JP6455855B2 - 水性金属表面処理剤 - Google Patents
水性金属表面処理剤 Download PDFInfo
- Publication number
- JP6455855B2 JP6455855B2 JP2015085759A JP2015085759A JP6455855B2 JP 6455855 B2 JP6455855 B2 JP 6455855B2 JP 2015085759 A JP2015085759 A JP 2015085759A JP 2015085759 A JP2015085759 A JP 2015085759A JP 6455855 B2 JP6455855 B2 JP 6455855B2
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- JP
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- Prior art keywords
- acid
- surface treatment
- resin
- metal surface
- parts
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052751 metal Inorganic materials 0.000 title claims description 139
- 239000002184 metal Substances 0.000 title claims description 139
- 239000012756 surface treatment agent Substances 0.000 title claims description 61
- 125000002091 cationic group Chemical group 0.000 claims description 65
- -1 phosphoric acid compound Chemical class 0.000 claims description 61
- 229920005989 resin Polymers 0.000 claims description 56
- 239000011347 resin Substances 0.000 claims description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 43
- 238000004381 surface treatment Methods 0.000 claims description 41
- 239000002253 acid Substances 0.000 claims description 40
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 38
- 238000011282 treatment Methods 0.000 claims description 37
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 36
- 238000000034 method Methods 0.000 claims description 29
- 150000003839 salts Chemical class 0.000 claims description 26
- 235000011007 phosphoric acid Nutrition 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 24
- 229910000831 Steel Inorganic materials 0.000 claims description 23
- 239000010959 steel Substances 0.000 claims description 23
- 238000000576 coating method Methods 0.000 claims description 22
- 150000001875 compounds Chemical class 0.000 claims description 22
- 239000004925 Acrylic resin Substances 0.000 claims description 21
- 229920000178 Acrylic resin Polymers 0.000 claims description 21
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 21
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 20
- 239000011248 coating agent Substances 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 15
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- 238000004519 manufacturing process Methods 0.000 claims description 13
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- 125000001494 2-propynyl group Chemical group [H]C#CC([H])([H])* 0.000 claims description 7
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- 125000005702 oxyalkylene group Chemical group 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- DBVJJBKOTRCVKF-UHFFFAOYSA-N Etidronic acid Chemical compound OP(=O)(O)C(O)(C)P(O)(O)=O DBVJJBKOTRCVKF-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910001297 Zn alloy Inorganic materials 0.000 claims description 3
- HJZKOAYDRQLPME-UHFFFAOYSA-N oxidronic acid Chemical compound OP(=O)(O)C(O)P(O)(O)=O HJZKOAYDRQLPME-UHFFFAOYSA-N 0.000 claims description 3
- 229960004230 oxidronic acid Drugs 0.000 claims description 3
- JZDMNWBZPLJKBT-UHFFFAOYSA-N F.[Zr] Chemical compound F.[Zr] JZDMNWBZPLJKBT-UHFFFAOYSA-N 0.000 claims 1
- 239000007859 condensation product Substances 0.000 claims 1
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- 239000006185 dispersion Substances 0.000 description 15
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 12
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- 229910052782 aluminium Inorganic materials 0.000 description 10
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 10
- 125000003277 amino group Chemical group 0.000 description 10
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 10
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- 239000001993 wax Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000002156 mixing Methods 0.000 description 9
- 229920005862 polyol Polymers 0.000 description 9
- 229910052719 titanium Inorganic materials 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 125000004432 carbon atom Chemical group C* 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 8
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphonic acid group Chemical group P(O)(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
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- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 7
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 7
- 239000000047 product Substances 0.000 description 7
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- 239000004593 Epoxy Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 238000002845 discoloration Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 235000021317 phosphate Nutrition 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 description 5
- 235000011054 acetic acid Nutrition 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 241001163841 Albugo ipomoeae-panduratae Species 0.000 description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 125000002947 alkylene group Chemical group 0.000 description 4
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 229910000365 copper sulfate Inorganic materials 0.000 description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
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- 238000005259 measurement Methods 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 238000007747 plating Methods 0.000 description 4
- 235000013824 polyphenols Nutrition 0.000 description 4
- 230000003449 preventive effect Effects 0.000 description 4
- PPASLZSBLFJQEF-RKJRWTFHSA-M sodium ascorbate Substances [Na+].OC[C@@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RKJRWTFHSA-M 0.000 description 4
- 235000010378 sodium ascorbate Nutrition 0.000 description 4
- 229960005055 sodium ascorbate Drugs 0.000 description 4
- PPASLZSBLFJQEF-RXSVEWSESA-M sodium-L-ascorbate Chemical compound [Na+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] PPASLZSBLFJQEF-RXSVEWSESA-M 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 3
- 239000004721 Polyphenylene oxide Substances 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 150000001845 chromium compounds Chemical class 0.000 description 3
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- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 125000001153 fluoro group Chemical group F* 0.000 description 3
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 3
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- 125000001302 tertiary amino group Chemical group 0.000 description 3
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 3
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- 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 3
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- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 3
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- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 2
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- 239000005051 trimethylchlorosilane Substances 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 229910001935 vanadium oxide Inorganic materials 0.000 description 1
- VLOPEOIIELCUML-UHFFFAOYSA-L vanadium(2+);sulfate Chemical compound [V+2].[O-]S([O-])(=O)=O VLOPEOIIELCUML-UHFFFAOYSA-L 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- XJUNLJFOHNHSAR-UHFFFAOYSA-J zirconium(4+);dicarbonate Chemical compound [Zr+4].[O-]C([O-])=O.[O-]C([O-])=O XJUNLJFOHNHSAR-UHFFFAOYSA-J 0.000 description 1
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 description 1
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Description
(1)重燐酸アルミニウムを含有する水溶液で処理した後、150〜550℃の温度で加熱する表面処理方法(例えば、特許文献1など参照)、
(2)タンニン酸を含有する水溶液で処理する方法(例えば、特許文献2 など参照)などが提案されている。
(b)フルオロ金属酸及び/又はその塩、
(c)アルミナゾル、
(d)カチオン性樹脂、並びに
(e)水、
を含有する処理剤であって、カチオン性樹脂(d)100質量部に基づき、
(a)リン酸系化合物を0.5〜10質量部、
(b)フルオロ金属酸及び/又はその塩を0.5〜10質量部、並びに
(c)アルミナゾルを5〜100質量部、含有することを特徴とする水性金属表面処理剤、を提供するものである。
本発明の水性金属表面処理剤の(a)成分であるリン酸系化合物は、リン酸基、ホスホン酸基又はこれらの基の塩を含有し、水溶性を有する化合物である。リン酸系化合物(a)としては、リン酸及び有機ホスホン酸並びにそれらの塩であることができる。
本発明の水系金属表面処理剤の(b)成分である、フルオロ金属酸及び/又はその塩は、本発明の水系金属表面処理剤から得られる表面処理皮膜の防錆性の向上などを目的に配合される。
本発明の水系金属表面処理剤の(c)成分である、アルミナゾルは、本発明の水系金属表面処理剤から得られる表面処理皮膜の防錆性の向上、耐溶剤性の向上などを目的に配合される。
本発明の金属表面処理組成物の(d)成分であるカチオン性樹脂は、水溶性ないし水分散性を有するカチオン性樹脂であり、その樹脂種としては、代表例として、アクリル樹脂、ポリウレタン樹脂、エポキシ樹脂、ポリエステル樹脂、アルキド樹脂、ポリブタジエン樹脂、フェノール樹脂などを挙げることができる。
(a)リン酸系化合物 0.5〜10質量部、好ましくは0.8〜7質量部、
(b)フルオロ金属酸及び/又はその塩 0.5〜10質量部、好ましくは0.8〜7質量部、
(c)アルミナゾル 5〜100質量部、好ましくは10〜40質量部。
本発明の水性金属表面処理剤に必要に応じて配合される(f)成分であるシランカップリング剤及びその加水分解縮合物は、得られる表面処理皮膜の基材表面への密着性の向上や、皮膜の耐食性、耐水性向上などに寄与することができる場合がある。
本発明の水性金属表面処理剤に必要に応じて配合される(g)成分は、プロパルギル基及び水酸基を有し、且つモノ又はポリ−オキシアルキレン基を有する、分子量100〜800の化合物(以下、「化合物(g)」と略称することがある。)であって、上記モノ又はポリ−オキシアルキレン基が、オキシエチレン基、ポリオキシエチレン基、オキシプロピレン基、ポリオキシプロピレン基、及びエチレンオキシドとプロピレンオキシドとの2価の共重合体基から選ばれる少なくとも1種である。
上記化合物(g)は、市販品であってもよく、好適なものとして、例えば、BASF社製の、Golpanol PME、Korantin PPなどを挙げることができる。Galpanol、Korantinは、登録商標である。
本発明の水性金属表面処理剤に必要に応じて配合されるワックス成分は、得られる表面処理皮膜に潤滑性を付与する成分であり、例えば、ポリオール化合物と脂肪酸とのエステル化物である脂肪酸エステルワックス、シリコン系ワックス、フッ素系ワックス、ポリエチレンやポリプロピレンなどのポリオレフィンワックス、ラノリン系ワックス、モンタンワックス、マイクロクリスタリンワックス及びカルナウバワックスなどを挙げることができる。これらは、1種で又は2種以上を組合せて使用することができる。
本発明の水性金属表面処理剤には、得られる処理皮膜の防錆性向上の目的で、必要に応じて、フルオロ金属酸及び/又はその塩(b)以外の防錆金属化合物を併用することができる。
本発明の水性金属表面処理剤は水性である。水性とは、溶媒が水を主成分とすることを意味する。溶媒は水のみでもよいが、皮膜の乾燥性、処理剤の粘度などを調整する目的で、1価又は多価のアルコール、ケトン、エーテルアルコール系などの各種の水溶性有機溶剤を1種または2種以上併用してもよい。本発明の水性金属表面処理剤は、溶媒中に水(e)を70質量%以上、好ましくは80質量%以上含有することが好ましい。
本発明の水性金属表面処理剤は、所望により、溶媒及び上記した成分以外に、必要に応じて、pH調整剤(酸もしくは塩基)、チタン含有水性液、充填剤、コロイダルシリカ、着色剤、界面活性剤、消泡剤、レベリング剤、抗菌剤などを配合することができる。これらは、得られる処理皮膜の性能や表面処理組成物の安定性を損なわない範囲で添加することができる。
本発明の金属表面処理方法は、上記本発明の水性金属表面処理剤を、金属基材上に塗布し、乾燥することを特徴とする金属表面処理方法であり、金属基材表面に本発明の水性金属表面処理組成物による処理皮膜を形成する方法である。本発明において、「処理皮膜」とは、連続した処理皮膜のみならず、処理付着量が少ないため連続した処理皮膜とならず、不連続となった処理物をも包含する。
本発明の表面処理金属板は、本発明の水性金属表面処理剤による表面処理が金属基材の表面になされてなる表面処理金属板である。本発明の表面処理金属板は、金属基材が板状形状であって、上記本発明の金属表面処理方法によって得ることができるものである。
製造例1
温度計、サーモスタット、攪拌装置、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、脱イオン水110部、「アデカリアソープER−40」(商品名、ADEKA製、乳化剤、有効成分60%)8部を仕込み、窒素気流中で攪拌混合し、60℃に昇温した。次いで、下記コア部用モノマー乳化物の全量のうちの5%量、10%「カヤブチルH−70」(商品名、化薬アクゾ製、重合開始剤、有効成分70%)水溶液1部及び3%アスコルビン酸ナトリウム水溶液1部を反応容器内に導入し60℃で1時間保持した。その後、コア部用モノマー乳化物の残部、10%「カヤブチルH−70」水溶液7部及び3%アスコルビン酸ナトリウム水溶液10部を2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時間熟成を行った。次に、下記シェル部用モノマー乳化物、10%「カヤブチルH−70」水溶液5部及び3%アスコルビン酸ナトリウム水溶液10部を2時間かけて滴下し、1時間熟成した後、酢酸0.6部を反応容器内に導入し30分間保持した。次に、30℃まで冷却し、脱イオン水で希釈して、平均粒子径170nm(サブミクロン粒度分布測定装置「COULTER N5型」(ベックマン・コールター社製)を用いて、20℃の条件下で測定した平均粒子直径)を有する、固形分30%のカチオン性アクリル樹脂水分散液(d1)を得た。得られたカチオン性アクリル樹脂は、アミン価10mgKOH/g樹脂、水酸基価16mgKOH/g樹脂、及び数平均分子量約65,000を有していた。
シェル部用モノマー乳化物:脱イオン水20部、「アデカリアソープER−40」3.5部、スチレン3部、メチルメタクリレート19部、n−ブチルメタクリレート3部、n−ブチルアクリレート2部、2−ヒドロキシエチルメタクリレート2部及びN,N−ジメチルアミノエチルメタクリレート1部を混合してなるモノマー乳化物。
温度計、サーモスタット、攪拌装置、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、プロピレングリコールモノプロピルエーテル50部を仕込み、窒素気流中で攪拌混合し、80℃に昇温後、スチレン20部、メチルメタクリレート40部、n−ブチルアクリレート10部、2−ヒドロキシエチルメタクリレート4部、N,N−ジメチルアミノエチルメタクリレート26部及びアゾビスイソブチルニトリル2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100℃に昇温し、さらに1時間熟成した。次に、50℃まで冷却し、酢酸5部反応容器内に導入し30分間保持した後、脱イオン水で希釈して固形分20%のカチオン性アクリル樹脂水分散液(d2)を得た。得られたカチオン性アクリル樹脂は、アミン価93mgKOH/g樹脂、水酸基価17mgKOH/g樹脂、及び数平均分子量約12,000を有していた。
温度計、サーモスタット、攪拌装置、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、固形分20%のカチオン性アクリル樹脂水分散液(d2)250部を仕込み、窒素気流中で攪拌混合し、80℃に昇温した後、アスコルビン酸ナトリウム0.3部と5%硫酸第一鉄水溶液0.3部を導入した。次に、メタクリル酸メチル25部、スチレン20部、n−ブチルアクリレート3部、2−ヒドロキシエチルメタクリレート2部の混合物及び30%過酸化水素水0.4部と脱イオン水20部との混合物を2時間かけて滴下し、ついで3時間熟成した後、脱イオン水で希釈して、平均粒子径70nm(サブミクロン粒度分布測定装置「COULTER N5型」(ベックマン・コールター社製)を用いて、20℃の条件下で測定した平均粒子直径)を有する、固形分30%のカチオン性アクリル樹脂水分散液(d3)を得た。得られたカチオン性アクリル樹脂は、アミン価46mgKOH/g樹脂、水酸基価9mgKOH/g樹脂、及び数平均分子量約34,500を有していた。
PP−400(三洋化成社製、商品名、ポリプロピレングリコール 分子量400)400部に、ε−カプロラクトン300部を加えて、130℃まで昇温した。その後、テトラブトキシチタン0.01部を加え、170℃に昇温した。この温度を保ちながら経時でサンプリングし、未反応のε−カプロラクトンが実質的になくなったことを確認した時点で冷却し、変性剤1を得た。
実施例1〜29及び比較例1〜10
後記表1に示す配合割合に従って配合し、固形分濃度が15質量%となるように脱イオン水を加えて調整し、十分攪拌を行って各金属表面処理剤を得た。なお、表1の配合量は固形分質量又は有効成分質量による。
○:液に沈殿物や浮遊物がなく、かつ液粘度10mPa・s以下、
△:液に僅かに沈殿物もしくは浮遊物が見られる、又は液粘度が10mPa・sを超えるが著しい増粘やゲル化は認めらない、
×:液にかなりの沈殿物もしくは浮遊物が見られる、又は著しい増粘もしくはゲル化が認められる。
a2:1−ヒドロキシエタン−1,1−ジホスホン酸、
b1:六フッ化チタン酸アンモニウム、
b2:六フッ化ジルコン酸アンモニウム。
c2:川研ファインケミカル株式会社製、商品名「アルミゾルCSA−10A」、アルミナコロイド、
c3:日産化学工業株式会社製、商品名「AS−200」、羽毛状コロイダルアルミナ、
c4:日産化学工業株式会社製、商品名「AS−520」、ベーマイト板状結晶コロイダルアルミナ、
c5:日揮触媒化成株式会社製、商品名「Cataloid AS−2」、高分子量アルミナ(擬ベーマイト)ゾル、
c6:日揮触媒化成株式会社製、商品名「Cataloid AS−3]高分子量アルミナ(擬ベーマイト)ゾル。
d2:製造例2で得たカチオン性アクリル樹脂水分散液(d2)、
d3:製造例3で得たカチオン性アクリル樹脂水分散液(d3)、
d4:製造例4で得たカチオン性エポキシ樹脂水分散液(d4)、
d5:株式会社ADEKA製、商品名「アデカボンタイターHUX−680」(ポリエステル系カチオン性ポリウレタン樹脂)、
d6:第一工業製薬社製、商品名「スーパーフレックス650」(ポリカーボネート系カチオン性ポリウレタン樹脂)。
f2:γ−メタクリロイルオキシプロピルトリメトキシシラン、
f3:3−メルカプトプロピルトリメトキシシラン。
g2:商品名「Korantin PP」(BASF製)、プロパルギル基、水酸基及びオキシプロピレン基を有し、ピーク分子量約260を有する、前記式(1)で表される化合物。
前記実施例及び比較例で得た各金属表面処理剤を用いて下記表2に示す仕様にて表面処理金属板を得た。
表2における金属板種類は下記のとおりである。
EG:メッキ付着量が片面20g/m2で、板厚0.8mmの両面電気亜鉛メッキ鋼板、
GI:メッキ付着量が片面60g/m2で、板厚0.8mmの両面溶融亜鉛メッキ鋼板、
GL:メッキ付着量が片面90g/m2で、板厚0.8mmの両面55%アルミニウム−亜鉛溶融メッキ鋼板、
GA:メッキ付着量が片面45g/m2で、板厚0.8mmの両面鉄−亜鉛合金化溶融メッキ鋼板。
各例において、表2に示す金属板を、アルカリ脱脂剤(日本シービーケミカル社製、商品名「ケミクリーナー561B」、珪酸3号相当品)を溶解した濃度2%の水溶液を使用して、液温65℃で60秒間スプレー処理により脱脂し、ついで液温50℃、スプレー時間20秒間の条件にて湯洗を行い乾燥してアルカリ脱脂金属板を得た。得られたアルカリ脱脂金属板について、前記各例で得られた金属表面処理剤を後記表2に示された組み合わせ及び乾燥皮膜質量に従ってバーコータにて塗布し、金属板の最高到達温度が80℃となるように12秒間加熱乾燥し、各表面処理金属板を得た。
◎:白錆の発生が認められない、
○:白錆の発生が認められるが、発生程度が処理膜面積の5%未満、
△:白錆の発生程度が処理膜面積の5%以上で、かつ30%未満、
×:白錆の発生程度が処理膜面積の30%以上。
◎:全く変化が認められない、
○:わずかにこすった跡が認められる、
×:こすった跡が明確に認められる。
◎:全く変色が認められない、
○:わずかな変色が認められる、
×:かなりの変色又は著しい変色が認められる。
◎:碁盤目塗膜の剥離が認められない、
○:1〜2個の碁盤目塗膜の剥離が認められる、
△:3〜10個の碁盤目塗膜の剥離が認められる、
×:11個以上の碁盤目塗膜の剥離が認められる。
a :10回全て
b :6〜9回
c :1〜5回
d :0回。
Claims (10)
- (a)リン酸系化合物、
(b)フルオロ金属酸及び/又はその塩、
(c)アルミナゾル、
(d)カチオン性樹脂、並びに
(e)水、
を含有する処理剤であって、カチオン性樹脂(d)100質量部に基づき、
(a)リン酸系化合物を0.5〜10質量部、
(b)フルオロ金属酸及び/又はその塩を0.5〜10質量部、並びに
(c)アルミナゾルを5〜100質量部、含有することを特徴とする、金属が亜鉛メッキ鋼板もしくは亜鉛合金メッキ鋼板である、水性金属表面処理剤。 - リン酸系化合物(a)が、オルトリン酸、ヒドロキシメタンジホスホン酸及び1−ヒドロキシエタン−1,1−ジホスホン酸から選ばれる少なくとも1種の化合物である請求項1記載の水性金属表面処理剤。
- フルオロ金属酸及び/又はその塩(b)が、チタンフッ化水素酸、ジルコニウムフッ化水素酸及びこれらの塩から選ばれる少なくとも1種の化合物である請求項1又は2記載の水性金属表面処理剤。
- カチオン性樹脂(d)が、水酸基価5〜100mgKOH/g樹脂で、且つアミン価3〜180mgKOH/g樹脂を有するカチオン性アクリル樹脂である請求項1〜3のいずれか一項に記載の水性金属表面処理剤。
- さらに、シランカップリング剤及び/又はその加水分解縮合物(f)を含有する請求項1〜4のいずれか一項に記載の水性金属表面処理剤。
- さらに、プロパルギル基及び水酸基を有し、且つモノ又はポリ−オキシアルキレン基を有する、分子量100〜800の化合物(g)を含有する請求項1〜5のいずれか一項に記載の水性金属表面処理剤。
- pHが3〜7で、固形分濃度が5〜30質量%である請求項1〜6のいずれか一項に記載の水性金属表面処理剤。
- 請求項1〜7のいずれか一項に記載の水性金属表面処理剤を、金属基材上に塗布し、乾燥させることを特徴とする金属表面処理方法。
- 請求項1〜7のいずれか一項に記載の水性金属表面処理剤による表面処理が金属基材の表面になされてなる表面処理金属板の製造方法。
- 請求項1〜7のいずれか一項に記載の水性金属表面処理剤による処理皮膜の皮膜量が、固形分で0.5〜3.5g/m2である請求項9に記載の表面処理金属板の製造方法。
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