CN100430518C - Surface conditioner containing zinc phosphate, phosphate chemical conversion treatment steelboard, coating steelboard and zinc phosphate dispersion liquid - Google Patents
Surface conditioner containing zinc phosphate, phosphate chemical conversion treatment steelboard, coating steelboard and zinc phosphate dispersion liquid Download PDFInfo
- Publication number
- CN100430518C CN100430518C CNB031430287A CN03143028A CN100430518C CN 100430518 C CN100430518 C CN 100430518C CN B031430287 A CNB031430287 A CN B031430287A CN 03143028 A CN03143028 A CN 03143028A CN 100430518 C CN100430518 C CN 100430518C
- Authority
- CN
- China
- Prior art keywords
- zinc phosphate
- phosphate
- dispersion
- chemical conversion
- surface conditioner
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 title claims abstract description 79
- 229910000165 zinc phosphate Inorganic materials 0.000 title claims abstract description 79
- 239000006185 dispersion Substances 0.000 title claims description 81
- 239000000126 substance Substances 0.000 title claims description 51
- 238000006243 chemical reaction Methods 0.000 title claims description 48
- 239000007788 liquid Substances 0.000 title claims description 48
- 229910019142 PO4 Inorganic materials 0.000 title claims description 24
- 239000010452 phosphate Substances 0.000 title claims description 24
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims description 22
- 239000011248 coating agent Substances 0.000 title description 5
- 238000000576 coating method Methods 0.000 title description 5
- 239000007769 metal material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims description 39
- 238000012545 processing Methods 0.000 claims description 22
- 229910000831 Steel Inorganic materials 0.000 claims description 19
- 239000010959 steel Substances 0.000 claims description 19
- OXHXATNDTXVKAU-UHFFFAOYSA-N phosphoric acid zinc Chemical compound [Zn].OP(O)(O)=O OXHXATNDTXVKAU-UHFFFAOYSA-N 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000001131 transforming effect Effects 0.000 claims description 4
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- 239000004094 surface-active agent Substances 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
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- 229920013701 VORANOL™ Polymers 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- ZUQAPLKKNAQJAU-UHFFFAOYSA-N acetylenediol Chemical compound OC#CO ZUQAPLKKNAQJAU-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002546 agglutinic effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000010407 ammonium alginate Nutrition 0.000 description 1
- 239000000728 ammonium alginate Substances 0.000 description 1
- KPGABFJTMYCRHJ-YZOKENDUSA-N ammonium alginate Chemical compound [NH4+].[NH4+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O KPGABFJTMYCRHJ-YZOKENDUSA-N 0.000 description 1
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000000305 astragalus gummifer gum Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- CYDRXTMLKJDRQH-UHFFFAOYSA-N benzododecinium Chemical class CCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 CYDRXTMLKJDRQH-UHFFFAOYSA-N 0.000 description 1
- 229960003237 betaine Drugs 0.000 description 1
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 1
- IQBJFLXHQFMQRP-UHFFFAOYSA-K calcium;zinc;phosphate Chemical compound [Ca+2].[Zn+2].[O-]P([O-])([O-])=O IQBJFLXHQFMQRP-UHFFFAOYSA-K 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229960000800 cetrimonium bromide Drugs 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229940117975 chromium trioxide Drugs 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N chromium trioxide Inorganic materials O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- GAMDZJFZMJECOS-UHFFFAOYSA-N chromium(6+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Cr+6] GAMDZJFZMJECOS-UHFFFAOYSA-N 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000010960 cold rolled steel Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Natural products C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- DDXLVDQZPFLQMZ-UHFFFAOYSA-M dodecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCC[N+](C)(C)C DDXLVDQZPFLQMZ-UHFFFAOYSA-M 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229950007655 esilate Drugs 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 150000002338 glycosides Chemical class 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical group [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 description 1
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 235000012204 lemonade/lime carbonate Nutrition 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 125000000250 methylamino group Chemical group [H]N(*)C([H])([H])[H] 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229940044652 phenolsulfonate Drugs 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 108010064470 polyaspartate Proteins 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 239000001397 quillaja saponaria molina bark Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920003987 resole Polymers 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229930182490 saponin Natural products 0.000 description 1
- 150000007949 saponins Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-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
- REZQBEBOWJAQKS-UHFFFAOYSA-N triacontyl alcohol Natural products CCCCCCCCCCCCCCCCCCCCCCCCCCCCCCO REZQBEBOWJAQKS-UHFFFAOYSA-N 0.000 description 1
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- SPDJAIKMJHJYAV-UHFFFAOYSA-H trizinc;diphosphate;tetrahydrate Chemical compound O.O.O.O.[Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SPDJAIKMJHJYAV-UHFFFAOYSA-H 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 229940077934 zinc phosphate tetrahydrate Drugs 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
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- C23C22/78—Pretreatment of the material to be coated
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
A zinc phosphate-containing surface conditioning agent to be used for surface conditioning as pretreatment for zinc phosphate conversion coating of a metallic material, which contains from 500 to 20,000 ppm of zinc phosphate and which has a pH of from 3 to 11, wherein said zinc phosphate has an average particle size of at most 3 mu m and D90 of at most 4 mum.
Description
Technical field
The present invention relates to a kind of surface conditioner, the pre-treatment that the zinc phosphate chemical conversion that it is used for that metallic substance is carried out is handled.
Background technology
Car body, household appliances etc. generally all are after metal material processing such as steel plate, steel plate galvanized are become the metal forming thing, again through application, the final product that forms of assembling.The application of this metal forming thing will be passed through each procedure such as degreasing, surface adjustment, chemical conversion processing, plating.
The purpose of carrying out adjust handling on the surface is in the phosphate chemical conversion processing as subsequent processing, on the whole surface of metal equably, apace, to high-density by the phosphate crystal film forming.Normally metallic substance is immersed in the surface and adjusts in the groove, form phosphatic nucleus in the metallic surface.Operation generally forms titanium phosphate in the metallic surface colloid is adjusted on this surface, utilizes this colloid to form good chemical conversion film in the metallic surface when chemical conversion is handled.
This surface conditioner that is used for adjusting on the surface has the spy opens the high-durability surface conditioner that flat 9-249978 communique discloses, it is that the value of a kind of titanium ion 1～50ppm, phosphate anion 50～1000ppm, tripolyphosphate radical ion 50～400ppm, 20～1500ppm, (tripolyphosphate ionic weight)/(weight of titanium ion) is 10～100, and pH is 5～10.0 the aqueous solution.
But there is shortcoming in these various titanium phosphate colloids as surface conditioner, and promptly process in time easily produces dissolving and aggegation, and it is shaped as powder inconvenience use.
Also have, open the 2000-96256 communique the spy and disclosed phosphate particle and the monose of conduct promotion composition and the surface adjustment treatment soln of polyose that contains divalent or 3 valency metals.But the present inventor studies show that, this surface is adjusted treatment soln and also had shortcoming, i.e. poor stability, and the processing that the deep trouth portion of aluminium alloy or complex structure member or this class of cast steel slab is difficult to carry out the steel plate that chemical conversion handles is not ideal enough.
The objective of the invention is at above-mentioned present situation, a kind of aqueous, excellent in stability is provided and the steel plate that deep trouth portion or this class of cast steel slab are difficult to carry out chemical conversion is also had the surface conditioner of good processing.
Summary of the invention
The present inventor has carried out deep research with regard to above-mentioned problem, found that and adopt the material that zinc phosphate is disperseed with specific state and obtain as surface conditioner, can obtain the configuration of surface excellent in chemical and transform steel plate, thereby finish the present invention, promptly the present invention includes:
(1) surface conditioner of phosphoric acid zinc, it is used for transforming the pretreated surface adjustment that film forming is handled as metallic substance being carried out phosphate chemical, and the feature of this surface conditioner is to contain zinc phosphate 500～20000ppm, the median size of above-mentioned zinc phosphate below 3 μ m, D
90Below 4 μ m, pH is 3～11.
(2) manufacture method of phosphate chemical conversion processing steel plate, the feature of this method be, metallic substance is immersed in the surface conditioner of above-mentioned (1) described phosphoric acid zinc, carries out the phosphate chemical conversion processing then.
(3) manufacture method of coated steel plate, the feature of this method be, metallic substance is immersed in the surface conditioner of above-mentioned (1) described phosphoric acid zinc, then carries out the phosphate chemical conversion processing, carries out application then.
(4) be used to prepare the zinc phosphate dispersion liquid of surface conditioner, it is used to prepare the surface conditioner of phosphoric acid zinc, this surface conditioner is used for transforming the pretreated surface adjustment that film forming is handled as metallic substance being carried out phosphate chemical, the feature of this zinc phosphate dispersion liquid is, contain zinc phosphate 0.5～50 weight %, the median size of above-mentioned zinc phosphate below 3 μ m, D
90Below 4 μ m, pH is 3～11.
Embodiment
Below describe the present invention in detail.
The surface conditioner of phosphoric acid zinc of the present invention, make the zinc phosphate colloid attached to metallic surfaces such as iron, zinc system, aluminium systems, so that in the zinc phosphate chemical conversion operation of then carrying out, generating with above-mentioned colloid rapidly is the zinc phosphate chemical conversion film of nucleus, and forms the good zinc phosphate chemical conversion rete of form.
(zinc phosphate)
Surface conditioner of the present invention contains zinc phosphate.The zinc phosphate here is with Zn
3(PO
4)
2Expression is generally the colourless crystallization solid, and what sell on the market then is white powder.
Obtain zinc phosphate, can mol ratio fusion in 3: 2 diluent of heating zinc sulfate and Sodium phosphate dibasic, generate tetrahydrate as the sedimentary zinc phosphate of crystallinity.Also can make the reaction of the dilute phosphoric acid aqueous solution and zinc oxide or zinc carbonate, obtain the zinc phosphate tetrahydrate.The crystallization of tetrahydrate is a rhombic system, and the form of 3 kinds of variations is arranged.To its heating, obtain under 100 ℃ obtaining under the dihydrate, 190 ℃ obtaining not having hydrate under the monohydrate, 250 ℃.Zinc phosphate among the present invention can adopt any one in tetrahydrate, dihydrate, monohydrate, the no hydrate.The facile tetrahydrate of general direct employing.
Also have, zinc phosphate can use and carry out various surface-treated materials.For example, can be to carry out the surface-treated material with metal alkoxides such as silane coupling agent and rosin, silicon compound, silicon alkoxide and aluminium-alcohol salts.
When zn cpds and phosphatase reaction, add silicon-dioxide and Tripyrophosphoric acid and can obtain particulate zinc phosphate (special public clear 49-2005 communique etc.), with mechanical means with zinc phosphate and the fusion of various metallic compound wet method and finish mechanico-chemical reaction, can make the part zinc in the zinc phosphate be replaced (spy opens flat 4-310, No. 511 communiques etc.) by metals such as magnesium, calcium, aluminium, for example, mixed the material of the composition beyond phosphorus such as silicon-dioxide, calcium, aluminium, oxygen, the zinc by aforesaid method or as the commercially available product of the zinc phosphate of silicic acid modification.In this case, the content of zinc phosphate should be more than 25 quality %, with P with the ZnO conversion
2O
5Conversion should be more than 15 quality %.
There is no particular limitation to the shape of zinc phosphate, and commercially available product is generally white powder, and the shape of powder can be arbitrary shapes such as particulate shape, plate shape, scale shape.Also there is no particular limitation to particle diameter, and normally median size is the powder of number μ m.It is desirable to especially through basic treatment and shock absorption commercially available suitable employing of rust-stabilising pigment such as enhanced product to some extent.As mentioned below, therefore the present invention can obtain stable surface treatment effect, and can not be subjected to the influence of the initial size and the shape of powder owing to can modulate the stable dispersion liquid of the fine dispersive of zinc phosphate.
(preparation of dispersion liquid)
Use the zinc phosphate of above explanation, preferably should be equipped with dispersion liquid in advance, make its fine dispersion.
There is no particular limitation to making zinc phosphate be dispersed in the modulator approach that forms aqueous liquid dispersion in the aqueous medium, and method is that zinc phosphate is blended in the dispersion medium such as water or organic solvent preferably, carries out wet pulverization and modulate in the presence of dispersion agent.
(dispersion medium)
As making phosphoric acid salt dispersive dispersion medium, the aqueous medium more than water accounts for 80 weight %, can also use various organic solvents as the medium beyond the water, but the content of organic solvent will be controlled in the lower scope, better be below 10 weight % of aqueous medium, be more preferably below 5 weight %.The present invention also can modulate the dispersion liquid of not moisture fully dispersion medium in addition.
To the not special regulation of water-miscible organic solvent, for example, alcoholic solvents such as methyl alcohol, Virahol, ethylene glycol, propyl cellosolve, varsols such as hexane, heptane, dimethylbenzene, toluene, hexanaphthene, petroleum naphtha, ketones solvents such as Methyl isobutyl ketone, butanone, isophorone, methyl phenyl ketone, amide solvent such as N,N-DIMETHYLACETAMIDE, methyl-2-pyrrolidone, esters solvents such as ethyl acetate, isobutyl acetate, octyl acetate, acetate methyl glycol ester, acetate diethylene glycol monomethyl ether ester.
These organic solvents both may be used alone, two or more kinds can also be used in combination.
When preparing the aqueous liquid dispersion of zinc phosphate, in the way that relatively is fit on the operation is when modulating dispersion liquid, zinc phosphate is blended in carries out wet pulverization in the aqueous medium, can also in the dispersion medium beyond the aqueous medium, carry out wet pulverization after, carry out solvent exchange again and modulate solution.
(dispersion agent)
During the preparation dispersion liquid, can use dispersion agent.There is no particular limitation to dispersion agent, for example can use macromolecule dispersing agent, tensio-active agent or coupler etc.
Macromolecule dispersing agent has natural polymer preferably, its object lesson comprises that gelatin, gelatin, casein or albumin etc. are protein-based, natural rubber such as gum arabic or tragacanth gum class, portugal glycosides such as Saponin/TSM, alginate derivatives such as alginic acid and Protanal Ester SD-LB, alginic acid trolamine or ammonium alginate, derivatived celluloses such as methylcellulose gum, carboxymethyl cellulose, Natvosol or ethyl hydroxylated cellulose.
These macromolecule dispersing agents both may be used alone, two or more kinds can also be used in combination.Wherein, be preferably methylcellulose gum, be more preferably carboxymethyl cellulose, Natvosol.
Other preferably macromolecule dispersing agent synthetic macromolecule is arranged, its object lesson comprises that polyamine is a resin, the polycarboxylic acid series resin, polyolefin-based resins, polyester based resin, polyurethane series resin, polyvinyl alcohol, the polyvinylpyrrolidone class, the polyacrylic resin, vinylformic acid-acrylonitrile copolymer, potassium acrylate-acrylonitrile copolymer, acrylic resin such as vinyl-acetic ester-acrylate copolymer or acrylic acid and acrylic ester copolymers, the styrene-propene acid copolymer, vinylbenzene-Sipacril 2739OF, vinylbenzene-methacrylic acid-acrylate copolymer, the acid of styrene-propene such as styrene--vinylformic acid or styrene--acrylic acid and acrylic ester copolymers is resin, styrene-maleic acid copolymer, styrene-maleic anhydride copolymer, vinylnaphthalene-acrylic copolymer, vinylnaphthalene-maleic acid and vinyl-acetic ester-ethylene copolymer, vinyl-acetic ester-fatty acid vinyl vinyl ester copolymers, vinyl-acetic ester-maleate copolymer, vinyl-acetic ester-butenoic acid multipolymer, vinyl-acetic ester based copolymer and their salt such as vinyl-acetic ester-acrylic copolymer.
These macromolecule dispersing agents both may be used alone, two or more kinds can also be used in combination.Wherein good especially is polyamine is resin, polycarboxylic acid series resin, polyester based resin, polyurethane series resin, polyvinyl alcohol, polyvinylpyrrolidone class, styrene-propene acid are resin, polyacrylic resin, styrene-maleic acid copolymer etc.
More particularly, as polyamine is the ュ ニ セ Application ス CP-102 (セ Application カ society system) of resin, KZ-125K (セ Application カ society system), ァ シ ス パ-PB821 (aginomoto society system) as polyester based resin, ソ Le ス パ-ス 24000GR (ゼ ネ カ society system), ソ Le ス パ-ス 32550 (ゼ ネ カ society system), Disperbyk190 (ピ ッ Network ケ ミ-society's system), EFKA-4046 (ゥ ィ Le バ-ェ リ ス society system) as polyurethane series resin, Disperbyk 161 (ピ ッ Network ケ ミ-society's system), Disperbyk 163 (ピ ッ Network ケ ミ-society's system), Disperbyk 165 (ピ ッ Network ケ ミ-society's system), polyvinyl alcohol, PVPK-90 (Wu Association industry society system as the polyvinylpyrrolidone class), acid is the ジ Application Network リ Le 61J of resin as styrene-propene, Disperbyk 191 (ピ ッ Network ケ ミ-society's system) as the polyacrylic resin, EFKA-4550 (ゥ ィ Le バ-ェ リ ス society system) is the SMA レ ジ Application 1440H (ATO society system) of resin as styrene-maleic acid, マ リ ァ リ system AKM-0531 (Japanese grease society system).
Tensio-active agent comprises the Voranol EP 2001 that belongs to nonionic surface active agent preferably, polyoxyalkylene alkyl, polyoxyethylene deriv, oxygen ethene-oxypropylene segmented copolymer, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, the polyoxyethylene sorbitol fatty acid ester, glycerol fatty acid ester, polyoxyethylene fatty acid ester, the polyoxyethylene alkanamine, the alkyl chain triacontanol acid amides, nonylphenol, the alkyl nonylphenol, polyoxyalkylene glycol, alkyl amine oxide, acetylenediol, the polyoxyethylene nonylplenyl ether, silicon such as polyxyethylated phenylate modification silicon are tensio-active agent, the fluorochemical surfactant that at least one hydrogen atom in the hydrophobic group of the hydrocarbon-surfactant that replaces with fluorine atom obtains.These nonionic surface active agent and other dispersion agents and usefulness can obtain better effect.
The alkyl trimethyl ammonium salt class that perhaps belongs to cationic surfactant, for example, Trimethyllaurylammonium chloride, cetrimonium bromide, the hard ester acyl of chlorination trimethyl ammonium; Or the alkyl dimethyl benzyl ammonium salt class, for example, the hard ester acyl of chlorination dimethyl benzyl ammonium, chloride benzylidene cicuta virosa Linn, chlorination lauryl dimethyl benzyl ammonium salt, ammonium phosphate salt etc.
The soap that perhaps belongs to aniorfic surfactant, alkyl sulfuric ester salt, alkyl ether sulphate salts, alkylbenzene sulfonate, sulfonated alkyl naphathalene, alkyl sulfo succinate, alkyl diphenyl ether disulfonate, poly-bis-phenol sulfonate, alkylphosphonic, polyoxy ethyl alkyl sulfuric ester salt, polyoxy ethyl alkyl allyl group sulfuric acid, sulfonated, the methylamino esilate, polyaspartic acid salts, ether carboxylate, naphthalene sulfonic acidformaldehyde condensation product, polyxyethylated phosphoric acid ester etc.These tensio-active agents both may be used alone, two or more kinds can also be used in combination.
Wherein, good especially is polyxyethylated phosphoric acid ester.More particularly polyxyethylated phosphoric acid ester can be used Off ォ ス Off ァ ノ-Le RS-610 (East nation chemistry (strain) system), Disperbyk 180 (ピ ッ Network ケ ミ-society's system), and phosphate amine salt can be used SN-デ ィ ス パ-サ Application ト 2060 (サ Application ノ プ コ society system).
Here the anionic property resin in aniorfic surfactant of Shi Yonging and the above-mentioned macromolecule dispersing agent can be that neutralizing agent neutralizes with ammonia or amine.Can as amine be neutralizing agent diethylamine (DEA), triethylamine (TEA), Monoethanolamine MEA BASF (META), diethanolamine (DETA), trolamine (TETA), dimethylethanolamine (DMEA), diethylethanolamine (DEEA), isopropyl alcohol amine (IPEA), diisopropanolamine (DIPA) (DIPA), 2-amino-2-methyl propyl alcohol (AMP), 2-(dimethylamino)-2-methylpropanol (DMAMP), morpholine (MOR), N-methylmorpholine (NMM), N-ethylmorpholine (NEM) etc. are arranged.
They both may be used alone, two or more kinds can also be used in combination.Wherein, good especially is 2-amino-2-methyl propyl alcohol (AMP).
Perhaps use the L-Ala system belong to amphoterics, Mi Zuo Evil betaine, amido propyl betaine system, amino dipropionate etc.
Perhaps using silane is that coupler, aluminium are that coupler, titanium are that coupler, zirconium are couplers such as coupler.
They both may be used alone, two or more kinds can also be used in combination.The wherein good especially silane that is to use is coupler.
Good especially dispersion agent is polyxyethylated phosphoric acid ester.
These dispersion agents both may be used alone, two or more kinds can also be used in combination.
Usually the blended amount of zinc phosphate is 0.5～50 weight % in dispersion liquid.If it is less than 0.5 weight %, then the content of zinc phosphate is very few, insufficient with the surface conditioner effect that this dispersion liquid obtains.If surpass 50 weight %, then be difficult to obtain even and fine size-grade distribution, and be difficult to form fine dispersion state by wet pulverization.Blended amount is that 1～50 weight % is then better.
Also have, the addition of dispersion agent should be 0.1～50 weight % in dispersion liquid, more preferably 0.5～20 weight %.If below 0.1 weight %, then dispersiveness is abundant inadequately, if more than 50 weight %, then because of unnecessary dispersion agent interacts to each other, dispersiveness on the contrary can variation, even and dispersed enough, but cost is too high.
(explanation of dispersion state)
Zinc phosphate compactly is distributed in the dispersion medium, and degree of scatter at this moment is that average mark shot footpath is below 3 μ m.
Here with D
50(volume 50% diameter) is as average mark shot footpath and median size.
There is no particular limitation with the preparation method of fine and closely woven dispersive dispersion liquid below the 3 μ m to zinc phosphate, reasonable method is that zinc phosphate, dispersion agent are added in the dispersion medium, and the content that makes them is respectively 0.5～50 weight %, 0.1～50 weight %, carries out wet pulverization then.There is no particular limitation to the method for wet pulverization, get final product with existing known method, for example, can use with disc mill, the pin mill pulverizer as representative, and high-pressure homogenizer, ultrasonic dispersing machine etc. are the media dispersion machine of representative etc.
If pulverize when pulverizing excessively, along with the increase dispersion agent meeting of specific surface area is not enough, excessively divided particles generation aggegation can form oversize particle on the contrary, the affected dispersion phenomenon of crossing of dispersion stabilization occurs.In addition, because of fusion and dispersion condition can occur dispersed discretely, cause that oversize particle and minuteness particle the most compactly fill the aggegation that causes and thickening or minuteness particle agglutinative phenomenon to each other.For preventing that this phenomenon from taking place, and should monitor D
90(volume 90% diameter) selects not produce dispersive fusion and dispersion condition.D among the present invention
90Be decided to be below the 4 μ m.
Here, D
50(volume 50% diameter) and D
90(volume 90% diameter) is according to the size-grade distribution in the dispersion liquid, is 100% when asking summation curve with the cumulative volume of particle, 50% on the summation curve and 90% 's particle diameter.More typical way is to measure D automatically with laser-Doppler formula sreen analysis meter (day machine dress (strain) system, (マ ィ Network ロ ト ラ ッ Network UPA150)) equigranular determinator
50And D
90
Adopt above method the mean value of the dispersion particle diameter of the zinc phosphate in the aqueous medium can be adjusted to below the 3 μ m, what can obtain excellent in stability has the aqueous liquid dispersion of premium properties as surface conditioner.Disperse the mean value of particle diameter to be generally 0.01～3 μ m, can be adjusted to desired degree.
With above method modulation aqueous liquid dispersion of the present invention,, also can be dispersed in the dispersion liquid by the following dispersion particle diameter of 3 μ m even particle diameter surpasses the zinc phosphate of 3 μ m.Initial size is that the zinc phosphate particle of tens of μ m also is like this.Even just meaning without initial size, this adopt wet pulverization also can reduce the initial size of pigment according to the method described above originally with regard to little zinc phosphate.Using aforesaid method, the mean value of the dispersion particle diameter in the aqueous liquid dispersion can be controlled at below the 3 μ m, can also be below 1 μ m, even below the 0.2 μ m.
The dispersion liquid of the present invention that obtains like this can be controlled at below the 3 μ m according to the mean value of purposes with the dispersion particle diameter of the zinc phosphate in the dispersion liquid, and it is the aqueous liquid dispersion that dispersion stabilization is good, have premium properties as surface conditioner.
Adopt above-mentioned wet pulverization method, can reduce oversize particle is that particle diameter surpasses D
90Therefore the ratio of particle can form the distribution D that disperses particle diameter
90Below the 4 μ m, can also be the dispersion liquid of narrow distribution that disperses the dispersion particle diameter of particle diameter in can suppress below the 2.6 μ m or even below 0.3 μ m greatly.Infer zinc phosphate thus with fine dispersion particle size dispersion, and dispersion state is extremely stable.And, help the zinc phosphate in the dispersion liquid to generate nucleus efficiently because the ratio of oversize particle is low, also owing to disperse the narrow diameter distribution uniform particle diameter, therefore can infer in surface adjustment treatment process and can form the more nucleus of homogeneous, thereby in ensuing chemical conversion is handled, can form the more zinc phosphate crystallization of homogeneous, the surface texture homogeneous of steel plate and good is handled in the chemical conversion that obtains, and can also improve the processing that the deep trouth portion of complex structure member and this class of cast steel slab is difficult to carry out the steel plate that chemical conversion handles.
Have, the dispersion particle diameter of the zinc phosphate in the dispersion liquid is decided size-grade distribution with laser-Doppler formula sreen analysis instrumentation and is tried to achieve again.
The zinc phosphate amount of fusion in the aqueous liquid dispersion of the present invention reaches more than the 10 weight %, can also be more than the 20 weight % or even more than the 30 weight %, can obtain the aqueous liquid dispersion of high density.Therefore be easy to modulate the high surface conditioner of performance.
As mentioned above, make fine be dispersed in the aqueous medium of zinc phosphate in advance and the aqueous liquid dispersion that forms, suitably add aqueous medium again to make surface conditioner, can reach stable fine dispersion state thus.
Phosphoric acid zinc 600～20000ppm in the surface conditioner of phosphoric acid zinc of the present invention, if the content of zinc phosphate, then forms the phosphoric acid salt deficiency of nucleus less than 600ppm, if surpass 20000ppm, then not only can not obtain desired effect, and cost is too high.
Content is then better at 50～1000ppm.
(additive)
In order further to improve stability, can add thickening material as required.It is thickening material that thickening material can use carclazyte, talcum powder, clay, diatomite, lime carbonate, barium sulfate, titanium oxide, aluminum oxide, silicon-dioxide, potter's clay, mica, aluminium hydroxide etc. inorganic, organic system resins such as polyacrylic ester, urethane, polyester, polyethylene, polypropylene, polyvinyl chloride, polyvinylidene dichloride, polystyrene, polysiloxane, thickening polyose, resol, Resins, epoxy, benzo guanamine or thickening material of being made of their polymkeric substance etc., these thickening materials promptly can use separately also and can be used in combination more than 2 kinds.
When using thickening material, can select suitable kind and addition etc.Generally, can add the thickening material of 0.01～10wt%, be more preferably the thickening material that adds 0.1～5wt% corresponding to dispersion liquid.
And the foaming phenomenon in the time of can also using defoamer to suppress operation is used for the fungi-proofing mildew-resistant of dispersion liquid with sanitas and mould inhibitor etc.During use, can select suitable kind and addition etc.
The pH of the surface conditioner of phosphoric acid zinc of the present invention is 3～11.
If the pH value that pH less than 3, then can make the chemical conversion of subsequent processing bathe descends, thereby harm the formation of chemical conversion film, if pH greater than 11, then the zinc phosphate particulate dissolves easily, the instability that becomes also can influence subsequent processing, pH is preferably 7～10.
In the present invention, more stable for making the zinc phosphate particulate so that transform the careful chemical conversion film of formation in the film forming treatment process at the phosphate chemical that then carries out, can add basic salts such as SODA ASH LIGHT 99.2.
(surface adjustment is handled)
Can carry out the surface adjustment of various metallic substance handles with above-mentioned surface conditioner of the present invention.
There is no particular limitation to method that the surface adjustment is handled, as long as adopt suitable known method that surface conditioner is contacted with the metallic surface.
Metallic substance can be immersed in the surface conditioner of phosphoric acid zinc of the invention described above, then carry out the zinc phosphate chemical conversion and handle, make the zinc phosphate chemical conversion and handle steel plate.More typical way is after metallic substance is immersed surface adjustment groove, to carry out the phosphate chemical conversion processing.To duration of contact of surface conditioner and metallic surface, there is no particular limitation for the temperature of surface conditioner, can adopt existing known method.
Also there is no particular limitation to the metallic substance as process object, can be used for generally being fit to carry out the various metals of phosphate chemical conversion processing, for example, and iron and steel, steel plate galvanized, aluminum or aluminum alloy and magnesium alloy.
In addition, surface conditioner of the present invention can be used for degreasing and operation is adjusted on the surface, so just can save the washing step after the skimming treatment.
In surface adjustment operation is held concurrently in degreasing, can add known inorganic alkaline synergistic agent, organic synergistic agent and tensio-active agent etc. for improving the rate of cleaning.Can also add known sequestrant and condensed phosphate etc.
(chemical conversion treatment process)
Metallic substance is immersed in the surface conditioner of phosphoric acid zinc of the invention described above, then carries out the zinc phosphate chemical conversion and handle, and then electroplate, can make coated steel plate.
Chemical conversion processing method to zinc phosphate is unqualified, can adopt various known method such as dip treating, hydrojet processing, electrolysis treatment.These methods can certainly be made up.The phosphoric acid salt rete of separating out so long as phosphoric acid salt get final product, unqualified fully to its composition, can be zinc phosphate, tertiary iron phosphate, manganous phosphate, calcium zinc orthophosphate activated by thallium etc.
Carry out carrying out application after the phosphate chemical conversion processing.The method of application generally adopts plating.There is no particular limitation to coating that application is used, can be the various coating that generally are used for the application of phosphate chemical conversion processing steel plate, and for example, epoxy melamine coating, cation electroplating paint and polyester are that intermediate layer coating and polyester are investment precoat etc.In addition, handling the back in chemical conversion can also adopt known method to carry out matting to application.
(embodiment 1)
With following method, make the zinc phosphate dispersion liquid.
In water 142.3 weight parts, mix commercially available zinc phosphate 100 weight parts and (be shaped as squamose standard type zinc phosphate, median size 3 μ m are measured by centrifugal light transmission type particle size distribution machine, water soluble ingredient is being measured by JIS-K-5101 below 1%, pH 6.9 is measured by JIS-K-5101, oil number is that 26ml/100g is measured by JIS-K-5101, density is that 3.0g/ml is measured by JIS-K-5101, screening residual component (45 μ m) is being measured by JIS-K-5101 below 1%, the ZnO component is 58% to measure P by the EDTA method
2O
5Component is 33% to be measured by colorimetric analysis).Then, add as the polyxyethylated phosphoric acid ester (Off of the commercially available aniorfic surfactant of dispersion agent
ォス Off ァ ノ-Le RS-610) (East nation chemistry (strain) system) 5 weight parts.Then, add AMP 1 weight part again,, and stir as xanthenes glue 0.3 weight part of thickening material as neutralizing agent.After the stirring, carry out wet pulverization, use laser-Doppler formula sreen analysis meter (day machine dress (strain) system, (マ ィ Network ロ ト ラ again with Highefficientpulverizer (φ 1mm alkali glass hollow bead)
ッNetwork UPA150)) measure size-grade distribution, monitoring D
50(median size of dispersion) and D
90, obtain D
50Be 0.49 μ m, D
90It is the dispersion liquid of 1.40 μ m.
After the dispersion, for making dispersion stable, add xanthenes glue 0.6 weight part, and stir as thickening material.
(embodiment 2)
With following method, make the zinc phosphate dispersion liquid.
(commercially available silicate modified zinc phosphate, median size 4～5 μ m are measured by centrifugal light transmission type particle size distribution machine to mix commercially available zinc phosphate 100 weight parts in water 142.3 weight parts, water soluble ingredient is 1.9% to have JIS-K-5101 to measure, pH 9.4 is measured by JIS-K-5101, ZnO component 40% is measured by the EDTA method, P
2O
5Be 24% to be measured by colorimetric analysis, CaO 9% measures SiO by the EDTA method
2Be 10% by gravimetric determination).Then add as the polyxyethylated phosphoric acid ester (Off of the commercially available aniorfic surfactant of dispersion agent
ォThe ス Off
ァノ-Le RS-610) (East nation chemistry (strain) system) 5 weight parts.Then, add AMP 1 weight part,, and stir as xanthenes glue 0.3 weight part of thickening material as neutralizing agent.After the stirring, carry out wet pulverization, use laser-Doppler formula sreen analysis meter (day machine dress (strain) system, (マ ィ Network ロ ト ラ again with Highefficientpulverizer (φ 1mm alkali glass hollow bead)
ッNetwork UPA150)) measure size-grade distribution, monitoring D
50And D
90, obtain D
50Be 0.49 μ m, D
90It is the dispersion liquid of 1.36 μ m.
After the dispersion, for making dispersion stable, add xanthenes glue 0.6 weight part, and stir as thickening material.
(comparative example 1)
In water 142.3 weight parts, mix with embodiment 1 in used identical commercially available zinc phosphate 100 weight parts, then add as the polyxyethylated phosphoric acid ester (Off of the commercially available aniorfic surfactant of dispersion agent
ォThe ス Off
ァノ-Le RS-610) (East nation chemistry (strain) system) 5 weight parts.Add AMP 1 weight part again as neutralizing agent, as xanthenes glue 0.3 weight part of thickening material, and stir.After the stirring, carry out wet pulverization, in pulverizing process, do not average particle diameter and D with Highefficientpulverizer (φ 1mm alkali glass hollow bead)
90Monitoring.
After the dispersion, for making dispersion stable, add xanthenes glue 0.6 weight part, and stir, obtain dispersion liquid as thickening material.
To this dispersion liquid, with laser-Doppler formula sreen analysis meter (day machine dress (strain) system, (マ ィ Network ロ ト ラ
ッNetwork UPA150)) measure size-grade distribution, consequently, D
50(median size of dispersion) is 4 μ m, D
90Be 5 μ m.
(comparative example 2)
Used Nippon Paint Co., Ltd's control surface to adjust agent (サ-Off Off
ァィ Application 5N-10) (powder).
[evaluation test]
Thin up and fully stirring makes its concentration that reaches regulation (see Table in 1 [surface treatment agent]) in the various zinc phosphate dispersion liquids that embodiment 1,2 and comparative example 1 obtain, and forms the surface and adjusts liquid.Adjust liquid with the surface that obtains and assess as follows, the results are shown in Table 1.The surface conditioner of comparative example 2 also adopts and adds the surface adjustment liquid that water fully stirs the concentration that reaches regulation, adjusts liquid with this surface and carries out identical assessment, the results are shown in Table 1.
(appraisal procedure)
1. the stability of liquid is adjusted on the surface
The surface of embodiment 1,2 is adjusted in the thermostatic bath that liquid is placed on 50 ℃, carried out ageing stability and promote test.Consequently,, do not find the phenomenon of sedimentation, thickening fully, and yet no change of size-grade distribution yet, show that thus this surface adjusts the excellent in stability of liquid even spent 1 month.
2. the chemical convertibility of zinc phosphate rete
At room temperature, ((70mm * 150mm * 0.8mm) immerses the surface respectively and adjusts in the liquid and handled 30 seconds for 70mm * 150mm * 0.8mm), aluminum steel plate (A6063S) with the cold-rolled steel sheet (SPC) that carried out skimming treatment in advance.After rolling slurry, use zinc phosphate treatment solution (Nippon Paint Co., Ltd's system (サ-Off ダ ィ Application SD6000)) to carry out chemical conversion with pickling process at 43 ℃ immediately and handled 2 minutes, washing then with the pure water washing, obtains test board again after the drying.
Zinc phosphate chemical conversion film with observable each test board of SEM (Japanese Electricity (strain) makes JSM5600).Crystallite size sees Table 1.What data showed that embodiment 1,2 obtains all is very careful crystallization.The assessment result of visual observations condition of surface sees Table [outward appearance] item in 1.◎ represents evenly not have rust staining, and zero expression is omited spottiness but do not had rust staining, * represent that spot is obvious and rust staining is arranged.
3. the weight of chemical conversion film (C/W)
The weight of the test board that obtains is 1. (g), the weight of peeling off behind the chemical conversion film from test board is 2. (g) by the following method, their difference (1.-2.) (g) is removed by the surface-area of test board again and the value of trying to achieve is the weight (C/W) of chemical conversion film, and it the results are shown in Table 1.
(1) stripping means of SPC test board
With test board dipping 5 minutes in being heated to 75 ℃ the 50g/l solution of chromium trioxide, peel off chemical conversion film.
(2) aluminium test board
At room temperature test board was flooded 1 minute in 30% aqueous nitric acid, peel off chemical conversion film.
[table 1]
The present invention adopts above-mentioned technology, can access a kind of and existing surface conditioner and compare, aqueous, stability preferably, be the surface conditioner that can obtain the zinc phosphate chemical conversion film of immaculate uniform and delicate in the zinc phosphate chemical conversion film formation process at subsequent processing.
Claims (4)
1. the surface conditioner of phosphoric acid zinc, it is used for transforming the pretreated surface that film forming handles and adjusting as metallic substance being carried out phosphate chemical, it is characterized in that, contains zinc phosphate 500～20000ppm, the median size of above-mentioned zinc phosphate below 3 μ m, D
90Below 4 μ m, pH is 3～11.
2. the manufacture method of phosphate chemical conversion processing steel plate is characterized in that, metallic substance is immersed in the surface conditioner of the described phosphoric acid zinc of claim 1, carries out the phosphate chemical conversion processing then.
3. the manufacture method of coated steel plate is characterized in that, metallic substance is immersed in the surface conditioner of the described phosphoric acid zinc of claim 1, then carries out the phosphate chemical conversion processing, carries out application then.
4. be used to prepare the zinc phosphate dispersion liquid of surface conditioner, it is used to prepare the surface conditioner of phosphoric acid zinc, this surface conditioner is used for transforming the pretreated surface adjustment that film forming is handled as metallic substance being carried out phosphate chemical, it is characterized in that, contain zinc phosphate 0.5～50 weight %, the median size of above-mentioned zinc phosphate below 3 μ m, D
90Below 4 μ m, pH is 3～11.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002172373 | 2002-06-13 | ||
| JP2002-172373 | 2002-06-13 | ||
| JP2002172373 | 2002-06-13 |
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| CN100430518C true CN100430518C (en) | 2008-11-05 |
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|---|---|---|---|
| CNB031430287A Expired - Lifetime CN100430518C (en) | 2002-06-13 | 2003-06-13 | Surface conditioner containing zinc phosphate, phosphate chemical conversion treatment steelboard, coating steelboard and zinc phosphate dispersion liquid |
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| Country | Link |
|---|---|
| US (1) | US20040011429A1 (en) |
| EP (1) | EP1378586B1 (en) |
| KR (1) | KR20030096065A (en) |
| CN (1) | CN100430518C (en) |
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| CZ2022448A3 (en) * | 2022-10-31 | 2024-03-27 | České vysoké učenà technické v Praze | A method of pre-treatment of the surface of steel components |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197849A (en) * | 1997-03-07 | 1998-11-04 | 日本巴可莱新株式会社 | Metallic surface pretreating liquid and method before formation and treatment of phosphate coating |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1084017A (en) * | 1963-09-30 | 1967-09-20 | Jawata Iron & Steel Co Ltd | Pretreating process for phosphate-treating steel sheets or plated steel sheets |
| ES2006347A6 (en) * | 1988-03-03 | 1989-04-16 | Colores Hispania | A corrosion inhibiting pigment and a process for the manufacturing thereof. |
| US6214132B1 (en) * | 1997-03-07 | 2001-04-10 | Henkel Corporation | Conditioning metal surfaces prior to phosphate conversion coating |
| US6361623B1 (en) * | 1997-06-13 | 2002-03-26 | Henkel Corporation | Method for phosphatizing iron and steel |
| US6478860B1 (en) * | 1998-07-21 | 2002-11-12 | Henkel Corporation | Conditioning metal surfaces before phosphating them |
| JP3545974B2 (en) * | 1999-08-16 | 2004-07-21 | 日本パーカライジング株式会社 | Phosphate conversion treatment method for metal materials |
-
2003
- 2003-06-11 DE DE60311708T patent/DE60311708D1/en not_active Expired - Lifetime
- 2003-06-11 EP EP03013178A patent/EP1378586B1/en not_active Revoked
- 2003-06-11 AT AT03013178T patent/ATE353987T1/en not_active IP Right Cessation
- 2003-06-12 US US10/459,575 patent/US20040011429A1/en not_active Abandoned
- 2003-06-12 KR KR10-2003-0038011A patent/KR20030096065A/en not_active Application Discontinuation
- 2003-06-13 CN CNB031430287A patent/CN100430518C/en not_active Expired - Lifetime
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197849A (en) * | 1997-03-07 | 1998-11-04 | 日本巴可莱新株式会社 | Metallic surface pretreating liquid and method before formation and treatment of phosphate coating |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1378586B1 (en) | 2007-02-14 |
| CN1470672A (en) | 2004-01-28 |
| ATE353987T1 (en) | 2007-03-15 |
| US20040011429A1 (en) | 2004-01-22 |
| EP1378586A1 (en) | 2004-01-07 |
| DE60311708D1 (en) | 2007-03-29 |
| KR20030096065A (en) | 2003-12-24 |
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