CN107805837A - A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent and its hole-sealing technology - Google Patents
A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent and its hole-sealing technology Download PDFInfo
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- CN107805837A CN107805837A CN201710792113.3A CN201710792113A CN107805837A CN 107805837 A CN107805837 A CN 107805837A CN 201710792113 A CN201710792113 A CN 201710792113A CN 107805837 A CN107805837 A CN 107805837A
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- 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 provides a kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, on the basis of its gross weight, including following components in percentage by weight:Magnesium acetate 3 15%, cobalt acetate 0 10%, tripropylene glycol methyl ether 5 15%, surfactant 5 15%, press down grey agent 0 10%, accelerator 0 8%, pH buffer 0.5 10%, corrosion inhibiter 0 10%, surplus is deionized water.The hole sealing agent stability and osmotic effect of the present invention is good, and sealing of hole film is fine and close, can completely enclose the space of workpiece surface, sealing of hole condition requires low, and workpiece surface smooth after sealing of hole, non-discolouring, powder, oil rub resistance and impression of the hand are not played, improves the intensity, hardness and corrosion resistance of workpiece;The element such as not nickeliferous, fluorine and chromium, safety and environmental protection is pollution-free to operating environment, will not insulting health;Cost is low, and energy consumption is small, suitable for industrializing large-scale production.
Description
Technical field
The invention belongs to corrosion protection of metal surface processing technology field, and in particular to a kind of aluminium and aluminium alloy environmental protection normal temperature
Hole sealing agent and its hole-sealing technology.
Background technology
Aluminium alloy has the advantages that light weight, corrosion resistance are strong, thermal conductivity is good, in Aeronautics and Astronautics, automobile, machinery system
Make, extensive use in civilian industry.Al-alloy products have individual shortcoming --- easily it are corroded, to avoid the corrosion of aluminium section bar, table
Face is handled typically based on anodic oxidation, can significantly improve the corrosion resisting property of aluminium and alloy, improves aluminium and its alloy surface
Hardness, wear resisting and corrosion resistance energy.But oxidation film layer is made up of the unformed aluminum oxide in a large amount of spaces, and hole generally extends to oxide
Near the interface of metal, the region around a hole forms a structure cell, has stronger chemism.In anodization
In journey barrier layer formation and dissolving occur simultaneously, and keep certain thickness constant, with the progress of oxidizing process, the depth in hole
Increase, so need to carry out sealing of hole surface treatment.
The country has carried out the research of many no nickel hole sealing agents at present, for example Chinese patent CN103614757A is disclosed
A kind of enclosure method of aluminum alloy surface perforated membrane rare earth, nitric acid rare earth salt and lithium salts are subjected to sealing of hole, sealing of hole temperature as main salt
Degree highest needs to reach 120 DEG C, and the sealing of hole time is most long to need 3h;Chinese patent CN101864589A discloses a kind of aluminium alloy sun
Pole aoxidizes practical no nickel hole sealing agent, and it carries out sealing of hole from organic compound, not metalline, sealing of hole temperature minimum 80
DEG C, the sealing of hole time is 20min or so;Chinese patent CN101323965A discloses aluminium alloy anode oxide film alkali metal salt, alkali
Earth metal salt enclosure method, under conditions of 75-90 DEG C, make the confining liquid of the main salt in position, sealing of hole with alkali metal salt, alkali salt
Time is more than 20-30min.The sealing of hole condition of these patents is all more harsh, and energy consumption is higher, tank liquor less stable, sealing of hole effect
Fruit is extremely difficult to industrial requirement.
With the development of industrialized production, the development of aluminium and oxidized aluminum alloy membrane technology, sealing quality it is also proposed
Higher requirement, shown according to the investigation in industrial processes, at present in industrial production without sealing of hole being present in nickel hole sealing technology
Film loss of gloss, gloss retention are poor;Aluminium workpiece surface out-of-flatness after sealing of hole, easily turn white, play powder;Sealing of hole speed is slow, detection sealing of hole is weightless
It is high;The problems such as energy-saving effect is poor, and bath life is short.
The content of the invention
The technical problems to be solved by the invention are to provide one kind can effectively closed work piece surface pore, and workpiece after sealing of hole
Surfacing aluminium that is bright, non-discolouring, not playing powder and aluminium alloy environmental protection normal-temperature hole sealing agent and its hole-sealing technology.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, on the basis of its gross weight, including following components in percentage by weight:Second
Sour magnesium 3-15%, cobalt acetate 0-10%, tripropylene glycol methyl ether 5-15%, surfactant 5-15%, press down grey agent 0-10%, accelerator 0-
8%, pH buffer 0.5-10%, corrosion inhibiter 0-10%, surplus are deionized water.
As preferable, above-mentioned surfactant is PVP, fatty acid methyl ester, aliphatic alcohol polyethenoxy
One in ether, cetyl sulfophenoxy benzene sulfonic acid disodium, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate, cetyl benzenesulfonic acid sodium
Kind is a variety of, can reduce the surface tension of system, improves wetting permeability energy, plays excellent emulsifiability, assurance function
Material is sufficiently contacted with oxide layer, gos deep into inside oxide layer micropore playing sealing of hole effect, energy of adsorption in aqueous
Power meets the requirement for promoting sealing of hole.
As preferable, above-mentioned suppression ash agent is 5- (2- aminoethyls ammonia) -1-naphthalene sulfonic aicd sodium, sodium methylene bis-naphthalene sulfonate, poly-
One or more in naphthalene formaldehyde sulfonate salt, thiocarbamide, polyethylene glycol, hydroxy alkyl phenol polyethenoxy ether, have and preferably divide
Performance is dissipated, prevents from excessively assembling between functional mass, keeps the stabilization of sealing of hole liquid system, effectively suppresses the production of pollen, lime
It is raw.
As preferable, above-mentioned accelerator is aliphatic derivatives, and molecular structural formula is:
,
Wherein, R1、R2For hydrogen atom, methyl, methylol or ethoxy, R3、R4And R5For hydroxyl, amino, methyl, methylol, hydroxyl
Ethyl or hydroxypropyl, n=1-3.
As preferable, above-mentioned pH buffer be acetic acid, citric acid, sodium citrate, tartaric acid, sodium potassium tartrate tetrahydrate, ammoniacal liquor,
One or more in dibastic sodium phosphate, sodium dihydrogen phosphate, phosphoric acid;The corrosion inhibiter is sodium tripolyphosphate, calgon, boron
One or more in acid, DC11, decanedioic acid, diethanol amine, triethanolamine, workpiece is black after effectively preventing sealing of hole
Change, grey change, the generation of white hair, loss of gloss, eclipsed bad phenomenon, it is ensured that glossiness, make surface more fine and close, fine and smooth.
The hole-sealing technology of above-mentioned aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, comprises the following steps:
(1)Anodic oxidation will be carried out after aluminum workpiece pre-treatment, forms the oxidation film layer of 10-15 μ m-thicks;
(2)Aluminum workpiece with oxidation film layer is impregnated in hole sealing agent, dip time 5-15min, the temperature of hole sealing agent
Spend for 20-35 DEG C, pH value 5.5-6.5;
(3)Aluminum workpiece is taken out, soaks 15-20min in 55-65 DEG C of water after cleaning, is air-dried, packaging.
As preferable, the temperature of above-mentioned hole sealing agent is 27-29 DEG C.
As preferable, above-mentioned steps(2)In dip time be 8-12min.
The beneficial effects of the invention are as follows:The hole sealing agent stability and osmotic effect of the present invention is good, and sealing of hole film is fine and close, can be complete
The space of totally-enclosed workpiece surface, sealing of hole condition requires low, and workpiece surface smooth after sealing of hole, non-discolouring, does not play powder, resists
Greasy dirt and impression of the hand, improve the intensity, hardness and corrosion resistance of workpiece;The element such as not nickeliferous, fluorine and chromium, safety and environmental protection, to behaviour
Make environmental nonpollution, will not insulting health;Cost is low, and energy consumption is small, suitable for industrializing large-scale production.
Embodiment:
The present invention is described in further details with reference to embodiments, but these embodiments are not limitation of the invention.
Embodiment 1
A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, on the basis of its gross weight, including following components in percentage by weight:Second
Sour magnesium 5%, cobalt acetate 0.5%, tripropylene glycol methyl ether 5%, PVP 8%, fatty acid methyl ester 3%, hydroxy alkyl phenol gather
Oxygen vinethene 4%, accelerator 1%, sodium citrate 2%, boric acid 2%, surplus are deionized water.Wherein, accelerator derives for aliphatic
Thing, the R in its molecular structural formula1For ethoxy, R2For ethoxy, R3For amino, R4For methyl, R5For methyl, n=1.
The hole-sealing technology of above-mentioned aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, comprises the following steps:
(1)Anodic oxidation will be carried out after aluminum workpiece pre-treatment, forms the oxidation film layer of 10 μ m-thicks;
(2)Aluminum workpiece with oxidation film layer is impregnated in hole sealing agent, dip time 8min, the temperature of hole sealing agent is
28 DEG C, pH value 5.8;
(3)Aluminum workpiece is taken out, soaks 15min in 55 DEG C of water after cleaning, is air-dried, packaging.
Aluminum workpiece surface to be visually inspected, aluminum workpiece surface-brightening after sealing of hole, color and luster is good, water stain-free,
Macula lutea and pollen;Electron-microscope scanning is carried out, the micropore on oxide-film surface almost completely encloses, and surfacing.
By national standard(The phosphorus chromic acid method of GB/T8753.2-2005 nitric acid preimpregnation)Aluminum workpiece is detected, sealed
Hole weightlessness is 13.1mg/dm2。
By national standard(Dye speck method after GB/T8753.4-2005 acid treatments)Aluminum workpiece is dyed,
It is 0 grade to dye grade, and anti-dye adsorption capacity is strong, shows that seal quality is qualified, contamination resistance is strong.
Embodiment 2
A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, on the basis of its gross weight, including following components in percentage by weight:Second
Sour magnesium 8%, cobalt acetate 1%, tripropylene glycol methyl ether 8%, AEO 10%, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate 3%,
Accelerator 1%, tartaric acid 2%, sodium tripolyphosphate 2%, surplus are deionized water.Wherein, accelerator is aliphatic derivatives, its point
R in subformula1For ethoxy, R2For ethoxy, R3For amino, R4For methyl, R5For methyl, n=1.
The hole-sealing technology of above-mentioned aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, comprises the following steps:
(1)Anodic oxidation will be carried out after aluminum workpiece pre-treatment, forms the oxidation film layer of 10 μ m-thicks;
(2)Aluminum workpiece with oxidation film layer is impregnated in hole sealing agent, dip time 10min, the temperature of hole sealing agent
For 27 DEG C, pH value 6.3;
(3)Aluminum workpiece is taken out, soaks 16min in 60 DEG C of water after cleaning, is air-dried, packaging.
Aluminum workpiece surface to be visually inspected, aluminum workpiece surface-brightening after sealing of hole, color and luster is good, water stain-free,
Macula lutea and pollen;Electron-microscope scanning is carried out, the micropore on oxide-film surface almost completely encloses, and surfacing.
By national standard(The phosphorus chromic acid method of GB/T8753.2-2005 nitric acid preimpregnation)Aluminum workpiece is detected, sealed
Hole weightlessness is 10.1mg/dm2。
By national standard(Dye speck method after GB/T8753.4-2005 acid treatments)Aluminum workpiece is dyed,
It is 0 grade to dye grade, and anti-dye adsorption capacity is strong, shows that seal quality is qualified, contamination resistance is strong.
Embodiment 3
A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, on the basis of its gross weight, including following components in percentage by weight:Second
Sour magnesium 10%, cobalt acetate 1.5%, tripropylene glycol methyl ether 8%, cetyl benzenesulfonic acid sodium 5%, fatty acid methyl ester 3%, hydroxy alkyl phenol
APEO 7%, thiocarbamide 1%, polyethylene glycol 2%, acetic acid 2%, calgon 2%, surplus are deionized water.Wherein, accelerator
For aliphatic derivatives, the R in its molecular structural formula1For hydrogen atom, R2For methyl, R3For hydroxyl, R4For methyl, R5For amino, n
=2。
The hole-sealing technology of above-mentioned aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, comprises the following steps:
(1)Anodic oxidation will be carried out after aluminum workpiece pre-treatment, forms the oxidation film layer of 12 μ m-thicks;
(2)Aluminum workpiece with oxidation film layer is impregnated in hole sealing agent, dip time 10min, the temperature of hole sealing agent
For 28 DEG C, pH value 6;
(3)Aluminum workpiece is taken out, soaks 15min in 60 DEG C of water after cleaning, is air-dried, packaging.
Aluminum workpiece surface to be visually inspected, aluminum workpiece surface-brightening after sealing of hole, color and luster is good, water stain-free,
Macula lutea and pollen;Electron-microscope scanning is carried out, the micropore on oxide-film surface almost completely encloses, and surfacing.
By national standard(The phosphorus chromic acid method of GB/T8753.2-2005 nitric acid preimpregnation)Aluminum workpiece is detected, sealed
Hole weightlessness is 15.2mg/dm2。
By national standard(Dye speck method after GB/T8753.4-2005 acid treatments)Aluminum workpiece is dyed,
It is 1 grade to dye grade, and anti-dye adsorption capacity is stronger, shows that seal quality is qualified, contamination resistance is stronger.
Embodiment 4
A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, on the basis of its gross weight, including following components in percentage by weight:Second
Sour magnesium 12%, tripropylene glycol methyl ether 8%, fatty acid methyl ester 5%, AEO 4%, sodium methylene bis-naphthalene sulfonate 4%, promote
Enter agent 3%, citric acid 2%, DC11 2%, triethanolamine 1.5%, surplus is deionized water.Wherein, accelerator is fat
Race's derivative, the R in its molecular structural formula1For ethoxy, R2For ethoxy, R3For methylol, R4For methyl, R5For hydroxyl, n=
2。
The hole-sealing technology of above-mentioned aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, comprises the following steps:
(1)Anodic oxidation will be carried out after aluminum workpiece pre-treatment, forms the oxidation film layer of 12 μ m-thicks;
(2)Aluminum workpiece with oxidation film layer is impregnated in hole sealing agent, dip time 12min, the temperature of hole sealing agent
For 29 DEG C, pH value 6;
(3)Aluminum workpiece is taken out, soaks 15min in 60 DEG C of water after cleaning, is air-dried, packaging.
Aluminum workpiece surface to be visually inspected, aluminum workpiece surface-brightening after sealing of hole, color and luster is good, water stain-free,
Macula lutea and pollen;Electron-microscope scanning is carried out, the micropore on oxide-film surface almost completely encloses, and surfacing.
By national standard(The phosphorus chromic acid method of GB/T8753.2-2005 nitric acid preimpregnation)Aluminum workpiece is detected, sealed
Hole weightlessness is 9.5mg/dm2。
By national standard(Dye speck method after GB/T8753.4-2005 acid treatments)Aluminum workpiece is dyed,
It is 0 grade to dye grade, and anti-dye adsorption capacity is strong, shows that seal quality is qualified, contamination resistance is strong.
Embodiment 5
A kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, on the basis of its gross weight, including following components in percentage by weight:Second
Sour magnesium 15%, cobalt acetate 3%, tripropylene glycol methyl ether 10%, PVP 10%, 5- (2- aminoethyls ammonia) -1-naphthalene sulfonic aicd
Sodium 6%, accelerator 3%, tartaric acid 3%, ammoniacal liquor 0.5%, DC11 2%, triethanolamine 1.5%, surplus are deionized water.Its
In, accelerator is aliphatic derivatives, the R in its molecular structural formula1For ethoxy, R2For ethoxy, R3For methylol, R4For
Methyl, R5For hydroxyl, n=3.
The hole-sealing technology of above-mentioned aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, comprises the following steps:
(1)Anodic oxidation will be carried out after aluminum workpiece pre-treatment, forms the oxidation film layer of 15 μ m-thicks;
(2)Aluminum workpiece with oxidation film layer is impregnated in hole sealing agent, dip time 15min, the temperature of hole sealing agent
For 35 DEG C, pH value 6.5;
(3)Aluminum workpiece is taken out, soaks 20min in 65 DEG C of water after cleaning, is air-dried, packaging.
Aluminum workpiece surface to be visually inspected, aluminum workpiece surface-brightening after sealing of hole, color and luster is good, water stain-free,
Macula lutea and pollen;Electron-microscope scanning is carried out, the micropore on oxide-film surface almost completely encloses, and surfacing.
By national standard(The phosphorus chromic acid method of GB/T8753.2-2005 nitric acid preimpregnation)Aluminum workpiece is detected, sealed
Hole weightlessness is 16.7mg/dm2。
By national standard(Dye speck method after GB/T8753.4-2005 acid treatments)Aluminum workpiece is dyed,
It is 1 grade to dye grade, and anti-dye adsorption capacity is stronger, shows that seal quality is qualified, contamination resistance is stronger.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, although with reference to foregoing reality
Apply example the present invention is described in detail, for those skilled in the art, it still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic.All essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (8)
1. a kind of aluminium and aluminium alloy environmental protection normal-temperature hole sealing agent, it is characterised in that on the basis of its gross weight, including following weight hundred
Divide the component of ratio:Magnesium acetate 3-15%, cobalt acetate 0-10%, tripropylene glycol methyl ether 5-15%, surfactant 5-15%, press down grey agent 0-
10%, accelerator 0-8%, pH buffer 0.5-10%, corrosion inhibiter 0-10%, surplus are deionized water.
2. aluminium according to claim 1 and aluminium alloy environmental protection normal-temperature hole sealing agent, it is characterised in that the surfactant is
PVP, fatty acid methyl ester, AEO, cetyl sulfophenoxy benzene sulfonic acid disodium, ten
One or more in dialkyl diphenyl ether sodium disulfonate, cetyl benzenesulfonic acid sodium.
3. aluminium according to claim 1 and aluminium alloy environmental protection normal-temperature hole sealing agent, it is characterised in that the grey agent of suppression is 5-
(2- aminoethyls ammonia) -1-naphthalene sulfonic aicd sodium, sodium methylene bis-naphthalene sulfonate, poly- naphthalene formaldehyde sulfonate salt, thiocarbamide, polyethylene glycol, hydroxyl
One or more in APES.
4. aluminium according to claim 1 and aluminium alloy environmental protection normal-temperature hole sealing agent, it is characterised in that the accelerator is fat
Race's derivative, molecular structural formula are:
,
Wherein, R1、R2For hydrogen atom, methyl, methylol or ethoxy, R3、R4And R5For hydroxyl, amino, methyl, methylol, hydroxyl
Ethyl or hydroxypropyl, n=1-3.
5. aluminium according to claim 1 and aluminium alloy environmental protection normal-temperature hole sealing agent, it is characterised in that the pH buffer is second
One kind in acid, citric acid, sodium citrate, tartaric acid, sodium potassium tartrate tetrahydrate, ammoniacal liquor, dibastic sodium phosphate, sodium dihydrogen phosphate, phosphoric acid or
It is a variety of;The corrosion inhibiter is sodium tripolyphosphate, calgon, boric acid, DC11, decanedioic acid, diethanol amine, three second
One or more in hydramine.
6. aluminium according to any one of claim 1 to 5 and the hole-sealing technology of aluminium alloy environmental protection normal-temperature hole sealing agent, its feature
It is, comprises the following steps:
(1)Anodic oxidation will be carried out after aluminum workpiece pre-treatment, forms the oxidation film layer of 10-15 μ m-thicks;
(2)Aluminum workpiece with oxidation film layer is impregnated in hole sealing agent, dip time 5-15min, the temperature of hole sealing agent
Spend for 20-35 DEG C, pH value 5.5-6.5;
(3)Aluminum workpiece is taken out, soaks 15-20min in 55-65 DEG C of water after cleaning, is air-dried, packaging.
7. hole-sealing technology according to claim 6, it is characterised in that the temperature of the hole sealing agent is 27-29 DEG C.
8. hole-sealing technology according to claim 6, it is characterised in that the step(2)In dip time be 8-
12min。
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Cited By (8)
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CN108950645A (en) * | 2018-09-28 | 2018-12-07 | 上海铝通化学科技有限公司 | A kind of aluminium and aluminium alloy anode oxide are without nickel sealer |
CN109056028A (en) * | 2018-07-20 | 2018-12-21 | 江苏飞拓界面工程科技有限公司 | A kind of aluminium and aluminium alloy anode oxide aftertreatment fluid and preparation method thereof |
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CN109056028B (en) * | 2018-07-20 | 2021-04-06 | 江苏飞拓界面工程科技有限公司 | Aluminum and aluminum alloy anodic oxidation post-treatment fluid and preparation method thereof |
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CN109440163A (en) * | 2018-12-28 | 2019-03-08 | 江苏飞拓界面工程科技有限公司 | A kind of aluminium and aluminium alloy anode oxide film are without nickel hole sealing agent and its application |
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CN109913926A (en) * | 2019-04-17 | 2019-06-21 | 安徽华淮新材料有限公司 | Aluminium alloy anode oxide film hole sealing agent and its method for sealing |
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 |
CN112877744A (en) * | 2020-12-31 | 2021-06-01 | 广东和胜工业铝材股份有限公司 | Hole sealing liquid, preparation method and application |
CN113279035A (en) * | 2021-05-15 | 2021-08-20 | 江门市优博科技有限公司 | Novel sealing agent for aluminum and aluminum alloy anodic oxide film and preparation method thereof |
CN114717630A (en) * | 2022-03-18 | 2022-07-08 | 江门市优博科技有限公司 | Novel environment-friendly sealing agent for aluminum and aluminum alloy anodic oxide film and preparation method thereof |
CN114717630B (en) * | 2022-03-18 | 2024-05-10 | 江门市优博科技有限公司 | Environment-friendly sealing agent for aluminum and aluminum alloy anodic oxide film and preparation method thereof |
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