CN105483682A - Phosphating solution for metal treatment and preparation method of phosphating solution - Google Patents
Phosphating solution for metal treatment and preparation method of phosphating solution Download PDFInfo
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- CN105483682A CN105483682A CN201510900020.9A CN201510900020A CN105483682A CN 105483682 A CN105483682 A CN 105483682A CN 201510900020 A CN201510900020 A CN 201510900020A CN 105483682 A CN105483682 A CN 105483682A
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- sodium
- phosphating solution
- phosphating
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910052751 metal Inorganic materials 0.000 title abstract description 19
- 239000002184 metal Substances 0.000 title abstract description 19
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims abstract description 42
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 34
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000011734 sodium Substances 0.000 claims abstract description 25
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 22
- UGTZMIPZNRIWHX-UHFFFAOYSA-K sodium trimetaphosphate Chemical compound [Na+].[Na+].[Na+].[O-]P1(=O)OP([O-])(=O)OP([O-])(=O)O1 UGTZMIPZNRIWHX-UHFFFAOYSA-K 0.000 claims abstract description 22
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 21
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 21
- 235000019395 ammonium persulphate Nutrition 0.000 claims abstract description 21
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 21
- 239000001509 sodium citrate Substances 0.000 claims abstract description 21
- 239000011775 sodium fluoride Substances 0.000 claims abstract description 21
- 235000013024 sodium fluoride Nutrition 0.000 claims abstract description 21
- -1 triazole compound Chemical class 0.000 claims abstract description 21
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000011787 zinc oxide Substances 0.000 claims abstract description 17
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- VGYYSIDKAKXZEE-UHFFFAOYSA-L hydroxylammonium sulfate Chemical compound O[NH3+].O[NH3+].[O-]S([O-])(=O)=O VGYYSIDKAKXZEE-UHFFFAOYSA-L 0.000 claims description 22
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 20
- 150000003839 salts Chemical class 0.000 claims description 20
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 20
- 229940038773 trisodium citrate Drugs 0.000 claims description 20
- 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 claims description 16
- 229910000165 zinc phosphate Inorganic materials 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 19
- 238000010422 painting Methods 0.000 abstract description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 abstract 2
- 229920000388 Polyphosphate Polymers 0.000 abstract 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 abstract 1
- 239000004312 hexamethylene tetramine Substances 0.000 abstract 1
- NXPHCVPFHOVZBC-UHFFFAOYSA-N hydroxylamine;sulfuric acid Chemical compound ON.OS(O)(=O)=O NXPHCVPFHOVZBC-UHFFFAOYSA-N 0.000 abstract 1
- 239000011656 manganese carbonate Substances 0.000 abstract 1
- 235000006748 manganese carbonate Nutrition 0.000 abstract 1
- 229940093474 manganese carbonate Drugs 0.000 abstract 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 abstract 1
- 239000001205 polyphosphate Substances 0.000 abstract 1
- 235000011176 polyphosphates Nutrition 0.000 abstract 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 abstract 1
- 239000011684 sodium molybdate Substances 0.000 abstract 1
- 235000015393 sodium molybdate Nutrition 0.000 abstract 1
- MFXMOUUKFMDYLM-UHFFFAOYSA-L zinc;dihydrogen phosphate Chemical compound [Zn+2].OP(O)([O-])=O.OP(O)([O-])=O MFXMOUUKFMDYLM-UHFFFAOYSA-L 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 55
- 230000000694 effects Effects 0.000 description 16
- 229910019142 PO4 Inorganic materials 0.000 description 15
- 238000005260 corrosion Methods 0.000 description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 13
- 239000010452 phosphate Substances 0.000 description 13
- 230000007797 corrosion Effects 0.000 description 12
- 238000012795 verification Methods 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 9
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 8
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000007921 spray Substances 0.000 description 6
- 230000008901 benefit Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000001680 brushing effect Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 238000002203 pretreatment Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 3
- 239000003929 acidic solution Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000021110 pickles Nutrition 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229960004418 trolamine Drugs 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000010494 dissociation reaction Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000003628 erosive effect Effects 0.000 description 2
- 229910001448 ferrous ion Inorganic materials 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012190 activator Substances 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
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-M dihydrogenphosphate Chemical compound OP(O)([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-M 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 230000003245 working effect Effects 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
- C23C22/40—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 molybdates, tungstates or vanadates
- C23C22/44—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 molybdates, tungstates or vanadates containing also fluorides or complex fluorides
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
The invention discloses a phosphating solution for phosphating the surface of a metal workpiece before painting and a preparation method of the phosphating solution, and further discloses a using method of the phosphating solution. The phosphating solution comprises the following raw materials in parts by weight: 80-150 parts of zinc dihydrogen phosphate, 10-30 parts of zinc oxide, 30-50 parts of phosphoric acid, 2-5 parts of manganese carbonate, 2-4 parts of sodium fluosilicate, 1-5 parts of hydroxylamine sulphate, 4-8 parts of a triazole compound, 2-3 parts of sodium citrate, 10-15 parts of a polyphosphate, 1-3 parts of sodium fluoride, 1-2 parts of ammonium peroxydisulfate, 3-8 parts of sodium molybdate, 1-2 parts of potassium chlorate, 1-3 parts of hexamethylenetetramine, and 3-5 parts of sodium trimetaphosphate.
Description
Technical field
The present invention relates to a kind of Phosphating Solution, especially relate to one and be applicable to parkerized Phosphating Solution of metal works japanning front surface and preparation method thereof, also disclose the using method of this Phosphating Solution simultaneously.
Background technology
Phosphatization is conventional pretreatment technology, principle should belong to the process of chemical transformation film, be mainly used in steel surface phosphatization, and non-ferrous metal (as aluminium, zinc) part also can apply phosphatization.The object of phosphatization mainly provides protection to matrix metal, prevents metal to be corroded to a certain extent; For front bottoming of painting, improve sticking power and the anti-corrosion capability of paint film layer; Antifriction lubrication is played in metal cold complete processing.Carry out processing in the bonderizing of the metal Phosphating Solution that to be iron and steel formed at dihydrogen phosphate, oxygenant, auxiliary agent etc. and the process of phosphatize phosphate coat in a few micron thickness of its Surface Creation, comprise the types such as zinc system zinc cathode, manganese system and iron system.Phosphatize phosphate coat is mainly used as the bottom of coating, and metal cold adds the lubricant film in man-hour, and metal surface protection layer etc., can play antirust, anti-attrition is wear-resisting, lubrication, promotes the multiple effect such as coating and metal base sticking power.Phosphatization can significantly improve sticking power, the protective capacities of coating, and being the gordian technique ensureing coating quality, is the necessary technique of automobile, household electrical appliances, machinery production.The phosphorization technology generally used at present is zinc system middle temperature phosphating, and phosphatization temperature is high, easily produces acid mist, tank liquor is unstable, and sediment is more simultaneously, and phosphatize phosphate coat is thick and heavy, after application, the sticking power of film is lower, and solidity to corrosion is also poor, the nitrite used and heavy-metal pollution environment.In recent years, along with the progress of phosphorization technology, both at home and abroad just at active development quick phosphorization process, its phosphatization temperature is low, less energy consumption, sediment are few, crystal grain is thin, film is thin, the sticking power of film and solidity to corrosion improve a lot.The ubiquitous problem of current domestic phosphorization technology is: phosphatization temperature is high, Phosphating Solution work-ing life is short, washing difficulty is large and cause the problems such as water pollution, not only brings burden to environmental improvement but also consumes the resources such as a large amount of water, phosphoric acid salt.
From the forming process principle of phosphatize phosphate coat, the acidity of solution, oxygenant, catalyzer are the important factors affecting phosphatization speed, conclusive effect is played to phosphatization quality, therefore Phosphating Solution component concentration configuration and adjustment must highly attach the importance, especially the component configuration of oxygenant, catalyzer plays keying action, and research experiment is also prepared at the positive formula to oxygenant, catalyzer by vast scientific research and enterprise.
Summary of the invention
Film forming is quick, film adhesion is strong, solidity to corrosion is good, undertaken operating by brushing or spray, simple to operate, low cost and other advantages to the object of the present invention is to provide one not only to have, and is applicable to Phosphating Solution of large-scale workpiece or outdoor equipment and preparation method thereof.
The raw material composition of this Phosphating Solution is by weight: primary zinc phosphate 80-150 part, zinc oxide 10-30 part, phosphoric acid 30-50 part, manganous carbonate 2-5 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part, triazole compounds 4-8 part, Trisodium Citrate 2-3 part, polyphosphoric acid salt 10-15 part, Sodium Fluoride 1-3 part, ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 part, vulkacit H 1-3 part, ring Trisodium trimetaphosphate 3-5 part, its preparation method is: first zinc oxide 10-30 part dissolved completely by suitable quantity of water in acid-resistant container or Phosphating Slot, add the continuation of phosphoric acid 30-50 part after abundant stirring again to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 80-150 part is added after fully reacting, manganous carbonate 2-5 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part, triazole compounds 4-8 part, Sodium Fluoride 1-3 part, ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 part, vulkacit H 1-3 part, ring Trisodium trimetaphosphate 3-5 part stirs, finally add polyphosphoric acid salt 10-15 part, Trisodium Citrate 2-3 part, and then add suitable quantity of water carry out pH value adjustment stir after.
Compared to existing Phosphating Solution composition and preparation method, above-mentioned Phosphating Solution has following advantage,
1) oxygenant adopted, promotor comprise manganous carbonate, Sodium Silicofluoride, oxammonium sulfate, triazole compounds, Trisodium Citrate, polyphosphoric acid salt, Sodium Fluoride, ammonium peroxydisulfate, Sodium orthomolybdate, Potcrate, vulkacit H, ring Trisodium trimetaphosphate, through verification experimental verification, the configuration of this component can make to prepare the features such as the Phosphating Solution film forming drawn is quick, film adhesion is strong, solidity to corrosion is good;
2) such as, adopt a small amount of appropriate amount of components of oxammonium sulfate can reduce the usage quantity of phosphoric acid to the full extent, thus reduce costs decreasing pollution, what is more important its can accelerate substrate corrosion speed of response and make Fe be oxidized to Fe
2+ferrous ion, thus consume a large amount of hydrogen ion fast, promote that in Phosphating Solution, dissociation goes out a large amount of PO4
3-, with Zn
2+, Fe
2+react and also grow fast at workpiece surface fast deposition place phosphatize phosphate coat nucleus;
3) configuration of the activation promotor of employing Sodium Fluoride 1-3 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part not only can accelerate the formation of phosphatization nucleus, the fine and close erosion resistance of nucleus is strengthened, the phosphatization speed of Phosphating Solution entirety can also be accelerated, promote that phosphate coating is careful;
4) oxygenant adopted is formed by components such as ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 parts, rise and there is very strong oxidisability in an acidic solution, especially between Sodium orthomolybdate and Phosphating Solution main component, there is good coordinating effect, effectively can reduce treatment temp, improve film forming speed, inhibiter can also be played and reduce the effect of phosphatize phosphate coat thickness;
5) add appropriate vulkacit H, mainly it can be used as the agent of buffering metallic material corrosion to use, also can play the effect that Phosphating Solution pH value is regulated; Add appropriate ring Trisodium trimetaphosphate, its role is to generate complex chemical compound and decompose the heavy metal that may exist, be used as dispersion agent and stablizer;
6) appropriate triazole compounds is added, mainly can there is absorption or form title complex in it in metallic surface, the passive film that Sodium orthomolybdate and metal are formed is formed again the new adsorption layer of heterogeneous ring compound, constitute the compound film of one deck three-dimensional net structure, the absorption of heterogeneous ring compound at micropore place plugs the diffusion admittance of metal ion effectively, also prevent CI-to permeate in metal simultaneously, thus significantly reduce the corrosion speed to metal works when having Sodium orthomolybdate component;
7) add polyphosphoric acid salt 10-15 part in the final stage preparing Phosphating Solution, Trisodium Citrate 2-3 part can give full play to it as nucleus adjusting agent and the effect of falling slag agent, through verification experimental verification, compared to conventional art, the method can reduce phosphatization slag and form more than 5-10%.
It should be noted that, oxygenant, promotor being realize low temperature phosphor conditio sune qua non, its solution acidity, oxygenant, catalyzer are the important factors affecting phosphatization speed, conclusive effect is played to phosphatization quality, the concentration low then phosphatization speed of oxygenant, promotor is slow, too low then not film forming, otherwise excessive concentration, phosphatization speed is fast, there will be reaction process too fast, not easily form the situations such as suitable thickness, therefore the formation of said components allocation ratio is determined to need could finally determine through creationary consideration and verification experimental verification.
The invention also discloses a kind of using method of Phosphating Solution, comprise and pending workpiece is carried out phosphatization pre-treatment and bonderizing two steps,
Wherein phosphatization pre-treatment mainly comprises:
1) oil removing: be immersed in acetone soln by pending workpiece, uses ultrasonic cleaner cleaning 10-15min, is fully cleaned by greasy dirt;
2) alkali cleaning: be immersed in by pending workpiece in thermostat water bath and keep 60 DEG C, embathe 15-20min, alkaline wash is the Na of 50g/L
2pO
4, 50g/L Na
2cO
3, and the N of 20g/L
2siO
3mixing solutions, pH value is 7, and thermostat water bath maintains the temperature at 60 DEG C of effects, time about 15-20min;
3) pickling: pickle solution used is the H of 150mL/L
2sO
4, 50mL/L the mixing solutions of trolamine of HF and 30mL/L, control temperature is at about 25 DEG C, and pickling time is about 2min;
4) wash: first clean with deionized water rinsing, but still remain acid solution at body surface especially surface concave, aperture position, easily again get rusty, need to carry out neutralizing treatment after water washing, the sodium carbonate solution of main use 20-40g/L, process 1-2min, then carry out secondary deionized water flushing, cold wind dries up rear stand-by;
Described bonderizing comprises: use acidproof brush directly will prepare gained Phosphating Solution even brushing one deck phosphatization liquid film on workpiece according to the claims 1 method, or use spray gun to spray one deck phosphatization liquid film, or carry out immersion treatment, then dry, the phosphatize phosphate coat compact crystallization that workpiece surface is formed, phosphatization surface without dust, highlight phenomenon generation, rete itself, without fragility, namely reaches processing requirement.
Compared with prior art, the advantage of Phosphating Solution of the present invention is, have that film forming is quick, film adhesion is strong, solidity to corrosion is good, undertaken operating by brushing or spray, simple to operate, low cost and other advantages, the Phosphating Solution of this preparation not only decreases Phosphating Solution sediment, ensures the quality of phosphatize phosphate coat, and even film layer is fine and smooth, applied range model, cost is low, easy to use, is conducive to suitability for industrialized production.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
The raw material composition of described Phosphating Solution is by weight: primary zinc phosphate 80-150 part, zinc oxide 10-30 part, phosphoric acid 30-50 part, manganous carbonate 2-5 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part, triazole compounds 4-8 part, Trisodium Citrate 2-3 part, polyphosphoric acid salt 10-15 part, Sodium Fluoride 1-3 part, ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 part, vulkacit H 1-3 part, ring Trisodium trimetaphosphate 3-5 part, its preparation method is: first zinc oxide 10-30 part dissolved completely by suitable quantity of water in acid-resistant container or Phosphating Slot, add the continuation of phosphoric acid 30-50 part after abundant stirring again to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 80-150 part is added after fully reacting, manganous carbonate 2-5 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part, triazole compounds 4-8 part, Sodium Fluoride 1-3 part, ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 part, vulkacit H 1-3 part, ring Trisodium trimetaphosphate 3-5 part stirs, finally add polyphosphoric acid salt 10-15 part, Trisodium Citrate 2-3 part, and then add suitable quantity of water carry out pH value adjustment stir after.
Compared to existing Phosphating Solution composition and preparation method, above-mentioned Phosphating Solution has following advantage,
1) oxygenant adopted, promotor comprise manganous carbonate, Sodium Silicofluoride, oxammonium sulfate, triazole compounds, Trisodium Citrate, polyphosphoric acid salt, Sodium Fluoride, ammonium peroxydisulfate, Sodium orthomolybdate, Potcrate, vulkacit H, ring Trisodium trimetaphosphate, through verification experimental verification, the configuration of this component has special role, can make to prepare the features such as the Phosphating Solution film forming drawn is quick, film adhesion is strong, solidity to corrosion is good;
2) such as, adopt a small amount of appropriate amount of components of oxammonium sulfate can reduce the usage quantity of phosphoric acid to the full extent, thus reduce costs decreasing pollution, what is more important its can accelerate substrate corrosion speed of response and make FE be oxidized to Fe
2+ferrous ion, thus consume a large amount of hydrogen ion fast, promote that in Phosphating Solution, dissociation goes out a large amount of PO4
3-, with Zn
2+, Fe
2+react and also grow fast at workpiece surface fast deposition place phosphatize phosphate coat nucleus;
3) configuration of the activation promotor of employing Sodium Fluoride 1-3 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part not only can accelerate the formation of phosphatization nucleus, the fine and close erosion resistance of nucleus is strengthened, the phosphatization speed of Phosphating Solution entirety can also be accelerated, promote that phosphate coating is careful;
4) oxygenant adopted is formed by components such as ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 parts, rise and there is very strong oxidisability in an acidic solution, especially between Sodium orthomolybdate and Phosphating Solution main component, there is good coordinating effect, effectively can reduce treatment temp, improve film forming speed, inhibiter can also be played and reduce the effect of phosphatize phosphate coat thickness;
5) add appropriate vulkacit H, mainly it can be used as the agent of buffering metallic material corrosion to use, also can play the effect that Phosphating Solution pH value is regulated; Add appropriate ring Trisodium trimetaphosphate, its role is to generate complex chemical compound and decompose the heavy metal that may exist, be used as dispersion agent and stablizer;
6) appropriate triazole compounds is added, mainly can there is absorption or form title complex in it in metallic surface, the passive film that Sodium orthomolybdate and metal are formed is formed again the new adsorption layer of heterogeneous ring compound, constitute the compound film of one deck three-dimensional net structure, the absorption of heterogeneous ring compound at micropore place plugs the diffusion admittance of metal ion effectively, also prevent CI-to permeate in metal simultaneously, thus significantly reduce the corrosion speed to metal works when having Sodium orthomolybdate component;
7) add polyphosphoric acid salt 10-15 part in the final stage preparing Phosphating Solution, Trisodium Citrate 2-3 part can give full play to it as nucleus adjusting agent and the effect of falling slag agent, through verification experimental verification, compared to conventional art, the method can reduce phosphatization slag and form more than 5-10%.
It should be noted that, oxygenant, promotor being realize low temperature phosphor conditio sune qua non, its solution acidity, oxygenant, catalyzer are the important factors affecting phosphatization speed, conclusive effect is played to phosphatization quality, the concentration low then phosphatization speed of oxygenant, promotor is slow, too low then not film forming, otherwise excessive concentration, phosphatization speed is fast, there will be reaction process too fast, not easily form the situations such as suitable thickness, therefore the formation of above-mentioned allocation ratio needs could finally determine through creationary consideration with through verification experimental verification.The total acidity TA of Phosphating Solution is 50-90 point, in the scope of acidity ratio (TA/FA) for 5-15 point.
Provide following examples and correlation data to prove the technique effect of the application
Embodiment 1
The raw material composition of described Phosphating Solution is by weight: primary zinc phosphate 100 parts, 15 parts, zinc oxide, phosphatase 24 0 part, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 4 parts, triazole compounds 4 parts, Trisodium Citrate 2 parts, polyphosphoric acid salt 10 parts, Sodium Fluoride 2 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 1 part, Potcrate, vulkacit H 1 part, ring Trisodium trimetaphosphate 3 parts
Its preparation method is: first dissolved completely by 15 parts, zinc oxide by suitable quantity of water in acid-resistant container or Phosphating Slot, add phosphatase 24 0 part after abundant stirring again to continue to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 100 parts is added after fully reacting, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 4 parts, triazole compounds 4 parts, Sodium Fluoride 2 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 1 part, Potcrate, vulkacit H 1 part, ring Trisodium trimetaphosphate 3 parts stirs, finally add polyphosphoric acid salt 10 parts, Trisodium Citrate 2 parts, and then add suitable quantity of water carry out pH value adjustment stir after.
Embodiment 2
The raw material composition of described Phosphating Solution is by weight: primary zinc phosphate 100 parts, 15 parts, zinc oxide, phosphatase 24 0 part, manganous carbonate 2 parts, Sodium Silicofluoride 3.5 parts, oxammonium sulfate 4 parts, triazole compounds 4 parts, Trisodium Citrate 2 parts, polyphosphoric acid salt 10 parts, Sodium Fluoride 3 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 2 parts, Potcrate, vulkacit H 1 part, ring Trisodium trimetaphosphate 3 parts, can find out, compared to embodiment 1, add activator component configuration.
Its preparation method is: first dissolved completely by 15 parts, zinc oxide by suitable quantity of water in acid-resistant container or Phosphating Slot, add phosphatase 24 0 part after abundant stirring again to continue to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 100 parts is added after fully reacting, manganous carbonate 2 parts, Sodium Silicofluoride 3.5 parts, oxammonium sulfate 4 parts, triazole compounds 4 parts, Sodium Fluoride 3 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 2 parts, Potcrate, vulkacit H 1 part, ring Trisodium trimetaphosphate 3 parts stirs, finally add polyphosphoric acid salt 10 parts, Trisodium Citrate 2 parts, and then add suitable quantity of water carry out pH value adjustment stir after.
Embodiment 3
The raw material composition of described Phosphating Solution is by weight: primary zinc phosphate 100 parts, 15 parts, zinc oxide, phosphatase 24 0 part, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 4 parts, triazole compounds 6 parts, Trisodium Citrate 2 parts, polyphosphoric acid salt 10 parts, Sodium Fluoride 2 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 8 parts, 2 parts, Potcrate, vulkacit H 1 part, ring Trisodium trimetaphosphate 3 parts, can find out, compared to embodiment 1, add oxidant constituents configuration.
Its preparation method is: first dissolved completely by 15 parts, zinc oxide by suitable quantity of water in acid-resistant container or Phosphating Slot, add phosphatase 24 0 part after abundant stirring again to continue to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 100 parts is added after fully reacting, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 4 parts, triazole compounds 6 parts, Sodium Fluoride 2 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 8 parts, 2 parts, Potcrate, vulkacit H 1 part, ring Trisodium trimetaphosphate 3 parts stirs, finally add polyphosphoric acid salt 10 parts, Trisodium Citrate 2 parts, and then add suitable quantity of water carry out pH value adjustment stir after.
Embodiment 4
The raw material composition of described Phosphating Solution is by weight: primary zinc phosphate 100 parts, 15 parts, zinc oxide, phosphatase 24 0 part, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 4 parts, triazole compounds 4 parts, Trisodium Citrate 2 parts, polyphosphoric acid salt 10 parts, Sodium Fluoride 2 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 1 part, Potcrate, vulkacit H 2 parts, ring Trisodium trimetaphosphate 5 parts, can find out, compared to embodiment 1, have adjusted vulkacit H and the configuration of ring Trisodium trimetaphosphate component.
Its preparation method is: first dissolved completely by 15 parts, zinc oxide by suitable quantity of water in acid-resistant container or Phosphating Slot, add phosphatase 24 0 part after abundant stirring again to continue to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 100 parts is added after fully reacting, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 4 parts, triazole compounds 4 parts, Sodium Fluoride 2 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 1 part, Potcrate, vulkacit H 2 parts, ring Trisodium trimetaphosphate 5 parts stirs, finally add polyphosphoric acid salt 10 parts, Trisodium Citrate 2 parts, and then add suitable quantity of water carry out pH value adjustment stir after.
Embodiment 5
The raw material composition of described Phosphating Solution is by weight: primary zinc phosphate 80 parts, 10 parts, zinc oxide, phosphoric acid 30 parts, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 2.5 parts, triazole compounds 6 parts, Trisodium Citrate 2 parts, polyphosphoric acid salt 10 parts, Sodium Fluoride 1.5 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 2 parts, Potcrate, vulkacit H 2 parts, ring Trisodium trimetaphosphate 4 parts
Its preparation method is: first dissolved completely by 10 parts, zinc oxide by suitable quantity of water in acid-resistant container or Phosphating Slot, add phosphoric acid 30 parts after abundant stirring again to continue to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 80 parts is added after fully reacting, manganous carbonate 2 parts, Sodium Silicofluoride 2 parts, oxammonium sulfate 2.5 parts, triazole compounds 6 parts, Sodium Fluoride 1.5 parts, ammonium peroxydisulfate 2 parts, Sodium orthomolybdate 5 parts, 2 parts, Potcrate, vulkacit H 2 parts, ring Trisodium trimetaphosphate 4 parts stirs, finally add polyphosphoric acid salt 10 parts, Trisodium Citrate 2 parts, and then add suitable quantity of water carry out pH value adjustment stir after.
The Phosphating Solution obtained by above-described embodiment 1-5 carries out bonderizing to same metal works, environmental parameter: room temperature 20 DEG C, normal pressure, humidity 70%, and its efficacy parameter is compared as follows:
Simultaneously, only pay attention to production link in the industrial production of current China and ignore practice construction application, the application that the product made can not get, and then corresponding technique effect cannot be realized, therefore the invention also discloses a kind of using method of Phosphating Solution, comprise and pending workpiece is carried out phosphatization pre-treatment and bonderizing two steps, phosphatization pre-treatment mainly comprises:
1) oil removing: be immersed in acetone soln by pending workpiece, uses ultrasonic cleaner cleaning 10-15min, is fully cleaned by greasy dirt;
2) alkali cleaning: be immersed in by pending workpiece in thermostat water bath and keep 60 DEG C, embathe 15-20min, alkaline wash is the Na of 50g/L
2pO
4, 50g/L Na
2cO
3, and the N of 20g/L
2siO
3mixing solutions, pH value is 7, and thermostat water bath maintains the temperature at 60 DEG C of effects, time about 15-20min, adopts the object of ultrasonic cleaning and alkali liquor oil removing to be the cold working chip, grease and the dirt that adhere to remove specimen surface better;
3) pickling: pickle solution used is the H of 150mL/L
2sO
4, 50mL/L the mixing solutions of trolamine of HF and 30mL/L, control temperature is at about 25 DEG C, and pickling time is about 2min.This pickle solution is with sulfuric acid for main acid, and coordinate and add fused with hydrofluoric acid and trolamine, adopt the acidic solution of this formulation components to be mainly used in high quality steel and stainless process, it fast and effeciently can remove the oxide compound of workpiece surface.
4) wash: first clean with deionized water rinsing, but still remain acid solution at body surface especially surface concave, aperture position, easily again get rusty, need to carry out neutralizing treatment after water washing, the sodium carbonate solution of main use 20-40g/L, process 1-2min, then carry out secondary deionized water flushing, cold wind dries up rear stand-by;
Described bonderizing comprises: use acidproof brush directly to be prepared by above-described embodiment 1-5 method gained Phosphating Solution even brushing one deck phosphatization liquid film on workpiece, or use spray gun to spray one deck phosphatization liquid film, or carry out immersion treatment, then dry, the phosphatize phosphate coat compact crystallization that workpiece surface is formed, phosphatization surface without dust, highlight phenomenon generation, rete itself, without fragility, namely reaches processing requirement.
Although give detailed description and explanation to the specific embodiment of the present invention above; but what should indicate is; we can carry out various equivalence according to conception of the present invention to above-mentioned embodiment and change and amendment; its function produced do not exceed that specification sheets contains yet spiritual time, all should within protection scope of the present invention.The above; be only preferred embodiment of the present invention; not in order to limit the present invention, every above embodiment is done according to technical spirit of the present invention any trickle amendment, equivalently replace and improve, within the protection domain that all should be included in technical solution of the present invention.
Claims (1)
1. the preparation method of a Phosphating Solution, the raw material composition of this Phosphating Solution is by weight: primary zinc phosphate 80-150 part, zinc oxide 10-30 part, phosphoric acid 30-50 part, manganous carbonate 2-5 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part, triazole compounds 4-8 part, Trisodium Citrate 2-3 part, polyphosphoric acid salt 10-15 part, Sodium Fluoride 1-3 part, ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 part, vulkacit H 1-3 part, ring Trisodium trimetaphosphate 3-5 part, concrete preparation method for first dissolving zinc oxide 10-30 part completely by suitable quantity of water in acid-resistant container or Phosphating Slot, add the continuation of phosphoric acid 30-50 part after abundant stirring again to stir, be heated to 100-120 DEG C of insulation fully react for 2 hours, primary zinc phosphate 80-150 part is added after fully reacting, manganous carbonate 2-5 part, Sodium Silicofluoride 2-4 part, oxammonium sulfate 1-5 part, triazole compounds 4-8 part, Sodium Fluoride 1-3 part, ammonium peroxydisulfate 1-2 part, Sodium orthomolybdate 3-8 part, Potcrate 1-2 part, vulkacit H 1-3 part, ring Trisodium trimetaphosphate 3-5 part stirs, finally add polyphosphoric acid salt 10-15 part, Trisodium Citrate 2-3 part, and then add suitable quantity of water carry out pH value adjustment stir after.
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| CN109136873A (en) * | 2018-09-05 | 2019-01-04 | 合肥久新不锈钢厨具有限公司 | A kind of preparation method of abrasion-proof stainless steel composite board |
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