CN114807920B - 一种锈蚀转化剂的制备 - Google Patents
一种锈蚀转化剂的制备 Download PDFInfo
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- CN114807920B CN114807920B CN202210484557.1A CN202210484557A CN114807920B CN 114807920 B CN114807920 B CN 114807920B CN 202210484557 A CN202210484557 A CN 202210484557A CN 114807920 B CN114807920 B CN 114807920B
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- gallate
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 53
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 230000000149 penetrating effect Effects 0.000 claims abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 15
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 claims description 13
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 7
- 235000004515 gallic acid Nutrition 0.000 claims description 7
- 229940074391 gallic acid Drugs 0.000 claims description 7
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 229920001223 polyethylene glycol Polymers 0.000 claims description 5
- 229920000180 alkyd Polymers 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 230000001131 transforming effect Effects 0.000 abstract description 6
- 239000003973 paint Substances 0.000 abstract description 4
- XOPOEBVTQYAOSV-UHFFFAOYSA-N butyl 3,4,5-trihydroxybenzoate Chemical compound CCCCOC(=O)C1=CC(O)=C(O)C(O)=C1 XOPOEBVTQYAOSV-UHFFFAOYSA-N 0.000 abstract description 2
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 230000002860 competitive effect Effects 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 25
- 239000010959 steel Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 25
- 239000007921 spray Substances 0.000 description 22
- 150000003839 salts Chemical class 0.000 description 21
- 230000000694 effects Effects 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- 239000010410 layer Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 6
- 230000007797 corrosion Effects 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910000975 Carbon steel Inorganic materials 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000010962 carbon steel Substances 0.000 description 4
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000007935 neutral effect Effects 0.000 description 4
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 3
- 239000001263 FEMA 3042 Substances 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products 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-PPKXGCFTSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- LRBQNJMCXXYXIU-QWKBTXIPSA-N gallotannic 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-QWKBTXIPSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 235000015523 tannic acid Nutrition 0.000 description 3
- 229940033123 tannic acid Drugs 0.000 description 3
- 229920002258 tannic acid Polymers 0.000 description 3
- 229910002588 FeOOH Inorganic materials 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- RAOSIAYCXKBGFE-UHFFFAOYSA-K [Cu+3].[O-]P([O-])([O-])=O Chemical compound [Cu+3].[O-]P([O-])([O-])=O RAOSIAYCXKBGFE-UHFFFAOYSA-K 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 239000012670 alkaline solution 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
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical group 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- -1 gallic acid n-pentyl ester Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- FLFJVPPJGJSHMF-UHFFFAOYSA-L manganese hypophosphite Chemical compound [Mn+2].[O-]P=O.[O-]P=O FLFJVPPJGJSHMF-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 229960004838 phosphoric acid Drugs 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000009466 transformation Effects 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
- 238000005303 weighing Methods 0.000 description 1
- LRXTYHSAJDENHV-UHFFFAOYSA-H zinc phosphate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LRXTYHSAJDENHV-UHFFFAOYSA-H 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
Classifications
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- 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
- C23C22/23—Condensed phosphates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- 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
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- 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
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- 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
- C23C22/12—Orthophosphates containing zinc cations
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- 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
- C23C22/18—Orthophosphates containing manganese cations
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- 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
- C23C22/18—Orthophosphates containing manganese cations
- C23C22/186—Orthophosphates containing manganese cations containing also copper cations
Abstract
本发明公开了一种锈蚀转化剂的制备，该锈蚀转化剂以质量计，总计100份，由如下按质量计的组份构成：主转化剂18‑22份，副转化剂5‑9份，成膜剂2‑4份，渗透剂40‑60份，去离子水5‑35份；其中主转化剂为没食子酸正戊酯，没食子酸正丁酯，没食子酸正己酯中的一种或几种。本发明的防锈蚀涂料防锈功能优良，转化层稳定，成本低，流程短，具有明显的竞争优势。
Description
技术领域
本发明属于钢件表面防锈蚀涂装技术领域，涉及一种新型锈蚀转化剂的制备。
背景技术
化工行业中钢构件为相当基本的材料，随着我国化工行业的逐渐发展，钢构件逐渐增多，逐年增加的钢构件也会由于天气和环境原因出现锈蚀的情况，对钢构件的质量会造成巨大的影响，进而产生生产安全隐患和经济损失。据统计，全球每年因锈蚀而报废的钢构件达14亿公斤以上，接近全世界钢铁产量的30％，因此开发一种实用性锈蚀转化剂具有重要的意义。对于传统的涂料，其在进行漆涂之前须将钢构件表面的锈层或其他杂质清除，表面除锈成本高且工作强度大，成本可以占据整个涂装工程的45％。同时，由于目前锈蚀转化剂所用的转化剂主要为磷酸，没食子酸，单宁酸等，其酸性体系会对内部的钢构件进行进一步的腐蚀，腐蚀过程中可能会产生的气体也会进一步影响到膜层的附着性。
专利CN105386065B公开了一种除锈和防锈体系，其使用了氢氟酸、盐酸和草酸等作为其主要成分，无机强酸易渗透过防锈体系将基底也腐蚀掉，同时这些强酸挥发也会造成空气污染以及对人体有害。专利CN102191492B采用了多聚磷酸和单宁酸醋酸作为锈转化体系的主成分，电化学表征表明其可以提高体系的电化学阻抗，然而其整体抗锈能力较低。专利CN103756512B公开了一种双组份的防腐蚀涂料，盐雾试验结果较好，然而其各组分的制备过程以及条件较为严苛。专利CN105585939B公开了一种利用了纳米容器缓释技术的自修复涂层锈转化功能体系，该体系的效果优良，然而对于工业条件而言，纳米容器技术所带来的技术和生产成本显然是不可承担的。
本发明针对上述问题进行了创新，提出了一种新型锈转化体系。
发明内容
本发明的目的在于解决上述问题，提供一种工艺简单、成本低廉、同时除锈防锈蚀效果优良的环保型锈蚀转化剂及其制备方法。
本发明提供的锈蚀转化剂由主转化剂、副转化剂、成膜剂、渗透剂、以及溶剂去离子水组成。
其中以质量计，总计100份，各组分及其含量如下：
主转化剂，18-22份
副转化剂，5-9份
成膜剂，2-4份
渗透剂，40-60份
去离子水，5-35份
所述主转化剂为没食子酸正戊酯，没食子酸正丁酯，没食子酸正己酯中的一种或几种。通过在没食子酸中引入直链单元醇，一方面通过酯化反应消除了没食子酸中较强的羧酸部分，而保护了用于跟铁原子螯合的羟基部分，另一方面通过引入多碳直链，通过其超共轭给电子作用，强化了电子云在羟基的密度分布，从而强化了羟基与铁原子的螯合作用。单元醇采用了4-6个碳原子的醇(正戊醇、正丁醇、正己醇)，以便避免由于侧链过长导致的空间位阻效应影响到成膜的质量，同时不会由于链长过长导致给电子效应降低。
所述副转化剂为多聚磷酸，三聚磷酸铝，磷酸铜，磷酸锌，次磷酸锰中的一种或几种。副转化剂中的磷酸基同样具有和铁原子鳌合的作用，其他金属离子的引入可以避免成膜过程中铁螯合物的过度凝聚而使防锈膜分布不均。
所述成膜剂为聚乙二醇，渗透剂为异丙醇。其中聚乙二醇相较于苯丙乳液具有无刺激性、稳定性好等特点，异丙醇具有良好的渗透性，可以将主转化剂带入锈层，且两者成本低廉，工艺简单。
本发明上述的主转化的制备方法，其特征在于，是经过以下流程制备得到，
将没食子酸、直链单元醇混合后，加入催化剂浓硫酸加热至溶液呈澄清；
保持温度并在微波反应器中反应；
分别采用碱液和饱和氯化钠溶液进行多次萃取；
减压蒸馏；
结晶干燥。
进一步优选的，所述直链单元醇为正戊醇、正丁醇、正己醇中的一种或几种。
进一步优选的，反应温度110-130℃，反应时间60-80min，醇酸比(8-10)∶1，催化剂用
量0.5-1ml。
进一步优选的，所述碱液为饱和碳酸氢钠溶液。
进一步优选的，所述减压蒸馏的真空度为0.065MPa。
附图说明
图1为制备例10的没食子酸正戊酯红外光谱图。
图2为制备例10的没食子酸正戊酯核磁共振氢谱图。
图3为不同浓度，pH值转锈剂处理后钢片微观形貌SEM图，
1)、6)0.05g/mL，pH＝4；2)、7)0.05g/mL，pH＝5；3)、8)0.05g/mL，pH＝6；
4)、9)0.10g/mL，pH＝4；5)10)0.20g/mL，pH＝4。
图4为经处理钢片与未处理钢片盐雾试验图，
a0)、a1)、a2)、a3)、a4)经处理钢片0h，12h，24h，36h，48h，
b0)、b1)、b2)、b3)、b4)未处理钢片0h，12h，24h，36h，48h。
图5为实施例15经盐雾试验之后的照片，
A)0小时，B)192小时，C)360小时，D)504小时。
图6为实施例17经盐雾试验之后的照片，
A)0小时，B)192小时，C)360小时，D)504小时。
图7为实施例15的504h盐雾试验之后的A3碳钢片高分辨率金相图。
图8为实施例17的504h盐雾试验之后的A3碳钢片高分辨率金相图。
图9为铁锈与实施例17转化后的锈蚀层的XRD图。
图10为实施例17的SEM图。
具体实施方式
没食子酸正戊酯的制备例
按表1所示质量比分别称取没食子酸和正戊醇，混合后加入浓硫酸，预加热至溶液呈澄清，于66W微波反应器中反应。冷却后，用等体积的饱和碳酸氢钠溶液萃取三次，再用等体积饱和氯化钠溶液萃取三次。将所得有机相进行减压蒸馏，真空度为0.065MPa。蒸馏完毕后用与蒸馏液等体积的乙醇溶解，减压蒸馏，真空度为0.065MPa。将所得的产物取出倒入500ml去离子水中，放入4℃冰箱冷却12hr。冷却完成之后抽滤，所得粘稠状产物加热至液态，然后搅拌，至没有气泡产生，停止加热。将所得的液体在搅拌环境下冷却，至液体变为固体颗粒，将固体颗粒研磨得到红棕色粉末。
表1.具体制备例中使用各工艺参数的说明
表2.具体制备例情况：
由表中数据可看出各因素对于产率的影响程度从大到小依次为：醇酸比，温度，反应时间，催化剂用量，醇酸比是对合成没食子酸正戊酯影响最大的条件。该反应为可逆反应，过量的正戊醇有利于反应向正方向进行，同时正戊醇也是带水剂，与水形成共沸物，将反应中的生成水带出，更加有利于反应的进行，所以合适的醇酸比对反应起着至关重要的作用。温度对反应也有着重要的作用，温度过低，分子间碰撞过少，较高的温度能加快反应的速率。反应时间也不能过短，过短的反应时间反应尚未进行完全，也会影响到最终的产率。
按产率，上述实施结果表明的优化的工艺条件范围为反应温度110-130℃，反应时间60-80min，醇酸比(8-10)∶1，催化剂用量0.5-1ml。
取制备例10的条件制备出来的没食子酸正戊酯进行下述表征实验。
将溴化钾和没食子酸正戊酯按质量比200∶1均匀混合，压成薄片进行红外光谱分析。
图1的红外结果说明，在3513cm-1，3413cm-1，3386cm-1出现三个酚羟基伸缩振动吸收峰，2958cm-1处出现-CH3基团的反对称伸缩振动及在2931cm-1处为-CH2基团的强吸收峰，在1683cm-1和1249cm-1处出现强的羰基和酯基伸缩振动特征吸收峰，表明有C＝O和-COO-基团存在，1083cm-1处为苯环C-H面内弯曲振动。在波长1033cm-1处为苯环C-H面外弯曲振动，综合红外图谱和特征基团的出峰信息，表明最终产物为没食子酸正戊酯。
图2的核磁共振氢谱图出现了7.05ppm2H，4.23pmm(m，2H)，1.74ppm(m，2H)，1.39ppm(m，4H)，0.90ppm(m，3H)的峰，基本与标准化学位移相符，表明该产物为没食子酸正戊酯，且纯度较高。
使用25mm×25mm×3mmA3碳钢样片，先将样片用60目砂纸进行打磨抛光，去除表面的保护层和油污，再用去离子水和酒精先后清洗多次，清洗完毕后放入真空干燥箱干燥1h，然后放入盐雾试验箱进48h的盐雾试验，中性盐雾试验参照GB/T10125-2012《人造气氛腐蚀试验盐雾试验》进行，在试验箱内，以浓度为5％的NaCl溶液进行喷雾实验，pH值控制在6.5-7.2之间，设定中性盐雾试验箱温度为35℃，将上述处理之后的钢片在盐雾箱中放置，使钢板测试面积与垂直方向成的夹角在15°-30°之间。48h后取出锈蚀钢片，放入真空干燥箱中干燥1h，干燥完毕后取出。
主转化剂的应用实施例。
实施例1-5：
使用电子天平精准称量一定量的没食子酸正戊酯，以异丙醇为溶剂溶解没食子酸正戊酯，用微量乙酸调节pH值，得到锈转化剂，用胶头滴管分别均匀滴于三块锈蚀钢板上，每次滴加六滴，每次间隔10min，滴加三次，30min后用吹风机吹干。
表3.具体实施方案：
| 实施例编号 | pH | 浓度(g/ml) |
| 1 | 4 | 0.05 |
| 2 | 5 | 0.05 |
| 3 | 6 | 0.05 |
| 4 | 4 | 0.10 |
| 5 | 4 | 0.2 |
从图3可知用浓度为0.2g/mL，pH＝4的转化剂处理后的钢片化面较为平整，且不存
在裂痕，膜的表观质量较好。同时也说明pH较高的情况下成膜效果不理想。
按上述条件配置溶液，用胶头滴管分别均匀滴于带锈钢片上，每次滴加六滴，每次间隔10min，滴加三次，30min后用吹风机吹干。将处理后的钢板放入盐雾试验箱，进行盐雾试验，参照GB/T10125-2012《人造气氛腐蚀试验盐雾试验》进行。经过主转化剂处理和前述未经主转化剂处理的盐雾试验结果如图4所示。
经过上述处理的钢板表明有了一层黑色转化物保护膜，可起到隔绝外界，减缓锈蚀。经过48h的中性盐雾试验，处理后的钢板表面转化层基本失去保护作用，锈蚀层基本布满整个钢板表面。
该实施例结果表明，仅使用没食子酸正戊酯和溶剂即可具备一定的防锈作用，但是效果比较差，远达不到使用效果。
锈蚀转化剂的实施例6-21：
取没食子酸正戊酯，多聚磷酸，聚乙二醇，异丙醇，去离子水，搅拌均匀得到棕红色溶液，即为锈蚀转化剂。
其中各组分的含量如下表所示：
表4.各实施例水平设计
| 序号 | A没食子酸正戊酯(％) | B多聚磷酸(％) | C聚乙二醇(％) | D异丙醇(％) |
| 1 | 10 | 3 | 1 | 30 |
| 2 | 15 | 5 | 2 | 40 |
| 3 | 20 | 7 | 3 | 50 |
| 4 | 25 | 9 | 4 | 60 |
表5.各实施例
| 编号 | A(g) | B(g) | C(g) | D(g) | 蒸馏水(g) | 阻锈时间(h) |
| 6 | A1(＝3) | B1(＝0.9) | C1(＝0.3) | D1(＝9) | 15.675 | 12 |
| 7 | A1 | B2(＝1.5) | C2(＝0.6) | D2(＝12) | 11.025 | 24 |
| 8 | A1 | B3(＝2.1) | C3(＝0.9) | D3(＝15) | 6.375 | 24 |
| 9 | A1 | B4(＝2.7) | C4(＝1.2) | D4(＝18) | 1.725 | 24 |
| 10 | A2(＝4.5) | B1 | C1 | D1 | 7.875 | 72 |
| 11 | A2 | B2 | C2 | D2 | 3.825 | 36 |
| 12 | A2 | B3 | C3 | D3 | 10.575 | 24 |
| 13 | A2 | B4 | C4 | D4 | 6.525 | 36 |
| 14 | A3(＝6) | B1 | C1 | D1 | 3.075 | 144 |
| 15 | A3 | B2 | C2 | D2 | 4.425 | 480 |
| 16 | A3 | B3 | C3 | D3 | 6.975 | 24 |
| 17 | A3 | B4 | C4 | D4 | 8.325 | 504 |
| 18 | A4(＝7.5) | B1 | C1 | D1 | 7.275 | 24 |
| 19 | A4 | B2 | C2 | D2 | 9.225 | 24 |
| 20 | A4 | B3 | C3 | D3 | 0 | 24 |
| 21 | A4 | B4 | C4 | D4 | 1.125 | 96 |
将制备好的锈蚀转化剂均匀涂在生锈的25mm×25mm×3mmA3碳钢片上，放入盐雾试验箱，在35℃的条件下进行盐雾试验(GB/T10125-2012)，每12h拍照观察，至表面出现铁锈。最终中性盐雾试验下生锈时间为504h。
图5-6展示了最优的实施例15和17经盐雾试验后的实物照片。
图7-8表明经过锈蚀转化剂处理，再经504h盐雾试验，实施例15样片表面出现小面积的铁锈，而实施例17号样片的铁锈就显得比较稀少。这两组转化剂的配比中主转化剂的含量相同，说明转化层中的磷酸基的含量影响了锈蚀层的转化能力。
对实施例17号进行如下分析。
经图9XRD分析，FeOOH的衍射峰在26.725°，35.161°，43.768°，48.862°，52.046°，52.882°出现。Fe3O4的衍射峰在36.82°出现，Fe2O3的衍射峰在33.152°，43.518°，56.15°，69.599°出现，FeO的衍射峰在72.582°和77.057°出现，说明铁锈中含有大量的FeOOH、Fe3O4和FeO，而经锈蚀转化剂处理之后样片表面物质分析，图谱中各锈蚀成分出峰强度明显降低，部分峰消失，说明锈蚀转化剂完成对铁锈组分的转化。
图10的SEM图表明该锈转化剂转化之后的锈转化层表面较为平整，无裂痕，锈层基本完全转化。
Claims (3)
1.一种锈蚀转化剂，其特征在于，以质量计，总计100份，由如下的组分构成：主转化剂没食子酸正戊酯20份，副转化剂多聚磷酸9份，成膜剂聚乙二醇4份，渗透剂异丙醇60份，去离子水7份；
所述主转化剂是经过以下流程制备得到：
将没食子酸、正戊醇混合后，加入浓硫酸加热至溶液呈澄清；
保持温度并在微波反应器中反应；
分别采用碱液和饱和氯化钠溶液萃取；
减压蒸馏；
结晶干燥；
反应温度110-130℃，反应时间60-80min，醇酸质量比10∶1，催化剂用量0.5-1ml。
2.一种如权利要求1所述的锈蚀转化剂，其特征在于，所述碱液为饱和碳酸氢钠溶液。
3.一种如权利要求1所述的锈蚀转化剂，其特征在于，所述减压蒸馏的真空度为0.065MPa。
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| FR1014694A (fr) * | 1949-03-16 | 1952-08-20 | Eastman Kodak Co | Concentrats de mélanges antioxygènes pour graisses et huiles |
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| CN101585769A (zh) * | 2009-07-09 | 2009-11-25 | 南京中医药大学 | 没食子酸酯的微波合成方法 |
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