CN115522191B - Phosphating solution for metal surface treatment and preparation method and application thereof - Google Patents
Phosphating solution for metal surface treatment and preparation method and application thereof Download PDFInfo
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- CN115522191B CN115522191B CN202211239151.3A CN202211239151A CN115522191B CN 115522191 B CN115522191 B CN 115522191B CN 202211239151 A CN202211239151 A CN 202211239151A CN 115522191 B CN115522191 B CN 115522191B
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 39
- 239000002184 metal Substances 0.000 title claims abstract description 39
- 238000004381 surface treatment Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 95
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 53
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 53
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 28
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 21
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 20
- 239000011787 zinc oxide Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000005260 corrosion Methods 0.000 claims abstract description 17
- 230000007797 corrosion Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000004321 preservation Methods 0.000 claims abstract description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 239000005543 nano-size silicon particle Substances 0.000 claims description 7
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Substances CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 239000008139 complexing agent Substances 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims description 2
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 2
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 2
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims 1
- 229940124274 edetate disodium Drugs 0.000 claims 1
- 125000005456 glyceride group Chemical group 0.000 claims 1
- 239000002893 slag Substances 0.000 abstract description 4
- 230000008961 swelling Effects 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 229910019142 PO4 Inorganic materials 0.000 description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 8
- 239000010452 phosphate Substances 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- 229910000976 Electrical steel Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 4
- 238000002161 passivation Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000008236 heating water Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 241000289690 Xenarthra Species 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000010953 base metal Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc 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
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/50—Treatment of iron or alloys based thereon
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 relates to a phosphating solution for metal surface treatment, and a preparation method and application thereof. The phosphating solution comprises the following components in parts by weight per liter: water liter, 41-45 g of phosphoric acid, 24.5-29 g of zinc oxide, 20-24.5 g of nitric acid and 1.5-2.2 g of polyvinyl alcohol. The preparation method of the phosphating solution for metal surface treatment comprises the following steps: (1) Adding the polyvinyl alcohol powder into the water, continuously stirring for a period of time to enable the polyvinyl alcohol powder to swell, and stirring the obtained mixed solution under the heating condition after the swelling is completed to enable the polyvinyl alcohol powder to be fully dissolved, so as to obtain a polyvinyl alcohol solution for standby. (2) And adding the phosphoric acid, zinc oxide and nitric acid under the condition of heat preservation, and stirring uniformly to obtain the phosphating solution. The phosphating solution disclosed by the invention not only can enable a denser phosphating film to be formed on the surface of a metal workpiece and improve corrosion resistance, but also can reduce the generation of phosphating slag.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a phosphating solution for metal surface treatment, and a preparation method and application thereof.
Background
The information disclosed in the background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an admission or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Phosphating is a common pretreatment technology, is mainly applied to the phosphating of the surface of steel, and is one of the purposes of phosphating is to provide protection for the base metal and prevent the metal from being corroded to a certain extent. At present, the phosphating treatment method mainly comprises the steps of immersing a metal workpiece in a phosphoric acid solution containing manganese, iron, zinc and the like, so that a phosphate protective film which is difficult to dissolve in water is formed on the surface of the metal workpiece. However, a certain pore exists in a phosphate film formed on the surface of a metal matrix by a lot of phosphate liquid, and the pore is an important factor influencing the corrosion resistance of the phosphate film, so that the reduction of the porosity of the surface of the phosphate film is beneficial to further improving the corrosion resistance of the material.
The prior method for solving the problems mainly comprises the following passivation treatment after phosphating, namely reprocessing the metal workpiece subjected to phosphating by using passivation solution, which not only increases the complexity of the phosphating process, but also causes the problem of environmental pollution if the waste passivation solution is improperly treated. In addition, the traditional phosphating solution is easy to generate more phosphating slag in the metal surface treatment process, the research surface is researched, a large amount of phosphating slag is generated, the service life of the phosphating solution is shortened, the phosphating cost is improved, the quality of a phosphating film is also influenced, and even the normal operation of production is influenced, so that the development of a novel phosphating solution capable of overcoming the problems is necessary.
Disclosure of Invention
In view of the above, the invention provides a phosphating solution for metal surface treatment, a preparation method and application thereof, which not only can enable a more compact phosphating film to be formed on the surface of a metal workpiece and improve corrosion resistance, but also can reduce the generation of phosphating slag. In order to achieve the above purpose, the present invention discloses the following technical solutions:
In a first aspect, the invention discloses a phosphating solution for metal surface treatment, which comprises the following components in percentage by liter of phosphating solution: water liter, 41-45 g of phosphoric acid, 24.5-29 g of zinc oxide, 20-24.5 g of nitric acid and 1.5-2.2 g of polyvinyl alcohol.
In some typical embodiments, the phosphating solution also includes complexing agent in the range of 0.05 to 0.2g/L. Optionally, the complexing agent includes any one of tartaric acid (C 4H6O6), citric acid (C 6H8O7), disodium edentate (EDTA-2 Na), and the like.
In some typical embodiments, the phosphating solution also includes 0.005 to 0.01g/L of corrosion inhibitor. Optionally, the corrosion inhibitor comprises any one of di-o-toluene thiourea, hexamethylenetetramine, thiourea, urea and the like.
In some typical embodiments, the phosphating solution further includes 0.002 to 0.04g/L of a surfactant. Alternatively, the surfactant includes any one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, fatty acid glyceride, and the like.
In some typical embodiments, the phosphating solution further includes inorganic nanoparticles in an amount of 0.5 to 0.85g/L. Alternatively, the inorganic nanoparticles include any one of nano silica, nano titania, nano silicon nitride, and the like. The inorganic nano ions are helpful for improving the corrosion resistance of the phosphating film.
In some typical embodiments, the phosphating solution further includes 0.7 to 1.1g/L of a promoter. Optionally, the metal accelerator includes a substance capable of providing a source of at least one metal ion of Ni 2+、Mn2+、Ca2+, preferably at least one of nickel nitrate, manganese nitrate, calcium nitrate, and the like. The accelerator is helpful for accelerating the generation of the phosphate film and the refinement of phosphate film grains, thereby promoting the compactness of the phosphate film.
In a first aspect, the invention discloses a preparation method of the phosphating solution for metal surface treatment, which comprises the following steps:
(1) Adding the polyvinyl alcohol powder into the water, continuously stirring for a period of time to enable the polyvinyl alcohol powder to swell, and stirring the obtained mixed solution under the heating condition after the swelling is completed to enable the polyvinyl alcohol powder to be fully dissolved, so as to obtain a polyvinyl alcohol solution for standby.
(2) And adding the phosphoric acid, zinc oxide and nitric acid under the condition of heat preservation, and stirring uniformly to obtain the phosphating solution.
In some typical embodiments, in step (1), the continuous stirring time is 20 to 35 minutes, facilitating the dispersion of the polyvinyl alcohol powder in water, preventing caking, affecting the subsequent dissolution rate in hot water.
In some typical embodiments, in step (1), the heating temperature is from 70 to 85 ℃ to facilitate sufficient dissolution of the polyvinyl alcohol powder.
In some typical embodiments, in step (2), the holding temperature is the same as the heating temperature in step (1).
Finally, the invention discloses application of the phosphating solution for metal surface treatment in the fields of materials, chemical engineering, construction and the like.
Compared with the prior art, the invention has the beneficial effects that: as described above, some conventional phosphating solutions have pores on the surface of the metal substrate, which are important factors affecting the corrosion resistance of the phosphating film. Therefore, the polyvinyl alcohol is added into the phosphating solution for metal surface treatment, and when the phosphating solution is used for forming the phosphating film, the lamellar phosphating film can be combined into a whole, the gaps among the phosphating film blocks are eliminated, the phosphating film can form a whole better, the surface of a metal workpiece can form a denser phosphating film, the corrosion resistance of the phosphating film is improved, and the binding force between the phosphating film and a metal substrate is stronger. In addition, the polyvinyl alcohol molecule contains a large number of hydroxyl groups, has good reducibility, and can reduce Fe 3+ ions dissolved in the phosphating solution in the phosphating process into Fe 2+ ions, so that the generation of FePO 4 sediments is effectively reduced, the problem that the traditional phosphating solution is easy to generate phosphating residues is solved, and the generated Fe 2+ ions can participate in the formation of a phosphating film, thereby being beneficial to increasing the thickness of the phosphating film and improving the corrosion resistance of the phosphating film.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. The invention will now be further illustrated by means of a specific implementation.
Example 1
A preparation method of phosphating solution for metal surface treatment comprises the following steps:
(1) Adding polyvinyl alcohol 1788 powder into water, continuously stirring for 30 minutes to swell the polyvinyl alcohol powder, heating the obtained mixed solution to 80 ℃ in a water bath, and stirring for 20 minutes to fully dissolve the polyvinyl alcohol powder to obtain a polyvinyl alcohol solution for later use.
(2) Continuously maintaining the polyvinyl alcohol solution at 80 ℃, then adding the phosphoric acid solution, the zinc oxide and the nitric acid solution, and then uniformly stirring to obtain phosphating solution with components of 42g/L phosphoric acid, 26g/L zinc oxide, 22.5g/L nitric acid and 1.8g/L polyvinyl alcohol powder.
Example 2
A preparation method of phosphating solution for metal surface treatment comprises the following steps:
(1) Adding polyvinyl alcohol 17-92 powder into water, continuously stirring for 35 minutes to swell the polyvinyl alcohol powder, heating the obtained mixed solution to 85 ℃ in a water bath, and stirring for 30 minutes to fully dissolve the polyvinyl alcohol powder to obtain a polyvinyl alcohol solution for later use.
(2) And continuously maintaining the polyvinyl alcohol solution at 85 ℃, adding a phosphoric acid solution, zinc oxide and a nitric acid solution, and uniformly stirring to obtain a phosphating solution with components of 45g/L phosphoric acid, 29g/L zinc oxide, 24.5g/L nitric acid and 2.2g/L polyvinyl alcohol powder.
Example 3
A preparation method of phosphating solution for metal surface treatment comprises the following steps:
(1) Adding polyvinyl alcohol 1788 powder into water, continuously stirring for 20 minutes to swell the polyvinyl alcohol powder, heating the obtained mixed solution to 70 ℃ in a water bath, and stirring for 35 minutes to fully dissolve the polyvinyl alcohol powder to obtain a polyvinyl alcohol solution for later use.
(2) And continuously maintaining the polyvinyl alcohol solution at 70 ℃, adding a phosphoric acid solution, zinc oxide and a nitric acid solution, and uniformly stirring to obtain a phosphating solution with components of 41g/L phosphoric acid, 24.5g/L zinc oxide, 20g/L nitric acid and 1.5g/L polyvinyl alcohol powder.
Example 4
A preparation method of phosphating solution for metal surface treatment comprises the following steps:
(1) Adding polyvinyl alcohol 1788 powder into water, continuously stirring for 30 minutes to swell the polyvinyl alcohol powder, heating the obtained mixed solution to 80 ℃ in a water bath, and stirring for 20 minutes to fully dissolve the polyvinyl alcohol powder to obtain a polyvinyl alcohol solution for later use.
(2) Continuously maintaining the polyvinyl alcohol solution at 80 ℃, then adding phosphoric acid solution, zinc oxide, nitric acid solution, tartaric acid, di-o-toluene thiourea, sodium dodecyl sulfate and nano silicon dioxide, and uniformly stirring to obtain phosphating solution with components of 42g/L phosphoric acid, 26g/L zinc oxide, 22.5g/L nitric acid, 1.8g/L polyvinyl alcohol powder, 0.2g/L tartaric acid, 0.01g/L di-o-toluene thiourea, 0.04g/L sodium dodecyl sulfate and 0.85g/L nano silicon dioxide.
Example 5
A preparation method of phosphating solution for metal surface treatment comprises the following steps:
(1) Adding polyvinyl alcohol 1788 powder into water, continuously stirring for 20 minutes to swell the polyvinyl alcohol powder, heating the obtained mixed solution to 70 ℃ in a water bath, and stirring for 35 minutes to fully dissolve the polyvinyl alcohol powder to obtain a polyvinyl alcohol solution for later use.
(2) Continuously maintaining the polyvinyl alcohol solution at 70 ℃, then adding phosphoric acid solution, zinc oxide, nitric acid solution, citric acid, urea, sodium dodecyl benzene sulfonate and nano titanium dioxide, and uniformly stirring to obtain phosphating solution with the components of 41g/L phosphoric acid, 24.5g/L zinc oxide, 20g/L nitric acid, 1.5g/L polyvinyl alcohol powder, 0.05g/L citric acid, 0.005g/L urea, 0.002g/L sodium dodecyl benzene sulfonate and 0.5g/L nano titanium dioxide.
Example 6
A preparation method of phosphating solution for metal surface treatment comprises the following steps: heating water to 80 ℃, adding a phosphoric acid solution, zinc oxide and a nitric acid solution, and uniformly stirring to obtain a phosphating solution with components of 42g/L phosphoric acid, 26g/L zinc oxide and 22.5g/L nitric acid.
Example 7
A preparation method of phosphating solution for metal surface treatment comprises the following steps: heating water to 80 ℃, adding phosphoric acid solution, zinc oxide, nitric acid solution, tartaric acid, di-o-toluene thiourea, sodium dodecyl sulfate and nano silicon dioxide, and uniformly stirring to obtain phosphating solution with components of 42g/L phosphoric acid, 26g/L zinc oxide, 22.5g/L nitric acid, 1.8g/L polyvinyl alcohol powder, 0.2g/L tartaric acid, 0.01g/L di-o-toluene thiourea, 0.04g/L sodium dodecyl sulfate and 0.85g/L nano silicon dioxide.
Performance testing
The silicon steel sheet was immersed in the phosphating solution prepared in the above examples for 20 minutes, and then three performance indexes of corrosion resistance, adhesion of the phosphating film and the amount of phosphated residue generated of the corresponding silicon steel sheet obtained by treating the phosphating solution in each example were tested. Wherein the corrosion resistance was measured in accordance with standard GBT6807-2001, a phosphated silicon steel sheet sample was immersed in a 3wt.% NaCl solution at 25℃and the time for occurrence of rust of the phosphated film was recorded, and the results are shown in Table 1.
TABLE 1
As can be seen from the test results of table 1, the phosphating solutions prepared in examples 1 to 5 were significantly superior to those of examples 6 and 7 in the phosphating solutions of examples 6 and 7 in the effect of phosphating treatment on silicon steel sheets, because the phosphating solutions of examples 6 and 7 were free from polyvinyl alcohol, resulting in the presence of many voids in the phosphating film formed on the surface of the silicon steel sheet, which affected the corrosion resistance of the phosphating film. The polyvinyl alcohol is added into the phosphating solution prepared in the embodiment 1 to the embodiment 5, and when the phosphating solution is formed, the lamellar phosphating films can be combined into a whole, so that gaps among the phosphating film blocks are eliminated, the phosphating film can form a whole better, a denser phosphating film can be formed on the surface of a metal workpiece, the corrosion resistance of the phosphating film is obviously improved, and the binding force between the phosphating film and the silicon steel sheet is stronger. In addition, the polyvinyl alcohol molecule contains a large number of hydroxyl groups, has good reducibility, and can reduce Fe 3+ ions dissolved in the phosphating solution in the phosphating process into Fe 2+ ions, so that the generation of FePO 4 sediments is effectively reduced, the problem that the traditional phosphating solution is easy to generate phosphating residues is solved, and the generated Fe 2+ ions can participate in the formation of a phosphating film, thereby being beneficial to increasing the thickness of the phosphating film and further improving the corrosion resistance of the phosphating film.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A phosphating solution for metal surface treatment, characterized in that it comprises the following components in content per liter of phosphating solution: water liter, 41-45 g of phosphoric acid, 24.5-29 g of zinc oxide, 20-24.5 g of nitric acid and 1.5-2.2 g of polyvinyl alcohol;
The phosphating solution also comprises 0.05-0.2 g/L of complexing agent and 0.005-0.01 g/L of corrosion inhibitor; the complexing agent comprises any one of tartaric acid, citric acid and edetate disodium; the corrosion inhibitor comprises any one of di-o-toluene thiourea, hexamethylenetetramine, thiourea and urea;
the phosphating solution also comprises 0.002-0.04 g/L of surfactant; the surfactant comprises any one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and fatty glyceride;
the phosphating solution also comprises 0.5-0.85 g/L of inorganic nano particles; the inorganic nano particles comprise any one of nano silicon dioxide, nano titanium dioxide and nano silicon nitride;
0.7-1.1 g/L of accelerator is also included in the phosphating solution; the promoter includes a substance capable of providing a source of at least one metal ion in Ni 2+、Mn2+、Ca2+.
2. The phosphating solution for metal surface treatment according to claim 1, wherein the accelerator is at least one of nickel nitrate, manganese nitrate, and calcium nitrate.
3. The method for producing a phosphating solution for metal surface treatment according to claim 1 or 2, comprising the steps of:
(1) Adding the polyvinyl alcohol powder into the water, continuously stirring for a period of time to enable the polyvinyl alcohol powder to swell, and stirring the obtained mixed solution under a heating condition to enable the polyvinyl alcohol powder to be fully dissolved to obtain a polyvinyl alcohol solution for later use;
(2) And adding the phosphoric acid, zinc oxide and nitric acid under the condition of heat preservation, and stirring uniformly to obtain the phosphating solution.
4. The method for producing a phosphating solution for metal surface treatment according to claim 3, wherein in the step (1), the continuous stirring time is 20 to 35 minutes.
5. The method for producing a phosphating solution for metal surface treatment according to claim 3, wherein in the step (1), the heating temperature is 70 to 85 ℃.
6. A method for producing a phosphating solution for metal surface treatment according to any one of claims 3 to 5, wherein in the step (2), the temperature of the heat preservation is the same as the heating temperature in the step (1).
7. Use of the phosphating solution for metal surface treatment according to claim 1 or 2 or the phosphating solution for metal surface treatment obtained by the preparation method according to any one of claims 3 to 6 in the fields of materials, chemical industry or construction.
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