CN110551997B - Chromium-free passivation solution for electrotinning steel plate and use method thereof - Google Patents
Chromium-free passivation solution for electrotinning steel plate and use method thereof Download PDFInfo
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- CN110551997B CN110551997B CN201810561989.1A CN201810561989A CN110551997B CN 110551997 B CN110551997 B CN 110551997B CN 201810561989 A CN201810561989 A CN 201810561989A CN 110551997 B CN110551997 B CN 110551997B
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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
- C23C22/34—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 fluorides or complex fluorides
- C23C22/36—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 fluorides or complex fluorides containing also phosphates
- C23C22/362—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 fluorides or complex fluorides containing also phosphates containing also zinc cations
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/30—Electroplating: Baths therefor from solutions of tin
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
- C25D5/505—After-treatment of electroplated surfaces by heat-treatment of electroplated tin coatings, e.g. by melting
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Abstract
The invention discloses a chromium-free passivation solution for an electrotinning steel plate and a use method thereof, which solve the technical problem of high manufacturing cost of the conventional chromium-free passivation solution for the electrotinning steel plate. A chromium-free passivation solution for an electrotinning steel plate contains water, and the chromium-free passivation solution contains zinc dihydrogen phosphate with the mass concentration of 5-20 g/L, 1-5 g/L sodium nitrate, 0.2-2 g/L OP-10 and 1-10 g/L ammonium fluotitanate; the pH value of the chromium-free passivation solution is 1.0-2.0; the pH value of the chromium-free passivation solution is adjusted by phosphoric acid; the service temperature of the chromium-free passivation solution is 30-50 ℃. The chromium-free passivation solution can be directly sprayed, no waste liquid is generated, and the manufacturing and using processes are green and environment-friendly.
Description
Technical Field
The invention relates to a steel plate surface treatment liquid, in particular to a chromium-free passivation liquid for an electrotinning steel plate and a use method thereof, belonging to the technical field of metal surface treatment.
Background
The cold-rolled electroplated tin steel plate is widely applied to the industries of food, beverage and packaging, and the main production processes of the electroplated tin steel plate are alkali washing, acid washing, electroplating, soft melting and passivation in sequence. The passivation is the last procedure in the production process of the tin plate and is a means for improving the apparent state, corrosion resistance and other performances of the tin plate. The method commonly used in the prior production is hexavalent chromium treatment, and a passive film obtained after chromate passivation treatment is very thin, has excellent corrosion resistance and simple process, and is the most common passivation treatment method in the production of tin plates for a long time. However, because the dichromate or chromic anhydride is used as the main salt in the passivation process, the hexavalent chromium contained in the dichromate is a strong toxic substance, and brings great harm to human bodies and the environment.
In recent years, certain chromium-free passivation solution formulas and matched post-treatment processes thereof also appear, and the conventional processes of alkali washing, acid washing, electroplating, reflow, passivation and oil coating are adopted in the preparation process of the chromium-free passivation tin plate.
The patent application publication No. CN101545107 discloses a surface treatment liquid, a surface treatment method and a tin-plated steel plate with surface treatment, and discloses a surface treatment liquid for a tin-plated steel plate, wherein the surface treatment liquid contains 1-50 g/L of phosphorus compound, 1-20 g/L of vanadium compound, 1-30 g/L of one or more compounds selected from molybdenum, zirconium, titanium, manganese or tungsten metal compound, and 1-10 g/L of one or more compounds with at least one functional group of hydroxyl, carbonyl, carboxyl or phosphate.
The Chinese patent application publication No. CN101638804 discloses a chromium-free passivation solution for tin-plated steel plates and a use method thereof, wherein the disclosed passivation solution contains inorganic salts of rare earth elements cerium (Ce) or lanthanum (La), inorganic salts of ammonium and water, and the weight parts of the three are as follows: 5-30 parts of inorganic salt of cerium or lanthanum, 5-40 parts of inorganic salt of ammonium and 1000 parts of water; the pH value range of the passivation solution is 2-7, and the pH value of the passivation solution is adjusted by dilute nitric acid or dilute sulfuric acid. The use method of the passivation solution comprises the following steps: when the tin-plated steel plate is immersed in the passivation solution for electrochemical treatment, the cathode current density during treatment is 0.1-20A/dm2The treatment time is 0.1-10 seconds, and the temperature is 30-65 ℃. The two patents adopt the conventional preparation process, the components of the passivation solution are more, expensive rare earth elements are involved, the transfer of the chromium-free passivation film layer to the surface of the steel plate needs to be realized through electrolytic passivation, the components need to be continuously supplemented in the production process to maintain balance, and the waste liquid and the like generated in the production process still pollute the environment.
Disclosure of Invention
The invention aims to provide a chromium-free passivation solution for an electrotinning steel plate and a using method thereof, and solves the technical problem that the existing chromium-free passivation solution for the electrotinning steel plate is high in manufacturing cost.
The technical scheme adopted by the invention is that the chromium-free passivation solution for the electrotinning steel plate contains water, and the chromium-free passivation solution contains zinc dihydrogen phosphate with the mass concentration of 5-20 g/L, sodium nitrate with the mass concentration of 1-5 g/L, OP-10 with the mass concentration of 0.2-2 g/L and ammonia fluotitanate with the mass concentration of 1-10 g/L; the pH value of the chromium-free passivation solution is 1.0-2.0; the pH value of the chromium-free passivation solution is adjusted by phosphoric acid; the service temperature of the chromium-free passivation solution is 30-50 ℃.
The zinc dihydrogen phosphate, the sodium nitrate and the ammonium fluotitanate are solid powder; OP-10 is analytically pure, OP-10 is liquid, and the mass density of OP-10 is 1.04g/cm3(ii) a The phosphoric acid is analytically pure, the phosphoric acid is liquid, and the mass density of the phosphoric acid is 1.69g/cm3。
The film forming mechanism of the chromium-free passivation solution is as follows: according to the invention, zinc dihydrogen phosphate and ammonium fluotitanate are used as main film forming substances, sodium nitrate is used as an oxidant, and a nonionic surfactant OP-10 plays a wetting role, so that a uniform film is formed on the surface of the electroplated tin steel plate. Because the titanium salt system has a fast film forming speed, and the titanium salt can be hydrolyzed when being dissolved in water, and a large amount of bubbles can be separated out when the steel plate is immersed into the passivation solution, the cathode electrolytic passivation mode can not be adopted, and the method is suitable for the spraying type process. The optimal use temperature range of the chromium-free passivation solution is 30-50 ℃, the liquid film of the passivation solution cannot be uniformly spread on the surface of a steel plate due to too low temperature, and an excessively thick dry film is formed before extrusion by a wringing roller due to too high temperature, so that the quality of the chromium-free passivation film is influenced. When the chromium-free passivation solution is sprayed on the surface of a tin-plated steel plate, a film-forming substance is formed by TiO2、Sn3(PO4)2And SnF2And the chemical reaction in the film forming process is as follows:
the preparation method of the chromium-free passivation solution for the electrotinning steel plate comprises the following steps:
1) preparing a base solution of a chromium-free passivation solution, weighing 5-20 g of zinc dihydrogen phosphate, 1-5 g of sodium nitrate, 0.2-2 g of OP-10 and 1-10 g of ammonium fluorotitanate respectively, and then adding water, uniformly mixing and fixing the volume to 1L to obtain the base solution of the chromium-free passivation solution;
2) and (3) regulating the pH value of the base solution of the chromium-free passivation solution to 1.0-2.0 by using phosphoric acid to obtain a finished product of the chromium-free passivation solution.
The use method of the chromium-free passivation solution for the tin-electroplated steel plate comprises the following steps:
1) electroplating a substrate of the electroplated tin steel plate, and after alkali washing and acid washing, carrying out cathode electrolysis on the cold-rolled continuous annealed steel plate in a tin methane sulfonate plating solution, wherein the temperature of the plating solution is 40-50 ℃, the concentration of tin ions is 10-30 g/L, the concentration of free acid is 40-60 g/L, and the current density is 0.5-1.5A/dm2The thickness of the obtained coating is 2.8g/m2The electrolytic tinned steel sheet of (1);
2) passivating an electrotinning steel plate, spraying a chromium-free passivation solution on the surface of the electrotinning steel plate, controlling the temperature of the chromium-free passivation solution to be 30-50 ℃, controlling the pressure of a squeezing roller to be 4.0-6.0 Kg, and controlling the thickness of a wet film of the chromium-free passivation solution to be 3-6 mu m;
3) drying the passivated electrotinning steel plate for 5-15 s at 80-100 ℃ in hot air;
4) reflow-melting the electroplated tin steel plate, and heating the electroplated tin steel plate in an induction reflow device at the temperature of 250-270 ℃ for 0.5-1.5 s.
Meanwhile, the tin-plated steel plate has no oxide on the surface and high surface roughness, is favorable for generating a compact chromium-free passivation film and enhances the binding force between the chromium-free passivation film and a plating layer.
Compared with the prior art of carrying out reflow treatment and then passivation, the operation steps of the process are simpler, and the production cost of the tin-plated steel plate is reduced.
Compared with the prior art, the invention has the following positive effects: 1. the chromium-free passivation solution can be directly sprayed, electric energy is not wasted, waste liquid is not generated, and the manufacturing and using processes are green and environment-friendly. 2. The invention adopts a new post-treatment process, realizes that the lower chromium-free passivation film thickness has more excellent performance, and the salt spray resistance grade, the porosity, the sulfur resistance, the adhesive force and the like of the invention exceed the level of a tin-plated steel plate of a chromate passivation process.
Detailed Description
The present invention will be further illustrated below with reference to specific embodiments, which are to be understood as merely illustrative and not limitative of the scope of the present invention.
The substrate of the electrotinning steel plate in the embodiment of the invention adopts a continuous annealing steel plate with the thickness of 0.2mm and the mark MR T4-CA.
Example 1, a chromium-free passivation solution for tin-electroplated steel sheets, which contains zinc dihydrogen phosphate at a mass concentration of 5g/L, sodium nitrate at 1g/L, ammonium fluorotitanate at 0.2g/L OP-10 at 1 g/L; the pH value of the chromium-free passivation solution is 1.0; the pH value of the chromium-free passivation solution is adjusted by phosphoric acid.
The use method of the chromium-free passivation solution for the tin-electroplated steel plate comprises the following steps:
1) electroplating the substrate of the electroplated tin steel plate, performing alkali washing and acid washing on the cold-rolled continuously annealed steel plate, performing cathodic electrolysis in a tin methanesulfonate plating solution, wherein the temperature of the plating solution is 45 ℃, the concentration of tin ions is 18g/L, the concentration of free acid is 50g/L, and the current density is 1.0A/dm2The thickness of the obtained coating is 2.8g/m2The electrolytic tinned steel sheet of (1);
2) passivating an electrotinning steel plate, spraying a chromium-free passivation solution on the surface of the electrotinning steel plate, controlling the temperature of the chromium-free passivation solution at 50 ℃, controlling the pressure of a squeezing roller at 6.0Kg, and controlling the thickness of a wet film of the chromium-free passivation solution to be 3 mu m;
3) drying the passivated electrotinning steel plate for 10s at the temperature of 90 ℃ in hot air;
4) the tin-electroplated steel plate is subjected to reflow treatment and heated in an induction reflow device at 250 ℃ for 0.5 s.
Example 2, a chromium-free passivation solution for tin-electroplated steel sheets, which contains zinc dihydrogen phosphate at a mass concentration of 20g/L, sodium nitrate at 5g/L, ammonium fluorotitanate at 2g/L OP-10, 10 g/L; the pH value of the chromium-free passivation solution is 2.0; the pH value of the chromium-free passivation solution is adjusted by phosphoric acid.
The use method of the chromium-free passivation solution for the tin-electroplated steel plate comprises the following steps:
1) electroplating the substrate of the electroplated tin steel plate, performing alkali washing and acid washing on the cold-rolled continuously annealed steel plate, performing cathodic electrolysis in a tin methanesulfonate plating solution, wherein the temperature of the plating solution is 45 ℃, the concentration of tin ions is 18g/L, the concentration of free acid is 50g/L, and the current density is 1.0A/dm2The thickness of the obtained coating is 2.8g/m2The electrolytic tinned steel sheet of (1);
2) passivating the electrotinning steel plate, spraying a chromium-free passivation solution on the surface of the electrotinning steel plate, controlling the temperature of the chromium-free passivation solution to be 30 ℃, controlling the pressure of a squeezing roller to be 4.0Kg, and controlling the thickness of a wet film of the chromium-free passivation solution to be 6 mu m;
3) drying the passivated electrotinning steel plate for 15s at 80 ℃ in hot air;
4) the tin electroplated steel plate is subjected to reflow treatment and heated in an induction reflow device at 270 ℃ for 1.5 s.
Example 3, a chromium-free passivation solution for tin-electroplated steel sheets, comprising zinc dihydrogen phosphate at a mass concentration of 15g/L, sodium nitrate at a mass concentration of 3g/L, ammonium fluorotitanate at a mass concentration of 1g/L OP-10, 6 g/L; the pH value of the chromium-free passivation solution is 1.5; the pH value of the chromium-free passivation solution is adjusted by phosphoric acid.
The use method of the chromium-free passivation solution for the tin-electroplated steel plate comprises the following steps:
1) electroplating the substrate of the electroplated tin steel plate, performing alkali washing and acid washing on the cold-rolled continuous annealed steel plate, performing cathodic electrolysis in a tin methane sulfonate plating solution, and maintaining the temperature of the plating solutionAt 45 ℃, the concentration of tin ions is 18g/L, the concentration of free acid is 50g/L, and the current density is 1.0A/dm2The thickness of the obtained coating is 2.8g/m2The electrolytic tinned steel sheet of (1);
2) passivating the electrotinning steel plate, spraying a chromium-free passivation solution on the surface of the electrotinning steel plate, controlling the temperature of the chromium-free passivation solution at 40 ℃, controlling the pressure of a squeezing roller at 5.0Kg, and controlling the thickness of a wet film of the chromium-free passivation solution to be 4.5 mu m;
3) drying the passivated electrotinning steel plate for 5s at 100 ℃ in hot air;
4) the tin electroplated steel plate is subjected to reflow treatment and heated in an induction reflow device at 260 ℃ for 1.0 s.
The performance of the electroplated tin steel plate subjected to chromium-free passivation treatment obtained in the embodiment 1-3 is sequentially tested, the salt spray resistance grade is tested by referring to GB/T10125-2012 'Artificial atmosphere Corrosion test', the porosity is tested by referring to GB/T17721-.
Comparative example 1A continuously annealed steel sheet having a thickness of 0.2mm and a trade name of MR T4-CA was cathodically electrolyzed in a tin methanesulfonate bath at a bath temperature of 45 deg.C and a tin ion concentration of 18g/L, a free acid concentration of 50g/L and a current density of 1.0A/dm2The thickness of the obtained coating is 2.8g/m2Then heating the mixture in an induction reflow device at 260 ℃ for 1.0 s; then cathode electrolytic passivation is carried out in sodium dichromate solution with the pH value of 4.5 and the mass concentration of 25g/L, and the current density is 0.8A/dm2Thickness of passivation film 5.0mg/m2。
The performance of the electroplated tin steel plate subjected to passivation treatment obtained in the comparative example 1 is tested, the salt spray resistance grade is tested according to GB/T10125-.
TABLE 1 Performance parameters of passivated electrotinning plates according to examples of the invention
From the performance data above, it can be seen that inventive examples 1-3 are overall superior to comparative example 1.
In addition to the above embodiments, the present invention may have other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (2)
1. A use method of a chromium-free passivation solution for an electrolytic tinned steel plate comprises the following steps:
1) electroplating a substrate of the electroplated tin steel plate, and after alkali washing and acid washing, carrying out cathode electrolysis on the cold-rolled continuous annealed steel plate in a tin methane sulfonate plating solution, wherein the temperature of the plating solution is 40-50 ℃, the concentration of tin ions is 10-30 g/L, the concentration of free acid is 40-60 g/L, and the current density is 0.5-1.5A/dm2The thickness of the obtained coating is 2.8g/m2The electrolytic tinned steel sheet of (1);
2) passivating an electrotinning steel plate, spraying a chromium-free passivation solution on the surface of the electrotinning steel plate, controlling the temperature of the chromium-free passivation solution to be 30-50 ℃, controlling the pressure of a squeezing roller to be 4.0-6.0 Kg, and controlling the thickness of a wet film of the chromium-free passivation solution to be 3-6 mu m; the chromium-free passivation solution contains water, and the chromium-free passivation solution contains zinc dihydrogen phosphate with the mass concentration of 5-20 g/L, sodium nitrate with the mass concentration of 1-5 g/L, OP-10 with the mass concentration of 0.2-2 g/L, and ammonium fluotitanate with the mass concentration of 1-10 g/L; the pH value of the chromium-free passivation solution is 1.0-2.0; the pH value of the chromium-free passivation solution is adjusted by phosphoric acid;
3) drying the passivated electrotinning steel plate for 5-15 s at 80-100 ℃ in hot air;
4) reflow-melting the electroplated tin steel plate, and heating the electroplated tin steel plate in an induction reflow device at the temperature of 250-270 ℃ for 0.5-1.5 s.
2. The method of using a chromium-free passivation solution for tin-electroplated steel sheets as claimed in claim 1, wherein OP-10 is analytically pure, and OP-10 has a mass density of 1.04g/cm3(ii) a The phosphoric acid is analytically pure, and the mass density of the phosphoric acid is 1.69g/cm3。
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| WO2012045791A1 (en) * | 2010-10-06 | 2012-04-12 | Tata Steel Ijmuiden Bv | Process for producing an iron-tin layer on a packaging steel substrate |
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