CN112126920A - Chromium-free conversion agent suitable for roller coating process and preparation method thereof - Google Patents
Chromium-free conversion agent suitable for roller coating process and preparation method thereof Download PDFInfo
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- CN112126920A CN112126920A CN202011023970.5A CN202011023970A CN112126920A CN 112126920 A CN112126920 A CN 112126920A CN 202011023970 A CN202011023970 A CN 202011023970A CN 112126920 A CN112126920 A CN 112126920A
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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
- C23C22/361—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 titanium, zirconium or hafnium compounds
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Abstract
The invention discloses a chromium-free conversion agent suitable for a roller coating process and a preparation method thereof, and is characterized in that the conversion agent comprises the following components in percentage by mass: 5.0-20.0% of phosphoric acid, 1.0-5.0% of nitric acid, 1.5-6.0% of sodium fluotitanate, 1.5-6.0% of sodium fluozirconate, 2.5-8.0% of tartaric acid, 1.0-12.0% of zirconium carbonate, 1.0-10.0% of film-forming assistant, 0.2-3.5% of thickening agent and the balance of deionized water. The conversion agent is a chromium-free green environment-friendly conversion agent, is suitable for various materials such as aluminum, aluminum alloy, ferrous metal and the like, and the generated conversion coating has strong binding force and corrosion resistance. The conversion agent of the invention can be applied to the conventional production processes such as dipping, spraying and the like, and is also particularly suitable for the continuous production processes such as roller coating and the like. In addition, the passivation time by using the conversion agent is short, the cost is low, and the efficiency is high.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, mainly relates to a chromium-free environment-friendly conversion agent, and is particularly suitable for obtaining high-quality conversion coatings from materials such as aluminum, aluminum alloy, ferrous metal and the like in continuous production processes such as roller coating and the like.
Background
The metal surface is treated to form a conversion coating, so that the corrosion of the metal can be delayed, and the service life of the metal is prolonged. Currently, the most widely used is still the chromate passivation process. Although the process is simple and mature, the generated conversion coating has better corrosion resistance and decoration, the chromate has high toxicity and carcinogenicity, and has great harm to human bodies and environment. In recent years, emission of chromium has been strictly regulated in various countries around the world. The European Union has issued ROHS, WEEE, ELV and other regulations to prohibit hexavalent chromium containing automobile and electronic parts from entering the market. China also requires zero discharge of chromium ions in wastewater. Chromate passivation technology has been strictly controlled, and therefore, it has become a current research focus to develop a non-toxic, environment-friendly, high-performance green passivation technology.
Recently, researchers have developed a variety of chromium-free passivation processes, and have made great progress. However, the existing passivators are generally only suitable for dipping or spraying processes, for example, a film forming agent and application thereof in a chromium-free passivating solution for surface treatment of aluminum profiles (CN 110629214A), wherein a layer of dense passivating film can be obtained after completely immersing aluminum materials in the passivating solution, and then washing, draining and baking the aluminum materials for 10-20 minutes. For another example, a chromium-free passivation composition, a chromium-free passivation agent and a preparation method thereof (CN 107653449B) need to soak an aluminum material in the passivation agent for 3-5 minutes, and then the aluminum material is cleaned and baked to obtain a passivation film. In addition, most of the existing passivators only aim at a single metal type and cannot simultaneously meet the requirements of different types of metal surface treatment, for example, a film-forming agent and the application thereof in a chromium-free passivating solution for aluminum profile surface treatment (CN 110629214A) are only suitable for aluminum profile surface treatment. For another example, an environmental protection process (CN 1614090A) for forming a conversion coating on the surface of aluminum and its alloys is also only suitable for the surface treatment of aluminum and its alloys. To date, no environment-friendly chromium-free passivator applicable to various different metals, applicable to continuous production processes such as roller coating and the like, and capable of generating high-performance conversion coatings exists.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a chromium-free conversion agent suitable for a roller coating process and a preparation method thereof, and the specific technical scheme is as follows:
a chromium-free conversion agent suitable for a roller coating process and a preparation method thereof are characterized in that the conversion agent comprises the following components in percentage by mass: 5.0-20.0% of phosphoric acid, 1.0-5.0% of nitric acid, 1.5-6.0% of sodium fluotitanate, 1.5-6.0% of sodium fluozirconate, 2.5-8.0% of tartaric acid, 1.0-12.0% of zirconium carbonate, 1.0-10.0% of film-forming assistant, 0.2-3.5% of thickening agent and the balance of deionized water.
The film forming assistant comprises one or more of dodecyl alcohol ester, ethylene glycol butyl ether and propylene glycol ethyl ether.
The thickener is one or more of carboxyethyl cellulose, sodium alginate, sodium polyacrylate and polyvinyl alcohol.
The conversion agent is made of various materials such as aluminum and alloy thereof, ferrous metal and the like.
The preparation method of the conversion agent comprises the following steps:
(1) according to the formula composition of raw materials, phosphoric acid, nitric acid, sodium fluotitanate, sodium fluozirconate and deionized water are fully stirred to prepare a solution A;
(2) dissolving tartaric acid, zirconium carbonate, a film forming aid, a thickening agent and the like in a proper amount of deionized water according to a formula of raw materials, and fully stirring until the tartaric acid, the zirconium carbonate, the film forming aid, the thickening agent and the like are dissolved to prepare a solution B;
(3) and slowly adding the solution B into the solution A, and fully stirring to obtain the chromium-free conversion agent.
The invention has the beneficial effects that:
(1) the conversion agent is a chromium-free green environment-friendly product;
(2) the conversion agent is not only suitable for the traditional processes of dipping, spraying and the like, but also particularly suitable for the continuous production process of a coil machine set such as roller coating and the like;
(3) the conversion agent of the invention can be suitable for surface treatment of various materials such as aluminum and alloy thereof, ferrous metal and the like;
(4) the conversion coating generated by the conversion agent has strong binding force and corrosion resistance;
(5) the conversion agent has the advantages of short passivation time, low cost and high efficiency.
Detailed Description
Example 1
A chromium-free conversion agent suitable for a roller coating process comprises the following components in percentage by weight: 7.5% of phosphoric acid, 2.5% of nitric acid, 3.0% of sodium fluotitanate, 3.0% of sodium fluozirconate, 4.0% of tartaric acid, 4.5% of zirconium carbonate, 2.5% of film-forming assistant, 0.35% of thickening agent and the balance of deionized water.
The film-forming assistant is: 2.5 percent of dodecyl alcohol ester;
the thickening agent is as follows: 0.35 percent of sodium alginate.
The preparation method of the conversion agent comprises the following steps:
(1) according to the formula composition of raw materials, phosphoric acid, nitric acid, sodium fluotitanate, sodium fluozirconate and deionized water are fully stirred to prepare a solution A;
(2) dissolving tartaric acid, zirconium carbonate, dodecyl alcohol ester, sodium alginate and the like in a proper amount of deionized water, and fully stirring until the materials are dissolved to prepare a solution B;
(3) and slowly adding the solution B into the solution A, and fully stirring to obtain the chromium-free conversion agent.
The conversion agent prepared in the embodiment is used for carrying out roller coating process treatment (10 m/min) on the surface of 4032 aluminum alloy, the conversion coating after treatment is compact and flat and has uniform color, and an anticorrosion and wear-resistant experiment (a neutral salt spray resistance experiment refers to the time required for a phenomenon of white corrosion or blistering under a sodium chloride atmosphere of 4%, a solvent resistance experiment refers to the time required for a phenomenon of white corrosion or blistering after being soaked in a 95% ethanol solution for 15 minutes and then placed under a neutral salt spray condition, and a yellowing resistance experiment refers to the time required for a phenomenon of white corrosion or blistering after being kept at 300 ℃ for 15 minutes in an atmospheric environment and then placed under a neutral salt spray condition) is carried out on the conversion coating. Meanwhile, the adhesion of the conversion coating is tested (the adhesion test method is to cut grids on the surface of the coating, the distance between cutter teeth is 2 mm, the adhesive tape with the adhesion larger than 10N/25mm is adhered on the grids, the air is compressed and removed, the adhesive tape is quickly pulled up at an angle vertical to the surface of the coating, and the surface of the coating is visually detected, wherein the grading shows that 0 grade is 0 grade, the cutting edge is completely smooth, no grid falls off, 1 grade is 1 grade, a little coating falls off at the intersection of the cut, but the cross cutting area is not obviously larger than 5 percent, 2 grade is 2 grade, the coating falls off at the intersection of the cut and/or along the edge of the cut, but the cross cutting area is obviously larger than 5 percent, but not obviously larger than 15 percent), and the following data are measured:
| 4032 aluminium alloy | 4032 aluminum alloy (commercially available chromate treatment) | |
| Neutral salt fog resistant (hour) | 108 | 79 |
| Solvent resistance (hours) | 82 | 63 |
| Yellowing resistance (hour) | 49 | 35 |
| Adhesion Property | Level 0 | Level 0 |
Example 2
A chromium-free conversion agent suitable for a roller coating process comprises the following components in percentage by weight: 10% of phosphoric acid, 3.5% of nitric acid, 3.5% of sodium fluotitanate, 3.5% of sodium fluozirconate, 5.5% of tartaric acid, 5.5% of zirconium carbonate, 3% of film-forming assistant, 0.3% of thickening agent and the balance of deionized water.
The film-forming assistant is: 2.5 percent of dodecyl alcohol ester and 0.5 percent of butyl cellosolve;
the thickening agent is as follows: sodium alginate 0.2%, and sodium polyacrylate 0.1%.
The preparation method of the conversion agent comprises the following steps:
(1) according to the formula composition of raw materials, phosphoric acid, nitric acid, sodium fluotitanate, sodium fluozirconate and deionized water are fully stirred to prepare a solution A;
(2) dissolving tartaric acid, zirconium carbonate, dodecyl alcohol ester, ethylene glycol butyl ether, sodium alginate, sodium polyacrylate and the like in a proper amount of deionized water, and fully stirring until the materials are dissolved to prepare a solution B;
(3) and slowly adding the solution B into the solution A, and fully stirring to obtain the chromium-free conversion agent.
The conversion agent prepared in the embodiment is used for carrying out roller coating process treatment (10 m/min) on the surface of a 3003 aluminum alloy, the conversion coating after treatment is compact and flat and has uniform color, and an anticorrosion and wear-resistant experiment (a neutral salt spray resistance experiment is carried out, wherein the time is required for a phenomenon of white corrosion or blistering under a sodium chloride atmosphere of 4%, a solvent resistance experiment is carried out, the time is required for a phenomenon of white corrosion or blistering under a neutral salt spray condition after being soaked in a 95% ethanol solution for 15 minutes, and a yellowing resistance experiment is carried out, the time is required for a phenomenon of white corrosion or blistering under a neutral salt spray condition after being kept at 300 ℃ for 15 minutes in an atmospheric environment. Meanwhile, the adhesion of the conversion coating is tested (the adhesion test method is to cut grids on the surface of the coating, the distance between cutter teeth is 2 mm, the adhesive tape with the adhesion larger than 10N/25mm is adhered on the grids, the air is compressed and removed, the adhesive tape is quickly pulled up at an angle vertical to the surface of the coating, and the surface of the coating is visually detected, wherein the grading shows that 0 grade is 0 grade, the cutting edge is completely smooth, no grid falls off, 1 grade is 1 grade, a little coating falls off at the intersection of the cut, but the cross cutting area is not obviously larger than 5 percent, 2 grade is 2 grade, the coating falls off at the intersection of the cut and/or along the edge of the cut, but the cross cutting area is obviously larger than 5 percent, but not obviously larger than 15 percent), and the following data are measured:
| 3003 aluminum alloy | 3003 aluminum alloy (commercially available chromate passivator treatment) | |
| Neutral salt fog resistant (hour) | 94 | 76 |
| Solvent resistance (hours) | 76 | 60 |
| Yellowing resistance (hour) | 44 | 32 |
| Adhesion Property | Level 0 | Level 1 |
Example 3
A chromium-free conversion agent suitable for a roller coating process comprises the following components in percentage by weight: 12% of phosphoric acid, 4% of nitric acid, 3% of sodium fluotitanate, 3% of sodium fluozirconate, 6% of tartaric acid, 6.5% of zirconium carbonate, 3.5% of film-forming assistant, 0.35% of thickening agent and the balance of deionized water.
The film-forming assistant is: 3% of dodecyl alcohol ester and 0.5% of propylene glycol ethyl ether;
the thickening agent is as follows: 0.15 percent of sodium polyacrylate and 0.15 percent of polyvinyl alcohol.
The preparation method of the conversion agent comprises the following steps:
(1) according to the formula composition of raw materials, phosphoric acid, nitric acid, sodium fluotitanate, sodium fluozirconate and deionized water are fully stirred to prepare a solution A;
(2) dissolving tartaric acid, zirconium carbonate, dodecyl alcohol ester, propylene glycol ethyl ether, sodium polyacrylate, polyvinyl alcohol and the like in a proper amount of deionized water, and fully stirring until the materials are dissolved to prepare a solution B;
(3) and slowly adding the solution B into the solution A, and fully stirring to obtain the chromium-free conversion agent.
The conversion agent prepared in the embodiment is used for carrying out roller coating process treatment (10 m/min) on the surface of HT100 steel, the conversion coating after treatment is compact and flat, has uniform color and luster, and is subjected to an anticorrosion wear-resistant experiment (a neutral salt spray experiment is that the time required for the phenomenon of white corrosion or blistering is generated under the sodium chloride atmosphere of 4 percent, a solvent resistance experiment is that the time required for the phenomenon of white corrosion or blistering is generated after the conversion coating is soaked in a 95 percent ethanol solution for 15 minutes and then placed under the neutral salt spray condition, and a yellowing resistance experiment is that the time required for the phenomenon of white corrosion or blistering is generated after the conversion coating is kept for 15 minutes under the atmospheric environment at 300 ℃ and then placed under the neutral salt spray condition). Meanwhile, the adhesion of the conversion coating is tested (the adhesion test method is to cut grids on the surface of the coating, the distance between cutter teeth is 2 mm, the adhesive tape with the adhesion larger than 10N/25mm is adhered on the grids, the air is compressed and removed, the adhesive tape is quickly pulled up at an angle vertical to the surface of the coating, and the surface of the coating is visually detected, wherein the grading shows that 0 grade is 0 grade, the cutting edge is completely smooth, no grid falls off, 1 grade is 1 grade, a little coating falls off at the intersection of the cut, but the cross cutting area is not obviously larger than 5 percent, 2 grade is 2 grade, the coating falls off at the intersection of the cut and/or along the edge of the cut, but the cross cutting area is obviously larger than 5 percent, but not obviously larger than 15 percent), and the following data are measured:
| HT100 steel | HT100 Steel (commercially available chromium salt passivator treatment) | |
| Neutral salt fog resistant (hour) | 85 | 66 |
| Solvent resistance (hours) | 71.5 | 53 |
| Yellowing resistance (hour) | 41 | 30 |
| Adhesion force | Level 1 | Level 1 |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and it will be apparent to those skilled in the art that various modifications and variations can be made in the formulation and preparation process of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A chromium-free conversion agent suitable for a roller coating process and a preparation method thereof are characterized in that the conversion agent comprises the following components in percentage by mass:
5.0-20.0% of phosphoric acid, 1.0-5.0% of nitric acid, 1.5-6.0% of sodium fluotitanate, 1.5-6.0% of sodium fluozirconate, 2.5-8.0% of tartaric acid, 1.0-12.0% of zirconium carbonate, 1.0-10.0% of film-forming assistant, 0.2-3.5% of thickening agent and the balance of deionized water.
2. The chromium-free conversion agent suitable for the roller coating process and the preparation method thereof as claimed in claim 1, wherein the film forming aid comprises one or more of dodecyl alcohol ester, ethylene glycol butyl ether and propylene glycol ethyl ether.
3. The chromium-free conversion agent suitable for the roller coating process and the preparation method thereof as claimed in claim 1, wherein the thickener is one or a mixture of several of carboxyethyl cellulose, sodium alginate, sodium polyacrylate and polyvinyl alcohol.
4. The chromium-free conversion agent suitable for the roller coating process as claimed in claim 1, wherein the material is aluminum and its alloy, ferrous metal, etc.
5. The chromium-free conversion agent suitable for the roller coating process and the preparation method thereof according to claim 1 are characterized in that the preparation method comprises the following steps:
(1) according to the formula composition of raw materials, phosphoric acid, nitric acid, sodium fluotitanate, sodium fluozirconate and deionized water are fully stirred to prepare a solution A;
(2) dissolving tartaric acid, zirconium carbonate, a film forming aid, a thickening agent and the like in a proper amount of deionized water according to a formula of raw materials, and fully stirring until the tartaric acid, the zirconium carbonate, the film forming aid, the thickening agent and the like are dissolved to prepare a solution B;
(3) and slowly adding the solution B into the solution A, and fully stirring to obtain the chromium-free conversion agent.
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