CN108546941B - Environment-friendly titanium salt color passivation solution - Google Patents
Environment-friendly titanium salt color passivation solution Download PDFInfo
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- CN108546941B CN108546941B CN201810593914.1A CN201810593914A CN108546941B CN 108546941 B CN108546941 B CN 108546941B CN 201810593914 A CN201810593914 A CN 201810593914A CN 108546941 B CN108546941 B CN 108546941B
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
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- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
The invention discloses an environment-friendly titanium salt color passivation solution which comprises 6-8 mL/L of titanium trichloride, 2-4 mL/L of hydroxyethylidene diphosphonic acid, 13-17 mL/L of hydrogen peroxide, 4-7 g/L of sodium fluosilicate, 4-6 g/L of silane, 1-1.5 g/L of nickel sulfate, 8-12 mL/L of phosphoric acid and 1-3 g/L of sodium dodecyl sulfate, wherein the pH value of the passivation solution is 1-2; the passivation solution does not contain toxic and harmful substances such as chromium and the like, and is an environment-friendly passivation solution; the passivation solution is simple in preparation process, high in corrosion resistance, strong in film adhesion, stable in passivation solution, low in production cost and uniform in film thickness, the appearance of a zinc coating treated by the passivation solution is a uniformly-distributed colored passivation film, the time of white rust appearing through a neutral salt spray test exceeds 85 hours, different market requirements can be met, after the zinc coating is aged and soaked in saline water for 48 hours, the cross cutting edge of a picture lattice hardly has a shedding phenomenon, the total shedding area of the passivation film is less than 5%, and the passivation film is a passivation film with good adhesion.
Description
Technical Field
The invention relates to an environment-friendly titanium salt color passivation solution, and belongs to the technical field of metal material surface treatment.
Background
Electrogalvanizing is a conventional surface protection technology which is most widely applied, is the most important one in a material surface anticorrosion protection method, and utilizes zinc ions to form a uniform and compact deposition layer on a metal surface to isolate a protected substrate from an external medium so as to achieve an anticorrosion effect. The technology has the advantages of simple equipment, simple operation and low cost, thereby having wide application.
If the zinc plating is not further processed, the coating quickly becomes dark and white corrosion products appear on the surface, which quickly corrode the protected material. Therefore, in order to improve the corrosion resistance and effectively protect the substrate, passivation treatment is generally performed on the substrate after galvanization, so that a compact conversion film layer is formed on the surface of the zinc layer, and the aim of more effective corrosion resistance is fulfilled.
At present, most production lines use chromate passivation, wherein hexavalent chromium is high in toxicity and easy to cause cancer, the environment and human bodies are greatly damaged, trivalent chromium can be converted into hexavalent chromium during long-term storage and use, and the use and discharge of chromate are strictly limited by governments. Therefore, it is urgent to develop passivation technology meeting the environmental protection requirements.
The existing chromium-free color passivation systems are numerous, wherein the silicate passivation has a good application prospect, but the stability and the corrosion resistance are to be improved; the molybdate system has good corrosion delaying effect and low toxicity, but has high requirement on the thickness of a film layer and high cost; the rare earth metal salt system has low toxicity, good stability and good corrosion inhibition effect, but has high cost; the organic matter system has high corrosion resistance, but the types of film forming agents are more, the passivation process is more complex, and the passivation cost is higher.
Disclosure of Invention
The invention aims to overcome the problems of low film-forming efficiency, easy generation of cracks and the like of the passivation of titanium salt, improve the defects of cracks and the like on the surface of a film layer by adding a coupling agent, and greatly improve the adhesion capability and the corrosion resistance of a passivation film.
The invention provides an environment-friendly titanium salt color passivation solution free of toxic substances, which comprises 6-8 mL/L of titanium trichloride, 2-4 mL/L of hydroxyethylidene diphosphonic acid, 13-17 mL/L of hydrogen peroxide, 4-7 g/L of fluosilicate, 4-6 g/L of silane, 1-1.5 g/L of nickel sulfate, 8-12 mL/L of phosphoric acid and 1-3 g/L of sodium dodecyl sulfate, wherein the pH value of the passivation solution is 1-2.
The sodium fluosilicate is replaced by potassium fluozirconate or a mixture of potassium fluozirconate and sodium fluosilicate mixed in any proportion.
The silane is aminosilane (KH-550).
The reagents are all commercially available analytical pure chemical reagents, and the solvent is deionized water.
The preparation method of the environment-friendly titanium salt color passivation solution comprises the following specific steps:
(1) adding deionized water with the volume of 50-70% of the volume of the passivation solution required for preparation into a beaker;
(2) sequentially adding required amounts of titanium trichloride, hydrogen peroxide, hydroxyethylidene diphosphonic acid, fluosilicate, silane, nickel sulfate, phosphoric acid and sodium dodecyl sulfate into the deionized water obtained in the step (1), and uniformly stirring until the titanium trichloride, the hydrogen peroxide, the hydroxyethylidene diphosphonic acid, the fluosilicate, the silane, the nickel sulfate, the phosphoric acid and the sodium dodecyl sulfate are completely dissolved to obtain a mixed solution;
(3) supplementing water into the mixed solution obtained in the step (2), adding dilute nitric acid or a sodium hydroxide solution with the mass fraction of 10%, adjusting the pH value to 1-2, and reaching the required volume to obtain the environment-friendly titanium salt color passivation solution.
The method for passivating the electrogalvanizing material by using the environment-friendly titanium salt color passivation solution comprises the following steps: and cleaning the electrogalvanized material, performing brightening treatment, cleaning, immersing the material in an environment-friendly titanium salt color passivation solution, soaking at room temperature for 20-40 seconds, taking out, cleaning and drying.
The light extraction treatment process comprises the following steps: putting the galvanized material into a bright dipping solution, soaking at room temperature for 3-5 seconds, and taking out, wherein the bright dipping solution is as follows: HNO with mass fraction of 3%3Aqueous solution。
The cleaning method of the galvanized, glazed and passivated material comprises the following steps: washing with tap water or rinsing in a tank or a pool filled with clean water until the surface of the plated part is cleaned.
The drying method comprises the following steps: naturally drying, drying by a blower or drying at a constant temperature of 60 ℃ by a constant temperature box.
The mechanism analysis of the related components of the invention:
(1) titanium trichloride and hydroxyethylidene diphosphonic acid are main film forming agents, and titanium salt and organic acid are compounded and passivated to improve the film forming efficiency of the titanium salt. The group in the organic acid can be complexed with zinc ions on the surface of a plated part to form a compact intermediate film with strong viscosity, and the film can form a stable complex compound with zinc and titanium ions to be attached to the surface of a zinc layer; and at the interface of the coating, Ti4+Can be reacted with OH-The reaction generates a layer of titanium dioxide hydrate colloid which is difficult to dissolve in water on the surface of the zinc coating, the colloid and the complex compound are subjected to shrinkage crosslinking to generate a compact passive film which is the main body of the passive film, and the hydroxyethylidene diphosphonic acid has the function of auxiliary film formation.
(2) Hydrogen peroxide is a main oxidant, so that zinc ions are quickly generated on the surface of a plated part to participate in film formation, the film formation process is accelerated, and the passivation efficiency is improved.
(3) Sodium fluosilicate is used as adhesive, additive and corrosion inhibitor, and can be decomposed to generate fluoride and SiO2The nano-scale particles are deposited on the surface of the passive film, the corrosion resistance is improved, and simultaneously F-The film forming speed and the film thickness can be controlled, and the fluoride can improve the stability of the passivation solution.
(4) Silane is a good coupling agent, and aminosilane (KH-550) has two functional groups, -NH2And C2H5O-metal Zn capable of being hydrolyzed and then being mixed with inorganic matters and metal surfaces2+The hybrid is combined, silane is between an inorganic interface and an organic interface, so that a bonding layer of an organic matrix, a silane coupling agent and an inorganic matrix can be formed, the adhesion performance and the film strength are improved, the surface property of a passive film is improved, and the corrosion resistance is further improved.
(5) The nickel sulfate is an activated metal ion and is a colorant for colorized passivation of titanium salt, so that the appearance and the corrosion resistance of the passivation film are influenced.
(6) Phosphoric acid is used as a solvent for replacing sulfuric acid and nitric acid as main film forming substances and H required by film forming reaction+The main source of the zinc-plating solution and the zinc-plating layer generate a phosphating reaction at the same time, and a continuous water-insoluble firm phosphating film, namely 3Zn, is generated on the surface of a substrate2++2PO3 4—+4H2O=Zn3(PO4)2▪4H2And O ↓andthe generated phosphate conversion film further improve the adhesive force and the anti-corrosion capability of the film layer.
(7) Sodium dodecyl sulfate is a wetting agent, is a nontoxic anionic surfactant, has the function of dispersing passivation components in passivation solution, enables the passivation solution to be better distributed on the surface of an object, generates a passivation film uniformly and compactly by reaction, and prevents defects such as pores and the like.
The invention has the beneficial effects that:
(1) the invention relates to a novel environment-friendly titanium salt color passivation solution used for a zinc plating post-treatment process of steel parts.
(2) The passivation solution is an organic acid assisted film-forming passivation solution, has simple process and short passivation time, overcomes the defect that a passivation film is easy to fall off, has better film adhesion compared with a common titanium salt passivation film, almost has no falling-off phenomenon at the cross cutting edge of a picture lattice after being aged and soaked in saline water for 48 hours, and has the total falling-off area of less than 5 percent.
(3) The coupling agent is added into the passivation solution, so that the defects of cracks and the like on the surface of the passivation film can be effectively improved, the passivation film is more compact, and the corrosion resistant effect of the traditional chromate can be achieved without sealing treatment after passivation.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the examples.
Example 1
The embodiment of the invention relates to an environment-friendly titanium salt color passivation solution, which comprises the following components in percentage by weight: 6mL/L of titanium trichloride, 2mL/L of hydroxyethylidene diphosphonic acid, 13mL/L of hydrogen peroxide, 4g/L of sodium fluosilicate, 4g/L of aminosilane (KH-550), 1g/L of nickel sulfate, 8mL/L of phosphoric acid, 1g/L of sodium dodecyl sulfate and the balance of water, wherein the pH value of the passivation solution is 1.
The method for preparing the environment-friendly titanium salt color passivation solution in the embodiment by taking 1L as a unit comprises the following specific steps:
(1) adding deionized water with the volume of 50% of the volume of the required passivation solution into a beaker, namely adding 500mL of deionized water;
(2) respectively adding 6mL of titanium trichloride solution, 13mL of hydrogen peroxide, 2mL of hydroxyethylidene diphosphonic acid, 4g of sodium fluosilicate, 4g of aminosilane (KH-550), 1g of nickel sulfate, 8mL of phosphoric acid and 1g of sodium dodecyl sulfate into the deionized water obtained in the step (1), and uniformly stirring until the mixture is completely dissolved to obtain a mixed solution;
(3) supplementing water into the mixed solution obtained in the step (2), and adding dilute nitric acid to adjust the pH value to 1 and reach 1L, so as to obtain the environment-friendly titanium salt color passivation solution.
The passivation solution prepared in the embodiment is used for passivating the electrogalvanized steel plate:
(1) the electrogalvanized steel sheet is obtained by the following method: the method comprises the following steps of (1) carrying out pretreatment such as rust removal, oil removal, activation and the like on a low-carbon steel plate with the thickness of 40mm multiplied by 50mm multiplied by 1.0mm according to a conventional method before electroplating, and then putting the low-carbon steel plate into a conventional electroplating solution for electroplating treatment, wherein the electroplating solution of the galvanizing treatment process comprises the following components: ZnCl270g/L, KCl 175g/L, 30g/L boric acid, 0.5ml/L brightener DK-SXG, 17ml/L softener DK-SXR, the pH value of the plating solution is 5.4, and the operation conditions are as follows: the current density is 1.5A/dm2The temperature is room temperature, the electroplating time is 20min, and the galvanized steel plate is obtained for standby;
(2) preparing a brightening liquid: chemically pure HNO3Preparing HNO with water3Brightening liquid with the mass fraction of 3% for later use;
(3) and (2) washing the electrogalvanized steel plate obtained in the step (1) with tap water, immersing the electrogalvanized steel plate into the bright dipping solution obtained in the step (2), standing at room temperature for 5 seconds, taking out the electrogalvanized steel plate, washing the electrogalvanized steel plate with tap water, immersing the electrogalvanized steel plate into the environment-friendly titanium salt color passivation solution prepared in the embodiment, soaking the electrogalvanized steel plate at room temperature for 20 seconds, taking out the electrogalvanized steel plate, washing the electrogalvanized steel plate with tap water, and drying the electrogalvanized steel plate with a.
The electrogalvanized steel plate treated by the passivating solution is uniform and bright in color, uniform in film formation, high in passivating efficiency and good in corrosion resistance of a film layer, after aging and soaking in saline water for 48 hours, the cross cutting edges of the picture lattices hardly fall off, and the total falling area of the passivating film is 4%; the time of white rust occurrence by a neutral salt spray test exceeds 85 hours.
Example 2
The embodiment of the invention relates to an environment-friendly titanium salt color passivation solution, which comprises the following components in percentage by weight: 7mL/L of titanium trichloride, 3mL/L of hydroxyethylidene diphosphonic acid, 15mL/L of hydrogen peroxide, 5g/L of potassium fluorozirconate, 5g/L of aminosilane (KH-550), 1.2g/L of nickel sulfate, 10mL/L of phosphoric acid, 2g/L of sodium dodecyl sulfate and the balance of water, wherein the pH value of the passivation solution is 1.5.
The method for preparing the environment-friendly titanium salt color passivation solution in the embodiment by taking 1L as a unit comprises the following specific steps:
(1) adding deionized water with the volume of 70% of the volume of the required passivation solution into a beaker, namely adding 700mL of deionized water;
(2) adding 7mL of titanium trichloride, 15mL of hydrogen peroxide, 3mL of hydroxyethylidene diphosphonic acid, 5g of potassium fluozirconate, 5g of aminosilane (KH-550), 1.2g of nickel sulfate, 10mL of phosphoric acid and 2g of sodium dodecyl sulfate into the deionized water obtained in the step (1) in sequence, and uniformly stirring until the mixture is completely dissolved to obtain a mixed solution;
(3) supplementing water into the mixed solution obtained in the step (2), and adding dilute nitric acid to adjust the pH value to 1.5 and reach 1L, so as to obtain the environment-friendly titanium salt color passivation solution.
The passivation solution prepared in the embodiment is used for passivating the electrogalvanized steel plate:
(1) the electrogalvanized steel sheet is obtained by the following method: the low carbon steel plate of 40mm multiplied by 50mm multiplied by 1.0mm is put into the conventional electroplating solution after the pretreatment of rust removal, oil removal, activation and the like is carried out according to the conventional method before the electroplatingElectroplating treatment is carried out, and the plating solution of the galvanizing treatment process comprises the following components: ZnCl270g/L, KCl 175g/L, 30g/L boric acid, 0.5ml/L brightener DK-SXG, 17ml/L softener DK-SXR, and the pH value of the plating solution is 5.6, wherein the operation conditions are as follows: the current density is 1.5A/dm2The temperature is room temperature, the electroplating time is 20 minutes, and the galvanized steel plate is obtained for standby;
(2) preparing a brightening liquid: chemically pure HNO3Preparing HNO with water3Brightening liquid with the mass concentration of 3% for later use;
(3) and (2) washing the electrogalvanized steel plate obtained in the step (1) with tap water, immersing the electrogalvanized steel plate into the bright dipping solution obtained in the step (2), standing at room temperature for 3 seconds, taking out the electrogalvanized steel plate, rinsing the electrogalvanized steel plate in a tank filled with clean water, immersing the electrogalvanized steel plate into the environment-friendly titanium salt color passivation solution prepared in the embodiment, immersing the electrogalvanized steel plate at room temperature for 30 seconds, taking out the electrogalvanized steel plate, washing the electrogalvanized steel plate with tap water, and drying the electrogalvanized steel plate at a constant temperature of 60.
The steel plate treated by the passivation solution is uniform and bright in color, uniform in film formation, high in passivation efficiency and good in film corrosion resistance, after aging and being soaked in saline water for 48 hours, the cross cutting edges of the picture lattices hardly fall off, and the total falling area of the passivation film is 3%; the time of white rust occurrence by a neutral salt spray test exceeds 96 hours.
Example 3
The embodiment of the invention relates to an environment-friendly titanium salt color passivation solution, which comprises the following components in percentage by weight: 8mL/L of titanium trichloride, 4mL/L of hydroxyethylidene diphosphonic acid, 17mL/L of hydrogen peroxide, 3g/L of sodium fluosilicate, 4g/L of potassium fluozirconate, 6g/L of aminosilane (KH-550), 1.5g/L of nickel sulfate, 12mL/L of phosphoric acid, 3g/L of sodium dodecyl sulfate and the balance of water, wherein the pH value of the passivation solution is 2.
The method for preparing the environment-friendly titanium salt color passivation solution in the embodiment by taking 1L as a unit comprises the following specific steps:
(1) adding deionized water with the volume of 60% of the volume of the required passivation solution into a beaker, namely adding 600mL of deionized water;
(2) respectively adding 8mL of titanium trichloride solution, 17mL of hydrogen peroxide, 4mL of hydroxyethylidene diphosphonic acid, 3g of sodium fluosilicate, 4g of potassium fluozirconate, 6g of aminosilane (KH-550), 1.5g of nickel sulfate, 12mL of phosphoric acid and 3g of sodium dodecyl sulfate into the deionized water obtained in the step (1), and uniformly stirring until the mixture is completely dissolved to obtain a mixed solution;
(3) supplementing water into the mixed solution obtained in the step (2), and adding dilute nitric acid to adjust the pH value to 2 and reach 1L, so as to obtain the environment-friendly titanium salt color passivation solution.
The passivation solution prepared in the embodiment is used for passivating the electrogalvanized steel plate:
(1) the electrogalvanized steel sheet is obtained by the following method: the method comprises the following steps of (1) carrying out pretreatment such as rust removal, oil removal, activation and the like on a low-carbon steel plate with the thickness of 40mm multiplied by 50mm multiplied by 1.0mm according to a conventional method before electroplating, and then putting the low-carbon steel plate into a conventional electroplating solution for electroplating treatment, wherein the electroplating solution of the galvanizing treatment process comprises the following components: ZnCl270g/L, KCl 175g/L, 30g/L boric acid, 0.5ml/L brightener DK-SXG, 17ml/L softener DK-SXR, and the pH value of the plating solution is 5.8, wherein the operation conditions are as follows: the current density is 1.5A/dm2The temperature is room temperature, the electroplating time is 20min, and the galvanized steel plate is obtained for standby;
(2) preparing a brightening liquid: chemically pure HNO3Preparing the mixture and water into brightening liquid with the mass concentration of 3% for later use;
(3) and (2) rinsing the electrogalvanized steel plate obtained in the step (1) in a pool filled with clean water, immersing the electrogalvanized steel plate into the bright dipping solution obtained in the step (2), standing at room temperature for 4 seconds, taking out the electrogalvanized steel plate, washing the electrogalvanized steel plate with tap water, immersing the electrogalvanized steel plate into the environment-friendly titanium salt color passivation solution prepared in the embodiment, soaking the electrogalvanized steel plate at room temperature for 40 seconds, taking out the electrogalvanized steel plate, washing the electrogalvanized steel plate with tap water, and naturally drying the electrogalvanized.
The steel plate treated by the passivation solution is uniform and bright in color, uniform in film formation, high in passivation efficiency and good in film corrosion resistance, after aging and being soaked in saline water for 48 hours, the cross cutting edges of the picture lattices hardly fall off, and the total falling area of the passivation film is 2%; the time of white rust occurrence by the neutral salt spray test exceeds 100 hours.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (2)
1. An environment-friendly titanium salt color passivation solution is characterized in that: the titanium trichloride-containing aqueous solution comprises 6-8 mL/L of titanium trichloride, 2-4 mL/L of hydroxyethylidene diphosphonic acid, 13-17 mL/L of hydrogen peroxide, 4-7 g/L of sodium fluosilicate, 4-6 g/L of silane, 1-1.5 g/L of nickel sulfate, 8-12 mL/L of phosphoric acid, 1-3 g/L of sodium dodecyl sulfate and the balance of water; the pH value of the passivation solution is 1-2; the silane is an aminosilane.
2. The environment-friendly titanium salt color passivation solution as claimed in claim 1, wherein: the sodium fluosilicate is replaced by potassium fluozirconate or a mixture of potassium fluozirconate and sodium fluosilicate mixed in any proportion.
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