JP5342719B2 - 金属表面処理剤、金属材料の表面処理方法及び表面処理金属材料 - Google Patents
金属表面処理剤、金属材料の表面処理方法及び表面処理金属材料 Download PDFInfo
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- JP5342719B2 JP5342719B2 JP2011172463A JP2011172463A JP5342719B2 JP 5342719 B2 JP5342719 B2 JP 5342719B2 JP 2011172463 A JP2011172463 A JP 2011172463A JP 2011172463 A JP2011172463 A JP 2011172463A JP 5342719 B2 JP5342719 B2 JP 5342719B2
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- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 description 1
- 229940099596 manganese sulfate Drugs 0.000 description 1
- 239000011702 manganese sulphate Substances 0.000 description 1
- 235000007079 manganese sulphate Nutrition 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 description 1
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 1
- QWYFOIJABGVEFP-UHFFFAOYSA-L manganese(ii) iodide Chemical compound [Mn+2].[I-].[I-] QWYFOIJABGVEFP-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- ALTWGIIQPLQAAM-UHFFFAOYSA-N metavanadate Chemical compound [O-][V](=O)=O ALTWGIIQPLQAAM-UHFFFAOYSA-N 0.000 description 1
- VHWYCFISAQVCCP-UHFFFAOYSA-N methoxymethanol Chemical compound COCO VHWYCFISAQVCCP-UHFFFAOYSA-N 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 1
- OOHAUGDGCWURIT-UHFFFAOYSA-N n,n-dipentylpentan-1-amine Chemical compound CCCCCN(CCCCC)CCCCC OOHAUGDGCWURIT-UHFFFAOYSA-N 0.000 description 1
- KBJFYLLAMSZSOG-UHFFFAOYSA-N n-(3-trimethoxysilylpropyl)aniline Chemical compound CO[Si](OC)(OC)CCCNC1=CC=CC=C1 KBJFYLLAMSZSOG-UHFFFAOYSA-N 0.000 description 1
- BPLYVSYSBPLDOA-GYOJGHLZSA-N n-[(2r,3r)-1,3-dihydroxyoctadecan-2-yl]tetracosanamide Chemical compound CCCCCCCCCCCCCCCCCCCCCCCC(=O)N[C@H](CO)[C@H](O)CCCCCCCCCCCCCCC BPLYVSYSBPLDOA-GYOJGHLZSA-N 0.000 description 1
- QJQAMHYHNCADNR-UHFFFAOYSA-N n-methylpropanamide Chemical compound CCC(=O)NC QJQAMHYHNCADNR-UHFFFAOYSA-N 0.000 description 1
- JACMPVXHEARCBO-UHFFFAOYSA-N n-pentylpentan-1-amine Chemical compound CCCCCNCCCCC JACMPVXHEARCBO-UHFFFAOYSA-N 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
- 229920005615 natural polymer Polymers 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- BMGNSKKZFQMGDH-FDGPNNRMSA-L nickel(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Ni+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O BMGNSKKZFQMGDH-FDGPNNRMSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- ZODDGFAZWTZOSI-UHFFFAOYSA-N nitric acid;sulfuric acid Chemical compound O[N+]([O-])=O.OS(O)(=O)=O ZODDGFAZWTZOSI-UHFFFAOYSA-N 0.000 description 1
- 239000002736 nonionic surfactant 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
- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 description 1
- 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
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000010292 orthophenyl phenol Nutrition 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- QBDSZLJBMIMQRS-UHFFFAOYSA-N p-Cumylphenol Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=CC=C1 QBDSZLJBMIMQRS-UHFFFAOYSA-N 0.000 description 1
- NRZWYNLTFLDQQX-UHFFFAOYSA-N p-tert-Amylphenol Chemical compound CCC(C)(C)C1=CC=C(O)C=C1 NRZWYNLTFLDQQX-UHFFFAOYSA-N 0.000 description 1
- FXLOVSHXALFLKQ-UHFFFAOYSA-N p-tolualdehyde Chemical compound CC1=CC=C(C=O)C=C1 FXLOVSHXALFLKQ-UHFFFAOYSA-N 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 125000004817 pentamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 1
- IGEIPFLJVCPEKU-UHFFFAOYSA-N pentan-2-amine Chemical compound CCCC(C)N IGEIPFLJVCPEKU-UHFFFAOYSA-N 0.000 description 1
- GTCCGKPBSJZVRZ-UHFFFAOYSA-N pentane-2,4-diol Chemical compound CC(O)CC(C)O GTCCGKPBSJZVRZ-UHFFFAOYSA-N 0.000 description 1
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 229940100595 phenylacetaldehyde Drugs 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 239000000467 phytic acid Substances 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- QLNJFJADRCOGBJ-UHFFFAOYSA-N propionamide Chemical compound CCC(N)=O QLNJFJADRCOGBJ-UHFFFAOYSA-N 0.000 description 1
- 229940080818 propionamide Drugs 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- ZVJHJDDKYZXRJI-UHFFFAOYSA-N pyrroline Natural products C1CC=NC1 ZVJHJDDKYZXRJI-UHFFFAOYSA-N 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000011684 sodium molybdate Substances 0.000 description 1
- 235000015393 sodium molybdate Nutrition 0.000 description 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 229910001631 strontium chloride Inorganic materials 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- UMBFGWVRZIHXCK-FDGPNNRMSA-L strontium;(z)-4-oxopent-2-en-2-olate Chemical compound [Sr+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O UMBFGWVRZIHXCK-FDGPNNRMSA-L 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 125000001174 sulfone group Chemical group 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000004347 surface barrier Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 0.000 description 1
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 description 1
- 150000000000 tetracarboxylic acids Chemical class 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- RIAJLMJRHLGNMZ-UHFFFAOYSA-N triazanium;trioxomolybdenum;phosphate Chemical compound [NH4+].[NH4+].[NH4+].O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.[O-]P([O-])([O-])=O RIAJLMJRHLGNMZ-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- 150000003628 tricarboxylic acids Chemical class 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 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
- 229940048102 triphosphoric acid Drugs 0.000 description 1
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 1
- JBIQAPKSNFTACH-UHFFFAOYSA-K vanadium oxytrichloride Chemical compound Cl[V](Cl)(Cl)=O JBIQAPKSNFTACH-UHFFFAOYSA-K 0.000 description 1
- 239000012002 vanadium phosphate Substances 0.000 description 1
- HQYCOEXWFMFWLR-UHFFFAOYSA-K vanadium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[V+3] HQYCOEXWFMFWLR-UHFFFAOYSA-K 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 239000004246 zinc acetate Substances 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
- 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
- 150000003755 zirconium compounds Chemical class 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
- Chemical Treatment Of Metals (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Description
また本発明で用いるカチオン性ウレタン樹脂(A)は水溶性のもの又は水系エマルジョン形態のものである。
1,000,000の範囲であるのが好ましく、2,000〜100,000の範囲であるのがより好ましい。数平均分子量が1,000未満では形成された皮膜のバリア性(緻密性)が劣り、耐食性や耐アルカリ性が低下する傾向となり、また1,000,000を超えると本金属表面処理剤の液安定性が損なわれる可能性がある。
本発明の金属表面処理剤及び表面処理方法は、冷延鋼板、炭素鋼板、ケイ素鋼板などの鋼板、メッキ鋼板、アルミニウム系金属材料に適している。メッキ鋼板は、例えば電気亜鉛メッキ、溶融亜鉛メッキ、55%アルミ亜鉛メッキ、5%アルミ亜鉛メッキ、アルミメッキ、鉄亜鉛メッキなどのメッキ処理が施された亜鉛含有メッキ鋼板を包含する。アルミニウム系金属材料は、純アルミニウム材、アルミニウム合金材、アルミニウムダイキャスト材等のアルミニウム又はアルミニウム合金を主成分とする金属材料を包含する。
本発明の金属表面処理剤は、金属材料に塗布され乾燥される工程において、金属材料表面と反応し密着性の良好な皮膜を形成すると共に樹脂成分が造膜し、優れた耐食性を素材に付与するものと考えられる。カチオン性フェノール系重縮合物(B)とチタン化合物(C)は、処理剤塗布時又は加熱乾燥工程において、緻密な3次元構造を形成して造膜すると共に、金属表面と反応して固着する。この際に、前記金属表面処理剤中に酸成分(E)が含有されることにより、エッチング作用が高まり、より金属表面との反応性が高まることによって、より強固な皮膜が金属表面との界面に形成される。
また、シランカップリング剤(G)はそれが加水分解して生じるシラノール基が金属材料の表面に吸着(水素結合)して金属材料が腐食環境下に置かれたときにこれを不活性化し、また、形成される皮膜においてシランカップリング剤同士が反応してシロキサン結合を生じこれにより皮膜のバリアー性が向上することで、耐食性や耐アルカリ性を向上させる。
また、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)とを組合せ、かつ両者の比率を限定することで耐水性が改善され、皮膜が溶解し難くなり、耐アルカリ性の向上につながる。
耐黄変性(耐熱性)に関しては、カチオン性フェノール系重縮合物(B)は芳香環を有しているため、加熱により変色しやすい傾向があるが、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)との使用比率を本発明に規定するようにすることで、耐食性、耐黒変性及び耐アルカリ性を維持しながら、耐黄変性を付与/向上させることができる。
I 電気亜鉛メッキ鋼板(板厚:0.8mm)
II 溶融亜鉛メッキ鋼板(板厚:0.8mm)
III 5%アルミ亜鉛メッキ鋼板(板厚:0.6mm)
IV 55%アルミ亜鉛メッキ鋼板(板厚:0.4mm)
(2−1)カチオン性ウレタン樹脂(A)
カチオン性ウレタン樹脂(A1)
ポリエーテルポリオール(合成成分:テトラメチレングリコール及びエチレングリコール、分子量1500)150質量部、トリメチロールプロパン6質量部、N−メチル−N,N−ジエタノールアミン24質量部、イソホロンジイソシアネート94質量部及びメチルエチルケトン135質量部を反応容器に入れ、70〜75℃に保ちながら1時間反応させてウレタンプレポリマーを生成させた。ついで該反応容器にジメチル硫酸15質量部を入れ、50〜60℃で30〜60分間反応させて、カチオン性ウレタンプレポリマーを生成させた。ついで該反応容器に水576質量部を入れ、混合物を均一に乳化させた後、メチルエチルケトンを回収して水溶性のカチオン性ウレタン樹脂(A1)を得た。
ポリエステルポリオール(合成成分:イソフタル酸、アジピン酸及び1,6−へキサンジオール、エチレングリコール、分子量1700)135質量部、トリメチロールプロパン5質量部、N−メチル−N,N−ジエタノールアミン22質量部、イソホロンジイソシアネート86質量部及びメチルエチルケトン120質量部を反応容器に入れ、70〜75℃に保ちながら1時間反応させてウレタンプレポリマーを生成させた。該反応容器にジメチル硫酸17質量部を入れ、50〜60℃で30〜60分間反応させてカチオン性ウレタンプレポリマーを生成させた。ついで該反応容器に水615質量部を入れ、混合物を均一に乳化させた後、メチルエチルケトンを回収して水溶性のカチオン性ウレタン樹脂(A2)を得た。
ポリカーボネートポリオール(合成成分:1.6−ヘキサンカーボネートジオール、エチレングリコール、分子量2000)130質量部、トリメチロールプロパン4質量部、N−メチル−N,N−ジエタノールアミン21質量部、イソホロンジイソシアネート75質量部及びメチルエチルケトン115質量部を反応容器に入れ、70〜75℃に保ちながら1時間反応をさせてウレタンプレポリマーを生成させた。ついで該反応容器にジメチル硫酸22質量部を入れ、50〜60℃で30〜60分間反応させてカチオン性ウレタンプレポリマーを生成させた。ついで該反応容器に水633質量部を入れ、混合物を均一に乳化させた後、メチルエチルケトンを回収して水溶性のカチオン性ポリウレタン樹脂(A3)を得た。
ポリエステルポリオール(合成成分:イソフタル酸、アジピン酸、1,6−ヘキサンジオール及びエチレングリコール、分子量2000)135質量部、トリメチロールプロパン5質量部、N−メチル−N,N−ジエタノールアミン22質量部、イソホロンジイソシアネート86質量部、γ−アミノプロピルトリエトキシシラン1質量部及びメチルエチルケトン120質量部を反応容器に入れ、70〜75℃に保ちながら1時間反応をさせてウレタンプレポリマーを生成させた。ついで該反応容器にジメチル硫酸17質量部を入れ、50〜60℃で30〜60分間反応させてカチオン性ウレタンプレポリマーを生成させた。ついで該反応容器に水615質量部を入れ、混合物を均一に乳化させた後、メチルエチルケトンを回収してシリル変性した、水溶性のカチオン性ポリウレタン樹脂(A4)を得た。
ポリカーボネートポリオール(合成成分:1,3−ジオキソラン−2−オン及び1,6−ヘキサンジオール、分子量1700)150質量部、トリメチロールプロパン6質量部、N−メチル−N,N−ジエタノールアミン24質量部、イソホロンジイソシアネート94質量部、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2質量部及びメチルエチルケトン135質量部を反応容器に入れ、70〜75℃に保ちながら1時間反応をさせてウレタンプレポリマーを生成させた。ついで該反応容器にジメチル硫酸15質量部を入れ、50〜60℃で30〜60分間反応させてカチオン性ウレタンプレポリマーを生成させた。ついで該反応容器に水576質量部を入れ、混合物を均一に乳化させた後、メチルエチルケトンを回収してシリル変性した、水溶性のカチオン性ポリウレタン樹脂(A5)を得た。
カチオン性フェノール系重縮合物(B1)
還流冷却機を備えた1000mLのフラスコ内に、ビスフェノールA1モル(228g)及び触媒としてp−トルエンスルホン酸0.3gを仕込み、内部温度を100℃まで上げ、ホルムアルデヒド水溶液0.85モル(69g)を1時間かけて添加し、100℃で2時間還流下に反応させた。その後、反応容器を水冷静置し、上層に分離する水層の濁りがなくなってから、デカンテーションして水層を除去し、さらに170〜175℃になるまで加熱攪拌して、未反応分及び水分を除去した。
次に、100℃まで温度を下げ、ブチルセロソルブ234gを添加して重縮合物を完全に溶解させた後、純水234gを加え、系内の温度が50℃まで下がったところで、ジエタノールアミン1モル(75g)を添加し、これにホルムアルデヒド水溶液1モル(81.1g)を50℃で約1時間かけて滴下した。さらに、80℃まで温度を上げ、約3時間攪拌しながら反応を続けカチオン性フェノール系重縮合物(B1)を得た。
還流冷却機を備えた1000mLのフラスコ内に、フェノール1モル(96g)及び触媒としてp−トルエンスルホン酸0.3gを仕込み、内部温度を100℃まで上げ、ホルムアルデヒド水溶液0.7モル(56.8g)を1時間かけて添加し、100℃で2時間還流下に反応させた。その後、反応容器を水冷静置し、上層に分離する水層の濁りがなくなってから、デカンテーションして水層を除去し、さらに170〜175℃になるまで加熱攪拌して、未反応分及び水分を除去した。
次に、100℃まで温度を下げ、ブチルセロソルブ234gを添加して重縮合物を完全に溶解させた後、純水234gを加え、系内の温度が50℃まで下がったところで、N−メチルプロパノールアミン1モル(89g)を添加し、これにホルムアルデヒド水溶液0.7モル(56.8g)を50℃で約1時間かけて滴下した。さらに、80℃まで温度を上げ、約3時間攪拌しながら反応を続けカチオン性フェノール系重縮合物(B2)を得た。
還流冷却機を備えた1000mLのフラスコ内に、O−クレゾール1モル(108g)及び触媒としてp−トルエンスルホン酸0.3gを仕込み、内部温度を100℃まで上げ、ホルムアルデヒド水溶液0.85モル(69g)を1時間かけて添加し、100℃で2時間還流下に反応させた。その後、反応容器を水冷静置し、上層に分離する水層の濁りがなくなってから、デカンテーションして水層を除去し、さらに170〜175℃になるまで加熱攪拌して、未反応分及び水分を除去した。
次に、100℃まで温度を下げ、ブチルセロソルブ234gを添加して重縮合物を完全に溶解させた後、純水234gを加え、系内の温度が50℃まで下がったところで、N,N−ジエチルエタノールアミン1モル(117g)を添加し、これにホルムアルデヒド水溶液1モル(81.1g)を50℃で約1時間かけて滴下した。さらに、80℃まで温度を上げ、約3時間攪拌しながら反応を続けカチオン性フェノール系重縮合物(B3)を得た。
C1:チタンラクテート
C2:ヘキサフルオロチタン酸
D1:酸化リチウム
D2:硝酸マグネシウム
D3:酸化マグネシウム
D4:アルミニウムアセチルアセトネート
D5:フッ化カルシウム
D6:リン酸二水素マンガン
D7:炭酸マンガン
D8:硝酸コバルト
D9:硝酸ニッケル
D10:炭酸ニッケル
D11:硝酸ストロンチウム
D12:酸化モリブデン
D13:メタタングステン酸アンモニウム
D14:酸化セリウム
D15:酸化亜鉛
D16:亜鉛アセチルアセトネート
E1:フッ化水素酸
E2:リン酸
E3:硝酸
E4:クエン酸
E5:シュウ酸
F1:メタバナジン酸アンモニウム
F2:バナジウムアセチルアセトネート
F3:リン酸バナジウム
F4:オキシ硫酸バナジウム
G1:ビニルトリメトキシシラン
G2:γ−グリシドキシプロピルトリメトキシシラン
G3: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
G4:γ−アミノプロピルトリエトキシシラン
(3−1)脱脂
日本パーカライジング(株)製アルカリ脱脂剤パルクリーン364S(20g/L建浴、60℃、10秒スプレー、スプレー圧0.5kg/cm2)で素材を脱脂した後、スプレー水洗を10秒行った。
(3−2)塗布及び乾燥
I:固形分濃度10質量%に調整した金属表面処理剤(媒体:水)を乾燥質量が700mg/m2になるようにバーコート塗布し、80℃(PMT:到達板温)で乾燥した。
II:固形分濃度16質量%に調整した金属表面処理剤(媒体:水)を乾燥質量が1000mg/m2になるようにバーコート塗布し、150℃(PMT)で乾燥した。
以下の評価において、□以上は実用性があると解される。
(4−1)耐食性
実施例、比較例において作製した処理板試料について、無加工(平面部)、NTカッターで素地到達までクロスカットしたもの(クロスカット部)、エリクセン7mm押し出し加工したもの(加工部)について、耐食性試験を行った。評価方法は次の通りである。
(平面部)塩水噴霧試験法JIS−Z−2371に基づき塩水噴霧360時間後の白錆発生面積を求め評価した。
評価基準:白錆発生面積
◎1%未満、○1%以上〜5%未満、□5%以上〜10%未満、△10%以上〜30%未満、×30%以上〜50%未満、××50%以上。
(クロスカット部)塩水噴霧試験法JIS−Z−2371に基づき塩水噴霧360時間後の白錆発生状況を肉眼で評価した。
評価基準:白錆発生状況 ◎ほとんど錆なし、○クロスカット部に白錆が発生していない部分が多い、△クロスカット部の全てが白錆になっているが、流れ錆なし、×クロスカット部から流れ錆が発生。
(加工部)塩水噴霧試験法JIS−Z−2371に基づき塩水噴霧360時間後の白錆発生状況を肉眼で評価した。
評価基準:白錆発生状況 ◎ほとんど錆なし、○加工部に白錆が発生していない部分が多い、△加工部の全てが白錆になっているが、流れ錆なし、×加工部から流れ錆が発生。
処理板試料に、日本パーカライジング(株)製アルカリ脱脂剤パルクリーン364Sを20g/L水に建浴し65℃に調整した脱脂剤水溶液を5分間スプレーし、水洗した後、80℃で乾燥した。この板について、上記(4−1)に記載した条件、評価法で耐食性を評価した。
(4−3)耐黒変性
処理板試料を温度70℃、湿度95%雰囲気に12日間放置した後、外観を肉眼で観察し評価した。
評価基準:◎白錆発生なし、黒変なし、○白錆発生なし、黒変僅かにあり、△白錆発生あり、黒変僅かにあり、×白錆発生あり、黒変かなりあり。
(4−3)耐黄変性
処理板試料を温度250℃雰囲気に2時間放置した後、外観を肉眼で観察し評価した。
評価基準:◎変色なし、○僅かに黄変、△全面黄変、×全面黄褐色。
Claims (12)
- カチオン性の水溶性もしくは水系エマルジョンウレタン樹脂(A)であってシリル変性されていないもの(以下、カチオン性ウレタン樹脂(A)という)、フェノール系化合物とアルデヒド類との重縮合物であってカチオン性のもの(B)(以下、カチオン性フェノール系重縮合物(B)という)、チタン化合物(C)、及びLi、Mg、Al、Ca、Co、Ni、Zn及びSrから選ばれる少なくとも1種の金属を含有する化合物(D)(以下、金属化合物(D)という)を水性媒体に配合してなる金属表面処理剤であって、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)との配合比率が、固形分質量比として、(A):(B)=99:1〜50:50である該金属表面処理剤。
- 無機酸及び有機酸から選ばれる少なくとも1種の酸成分(E)(以下、酸成分(E)という)を配合した請求項1記載の金属表面処理剤。
- バナジウム化合物(F)を配合した請求項1又は2記載の金属表面処理剤。
- シランカップリング剤(G)を配合した請求項1〜3のいずれか1項に記載の金属表面処理剤。
- シランカップリング剤(G)がアミノ基を有するシランカップリング剤及びエポキシ基を有するシランカップリング剤から選ばれる少なくとも1種である請求項1〜4のいずれか1項に記載の金属表面処理剤。
- チタン化合物(C)の配合割合が、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)との合計固形分100質量部に対し、チタンとして0.1〜20質量部である請求項1〜5のいずれか1項に記載の金属表面処理剤。
- 金属化合物(D)の配合割合が、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)との合計固形分100質量部に対し、該金属として0.01〜10質量部である請求項1〜6のいずれか1項に記載の金属表面処理剤。
- 酸成分(E)の配合割合が、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)との合計固形分100質量部に対し、水を含まない酸成分そのものとして1〜30質量部である請求項1〜7のいずれか1項に記載の金属表面処理剤。
- バナジウム化合物(F)の配合割合が、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)との合計固形分100質量部に対し、バナジウムとして0.01〜20質量部である請求項1〜8のいずれか1項に記載の金属表面処理剤。
- シランカップリング剤(G)の配合割合が、カチオン性ウレタン樹脂(A)とカチオン性フェノール系重縮合物(B)との合計固形分100質量部に対し、固形分として0.5〜30質量部である請求項1〜9のいずれか1項に記載の金属表面処理剤。
- 金属材料表面に、請求項1〜10のいずれか1項に記載の金属表面処理剤を塗布した後、乾燥することによって該金属材料表面に皮膜を形成させることを特徴とする金属材料の表面処理方法。
- 請求項11記載の表面処理方法を用いて形成された皮膜を有する金属材料。
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