CN110029389B - Solution for removing hole sealing ash of aluminum alloy anodic oxide film - Google Patents
Solution for removing hole sealing ash of aluminum alloy anodic oxide film Download PDFInfo
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- CN110029389B CN110029389B CN201910310050.2A CN201910310050A CN110029389B CN 110029389 B CN110029389 B CN 110029389B CN 201910310050 A CN201910310050 A CN 201910310050A CN 110029389 B CN110029389 B CN 110029389B
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- oxide film
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- hole sealing
- aluminum alloy
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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
Abstract
The invention provides a solution for removing hole sealing ash of an aluminum alloy anode oxide film, which comprises the following components in percentage by weight: 1.5-3 g/L of alcohol amine, 0.3-1.5 g/L of organic acid, 0.2-1 g/L of complexing agent, 0.5-2 ml/L of scale inhibitor, 10-50 mg/L of anionic surfactant and the balance of deionized water. The solution has the following beneficial effects: 1. removing hole sealing ash formed on the surface of the oxidation film in the hole sealing process, so as to avoid forming a dirty surface; 2. the sealing of the oxide film is promoted, so that the sealing of the oxide film is more thorough; 3. the hole sealing ash is removed, and meanwhile, the oxide film is not damaged; 4. the oxide film after hole sealing can remove hole sealing ash only by soaking for a plurality of minutes, and compared with the method for removing the hole sealing ash by wiping the surface of the oxide film, the method can improve the production efficiency; 5. the solution of the invention is an environment-friendly formula, and the wastewater treatment is simple.
Description
Technical Field
The invention relates to a solution for removing hole sealing ash of an aluminum alloy anodic oxide film, belonging to the technical field of aluminum alloy anodic oxidation.
Background
Aluminum alloy anodic oxidation is a common technology in aluminum alloy surface treatment, and an oxide film with high hardness and bright color is obtained on the surface of the aluminum alloy. However, in order to further improve the performance of the oxide film, especially the anti-fouling capability of the oxide film, the oxide film needs to be subjected to hole sealing treatment, a layer of hole sealing ash is easily formed on the surface of the oxide film in the hole sealing process, and the hole sealing ash is more serious when the hole sealing solution is close to aging.
For the sealing ash on the surface of the oxide film, a method of soaking and wiping with dilute acid is commonly used for removing the sealing ash. Although the dilute acid immersion method is low in cost, it is corrosive to the oxide film, and the corrosion resistance of the oxide film is lowered, resulting in a change in the color tone of the surface of the dyed oxide film. The wiping method for removing the sealing ash is heavy in workload, and particularly, small workpieces with complex surfaces are not suitable for the wiping method.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a solution for removing hole sealing ash of an aluminum alloy anodic oxide film. The sealing ash formed on the surface of the oxide film in the sealing process can be removed, the sealing of the oxide film can be promoted, the oxide film after sealing can be soaked for several minutes to remove the sealing ash, and the production efficiency is obviously improved.
The purpose of the invention is realized by the following technical scheme:
the invention provides a solution for removing hole sealing ash of an aluminum alloy anode oxide film, which comprises the following components in percentage by weight: 1.5-3 g/L of alcohol amine, 0.3-1.5 g/L of organic acid, 0.2-1 g/L of complexing agent, 0.5-2 ml/L of scale inhibitor, 10-50 mg/L of anionic surfactant and the balance of deionized water.
Preferably, the alcohol amine is selected from at least one of triethanolamine or diethanolamine.
Preferably, the organic acid provides an acidic environment and is selected from one or more of citric acid, acetic acid, glycolic acid, tartaric acid.
Preferably, the complexing agent is selected from one or both of EDTA-2Na and NTA.
Preferably, the scale inhibitor is selected from one or more of PBTCA, ATMP and EDTMPS.
Preferably, the anionic surfactant is selected from one of sodium dodecyl diphenyl ether disulfonate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
Preferably, the solution is further added with an organic acid solution or diluted ammonia water to adjust the pH value to 4.0-5.0.
Preferably, the solution for removing the hole sealing ash of the aluminum alloy anodic oxide film comprises the following components in percentage by weight: 2-2.5 g/L triethanolamine, 1.2-1.5 g/L citric acid, 0.3-0.5 g/L EDTA-2Na, 1-1.2 ml/L PBTCA, 30-50 mg/L sodium dodecyl benzene sulfonate and the balance of deionized water.
The triethanolamine is used as a surfactant and a complexing agent in the solution of the invention, and has a promoting effect on hole sealing of an oxide film;
the citric acid is used as an organic acid, and has the functions of providing an acidic environment and a complexing agent in the solution, so that the hole sealing ash is dissolved;
the EDTA-2Na is used as an efficient complexing agent in the solution of the invention to promote the dissolution of the hole sealing ash;
the PBTCA (2-phosphonic acid-1, 2, 4-butane tricarboxylate) is used as a scale inhibitor and a dispersant in the solution of the invention to inhibit the formation of hole sealing ash;
the sodium dodecyl benzene sulfonate is used as an anionic surfactant in the solution, so that the dispersibility of the solution is improved, and the removal of hole sealing ash is accelerated.
Preferably, citric acid solution or diluted ammonia water is added into the solution to adjust the pH value to be 4.0-5.0.
The invention also provides a method for removing the hole sealing ash of the aluminum alloy anodic oxide film according to the solution, which comprises the following steps:
and (3) soaking the aluminum alloy workpiece subjected to hole sealing treatment in the solution, and then cleaning and drying the aluminum alloy workpiece.
Preferably, the soaking temperature is 80-90 ℃, and the soaking time is 2-10 min. More preferably, the soaking time is 3-8 min, and most preferably 4-6 min.
Preferably, the step of cleaning specifically comprises: and cleaning at least 3 times by using EDI treatment water.
Preferably, the drying temperature is 80-85 ℃.
The appearance quality of the treated anodic oxide film can be visually inspected, a workpiece with serious hole sealing ash on the surface is used as an experimental object, the hole sealing ash on the surface of the workpiece after soaking can be completely removed, and the color tone of the surface of the dyed oxide film is not influenced.
Compared with the prior art, the invention has the following beneficial effects:
1. removing hole sealing ash formed on the surface of the oxidation film in the hole sealing process, so as to avoid forming a dirty surface;
2. the sealing of the oxide film is promoted, so that the sealing of the oxide film is more thorough;
3. the hole sealing ash is removed, and meanwhile, the oxide film is not damaged;
4. the oxide film after hole sealing can remove hole sealing ash only by soaking for a plurality of minutes, and compared with the method for removing the hole sealing ash by wiping the surface of the oxide film, the method can improve the production efficiency;
5. the solution of the invention is an environment-friendly formula, and the wastewater treatment is simple.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
The treatment method of the aluminum alloy anodic oxide film specifically comprises the following steps:
1. degreasing
Immersing an aluminum alloy workpiece into a degreasing solution containing 10-15% of sulfuric acid by mass and 1-5 g/L of OP-10 emulsifier for 2-8 min at 40-50 ℃;
2. alkali washing
Immersing the degreased aluminum piece into alkali liquor with the concentration of 50-150 g/L of sodium hydroxide, 1-5 g/L of sodium gluconate and the temperature of 50-60 ℃ for 15-60 s, and removing oxides and dirt naturally formed on the surface of the aluminum piece;
3. neutralization
Hanging ash on the surface of the aluminum piece after alkali washing, immersing the aluminum piece into a nitric acid solution with the concentration of 5-20%, and soaking for 10-60 s at normal temperature;
4. chemical polishing
Using a mixture mainly comprising phosphoric acid (85%) and sulfuric acid (98%) as a chemical polishing solution, wherein the mass ratio of the phosphoric acid to the sulfuric acid is 4:1, the dissolved aluminum is 15-20 g/L, the temperature is 90-100 ℃, 0.1-0.5 g/L copper sulfate is added as a brightening additive, and the chemical polishing time is 10-60 s;
5. neutralization
Ash is hung on the surface of the aluminum piece after chemical polishing, and the neutralization method is the same as the step 3;
6. anodic oxidation
Using an aqueous solution with sulfuric acid concentration of 180-200 g/L as an electrolyte for anodic oxidation, wherein the temperature is 18-20 ℃, the direct-current voltage is 14V, the aluminum content is 2-15 g/L, and the oxidation time is 40 min;
7. dyeing process
Dyeing with black Orye 415 dye, wherein the concentration is 8-12 g/L, the pH value is 5.5-6.0, the temperature is 30-40 ℃, and dyeing is carried out for 5-15 min to obtain dark black;
8. hole sealing
The hole sealing is carried out in the hole sealing solution of the nickel acetate which is close to aging for a long time, and the anodic oxide film with the hole sealing ash can be obtained. The hole sealing time is 40min, and the temperature is 85-95 ℃;
9. soaking for ash removal
Immersing the workpiece after hole sealing into the hole sealing dedusting solution described in each embodiment and comparative example, cleaning for 3 times by using EDI (EDI) processing water after finishing the hole sealing, and drying at 80 ℃;
10. the appearance of the anodized film was examined.
Example 1
The embodiment provides a solution for removing hole sealing ash of an aluminum alloy anode oxide film, which comprises the following components:
the process conditions for soaking and dedusting are as follows: the pH value is 4.4 (adjusted by citric acid or ammonia water), the temperature is 82 ℃, and the soaking time is 4 min; after the completion, the mixture is washed by EDI treated water for 3 times and then dried at 80 ℃.
The surfaces of the dyed oxide film and the oxide film which is immersed into the dust removing solution after the hole sealing of the natural oxide film are not obviously changed by visual inspection, and the surface of the oxide film is wiped by using the wet clean dust-free cloth, so that the hole sealing dust is not detected.
Example 2
The embodiment provides a solution for removing hole sealing ash of an aluminum alloy anode oxide film, which comprises the following components:
the process conditions for soaking and dedusting are as follows: the pH value is 4.7 (adjusted by citric acid or ammonia water), the temperature is 86 ℃, and the soaking time is 6 min; after the completion, the mixture is washed by EDI treated water for 3 times and then dried at 80 ℃.
After the aluminum alloy anodic oxide film is sealed, the aluminum alloy anodic oxide film is soaked by using the sealing ash removal solution of the embodiment, the sealing ash of the black oxide film and the natural color oxide film is completely removed, and the color tone of the surface of the black anodic oxide film is stable.
Example 3
The embodiment provides a solution for removing hole sealing ash of an aluminum alloy anode oxide film, which comprises the following components:
the process conditions for soaking and dedusting are as follows: soaking at 80 deg.C for 10min with pH of 4.0 (adjusted with tartaric acid or ammonia water); after the completion, the mixture is washed by EDI treated water for 3 times and then dried at 80 ℃.
The surfaces of the dyed oxide film and the oxide film which is immersed into the dust removing solution after the hole sealing of the natural oxide film are not obviously changed by visual inspection, and the surface of the oxide film is wiped by using the wet clean dust-free cloth, so that the hole sealing dust is not detected.
Example 4
The embodiment provides a solution for removing hole sealing ash of an aluminum alloy anode oxide film, which comprises the following components:
the process conditions for soaking and dedusting are as follows: soaking at 90 deg.C for 2min with pH of 5.0 (adjusted with glycolic acid or ammonia water); after the completion, the mixture is washed by EDI treated water for 3 times and then dried at 85 ℃.
The surfaces of the dyed oxide film and the oxide film which is immersed into the dust removing solution after the hole sealing of the natural oxide film are not obviously changed by visual inspection, and the surface of the oxide film is wiped by using the wet clean dust-free cloth, so that the hole sealing dust is not detected.
Comparative example 1
The present embodiment provides a solution for removing hole sealing ash of an aluminum alloy anodic oxide film, which has substantially the same composition as that of embodiment 1, except that: EDTA-2Na was not added to the components of this comparative example.
And after the dyed oxide film and the natural-color oxide film are sealed, the oxide film which is immersed into the dust removal solution for treatment is visually checked to have a small amount of dust stain residues on the surface, the wet clean dust-free cloth is used for wiping the surface of the oxide film, and the surface of the dust-free cloth has hole sealing dust traces. But the sealing ash can be completely removed by prolonging the soaking time.
Comparative example 2
The present embodiment provides a solution for removing hole sealing ash of an aluminum alloy anodic oxide film, which has substantially the same composition as that of embodiment 1, except that: EDTA-2Na was not added to the composition of this comparative example, and the triethanolamine content was 2.5 g/L.
The surfaces of the dyed oxide film and the oxide film which is immersed into the dust removal solution after the holes of the natural oxide film are sealed are slightly remained with hole sealing ash through visual inspection, the surface of the oxide film is wiped by using wet clean dust-free cloth, and the dust-free cloth also has hole sealing ash.
Comparative example 3
The present embodiment provides a solution for removing hole sealing ash of an aluminum alloy anodic oxide film, which has substantially the same composition as that of embodiment 3, except that: the scale inhibitor ATMP was not added to the components of this comparative example.
And (3) visually checking the surface of the oxide film subjected to the treatment of immersing the dyed oxide film and the natural-color oxide film in a dust removal solution after hole sealing to have hole sealing ash, wiping the surface of the oxide film by using wet clean dust-free cloth, and leaving hole sealing ash residues on the dust-free cloth.
Comparative example 4
The present embodiment provides a solution for removing hole sealing ash of an aluminum alloy anodic oxide film, which has substantially the same composition as that of embodiment 4, except that: the components of the comparative example were not added with sodium dodecyl diphenyl ether disulfonate.
And (3) visually checking the watermarks at the bottom of the aluminum alloy workpiece by using the dyed oxide film and the oxide film which is immersed in the ash removal solution after the holes of the natural color oxide film are sealed, wiping the surface of the oxide film by using the wet clean dust-free cloth, and leaving no hole sealing ash residue except the bottom watermarks.
In summary, the solution for removing the hole sealing ash of the aluminum alloy anodic oxide film provided by the invention has the following advantages:
1. removing hole sealing ash formed on the surface of the oxidation film in the hole sealing process, so as to avoid forming a dirty surface;
2. the sealing of the oxide film is promoted, so that the sealing of the oxide film is more thorough;
3. the hole sealing ash is removed, and meanwhile, the oxide film is not damaged;
4. the oxide film after hole sealing can remove hole sealing ash only by soaking for a plurality of minutes, and compared with the method for removing the hole sealing ash by wiping the surface of the oxide film, the method can improve the production efficiency;
5. the solution of the invention is an environment-friendly formula, and the wastewater treatment is simple.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (9)
1. The solution for removing the hole sealing ash of the aluminum alloy anodic oxide film is characterized by comprising the following components in parts by weight: 1.5-3 g/L of alcohol amine, 0.3-1.5 g/L of organic acid, 0.2-1 g/L of complexing agent, 0.5-2 ml/L of scale inhibitor, 10-50 mg/L of anionic surfactant and the balance of deionized water;
the scale inhibitor is selected from one or more of PBTCA, ATMP and EDTMPS.
2. The solution for removing the sealing ash of the aluminum alloy anodic oxide film according to claim 1, wherein the alcohol amine is at least one selected from the group consisting of triethanolamine and diethanolamine.
3. The solution for removing the sealing ash of the aluminum alloy anodic oxide film according to claim 1, wherein the organic acid provides an acidic environment and is selected from one or more of citric acid, acetic acid, glycolic acid and tartaric acid.
4. The solution for removing the sealing ash of the aluminum alloy anodic oxide film according to claim 1, wherein the complexing agent is one or two selected from EDTA-2Na and NTA.
5. The solution for removing the sealing ash of the aluminum alloy anodic oxide film according to claim 1, wherein the anionic surfactant is one selected from the group consisting of sodium dodecyl diphenyl oxide disulfonate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
6. The solution for removing the hole sealing ash of the aluminum alloy anode oxide film according to claim 1, wherein an organic acid solution or dilute ammonia water is further added to the solution to adjust the pH value to 4.0-5.0.
7. The method for removing the hole sealing ash of the aluminum alloy anodic oxide film by using the solution as claimed in claim 1 is characterized by comprising the following steps:
and (3) soaking the aluminum alloy workpiece subjected to hole sealing treatment in the solution, and then cleaning and drying the aluminum alloy workpiece.
8. The method for removing the hole sealing ash of the aluminum alloy anodic oxide film according to claim 7, wherein the soaking temperature is 80 to 90 ℃ and the soaking time is 2 to 10 min.
9. The method for removing the hole sealing ash of the aluminum alloy anodic oxide film according to claim 7, wherein the drying temperature is 80-85 ℃; the cleaning steps are specifically as follows: and cleaning at least 3 times by using EDI treatment water.
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| TWI444508B (en) * | 2012-05-07 | 2014-07-11 | Catcher Technology Co Ltd | Method for manufacturing a metallic substrate with skidproof leather-like surface |
| US9187841B2 (en) * | 2012-08-16 | 2015-11-17 | Catcher Technology Co., Ltd. | Method of forming skid-proof leather-texture surface on metallic substrate |
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| CN87102467A (en) * | 1987-03-29 | 1988-10-12 | 广东有色金属加工厂 | The pore sealing method of aluminium and alloy anodized film thereof |
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