CN116670236A - 用于涂锌铝钢的基于Cr(III)的改善钝化 - Google Patents
用于涂锌铝钢的基于Cr(III)的改善钝化 Download PDFInfo
- Publication number
- CN116670236A CN116670236A CN202180089122.0A CN202180089122A CN116670236A CN 116670236 A CN116670236 A CN 116670236A CN 202180089122 A CN202180089122 A CN 202180089122A CN 116670236 A CN116670236 A CN 116670236A
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- CN
- China
- Prior art keywords
- composition
- aluminum
- acid
- zinc
- chromate
- Prior art date
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- Pending
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 65
- 238000002161 passivation Methods 0.000 title claims abstract description 64
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 47
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 239000011701 zinc Substances 0.000 title claims abstract description 35
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 33
- 229910000831 Steel Inorganic materials 0.000 title description 12
- 239000010959 steel Substances 0.000 title description 12
- 239000000203 mixture Substances 0.000 claims abstract description 187
- -1 aluminum carboxylate Chemical class 0.000 claims abstract description 137
- 239000011651 chromium Substances 0.000 claims abstract description 63
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 47
- 238000000576 coating method Methods 0.000 claims abstract description 26
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 23
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 23
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 23
- 229910001297 Zn alloy Inorganic materials 0.000 claims abstract description 22
- 229920000642 polymer Polymers 0.000 claims abstract description 20
- 239000004814 polyurethane Substances 0.000 claims abstract description 20
- 229920002635 polyurethane Polymers 0.000 claims abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 13
- 229920005601 base polymer Polymers 0.000 claims abstract description 12
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 11
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 11
- 239000007983 Tris buffer Substances 0.000 claims abstract description 10
- 150000001399 aluminium compounds Chemical class 0.000 claims abstract description 10
- 239000000344 soap Substances 0.000 claims abstract description 7
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 6
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 6
- XWTXZJITNNRDLC-UHFFFAOYSA-K bis[(2-hydroxyacetyl)oxy]alumanyl 2-hydroxyacetate Chemical compound [Al+3].OCC([O-])=O.OCC([O-])=O.OCC([O-])=O XWTXZJITNNRDLC-UHFFFAOYSA-K 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 66
- 239000000758 substrate Substances 0.000 claims description 43
- 239000002253 acid Substances 0.000 claims description 29
- 229940117975 chromium trioxide Drugs 0.000 claims description 28
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 28
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 125000000217 alkyl group Chemical group 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 20
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 16
- 229910052804 chromium Inorganic materials 0.000 claims description 16
- 239000006185 dispersion Substances 0.000 claims description 14
- 239000011734 sodium Substances 0.000 claims description 12
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 150000002978 peroxides Chemical class 0.000 claims description 9
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 7
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical class [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- 150000007513 acids Chemical class 0.000 claims description 6
- BCFSVSISUGYRMF-UHFFFAOYSA-N calcium;dioxido(dioxo)chromium;dihydrate Chemical compound O.O.[Ca+2].[O-][Cr]([O-])(=O)=O BCFSVSISUGYRMF-UHFFFAOYSA-N 0.000 claims description 6
- RMISVBXFFXBNAD-UHFFFAOYSA-N calcium;oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [Ca+2].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O RMISVBXFFXBNAD-UHFFFAOYSA-N 0.000 claims description 6
- CRGGPIWCSGOBDN-UHFFFAOYSA-N magnesium;dioxido(dioxo)chromium Chemical compound [Mg+2].[O-][Cr]([O-])(=O)=O CRGGPIWCSGOBDN-UHFFFAOYSA-N 0.000 claims description 6
- GIOZLVMCHDGNNZ-UHFFFAOYSA-N magnesium;oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [Mg+2].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O GIOZLVMCHDGNNZ-UHFFFAOYSA-N 0.000 claims description 6
- NDKWCCLKSWNDBG-UHFFFAOYSA-N zinc;dioxido(dioxo)chromium Chemical compound [Zn+2].[O-][Cr]([O-])(=O)=O NDKWCCLKSWNDBG-UHFFFAOYSA-N 0.000 claims description 6
- KHADWTWCQJVOQO-UHFFFAOYSA-N zinc;oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [Zn+2].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KHADWTWCQJVOQO-UHFFFAOYSA-N 0.000 claims description 6
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 claims description 5
- JHWIEAWILPSRMU-UHFFFAOYSA-N 2-methyl-3-pyrimidin-4-ylpropanoic acid Chemical compound OC(=O)C(C)CC1=CC=NC=N1 JHWIEAWILPSRMU-UHFFFAOYSA-N 0.000 claims description 5
- PXLIDIMHPNPGMH-UHFFFAOYSA-N sodium chromate Chemical compound [Na+].[Na+].[O-][Cr]([O-])(=O)=O PXLIDIMHPNPGMH-UHFFFAOYSA-N 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- PMJNEQWWZRSFCE-UHFFFAOYSA-N 3-ethoxy-3-oxo-2-(thiophen-2-ylmethyl)propanoic acid Chemical compound CCOC(=O)C(C(O)=O)CC1=CC=CS1 PMJNEQWWZRSFCE-UHFFFAOYSA-N 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 3
- JOSWYUNQBRPBDN-UHFFFAOYSA-P ammonium dichromate Chemical compound [NH4+].[NH4+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O JOSWYUNQBRPBDN-UHFFFAOYSA-P 0.000 claims description 3
- JQVALDCWTQRVQE-UHFFFAOYSA-N dilithium;dioxido(dioxo)chromium Chemical compound [Li+].[Li+].[O-][Cr]([O-])(=O)=O JQVALDCWTQRVQE-UHFFFAOYSA-N 0.000 claims description 3
- GLGSRACCZFMWDT-UHFFFAOYSA-N dilithium;oxido-(oxido(dioxo)chromio)oxy-dioxochromium Chemical compound [Li+].[Li+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O GLGSRACCZFMWDT-UHFFFAOYSA-N 0.000 claims description 3
- 238000002296 dynamic light scattering Methods 0.000 claims description 3
- 230000009477 glass transition Effects 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 56
- 238000011282 treatment Methods 0.000 description 51
- 239000000178 monomer Substances 0.000 description 29
- 239000001993 wax Substances 0.000 description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 25
- 229910052751 metal Inorganic materials 0.000 description 24
- 239000002184 metal Substances 0.000 description 24
- 150000003839 salts Chemical class 0.000 description 23
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- 125000004432 carbon atom Chemical group C* 0.000 description 16
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- 235000011114 ammonium hydroxide Nutrition 0.000 description 12
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- JJTUDXZGHPGLLC-UHFFFAOYSA-N lactide Chemical compound CC1OC(=O)C(C)OC1=O JJTUDXZGHPGLLC-UHFFFAOYSA-N 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
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- 239000000314 lubricant Substances 0.000 description 1
- 235000001055 magnesium Nutrition 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
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- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
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- 229940099596 manganese sulfate Drugs 0.000 description 1
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- 235000007079 manganese sulphate Nutrition 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 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
- 150000002734 metacrylic acid derivatives Chemical class 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M methacrylate group Chemical group C(C(=C)C)(=O)[O-] CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- 125000004184 methoxymethyl group Chemical group [H]C([H])([H])OC([H])([H])* 0.000 description 1
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 1
- 239000004200 microcrystalline wax Substances 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
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- BXWNKGSJHAJOGX-UHFFFAOYSA-N n-hexadecyl alcohol Natural products CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
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- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- UMRZSTCPUPJPOJ-KNVOCYPGSA-N norbornane Chemical compound C1C[C@H]2CC[C@@H]1C2 UMRZSTCPUPJPOJ-KNVOCYPGSA-N 0.000 description 1
- OEIJHBUUFURJLI-UHFFFAOYSA-N octane-1,8-diol Chemical compound OCCCCCCCCO OEIJHBUUFURJLI-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229940049964 oleate Drugs 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 1
- 150000001451 organic peroxides Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004209 oxidized polyethylene wax Substances 0.000 description 1
- 125000004043 oxo group Chemical group O=* 0.000 description 1
- 230000021962 pH elevation Effects 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- UCUUFSAXZMGPGH-UHFFFAOYSA-N penta-1,4-dien-3-one Chemical class C=CC(=O)C=C UCUUFSAXZMGPGH-UHFFFAOYSA-N 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-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
- 125000005007 perfluorooctyl group Chemical group FC(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)* 0.000 description 1
- NQFOGDIWKQWFMN-UHFFFAOYSA-N phenalene Chemical compound C1=CC([CH]C=C2)=C3C2=CC=CC3=C1 NQFOGDIWKQWFMN-UHFFFAOYSA-N 0.000 description 1
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 1
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 description 1
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- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
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- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
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- 235000011151 potassium sulphates Nutrition 0.000 description 1
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- 239000002243 precursor Substances 0.000 description 1
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- 230000002335 preservative effect Effects 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- VSVCAMGKPRPGQR-UHFFFAOYSA-N propan-2-one;sulfurous acid Chemical compound CC(C)=O.OS(O)=O VSVCAMGKPRPGQR-UHFFFAOYSA-N 0.000 description 1
- 229960000380 propiolactone Drugs 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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- 238000003908 quality control method Methods 0.000 description 1
- 238000007342 radical addition reaction Methods 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
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- 230000002441 reversible effect Effects 0.000 description 1
- WBHHMMIMDMUBKC-XLNAKTSKSA-N ricinelaidic acid Chemical compound CCCCCC[C@@H](O)C\C=C\CCCCCCCC(O)=O WBHHMMIMDMUBKC-XLNAKTSKSA-N 0.000 description 1
- 229960003656 ricinoleic acid Drugs 0.000 description 1
- FEUQNCSVHBHROZ-UHFFFAOYSA-N ricinoleic acid Natural products CCCCCCC(O[Si](C)(C)C)CC=CCCCCCCCC(=O)OC FEUQNCSVHBHROZ-UHFFFAOYSA-N 0.000 description 1
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- 238000007761 roller coating Methods 0.000 description 1
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- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- SNOOUWRIMMFWNE-UHFFFAOYSA-M sodium;6-[(3,4,5-trimethoxybenzoyl)amino]hexanoate Chemical compound [Na+].COC1=CC(C(=O)NCCCCCC([O-])=O)=CC(OC)=C1OC SNOOUWRIMMFWNE-UHFFFAOYSA-M 0.000 description 1
- BFXAWOHHDUIALU-UHFFFAOYSA-M sodium;hydron;difluoride Chemical compound F.[F-].[Na+] BFXAWOHHDUIALU-UHFFFAOYSA-M 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
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- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-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
- 150000003512 tertiary amines Chemical class 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- 150000005622 tetraalkylammonium hydroxides Chemical class 0.000 description 1
- 125000001712 tetrahydronaphthyl group Chemical group C1(CCCC2=CC=CC=C12)* 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
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical class [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical class [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 230000002110 toxicologic effect Effects 0.000 description 1
- 231100000723 toxicological property Toxicity 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 1
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- MXSVLWZRHLXFKH-UHFFFAOYSA-N triphenylborane Chemical compound C1=CC=CC=C1B(C=1C=CC=CC=1)C1=CC=CC=C1 MXSVLWZRHLXFKH-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 150000003672 ureas Chemical class 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- LXNOENXQFNYMGT-UHFFFAOYSA-N xi-5-Hydroxydodecanoic acid Chemical compound CCCCCCCC(O)CCCC(O)=O LXNOENXQFNYMGT-UHFFFAOYSA-N 0.000 description 1
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical class F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C23C22/00—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
- C23C22/05—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
- C23C22/06—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 acidic solutions with pH less than 6
- C23C22/48—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 acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/53—Treatment of zinc or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
本申请涉及一种用于处理锌或锌合金涂层的水性钝化组合物,所述组合物具有6.5至9的pH,并且基于组合物的重量,包含:5至60重量%的a)至少一种选自丙烯酸聚合物和非离子聚氨酯聚合物的基础聚合物;0.1至2.5重量%的b)三价Cr(III)离子,以Cr计算;c)抗坏血酸;0.1至2.5重量%的d)至少一种选自以下组中的铝化合物:氢氧化铝;偏氢氧化铝;三氯化铝;醇化铝;乙醇酸铝;三(β–酮)铝;三(β–酮酯)铝;铝皂;和羧酸铝;及最多10重量%的e)至少一种细碎蜡,其中所述组合物的特征在于,其基本上不含硝酸根阴离子并且基本上不含六价铬(Cr(VI))。
Description
技术领域
本发明涉及包含抗坏血酸的水性钝化组合物。更具体地,本发明涉及水性钝化组合物,其特征在于包含抗坏血酸、成膜聚合物和三价铬化合物。
背景技术
用金属(如锌)对基础金属基材进行涂覆或电镀以对该基础金属基材提供装饰性修整和/或腐蚀防护是本领域中早已确立的。当然,对经涂覆的和经电镀的基材的质量控制标准可能很苛刻,消费者因此将密切查看经处理的表面的光洁度和外观。考虑到基于锌和锌合金的保护涂层,被称为“白膜(wet storage stain)”的表面状况可能不美观,并且可能会损害基材的其它电镀或涂覆。这种也被称为“白锈”或“黑锈”(对于涂层)的白膜(stain)可归因于氧化锌和氢氧化锌的形成,并且在沉积的锌或锌合金暴露于大气氧气和湿气时产生。
消除新镀锌基材上的白膜的技术是已知的,并且尤其包括:双重涂层或粉末涂层的施用;蜡和油的施用,特别是对于片材、横梁和线材形式的基础金属基材;以及钝化处理。本发明涉及用钝化组合物处理锌涂层或镀层,该钝化组合物除了提供耐腐蚀性外,还可以提供各种颜色涂层(包括蓝色、黄色、橄榄色或黑色)以及对于后续染色和涂覆操作有效的基底。
现有技术的钝化组合物主要基于铬酸盐的酸性水溶液。在将酸性铬酸盐钝化溶液施用到经锌涂覆或电镀的基材上时,表面锌原子被氧化,以实际上形成水合碱式铬酸铬(Cr2O3CrO3·xH2O)与铬和锌二者的水合氧化物的界面层。然而,因为酸在氧化反应中被消耗,表面-液体界面处的pH会升高:这会降低水相中铬的结合力,并导致包含氢氧化铬以及铬离子与锌的络合物的凝胶状薄膜的沉淀。这种膜会一直堆积,直到酸质子不再能够接触锌金属,表面氧化还原反应因此停止:然后可以使所得的凝胶状膜硬化。
传统上,在钝化组合物中使用六价铬(Cr6+或Cr(VI))以提供存在于钝化膜或转化涂层中的铬。然而,铬(VI)的毒理学特性存在问题,尤其是EC指令2000/53/EC也强烈限制了含铬(VI)的钝化处理的使用。因此,本领域已经存在一些对用钝化组合物处理锌表面的关注,其中铬至少部分处于三价状态:在这方面可提及以下陈旧的公开内容:美国专利号2,559,878;美国专利号3,932,198;美国专利号3,647,569;美国专利号3,501,352;美国专利号4,359,345;美国专利号4,359,346;美国专利号4,359,347;美国专利号4,359,348;美国专利号4,349,392;美国专利号4,367,099;德国专利号DE 2526832;和英国专利号GB 1,461,244。在这些引用文献中使用的Cr(III)是无毒的,并且伴随的Cr(III)的废物去除不如六价铬那样昂贵。
前述专利中描述的铬(III)钝化组合物几乎不变地使用过氧化物型氧化剂,例如H2O2,一种必要的浴成分。这些氧化剂和类似的氧化剂(例如过硫酸盐)可以促进一些三价铬在转化涂层形成期间转化为六价铬。与此相关的另一个问题是过氧化物或过硫酸盐氧化剂的高消耗速率和损失,这就需要它们的频繁补充,而且需要仔细控制组合物的pH以避免伴随的pH升高。过氧化物(和过硫酸盐)化合物的消耗部分是由于存在各种活化金属离子(作为添加剂或污染物存在于溶液中),这些金属离子往往会催化氧化剂的分解。过氧化物和过硫酸盐化合物的频繁补充代表进行该钝化或转化过程的经济和精力成本。
当然,本领域已知基于铬酸盐(III)的钝化组合物,其不使用过氧化物或过硫酸盐型氧化剂。例如,美国专利号4,578,122A(Crotty)描述了不含过氧化物的酸性水溶液,其在用于处理接受金属表面以在其上赋予铬钝化膜的方法中使用。所描述的水溶液含有:铬离子,基本上所有铬离子都处于三价状态;氢离子,以提供约1.2至约2.5的pH;至少一种选自铁、钴、镍、钼、锰、镧、铈和镧系元素的另外的金属离子,所述离子以有效活化铬酸盐钝化膜形成的量存在;和作为必需氧化剂的硝酸根离子,所述硝酸根离子以提供至少4:1的硝酸根离子与铬离子和活化金属离子之和的摩尔比的量存在。硝酸根离子的量应进一步足以活化水合三价铬以在基材上形成铬酸盐膜。酸性水溶液可任选地进一步含有受控量的:硫酸根离子;卤素离子;有机羧酸;浴可溶和相容的硅酸盐化合物;和至少一种润湿剂。
美国专利号4,578,122的组合物中硝酸盐的存在被认为是非常不利的。这些盐在自发分解或预期氧化活性期间被转化成NOx,并且该NOx作为污染物扩散到大气中。
进一步认为,低pH钝化组合物在某些应用中也可能是有害的。特别地,低pH被认为会通过颗粒聚集使在组合物中作为成膜组分被包含的任何水性聚合物丙交酯(lactice)不稳定。此外,低pH钝化组合物可以促进基材表面的显著蚀刻,并且可以提供不稳定的钝化浴。
因此,在本领域中仍然需要开发包含成膜组分的酸性较小的钝化组合物,该组合物特别适用于涂覆有锌或锌合金的钢表面,并且其中化合物诸如铬酸盐(VI)、过氧化物、过硫酸盐和硝酸盐的水平可以被最小化,但其中这样开发的组合物中的这些化合物的减少不能通过组合物性能的下降来补偿。
发明内容
根据本发明的第一方面,提供一种用于处理锌或锌合金涂层的水性钝化组合物,所述组合物具有6.5至9的pH,并且基于组合物的重量,包含:
5至60重量%的a)至少一种选自丙烯酸聚合物和非离子聚氨酯聚合物的基础聚合物;
0.1至2.5重量%的b)三价Cr(III)离子,以Cr计算;
c)抗坏血酸;
0.1至2.5重量%的d)至少一种选自以下组中的铝化合物:氢氧化铝、偏氢氧化铝、三氯化铝、醇化铝、乙醇酸铝、三(β–酮)铝、三(β–酮酯)铝、铝皂、和羧酸铝;及
最多10重量%的e)至少一种细碎蜡,
其中所述组合物的特征在于,其基本上不含硝酸根阴离子并且基本上不含六价铬(Cr(VI))。该组合物优选进一步的特征在于,基本上不含过氧化物和过硫酸盐化合物。
例如,提供一种用于处理锌或锌合金涂层的水性钝化组合物,所述组合物具有7.0至8.5、优选7.0至8.0的pH,并且基于组合物的重量,所述组合物包含:
15至40重量%、优选20至35重量%的a)所述至少一种选自丙烯酸聚合物和非离子聚氨酯聚合物的基础聚合物;
0.1至2.0重量%、优选0.1至1.5重量%的b)所述Cr(III)离子,以Cr计算;
0.1至1.0重量%、优选0.1至0.5重量%的c)抗坏血酸;
0.1至2.0重量%、优选0.2至1.0重量%的d)所述至少一种选自以下组中的铝化合物:氢氧化铝、偏氢氧化铝、三氯化铝、醇化铝、乙醇酸铝、三(β–酮)铝、三(β–酮酯)铝、铝皂和羧酸铝;
1至8重量%、优选1至5重量%的e)所述蜡;及
10至50重量%、优选10至40重量%的水,
其中所述组合物的特征在于,其基本上不含硝酸根阴离子并且基本上不含六价铬(Cr(VI))。
上述三价铬离子可以通过选自以下的盐而在组合物中直接提供:硫酸铬(Cr2(SO4)3)、铬矾(KCr(SO4)2)、氯化铬(CrCl3)和溴化铬(CrBr3)、以及它们的混合物。
替代地或附加地,三价铬离子是通过还原作为一种或多种六价铬化合物提供的铬(VI)来获得的:该组合物然后将包含足以确保六价铬完全还原为三价铬的量的至少一种还原剂。在某些实施方案中,六价铬离子(Cr(VI))的来源可以选自:三氧化铬(CrO3)、铬酸锂(Li2CrO4)、重铬酸锂(Li2Cr2O7)、铬酸钠(Na2CrO4)、重铬酸钠(Na2Cr2O7)、铬酸钾(K2CrO4)、重铬酸钾(K2Cr2O7)、铬酸铵((NH4)2CrO4)、重铬酸铵((NH4)2Cr2O7)、铬酸镁(MgCrO4)、重铬酸镁(MgCr2O7)、铬酸钙(CaCrO4)、重铬酸钙(CaCr2O7)、铬酸锌(ZnCrO4)、重铬酸锌(ZnCr2O7)、以及它们的混合物。在该实施方案中,抗坏血酸应包含在组合物中以允许完全转化为三价Cr(III),并且应优选包含使得抗坏血酸:铬的摩尔比为1:3至4:5的量。
优选的是d)所述至少一种铝化合物选自三羧酸铝(Al(OOCR)3)、单羟基二羧酸铝(RCOO)2Al(OH)和二羟基单羧酸铝(RCOOAl(OH)2),其中R是C1-C8烷基。
在一个重要的实施方案中,如上文和所附权利要求中定义的钝化组合物可通过以下方式获得:将包含溶解在水中的作为组分b)的六价铬的部分与摩尔过量的根据组分c)的抗坏血酸混合,优选地其中抗坏血酸与铬的摩尔比在1:3至4:5的范围内;并且之后将组分a)、d)和e)加入到所述混合物中。
根据本发明的第二方面,提供一种将铬酸盐钝化膜赋予其至少一个表面上已施用锌或锌合金涂层的基材的方法,所述方法包括在20℃至90℃的温度下使基材的所述至少一个经涂覆的表面与上文和所附权利要求中定义的水性组合物接触足以在其上形成钝化膜的时间段。
根据本发明的第三方面,提供一种钝化基材,该钝化基材通过上文和所附权利要求中定义的方法获得。钝化基材已被证明提供有效的耐腐蚀性。
定义
如本文中所用,单数形式“一个(a)”、“一种(an)”和“该(the)”包括复数指代物,除非上下文另外明确指出。
如本文中所用,术语“包含(comprising)”、“包含(comprises)”和“包含(comprised of)”与“包括(including)”、“包括(includes)”、“含有(containing)”或“含有(contains)”同义,并且是包括性的或开放式的,并且不排除附加的非引用的成员、元素或方法步骤。如果使用,短语“由……组成”是封闭的,并排除所有附加元素。此外,短语“基本上由……组成”排除了附加的物质元素,但允许包含不实质上改变发明性质的非物质元素。
在量、浓度、尺寸和其他参数以范围、优选范围、上限值、下限值或优选的上下限值的形式表示时,应理解不论是否在上下文中明确提及所获得的范围,还具体公开了通过将任何上限值或者优选值与任何下限值或优选值组合可获得的任何范围。
词语“更好的”、“优选的”、“优选地”、“特别地”和“理想地”在本文中通常用于指代在某些情况下可以提供特定益处的本公开的实施方案。然而,一个或多个更好的、优选的、特别的或理想的实施方案的列举并不意味着其他实施方案没有用,并且不旨在将那些其他实施方案排除在本公开的范围之外。
如本申请中通篇使用的,词语“可以”是在允许的意义上使用的,即意味着有……的潜力,而不是在强制性意义上使用。
如本文所用,室温为23℃±2℃。
如本文所用,数均分子量(Mn)和重均分子量(Mw)是根据DIN 55672-1:2007-08,通过凝胶渗透色谱法(GPC)以四氢呋喃(THF)作为洗脱液测定的。术语多分散性(PD)由Mw和Mn导出,并计算为(Mw/Mn)。
如有说明,根据标准测试方法ASTM D4274-11分析羟基值。
组合物的粘度可以使用Brookfield粘度计(型号RVT)在20℃和50%相对湿度(RH)的标准条件下测量。粘度计使用已知粘度(其在5,000cps至50,000cps之间变化)的硅油进行校准。一组连接到粘度计的RV转子用于校准。钝化组合物的测量通过使用6号转子以20转/分钟的速度进行1分钟直到粘度计平衡而进行。然后使用校准来计算对应于平衡读数的粘度。
如本文所用,“玻璃化转变温度”(Tg)是根据DIN 53 765通过应用20K/min升温速率和中点测量的差示扫描量热法而测定的。
如本文所用,“d50粒径”是指粒径分布为使得至少50重量%的颗粒具有小于规定值的粒径直径。除非另有说明,否则粒径由激光衍射确定。
如本文所定义,术语“转化涂层”或“转化处理”是指使表面材料化学转化为不同材料的对基材的表面处理。
术语“钝化”是指在所述表面上形成对腐蚀条件的阻挡层,但在所述表面和钝化层之间没有形成化学键的内聚膜的对基材的表面处理。如本文中所用的术语“钝化组合物”是指实际上与经锌涂覆的或经锌合金涂覆的基材接触的那种组合物。如本领域已知的,这样的接触发生在所谓的“浴”中,所述浴的形状、尺寸和布置使得基材的至少部分能够浸入其中。此外,钝化浴的尺寸应允许组合物在负载的基材周围和在整个负载的基材移动,所述移动可以通过再循环和/或超声波被进一步增强。浴中组合物的pH、浴的温度和基材的接触时间是结果有效的变量,其应尽可能地手动或自动监测。
除非另外说明,否则在本文中给出关于“相对于铬”的摩尔比的情况下,这是指组合物中铬的总含量,与所述金属的氧化态无关。
如本文所用,术语“合金”是指由两种或更多种金属或者由金属和非金属组成的物质,所述两种或更多种金属或者所述金属和非金属通常通过熔融在一起并在熔化时溶解在彼此中而紧密结合。因此,术语“锌合金”表示其中锌金属是构成组分的合金,基于金属计,所述锌通常构成所述合金的至少40重量%、更通常至少50重量%或至少60重量%。可以与锌合金化的金属包括但不限于铝、锡、镍、钛和钴。在本文中,对于锌/铝合金,优选的是,基于金属计,锌构成所述合金的至少40重量%,并且相反地,基于金属计,铝构成所述合金的最多60重量%。
如本文所用,“矿物酸”是指源自一种或多种无机化合物的酸。矿物酸不是有机的,并且所有矿物酸在溶解于水中时都会释放氢离子。
如本文所用,“磷酸”是指具有式H3PO4的正磷酸,该酸通常可以浓度为最多75重量%H3PO4的水溶液的形式获得。如本文所用,“膦酸”是指具有式H3PO3的磷的含氧酸(oxoacid),其由经由单键与单个氢和两个羟基共价键合并且经由双键与氧共价键合的单个五价磷组成。
如本文所用,术语“α–羟基羧酸”是指具有至少一个羟基官能团的羧酸,其中所述羟基官能团占据所述酸的α–位(与羧酸官能团相邻的碳)。不排除占据分子中除了所述酸上的α–位以外的位置的羟基的存在。该α–羟基羧酸以游离酸的形式包含在本发明的组合物中。
如本文所用,术语“单体”是指可以进行聚合反应以对聚合物的化学结构贡献结构单元的物质。如本文所用,术语“单官能”是指具有一个可聚合部分。如本文所用,术语“多官能”是指具有多于一个可聚合部分。
如本文所用,术语“烯属不饱和单体”是指在自由基加成聚合的正常条件下能够聚合的含有末端双键的任何单体。
如本文所用,术语“活性氢化合物”是指包括至少一个可在水环境中容易解离的氢原子的化合物。优选地,氢原子连接到氮原子、氧原子、磷原子或硫原子。
如本文所用,“非离子聚氨酯”是不包含亲水可电离基团的聚氨酯。
如本文所用,“(甲基)丙烯酰基”是关于“丙烯酰基”和/或“甲基丙烯酰基”的简写术语。因此,术语“(甲基)丙烯酸酯”统指丙烯酸酯和甲基丙烯酸酯。
“烃基”在本文中以其为本领域技术人员所熟知的普通意义使用。
如本文所用,“C1-Cn烷基”基团是指含有1至n个碳原子的一价基团,其是烷烃的基团并且包括直链和支链有机基团。照此,“C1-C30烷基”基团是指含有1至30个碳原子的一价基团,其是烷烃的基团并且包括直链和支链有机基团。烷基的实例包括但不限于:甲基、乙基、丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基、正戊基、正己基、正庚基和2–乙基己基。在本发明中,这样的烷基可以是未取代的,或者可以被一个或多个卤素取代。在适用的情况下,将在说明书中注明对给定取代基的偏好。通常,在陈述条件“C1-C30烷基”的情况下,应注意优选的是含有1至18个碳原子的烷基(C1-C18烷基),例如含有1至12个碳原子的烷基(C1-C12烷基)或含有1至6个碳原子的烷基(C1-C6烷基)。
如本文所用,术语“C1-C18羟烷基”是指具有1至18个碳原子的HO–(烷基)基团,其中取代基的连接点是通过氧原子并且烷基是如以上所定义的。
“烷氧基”是指由–OA表示的一价基团,其中A是烷基:其非限制性实例是甲氧基、乙氧基和异丙氧基。如本文所用,术语“C1-C18烷氧基烷基”是指具有如上定义的烷氧基取代基的烷基,并且其中(烷基–O–烷基)部分总共包含1至18个碳原子:此类基团包括甲氧基甲基(–CH2OCH3)、2–甲氧基乙基(–CH2CH2OCH3)和2–乙氧基乙基。
如本文所用,术语“C2-C4亚烷基”定义为具有2至4个碳原子的饱和二价烃基。
术语“C3–C30环烷基”应理解为意指具有3至30个碳原子的饱和的、单环、双环或三环烃基。在本发明中,这样的环烷基可以是未取代的,或者可以被一个或多个卤素取代。通常,应注意优选的是含有3至18个碳原子的环烷基(C3-C18环烷基)。环烷基的实例包括:环丙基、环丁基、环戊基、环己基、环庚基、环辛基、金刚烷和降莰烷。
如本文中所用,单独使用或作为较大部分的一部分使用(如在“芳烷基”中一样)的“C6-C18芳基”基团是指单环、双环和三环体系,其中单环体系是芳族的,或者双环或三环体系中的环中的至少一个是芳族的。双环和三环环体系包括苯并稠合的2至3元碳环。在本发明中,这样的芳基可以是未取代的,或者可以被一个或多个卤素取代。示例性芳基包括:苯基;(C1-C4)烷基苯基,例如甲苯基和乙基苯基;茚基;萘基、四氢萘基、四氢茚基;四氢蒽基;和蒽基。并且可以注意对苯基的偏好。
如本文所用,“C2-C20烯基”是指具有2至20个碳原子和至少一个烯键式不饱和单元的烃基。烯基可以是直链、支链或环状的,并且可以任选地被一个或多个卤素取代。如本领域普通技术人员所理解的,术语“烯基”还包括具有“顺式(cis)”和“反式(trans)”构型,或者“E”和“Z”构型的基团。然而,通常应注意对含有2至10个(C2-10)或2至6个(C2-6)碳原子的未取代烯基的偏好。所述C2-C6烯基的实例包括但不限于:–CH=CH2;–CH=CHCH3;–CH2CH=CH2;–C(=CH2)(CH3);–CH=CHCH2CH3;–CH2CH=CHCH3;–CH2CH2CH=CH2;–CH=C(CH3)2;–CH2C(=CH2)(CH3);–C(=CH2)CH2CH3;–C(CH3)=CHCH3;
–C(CH3)CH=CH2;–CH=CHCH2CH2CH3;–CH2CH=CHCH2CH3;
–CH2CH2CH=CHCH3;–CH2CH2CH2CH=CH2;–C(=CH2)CH2CH2CH3;
–C(CH3)=CHCH2CH3;–CH(CH3)CH=CHCH;–CH(CH3)CH2CH=CH2;
–CH2CH=C(CH3)2;1–环戊–1–烯基;1–环戊–2–烯基;1–环戊–3–烯基;1–环己–1–烯基;1–环己–2–烯基;和1–环己–3–烯基。
如本文所用,“烷基芳基”是指烷基取代的芳基,并且“取代的烷基芳基”是指进一步带有一个或多个取代基(例如卤素、硝基、氰基、酰胺基、氨基、磺酰基、亚磺酰基、硫烷基(sulfanyl)、硫氧基(sulfoxy)、脲、硫脲、胺磺酰基、磺酰胺和羟基)的烷基芳基。此外,如本文所用,“芳烷基”意指被如上定义的芳基取代的烷基。
如本文中所用,术语“杂”是指含有一个或多个杂原子诸如N、O、Si和S的基团或部分。因此,例如“杂环”是指具有例如N、O、Si或S作为环结构的一部分的环状基团。“杂烷基”、“杂环烷基”和“杂芳基”部分分别是包含N、O、Si或S作为其结构的一部分的如上文所定义的烷基、环烷基和芳基。
本发明的组合物在本文中被限定为“基本上不含”某些化合物、元素、离子或其它类似组分。术语“基本上不含”旨在表示该化合物、元素、离子或其它类似组分不是被有意地添加到该组合物中,并且至多仅以痕量存在,所述痕量对涂层的所需特性没有(不利的)影响。示例性痕量按组合物的重量计小于1000ppm。术语“基本上不含”涵盖其中指定的化合物、元素、离子或其它类似组分完全不存在于组合物中或不以可通过本领域中通常使用的技术测量的任何量存在的那些实施方案。
具体实施方式
A:基础聚合物
本发明的组合物包含5至60重量%的a)至少一种选自丙烯酸聚合物和非离子聚氨酯聚合物的基础聚合物。优选的是组分a)构成组合物的15至40重量%,例如20至35重量%。
(A1):丙烯酸乳液聚合物
在一个实施方案中,可以包含一种或多种丙烯酸聚合物作为组合物的基础聚合物。优选的是,所包含的丙烯酸聚合物的特征在于以下中的至少一个:–30℃至60℃的玻璃化转变温度(Tg);和50000至500000道尔顿的重均分子量。
没有特别的意图限制从其衍生丙烯酸聚合物的组成单体。然而,优选的是,基于单体的总重量,至少70重量%、优选至少80重量%的从其衍生聚合物的单体是(甲基)丙烯酸酯单体。特别地,所述(甲基)丙烯酸酯单体可以根据下文给出的定义a1)至a3)。
a1)脂族和脂环族(甲基)丙烯酸酯单体
在一个实施方案中,聚合物可以包含a1)至少一种由式I表示的(甲基)丙烯酸酯单体:
H2C=CGCO2R1(I)
其中:
G是氢、卤素或C1-C4烷基;及
R1选自:C1-C30烷基;C2-C30杂烷基;C1-C18羟烷基;C3-C30环烷基;C2-C8杂环烷基;C2-C20烯基;和C2-C12炔基。
例如,R1可以选自C1-C18烷基、C2-C18杂烷基、C1-C18羟烷基、C3-C18环烷基、C2-C8杂环烷基、C2-C8烯基和C2-C8炔基。理想地,所述单体a1)的特征在于R1选自C1-C12烷基、C1-C6羟烷基和C3-C12环烷基。
根据式(I)的(甲基)丙烯酸酯单体a1)的实例包括但不限于:(甲基)丙烯酸甲酯;(甲基)丙烯酸乙酯;(甲基)丙烯酸丁酯;(甲基)丙烯酸己酯;(甲基)丙烯酸2–乙基己酯;(甲基)丙烯酸十二烷基酯;(甲基)丙烯酸月桂酯;(甲基)丙烯酸环己酯;(甲基)丙烯酸异冰片酯;(甲基)丙烯酸2–羟乙酯(HEMA);(甲基)丙烯酸2–羟丙酯;乙二醇单甲醚(甲基)丙烯酸酯;乙二醇单乙醚(甲基)丙烯酸酯;乙二醇单十二烷基醚(甲基)丙烯酸酯;二甘醇单甲醚(甲基)丙烯酸酯;(甲基)丙烯酸三氟乙酯;和(甲基)丙烯酸全氟辛酯。
a2)芳族(甲基)丙烯酸酯单体
在与上面给出的实施方案不相互排斥的另一实施方案中,聚合物可包含a2)至少一种由式II表示的(甲基)丙烯酸酯单体:
H2C=CQCO2R2(II)
其中:
Q可以是氢、卤素或C1-C4烷基;及
R2可以选自C6-C18芳基、C1-C9杂芳基、C7-C18烷芳基和C7-C18芳烷基。
根据式(II)的示例性(甲基)丙烯酸酯单体a2),其可以单独或组合使用,包括但不限于:(甲基)丙烯酸苄酯;(甲基)丙烯酸苯氧基乙酯;苯氧基二甘醇(甲基)丙烯酸酯;(甲基)丙烯酸苯氧基丙酯;和苯氧基二丙二醇(甲基)丙烯酸酯。
a3)(甲基)丙烯酸酯官能化低聚物
在再次不旨在与包括脂族和脂环族单体(a1)和芳族单体(a2)相互排斥的又一实施方案中,聚合物可包含a3)至少一种(甲基)丙烯酸酯官能化低聚物。所述低聚物可以具有一个或多个连接到低聚物主链的丙烯酸酯和/或甲基丙烯酸酯基团,这些(甲基)丙烯酸酯官能团可以位于低聚物上的末端位置中和/或可以沿着低聚物主链分布。
优选的是,所述至少一种(甲基)丙烯酸酯官能化低聚物:i)每分子具有两个或更多个(甲基)丙烯酸官能团;和/或ii)具有300至1000道尔顿的重均分子量(Mw)。
可单独或组合使用的此类低聚物的实例包括但不限于:(甲基)丙烯酸酯官能化氨基甲酸酯低聚物,例如(甲基)丙烯酸官能化聚酯氨基甲酸酯和(甲基)丙烯酸酯官能化聚醚氨基甲酸酯;(甲基)丙烯酸官能化聚环氧化物树脂;(甲基)丙烯酸官能化聚丁二烯;(甲基)丙烯酸多元醇(甲基)丙烯酸酯;聚酯(甲基)丙烯酸酯低聚物;聚酰胺(甲基)丙烯酸酯低聚物;和聚醚(甲基)丙烯酸酯低聚物。此类(甲基)丙烯酸酯官能化低聚物以及它们的制备方法尤其公开于:美国专利号4,574,138;美国专利号4,439,600;美国专利号4,380,613;美国专利号4,309,526;美国专利号4,295,909;美国专利号4,018,851;美国专利号3,676,398;美国专利号3,770,602;美国专利号4,072,529;美国专利号4,511,732;美国专利号3,700,643;美国专利号4,133,723;美国专利号4,188,455;美国专利号4,206,025;美国专利号5,002,976。在上述聚醚(甲基)丙烯酸酯低聚物中,具体实例包括但不限于:PEG 200DMA(n≈4);PEG 400DMA(n≈9);PEG 600DMA(n≈14);和PEG 800DMA(n≈19),其中指定的数字(例如400)表示分子的二醇部分的重均分子量。
本发明不排除聚合物a)衍生自不符合a1)、a2)和a3)的定义的烯属不饱和非离子单体。无意限制本发明,此类其他烯属不饱和非离子单体可包括:硅酮(甲基)丙烯酸酯单体,例如美国专利号5,605,999(Chu)所教导并要求保护的那些;含有3至5个碳原子的α,β–烯属不饱和单羧酸,例如丙烯酸、甲基丙烯酸、巴豆酸;巴豆酸的C1-C18烷基酯;含有4至6个碳原子的α,β–烯属不饱和二羧酸以及那些酸的酸酐、单酯和二酯;乙烯基酯,例如乙酸乙烯酯、丙酸乙烯酯和可从Shell Chemical Company获得的VEOVATM系列的单体;乙烯基卤化物和亚乙烯基卤化物;乙烯基醚,例如乙烯基乙醚;乙烯基酮,包括烷基乙烯基酮、环烷基乙烯基酮、芳基乙烯基酮、芳基烷基乙烯基酮和芳基环烷基乙烯基酮;芳族或杂环脂族乙烯基化合物;烷烃多元醇的聚(甲基)丙烯酸酯,例如乙二醇二(甲基)丙烯酸酯、丙二醇二(甲酯)丙烯酸酯、丁二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、己二醇二(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、甘油三(甲基)丙烯酸酯和季戊四醇四(甲基)丙烯酸酯;氧烷烃多元醇的聚(甲基)丙烯酸酯,例如二甘醇二(甲基)丙烯酸酯、二丙二醇二(甲基)丙烯酸酯、三甘醇二(甲基)丙烯酸酯、四甘醇二(甲基)丙烯酸酯、二丁二醇二(甲基)丙烯酸酯、二(戊二醇)二甲基丙烯酸酯;聚乙二醇二(甲基)丙烯酸酯;和双酚A二(甲基)丙烯酸酯,例如乙氧基化双酚A(甲基)丙烯酸酯(“EBIPMA”)。
其他烯属不饱和可聚合非离子单体的代表性实例包括但不限于:乙二醇二甲基丙烯酸酯(EGDMA);富马酸酐、马来酸酐和衣康酸酐、与C1-C4醇(例如甲醇、乙醇、丙醇、异丙醇、丁醇、异丁醇和叔丁醇)的单酯和二酯。乙烯基单体的代表性实例包括但不限于诸如以下的的化合物:乙酸乙烯酯;丙酸乙烯酯;乙烯基醚,例如乙烯基乙基醚;和乙烯基乙基酮。芳族或杂环脂族乙烯基化合物的代表性实例包括但不限于诸如以下的化合物:苯乙烯、α–甲基苯乙烯、乙烯基甲苯、叔丁基苯乙烯、2–乙烯基吡咯烷酮、5–亚乙基–2–降冰片烯和1–、3–和4–乙烯基环己烯。
如本领域已知的,丙烯酸基础聚合物可以在水溶性自由基引发剂的存在下并且在适当的加热下,通过水性乳液聚合方法由起始单体制备。聚合介质可以包括水和与水混溶的液体,例如C1-C4链烷醇,但优选仅由水组成。聚合温度可以在30℃至120℃,例如50℃至100℃的范围内:该温度不需要保持恒定,但可以在乳液聚合期间升高。
合适的自由基引发剂(其通常以基于所用单体的总重量在0.05至5重量%之间的量使用)包括:过氧化氢;烷基氢过氧化物,例如叔丁基氢过氧化物和氢过氧化枯烯;过硫酸盐,例如过硫酸铵、过硫酸钾和过硫酸钠;有机过氧化物,例如酰基过氧化物,包括过氧化苯甲酰;二烷基过氧化物,例如二叔丁基过氧化物;过氧酯,例如过苯甲酸叔丁酯;以及偶氮官能引发剂,例如偶氮双(异丁腈)(AIBN)、2,2'–偶氮双(2–甲基丁烷腈)(ANBN)和4,4'–偶氮双(4–氰基戊酸)。
上述过氧引发剂化合物在某些情况下可以有利地与合适的还原剂组合使用以形成氧化还原体系。作为合适的还原剂,可以提及:焦亚硫酸钠;焦亚硫酸钾;亚硫酸氢钠;硫酸氢钾;丙酮亚硫酸氢盐;羟基甲烷亚磺酸;和异抗坏血酸。诸如Fe.EDTA的金属化合物也可用作氧化还原引发剂体系的一部分。
本领域技术人员能够选择在自由基水性乳液聚合期间将引发剂添加到聚合容器中的合适方案。它既可以完全引入聚合容器,也可以根据其在自由基水性乳液聚合过程中的消耗连续或分阶段使用。优选地,一部分初始进料,剩余部分根据聚合的消耗来供应。
水性聚合通常在基于单体的总重量为0.1至5.0重量%乳化剂的存在下进行。优选使用非离子乳化剂,任选与阴离子乳化剂组合使用。作为合适的非离子乳化剂,可以提及具有5至50个环氧乙烷(EO)单元的直链或支链聚氧乙烯醇。作为合适的阴离子乳化剂,可以提及C1-C18烷基硫酸盐、C1-C18烷基磺酸盐和磷酸酯。
在根据本发明的乳液聚合中,通常获得固体含量大于60重量%的聚合物的水性分散体。此外,丙烯酸乳液聚合物应获得为具有单峰粒径分布,其特征在于水性分散体中聚合物颗粒的平均粒径(d50)为50至400nm,例如50至200nm。如所取得的水性分散体可以进一步加工,或者可以直接与其他组分混合以形成水性涂层组合物。
A2:非离子聚氨酯乳液聚合物
在另一备选方案中,并且如本领域已知的,合适的非离子聚氨酯可以由以下物质的反应获得:i)至少一种多元醇;ii)任选的其他活性氢化合物;和iii)至少一种多异氰酸酯化合物。应选择反应物的活性氢与NCO基团的当量比,以确保不存在游离NCO基团:因此当量比可以为至少1:1,优选为1:1至1.2:1。
如本文所用,“多元醇”是指含有两个或更多个羟基的任何化合物:因此,该术语旨在包括二醇、三醇和含有四个或更多个–OH基团的化合物。此外,所述至少一种反应物多元醇在本文中应选自:聚酯多元醇、聚醚多元醇和聚碳酸酯多元醇。多元醇应优选具有1000至50,000g/mol,例如1000至25,000g/mol的数均分子量(Mn)。作为该分子量表征的替代或附加,反应物多元醇的羟值应优选为20至850mg KOH/g,例如25至500mg KOH/g。
聚碳酸酯二醇可以通过使碳酸衍生物与二醇反应来获得。示例性碳酸衍生物是碳酸二芳基酯,包括但不限于碳酸二苯酯、碳酸二(C1-C6)烷基酯和光气。示例性二醇包括但不限于:乙二醇;1,2–丙二醇;1,3–丙二醇;1,3–丁二醇;1,4–丁二醇;1,5–戊二醇;1,6–己二醇;环己烷二甲醇;二甘醇;二丙二醇;新戊二醇;以及它们的混合物。
聚酯二醇可通过使二醇与脂族、芳族或脂环族二羧酸或在某些情况下与其相应的酸酐反应而获得:反应可任选在酯化催化剂存在下进行。合适的二羧酸的实例包括但不限于:己二酸;戊二酸;庚二酸;辛二酸;壬烷二羧酸;癸烷二羧酸;琥珀酸;马来酸;癸二酸;壬二酸;对苯二甲酸;间苯二甲酸;邻苯二甲酸;四氢邻苯二甲酸;六氢邻苯二甲酸;偏苯三酸;和1,4–环己烷二羧酸。合适的酸酐的实例包括琥珀酸酐、邻苯二甲酸酐和偏苯三酸酐。值得注意的是,各种市售的饱和(氢化)或不饱和形式的二聚脂肪酸也可以用作二羧酸。并且用于制备聚酯二醇的合适二醇的实例是:乙二醇;二甘醇、三甘醇或四甘醇;1,2–丙二醇;二丙二醇、三丙二醇、四丙二醇;1,3–丙二醇;1,4–丁二醇;1,3–丁二醇;2,3–丁二醇;1,6–己二醇;1,5–戊二醇;2,2–二甲基–1,3–丙二醇(新戊二醇);1,4–二羟基环己烷;1,4–二甲基环己烷;1,8–辛二醇;1,10–癸二醇;1,12–癸二醇;2,2,4–和/或2,4,4–三甲基–1,3–戊二醇;以及它们的混合物。
其他有用的聚酯二醇是可从含有2至12个碳原子的羟基羧酸或其内酯的二醇引发的聚合中获得的那些。羟基羧酸可以是饱和的或不饱和的、直链的或支链的,其实例包括:乙醇酸;乳酸;5–羟基戊酸;6–羟基己酸;蓖麻油酸;12–羟基硬脂酸;12–羟基十二烷酸;5–羟基十二烷酸;5–羟基癸酸;和4–羟基癸酸。合适的内酯的实例是β–丙内酯、δ–戊内酯、(C1-C6)烷基戊内酯、ε–己内酯和(C1-C6)烷基–ε–己内酯。
除此之外,优选的是,从其衍生聚氨酯的多元醇是聚醚多元醇,特别是多分散性(PD)小于2、优选小于1.5、更优选小于1.3的聚醚多元醇。为完整性起见,出于本发明的目的,“聚醚”被理解为其重复单元在主链中包含醚官能团C–O–C的聚合物。因此,具有侧醚基团的聚合物,例如纤维素醚、淀粉醚和乙烯基醚聚合物以及聚缩醛,不被该定义所覆盖。理想地,聚醚多元醇是聚氧化烯,特别是聚氧化(C2-C3)烯。
尤其如美国专利号3,905,929和美国专利号3,920,598所述,在反应物多元醇中存在聚氧化(C2-C3)烯链可以使水分散体中的非离子聚氨酯稳定化。这可以最小化或消除在分散体中包括乳化剂以提供非离子聚氨酯的外部稳定性的需要。
值得注意的是,在合成非离子聚氨酯时可以优选使用至少一种单醇作为进一步的活性氢反应物ii)。例如,可以将单官能亲水性聚氧化烯(例如聚氧化乙烯或聚氧化丙烯)掺入聚氨酯中,作为改变乳胶性能和提高其乳液形成容易性的手段。当存在时,基于反应物i)至iii)的重量,单醇以0.1至5重量%的量存在。
如本文所用,“多异氰酸酯”是指包含至少两个–N=C=O官能团的化合物,例如2至5个或2至4个–N=C=O官能团。合适的多异氰酸酯包括脂族、脂环族、芳族和杂环异氰酸酯、它们的二聚体和三聚体以及它们的混合物。
脂族和脂环族多异氰酸酯可以包含6至100个以直链连接或环化的碳原子,并且具有至少两个异氰酸酯反应性基团。合适的脂族异氰酸酯的实例包括但不限于直链异氰酸酯,例如亚乙基二异氰酸酯、三亚甲基二异氰酸酯、四亚甲基二异氰酸酯、1,6–六亚甲基二异氰酸酯(HDI)、八亚甲基二异氰酸酯、九亚甲基二异氰酸酯、十亚甲基二异氰酸酯、1,6,11–十一烷三异氰酸酯、1,3,6–六亚甲基三异氰酸酯、双(异氰酸基乙基)碳酸酯和双(异氰酸基乙基)醚。示例性脂环族多异氰酸酯包括但不限于二环己基甲烷4,4′–二异氰酸酯(H12MDI)、1–异氰酸基甲基–3–异氰酸基–1,5,5–三甲基–环己烷(异佛尔酮二异氰酸酯,IPDI)、环己烷1,4–二异氰酸酯、氢化亚二甲苯基二异氰酸酯(H6XDI)、1–甲基–2,4–二异氰酸基–环己烷、间–或对–四甲基二甲苯二异氰酸酯(m–TMXDI、p–TMXDI)和二聚脂肪酸二异氰酸酯。
术语“芳族多异氰酸酯”在本文中用于描述有机异氰酸酯,其中异氰酸酯基团直接连接到单核或多核芳烃基团的环上。单核或多核芳烃基团又指共轭双键的基本上平面的环状烃部分,其可以是单个环,或可以包括多个缩合(稠合)或共价连接的环。术语芳族也包括烷基芳基。通常,烃(主)链在一个环中包括5、6、7或8个主链原子。这种平面环状烃部分的实例包括但不限于环戊二烯基、苯基、萘基、[10]环烯基–(1,3,5,7,9–环癸五烯基–)、[12]环烯基–、[8]环烯基–、迫苯并萘(非那烯)、1,9–二氢芘、(1,2–苯并菲)。烷基芳基部分的实例是苄基、苯乙基、1–苯基丙基、2–苯基丙基、3–苯基丙基、1–萘基丙基、2–萘基丙基、3–萘基丙基和3–萘基丁基。
示例性芳族多异氰酸酯包括但不限于:甲苯二异氰酸酯(TDI)的所有异构体,其为异构纯形式或几种异构体的混合物的形式;萘–1,5–二异氰酸酯;二苯基甲烷4,4′–二异氰酸酯(MDI);二苯基甲烷2,4′–二异氰酸酯,和二苯基甲烷4,4′–二异氰酸酯与2,4′异构体的混合物或其与更高官能度低聚物的混合物(所谓的粗MDI);亚二甲苯基二异氰酸酯(XDI);二苯基二甲基甲烷4,4′–二异氰酸酯;二烷基和四烷基二苯基甲烷二异氰酸酯;二苄基4,4′–二异氰酸酯;亚苯基1,3–二异氰酸酯;和亚苯基1,4–二异氰酸酯。
在需要的情况下,多异氰酸酯可以通过通常已知的方法(例如在英国专利号889,050中描述的方法)进行缩二脲化和/或异氰脲酸酯化。还应注意,术语“多异氰酸酯”旨在包括通过上述脂族、脂环族、芳族和杂环异氰酸酯与多元醇的部分反应以获得异氰酸酯官能低聚物而形成的预聚物,该低聚物可单独使用或与游离异氰酸酯组合使用。
为了便于将它们包含在本发明的组合物中,所述至少一种非离子聚氨酯可以最初以水性分散体的形式提供,所述分散体的颗粒可以期望地以具有小于1微米,例如50至400nm的d50粒径(如通过动态光散射测量的)的单峰粒径分布为特征。
在水中形成聚氨酯分散体最好通过以下方式实现:i)在无水条件下或在有机溶剂存在下,由上述反应物首先形成具有游离NCO基团的预聚物;和ii),在以高内相比(HIPR)方法为例的连续方法中,或者在以反相方法为例的间歇方法中将预聚物分散在水相中。反应i)可以在催化下并且例如在25至100℃的温度下进行。所产生的预聚物的特征应优选为以下中的至少一个:i)基于预聚物重量计,5至30重量%、优选10至25重量%的NCO含量;ii)2.2至3.0、优选2.2或2.4至2.9的NCO官能度;iii)300至35,000mPa.s、优选1,000至10,000mPa.s的在20℃下的粘度;和,iv)500至30,000,例如500至15,000、或500至10,000g/mol的数均分子量(Mn)。为了完整性,这些特征i)至iv)并不旨在相互排斥:事实上,预聚物可以满足这些所述特征中的一个、两个、三个或四个。
本领域已知的标准聚氨酯催化剂包括:羧酸的亚锡盐,例如辛酸亚锡、油酸亚锡、乙酸亚锡和月桂酸亚锡;二羧酸二烷基锡,例如二月桂酸二丁基锡和二乙酸二丁基锡;叔胺;链烷醇胺化合物;2,3–二甲基–3,4,5,6–四氢嘧啶;氢氧化四烷铵;碱金属氢氧化物;碱金属醇化物;锡烷氧化物,例如二丁基二甲氧基锡、二丁基二苯氧基锡和二丁基二异丙氧基锡;锡氧化物,例如二丁基氧化锡和二辛基氧化锡;二丁基氧化锡和邻苯二甲酸酯的反应产物;硫醇锡;烷基钛酸盐;有机铝化合物,例如三乙酰丙酮铝、三乙基乙酰乙酸铝和二异丙氧基乙基乙酰乙酸铝;螯合化合物,例如四乙酰丙酮锆和四乙酰丙酮钛;有机硅钛化合物;三–2–乙基己酸铋;酸性化合物,例如磷酸和对甲苯磺酸;三苯基硼烷;三苯基膦;1,8–二氮杂双环十一碳–7–烯(DBU);1,5–二氮杂双环[4.3.0]壬–5–烯;1,4–二氮杂双环[2.2.2]辛烷;4–二甲氨基吡啶;1,5,7–三氮杂双环[4.4.0]癸–5–烯;7–甲基–1,5,7–三氮杂双环[4.4.0]癸–5–烯;1,8–双(四甲基胍基)萘;和2–叔丁基–1,1,3,3–四甲基胍。根据异氰酸酯的性质,所用催化剂的量通常在被催化的混合物的0.005至10重量%的范围内。
如前所述,预聚物可以任选地在溶剂存在下制备,并且在制备水性分散体之前或之后至少部分且优选全部除去溶剂。当使用溶剂时,不与异氰酸酯反应的溶剂的实例包括:酮,例如丙酮和丁酮;醚,例如四氢呋喃、二氧杂环己烷和二甲氧基乙烷;醚酯,例如乙酸甲氧基丙酯;(环状)酰胺和脲,例如二甲基甲酰胺和二甲基乙酰胺;N,N′–二甲基–2,5–二氮戊酮;N–甲基吡咯烷酮;和封端的二醇醚。这种溶剂可以在预聚物制备的任何阶段加入。
优选的是上述预聚物用扩链剂进行扩展。如本领域技术人员所知,典型的扩链剂具有18至500g/mol的重均分子量(Mw),并且具有至少两个活性含氢基团。特别地,多胺和/或水可以用作扩链剂,其中水和多胺的混合物是特别优选的。作为可以单独或组合使用的示例性多胺,可以提及:胺化聚丙二醇,例如Jeffamine D-400,可从Huntsman ChemicalCompany获得;肼;哌嗪;氨基乙基哌嗪;2–甲基哌嗪;1,5–二氨基–3–甲基戊烷;异佛尔酮二胺;乙二胺;二氨基丁烷;己二胺;六亚甲基二胺;四亚甲基四胺;氨基乙基丙基三甲氧基硅烷;二亚乙基三胺;三亚乙基四胺;三亚乙基五胺;乙醇胺;和赖氨酸。
在制备本发明的非离子聚氨酯聚合物中,使用除水(作为分散介质)以外的扩链剂,由扩链剂提供的活性氢与预聚物的NCO基团的当量比应选择为确保在最终聚氨酯中不存在游离NCO基团:因此当量比可为至少1:1,优选为1:1至1.2:1。
B:三价铬
基于组合物的重量,本发明的组合物包含0.1至2.5重量%的Cr(III)离子,以Cr计算。优选地,所述组合物将包含0.1至2.0重量%,例如0.1至1.5重量%的所述Cr(III)离子。
三价铬离子可以以浴可溶且相容的铬(III)化合物的形式直接引入钝化组合物中,盐诸如硫酸铬(Cr2(SO4)3)、铬矾(硫酸铬钾,KCr(SO4)2)、氯化铬(CrCl3)和溴化铬(CrBr3)特别适合于此目的。
在一个优选的替代方案中,通过用抗坏血酸还原水相中的六价铬离子,将铬(III)离子引入组合物中。可以单独或组合使用的示例性水溶性六价铬化合物包括:三氧化铬(CrO3);铬酸锂(Li2CrO4);重铬酸锂(Li2Cr2O7);铬酸钠(Na2CrO4);重铬酸钠(Na2Cr2O7);铬酸钾(K2CrO4);重铬酸钾(K2Cr2O7);铬酸铵((NH4)2CrO4);重铬酸铵((NH4)2Cr2O7);铬酸镁(MgCrO4);重铬酸镁(MgCr2O7);铬酸钙(CaCrO4);重铬酸钙(CaCr2O7);铬酸锌(ZnCrO4);和重铬酸锌(ZnCr2O7)。可以提及优选使用三氧化铬(CrO3)、铬酸钠(Na2CrO4)、重铬酸钠(Na2Cr2O7)、铬酸钾(K2CrO4)和重铬酸钾(K2Cr2O7)。特别是在使用三氧化铬的情况下获得良好的结果:该化合物在本领域中可以替代地称为无水铬酸。
C:抗坏血酸
如本文所用,术语“抗坏血酸”旨在包括化合物或其混合物的对映体形式。本发明的组合物包含抗坏血酸,该抗坏血酸必须添加到铬(Cr)中,其中要求首先引入到水性组合物中的所有六价铬转化为Cr(III)。然而,对于经处理的锌或锌合金涂覆的钢表面的外观,本文优选的是用于处理锌或锌金属涂层的组合物中的抗坏血酸:铝的摩尔比不大于1:1、更优选不大于1:2、尤其优选不大于1:3,但优选至少1:10、更优选至少1:5,其中铝的量优选来源于d)根据本发明的组合物的至少一种铝化合物,并因此来源于如下文进一步规定的组分D。
因此,在某些实施方案中,所述组合物的特征还可以在于基于所述组合物的重量,包含0.1至1.0重量%的抗坏血酸。优选地,所述组合物将包含0.1至0.5重量%的抗坏血酸。
为了完整性,本发明并不排除在组合物中存在无机还原剂,事实上,这可能有助于保证所添加的Cr(VI)的完全还原。合适的无机还原剂包括但不限于:碱金属碘化物;锡(II)化合物,例如SnSO4和SnCl2.2H2O;锑(III)化合物;亚铁盐,例如七水硫酸亚铁(HH)、一水硫酸亚铁(MH)和硫酸亚铁铵;二氧化硫;以及碱金属亚硫酸盐、亚硫酸氢盐和偏亚硫酸氢盐。
D:铝化合物
本发明组合物包含基于组合物的重量0.1至2.5重量%的至少一种铝化合物,所述铝化合物选自:氢氧化铝;偏氢氧化铝;三氯化铝;醇化铝(烷醇铝);乙醇酸铝;三(β–酮)铝;三(β–酮酯)铝;铝皂;和羧酸铝。优选的是所述组合物包含0.1至2.0重量%,例如0.2至1.0重量%的所述至少铝化合物。
可以用作醇化物配体的示例性醇化合物包括:C1-C8烷基醇,例如甲醇、乙醇、丙醇、异丙醇、丁醇、仲丁醇、异丁醇、叔丁醇、戊醇、异戊醇和叔戊醇;以及C1-C8醚醇,例如2–甲氧基乙醇、2–乙氧基乙醇、2–丁氧基乙醇、2–(2–甲氧基乙氧基)乙醇、2–甲氧基–1–甲基乙醇、2–甲氧基–1,1–二甲基乙醇、2–乙氧基–1,1–二甲基乙醇、2–异丙氧基–1,1–二甲基乙醇、2–丁氧基–1,1–二甲基乙醇、2–(2–甲氧基乙氧基)–1,1–二甲基乙醇、2–丙氧基–1,1–二乙基乙醇、2–仲丁氧基–1,1–二乙基乙醇和3–甲氧基–1,1–二甲基丙醇。
可以形成乙醇酸酯配体的示例性二醇化合物是C2-C8二醇化合物,包括:1,2–乙二醇;1,2–丙二醇;1,3–丙二醇;2,4–己二醇、2,2–二甲基–1,3–丙二醇;2,2–二乙基–1,3–丙二醇;1,3–丁二醇;2,4–丁二醇;2,2–二乙基–1,3–丁二醇;2–乙基–2–丁基–1,3–丙二醇;2,4–戊二醇;2–甲基–1,3–丙二醇;2–甲基–2,4–戊二醇;2,4–己二醇;和2,4–二甲基–2,4–戊二醇。
关于所述三(β–酮)铝,可以形成配体的示例性β–二酮化合物包括:C1-C8烷基取代的β–酮,例如乙酰丙酮、己烷–2,4–二酮、5–甲基己烷–2,4二酮、庚烷–2,4–二酮、2–甲基庚烷–3,5–二酮和2,6–二甲基庚烷–3,5–二酮;氟烷基取代的β–二酮,例如1,1,1–三氟戊烷–2,4–二酮、1,1,1–三氟–5,5–二甲基己烷–2,4–二酮、1,1,1,5,5,5–六氟戊烷–2,4–二酮和1,3–二全氟己基丙烷–1,3–二酮;和C1-C8醚取代的β–二酮,例如1,1,5,5–四甲基–1–甲氧基己烷–2,4–二酮、2,2,6,6–四甲基–1–甲氧基庚烷–3,5–二酮和2,2,6,6–四甲基–1–(2–甲氧基乙氧基)庚烷–3,5–二酮。
关于所述三(β–酮酯)铝,合适的配体包括但不限于C1-C8烷基丙二酸酯和C1-C8烷丙酮酸酯。铝皂包括但不限于单月桂酸铝、二月桂酸铝、三月桂酸铝、单豆蔻酸铝、二豆蔻酸铝、三豆蔻酸铝、单棕榈酸铝、二棕榈酸铝、三棕榈酸铝、单硬脂酸铝、二硬脂酸铝和三硬脂酸铝。
作为合适的羧酸铝,可以提到三羧酸铝(Al(OOCR)3)、单羟基(一元)二羧酸铝(RCOO)2Al(OH)和二羟基(二元)单羧酸铝(RCOOAl(OH)2),其中R是C1-C8烷基。具体但非限制性实例包括:一元甲酸铝、二元甲酸铝、三甲酸铝、一元乙酸铝、二元乙酸铝、三乙酸铝、一元丙酸铝、二元丙酸铝、三丙酸铝和三辛酸铝。
在一个优选的实施方案中,钝化组合物包含基于组合物的重量为0.1至2.5重量%的至少一种羧酸铝,所述羧酸铝选自三甲酸铝、三乙酸铝、三丙酸铝和三辛酸铝。可以提及的是,三乙酸铝是优选的。
E:蜡
本发明的组合物包含基于组合物重量最多10重量%的至少一种细碎蜡。例如,基于组合物的重量,组合物可以包含1至8重量%,例如1至5重量%或2至5重量%的所述蜡。
术语“蜡”是本领域技术人员已知的并且可以参考Ullmann'sEncyclopedia ofIndustrial Chemistry,6th Edition,Electronic Release(1998)中的定义。然而,无意限制本发明,示例性蜡包括:石蜡[CAS号8002-74-2];聚乙烯蜡[CAS号9002-88-4];聚乙烯-聚丙烯蜡;共聚聚乙烯蜡,例如乙烯与至少一种选自(甲基)丙烯酸、马来酸酐、乙酸乙烯酯和乙烯醇的单体的共聚物,这些共聚物可以例如CAS号38531-18-9、104912-80-3和219843-86-4获得;聚丁烯蜡;费托蜡;氧化蜡,例如氧化聚乙烯蜡[CAS号68441-17-8];极性改性聚丙烯蜡;微晶蜡,例如微晶石蜡[CAS号63231-60-7];褐煤蜡和褐煤蜡萃余液;褐煤酸及其盐和酯;脂肪酸酰胺,例如芥子酰胺[CAS号112-84-5]、油酰胺[CAS号301-02-0]和1,2–乙烯双(硬脂酰胺)[CAS号110-30-5];和巴西棕榈蜡。
优选的是,包含在本组合物中的任何蜡满足以下条件中的至少一个:i)小于200mgKOH/g、优选小于100mg KOH/g的酸值;ii)40至200℃、优选60至180℃的熔点;和,iii)至少200g/mol、优选至少400g/mol的数均分子量(Mn)。为了完整起见,这些条件并非相互排斥:蜡可能满足这些条件中的一个、两个或三个。
可以注意特别优选使用至少一种选自聚乙烯蜡、氧化聚乙烯蜡、聚丙烯蜡、氧化聚丙烯蜡和基于乙烯或丙烯的共聚蜡的蜡作为主要单体,其中所述至少一种蜡的进一步特征在于400至30 000g/mol、优选1000至25 000g/mol的数均分子量(Mn)。
为了便于将它们包含在本发明的组合物中,可以提供以下形式的蜡:i)以细碎粉末形式,特别是以特征在于通过激光衍射测量的d50粒径小于5微米的微粉化形式;和/或ii)以水性分散体的形式,所述分散体的颗粒的特征合意地在于通过动态光散射测量的小于1微米,例如20至500nm的d50粒径。
F:辅助成分
本发明的组合物通常进一步包含辅助材料,所述辅助材料必然是次要组分,但其仍然可以赋予这些组合物改善的性能。组合物中辅助材料的总量基于组合物的总重量为0至10重量%,优选为0.1至10重量%或0.1至7.5重量%。组合物的所需粘度通常决定所添加的辅助材料的总量,但上述钝化组合物的pH可能决定辅助酸性成分的添加量。
包括在此类辅助材料之中的是:氨;矿物酸;二价金属;水溶性或水分散性的氟代酸或其盐;腐蚀抑制剂,例如二烷基硫脲、正硫酸铜和硫酸铜;粘合促进剂;润湿剂;消泡剂;螯合剂;润滑剂;及其混合物。作为进一步的示例性腐蚀抑制剂,可提及以下商业材料:系列,可从JMN Specialties,Inc和Henkel Corporation获得;系列,可从Clariant AG获得;和系列,可从Akzo Nobel Surfactants LLC获得。
如前所述,本发明的组合物可以任选地包括氨(NH3)。优选地,基于组合物的重量,组合物将包含最多2重量%,例如0.1至2重量%、或0.2至1重量%的氨。为了完整起见,氨的组成重量是基于NH3计算的。氨将以氨溶液NH3(水的)的形式存在于本发明的水性组合物中,该氨溶液包含氨在水中的弱碱性溶液,其在本领域中可以称为氢氧化铵、氨水(ammoniawater)、液体氨(ammonia liquor)、氨水(aqua ammonia)、水合氨(aqueous ammonia)或简单的氨。虽然术语“氢氧化铵”暗示一种具有[NH4 +][OH-]组成的碱,但实际上不可能分离出NH4OH的样品,因为这些离子在氨溶液中不构成氨总量的很大一部分,除非是在极稀的氨溶液的情况下。
关于矿物酸的任选加入,硝酸的使用并不排除,但不是优选的;相反,加入磷酸、膦酸、亚硫酸、硫酸、盐酸和氢溴酸中的至少一种被认为是特别合适的。可以提到特别优选使用磷酸、膦酸、亚硫酸和硫酸中的至少一种。
钝化组合物可以进一步包含至少一种二价金属阳离子(M2+)。在优选的实施方案中,所述至少一种二价金属阳离子(M)选自:Mg2+、Ca2+、Mn2+、Co2+、Ni2+、Sr2+、Ba2+和Zn2+。上述金属离子或其混合物最方便地以金属氧化物、金属氢氧化物和/或可溶性和相容的金属盐(包括但不限于硫酸盐和卤化物盐)的形式引入组合物中。然而,不优选将硝酸盐和氟化物盐用于此目的。
在本发明的某些实施方案中,钝化组合物包含镁(Mg2+)和/或锰(Mn2+)。希望将这种镁和锰以以下物质中的一种或多种的形式引入水性钝化组合物中:氯化锰、硫酸锰、氧化镁、氢氧化镁、硫酸镁、以及氯化镁。可以注意到对氧化镁或氢氧化镁的偏好。
当存在时,基于组合物的重量,水性组合物中二价金属阳离子(M2+)的总量不应超过5重量%,优选不应超过2.5重量%。
钝化组合物可以任选地包含至少一种水溶性或水分散性的氟代酸或其盐,其中所述氟代酸是由以下经验通式(II)定义的:
HpTqFrOs(II)其中:
q和r中的每一个表示1至10的整数;
p和s中的每一个表示0至10的整数;及
T表示选自Ti、Zr、Hf、Si、Sn、Al、Ge和B的元素。
优选的经验式(II)的氟代酸包括以下化合物,其中:T选自Ti、Zr或Si;p为1或2;q为1;r为2、3、4、5或6;并且s为0、1或2。
本发明中使用的示例性氟代酸可以选自:氟钛酸(H2TiF6);氟锆酸(H2ZrF6);氟硅酸(H2SiF6);氟硼酸(HBF4);氟锡酸(H2SnF6);氟锗酸(H2GeF6);氟铪酸(H2HfF6);以及氟铝酸(H3AlF6)。优选的氟代酸是:氟钛酸(H2TiF6)和氟锆酸(H2ZrF6)。
在盐是水溶性或水分散性的条件下,上述氟代酸的一个或多个H原子可以被合适的阳离子(例如铵、碱土金属阳离子或碱金属阳离子)取代。碱金属阳离子和铵的盐在本文中是优选的,因此可以提及合适的氟代酸盐的以下实例:(NH4)2ZrF6、H(NH4)ZrF6、(NH4)2TiF6、H(NH4)2TiF6、Na2ZrF6、K2ZrF6、Li2ZrF6、Na2TiF6、K2TiF6、以及Li2TiF6。
这种盐可直接添加到所述组合物中,或可在水性钝化组合物中通过用适当的碱部分或完全中和酸性氟化物或酸性氟氧化物而原位产生。值得注意的是,所述碱在性质上可以是有机的或无机的:例如,可以使用碳酸氢铵和羟胺。
当氟代酸和矿物酸都存在时,氟代酸或其盐通常包含在组合物中,使得矿物酸与所述氟代酸的金属(T)的摩尔比在10:1至2:1、优选9:1至3:1、更优选8:1至4:1的范围内。当矿物酸的水平在上述范围之外时,制剂的稳定性降低:在所述范围内的较低水平的矿物酸下,可以通过增加组合物中二价金属阳离子的量来减轻制剂稳定性的伴随损失。当金属(T)的水平降至所述摩尔范围以下时,组合物的稳定性可能会受到实质性影响,但在中性盐雾(NSS)中可能会观察到性能下降。
在备选的但并非相互排斥的表达中,基于组合物的重量,氟代酸或其盐应以1至5重量%,例如1至2.5重量%的量包含在钝化组合物中。
钝化组合物中不排除存在其他络合的氟化物阴离子,在这方面可以提及:氟铟酸盐(例如InF4 -1);氟磷酸盐(例如PF6 -1);氟砷酸盐(例如AsF6 -1);氟锑酸盐(例如SbF6 -1);氟铋酸盐(例如BiF6 -1);氟硫酸盐(例如SF6 -2);氟硒酸盐(例如SeF6 -2);氟碲酸盐(例如TeF6 -2或TeOF5 -1);氟铜酸盐(例如CuF3 -1);氟银酸盐;氟锌酸盐(例如ZnF4 -2);氟钒酸盐(例如VF7 -2);氟铌酸盐(例如NbF7 -2);氟钽酸盐(例如TaF7 -2);氟钼酸盐(例如MoF6 -3);氟钨酸盐(例如WF6 -1);氟钇酸盐(例如YF6 -3);氟镧酸盐(例如LaF6 -3);氟铈酸盐(例如CeF6 -3或CeF6 -2);氟锰酸盐(例如MnF6 -2);氟高铁酸盐(例如FeF6 -3);氟镍酸盐;和氟钴酸盐。这种阴离子可以以水溶性盐或水分散性盐(特别是铵盐、碱土金属盐或碱金属盐)的形式包括。当存在时,所述络合的氟化物阴离子应以最多0.1摩尔/升,例如最多0.05摩尔/升的量包含在组合物中。
也不排除钝化组合物中存在未以络合形式结合的游离氟离子,因为氟阴离子可以在钝化涂层的形成中起到促进剂的作用,并且存在于转化涂层和金属基体之间的界面处。这样的游离氟化物阴离子可以通过将以下物质添加到钝化组合物中而被包括,例如:氢氟酸、碱金属氟化物,例如氟化钠、碱金属氢氟化物,例如氟化氢钠、氟化铵、以及氟化氢铵。
除此之外,游离氟离子的存在(不以络合形式结合)是不优选的。尽管氟化物物种在钝化组合物中的使用,但氟化物的环境释放是有问题的,如https://www.cdc.gov/niosh/所记录的。因此,优选的是钝化组合物基本上不含游离的氟化物阴离子。
基于组合物的重量,钝化组合物可以包括最多2.5重量%,例如0.1至2.5重量%的非离子表面活性剂。虽然其他非离子表面活性剂在本发明中可能有用,但可以提及的是,特别优选使用脂肪醇乙氧基化物,其实例包括乙氧基化月桂醇、硬脂醇、山嵛醇和油基鲸蜡醇。
更进一步地,本发明的组合物可以任选地包含至少一种由以下通式(III)表示的α–羟基羧酸:
R1CH(OH)COOH(III)其中:R1表示氢原子、C1-C4烷基、C2-C6烯基、C1-C6烷氧基、C3-C6环烷基或C6-C10芳基。在适用的情况下,R1可以任选地被一个或多个选自以下的基团取代:卤素;氧代基;或–COOH。
合适的α–羟基羧酸包括但不限于:乙醇酸;乳酸(2–羟基丙酸);2–羟基丁酸;2–羟基戊酸;2–羟基己酸;葡萄糖醛酸;柠檬酸;扁桃酸;半乳糖醛酸;核糖酸(2,3,4,5–四羟基戊酸);葡萄糖酸(2S,3S,4R,5S)–2,3,4,5,6–五羟基己酸;丙醇二酸;酒石酸;和苹果酸。
在一个实施方案中,所述至少一种α–羟基羧酸选自:乙醇酸;葡萄糖酸;乳酸(2–羟基丙酸);2–羟基丁酸;2–羟基戊酸;和2–羟基己酸。更特别地,涂层组合物的α–羟基羧酸应包括葡萄糖酸或由葡萄糖酸组成。
为了完整性,再次注意到钝化组合物的上述pH在某种程度上决定这种α–羟基羧酸的添加量。当在该pH限制范围内添加时,α–羟基羧酸通常应以最多0.1摩尔/升,例如最多0.05摩尔/升的量包含在水性钝化组合物中。
人们认为,所公开的钝化组合物以及由此产生的钝化膜的防腐性能可以通过在其中掺入过渡金属盐和/或过渡金属络合物来增强。在这方面被认为特别有用的是选自Ce、Ni、Co、V、Fe、Zn、Zr、Mn、Mo、W、Ti、Zr,Hf、Bi和镧系元素的过渡金属的盐或络合物。
虽然所述过渡金属可以以上文提及的络合氟化物阴离子存在,但这些过渡金属替代地或另外以与其它配体的络合物的形式和/或以与其它阴离子的盐的形式包含在组合物中,条件是所述盐至少部分溶于水。作为阴离子的实例,可以提及:氧化物;氢氧根;硫酸根;氯离子;碘离子;柠檬酸根;乳酸根;琥珀酸根;甲酸根;草酸根;丙二酸根;和乙酸根。作为过渡金属络合物的示例性配体,可以提及:乙二胺四乙酸(EDTA);二亚乙基三胺五乙酸(DTPA);羟乙基乙二胺三乙酸(HEDTA);次氮基三乙酸(NTA);以及甲基甘氨酸二乙酸(MGDA)。
钝化组合物的制备
通过简单混合各种组分以及任何辅助成分来配制水性钝化组合物。虽然组分的混合顺序不受限制,但在混合所述分散体和其它组分之前,可以谨慎地首先形成基础聚合物和/或蜡的水性分散体。在这种情况下,丙烯酸聚合物、非离子聚氨酯和蜡的水分散体可以例如以45至60重量%的固体含量制备。此外,还可以谨慎地进行将溶解在水中的任何六价铬(Cr(VI))源与抗坏血酸混合的初步步骤:这种含有通过还原获得的Cr(III)离子的前体溶液可以与其他原始的分散或溶解的成分混合以形成最终的水性组合物。
如果需要,组合物可以在其施用之前很好地制备。然而,在令人感兴趣的替代实施方案中,浓缩的钝化组合物可以首先通过将各组分与仅一部分的在所施用的钝化组合物中会存在的水混合而获得;然后可以将浓缩的钝化组合物在其施用之前不久用剩余的水稀释。据认为,这种浓缩组合物要么可以作为单包装浓缩物(其可以通过仅用水稀释而转化)制备和储存,要么可以作为多部分浓缩物(必须将其中的两种或更多种混合并稀释以形成根据本发明的完整工作组合物)制备和储存。任何稀释都可以简单地通过在混合下添加水(特别是去离子水和/或软化水)来实现。该组合物可以同样地在冲洗流中制备,由此将一种或多种浓缩物流注入连续的水流中。
在没有特别意图限制钝化组合物中包含的水的量的情况下,优选的是,基于所述组合物的重量,所述组合物包含10至50重量%、优选10至40重量%、更优选地20至40重量%的水。在替代性但非互斥的表征中,钝化组合物可以由使用布氏粘度计在25℃下测量的0.005至1Pa.s(50cps至1000cps)的粘度来限定。
方法和应用
虽然本发明涉及对锌或锌合金的表面的钝化,但不意图限制可能已经施用锌或锌合金的基础基材,也不意图限制这种施用的方法。因此,合适的基础金属基材可以包括但不限于铁、镍、铜、铝及其合金:可以特别提及包含钢或由钢组成的基材。这些金属和合金可以以各种形式提供,包括片材、板、立方体、球体、环形、实心圆柱体、管和线材:当然不排除以更复杂、成形的形式(通过常规技术诸如弯曲、冲裁、铸造、锻造、轧制和焊接获得)提供基材。而且,可以通过以下方法将锌或锌合金的镀层或涂层施用到这些基础基材上:电镀;镀锌,包括热浸镀锌和热扩散镀锌;和镀锌层退火处理(galvannealing)。仅作为示例,本发明的钝化组合物和方法可用于处理:满足ASTM Designation A653要求的镀锌和镀锌层扩散处理钢;一种可从Bethlehem Steel Corporation获得的经55%Al/43.4%Zn/1.6%Si合金涂覆的钢板;以及一种可从Weirton SteelCorporation获得的经5%Al/95%Zn合金涂覆的钢板。
根据本发明的方法方面,常常可取的是将异物从经涂覆或镀覆的金属基材上通过对有关表面进行清洁和脱脂而去除。这样的处理是本领域中已知的,并且可以以单阶段或多阶段方式进行,所述方式通过例如使用以下中的一种或多种构成:含水碱性脱脂浴;含水清洁乳液;清洁溶剂,例如四氯化碳或三氯乙烯;以及水冲洗,优选去离子或软化水的水冲洗。在使用含水碱性脱脂浴的那些情况下,任何残留在表面上的脱脂剂都应理想地通过用去离子水或软化水冲洗基材表面而去除。无论所施用的清洁剂或脱脂剂,经如此处理的基材不应在钝化处理之前或所述钝化处理之前的任何后续预处理步骤之前经受中间干燥步骤。
因此如上所暗示的,本发明不排除对锌或锌合金表面的预处理,与清洁和/或脱脂步骤的实施无关。这样的预处理是本领域已知的,这方面可以参考:德国专利申请号DE 19733 972A1;德国专利申请号DE 10 2010 001 686A1;德国专利申请号DE 10 2007021364A1;和美国专利申请号2014/360630。特别地,表面可以用底漆处理,目的是促进钝化膜的后期粘附。
在所述清洁、脱脂和/或预处理步骤之后,将钝化组合物施用于基材。钝化组合物可以在环境温度下施用,或者钝化组合物的温度可以在施用之前升高到例如30℃至90℃范围内的温度,例如30℃至70℃。
为了生产双面镀板,商业上常规的是制备如上所述的操作浴,并且将钝化组合物通过但不限于浸渍、溢流、空气雾化喷涂、空气辅助喷涂、无气喷涂、大容量低压喷涂和空气辅助无气喷涂而施用于基材。组合物与基材的最小接触时间最宽泛地是足以在其上形成所需钝化膜的时间:在其中对将要冷加工的金属进行钝化或转化处理的情况下,接触时间可以短至1秒或长至15分钟;然而,取决于所施用溶液的pH和浓度,5至300秒、例如5至50秒的接触时间是更典型的。
在某些情况下,只需要在基材的单个表面上形成钝化膜。在本发明的背景下,钝化膜可以仅施用于钢基材的经电镀的表面,该经电镀的表面将形成燃料箱的内侧,即接触储存在其中的燃料的一侧:在这种经电镀的钢基材的内表面和外表面上形成钝化膜可能对该基材的后续可焊性有害。将钝化组合物仅施用于单个表面的技术包括但不限于:涂漆;刷涂;辊涂;擦拭;空气雾化喷涂;空气辅助喷涂;无气喷涂;大容量低压喷涂;以及空气辅助无气喷涂。
在施用步骤结束时,使用例如环境空气干燥、循环暖空气、强制空气干燥或红外加热来干燥制品。基材的表面温度在干燥期间受到控制:峰值金属温度(PMT)不需要超过100℃,并且更特别地,应在20至90℃的范围内,例如50至75℃。
干燥之后,不排除使该制品经受:至少一种水冲洗以从中除去残留的钝化组合物;和/或用硅酸盐稀溶液冲洗。可将经冲洗的基材在一个或多个冲洗步骤完成后或在每种冲洗溶液之后(如果适用)干燥。
上述处理应合意地在锌或锌合金上产生保护性钝化单层,该单层具有25至500mg/m2、优选25至250mg/m2或25至100mg/m2的膜重。如果膜量小于25mg/m2,则钝化膜可能赋予不充分的耐腐蚀性。如果膜量大于500mg/m2,则钝化膜对表面的粘附力将不足,使得在基材的进一步处理期间可能发生涂层的剥离。
根据本发明的组合物产生颜色为无色、或蓝色或橄榄色的钝化膜,所述膜具有平坦至有光泽的光洁度。该光洁度的确切性质主要由基础基材、锌或锌合金涂料和在转化涂层组合物中的浸渍时间决定。根据本发明钝化的锌或锌合金涂层在观察到的白锈腐蚀开始前至少250小时内显示出腐蚀防护,如ASTM B-201所定义。替代地或另外地,当根据ASTMB-117的方法在稳态条件下用中性盐雾(NSS,5重量%NaCl,95重量%H2O)处理时,根据本发明钝化的所述锌或锌合金涂层在观察到的白锈腐蚀开始前至少250小时内显示出腐蚀防护(如ASTMB-201所定义)。
本发明不排除对根据本发明获得的钝化膜施用补充转化涂层;实际上,这种补充涂层可以进一步延长最终制品的腐蚀防护。可以提及基于硅酸盐的无机涂层和基于环氧树脂的有机转化涂层作为补充转化涂层的非限制性实例:在这方面尤其可以参考美国专利号5,743,971(Inoue)和美国专利号5,855,695(McMillen)。这些补充转化涂层可以通过本领域已知的任何合适的方式施用,例如通过浸涂、喷涂、辊涂、电涂或粉末涂覆。
在以下实施例中描述本公开的各种特征和实施方案,其旨在是代表而非限制性的。
实施例
在实施例1中使用代表根据本发明的组合物的以下商业和主要产品:氨溶液:25%的氨在水中的溶液丙烯酸乳液:Acrystar HP Cresta,购自EOC Tailor Made PolymersIndia Ltd.润湿剂/偶联剂:Rhodoline WA 40,购自Solvay Group
聚乙烯蜡:Aquaslip 671,购自The Lubrizol Corporation
抗菌剂:BYK 331,购自BYK Altana Group
消泡剂:Timet W 288S
通过混合以下表1中给出的成分来制备水性钝化组合物:
表1
此外,作为对比实施例,提供从GTZ India Private Ltd.获得的商业制剂QUALACTM3732。该组合物是基于铬(III)化合物和苯乙烯-丙烯酸酯共聚物水乳液:该商业制剂不含抗坏血酸。
标准测试板制备:将Advanced Coating Technology(ACT)G-90热浸镀锌钢的试件机械切割成4cm×4cm尺寸的正方形。将每个获得的板用碱性清洁剂在55℃下处理10秒,用自来水在室温下冲洗,然后通过刮擦干燥。通过辊涂机将选择用于评价的每种钝化组合物施用于所述板的一个表面:由根据本发明的水性钝化组合物制备九个板;针对每种参考钝化组合物制备一式四份的板。然后将所得的涂覆的测试板烘烤至在下文表2中给出的峰值金属温度(PMT)。所获得的测试板的涂层重量是在金属的基础上确定的,并且也在表2中给出。
基于这些制成表的水性组合物,使用本发明的水性钝化组合物和参考组合物进行以下测试。
摩擦系数测试:在适用的情况下,根据ASTM G115用于测量和报告摩擦系数的标准指南(Standard Guide for Measuring and Reporting Friction Coefficients),对(经涂覆)的板测试该参数。未涂覆的钢G-90热浸镀锌钢(μ)板具有0.35至0.4的摩擦系数。
中性盐雾(NSS):该测试根据ASTM B117用5%NaCl溶液于35℃下进行(https://www.astm.org/Standards/B117)。将经涂覆的板在喷雾室(ERICHSEN 606/400L型)中以与垂直方向成15–30°放置96小时,并且如果适用放置500小时。不允许测试板接触所述室中的其它表面,并且不允许它们的表面上的冷凝或腐蚀产物相互交叉污染。每24小时对测试板进行照相记录。暴露后,将测试板在去离子水中冲洗,以从它们的表面除去盐沉积物,然后立即干燥。500小时后对经涂覆的板进行目视检查:
表2
测试 | 对比例 | 实施例1 |
外观 | 绿色至蓝色液体 | 绿色至蓝色液体 |
pH | 6.3 | 7.5 |
固体含量(%) | 35.0 | 29.5 |
比重(23℃) | 1.06 | 1.03 |
金属峰值温度(℃) | 80–85 | 80–85 |
摩擦系数(μ) | 0.11 | 0.11 |
总涂层重量(gm-2/侧) | 1.5–1.8 | 1.5–1.8 |
NSS(96小时) | 一些白锈和观察到的斑点 | 无白锈,无观察到的斑点 |
NSS(500小时) | 停止使用 | 按面积计小于5%锈 |
鉴于前述描述和实施例,本领域技术人员明白在不脱离权利要求的范围的情况下可以对其进行等效修改。
Claims (15)
1.用于处理锌或锌合金涂层的水性钝化组合物,所述组合物具有6.5至9的pH,并且基于所述组合物的重量,所述组合物包含:
5至60重量%的a)至少一种选自丙烯酸聚合物和非离子聚氨酯聚合物的基础聚合物;
0.1至2.5重量%的b)三价Cr(III)离子,以Cr计算;
c)抗坏血酸;
0.1至2.5重量%的d)至少一种选自以下组中的铝化合物:氢氧化铝、偏氢氧化铝、三氯化铝、醇化铝、乙醇酸铝、三(β–酮)铝、三(β–酮酯)铝、铝皂、和羧酸铝;及
最多10重量%的e)至少一种细碎蜡,
其中所述组合物的特征在于,其基本上不含硝酸根阴离子并且基本上不含六价铬(Cr(VI))。
2.根据权利要求1所述的组合物,所述组合物具有7.0至8.5、优选7.0至8.0的pH,并且基于所述组合物的重量,所述组合物包含:
15至40重量%、优选20至35重量%的a)所述至少一种选自丙烯酸聚合物和聚氨酯聚合物的基础聚合物;
0.1至2.0重量%、优选0.1至1.5重量%的b)所述Cr(III)离子,以Cr计算;
0.1至1.0重量%、优选0.1至0.5重量%的c)抗坏血酸;
0.1至2.0重量%、优选0.2至1.0重量%的d)所述至少一种选自以下组中的铝化合物:氢氧化铝、偏氢氧化铝、三氯化铝、醇化铝、乙醇酸铝、三(β–酮)铝、三(β–酮酯)铝、铝皂、和羧酸铝;
1至8重量%、优选1至5重量%的e)所述蜡;及
10至50重量%、优选10至40重量%的水,
其中所述组合物的特征在于,其基本上不含硝酸根阴离子并且基本上不含六价铬(Cr(VI))。
3.根据权利要求1或2所述的组合物,其中作为基础聚合物被包含的所述或每种丙烯酸聚合物的特征在于以下中的至少之一:–30℃至60℃的玻璃化转变温度、和50000至500000道尔顿的重均分子量(Mw)。
4.根据权利要求1至3之一所述的组合物,其中所述至少一种基础聚合物分散在所述组合物中,并且具有单峰粒径分布,其特征在于水性分散体中聚合物颗粒的平均粒径(d50)为50至400nm。
5.根据权利要求1至4之一所述的组合物,其中所述铬(III)离子是通过还原作为一种或多种六价铬化合物提供的铬(VI)而获得的。
6.根据权利要求5所述的组合物,其中所述提供的六价铬化合物选自以下组中:三氧化铬(CrO3)、铬酸锂(Li2CrO4)、重铬酸锂(Li2Cr2O7)、铬酸钠(Na2CrO4)、重铬酸钠(Na2Cr2O7)、铬酸钾(K2CrO4)、重铬酸钾(K2Cr2O7)、铬酸铵((NH4)2CrO4)、重铬酸铵((NH4)2Cr2O7)、铬酸镁(MgCrO4)、重铬酸镁(MgCr2O7)、铬酸钙(CaCrO4)、重铬酸钙(CaCr2O7)、铬酸锌(ZnCrO4)、重铬酸锌(ZnCr2O7)、以及它们的混合物。
7.根据权利要求5所述的组合物,其中所述提供的六价铬化合物选自以下组中:三氧化铬(CrO3)、铬酸钠(Na2CrO4)、重铬酸钠(Na2Cr2O7)、铬酸钾(K2CrO4)、重铬酸钾(K2Cr2O7)、以及它们的混合物。
8.根据权利要求1至7之一所述的组合物,其中抗坏血酸:铝的摩尔比不大于1:1,优选为不大于1:2,更优选为不大于1:3,其中铝的量优选来源于所述组合物的d)所述至少一种铝化合物。
9.根据权利要求1至8之一所述的组合物,其中d)所述至少一种铝化合物选自三羧酸铝(Al(OOCR)3)、单羟基二羧酸铝((RCOO)2Al(OH))和二羟基单羧酸铝(RCOOAl(OH)2),其中R是C1-C8烷基。
10.根据权利要求1至9之一所述的组合物,其中包含在本发明组合物中的e)所述蜡或每种蜡满足以下条件中的至少之一:
小于200mg KOH/g、优选小于100mg KOH/g的酸值;
40至200℃、优选60至180℃的熔点;及
至少200g/mol、优选至少400g/mol的数均分子量(Mn)。
11.根据权利要求1至10之一所述的组合物,其中所述组合物中包含的e)所述蜡或每种蜡以微粉化形式提供或者作为水性分散体提供,所述微粉化形式的特征在于通过激光衍射测量的d50粒径小于5微米,所述分散体的颗粒的特征在于通过动态光散射测量的d50粒径小于1微米。
12.根据权利要求1至11之一所述的组合物,其中所述组合物的特征在于基本上不含过氧化物和过硫酸盐化合物。
13.根据权利要求1至12之一所述的组合物,其可如下获得:
将包含溶解在水中的作为组分b)的六价铬的部分与根据组分c)的抗坏血酸混合,优选地其中抗坏血酸与铬的摩尔比为1:3至4:5;并且之后;
将所述组分a)、d)和e)加入到所述混合物中。
14.赋予基材以铬酸盐钝化膜的方法,其中所述基材在其至少一个表面上已施用锌或锌合金涂层,所述方法包括在20℃至90℃的温度下使所述基材的所述至少一个经涂覆的表面与根据权利要求1至13之一所限定的水性组合物接触足以在其上形成钝化膜的时间段。
15.通过根据权利要求14所限定的方法获得的钝化基材。
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