CN108796579B - Nickel-free hole sealing agent for aluminum anodic oxidation - Google Patents
Nickel-free hole sealing agent for aluminum anodic oxidation Download PDFInfo
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- CN108796579B CN108796579B CN201810801849.7A CN201810801849A CN108796579B CN 108796579 B CN108796579 B CN 108796579B CN 201810801849 A CN201810801849 A CN 201810801849A CN 108796579 B CN108796579 B CN 108796579B
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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
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
- C25D11/246—Chemical after-treatment for sealing layers
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Abstract
The invention discloses an aluminum-oxidized nickel-free layer hole sealing agent which mainly comprises 10.5-12.5% of acetate, 0.5-1% of surfactant, 0.2-0.5% of silane coupling agent and 0.5-2% of brightener, and can also comprise the following raw materials in percentage by mass: 0.5-5% of fluorine-containing compound, 0.2-3% of sodium silicate and the balance of water. The aluminum anodic oxidation nickel-free hole sealing agent prepared by the invention mainly comprises low-viscosity organic compounds and inorganic compounds, alkaline earth metal ions are selected, heavy metal ions are avoided, the environment-friendly performance is improved, the stability of a solution system is good, the hole sealing permeation effect is good, a hole sealing film is compact, and pores on the surface of a workpiece can be completely sealed. The surface of the workpiece after hole sealing is flat and bright, does not change color or generate powder, can effectively prevent fingerprints, and is oil-resistant. The strength, hardness and corrosion resistance of the workpiece are improved. The sealant has low price and low energy consumption, and is suitable for industrial mass production.
Description
Technical Field
The invention relates to the technical field of hole sealing of an oxide film, in particular to a nickel-free hole sealing agent for aluminum anodic oxidation.
Background
The aluminum alloy has the advantages of light weight, high strength, high plasticity, high corrosion resistance, high heat conductivity, high electric conductivity and the like, is close to or superior to high-quality steel, can be processed into various sections, and is widely applied to the aviation, aerospace, automobile, mechanical manufacturing and civil industries. The aluminum alloy product has the defects of poor weather resistance and easy corrosion, the surface of aluminum and aluminum alloy must be treated to avoid the corrosion of aluminum profiles, at present, two methods are mainly used, one method is to clean, passivate and spray the surface of the aluminum alloy, the other method is mainly a process of chemical reaction to generate a protective film and improve the corrosion resistance and the binding force, and then the spraying is carried out. However, the workpieces treated by the method mainly relate to the adhesion problem of the coating, and once the coating falls off, the corrosion resistance is greatly influenced. The other is aluminum anodizing, in which an electric field is applied to generate an oxide film on the metal, the oxide film is porous and has strong chemical activity, and after the anodizing is completed, hole sealing surface treatment is performed. The aluminum material treated by the method can obviously improve the weather resistance of the aluminum material, and improve the hardness, wear resistance and corrosion resistance of the surface of the aluminum and the alloy thereof. The outward appearance is more even, can carry out the processing of multiple colour according to the requirement of difference, and the thickness of oxide film can be adjusted according to different technological requirements, and the oxide layer is difficult to suffer destruction easily, can satisfy the higher aluminium alloy production of technological requirement.
With the development of industrial mass production and the development of aluminum and aluminum alloy anodic oxide film technology, higher requirements are provided for hole sealing quality. At present, the anodic oxidation sealant has two problems, namely 1, the nickel-containing sealant occupying most of market shares before is about to gradually exit the market due to the environmental protection problem; 2. the prior nickel-free hole sealing technology in industrial production has the problems of light loss and poor light retention of a hole sealing film, easy whitening and powdering of the surface of an aluminum workpiece after hole sealing, high weight loss of the detected hole sealing, poor stability of bath solution, short service life and the like.
In order to solve the problems, the development and development of a non-toxic environment-friendly bright and smooth green aluminum material hole sealing agent with good hole sealing effect is very high in industrial value.
Disclosure of Invention
In order to solve the problems, the invention discloses a nickel-free sealant for aluminum anodic oxidation.
The technical scheme of the invention is as follows: the nickel-free sealant for aluminum anodic oxidation comprises the following raw materials in percentage by mass:
acetate 10.5-12.5%
0.5 to 1 percent of surfactant
0.2 to 0.5 percent of silane coupling agent
0.5 to 2 percent of brightener
Balance of water
Wherein the acetate is lithium acetate and magnesium acetate, the magnesium acetate is main salt, the lithium acetate is auxiliary salt, and the brightener is sodium polyacrylate or the combination of the sodium polyacrylate and sodium saccharin.
The nickel-free sealant for aluminum anodic oxidation comprises the following raw materials in percentage by mass:
0.5 to 5 percent of fluorine-containing compound
0.2-3% of sodium silicate.
Further, the mass percent of the lithium acetate is 4.5-5.0%, and the mass percent of the magnesium acetate is 6.0-7.5%.
Further, the surfactant is one or more of sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, disodium hexadecyl sulfophenoxy benzene sulfonate, sodium dodecyl diphenyl ether disulfonate and sodium hexadecyl benzene sulfonate.
Further, the fluoride is one or more of potassium fluoride, ammonium bifluoride, fluorozirconic acid and fluotitanic acid.
The aluminum anodic oxidation nickel-free hole sealing agent has the following use process parameters:
1) the aluminum anodic oxidation nickel-free hole sealing agent is in working bath solution, and the content of the hole sealing agent in the bath solution is 1.5-5%;
2) temperature of the solution: 20-45 DEG C
3) Workpiece soaking time: 5-25 min, the hole sealing rate is about 1 μm/min,
4) the pH value of the solution is as follows: 8.0 to 9.5, and the optimum pH is 8.5.
The invention has the advantages that: the aluminum anodic oxidation nickel-free hole sealing agent prepared by the invention mainly comprises low-viscosity organic compounds and inorganic compounds, alkaline earth metal ions are selected, heavy metal ions are avoided, the environment-friendly performance is improved, the stability of a solution system is good, the hole sealing permeation effect is good, a hole sealing film is compact, and pores on the surface of a workpiece can be completely sealed. The surface of the workpiece after hole sealing is flat and bright, does not change color or generate powder, can effectively prevent fingerprints, and is oil-resistant. The strength, hardness and corrosion resistance of the workpiece are improved. The sealant has low price and low energy consumption, and is suitable for industrial mass production.
Detailed Description
The present invention will be described in more detail with reference to examples.
Example 1
The nickel-free sealant for aluminum anodic oxidation comprises the following raw materials in percentage by mass:
5 percent of lithium acetate
Magnesium acetate 5.5%
Sodium dodecyl benzene sulfonate 0.5%
0.2 percent of silane coupling agent
0.5 percent of sodium polyacrylate
Balance of water
The working bath solution contains 2% of a hole sealing agent, and the weight ratio of ph: and 8, the temperature is: at a temperature of 27 ℃.
Pretreating an aluminum product workpiece, carrying out anodic oxidation to prepare an oxide film layer with the thickness of 5-15 microns, soaking the aluminum product workpiece in the sealing liquid for 5-15 minutes, taking out the aluminum product workpiece, cleaning, taking out and air-drying.
By visual inspection: the surface of the aluminum product workpiece after hole sealing is bright and flat, and has no water stain, yellow spots and frost.
The hole sealing weight loss of the aluminum product workpiece which is sealed is detected according to the national standard (GB/T8753.2-2005 nitric acid presoaked phosphoric chromic acid method) and is 15.9mg/dm 2. And dyeing the aluminum product workpiece according to the national standard (a dyeing spot method after acid treatment GB/T8753.4-2005), wherein the dyeing grade is grade 1, the anti-dyeing adsorption capacity is strong, and the sealing quality is qualified and the anti-pollution capacity is strong.
Example 2
The aluminum anodic oxidation nickel-free sealant is characterized in that: the treatment fluid comprises the following components in percentage by weight:
5 percent of lithium acetate
6.5 percent of magnesium acetate
0.6 percent of sodium dodecyl diphenyl ether disulfonate
0.3 percent of silane coupling agent
0.5 percent of sodium polyacrylate
0.1 percent of saccharin sodium
1 percent of potassium fluoride
0.5 percent of sodium silicate
Balance of water
The working solution contains 2.5 percent of hole sealing agent, ph: 8.5, the temperature is: 35 ℃ is carried out.
Pretreating an aluminum product workpiece, carrying out anodic oxidation to prepare an oxide film layer with the thickness of 5-15 microns, soaking the aluminum product workpiece in the sealing liquid for 5-15 minutes, taking out the aluminum product workpiece, cleaning, taking out and air-drying.
By visual inspection: the surface of the aluminum product workpiece after hole sealing is bright and flat, and has no water stain, yellow spots and frost.
The hole sealing weight loss of the aluminum product workpiece which is sealed is detected according to the national standard (GB/T8753.2-2005 nitric acid presoaked phosphoric chromic acid method) and is 12.3mg/dm 2. And (3) dyeing the aluminum product workpiece according to the national standard (a dyeing spot method after acid treatment GB/T8753.4-2005), wherein the dyeing grade is 0 grade, the anti-dyeing adsorption capacity is strong, and the sealing quality is qualified and the anti-pollution capacity is strong.
Example 3
The aluminum anodic oxidation nickel-free sealant is characterized in that: the treatment fluid comprises the following components in percentage by weight:
lithium acetate 4%
6 percent of magnesium acetate
0.3 percent of sodium dodecyl benzene sulfonate
0.3 percent of silane coupling agent
0.6 percent of sodium polyacrylate
0.2 percent of saccharin sodium
2 percent of fluozirconic acid
0.5 percent of sodium silicate
Balance of water
The working solution contains 3% of a hole sealing agent, ph: 8.7, the temperature is: 35 ℃ is carried out.
Pretreating an aluminum product workpiece, carrying out anodic oxidation to prepare an oxide film layer with the thickness of 5-15 microns, soaking the aluminum product workpiece in the sealing liquid for 5-15 minutes, taking out the aluminum product workpiece, cleaning, taking out and air-drying.
By visual inspection: the surface of the aluminum product workpiece after hole sealing is bright and flat, and has no water stain, yellow spots and frost.
The hole sealing weight loss of the aluminum product workpiece which is sealed is detected according to the national standard (GB/T8753.2-2005 nitric acid presoaked phosphoric chromic acid method) and is 9.8mg/dm 2. And (3) dyeing the aluminum product workpiece according to the national standard (a dyeing spot method after acid treatment GB/T8753.4-2005), wherein the dyeing grade is 0 grade, the anti-dyeing adsorption capacity is strong, and the sealing quality is qualified and the anti-pollution capacity is strong.
Example 4
The aluminum anodic oxidation nickel-free sealant is characterized in that: the treatment fluid comprises the following components in percentage by weight:
lithium acetate 4%
8 percent of magnesium acetate
0.3 percent of polyvinylpyrrolidone
0.3 percent of silane coupling agent
0.8 percent of sodium polyacrylate
0.3 percent of saccharin sodium
Fluotitanic acid 3%
0.5 percent of sodium silicate
Balance of water
The working solution contains 4% of a hole sealing agent, and the weight ratio of ph: and 8, the temperature is: at 30 ℃.
Pretreating an aluminum product workpiece, carrying out anodic oxidation to prepare an oxide film layer with the thickness of 5-15 microns, soaking the aluminum product workpiece in the sealing liquid for 5-15 minutes, taking out the aluminum product workpiece, cleaning, taking out and air-drying.
By visual inspection: the surface of the aluminum product workpiece after hole sealing is bright and flat, and has no water stain, yellow spots and frost.
The hole sealing weight loss of the aluminum product workpiece which is sealed is detected according to the national standard (GB/T8753.2-2005 nitric acid presoaked phosphoric chromic acid method) and is 16.3mg/dm 2. And dyeing the aluminum product workpiece according to the national standard (a dyeing spot method after acid treatment GB/T8753.4-2005), wherein the dyeing grade is grade 1, the anti-dyeing adsorption capacity is strong, and the sealing quality is qualified and the anti-pollution capacity is strong.
Example 5
The aluminum anodic oxidation nickel-free sealant is characterized in that: the treatment fluid comprises the following components in percentage by weight:
6 percent of lithium acetate
6.5 percent of magnesium acetate
0.4 percent of sodium dodecyl benzene sulfonate
0.3 percent of silane coupling agent
0.3 percent of sodium polyacrylate
0.6 percent of saccharin sodium
5 percent of ammonium fluoride
0.8 percent of sodium silicate
Balance of water
The working solution contains 5% of a hole sealing agent, ph: 9, the temperature is: at 45 ℃.
Pretreating an aluminum product workpiece, carrying out anodic oxidation to prepare an oxide film layer with the thickness of 5-15 microns, soaking the aluminum product workpiece in the sealing liquid for 5-15 minutes, taking out the aluminum product workpiece, cleaning, taking out and air-drying.
By visual inspection: the surface of the aluminum product workpiece after hole sealing is bright and flat, and has no water stain, yellow spots and frost.
The hole sealing weight loss of the aluminum product workpiece which is sealed is detected according to the national standard (GB/T8753.2-2005 nitric acid presoaked phosphoric chromic acid method) and is 10.3mg/dm 2. And (3) dyeing the aluminum product workpiece according to the national standard (a dyeing spot method after acid treatment GB/T8753.4-2005), wherein the dyeing grade is 0 grade, the anti-dyeing adsorption capacity is strong, and the sealing quality is qualified and the anti-pollution capacity is strong.
Claims (6)
1. The nickel-free hole sealing agent for aluminum anodic oxidation is characterized by comprising the following raw materials in percentage by mass:
acetate 10.5-12.5%
0.5 to 1 percent of surfactant
0.2 to 0.5 percent of silane coupling agent
0.5 to 2 percent of brightener
Balance of water
Wherein the acetate is lithium acetate and magnesium acetate, the magnesium acetate is a main salt, the lithium acetate is an auxiliary salt, and the brightener is sodium polyacrylate or a combination of the sodium polyacrylate and sodium saccharin.
2. The aluminum anodic oxidation nickel-free sealant according to claim 1, comprising the following raw materials by mass percent:
0.5 to 5 percent of fluorine-containing compound
0.2-3% of sodium silicate.
3. The aluminum anodic oxidation nickel-free sealant according to claim 1, wherein: the mass percent of the lithium acetate is 4.5-5.0%, and the mass percent of the magnesium acetate is 6.0-7.5%.
4. The aluminum anodic oxidation nickel-free sealant according to claim 1, wherein: the surfactant is one or more of sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, disodium hexadecyl sulfophenoxy benzene sulfonate, sodium dodecyl diphenyl ether disulfonate and sodium hexadecyl benzene sulfonate.
5. The aluminum anodic oxidation nickel-free sealant according to claim 2, wherein: the fluoride is one or more of potassium fluoride, ammonium bifluoride, fluorozirconic acid and fluotitanic acid.
6. The aluminum anodic oxidation nickel-free sealant according to claim 1 or 2, characterized in that the following process parameters are used:
1) the aluminum anodic oxidation nickel-free hole sealing agent is in working bath solution, and the content of the hole sealing agent in the bath solution is 1.5-5%;
2) temperature of the solution: 20-45 DEG C
3) Workpiece soaking time: 5-25 min, the hole sealing rate is about 1 μm/min,
4) the pH value of the solution is as follows: 8.0 to 9.5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810801849.7A CN108796579B (en) | 2018-07-20 | 2018-07-20 | Nickel-free hole sealing agent for aluminum anodic oxidation |
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| CN201810801849.7A CN108796579B (en) | 2018-07-20 | 2018-07-20 | Nickel-free hole sealing agent for aluminum anodic oxidation |
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| CN108796579B true CN108796579B (en) | 2021-07-06 |
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| CN109440163B (en) * | 2018-12-28 | 2022-02-22 | 江苏飞拓界面工程科技有限公司 | Nickel-free hole sealing agent for aluminum and aluminum alloy anodic oxide films and application thereof |
| CN109778284A (en) * | 2019-01-18 | 2019-05-21 | 广州欧邦联合建材有限公司 | A kind of aluminium ring is protected without nickel sealer, preparation method and its enclosure method |
| CN110359073A (en) * | 2019-07-06 | 2019-10-22 | 彭斌 | A kind of aluminium alloy anode oxide film hole sealing agent and its application method |
| CN110230083A (en) * | 2019-07-09 | 2019-09-13 | 江苏飞拓界面工程科技有限公司 | A kind of aluminium and aluminium alloy anode oxide hole sealing agent and its application |
| CN110512258B (en) * | 2019-10-11 | 2021-03-26 | 东莞市慧泽凌化工科技有限公司 | Nickel-free hole sealing process |
| CN115433985A (en) * | 2022-09-14 | 2022-12-06 | 武汉材料保护研究所有限公司 | Aluminum alloy anodic oxide film low-nickel sealant, aluminum alloy anodic oxide film sealant solution and preparation method thereof |
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| US6506263B1 (en) * | 1999-11-18 | 2003-01-14 | Houghton Metal Finishing Company | Sealant composition |
| US8609254B2 (en) * | 2010-05-19 | 2013-12-17 | Sanford Process Corporation | Microcrystalline anodic coatings and related methods therefor |
| CN102703892B (en) * | 2012-01-14 | 2014-08-20 | 哈尔滨工程大学 | Microarc-oxidized coating silylation fluid and hole sealing method thereby |
| CN104862762B (en) * | 2015-04-27 | 2017-05-10 | 武汉菲尼克化学有限公司 | Aluminum or aluminum alloy anode oxide film hole sealing treatment method |
| CN106191959A (en) * | 2015-05-08 | 2016-12-07 | 广州市汉科建材科技有限公司 | A kind of environment-friendly type aluminium alloy sealing agent |
| US10138566B2 (en) * | 2017-01-13 | 2018-11-27 | Macdermid Acumen, Inc. | Sealing anodized aluminum using a low-temperature nickel-free process |
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