキシド60〜40質量部を含有するクリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程
工程(4):前記工程(1)〜(3)で形成された中塗り塗膜、ベース塗膜及びクリヤー塗膜を加熱硬化する工程
前記水性中塗り塗料(X)が、ガラス転移温度(Tg)が5〜15℃の範囲内であり、かつ重量平均分子量が30,000〜40,000の範囲内である水酸基含有アクリル樹脂(A)、ガラス転移温度(Tg)が−50℃以下であり、ポリエーテル骨格を有するポリウレタン樹脂(B)、水酸基含有ポリエステル樹脂(C)、メラミン樹脂(D)及び活性メチレンブロックポリイソシアネート化合物(E)を含有し、該水酸基含有アクリル樹脂(A)と該ポリウレタン樹脂(B)との使用比が固形分比で、20/10〜30/10の範囲内であり、該水性中塗り塗料(X)による加熱硬化後の形成塗膜の20℃における破断伸び率が20〜30%の範囲内であり、ヤング率が5,000〜6,000MPaの範囲内であり、ツーコン硬度が4〜6の範囲内の範囲内であることを特徴とする複層塗膜形成方法、に係るものである。
工程(1):電着塗膜上に、水性中塗り塗料(X)を塗装して中塗り塗膜を形成する工程
工程(2):前記工程(1)で形成された中塗り塗膜を予備加熱後、その上に、水性ベース塗料(Y)を塗装してベース塗膜を形成する工程
工程(3):前記工程(2)で形成されたベース塗膜を予備加熱後、その上に、塗料中の樹脂成分固形分100質量部を基準として、カルボキシル基含有化合物40〜60質量部及びポリエポキシド60〜40質量部を含有するクリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程
工程(4):前記工程(1)〜(3)で形成された中塗り塗膜、ベース塗膜及びクリヤー塗膜を加熱硬化する工程
本発明の方法によれば、まず、工程(1)として、電着塗装された合金化溶融亜鉛めっき鋼板の電着塗膜上に、水性中塗り塗料(X)が塗装され、中塗り塗膜が形成される。一般に、中塗り塗料は、下塗り塗膜と上塗り塗膜の間に中塗り塗膜層を形成させ、複層塗膜層間の付着性向上に寄与し、被塗物表面の粗度隠蔽による仕上がり外観、及び耐チッピング性向上等の目的で塗装される塗料である。
本発明の方法において、水性中塗り塗料(X)は、水酸基含有アクリル樹脂(A)、ポリウレタン樹脂(B)、水酸基含有ポリエステル樹脂(C)、メラミン樹脂(D)及び活性メチレンブロックポリイソシアネート化合物(E)を含有し、その他必要に応じて顔料(F)、有機溶剤(G)を含有する塗料組成物である。
水酸基含有アクリル樹脂(A)は、例えば、水酸基含有不飽和モノマー及び場合によりさらに該モノマーと共重合可能な他の不飽和モノマーを包含する少なくとも1種の不飽和モノマー成分を通常の条件で(共)重合せしめることによって製造することができる。
アミノエチル(メタ)アクリレート、グリシジル(メタ)アクリレートとアミン類との付加物などの含窒素不飽和モノマー;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などのエポキシ基含有不飽和モノマー;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;2−アクリルアミド−2−メチルプロパンスルホン酸、アリルスルホン酸、スチレンスルホン酸ナトリウム塩、スルホエチルメタクリレート及びそのナトリウム塩やアンモニウム塩などのスルホン酸基を有する不飽和モノマー;2−アクリロイルオキシエチルアシッドホスフェート、2−メタクリロイルオキシエチルアシッドホスフェート、2−アクリロイルオキシプロピルアシッドホスフェート、2−メタクリロイルオキシプロピルアシッドホスフェートなどのリン酸基を有する不飽和モノマー;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’−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などの紫外線吸収性基を有する不飽和モノマー;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などの紫外線安定化性能を有する不飽和モノマー;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)などのカルボニル基を有する不飽和モノマー化合物などが挙げられ、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。
1/Tg(K)=W1/T1+W2/T2+・・・Wn/Tn
Tg(℃)=Tg(K)−273
式中、W1、W2、・・・Wnは各モノマーの質量分率であり、T1、T2・・・Tnは各モノマーのホモポリマーのガラス転移温度Tg(K)である。
なお、各モノマーのホモポリマーのガラス転移温度は、POLYMER HANDBOOK Fourth Edition,J.Brandrup,E.h.Immergut,E.A.Grulke編(1999年)による値であり、該文献に記載されていないモノマーのガラス転移温度は、該モノマーのホモポリマーを重量平均分子量が50,000程度になるようにして合成し、そのガラス転移温度を示差走査型熱分析により測定したときの値を使用する。
ポリウレタン樹脂(B)は、ガラス転移温度(Tg)が−50℃以下であり、ポリエーテル骨格を有する。ポリウレタン樹脂(B)としては、下記のウレタン樹脂エマルション(B1)が好ましい。
水酸基含有ポリエステル樹脂(C)は、既知の方法で、常法に従い、多塩基酸と多価アルコ−ルとをエステル化反応させることによって合成することができる。水酸基含有ポリエステル樹脂(C)は、カルボキシル基等の酸基を有しているものが好ましい。
本発明において、水性中塗り塗料(X)の架橋剤成分として、メラミン樹脂(D)を含有する。
活性メチレンブロックポリイソシアネート化合物(E)としては、ポリイソシアネート化合物中のイソシアネート基に、活性メチレン化合物を反応させて得られるブロックポリイソシアネート化合物を挙げることができる。本発明では特に、親水基を有する活性メチレンブロックポリイソシアネート化合物(E1)が好ましい。このような化合物(E1)としては、ポリイソシアネート化合物(e1)中の一部のイソシアネート基に親水基を有する活性水素含有化合物を反応させて親水基を導入し、さらにポリイソシアネート化合物(e1)中のイソシアネート基に、活性メチレン化合物(e2)を反応させて得られるブロックポリイソシアネート化合物(e3)が好適に使用でき、さらにかかるブロックポリイソシアネート化合物(e3)に炭素数6以上の2級アルコール(e4)を反応させることによって得られるものが好適に使用できる。
水酸基含有アクリル樹脂(A):通常5〜30質量部、好ましくは10〜30質量部、より好ましくは20〜30質量部、
ポリウレタン樹脂(B):通常5〜20質量部、好ましくは5〜15質量部、より好ましくは8〜12質量部、
水酸基含有ポリエステル樹脂(C):通常10〜40質量部、好ましくは15〜35質量部、より好ましくは20〜30質量部、
メラミン樹脂(D):通常10〜40質量部、好ましくは15〜35質量部、より好ましくは20〜30質量部、
活性メチレンブロックポリイソシアネート化合物(E):通常5〜25質量部、好ましくは5〜15質量部、より好ましくは8〜12質量部。
顔料(F)としては、通常、塗料に用いられる顔料を使用することができる。具体的には、例えば、二酸化チタン、亜鉛華、カーボンブラック、フタロシアニンブルー、プルシアンブルー、コバルトブルー、アゾ顔料、フタロシアニン顔料、キナクリドン顔料、イソインドリン顔料、スレン系顔料、ペリレン顔料等の着色顔料;クレー、カオリン、バリタ、硫酸バリウム、炭酸バリウム、炭酸カルシウム、シリカ、アルミナホワイト、タルク等の体質顔料;アルミニウムフレーク、雲母フレーク等の光輝性顔料等を好適に使用することができる。
有機溶剤(G)としては、例えばヘキサン、ヘプタン、キシレン、トルエン等の炭化水素系;酢酸エチル、酢酸ブチル等のエステル類;エチレングリコールモノメチルエーテル等のエーテル系;エタノール、プロパノール、2−エチルヘキシルアルコール等のアルコール系;メチルエチルケトン、メチルイソブチルケトン等のケトン系;スワゾール310、スワゾール1000(コスモ石油株式会社製)等の芳香族炭化水素系;脂肪族炭化水素系、脂環族炭化水素系、アミド系等の溶剤を挙げることができる。これらの有機溶剤は単独でもしくは2種以上を併用して使用することができる。
本発明の方法によれば、次に、工程(1)で形成された中塗り塗膜を、予備加熱後、該中塗り塗膜上に、水性ベース塗料(Y)が塗装され、ベース塗膜が形成される。水性ベース塗料(Y)は、本発明により形成される複層塗膜の意匠性の付与、中塗り塗膜との積層による意匠性及び深み感を向上させる塗料である。
本発明の方法によれば、上記の如くして水性ベース塗料(Y)を塗装して得られたベース塗膜を、塗膜が実質的に硬化しない加熱条件で予備加熱し、該ベース塗膜上に、クリヤー塗料(Z)を塗装して、クリヤー塗膜を形成する。
クリヤー塗料(Z)としては、例えば、塗料中の樹脂成分固形分100質量部を基準として、カルボキシル基含有化合物を通常40〜60質量部、好ましくは45〜55質量部の範囲内、及びポリエポキシドを通常60〜40質量部の範囲内、好ましくは55〜45質量部の範囲内で含有するクリヤー塗料を使用することができる。
ここで、酸無水基をハーフエステル化してなる基とは、酸無水基に脂肪族モノアルコールを付加せしめて開環させる(即ち、ハーフエステル化する)ことにより得られるカルボキシル基とカルボン酸エステル基とからなる基を意味する。以下、この基を単にハーフエステル基ということがある。
重合体(2)は、カルボキシル基含有不飽和モノマー及びその他の重合性不飽和モノマーを、重合体(1)の場合と同様の方法により共重合させることによって容易に得ることができる。
カルボキシル基含有ポリエステル系重合体は、例えば、エチレングリコール、ブチレングリコール、1,6−ヘキサンジオール、トリメチロールプロパン、ペンタエリスリトールなどの多価アルコールと、例えば、アジピン酸、テレフタル酸、イソフタル酸、無水フタル酸、ヘキサヒドロ無水フタル酸などの多価カルボン酸との縮合反応によって容易に得ることができる。例えば、多価カルボン酸のカルボキシル基過剰配合の条件下で1段階の反応により、カルボキシル基含有ポリエステル系重合体を得ることができ、また、逆に多価アルコールの水酸基過剰配合の条件下でまず水酸基末端のポリエステル系重合体を合成した後、無水フタル酸、ヘキサヒドロ無水フタル酸、無水コハク酸などの酸無水基含有化合物を後付加させることによっても、カルボキシル基含有ポリエステル系重合体を得ることができる。
ハーフエステルは、ポリオールと1,2−酸無水物とを、酸無水物の開環反応が起こり且つ実質上ポリエステル化反応が起こらないような条件下で反応させることにより得ることができ、その反応生成物は一般に低分子量でありかつ狭い分子量分布を有している。また、該反応生成物は塗料組成物中において低い揮発性有機物含有量を示し、しかも、形成される塗膜に優れた耐酸性などを付与する。
本発明の複層塗膜形成方法においては、上記工程(1)〜(3)で形成される中塗り塗膜、ベース塗膜及びクリヤー塗膜が加熱硬化される。クリヤー塗料(Z)を塗装してなるクリヤー塗膜は、通常、未硬化のベース塗膜と一度に加熱硬化される。
本発明の方法によれば、自動車車体本体とガラス部材等の接着のため、クリヤー塗膜上に、一般に、固定されるガラス部材の形状に相応する枠状に、接着剤層が形成される。
製造例a1
フラスコ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、2−ヒドロキシエチルメタクリレート10部、スチレン20部、イソブチルメタクリレート22部、n−ブチルメタクリレート42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)2.0部の混合物を4時間かけてフラスコに滴下し、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時間かけてフラスコに滴下し、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、プロピレングリコールモノプロピルエーテル13部を加え、固形分濃度55%の水酸基含有アクリル樹脂(A1)を得た。得られた水酸基含有アクリル樹脂(A1)のガラス転移温度は5℃、重量平均分子量は35,000、水酸基価は43mgKOH/g、酸価は47mgKOH/gであった。
製造例1において、モノマー混合物の配合組成及び反応温度を表1に示すものとする以外は、製造例1と同様にして、固形分濃度55%の水酸基含有アクリル樹脂(A2)〜(A6)溶液を得た。各水酸基含有アクリル樹脂のガラス転移温度、重量平均分子量、水酸基価及び酸価を表1にあわせて示す。
製造例x1
製造例a1で得た水酸基含有アクリル樹脂(A1)36部(樹脂固形分20部)、「JR−806」(テイカ社製、商品名、ルチル型二酸化チタン)90部、「カーボンMA−100」(三菱化学社製、商品名、カーボンブラック)0.1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に調整した後、ペイントシェーカーで30分間分散して顔料分散ペーストを得た。次に、得られた顔料分散ペースト131部、下記ポリウレタン樹脂(B1)10部、水酸基含有ポリエステル樹脂(C1)30部、メラミン樹脂(D1)30部及び活性メチレンブロックポリイソシアネート化合物(E1)10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、20℃におけるフォードカップNo.4による粘度が45秒の水性中塗り塗料(X1)を得た。
製造例x1において、各原材料を下記表2に示す組成の各原材料に変更する以外は、製造例x1と同様にして、20℃におけるフォードカップNo.4による粘度が45秒の水性中塗り塗料(X2)〜(X16)を得た。なお、各成分の配合量は固形分量(部)である。
ポリウレタン樹脂(B2):「スーパーフレックス E−2000」(商品名、第一工業製薬社製、ポリエステル骨格を有するポリウレタン樹脂、ガラス転移温度=−38℃)
温度計、サーモスタット、撹拌装置、還流冷却器、窒素導入管、滴下装置及び除去溶媒簡易トラップを備えた反応容器に、「スミジュールN−3300」」(商品名、住化バイエルウレタン社製、ヘキサメチレンジイソシアネート由来のイソシアヌレート構造含有ポリイソシアネート、固形分約100%、イソシアネート基含有率21.8%)360部、「ユニオックスM−550」(日油社製、ポリエチレングリコールモノメチルエーテル、平均分子量 約550)60部及び2,6−ジ−tert−ブチル−4−メチルフェノール0.2部を仕込み、よく混合して、窒素気流下で130℃で3時間加熱した。次いで、酢酸エチル110部及びマロン酸ジイソプロピル252部を仕込み、窒素気流下で攪拌しながら、ナトリウムメトキシドの28%メタノール溶液3部を加え、65℃で8時間攪拌した。得られた樹脂溶液中のイソシアネート量は0.12モル/kgであった。これに4−メチル−2−ペンタノール683部を加え、系の温度を80〜85℃に保ちながら減圧条件下で3時間かけて溶剤を留去し、活性メチレンブロックポリイソシアネート化合物(E1)1010部を得た。除去溶媒簡易トラップには、イソプロパノールが95部含まれていた。得られた活性メチレンブロックポリイソシアネート化合物(E1)の固形分濃度は約60%であった。
(光輝性顔料濃厚液の製造)
攪拌混合容器内において、アルミニウム顔料ペースト「GX−180A」(商品名、旭化成メタルズ社製、金属含有量74%)19部、2−エチル−1−ヘキサノール35部、リン酸基含有樹脂溶液(注1)8部及び2−(ジメチルアミノ)エタノール0.2部を均一に混合して、光輝性顔料濃厚液(P−1)を得た。
水酸基含有アクリル樹脂分散液(i)100部(固形分30部)、水酸基含有水溶性アクリル樹脂(ii)73部(固形分40部)、前記光輝性顔料濃厚液(P−1)62部及び「サイメル325」(商品名、オルネクスジャパン社製、メラミン樹脂、固形分80%)37.5部(固形分30部)を均一に混合し、更に、「プライマルASE−60」(商品名、ロームアンドハース社製、増粘剤)、2−(ジメチルアミノ)エタノール及び脱イオン水を加えて、pH8.0、塗料固形分25%、20℃におけるフォードカップNo.4による粘度が40秒の水性ベース塗料(Y1)を得た。
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脱イオン水130部、「アクアロンKH−10」(商品名、第一工業製薬株式会社製、ポリオキシエチレンアルキルエーテル硫酸塩エステルアンモニウム塩、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(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。次いで、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た。滴下終了後、1時間熟成した。
モノマー乳化物(2):脱イオン水18部、「アクアロンKH−10」0.31部、過硫酸アンモニウム0.03部、メタクリル酸5.1部、2−ヒドロキシエチルアクリレート5.1部、スチレン3部、メチルメタクリレート6部、エチルアクリレート1.8部及びn−ブチルアクリレート9部を混合攪拌して、モノマー乳化物(2)を得た。
フラスコ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、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時間かけてフラスコに滴下し、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時間かけてフラスコに滴下し、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、固形分濃度55%、酸価47mgKOH/g、水酸基価72mgKOH/gの水酸基含有水溶性アクリル樹脂(ii)を得た。
(カルボキシル基含有化合物の製造)
温度計、サーモスタット、撹拌器、還流冷却器、窒素ガス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、炭化水素系有機溶剤)680部を仕込み、窒素ガス通気下で125℃に昇温した。125℃に達した後、窒素ガスの通気を止め、下記モノマー混合物を一定の速度で4時間かけて滴下した。なお、p−tert−ブチルパーオキシ−2−エチルヘキサノエートは重合開始剤である。
温度計、サーモスタット、撹拌器、還流冷却器、窒素ガス導入管及び滴下装置を備えた反応容器に、キシレン410部及びn−ブタノール77部を仕込み、窒素ガス通気下で125℃に昇温した。125℃に達した後、窒素ガスの通気を止め、下記モノマー混合物を一定の速度で4時間かけて滴下した。なお、アゾビスイソブチロニトリルは重合開始剤である。
前記で得たカルボキシル基含有化合物溶液91部(固形分50部)、前記で得たポリエポキシド溶液71部(固形分50部)、「TBAB」(商品名、LION AKZO社製、テトラブチルアンモニウムブロマイド、有効成分100%)1部及び「BYK−300」(商品名、ビックケミー社製、表面調整剤、有効成分52%)0.2部を均一に混合し、さらに、スワゾール1000(商品名、コスモ石油社製、炭化水素系溶剤)を加えて、20℃におけるフォードカップNo.4による粘度が25秒のクリヤー塗料(Z1)を得た。
(試験用被塗物の作製)
リン酸亜鉛処理された合金化溶融亜鉛めっき鋼板に「エレクロンGT−10」(商品名、関西ペイント株式会社製、熱硬化性エポキシ樹脂系カチオン電着塗料)を膜厚20μmとなるように電着塗装し、170℃で30分間加熱して硬化させて試験用被塗物とした。
1)試験用被塗物に、前記で得た水性中塗り塗料(X1)をハンドスプレーガンで硬化塗膜15μmになるように塗装し、5分間放置後、80℃で3分間予備加熱を行なった。次いで、該中塗り塗膜上に前記で得た水性ベース塗料(Y1)をハンドスプレーガンで硬化膜厚10μmとなるように塗装し、5分間放置後、80℃で3分間予備加熱を行なった。
実施例1において、水性中塗り塗料(X1)を水性中塗り塗料(X2)〜(X16)のいずれかに変更する以外は、実施例1と同様にして各試験板(2種類)を作製した。
上記作製した各試験板Aを40℃に設定した恒温水槽中に240時間浸漬させ、その後、23℃の水中に1時間浸漬させて冷却した後、以下の剥離試験を行った。
硬化した接着剤層を塗膜に対して90度以上の方向に手で引っ張りながら2〜3mm間隔で、塗膜に対して約60度の角度で塗膜表面に達するところまでカッターナイフでカットを入れる。接着剤層を剥がした後の剥離状態を以下の「◎」、「○」、「△」、「×」の基準により評価した。
◎:接着剤層の剥れが認められず、塗膜の露出も認められない。
○:塗膜は破壊されず、接着剤層のみが凝集破壊を起こして剥れるが、塗膜と接着剤層の付着はほぼ保たれている。
△:塗膜が凝集破壊を起こして剥れる。
×:塗膜と接着剤層との界面で剥れが認められる。
スガ試験機社製の飛石試験機JA−400型(チッピング試験装置)の試片保持台に試験板Bを設置し、−20℃において、30cmの距離から0.392MPa(4kgf/cm2)の圧縮空気により、粒度7号の花崗岩砕石50gを試験板Bに45度の角度で衝突させた。その後、得られた試験板Bを水洗して、乾燥し、塗面に布粘着テープ(ニチバン社製)を貼着して、それを剥離した後、塗膜のキズの発生程度等を目視で観察し、下記基準により評価した。
◎:キズの大きさが極めて小さく、電着面や素地の鋼板が露出していない
○:キズの大きさが小さく、電着面や素地の鋼板が露出していない
△:キズの大きさは小さいが、電着面や素地の鋼板が露出している
×:キズの大きさはかなり大きく、素地の鋼板も大きく露出している
Claims (1)
- 電着塗装された合金化溶融亜鉛めっき鋼板上に、下記工程(1)〜(4)を順次行なう複層塗膜形成方法であって、
工程(1):電着塗膜上に、水性中塗り塗料(X)を塗装して中塗り塗膜を形成する工程
工程(2):予備加熱後、中塗り塗膜上に、水性ベース塗料(Y)を塗装してベース塗膜を形成する工程
工程(3):予備加熱後、ベース塗膜上に、塗料中の樹脂成分固形分100質量部を基準として、カルボキシル基含有化合物40〜60質量部及びポリエポキシド60〜40質量部を含有するクリヤー塗料(Z)を塗装してクリヤー塗膜を形成する工程
工程(4):前記工程(1)〜(3)で形成された中塗り塗膜、ベース塗膜及びクリヤー塗膜を加熱硬化する工程
前記水性中塗り塗料(X)が、ガラス転移温度(Tg)が5〜15℃の範囲内であり、かつ重量平均分子量が30,000〜40,000の範囲内である水酸基含有アクリル樹脂(A)、ガラス転移温度(Tg)が−50℃以下であり、ポリエーテル骨格を有するポリウレタン樹脂(B)、水酸基含有ポリエステル樹脂(C)、メラミン樹脂(D)及び活性メチレンブロックポリイソシアネート化合物(E)を含有し、該水酸基含有アクリル樹脂(A)と該ポリウレタン樹脂(B)との使用比が固形分比で、20/10〜30/10の範囲内であり、該水性中塗り塗料(X)による加熱硬化後の形成塗膜の20℃における破断伸び率が20〜30%の範囲内であり、ヤング率が5,000〜6,000MPaの範囲内であり、ツーコン硬度が4〜6の範囲内の範囲内であることを特徴とする複層塗膜形成方法。
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