CN107488844A - 一种用于镀锡钢板的无氟无铬钝化液及其使用方法 - Google Patents
一种用于镀锡钢板的无氟无铬钝化液及其使用方法 Download PDFInfo
- Publication number
- CN107488844A CN107488844A CN201610405914.5A CN201610405914A CN107488844A CN 107488844 A CN107488844 A CN 107488844A CN 201610405914 A CN201610405914 A CN 201610405914A CN 107488844 A CN107488844 A CN 107488844A
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- free
- chromium
- fluoride
- passivating solution
- tin plate
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Links
- 239000005028 tinplate Substances 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 238000002161 passivation Methods 0.000 claims abstract description 26
- 239000008139 complexing agent Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 150000001875 compounds Chemical class 0.000 claims abstract description 15
- 150000003608 titanium Chemical class 0.000 claims abstract description 15
- 239000007800 oxidant agent Substances 0.000 claims abstract description 13
- 230000001590 oxidative effect Effects 0.000 claims abstract description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011574 phosphorus Substances 0.000 claims abstract description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 12
- 238000005507 spraying Methods 0.000 claims abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 229910019142 PO4 Inorganic materials 0.000 claims description 6
- 239000010452 phosphate Substances 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 3
- HHDOORYZQSEMGM-UHFFFAOYSA-L potassium;oxalate;titanium(4+) Chemical compound [K+].[Ti+4].[O-]C(=O)C([O-])=O HHDOORYZQSEMGM-UHFFFAOYSA-L 0.000 claims description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 3
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 2
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 2
- 239000004471 Glycine Substances 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 claims description 2
- 229940006460 bromide ion Drugs 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 230000000536 complexating effect Effects 0.000 claims description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 2
- 229960004275 glycolic acid Drugs 0.000 claims description 2
- 239000004310 lactic acid Substances 0.000 claims description 2
- 235000014655 lactic acid Nutrition 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 241000370738 Chlorion Species 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- 229910052731 fluorine Inorganic materials 0.000 abstract description 11
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract description 10
- 239000011737 fluorine Substances 0.000 abstract description 10
- 239000011651 chromium Substances 0.000 abstract description 9
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052804 chromium Inorganic materials 0.000 abstract description 6
- 238000004532 chromating Methods 0.000 abstract description 5
- 238000001978 electrochemical passivation Methods 0.000 abstract description 4
- 239000002699 waste material Substances 0.000 abstract description 4
- 238000005097 cold rolling Methods 0.000 abstract description 3
- 239000003973 paint Substances 0.000 abstract description 3
- 230000005611 electricity Effects 0.000 abstract description 2
- 238000005987 sulfurization reaction Methods 0.000 abstract description 2
- 238000010129 solution processing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 34
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 6
- 229910052718 tin Inorganic materials 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910052717 sulfur Inorganic materials 0.000 description 5
- 239000011593 sulfur Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 230000009849 deactivation Effects 0.000 description 3
- SOCTUWSJJQCPFX-UHFFFAOYSA-N dichromate(2-) Chemical compound [O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O SOCTUWSJJQCPFX-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000004381 surface treatment Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- -1 fluoride ions Chemical class 0.000 description 2
- 229910021331 inorganic silicon compound Inorganic materials 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- YOYLLRBMGQRFTN-SMCOLXIQSA-N norbuprenorphine Chemical compound C([C@@H](NCC1)[C@]23CC[C@]4([C@H](C3)C(C)(O)C(C)(C)C)OC)C3=CC=C(O)C5=C3[C@@]21[C@H]4O5 YOYLLRBMGQRFTN-SMCOLXIQSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
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- 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 description 1
- 208000006820 Arthralgia Diseases 0.000 description 1
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
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- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
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- 206010040943 Skin Ulcer Diseases 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 208000010513 Stupor Diseases 0.000 description 1
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- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 208000026935 allergic disease Diseases 0.000 description 1
- 230000007815 allergy Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
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- NMGYKLMMQCTUGI-UHFFFAOYSA-J diazanium;titanium(4+);hexafluoride Chemical compound [NH4+].[NH4+].[F-].[F-].[F-].[F-].[F-].[F-].[Ti+4] NMGYKLMMQCTUGI-UHFFFAOYSA-J 0.000 description 1
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- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
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- 239000000467 phytic acid Substances 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
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- 231100000614 poison Toxicity 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
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- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
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- MFXMOUUKFMDYLM-UHFFFAOYSA-L zinc;dihydrogen phosphate Chemical compound [Zn+2].OP(O)([O-])=O.OP(O)([O-])=O MFXMOUUKFMDYLM-UHFFFAOYSA-L 0.000 description 1
- 150000003755 zirconium compounds Chemical class 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
- C23C22/07—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 containing phosphates
- C23C22/08—Orthophosphates
- C23C22/10—Orthophosphates containing oxidants
-
- C—CHEMISTRY; METALLURGY
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Abstract
本发明公开了一种用于镀锡钢板的无氟无铬钝化液及其使用方法，该钝化液不含有铬和氟，解决现有铬酸盐钝化液中含铬以及无铬钝化液中含氟的技术问题。一种用于镀锡钢板的无氟无铬钝化液，该无氟无铬钝化液的组分和配比为：钛盐，且其含量为0.1～50g/L；含有磷的化合物，且其含量为0.1～50g/L；氧化剂，且其含量为1～100g/L；络合剂，且其含量为1～100g/L；余量为水。本发明无氟无铬钝化液处理后的冷轧镀锡钢板具有优异的耐腐蚀性能、抗硫化性能、涂料附着性能；本发明无氟无铬钝化液直接采用喷涂，相比电解钝化工艺，节电显著，且不产生废液，对环境友好。
Description
技术领域
本发明涉及镀锡钢板钝化处理用的钝化液，特别涉及一种用于镀锡钢板的无氟无铬钝化液及其使用方法，属于金属材料表面处理技术领域。
背景技术
冷轧镀锡钢板生产的过程中，钢板经镀锡、软熔以后，为了提高镀锡钢板的耐蚀性能，防止镀锡钢板在贮存或涂料烘烤时镀锡层氧化发黄，同时提高镀锡钢板的耐硫化变黑等性能，需要对镀锡后的钢板进行钝化处理。
目前，最常用的钝化处理方法是用含有六价铬的重铬酸盐进行阴极钝化处理。用重铬酸盐钝化处理后的得到钝化膜很薄，耐蚀性能很好，且工艺简单，长久以来都是工厂中最普遍的一种钝化处理方法。但是，由于其钝化过程中采用重铬酸盐或铬酐为主盐，重铬酸盐中所含的六价铬是一种强毒性物质。六价铬为吞入性/吸入性毒物，皮肤接触可能导致过敏；更可能造成遗传性基因缺陷，吸入可能致癌，长期接触会引起人头痛、昏迷、鼻粘膜萎缩、鼻穿孔、皮肤溃疡甚至引发各种癌变等症状。对人类的健康危害极大，并且对环境有持久危险性。特别是用于食品饮料行业的镀锡板的钝化处理，采用铬酸盐钝化工艺对人体造成的危害更是不可忽视。此外，在镀锡板生产过程中还会排放出一些废液，这些废液同样也会严重地污染环境。
近些年来，越来越多的工作者投入到无铬钝化液的开发，也出现了一些无铬钝化液配方。中国专利文献CN1726304A，公开了金属表面处理用处理液和表面处理方法，包含5～5000ppm锆或钛的1种以上化合物，还含有0.1～100ppm游离氟离子，且pH为2～6。
中国专利文献CN101535528A，公开了用于钝化金属复合材料表面的含Zr/Ti的磷酸盐化溶液，溶液组成为5～50g/L的磷酸根离子，0.3～3g/L的锌离子，1～200ppm的锆和/或钛的一种或多种水溶性化合物，1～400ppm的游离氟离子。
中国专利文献CN101631895A，公开了处理金属表面的方法，该方法需用氧化酸性预洗剂处理后，与包含选自钛、锆、铪、硅、锡、锗、铝和硼的一种或多种元素的一种或多种氟酸接触。
中国专利文献CN102373453A，公开了一种无铬钝化液，该无铬钝化液所述原料混合物含有硅烷偶联剂和水，还含有钛化合物、无机硅化合物、水溶性成膜剂以及单宁酸和/或植酸，其中所述钛化合物为六氟钛酸、六氟钛酸铵、六氟钛酸钾、偏钛酸或硫酸氧钛中的一种或多种，所述无机硅化合物为纳米二氧化硅粉、硅溶胶和硅酸钠中的一种或多种。
中国专利文献CN102027157A，公开了用钝化剂涂覆金属表面的方法该钝化剂及其用途，该溶液组合物包含至少一种磷酸盐，至少3g/L的至少一种钛或/和锆化物和至少一种络合剂，以及还设计相应的含水组合物，其中络合剂包含的游离氟化物的含量是0.01～5g/L。
中国专利文献CN102066612A，公开了用于金属表面的基于Ti/Zr的最佳钝化，试剂中包含选自元素钛和/或锆中的至少一种原子的一种或多种水溶性化合物，含有至少一个氟原子的一种或多种水溶性化合物。
中国专利文献CN102851660A，公开了一种钢铁表面无磷无铬钝化成膜液及其使用方法，每升水溶液中含有氟化物1％～20％，钛离子0.001％～1％，氧化剂0.1％～20％，三价金属盐0.001％～1％，表面活性剂0.001％～1％。
氟广泛存在于自然水体中，人体各组织中都含有氟，但主要积聚在牙齿和骨筋中，适当的氟是人体所必需的，但过量的氟对人体有危害。氟化钠对人的致死量为6～12g，长期接触(约10～20年)高水平氟化物(10mg/日)可导致骨氟中毒，骨氟中毒主要表现为关节疼痛和硬化，韧带的硬化和钙化，并可造成骨畸形、肌肉衰弱和神经缺损，致使骨骼变得易碎。
因此，开发一种无铬无氟绿色环保的钝化液具有迫切的需求，对镀锡钢板生产具有重要意义。
发明内容
本发明的目的是提供一种用于镀锡钢板的无氟无铬钝化液及其使用方法，该钝化液不含有铬和氟，解决现有铬酸盐钝化液中含铬以及无铬钝化液中含氟的技术问题；实现钝化液的无毒和绿色环保，采用该钝化液处理后的冷轧镀锡钢板具有优异的耐腐蚀性能、抗硫化性能、涂料附着性能。
本发明采用的技术方案是：一种用于镀锡钢板的无氟无铬钝化液，该无氟无铬钝化液的组分和配比为：钛盐，且其含量为0.1～50g/L；含有磷的化合物，且其含量为0.1～50g/L；氧化剂，且其含量为1～100g/L；络合剂，且其含量为1～100g/L；余量为水。
所述钛盐为可溶性钛盐，为草酸钛钾、硫酸钛、硫酸氧钛和四氯化钛中的一种或几种；
所述含有磷的化合物为可溶性的磷酸、磷酸一氢盐、磷酸二氢盐和磷酸盐中的一种或几种。
所述氧化剂为弱氧化剂，为过氧化钠、双氧水、过硫酸盐和次氯酸钠中的一种或几种。
所述络合剂为无机类络合剂或者有机类络合剂，络合剂为无机类络合剂，为溴离子、氯离子、硝酸根离子、焦磷酸根离子和过氧化氢中的一种或几种；络合剂为有机类络合剂，为苹果酸、柠檬酸、酒石酸、乳酸、丙酸、羟基乙酸、三乙醇胺和甘氨酸中的一种或几种。
上述无氟无铬钝化液的制备方法，包括以下步骤：
1)按配比分别量取或称量钛盐、含有磷的化合物、氧化剂、络合剂和水；
2)将钛盐和水置入容器中混匀，使钛盐完全溶于水；后在水中加入络合剂，使溶液充分络合；再依次在溶液中加入氧化剂和含有磷的化合物；充分搅拌均匀，得到成品无氟无铬钝化液。
步骤1)中所述的钛盐、含有磷的化合物、氧化剂和络合剂均为分析纯。
用上述无氟无铬钝化液对镀锡钢板进行钝化的方法，包括以下步骤：
1)将所述无氟无铬钝化液加热至30℃～50℃；
2)将无氟无铬钝化液喷涂到软熔后的镀锡钢板表面，控制镀锡钢板表面无铬钝化液湿膜的厚度为3～6μm；
3)将步骤2)中得到的镀锡钢板在80℃～100℃热风下干燥5s～15s。
本发明相比现有技术具有如下积极效果：1、本发明无铬钝化解决现有铬酸盐钝化液中含铬以及无铬钝化液中含氟的技术难题，本发明无铬钝化液钝化处理无需电解钝化，直接采用喷涂，相比电解钝化工艺，节电显著，且不产生废液，对环境友好。2、经本发明无氟无铬钝化液钝化处理的镀锡钢板，其耐盐雾等级、孔隙率、抗硫和附着力等均达到或超过铬酸盐钝化工艺的镀锡钢板水平。
具体实施方式
下面结合具体实施方式，进一步阐明本发明，应理解下述具体实施方式仅用于说明本发明而不用于限制本发明的范围。
实施例1—3和对比例1钝化处理的镀锡钢板牌号为MRT4-CA，钢板厚度为0.2mm，钢板的镀锡层厚度为2.8g/m2。
实施例1，一种用于镀锡钢板的无氟无铬钝化液，该无氟无铬钝化液的组分和配比为：硫酸钛，且其含量为10g/L；磷酸，且其含量为5g/L；过硫酸钠，且其含量为10g/L；柠檬酸，且其含量为20g/L；余量为水
用上述无氟无铬钝化液对镀锡钢板进行钝化的方法，包括以下步骤：
1)将所述无氟无铬钝化液加热至50℃；
2)将无氟无铬钝化液喷涂到软熔后的镀锡钢板表面，控制镀锡钢板表面无铬钝化液湿膜的厚度为5μm；
3)将步骤2)中得到的镀锡钢板在80℃热风下干燥10s。
将按实施例1的方法钝化处理后镀锡钢板分别进行如下检测：按照GB/T 10125-2012《人造气氛腐蚀试验》进行耐盐雾等级检测；按照GB/T 17721-1999《金属覆盖层孔隙率试验》进行孔隙率检测，按照QB/T 2763-2006《涂覆镀锡(或铬)薄钢板测试》进行抗硫性能和附着力检测，检测结果见表1。
实施例2，一种用于镀锡钢板的无氟无铬钝化液，该无氟无铬钝化液的组分和配比为：草酸钛钾，且其含量为5g/L；磷酸二氢锌，且其含量为10g/L；次氯酸钠，且其含量为10g/L；盐酸，且其含量为5g/L；余量为水
用上述无氟无铬钝化液对镀锡钢板进行钝化的方法，包括以下步骤：
1)将所述无氟无铬钝化液加热至40℃；
2)将无氟无铬钝化液喷涂到软熔后的镀锡钢板表面，控制镀锡钢板表面无铬钝化液湿膜的厚度为4μm；
3)将步骤2)中得到的镀锡钢板在90℃热风下干燥15s。
将按实施例2的方法钝化处理后镀锡钢板分别进行耐盐雾等级、孔隙率、抗硫性能和附着力检测，检测方法同实施例1，检测结果见表1。
实施例3，一种用于镀锡钢板的无氟无铬钝化液，该无氟无铬钝化液的组分和配比为：四氯化钛，且其含量为15g/L；磷酸一氢锌，且其含量为20g/L；双氧水，且其含量为30g/L；酒石酸，且其含量为5g/L；余量为水
用上述无氟无铬钝化液对镀锡钢板进行钝化的方法，包括以下步骤：
1)将所述无氟无铬钝化液加热至50℃；
2)将无氟无铬钝化液喷涂到软熔后的镀锡钢板表面，控制镀锡钢板表面无铬钝化液湿膜的厚度为6μm；
3)将步骤2)中得到的镀锡钢板在90℃热风下干燥8s。
将按实施例3的方法钝化处理后镀锡钢板分别进行耐盐雾等级、孔隙率、抗硫性能和附着力检测，检测方法同实施例1，检测结果见表1。
对比例1，采用铬酸盐钝化液对镀锡钢板进行钝化处理，重铬酸钠溶液浓度为25g/L，PH值为4.5，阴极电解钝化电流密度为0.8A/m2，通电时间为5s，钝化膜厚度为5.0mg/m2。
将按对比例1的方法钝化处理后镀锡钢板分别进行耐盐雾等级、孔隙率、抗硫性能和附着力检测，检测方法同实施例1，检测结果见表1。
表1 本发明实施例镀锡钢板钝化处理后的性能参数
以上所述的仅是本发明的优选实施方式，除上述实施例外，本发明还可以有其他实施方式。凡采用等同替换或等效变换形成的技术方案，均落在本发明要求的保护范围。
Claims (3)
1.一种用于镀锡钢板的无氟无铬钝化液，其特征在于，无氟无铬钝化液的组分和配比为：钛盐，且其含量为0.1～50g/L；含有磷的化合物，且其含量为0.1～50g/L；氧化剂，且其含量为1～100g/L；络合剂，且其含量为1～100g/L；余量为水；所述钛盐为可溶性钛盐，为草酸钛钾、硫酸钛、硫酸氧钛和四氯化钛中的一种或几种；所述含有磷的化合物为可溶性的磷酸、磷酸一氢盐、磷酸二氢盐和磷酸盐中的一种或几种；所述氧化剂为弱氧化剂，为过氧化钠、双氧水、过硫酸盐和次氯酸钠中的一种或几种；所述络合剂为无机类络合剂或者有机类络合剂，络合剂为无机类络合剂，为溴离子、氯离子、硝酸根离子、焦磷酸根离子和过氧化氢中的一种或几种；络合剂为有机类络合剂，为苹果酸、柠檬酸、酒石酸、乳酸、丙酸、羟基乙酸、三乙醇胺和甘氨酸中的一种或几种。
2.一种制备权利要求1所述的无氟无铬钝化液的方法，包括以下步骤：
1)按配比分别量取或称量钛盐、含有磷的化合物、氧化剂、络合剂和水，所述的钛盐、含有磷的化合物、氧化剂和络合剂均为分析纯；
2)将钛盐和水置入容器中混匀，使钛盐完全溶于水；后在水中加入络合剂，使溶液充分络合；再依次在溶液中加入氧化剂和含有磷的化合物；充分搅拌均匀，得到成品无氟无铬钝化液。
3.用权利要求1所述的无氟无铬钝化液对镀锡钢板进行钝化的方法，包括以下步骤：
1)将所述无氟无铬钝化液加热至30℃～50℃；
2)将无氟无铬钝化液喷涂到软熔后的镀锡钢板表面，控制镀锡钢板表面无铬钝化液湿膜的厚度为3～6μm；
3)将步骤2)中得到的镀锡钢板在80℃～100℃热风下干燥5s～15s。
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| CN110551997A (zh) * | 2018-06-04 | 2019-12-10 | 上海梅山钢铁股份有限公司 | 一种用于电镀锡钢板的无铬钝化液及其使用方法 |
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| WO2019006608A1 (zh) * | 2017-07-03 | 2019-01-10 | 深圳市宏昌发科技有限公司 | 钝化剂、金属镀件表面钝化方法和金属工件 |
| CN110551997A (zh) * | 2018-06-04 | 2019-12-10 | 上海梅山钢铁股份有限公司 | 一种用于电镀锡钢板的无铬钝化液及其使用方法 |
| CN110551997B (zh) * | 2018-06-04 | 2022-03-15 | 上海梅山钢铁股份有限公司 | 一种用于电镀锡钢板的无铬钝化液及其使用方法 |
| CN115074714A (zh) * | 2022-06-16 | 2022-09-20 | 广州三孚新材料科技股份有限公司 | 镀锡板表面复合转化膜处理液及其制备转化膜的工艺 |
| CN115074714B (zh) * | 2022-06-16 | 2024-06-18 | 广州三孚新材料科技股份有限公司 | 镀锡板表面复合转化膜处理液及其制备转化膜的工艺 |
| CN115786894A (zh) * | 2023-01-06 | 2023-03-14 | 广东腐蚀科学与技术创新研究院 | 一种含钒处理液及其制备方法 |
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