CN107604414B - Aluminum and aluminum alloy anodic oxidation high-temperature nickel-free sealing agent - Google Patents
Aluminum and aluminum alloy anodic oxidation high-temperature nickel-free sealing agent Download PDFInfo
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Abstract
The invention discloses an aluminum and aluminum alloy anodic oxidation high-temperature nickel-free sealing agent, which comprises the following raw materials in mass by volume: 0.5-2.0g/L of surfactant, 0.1-0.5g/L of fading inhibitor, 0.2-1.0g/L of chelating agent, 1.0-5.0g/L of pH buffering agent and the balance of deionized water; the pH value of the sealant working solution is 6.5-8.0, the working temperature is 85-95 ℃, and the sealing speed is 0.5-1.0 mu m/min; the aluminum and aluminum alloy anode oxide film subjected to sealing treatment by the sealant has good corrosion resistance and meets the GB/T8753.2-2005 requirement.
Description
Technical Field
The invention belongs to the technical field of metal surface treatment, and particularly relates to an aluminum and aluminum alloy anodic oxidation high-temperature nickel-free sealing agent, a preparation method and a sealing treatment process of the aluminum and aluminum alloy after anodic oxidation dyeing.
Background
Aluminum and aluminum alloy anodizing techniques are important surface treatment techniques that improve the protective, decorative, and functional properties of aluminum and aluminum alloys. The anodic oxide film which is not sealed has a large number of micropores, is easy to corrode when exposed to the environment, and the corrosion resistance, weather resistance, pollution resistance and the like of the anodic oxide film can not meet the use requirements, so that the micropores for anodic oxidation of aluminum and aluminum alloy need to be sealed in consideration of practical application.
The closure of the aluminum and aluminum alloy anodized films generally employs physical or chemical methods to block the nanopores, thereby reducing the porosity and adsorption properties of the film and improving the hardness and corrosion resistance of the film. At present, nickel salt sealing is the anodic oxide film sealing technology which is most widely applied in domestic and foreign markets in all sealing technologies, the sealing technology is fast in hole sealing, little in organic dye seepage in the hole sealing process, and the corrosion resistance, weather resistance and pollution resistance of the surface of a product after hole sealing are excellent. However, the sealant contains a large amount of heavy metal ions, namely nickel, which has serious harm to natural ecology, strict discharge standards are established for the metal ions in countries of Europe, America and China, and the sealed waste liquid can be discharged only after being strictly treated. Meanwhile, the nickel content of part of the product surface contacting with the human body is also strictly limited.
Therefore, the development of an environment-friendly sealant for replacing nickel salt sealing is called as a hot spot of domestic and foreign research in recent years. The nickel-free sealing agent which is mainly magnesium salt and calcium salt and is released in the market has the defects of unstable tank liquor, easy generation of sealing ash, serious color bleeding during the sealing of a dyeing piece and uneven surface color.
Disclosure of Invention
In order to overcome the defects of the high-temperature nickel-free sealing technology, the invention aims to provide the high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anode oxide film without containing heavy metal ions such as nickel and the like, the comprehensive performance of the high-temperature nickel-free sealing agent is close to that of nickel sealing, and the sealed oxide film has good corrosion resistance and dirt resistance and meets the requirements of GB/T8753.2-2005.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume: 0.5-2.0g/L of surfactant, 0.1-0.5g/L of fading inhibitor, 0.2-1.0g/L, pH g/1.0 g/L of chelating agent and 1.0-5.0g/L of buffering agent, and the balance of deionized water.
Preferably, the surfactant is an anionic surfactant having a sulfonic acid group.
Further preferably, the anionic surfactant containing sulfonic acid group includes, but is not limited to, one or more of sodium alkyl benzene sulfonate, alkyl diphenyl sulfonate, octyl sulfonate, methyl disulfonate, diethyl succinate sodium sulfonate, unsaturated alkyl sodium sulfonate.
Preferably, the fading inhibitor is a polyvinyl pyridine derivative.
Further preferably, the polyvinyl pyridine derivatives include but are not limited to one or two of quaternized polyvinyl pyridine betaine and polyvinyl pyridine oxide.
Preferably, the chelating agent (accelerator) is one or more of ethylenediaminetetraacetic acid, ethylene glycol bis (2-aminoethyl ether) tetraacetic acid, ethylenediaminetetramethylenephosphonic acid (EDTMP), diethylenetriaminepentamethylenemethylenephosphonic acid (DTPMP), hexamethylenediaminetetramethylenephosphonic acid (HDTMP), 2-phospho-1, 2, 4-tricarboxylic acid butane (PBTC), polyol phosphate, sodium polyacrylate, acrylic acid-vinylsulfonic acid copolymer.
Preferably, the pH buffering agent is one or two of ammonium acetate, benzoic acid and ammonium phthalate.
The surface active agent in the high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film is an anionic surface active agent containing sulfonic groups, is a main salt of the high-temperature nickel-free sealing agent, does not contain metal ions easy to hydrolyze and deposit, has excellent hydrophilic performance, can be easily washed clean on the surface of a workpiece after sealing, and has good effect on inhibiting powder frost and water marks. The fading inhibitor has good color fixing effect on an anodic oxide film dyed by organic dye, has less bleeding, and has uniform surface color of a product after hole sealing. The chelating agent (accelerator) can inhibit the influence of harmful ions and accelerate the hydration and blocking process of alumina.
The preparation method of the aluminum and aluminum alloy anodic oxide film high-temperature nickel-free sealing agent comprises the following steps:
(1) adding deionized water with the required amount of 2/3 into a reaction vessel, heating to 45-50 ℃,
(2) sequentially adding surfactant, fading inhibitor, chelating agent, PH buffer agent and the rest deionized water under the stirring speed of 30-40 r/min,
(3) stirring for 5-20 min at the stirring speed of 30-40 rpm,
(4) the test adjusts the pH value to 6.5-7.5,
(5) stirring is continued for 5 to 20 minutes at a stirring speed of 30 to 40 revolutions per minute.
The application process of the aluminum and aluminum alloy anodic oxide film high-temperature nickel-free sealing agent comprises the following steps:
(1) degreasing and deoiling an aluminum and aluminum alloy workpiece, (2) washing; (3) alkaline etching or chemical polishing; (4) washing with water; (5) removing stains and ash; (6) anodizing; (7) washing with water; (8) dyeing; (9) washing with water; (10) sealing treatment is carried out by adopting a sealing agent; (11) washing with water; (12) and (5) drying. Wherein, the degreasing, the alkaline etching, the chemical polishing, the ash removal, the anodic oxidation and the dyeing can adopt the materials and the processes known in the prior art.
Preferably, the pH value of the sealing liquid is 6.5-8.0, the sealing temperature is 85-95 ℃, and the sealing time is 20-30 minutes.
The application process of the aluminum and aluminum alloy anodic oxide film high-temperature nickel-free sealing agent is further improved in that the application process comprises the following steps:
(1) degreasing and deoiling: soaking an aluminum and aluminum alloy workpiece in an alkaline degreasing solution with the concentration of 40-60 g/L and the temperature of 30-70 ℃ for 3-10 minutes to remove oil and dirt, wherein the alkaline degreasing solution is SF-514 of the Aomelon corporation of the Zhuhai;
(2) washing with water: fully washing the surface of the workpiece by using tap water;
(3) alkaline etching or chemical polishing: soaking the aluminum and aluminum alloy workpiece treated in the step (2) in a caustic soda solution with the concentration of 5-10% and the temperature of 40-60 ℃ for 2-5 minutes to remove a natural oxide film on the surface of the workpiece;
(4) washing with water: fully washing the surface of the workpiece by using tap water;
(5) removing stains and ash: putting the aluminum and aluminum alloy workpieces treated in the step (4) into an aqueous solution of nitric acid with the concentration of 10-15% and SF-531 with the concentration of 5-10%, deashing at normal temperature for 30-90 seconds, washing the workpieces with tap water, and then washing the workpieces with pure water, wherein SF-531 is a product of Aomelania, Zhuhai corporation;
(6) anodic oxidation: placing the aluminum and aluminum alloy workpieces treated in the step (5) in an electrolytic solution with the sulfuric acid concentration of 190g/L, and carrying out direct-current oxidation for 30 minutes at the solution temperature of 20 +/-2 ℃ and at the current density of 1.5A/dm2The thickness of the oxide film is 11-13 mu m;
(7) washing with water: washing with deionized water;
(8) dyeing: placing the aluminum and aluminum alloy workpieces treated in the step (7) into a dye for soaking for 10 minutes for coloring, wherein the pH value of a dyeing solution is 6.0;
(9) washing with deionized water to remove loose color;
(10) sealing, namely placing the aluminum and aluminum alloy workpieces treated in the step (9) into the nickel-free sealing agent, wherein the pH value of the sealing liquid is 6.5-8.0, the sealing temperature is 85-95 ℃, and the sealing time is 20-30 minutes;
(11) washing with deionized water;
(12) and (5) drying.
The invention has the advantages of
1. The high-temperature sealing agent prepared by adopting the raw material without containing heavy metal ions such as nickel and the like has no toxicity and harm to the product, and the treatment of the sealed waste liquid is simple;
2. the high-temperature nickel-free sealing agent is particularly suitable for a dyeing process, and has good adaptability to dyes and less fading;
3. the sealing effect of the high-temperature nickel-free sealing agent is comparable to that of nickel salt sealing, and the sealing agent meets the GB/T8753.2-2005 requirement.
Detailed Description
The specific implementation method of the blocking agent of the present invention will now be further illustrated with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The preparation method of the high-temperature nickel-free sealing agent comprises the following steps:
(1) adding deionized water with the required amount of 2/3 into a reaction vessel, heating to 45 ℃,
(2) under the stirring speed of 40 r/min, adding unsaturated alkyl sodium sulfonate, quaternized polyvinyl pyridine betaine, sodium polyacrylate, ammonium acetate and residual deionized water in turn,
(3) stirring for 10 minutes at a stirring speed of 40 revolutions per minute,
(4) the test adjusted the pH to 7,
(5) stirring was continued for 10 minutes at 40 rpm.
Example 2
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The high temperature nickel-free blocking agent was prepared as in example 1.
Example 3
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The high temperature nickel-free blocking agent was prepared as in example 1.
Example 4
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The high temperature nickel-free blocking agent was prepared as in example 1.
Example 5
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The high temperature nickel-free blocking agent was prepared as in example 1.
Example 6
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The high temperature nickel-free blocking agent was prepared as in example 1.
Example 7
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The high temperature nickel-free blocking agent was prepared as in example 1.
Example 8
The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film comprises the following raw materials in mass by volume:
the balance being deionized water.
The high temperature nickel-free blocking agent was prepared as in example 1.
Comparative example 1
The high temperature nickel-free sealant of comparative example 1 was SF-558 from Oumeon, Calif. at a concentration of 7 g/L.
Comparative example 2
The high temperature nickel-free blocking agent of comparative example 2 was DX-500 available from Oney pharmaceutical Co., Ltd at a concentration of 7 g/L.
Application example
Taking 50 identical aluminum alloy workpieces, dividing the aluminum alloy workpieces into 10 groups, dividing each group into 5 blocks, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 1 in group 1, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 2 in group 2, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 3 in group 3, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 4 in group 4, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 5 in group 5, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 6 in group 6, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 7 in group 7, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-free sealing agent in example 8 in group 8, carrying out anodic oxidation sealing treatment by using the high-temperature nickel-, group 10 anodized capping treatment was performed using the high temperature nickel-free capping reagent of comparative example 2.
The method for carrying out anodic oxidation sealing treatment on the aluminum alloy workpiece comprises the following steps:
(1) degreasing and deoiling: taking an aluminum alloy workpiece, and soaking the aluminum alloy workpiece in an alkaline degreasing solution with the concentration of 40-60 g/L and the temperature of 30-70 ℃ for 3-10 minutes to remove oil and dirt, wherein the alkaline degreasing solution is SF-514 of the Aomelon corporation of the Zhuhai;
(2) washing with water: fully washing the surface of the aluminum alloy workpiece by using tap water;
(3) alkaline etching or chemical polishing: soaking the aluminum alloy workpiece treated in the step (2) in a caustic soda solution with the concentration of 5-10% and the temperature of 40-60 ℃ for 2-5 minutes to remove a natural oxide film on the surface of the workpiece;
(4) washing with water: fully washing the surface of the aluminum alloy workpiece by using tap water;
(5) removing stains and ash: placing the aluminum alloy workpiece treated in the step (4) in an aqueous solution of nitric acid with the concentration of 10-15% and SF-531 with the concentration of 5-10%, deashing at normal temperature for 30-90 seconds, washing the aluminum alloy workpiece with tap water, and then washing the aluminum alloy workpiece with pure water, wherein the SF-531 is a product of Aomelon of Zhuhai;
(6) anodic oxidation: placing the aluminum alloy workpiece treated in the step (5) into a furnace with the sulfuric acid concentration of 190In g/L electrolytic solution, direct current oxidation is carried out for 30 minutes under the condition that the solution temperature is 20 +/-2 ℃, and the current density is 1.5A/dm2The thickness of the oxide film is 11-13 um;
(7) washing with water: washing with deionized water;
(8) dyeing: preparing organic dyes with the concentration of 10g/L in five colors of black (3016#), red (4017#), blue (6014#), yellow (200J) and green (7004#), respectively soaking 5 aluminum alloy workpieces in each group treated in the step (7) in the 5 dyes for 10 minutes for coloring, wherein the pH value of a dyeing solution is 6.0;
(9) washing with deionized water to remove loose color;
(10) sealing, namely respectively placing the 1 st to 8 th groups of aluminum alloy workpieces treated in the step (9) into the high-temperature nickel-free sealing agents of the embodiments 1 to 8, wherein the pH value of the sealing liquid is 6.5 to 8.0 (adjusted by acetic acid or ammonia water), the sealing temperature is 85 to 95 ℃, and the sealing time is 30 minutes; respectively placing the aluminum alloy workpieces of the 9 th-10 th groups treated in the step (9) into the high-temperature nickel-free sealing agent of the comparative examples 1-2, wherein the pH value of the sealing liquid is 5.3-5.8 (adjusted by acetic acid or ammonia water), the sealing temperature is 85-90 ℃, and the sealing time is 15 minutes;
(11) washing with deionized water;
(12) and (5) drying.
Performance testing
1. Quality of hole sealing
The method for detecting the sealing quality of the anodic oxide film by using the nitric acid pre-immersion method GB/T8753.2-2005 comprises the following specific steps:
(1) 1 aluminum alloy workpiece of the 1 st group to the 10 th group is stored for 4 hours under natural conditions after being subjected to anodic oxidation sealing;
(2) pre-soaking an aluminum alloy workpiece in a pre-soaking solution at the pre-soaking temperature of 19 +/-1 ℃ for 10 min;
(3) immersing the aluminum alloy workpiece treated in the step (3) in a phosphorus-chromic acid solution at the immersion temperature of 38 +/-1 ℃ for 15 min;
(4) the weight loss per unit area of the workpiece was calculated according to the test method specified in GB/T8753.2-2005 and the result is shown in FIG. 1.
2. Discoloration of organic dyeings
(1) Before dyeing all the workpieces in the groups 1 to 10, after natural air drying or cold air drying, selecting points by using an HP-200 precision color difference instrument to measure colors and sampling;
(2) all the workpieces in the groups 1 to 10 are respectively subjected to sealing treatment by the sealing agents in the embodiments 1 to 8 and the comparative examples 1 to 2, and then are washed clean by deionized water and dried by natural air or cold air;
(3) the color was measured at the selected point in step (1) using an HP-200 precision colorimeter, and the color change △ E of the workpiece surface before and after sealing was compared, the result being shown in FIG. 1.
3. Appearance of the workpiece
The surfaces of the workpieces treated in the groups 1 to 8 are smooth, have no water stain or frost, and the surface color of the dyed workpiece is uniform;
the workpiece treated by the 9 th and 10 th groups has smooth surface, no water stain and no frost, and the surface of the dyed workpiece has uniform color.
TABLE 1 Performance test results for high temperature nickel-free sealants of examples 1-8 and comparative examples 1-2
Claims (6)
1. The high-temperature nickel-free sealing agent for the aluminum and aluminum alloy anodic oxide film is characterized by comprising the following raw materials in mass by volume: 0.5-2.0g/L of surfactant, 0.1-0.5g/L of fading inhibitor, 0.2-1.0g/L, pH g/1.0 g/L of chelating agent and 1.0-5.0g/L of buffering agent, and the balance of deionized water;
the surfactant is an anionic surfactant containing sulfonic acid groups; the sulfonic group-containing anionic surfactant comprises one or more of sodium alkyl benzene sulfonate, alkyl diphenyl sulfonate, octyl sulfonate, methyl disulfonate, diethyl succinate sodium sulfonate and unsaturated alkyl sodium sulfonate;
the fading inhibitor is a polyvinyl pyridine derivative; the polyvinyl pyridine derivative contains one or two of quaternized polyvinyl pyridine betaine and polyvinyl pyridine oxide.
2. The aluminum and aluminum alloy anodized film high-temperature nickel-free sealing agent as recited in claim 1, wherein the chelating agent is one or more of ethylene diamine tetraacetic acid, ethylene glycol bis (2-aminoethyl ether) tetraacetic acid, ethylene diamine tetra methylene phosphonic acid (EDTMP), diethylene triamine penta methylene phosphonic acid (DTPMP), hexamethylene diamine tetra methylene phosphonic acid (HDTMP), 2-phosphate-1, 2, 4-butane tricarboxylate (PBTC), polyol phosphate, sodium polyacrylate, acrylic acid-vinyl sulfonic acid copolymer.
3. The aluminum and aluminum alloy anodized film high-temperature nickel-free sealant as claimed in claim 1, wherein the pH buffer is one or two of ammonium acetate, benzoic acid and ammonium phthalate.
4. The method for preparing the aluminum and aluminum alloy anodic oxide film high-temperature nickel-free sealing agent as recited in any one of claims 1 to 3, comprising the following steps:
(1) adding deionized water with the required amount of 2/3 into a reaction vessel, heating to 45-50 ℃,
(2) sequentially adding surfactant, fading inhibitor, chelating agent, pH buffer and residual deionized water under stirring,
(3) stirring the mixture for 5 to 20 minutes to obtain a mixture,
(4) the test adjusts the pH value to 6.5-7.5,
(5) stirring is continued for 5-20 minutes.
5. The application process of the aluminum and aluminum alloy anodic oxide film high-temperature nickel-free sealing agent as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps:
(1) degreasing and deoiling an aluminum alloy workpiece, (2) washing; (3) alkaline etching or chemical polishing; (4) washing with water; (5) removing stains and ash; (6) anodizing; (7) washing with water; (8) dyeing; (9) washing with water; (10) sealing treatment is carried out by adopting a sealing agent; (11) washing with water; (12) and (5) drying.
6. The application process of the aluminum and aluminum alloy anodic oxide film high-temperature nickel-free sealing agent as claimed in claim 5, wherein the pH value of the sealing agent is 6.5-8.0, the sealing temperature is 85-95 ℃, and the sealing time is 20-30 minutes.
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CN108950645B (en) * | 2018-09-28 | 2020-10-23 | 上海铝通化学科技有限公司 | Aluminum and aluminum alloy anodic oxidation nickel-free sealing agent |
CN109972184B (en) * | 2019-01-23 | 2020-11-06 | 浙江祥可铝塑包装有限公司 | Aluminum cap oxidation process |
CN111074323B (en) * | 2020-01-19 | 2021-10-29 | 南昌航空大学 | Normal-temperature nickel-free sealing liquid for aluminum and aluminum alloy anodic oxidation and sealing method |
CN114959829A (en) * | 2022-06-16 | 2022-08-30 | 江门市优博科技有限公司 | Normal-temperature environment-friendly sealant for dyeing aluminum and aluminum alloy anodic oxide films and preparation method and application process thereof |
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