CN107829081A - A kind of special passivation film agent of aluminum products and preparation method thereof - Google Patents
A kind of special passivation film agent of aluminum products and preparation method thereof Download PDFInfo
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- CN107829081A CN107829081A CN201711085272.6A CN201711085272A CN107829081A CN 107829081 A CN107829081 A CN 107829081A CN 201711085272 A CN201711085272 A CN 201711085272A CN 107829081 A CN107829081 A CN 107829081A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/34—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing fluorides or complex fluorides
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
The present invention relates to special passivation film agent of a kind of aluminum products and preparation method thereof, this kind of film agent, count in parts by weight, its raw material includes, 10 20 parts of fluorine zirconic acid, 6 12 parts of phytate, 24 parts of high-molecular compound, 10 20 parts of water-soluble resin, 46 parts of silane coupler, 46 parts of titanium dioxide, 12 14 parts of chelating agent；The high-molecular compound is the glycol of 2,3,5,6 tetramethyl, 1,4 dioxane 2,5, polyvinyl alcohol, the mixture of polyethylene glycol.This kind of film agent is a kind of nontoxic water base processing product, and one layer of fine and close epithelium can be quickly formed in aluminium and its alloy surface by way of spraying or soaking, and has good oxidation-protective effect, increases the adhesive force and corrosion resistance of coating and matrix.
Description
Technical field
The present invention relates to field of metal surface treatment technology, and in particular, it is related to a kind of special passivation skin of aluminum products
Film and preparation method thereof.
Background technology
Film agent is a kind of metal conditioner, and it can react with metal, is removing the same of metal surface corrosion
When, form a kind of not soluble in water, chemical inertness, be firmly attached to the diaphragm of metal surface, this diaphragm is advantageous to prevent
Metal aoxidizes, and is also advantageously used in follow-up metal surface spraying process, makes the combination of the paint film of spraying, molding powder and metal
Power, Adhesion enhancement.
Traditional film agent is mainly passivated processing to metal surface using chromate, because chromaking has stability
By force, water quality is not selected, technology maturation, the advantages that cost is cheap, therefore chromaking product is in occupation of the market of aluminium product more than 90%.
But in traditional chromate processing procedure, the toxicity for the treatment of fluid is larger, and environmental pollution is serious, particularly Cr VI have compared with
Strong toxicity, may cause allergic, cause the infringement of inherited genetic, and suction is also possible to carcinogenic, is generally acknowledged at present lead
Cause the inducement of lung cancer.
The content of the invention
It is an object of the invention to provide special passivation film agent of a kind of aluminum products and preparation method thereof, this kind of aluminum products are special
It is a kind of nontoxic water base processing product with passivation film agent, can be in aluminium and its alloy by way of spraying or soaking
Surface quickly forms one layer of fine and close epithelium, has a good oxidation-protective effect, increases the adhesive force of coating and matrix and anti-corrosion
Property.
The present invention above-mentioned purpose technical scheme is that：A kind of film agent, is counted in parts by weight,
Its raw material includes, fluorine zirconic acid 10-20 parts, phytate 6-12 parts, high-molecular compound 2-4 parts, water-soluble resin 10-20 parts, silicon
Alkane coupling agent 4-6 parts, titanium dioxide 4-6 parts, chelating agent 12-14 parts；
The high-molecular compound is 2,3,5,6- tetramethyl -1,4- dioxane -2,5- glycol, polyvinyl alcohol, polyethylene glycol
Mixture.
Preferably, described 2,3,5,6- tetramethyls-Isosorbide-5-Nitrae-dioxane -2,5- glycol, polyvinyl alcohol, the matter of polyethylene glycol
Amount is than being 2:1:1.
Preferably, the chelating agent is ethylenediamine tetra-acetic acid or sodium ethylene diamine tetracetate.
Preferably, the water-soluble resin is epoxy resin or acrylic resin.
Preferably, the silane coupler is vinyltrimethoxy silane or 3- aminopropyl trimethoxy silicon.
Preferably, the phytate is sodium phytate or POTASSIUM PHYTATE.
It is another object of the present invention to provide the preparation method of the special passivation film agent of aluminum products described above.
The present invention above-mentioned purpose technical scheme is that, a kind of special passivation film agent of aluminum products
Preparation method, including at least following steps：
S1：Fluorine zirconic acid, silane coupler, phytate is taken to add in pure water, after solid matter is completely dissolved, into mixed liquor
High-molecular compound is slowly added into, the addition time is 10-20min, and uniform stirring is until solid matter is completely dissolved；
S2：Water-soluble resin is added in the mixed liquor that S1 is obtained, and uniform stirring 20-30min is until solid matter is completely dissolved；
S3：Titanium dioxide, chelating agent is taken to add in the mixed liquor that S2 is obtained, uniform stirring 20-30min, until solid matter is complete
Fully dissolved, the special passivation film agent of aluminum products is prepared.
Preferably, in the step S1, system temperature is 42-46 DEG C.
Preferably, in the step S2, system temperature is 51-59 DEG C.
Preferably, in the step S3, system temperature is 31-37 DEG C.
In summary, the invention has the advantages that：
1st, the special passivation film agent of aluminum products that the present invention is prepared is free of chromium ion, is a kind of nontoxic water base processing
Product, one layer of fine and close epithelium can be quickly formed in aluminium and its alloy surface by way of spraying or soaking, had good
Oxidation-protective effect, increase the adhesive force and corrosion resistance of coating and matrix.
2nd, during the present invention prepares the special passivation film agent of aluminum products, fluorine zirconic acid provides acidity for film agent, simultaneously
The zirconium oxide gel as film forming matter can be produced after being hydrolyzed under certain pH value；Phytate have it is stronger sequestering and into
Film concertedness；Water-soluble resin can make film forming high resilience to film forming, to prevent the process of creep；Silane is even
Join agent to improve the adhesive ability of product.
3rd, during the present invention prepares the special passivation film agent of aluminum products, using the hydroxyl in high-molecular compound and
Long chain organically combines silane hydrolysates and zirconium oxide gel, it is quickly closely incorporated into metal surface, increases
Add the compactness of epithelium, improve the oxidation-protective effect of aluminium and its product.
Brief description of the drawings
Fig. 1 is the crystalline state schematic diagram of the special passivation epithelium of aluminum products.
Embodiment
Involved all substances are commercially available in the embodiment of the present invention.
First, embodiment is made
Embodiment 1
S1：Take fluorine zirconic acid 15kg, vinyltrimethoxy silane 5kg, sodium phytate 9kg to add in pure water 200kg, treat solids
After matter is completely dissolved, 2 are slowly added into mixed liquor, 3,5,6- tetramethyls-Isosorbide-5-Nitrae-dioxane -2,5- glycol 1.5kg, poly- second
Enol 0.75kg, polyethylene glycol 0.75kg, addition time are 15min, and uniform stirring is completely dissolved up to solid matter, wherein,
System temperature is 44 DEG C；
S2：Extracting epoxy resin 15kg is added in the mixed liquor that S1 is obtained, and uniform stirring 25min is completely dissolved up to solid matter,
Wherein, system temperature is 55 DEG C；
S3：Titanium dioxide 5kg, ethylenediamine tetra-acetic acid 13kg is taken to add in the mixed liquor that S2 is obtained, uniform stirring 25min, until
Solid matter is completely dissolved, and the special passivation film agent of aluminum products is prepared, wherein, system temperature is 34 DEG C.
Embodiment 2
S1：Take fluorine zirconic acid 10kg, 3- aminopropyl trimethoxy silicon 4kg, POTASSIUM PHYTATE 6kg to add in pure water 200kg, treat solid
After material is completely dissolved, 2 are slowly added into mixed liquor, 3,5,6- tetramethyls-Isosorbide-5-Nitrae-dioxane -2,5- glycol 2kg, poly- second
Enol 1kg, polyethylene glycol 0.5kg, addition time are 15min, and uniform stirring is completely dissolved up to solid matter, wherein, system
Temperature is 46 DEG C；
S2：Acrylic resin 10kg is taken to add in the mixed liquor that S1 is obtained, uniform stirring 20min is until solid matter is completely molten
Solution, wherein, system temperature is 51 DEG C；
S3：Titanium dioxide 4kg, sodium ethylene diamine tetracetate 14kg is taken to add in the mixed liquor that S2 is obtained, uniform stirring 30min, directly
It is completely dissolved to solid matter, the special passivation film agent of aluminum products is prepared, wherein, system temperature is 31 DEG C.
Embodiment 3
S1：Take fluorine zirconic acid 20kg, vinyltrimethoxy silane 4kg, POTASSIUM PHYTATE 6kg to add in pure water 200kg, treat solids
After matter is completely dissolved, 2 are slowly added into mixed liquor, 3,5,6- tetramethyls-Isosorbide-5-Nitrae-dioxane -2,5- glycol 2kg, polyethylene
Alcohol 0.5kg, polyethylene glycol 1kg, addition time are 20min, and uniform stirring is completely dissolved up to solid matter, wherein, system temperature
Spend for 46 DEG C；S2：Extracting epoxy resin 10kg is added in the mixed liquor that S1 is obtained, and uniform stirring 30min is until solid matter is complete
Dissolving, wherein, system temperature is 51 DEG C；
S3：Titanium dioxide 4kg, sodium ethylene diamine tetracetate 14kg is taken to add in the mixed liquor that S2 is obtained, uniform stirring 20min, directly
It is completely dissolved to solid matter, the special passivation film agent of aluminum products is prepared, wherein, system temperature is 37 DEG C.
Embodiment 4
S1：Take fluorine zirconic acid 10kg, 3- aminopropyl trimethoxy silicon 4kg, sodium phytate 12kg to add in pure water 200kg, treat solid
After body material is completely dissolved, 2 are slowly added into mixed liquor, 3,5,6- tetramethyls-Isosorbide-5-Nitrae-dioxane -2,5- glycol 1kg, is gathered
Vinyl alcohol 0.75kg, polyethylene glycol 1kg, addition time are 10min, and uniform stirring is completely dissolved up to solid matter, wherein, body
It is that temperature is 44 DEG C；
S2：Acrylic resin 20kg is taken to add in the mixed liquor that S1 is obtained, uniform stirring 20min is until solid matter is completely molten
Solution, wherein, system temperature is 51 DEG C；
S3：Titanium dioxide 6kg, sodium ethylene diamine tetracetate 12kg is taken to add in the mixed liquor that S2 is obtained, uniform stirring 30min, directly
It is completely dissolved to solid matter, the special passivation film agent of aluminum products is prepared, wherein, system temperature is 34 DEG C.
Embodiment 5
S1：Take fluorine zirconic acid 20kg, vinyltrimethoxy silane 6kg, POTASSIUM PHYTATE 12kg to add in pure water 200kg, treat solid
After material is completely dissolved, 2 are slowly added into mixed liquor, 3,5,6- tetramethyls-Isosorbide-5-Nitrae-dioxane -2,5- glycol 1kg, poly- second
Enol 0.5kg, polyethylene glycol 0.5kg, addition time are 15min, and uniform stirring is completely dissolved up to solid matter, wherein, body
It is that temperature is 44 DEG C；
S2：Acrylic resin 20kg is taken to add in the mixed liquor that S1 is obtained, uniform stirring 30min is until solid matter is completely molten
Solution, wherein, system temperature is 59 DEG C；
S3：Titanium dioxide 6kg, ethylenediamine tetra-acetic acid 12kg is taken to add in the mixed liquor that S2 is obtained, uniform stirring 20min, until
Solid matter is completely dissolved, and the special passivation film agent of aluminum products is prepared, wherein, system temperature is 31 DEG C.
Embodiment 6
S1：Take fluorine zirconic acid 10kg, 3- aminopropyl trimethoxy silicon 6kg, sodium phytate 6kg to add in pure water 200kg, treat solid
After material is completely dissolved, 2 are slowly added into mixed liquor, 3,5,6- tetramethyls-Isosorbide-5-Nitrae-dioxane -2,5- glycol 1kg, poly- second
Enol 1kg, polyethylene glycol 1kg, addition time are 20min, and uniform stirring is completely dissolved up to solid matter, wherein, system temperature
Spend for 42 DEG C；
S2：Acrylic resin 20kg is taken to add in the mixed liquor that S1 is obtained, uniform stirring 20min is until solid matter is completely molten
Solution, wherein, system temperature is 59 DEG C；
S3：Titanium dioxide 4kg, sodium ethylene diamine tetracetate 12kg is taken to add in the mixed liquor that S2 is obtained, uniform stirring 30min, directly
It is completely dissolved to solid matter, the special passivation film agent of aluminum products is prepared, wherein, system temperature is 37 DEG C.
2nd, comparative example is made
Comparative example 1：Commercially available film agent containing chromium.
Comparative example 2：
S1：Fluorine zirconic acid 15kg, vinyltrimethoxy silane 5kg, sodium phytate 9kg is taken to add in pure water 200kg, uniform stirring
Until solid matter is completely dissolved, wherein, system temperature is 44 DEG C；
S2：Extracting epoxy resin 15kg is added in the mixed liquor that S1 is obtained, and uniform stirring 25min is completely dissolved up to solid matter,
Wherein, system temperature is 55 DEG C；
S3：Titanium dioxide 5kg, ethylenediamine tetra-acetic acid 13kg is taken to add in the mixed liquor that S2 is obtained, uniform stirring 25min, until
Solid matter is completely dissolved, and the special passivation film agent of aluminum products is prepared, wherein, system temperature is 34 DEG C.
Comparative example 3
Take fluorine zirconic acid 15kg, vinyltrimethoxy silane 5kg, sodium phytate 9kg, 2,3,5,6- tetramethyl -1,4- dioxanes -
2,5- glycol 1.5kg, polyvinyl alcohol 0.75kg, polyethylene glycol 0.75kg, epoxy resin 15kg, titanium dioxide 5kg, ethylenediamine tetraacetic
Acetic acid 13kg is added in pure water 200kg, and it is special blunt that aluminum products are prepared after solid matter is completely dissolved in uniform stirring
Change film agent, wherein, system temperature is 34 DEG C.
3rd, the performance of above example and the film agent of comparative example is tested.
Film agent in above-described embodiment and comparative example is added to the water, is configured to the treatment fluid that concentration is 3%, regulation
For the pH value for the treatment of fluid to 3, electrical conductivity is 1800 μ s/m.Control process liquid temperature degree is 25 DEG C, sprays the aluminium test specimen of surface degreasing
2min, after spray, aluminium surface of test piece forms skin membrane, after aluminium test specimen is positioned over 140 DEG C at a temperature of dry 20min.
After skin membrane drying, the corrosion resistance of epithelium is detected.The skin membrane of aluminium surface of test piece is painted afterwards, detects the resistance to of paint film
Corrosion and adhesive force.Wherein, spraying lacquer is varnish.
Epithelium neutral salt spray test, paint film neutral salt spray test：According in artificial atmosphere corrosion test in GB 10125
Salt spray test standard is tested.
Paint film adhesion grade:Tested according to the cross cut test standard of paint film in GB9286 paint and varnish.
Each evaluation index result is as shown in table 1.
The performance test results of the film agent of 1 each embodiment of table and comparative example
It is a kind of as can be seen that the special passivation film agent of aluminum products that the present invention is prepared is free of chromium ion from above-mentioned table
Nontoxic water base processing product, one layer of cause can be quickly formed in aluminium and its alloy surface by way of spraying or soaking
Close epithelium, there is good oxidation-protective effect, increase the adhesive force and corrosion resistance of coating and matrix.
Wherein, treatment fluid uses commercially available film agent containing chromium in comparative example 1, although film agent containing chromium can be in aluminium surface of test piece
One layer of anti-oxidation skin membrane is formed, but the content of chromium ion in treatment fluid is larger, it is serious to pollute environment and underground water, give up
Liquid processing is more difficult.
2,3,5,6- tetramethyl -1,4- dioxane -2,5- glycol, polyvinyl alcohol and poly- second are added without in comparative example 2
Glycol, because the binding ability of hydroxyl is stronger, during the special passivation film agent of aluminum products is prepared, do not have in reaction system
Hydroxyl and long chain combine silane hydrolysates and zirconium oxide gel, it is impossible to make skin membrane quickly close
Ground is incorporated into metal surface, meanwhile, the compactness of skin membrane reduces, and the decay resistance of aluminium test specimen weakens.Meanwhile the table of matrix
The group in face is reduced, and the adhesive ability of its paint film also decreases.
Reaction raw materials mixed once is prepared film agent in comparative example 3, the group in raw material can not be combined fully, fluorine
The zirconium oxide gel of zirconic acid hydrolysis generation is reunited first, is treated to aluminium surface of test piece in journey, is caused to generate
Skin membrane is not fine and close, and its corrosion resistance is less than the film agent that embodiment 1 is prepared.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
Member can make the modification of no creative contribution to the present embodiment as needed after this specification is read, but as long as at this
All protected in the right of invention by Patent Law.
Claims (10)
1. a kind of special passivation film agent of aluminum products, it is characterized in that, count in parts by weight, its raw material includes, fluorine zirconic acid 10-20
Part, phytate 6-12 parts, high-molecular compound 2-4 parts, water-soluble resin 10-20 parts, silane coupler 4-6 parts, titanium dioxide
4-6 parts, chelating agent 12-14 parts；
The high-molecular compound is 2,3,5,6- tetramethyl -1,4- dioxane -2,5- glycol, polyvinyl alcohol, polyethylene glycol
Mixture.
2. the special passivation film agent of a kind of aluminum products according to claim 1, it is characterized in that, described 2,3,5,6- tetramethyls
Base -1,4- dioxane -2,5- glycol, polyvinyl alcohol, the mass ratio of polyethylene glycol are 2:1:1.
3. the special passivation film agent of a kind of aluminum products according to claim 1, it is characterized in that, the chelating agent is ethylenediamine
Tetraacethyl or sodium ethylene diamine tetracetate.
4. the special passivation film agent of a kind of aluminum products according to claim 1, it is characterized in that, the water-soluble resin is ring
Oxygen tree fat or acrylic resin.
5. the special passivation film agent of a kind of aluminum products according to claim 1, it is characterized in that, the silane coupler is second
Alkenyl trimethoxy silane or 3- aminopropyl trimethoxy silicon.
6. the special passivation film agent of a kind of aluminum products according to claim 1, it is characterized in that, the phytate is sodium phytate
Or POTASSIUM PHYTATE.
7. it is a kind of prepare aluminum products as claimed in claim 1 it is special passivation film agent method, it is characterized in that, including at least with
Lower step：
S1：Fluorine zirconic acid, silane coupler, phytate is taken to add in pure water, after solid matter is completely dissolved, into mixed liquor
High-molecular compound is slowly added into, the addition time is 10-20min, and uniform stirring is until solid matter is completely dissolved；
S2：Water-soluble resin is added in the mixed liquor that S1 is obtained, and uniform stirring 20-30min is until solid matter is completely dissolved；
S3：Titanium dioxide, chelating agent is taken to add in the mixed liquor that S2 is obtained, uniform stirring 20-30min, until solid matter is complete
Fully dissolved, film agent is prepared.
8. a kind of preparation method of the special passivation film agent of aluminum products according to claim 7, it is characterized in that, the step
In S1, system temperature is 42-46 DEG C.
9. a kind of preparation method of the special passivation film agent of aluminum products according to claim 7, it is characterized in that, the step
In S2, system temperature is 51-59 DEG C.
10. a kind of preparation method of the special passivation film agent of aluminum products according to claim 7, it is characterized in that, the step
In rapid S3, system temperature is 31-37 DEG C.
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| CN112921312A (en) * | 2019-12-07 | 2021-06-08 | 东莞市集田新材料科技有限公司 | Preparation method of environment-friendly nano-coating agent |
| CN113373435A (en) * | 2021-04-15 | 2021-09-10 | 马鞍山佰斯予菲环保新材料科技有限公司 | Non-phosphorus film agent and preparation method thereof |
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| CN109321906A (en) * | 2018-12-05 | 2019-02-12 | 湖南恒佳新材料科技有限公司 | A kind of anticorrosion aluminium material and preparation method thereof |
| CN112921312A (en) * | 2019-12-07 | 2021-06-08 | 东莞市集田新材料科技有限公司 | Preparation method of environment-friendly nano-coating agent |
| CN113373435A (en) * | 2021-04-15 | 2021-09-10 | 马鞍山佰斯予菲环保新材料科技有限公司 | Non-phosphorus film agent and preparation method thereof |
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