CN107201514B - Magnesium alloy chromium-free passivator and use method thereof - Google Patents
Magnesium alloy chromium-free passivator and use method thereof Download PDFInfo
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- CN107201514B CN107201514B CN201710339367.XA CN201710339367A CN107201514B CN 107201514 B CN107201514 B CN 107201514B CN 201710339367 A CN201710339367 A CN 201710339367A CN 107201514 B CN107201514 B CN 107201514B
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- passivator
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- chromium
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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
- C23C22/48—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
- C23C22/57—Treatment of magnesium or alloys based thereon
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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
- C23C22/68—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 solutions with pH between 6 and 8
Abstract
The invention discloses a magnesium alloy chromium-free passivator and a use method thereof, wherein the magnesium alloy chromium-free passivator comprises the following components: titanium compounds and derivatives thereof, zirconium compounds and derivatives thereof, nanoparticles, thiourea and coupling agents; the titanium compound and the derivative thereof are one or the combination of diethanol amine diisopropyl titanate and triethanol amine diisopropyl titanate, and the zirconium compound and the derivative thereof are one or the combination of fluozirconic acid, fluotitanic acid and triethanol amine zirconate; the coupling agent is one or the combination of a titanate coupling agent, a zirconic acid coupling agent, a molybdate coupling agent and a vanadate coupling agent. The magnesium alloy chromium-free passivator and the use method provided by the invention can solve the problem of large amount of wastewater pollution caused by traditional chromizing water washing, and also solve the problem that the corrosion protection performance of a chromium-free product on metal and the adhesive force performance of the chromium-free product with a coating can not reach the effect of a chromizing product.
Description
Technical Field
The invention relates to a passivator and a use method thereof, in particular to a magnesium alloy chromium-free passivator and a use method thereof.
Background
Magnesium alloys are currently the lightest metallic structural materials, with strengths close to those of aluminum alloys. The specific strength is higher than that of aluminum alloy and steel and slightly lower than that of the fiber reinforced plastic with the highest specific strength. The shock absorber has good shock absorption and can bear larger impact vibration load. Magnesium alloy is known as an ideal substitute material for electronic product housings and light vehicles in the 21 st century. However, magnesium is an extremely active metal and has poor corrosion resistance, which restricts the use of magnesium alloys. Therefore, when magnesium alloys are used as structural materials, appropriate surface treatment is required to improve corrosion resistance.
The chemical conversion treatment in the existing anticorrosion measures has the problem of environmental pollution, and most of anticorrosion treatment agents contain chromium or nonferrous metal elements, so that the anticorrosion treatment agents have different degrees of harm to the environment and human bodies. In view of the environmental protection pressure, the use of chromium-free environmental-friendly treatment solutions is increasing, and researchers in various countries strive to develop more effective and environmentally-friendly surface treatment technologies for magnesium and magnesium alloys. The prior patent results show that most of the chromium-free passivation film systems applied in industry are in the direction of molybdate system, zirconate system, silane system or rare earth system, but the current research in all directions does not obtain satisfactory research results, and the corrosion protection performance of products in all directions on metal and the adhesion performance of products in all directions can not be comparable to those of chromated passivation films.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a magnesium alloy chromium-free passivator and a use method thereof, which can solve the problem of large amount of wastewater pollution caused by traditional chromizing water washing, and simultaneously solve the problem that the corrosion protection performance of a chromium-free product on metal and the adhesive force performance of the chromium-free product with a coating can not reach the effect of a chromizing product.
The technical scheme adopted by the invention for solving the technical problems is to provide a magnesium alloy chromium-free passivator and a use method thereof, wherein the magnesium alloy chromium-free passivator comprises the following components: titanium compounds and derivatives thereof, zirconium compounds and derivatives thereof, nanoparticles, thiourea and coupling agents.
The magnesium alloy chromium-free passivator comprises a titanium compound and a derivative thereof, wherein the titanium compound and the derivative thereof are one or a combination of diethanol amine diisopropyl titanate and triethanol amine diisopropyl titanate, and the zirconium compound and the derivative thereof are one or a combination of fluozirconic acid, fluotitanic acid and triethanol amine zirconate.
The magnesium alloy chromium-free passivator is characterized in that the coupling agent is one or a combination of a titanate coupling agent, a zirconic acid coupling agent, a molybdate coupling agent and a vanadate coupling agent.
The magnesium alloy chromium-free passivator is characterized in that the nano particles are one or a combination of nano zirconium dioxide, nano titanium dioxide, nano silicon dioxide, nano zinc dioxide, nano aluminum oxide and nano copper oxide.
The magnesium alloy chromium-free passivator also comprises the following components: organic matter of carboxylic acid group, organic matter of hydroxyl group and fatty alcohol polyoxyethylene ether.
The magnesium alloy chromium-free passivator comprises the following components in percentage by weight:
compounds of titanium and derivatives thereof: 0.1-3 mol/L;
zirconium compounds and derivatives thereof: 0.1-3 mol/L;
nanoparticle: 0.1-1 mol/L;
thiourea: 0.1-1 mol/L;
coupling agent: 10 to 1000 ppm;
organic carboxylic group: 10 to 1000 ppm;
hydroxyl group-containing organic material: 10 to 1000 ppm;
fatty alcohol polyoxyethylene ethers: 10 to 1000 ppm.
The magnesium alloy chromium-free passivator is characterized in that the molecular formula of the organic matter of the carboxylic group is R-COOH, R- (COOH) n or R- (COO) n-R', and the molecular formula of the organic matter of the hydroxyl group is R-OH or R- (OH) n; the fatty alcohol-polyoxyethylene ether is a C2-C20 fatty alcohol-polyoxyethylene ether organic substance and a polymer thereof, R and R' are carbon-containing organic functional groups, and n > is 1.
The invention also provides a use method of the magnesium alloy chromium-free passivator for solving the technical problems, wherein the use method comprises the following steps: s1, adding a titanium compound and a derivative thereof, a zirconium compound and a derivative thereof, nano particles, thiourea and a coupling agent into water in proportion, uniformly mixing, and adjusting the pH value of the passivating agent to 4.5-6.5 to obtain a washing-free chromium-free passivating agent; s2, soaking the material to be treated in the passivator after oil removal and cleaning, taking out, cleaning and drying or naturally airing to obtain the material with the surface provided with the chromate-free passivation film; s3, or spraying the passivator on the surface of the material to be treated, and drying or naturally airing the material after cleaning to obtain the material with the surface provided with the chromate-free passivation film; and S4, or coating the passivator on the surface of the material to be treated, cleaning and drying to obtain the material with the surface provided with the water-washing-free chromized passivation film.
The use method of the magnesium alloy chromium-free passivator comprises the following steps of preparing a passivator in step S1, wherein the water is pure water or tap water, and the dilution ratio is 1: (10-60); in the step S1, nitric acid, acetic acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammonia water, or ammonium bicarbonate is used to adjust the pH of the passivation agent.
The use method of the magnesium alloy chromium-free passivator comprises the following steps of soaking for 1-40 minutes in the step S2; in the step S3, the spraying pressure is 0.5-1.5 bar, and the spraying time is 20-180 seconds; and in the step S4, the coating mode is roll coating, blade coating or dip coating, and the coating time is 10-60 seconds.
Compared with the prior art, the invention has the following beneficial effects: the invention provides a magnesium alloy chromium-free passivator and a use method thereof.A titanium titanate is used as an inorganic passivation film of a main film forming salt, and is matched with silicon-containing nano particles, zirconate and the like to form an organic passivation film which can form a passivation film on the surface of magnesium and magnesium alloy; the passive film has excellent anticorrosive performance of a bare film and simultaneously has excellent adhesion performance with powder or paint; thereby solving the problem of large amount of wastewater pollution caused by the traditional chromizing water washing and simultaneously solving the problem that the corrosion protection performance of the chromium-free product to metal and the adhesive force performance of the chromium-free product to a coating can not reach the effect of the chromizing product.
Detailed Description
The present invention will be further described with reference to the following examples.
The invention provides a magnesium alloy chromium-free passivator, which mainly comprises at least one of zirconium/titanium-containing compounds and derivatives thereof, corrosion inhibitors, deionized water and coupling agents, and at least one of nano particles and thiourea.
The zirconium compound and the derivative thereof are one or a compound of fluozirconic acid/fluotitanic acid/triethanolamine zirconate and other chemical substances.
The titanium compound and the derivative thereof are one or a compound of titanate chemicals such as diethanol amine diisopropyl titanate or triethanol amine diisopropyl titanate and the like.
The corrosion inhibitor is one or a compound of triethanolamine, monoethanolamine, a coupling agent and derivatives thereof or thiourea.
The nano particles can comprise at least one of nano zirconium dioxide, nano titanium dioxide, nano silicon dioxide, nano zinc dioxide, nano aluminum oxide and nano copper oxide or a compound.
The coupling agent can be at least one of zirconate coupling agent, titanate coupling agent, molybdate coupling agent and vanadate coupling agent or a compound.
The passivator of the invention also comprises the following components: organic matter of carboxylic acid group, organic matter of hydroxyl group and fatty alcohol polyoxyethylene ether. The concrete components are as follows:
compounds of titanium and derivatives thereof: 0.1 to 3mol/L
Zirconium compounds and derivatives thereof: 0.1 to 3mol/L
Nanoparticle: 0.1 to 1mol/L
Thiourea: 0.1 to 1mol/L
Coupling agent: 10 to 1000ppm
Organic carboxylic group: 10 to 1000ppm
Hydroxyl group-containing organic material: 10 to 1000ppm
Fatty alcohol polyoxyethylene ethers: 10 to 1000ppm
And at least one of nitric acid, acetic acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammonia water and ammonium bicarbonate is used for regulating the pH value of the passivating agent.
The organic matter with carboxylic acid group in the invention can be organic matter with a general formula of R-COOH, R- (COOH) n or R- (COO) n-R '(wherein R and R' are organic functional groups containing carbon, and n is equal to or more than 1), and polymer and modified molecular structure thereof; the hydroxyl group organic matter can be an organic matter with a general formula of R-OH or R- (OH) n (wherein R and R' are organic functional groups containing carbon, and n is equal to or greater than 1), and a polymer and a modified molecular structure thereof; the fatty alcohol polyoxyethylene ether containing organic matter can be C2-C20 fatty alcohol polyoxyethylene ether organic matter and polymer and modified molecular structure thereof.
The invention also provides a using method of the passivator, which comprises the following steps:
1. adding a titanium compound and a derivative thereof, a zirconium compound and a derivative thereof, nano particles, thiourea and a coupling agent into water in proportion, uniformly mixing, and adjusting the pH value of the passivating agent to be 4.5-6.5 to obtain the water-washing-free chromium-free passivating agent.
2. And (3) soaking the material to be treated in the passivator after oil removal and cleaning, taking out, cleaning and drying or naturally airing to obtain the material with the surface provided with the chromate-free passivation film.
3. Or spraying the passivating agent on the surface of the material to be treated, and drying or naturally airing the material after cleaning to obtain the material with the surface provided with the chromium-free passivation film.
4. Or coating the passivator on the surface of the material to be treated, cleaning and drying to obtain the material with the surface provided with the water-washing-free chromized passivation film.
5. The water used for preparing the passivating agent in the step 1 can be pure water or tap water
6. The passivating agent in the step 1 can be diluted by water for reuse, and the dilution ratio is 1: (10 to 60)
7. The pH value can be adjusted according to the actual production requirement in the step 1, and the pH value of the passivating agent can be adjusted by at least one of nitric acid, acetic acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammonia water and ammonium bicarbonate
8. The soaking time in the step 2 can be adjusted according to the actual production requirements, and the soaking time is preferably 1-40 minutes
9. The spraying treatment pressure and time in the step 3 can be adjusted according to actual production requirements, the spraying pressure is preferably 0.5-1.5 bar, and the spraying time is 20-180 seconds.
10. The coating method in the step 4 is a coating method commonly used in the field, such as roll coating, blade coating, dip coating and the like, the coating time can be adjusted according to the actual production requirement, and the preferable coating time is 10-60 seconds.
11. The material treated by the passivating agent needs to be washed, naturally dried or dried to directly carry out subsequent processing, and the drying temperature is preferably less than 120 ℃.
12. The material may be a metallic material, steel, zinc, aluminium, copper, magnesium and alloys thereof, preferably magnesium and alloys thereof. The material can have the following properties after subsequent treatment:
therefore, the magnesium alloy chromium-free passivator and the use method thereof provided by the invention have the advantages that an inorganic passivation film taking titanate as main film forming salt is matched with silicon-containing nano particles, zirconate and the like to form an organic passivation film, and the passivation film can be formed on the surfaces of magnesium and magnesium alloy; the passive film has excellent anticorrosive performance of bare film and excellent adhesion performance to powder or paint. The chromium-free water washing method has excellent corrosion protection performance on metal and adhesive force performance with a coating in the traditional chromium-free water washing process, and simultaneously solves the problem that the corrosion protection performance on the metal and the adhesive force performance with the coating of a chromium-free product can not reach the effect of a chromium-free product.
Claims (6)
1. The magnesium alloy chromium-free passivator is characterized by comprising the following components: titanium compounds and derivatives thereof, zirconium compounds and derivatives thereof, nanoparticles, thiourea and coupling agents;
also comprises the following components: organic matters of carboxylic acid group groups, organic matters of hydroxyl group groups and fatty alcohol polyoxyethylene ether;
the proportion of each component is as follows:
compounds of titanium and derivatives thereof: 0.1-3 mol/L;
zirconium compounds and derivatives thereof: 0.1-3 mol/L;
nanoparticle: 0.1-1 mol/L;
thiourea: 0.1-1 mol/L;
coupling agent: 10 to 1000 ppm;
organic carboxylic group: 10 to 1000 ppm;
hydroxyl group-containing organic material: 10 to 1000 ppm;
fatty alcohol polyoxyethylene ethers: 10 to 1000 ppm;
the titanium compound and the derivative thereof are one or the combination of diethanol amine diisopropyl titanate and triethanol amine diisopropyl titanate, and the zirconium compound and the derivative thereof are triethanol amine zirconate;
the coupling agent is one or the combination of a titanate coupling agent and a zirconic acid coupling agent.
2. The magnesium alloy chromium-free passivator according to claim 1, wherein the nano particles are one or a combination of nano zirconium dioxide, nano titanium dioxide, nano silicon dioxide, nano zinc dioxide, nano aluminum oxide and nano copper oxide.
3. The magnesium alloy chromium-free passivator according to claim 1, wherein the organic formula of the carboxylic group is R-COOH, R- (COOH) n or R- (COO) n-R', and the organic formula of the hydroxyl group is R-OH or R- (OH) n; the fatty alcohol-polyoxyethylene ether is a C2-C20 fatty alcohol-polyoxyethylene ether organic substance and a polymer thereof, R and R' are carbon-containing organic functional groups, and n > = 1.
4. The use method of the magnesium alloy chromium-free passivator as defined in any one of claims 1-3, characterized by comprising the following steps:
s1, adding a titanium compound and a derivative thereof, a zirconium compound and a derivative thereof, nano particles, thiourea and a coupling agent into water in proportion, uniformly mixing, and adjusting the pH value of the passivating agent to 4.5-6.5 to obtain a water-washing-free chromium-free passivating agent;
s2, soaking the material to be treated in the passivator after oil removal and cleaning, taking out, cleaning and drying or naturally airing to obtain the material with the surface provided with the chromate-free passivation film;
s3, or spraying the passivator on the surface of the material to be treated, and drying or naturally airing the material after cleaning to obtain the material with the surface provided with the chromate-free passivation film;
and S4, or coating the passivator on the surface of the material to be treated, cleaning and drying to obtain the material with the surface provided with the water-washing-free chromized passivation film.
5. The method for using the magnesium alloy chromium-free passivator according to claim 4, wherein the water for preparing the passivator in the step S1 is pure water or tap water, and the dilution ratio is 1: (10-60); in the step S1, nitric acid, acetic acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, sodium hydroxide, potassium hydroxide, ammonia water, or ammonium bicarbonate is used to adjust the pH of the passivation agent.
6. The use method of the magnesium alloy chromium-free passivator according to claim 4, wherein the soaking time in the step S2 is 1-40 minutes; in the step S3, the spraying pressure is 0.5-1.5 bar, and the spraying time is 20-180 seconds; and in the step S4, the coating mode is roll coating, blade coating or dip coating, and the coating time is 10-60 seconds.
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| CN108642482A (en) * | 2018-07-03 | 2018-10-12 | 苏州大韩化工有限公司 | A kind of chromium-free passivation liquid and preparation method thereof |
| CN115613022A (en) * | 2022-09-28 | 2023-01-17 | 湖南金裕环保科技有限公司 | Chromium-free natural color passivating agent for aluminum and aluminum alloy and preparation method thereof |
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| CN1381532A (en) * | 2001-04-19 | 2002-11-27 | 日本油漆株式会社 | Nonchromate metal surface finishing agent, surface handling and method and processed steel products |
| JP4629987B2 (en) * | 2004-03-19 | 2011-02-09 | 日本ペイント株式会社 | Sealing agent, phosphating steel sheet coating method and phosphating steel sheet |
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Effective date of registration: 20210316 Address after: 246000 No.1, Weisan Road, high tech Industrial Development Zone, Daguan District, Anqing City, Anhui Province Patentee after: Anhui Guanghua DIYe Chemical Co.,Ltd. Address before: No.28, Lane 156, Changji Road, Jiading District, Shanghai, 201800 Patentee before: EMPIRECHEM (SHANGHAI) Co.,Ltd. |