CN105200493A - Nickel-free hole sealing agent for bright and smooth aluminum alloy anode oxide film and preparation method of nickel-free hole sealing agent - Google Patents
Nickel-free hole sealing agent for bright and smooth aluminum alloy anode oxide film and preparation method of nickel-free hole sealing agent Download PDFInfo
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- CN105200493A CN105200493A CN201510614452.3A CN201510614452A CN105200493A CN 105200493 A CN105200493 A CN 105200493A CN 201510614452 A CN201510614452 A CN 201510614452A CN 105200493 A CN105200493 A CN 105200493A
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- 238000007789 sealing Methods 0.000 title claims abstract description 42
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- -1 2-mercapto benzimidazole rare earth Chemical class 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052912 lithium silicate Inorganic materials 0.000 claims abstract description 8
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229940069446 magnesium acetate Drugs 0.000 claims abstract description 8
- 235000011285 magnesium acetate Nutrition 0.000 claims abstract description 8
- 239000011654 magnesium acetate Substances 0.000 claims abstract description 8
- 239000004094 surface-active agent Substances 0.000 claims abstract description 8
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000005695 Ammonium acetate Substances 0.000 claims abstract description 7
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940043376 ammonium acetate Drugs 0.000 claims abstract description 7
- 235000019257 ammonium acetate Nutrition 0.000 claims abstract description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 6
- 239000011701 zinc Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 30
- 229910052759 nickel Inorganic materials 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- 238000013329 compounding Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000000839 emulsion Substances 0.000 claims description 6
- 229960004418 trolamine Drugs 0.000 claims description 6
- YCPXWRQRBFJBPZ-UHFFFAOYSA-N 5-sulfosalicylic acid Chemical compound OC(=O)C1=CC(S(O)(=O)=O)=CC=C1O YCPXWRQRBFJBPZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 abstract description 2
- WXHLLJAMBQLULT-UHFFFAOYSA-N 2-[[6-[4-(2-hydroxyethyl)piperazin-1-yl]-2-methylpyrimidin-4-yl]amino]-n-(2-methyl-6-sulfanylphenyl)-1,3-thiazole-5-carboxamide;hydrate Chemical compound O.C=1C(N2CCN(CCO)CC2)=NC(C)=NC=1NC(S1)=NC=C1C(=O)NC1=C(C)C=CC=C1S WXHLLJAMBQLULT-UHFFFAOYSA-N 0.000 abstract 2
- LBTSNEJGMVFUEW-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,8,8,8-dodecafluorooctoxy-dimethoxy-propylsilane Chemical compound FC(C(C(C(C(F)(F)CO[Si](OC)(OC)CCC)(F)F)(F)F)(F)F)CC(F)(F)F LBTSNEJGMVFUEW-UHFFFAOYSA-N 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract 1
- 239000000908 ammonium hydroxide Substances 0.000 abstract 1
- 230000003373 anti-fouling effect Effects 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 abstract 1
- 239000011737 fluorine Substances 0.000 abstract 1
- 239000012466 permeate Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 239000011148 porous material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- VRAIHTAYLFXSJJ-UHFFFAOYSA-N alumane Chemical compound [AlH3].[AlH3] VRAIHTAYLFXSJJ-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000008393 encapsulating agent Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 229910000553 6063 aluminium alloy Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 238000004500 asepsis Methods 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- Sealing Battery Cases Or Jackets (AREA)
- Gasket Seals (AREA)
Abstract
The invention discloses a nickel-free hole sealing agent for a bright and smooth aluminum alloy anode oxide film. The nickel-free hole sealing agent is prepared from, by weight, 8-8.5 parts of magnesium acetate, 19-20 parts of triethanolamine, 3-3.2 parts of ammonium acetate, a proper amount of deionized water, 1.1-1.2 parts of LiF, 0.4-0.5 part of sulfosalicylic acid, 0.4-0.5 part of zinc polysilicate, 0.4-0.5 part of 2-mercapto benzimidazole rare earth complex, 0.4-0.5 part of lithium silicate, 2.6-2.8 parts of dodecafluoroheptyl-propyl-trimethoxysilane, 1-1.2 parts of tetrabutyl titanate, 45-48 parts of ethyl alcohol, 8.6-9 parts of ammonium hydroxide and 0.3-0.4 part of fluorine-containing surfactant. According to the hole sealing agent, LiF, sulfosalicylic acid, zinc polysilicate and 2-mercapto benzimidazole rare earth complex are used, the affinity to aluminum alloy is high, the hole sealing agent can permeate into holes, the sealing performance is good, the surface of the oxide film obtained after hole sealing can be bright and good in smoothness, and corrosion resistance and anti-fouling performance are greatly improved.
Description
Technical field
The present invention relates to aluminium alloy anode oxide film without nickel hole sealing agent technical field, particularly relate to a kind of bright smooth aluminium alloy anode oxide film without nickel hole sealing agent and preparation method thereof.
Background technology
At present, Aluminum-aluminum alloy generally adopts anodized surface guard technology, certain thickness oxide film is formed on Aluminum-aluminum alloy surface, there is a large amount of micropore in the surface due to oxide film, must suitable sealing treatment be carried out, common enclosure method mainly contain boiling water (or steam) close, nickel salt close, macromolecule resin close.Boiling water (or steam) enclosure method energy consumption is high and cannot meet the requirement compared with high anti-corrosion; Conventional nickel salt encapsulant is containing Ni
2+, F
-to human body and the effect of environmental toxic evil, its stripping quantity is subject to the strict restriction of the regulations such as European Union 94/27/EEC nickel instruction; The molecular volume of macromolecule resin is too large, cannot diffuse into pore interior and realize good closed performance.Therefore, the demand energy-efficient, the green aluminum anodized film sealing technique of asepsis environment-protecting is developed is urgent, wherein, the hole sealing agent being main component with an alkali metal salt or alkaline earth salt has the characteristics such as resource is wide, with low cost, environmental friendliness, is a kind of novel green anode oxide film hole sealing agent.The U.S., Wuhan Inst. of Material Protection of China have successively carried out the technical study of alkaline earth salt sealing of hole." 6063 aluminium alloy anode oxide films are without the optimization of nickel hole-sealing technology " literary composition take magnesium acetate as hole sealing agent main component, orthogonal experiment is adopted to have studied the impact of hole-sealing technology parameter on sealing quality, obtain the Optimization Technology without nickel hole sealing technology, and the technique applied research of anti-ion interference has been carried out to this technique.Result shows, can the realizing in 80 DEG C antianode oxide film under temperature without nickel hole-sealing technology and carry out sealing pores of optimization, and sealing quality is good, anti-Na
+interference performance is given prominence to, and achieves sealing of hole process without Ni
2+deng environomental pollution source, environmental protection, and the reduction of sealing of hole temperature is conducive to reducing energy consumption, and energy-saving benefit is remarkable.But this technique still has weak point, anti-SO
4 2-disturb poor, and perviousness is bad, the space closure of the oxide film bottom of bottom is bad, also there is the problem that the performances such as germ resistance, solidity to corrosion, thermotolerance, salt fog resistance, wear resistance, oxidation-resistance are not good, and the toughness of encapsulant, hardness, shrinking percentage etc. also can affect closure, need to improve.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of bright smooth aluminium alloy anode oxide film without nickel hole sealing agent and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of bright smooth aluminium alloy anode oxide film, without nickel hole sealing agent, is made up of the raw material of following weight part: magnesium acetate 8-8.5, trolamine 19-20, ammonium acetate 3-3.2, deionized water are appropriate, LiF1.1-1.2, sulphosalicylic acid 0.4-0.5, zinc polysilicate 0.4-0.5,2-mercaptobenzimidazole rare earth compounding 0.4-0.5, lithium silicate 0.4-0.5, ten difluoro heptyl propyl trimethoxy silicane 2.6-2.8, tetrabutyl titanate 1-1.2, ethanol 45-48, ammoniacal liquor 8.6-9, fluorochemical surfactant 0.3-0.4.
The smooth aluminium alloy anode oxide film of described light, without the preparation method of nickel hole sealing agent, comprises the following steps:
(1) by tetrabutyl titanate, ethanol mixing, stirring obtains tetrabutyl titanate ethanolic soln, by lithium silicate, ten difluoro heptyl propyl trimethoxy silicanes, fluorochemical surfactant, the mixing of 2-mercaptobenzimidazole rare earth compounding, the water adding 5-6 weight part stirs, obtain solution, to instill in tetrabutyl titanate ethanolic soln under described solution stirring, 1.5-1.8h is stirred under 250-300r/min condition, obtain mixture, then ammoniacal liquor is slowly dripped in people's said mixture, at 30-35 DEG C, obtain emulsion after stirring reaction 3-3.5h;
(2) mixing solutions is prepared, magnesium acetate 8g/L, trolamine 19g/L, ammonium acetate 3g/L;
(3) emulsion (1) step obtained adds in the solution that (2) step obtains by 1.6-1.8g/L, then adds other remaining component, mixes, and regulates pH=5, is heated to 80-82 DEG C, aluminium section bar is flooded 20-30min, to obtain final product.
Advantage of the present invention is: the present invention uses tetrabutyl titanate to form nano titanium oxide, employ lithium silicate, ten difluoro heptyl propyl trimethoxy silicanes, fluorochemical surfactant simultaneously, through reaction, the perviousness of hole sealing agent, cohesiveness, hydrophobicity can be improved, improve sealing of hole effect, improve the oxidation-resistance of oxide film and anti-SO simultaneously
4 2-interference; By using LiF, sulphosalicylic acid, zinc polysilicate, 2-mercaptobenzimidazole rare earth compounding, strong to the avidity of aluminium alloy, can pore interior be infiltrated into, closure is good, and the oxide film surface-brightening after sealing of hole can be made, planeness is good, and corrosion-resistant, didirtresistance improves greatly.
Embodiment
A kind of bright smooth aluminium alloy anode oxide film, without nickel hole sealing agent, is made up of the raw material of following weight part (kilogram): magnesium acetate 8, trolamine 19, ammonium acetate 3, deionized water are appropriate, LiF1.1, sulphosalicylic acid 0.4, zinc polysilicate 0.4,2 mercaptobenzimidazole rare earth compounding 0.4, lithium silicate 0.4, ten difluoro heptyl propyl trimethoxy silicane 2.6, tetrabutyl titanate 1, ethanol 45, ammoniacal liquor 8.6, fluorochemical surfactant 0.3.
The smooth aluminium alloy anode oxide film of described light, without the preparation method of nickel hole sealing agent, comprises the following steps:
(1) by tetrabutyl titanate, ethanol mixing, stirring obtains tetrabutyl titanate ethanolic soln, by lithium silicate, ten difluoro heptyl propyl trimethoxy silicanes, fluorochemical surfactant, 2 mercaptobenzimidazole rare earth compounding mixing, the water adding 5 weight parts stirs, obtain solution, to instill in tetrabutyl titanate ethanolic soln under described solution stirring, 1.5h is stirred under 250r/min condition, obtain mixture, then ammoniacal liquor is slowly dripped in people's said mixture, at 30 DEG C, obtain emulsion after stirring reaction 3h;
(2) mixing solutions is prepared, magnesium acetate 8g/L, trolamine 19g/L, ammonium acetate 3g/L;
(3) emulsion (1) step obtained adds in the solution that (2) step obtains by 1.6g/L, then adds other remaining component, mixes, and regulates pH=5, is heated to 80 DEG C, aluminium section bar is flooded 20min, to obtain final product.
Experimental data:
Detect according to GB/T8753.2-2005, sealing of hole weightlessness is 10.5mg/dm
2; According to GB/T8753.4-2005, dyeing grade is 0, and anti-dye high adsorption capacity, illustrates that seal quality is qualified.
Studied by anti-ion interference, even if when result display Na+ content increases to 400mg/L, sealing of hole weightlessness is also only 11.8mg/dm
2, be less than 30mg/dm
2, sealing quality is good, anti-Na
+interference performance is given prominence to; Work as SO
4 2-content when being 500mg/L, sealing of hole weightlessness is 13.2mg/dm
2, be less than 30mg/dm
2, sealing of hole effect is better, anti-SO
4 2-disturb.
By carrying out electron-microscope scanning to oxide film surface, see that a large amount of micropores on the surface of oxide film are nearly all closed, pore space structure is few, and sealing of hole is comparatively even.
Claims (2)
1. the smooth aluminium alloy anode oxide film of light is without a nickel hole sealing agent, it is characterized in that being made up of the raw material of following weight part: magnesium acetate 8-8.5, trolamine 19-20, ammonium acetate 3-3.2, deionized water are appropriate, LiF1.1-1.2, sulphosalicylic acid 0.4-0.5, zinc polysilicate 0.4-0.5,2-mercaptobenzimidazole rare earth compounding 0.4-0.5, lithium silicate 0.4-0.5, ten difluoro heptyl propyl trimethoxy silicane 2.6-2.8, tetrabutyl titanate 1-1.2, ethanol 45-48, ammoniacal liquor 8.6-9, fluorochemical surfactant 0.3-0.4.
2. the smooth aluminium alloy anode oxide film of light according to claim 1 is without the preparation method of nickel hole sealing agent, it is characterized in that comprising the following steps:
(1) by tetrabutyl titanate, ethanol mixing, stirring obtains tetrabutyl titanate ethanolic soln, by lithium silicate, ten difluoro heptyl propyl trimethoxy silicanes, fluorochemical surfactant, the mixing of 2-mercaptobenzimidazole rare earth compounding, the water adding 5-6 weight part stirs, obtain solution, to instill in tetrabutyl titanate ethanolic soln under described solution stirring, 1.5-1.8h is stirred under 250-300r/min condition, obtain mixture, then ammoniacal liquor is slowly dripped in people's said mixture, at 30-35 DEG C, obtain emulsion after stirring reaction 3-3.5h;
(2) mixing solutions is prepared, magnesium acetate 8g/L, trolamine 19g/L, ammonium acetate 3g/L;
(3) emulsion (1) step obtained adds in the solution that (2) step obtains by 1.6-1.8g/L, then adds other remaining component, mixes, and regulates pH=5, is heated to 80-82 DEG C, aluminium section bar is flooded 20-30min, to obtain final product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510614452.3A CN105200493A (en) | 2015-09-24 | 2015-09-24 | Nickel-free hole sealing agent for bright and smooth aluminum alloy anode oxide film and preparation method of nickel-free hole sealing agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510614452.3A CN105200493A (en) | 2015-09-24 | 2015-09-24 | Nickel-free hole sealing agent for bright and smooth aluminum alloy anode oxide film and preparation method of nickel-free hole sealing agent |
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| CN105200493A true CN105200493A (en) | 2015-12-30 |
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ID=54948441
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107805837A (en) * | 2017-09-05 | 2018-03-16 | 江苏飞拓界面工程科技有限公司 | A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent and its hole-sealing technology |
| CN108441923A (en) * | 2018-03-23 | 2018-08-24 | 长沙小新新能源科技有限公司 | A kind of hole-sealing technology of magnesium alloy |
| JP2020503460A (en) * | 2017-01-13 | 2020-01-30 | マクダーミッド アキューメン インコーポレーテッド | Sealing anodized aluminum using a low temperature nickel-free process |
| CN115537891A (en) * | 2022-10-09 | 2022-12-30 | 广东华昌集团有限公司 | Medium-temperature nickel-free sealing agent for aluminum and aluminum alloy anodic oxide film and sealing process |
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