CN105331964A - Rust-protection aluminum alloy curing film and preparation method thereof - Google Patents
Rust-protection aluminum alloy curing film and preparation method thereof Download PDFInfo
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- CN105331964A CN105331964A CN201510633017.5A CN201510633017A CN105331964A CN 105331964 A CN105331964 A CN 105331964A CN 201510633017 A CN201510633017 A CN 201510633017A CN 105331964 A CN105331964 A CN 105331964A
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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
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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
- 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
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Abstract
The invention discloses a rust-protection aluminum alloy curing film. The rust-protection aluminum alloy curing film is composed of, by weight, 10-12 parts of butyl titanate, 1.6-2 parts of aluminum sulfate, 3-4 parts of inositol hexaphosphate, 100-110 parts of bis-(gamma-triethoxysilylpropyl)-tetrasulfide, 3-5 parts of multiwalled carbon nanotubes, 0.8-1 part of cerous nitrate, 0.08-0.1 part of polytetrafluoroethylene, 0.3-1 part of sodium alcohol ether sulphate, 2-3 parts of dodeceny succinicanhydride, 0.7-1 part of salatrim and 0.3-1 part of thrihydroxymethyl propane. According to the curing film, rust protection emulsion is added, the rust protection effect on the surface of the curing film can be improved remarkably, the service life of aluminum alloy is prolonged, and the corrosion loss is lowered.
Description
Technical field
The present invention relates to technical field of aluminum alloy surface treatment, particularly relate to a kind of aluminium alloy solidification anti-rust film and preparation method thereof.
Background technology
Silane due to its uniqueness molecular structure, asepsis environment-protecting, cost is low, consistency is good etc., and feature starts to be applied to anti-corrosion of metal field by people.Silane can be combined with metallic matrix closely through hydrolysis, forms fine and close rete, have good protected effect to metal on surface.But when the porous of silane film own, resistibility is corroded to corrosive medium more weak, in corrosive environment, Cl-etc. are easy especially to be corroded along these defects, the accumulation of corrosion product in interface can make formation stressed zone, interface, and cause the stripping of rete to come off, such silane film is once be destroyed, cannot selfreparing be carried out, be easy to the corrosion causing metallic matrix.Research finds to prepare organic and inorganic silane complex film by the inorganic nano-particle that adulterates in silane film with the material (as rare earth ions such as Ce, La) with self-repair function, effectively can prevent these defects of silane complex film.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides a kind of aluminium alloy to solidify anti-rust film and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of aluminium alloy solidification anti-rust film, it is made up of the raw material of following weight parts:
Butyl (tetra) titanate 10-12, Tai-Ace S 150 1.6-2, myo-Inositol hexaphosphate 3-4, two (the silica-based propyl group of γ-triethoxy) tetrasulfide 100-110, multi-walled carbon nano-tubes 3-5, cerous nitrate 0.8-1, tetrafluoroethylene 0.08-0.1, ethoxylated alkyl ammonium sulfate 0.3-1, dodecenylsuccinic acid acid anhydride 2-3, short and long-chain acyl triglyceride molecules 0.7-1, TriMethylolPropane(TMP) 0.3-1.
A preparation method for described aluminium alloy solidification anti-rust film, comprises the following steps:
(1) above-mentioned dodecenylsuccinic acid acid anhydride is joined its weight 10-13 doubly, in the ethanolic soln of 30-35%, stir, add short and long-chain acyl triglyceride molecules, raised temperature is 70-80 DEG C, insulated and stirred 7-10 minute, obtains rust protection liquid a;
(2) joined in 10-12 times of water by above-mentioned myo-Inositol hexaphosphate, stirring and dissolving, adds Tai-Ace S 150, and insulated and stirred 20-30 minute at 50-60 DEG C obtains rust protection liquid b;
(3) above-mentioned rust protection liquid a, rust protection liquid b are mixed, add ethoxylated alkyl ammonium sulfate, 200-300 rev/min is stirred 5-10 minute, obtains antirust emulsion;
(4) above-mentioned two (the silica-based propyl group of γ-triethoxy) tetrasulfide mixes by the volume ratio of 1-2:3-4:90-100 with deionized water, dehydrated alcohol, ultrasonic disperse 10-20 minute, adds Glacial acetic acid, and adjustment PH is 4-5, at 20-30 DEG C, be incubated 46-50 hour, obtain coupling agent solution;
(5) above-mentioned cerous nitrate is joined its volume 200-300 doubly, in the ethanolic soln of 4-6%, ultrasonic 1-2 minute, adds above-mentioned antirust emulsion, continues ultrasonic 2-3 minute, is the antirust alcohol liquid of rare earth;
(6) above-mentioned butyl (tetra) titanate is mixed by the volume ratio of 1-2:25-30:2-3 with dehydrated alcohol, acetic acid, stir, drip the antirust alcohol liquid of above-mentioned rare earth, dropwise rear ageing 20-24 hour, obtain TiO 2 sol;
(7) be mixed to join in resistance furnace by above-mentioned tetrafluoroethylene, multi-walled carbon nano-tubes, reacting by heating 5-6 hour at 480-500 DEG C, cooling is come out of the stove, and is washed by product, dries, obtain carbon fluoride nano-tube;
(8) above-mentioned TriMethylolPropane(TMP) is joined in 80-100 times of dehydrated alcohol, stir, add carbon fluoride nano-tube, ultrasonic 17-20 minute, mix with above-mentioned coupling agent solution, TiO 2 sol, add each raw material of residue, stir, at 75-80 DEG C, distill 1-2 hour, cool and get final product.
Described a kind of aluminium alloy solidification anti-rust film shaping dope, the using method of this aluminium alloy cured film shaping dope is:
(1) after aluminium alloy being polished with carborundum paper, use the diamond paste polishing of 0.5 μm again, afterwards successively with acetone, ethanol, water three kinds of solvent supersonic cleanings, cleaned sample is processed respectively in the HNO3 solution of 1.8-2%NaOH solution and 4-5%, finally use deionized water ultrasonic cleaning, nitrogen drying is for subsequent use;
(2) the aluminium alloy pickling process pulling film forming in above-mentioned solution will handled well, sends into after film forming in loft drier, solidifies 110-120min, obtain cured film at 115-120 DEG C.
Advantage of the present invention is:
The carbon nanotube chemical character that the present invention adds is highly stable, and its C-C singly-bound is the most stable chemical bond of occurring in nature, effectively can improve solidity to corrosion and the mechanical property of substrate surface film;
Present invention adds rare earth nitrate, the oxide compound formed through passivation and oxyhydroxide can be formed with the reticulated structure of organosilane and act synergistically, fine and close coating is formed with carbon nanotube, carbonic acid gas, cathodic depolarization is effectively inhibit to react and anode dissolution reaction, reduce erosion rate, play good protective effect;
In the present invention, adding of titanium dioxide makes the compactness of silane complex film increase, effectively prevent the erosion of the corrosive ions such as Cl-, H2O and O2, the diffusion of corrosion product can be suppressed, due to aperture blocking effect, stop the further generation of corrosion, this is because a part of TiOH group will react with the hydroxyl of metallic surface, Si-OH, at aluminium alloy matrix surface synergistic sorption, this just effectively enhances the bonding force of rete and matrix, overcomes the shortcoming that simple silane film is easy to peel off at matrix surface;
The present invention is C-F key at multi-walled carbon nano-tubes Surface Creation, can improve the dispersiveness in film with TiO 2 particles, effectively reduces reunion, can also improve the water resisting property of film coated surface simultaneously;
Composite membrane of the present invention has excellent protective value to alloy matrix aluminum; can anode dissolution be effectively suppressed to react; multi-walled carbon nano-tubes can with the functional groups Cheng Jian of titanium dioxide, two (the silica-based propyl group of γ-triethoxy) tetrasulfide; serve the compactness increasing film; improve the effect of the stability of film; effectively can stop the immersion of corrosive medium, thus improve corrosion resistance.
Cured film of the present invention adds antirust emulsion, can significantly improve the rust-proof effect on cured film surface, improves the life-span of aluminium alloy, reduces corrosive wear.
Embodiment
A kind of aluminium alloy solidification anti-rust film, it is made up of the raw material of following weight parts:
Butyl (tetra) titanate 10, Tai-Ace S 150 1.6, myo-Inositol hexaphosphate 3, two (the silica-based propyl group of γ triethoxy) tetrasulfide 100, multi-walled carbon nano-tubes 3, cerous nitrate 0.8, tetrafluoroethylene 0.08, ethoxylated alkyl ammonium sulfate 0.3, dodecenylsuccinic acid acid anhydride 2, short and long-chain acyl triglyceride molecules 0.7, TriMethylolPropane(TMP) 0.3.
A preparation method for described aluminium alloy solidification anti-rust film, comprises the following steps:
(1) above-mentioned dodecenylsuccinic acid acid anhydride is joined its weight 10 times, 30% ethanolic soln in, stir, add short and long-chain acyl triglyceride molecules, raised temperature is 70 DEG C, and insulated and stirred 7 minutes, obtains rust protection liquid a;
(2) joined in 10 times of water by above-mentioned myo-Inositol hexaphosphate, stirring and dissolving, adds Tai-Ace S 150, and at 50 DEG C, insulated and stirred 20 minutes, obtains rust protection liquid b;
(3) above-mentioned rust protection liquid a, rust protection liquid b are mixed, add ethoxylated alkyl ammonium sulfate, 200 revs/min are stirred 5 minutes, obtain antirust emulsion;
(4) above-mentioned two (the silica-based propyl group of γ triethoxy) tetrasulfide mixes by the volume ratio of 1:3:90 with deionized water, dehydrated alcohol, and ultrasonic disperse 10 minutes, adds Glacial acetic acid, regulates PH to be 4, is incubated 46 hours, obtains coupling agent solution at 20 DEG C;
(5) above-mentioned cerous nitrate is joined its volume 200 times, 4% ethanolic soln in, ultrasonic 1 minute, adding above-mentioned antirust emulsion, continue ultrasonic 2 minutes, is the antirust alcohol liquid of rare earth;
(6) above-mentioned butyl (tetra) titanate is mixed by the volume ratio of 1:25:2 with dehydrated alcohol, acetic acid, stir, drip the antirust alcohol liquid of above-mentioned rare earth, dropwise rear ageing 20 hours, obtain TiO 2 sol;
(7) be mixed to join in resistance furnace by above-mentioned tetrafluoroethylene, multi-walled carbon nano-tubes, reacting by heating 5 hours at 480 DEG C, cooling is come out of the stove, and is washed by product, dries, obtain carbon fluoride nano-tube;
(8) above-mentioned TriMethylolPropane(TMP) is joined in 80 times of dehydrated alcohols, stir, add carbon fluoride nano-tube, ultrasonic 17 minutes, mix with above-mentioned coupling agent solution, TiO 2 sol, add each raw material of residue, stir, distill 1 hour at 75 DEG C, cool and get final product.
Described a kind of aluminium alloy solidification anti-rust film shaping dope, the using method of this aluminium alloy cured film shaping dope is:
(1) after aluminium alloy being polished with carborundum paper, use the diamond paste polishing of 0.5 μm again, afterwards successively with acetone, ethanol, water three kinds of solvent supersonic cleanings, by cleaned sample respectively 1.8%NaOH solution and 4% HNO3 solution in process, finally use deionized water ultrasonic cleaning, nitrogen drying is for subsequent use;
(2) the aluminium alloy pickling process pulling film forming in above-mentioned solution will handled well, sends into after film forming in loft drier, solidifies 110min, obtain cured film at 115 DEG C.
Performance test:
Bending viscosity:
By cured film shaping dope process aluminum alloy sheet of the present invention, after film-forming, by bending 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless;
Aluminum alloy sheet after film-forming is soaked 1 hour in boiling water, at room temperature places 24 hours, then by bending 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless;
Erosion resistance:
By cured film shaping dope process aluminum alloy sheet of the present invention, after film-forming, by this material lateral dissection, carry out spray test, agents useful for same to be concentration be 5% sodium chloride solution, test period 300 hours, measure the bubbling width formed in line of cut side, result bubbling width is 0;
Aluminum alloy sheet after film-forming being immersed in concentration is in the sodium chloride solution of 5%, and soak 300 hours, material surface is substantially unchanged, and soak 400 hours, minute quantity rust staining appears in edge.
Claims (3)
1. an aluminium alloy solidification anti-rust film, is characterized in that what it was made up of the raw material of following weight parts:
Butyl (tetra) titanate 10-12, Tai-Ace S 150 1.6-2, myo-Inositol hexaphosphate 3-4, two (the silica-based propyl group of γ-triethoxy) tetrasulfide 100-110, multi-walled carbon nano-tubes 3-5, cerous nitrate 0.8-1, tetrafluoroethylene 0.08-0.1, ethoxylated alkyl ammonium sulfate 0.3-1, dodecenylsuccinic acid acid anhydride 2-3, short and long-chain acyl triglyceride molecules 0.7-1, TriMethylolPropane(TMP) 0.3-1.
2. a preparation method for aluminium alloy solidification anti-rust film as claimed in claim 1, is characterized in that comprising the following steps:
(1) above-mentioned dodecenylsuccinic acid acid anhydride is joined its weight 10-13 doubly, in the ethanolic soln of 30-35%, stir, add short and long-chain acyl triglyceride molecules, raised temperature is 70-80 DEG C, insulated and stirred 7-10 minute, obtains rust protection liquid a;
(2) joined in 10-12 times of water by above-mentioned myo-Inositol hexaphosphate, stirring and dissolving, adds Tai-Ace S 150, and insulated and stirred 20-30 minute at 50-60 DEG C obtains rust protection liquid b;
(3) above-mentioned rust protection liquid a, rust protection liquid b are mixed, add ethoxylated alkyl ammonium sulfate, 200-300 rev/min is stirred 5-10 minute, obtains antirust emulsion;
(4) above-mentioned two (the silica-based propyl group of γ-triethoxy) tetrasulfide mixes by the volume ratio of 1-2:3-4:90-100 with deionized water, dehydrated alcohol, ultrasonic disperse 10-20 minute, adds Glacial acetic acid, and adjustment PH is 4-5, at 20-30 DEG C, be incubated 46-50 hour, obtain coupling agent solution;
(5) above-mentioned cerous nitrate is joined its volume 200-300 doubly, in the ethanolic soln of 4-6%, ultrasonic 1-2 minute, adds above-mentioned antirust emulsion, continues ultrasonic 2-3 minute, is the antirust alcohol liquid of rare earth;
(6) above-mentioned butyl (tetra) titanate is mixed by the volume ratio of 1-2:25-30:2-3 with dehydrated alcohol, acetic acid, stir, drip the antirust alcohol liquid of above-mentioned rare earth, dropwise rear ageing 20-24 hour, obtain TiO 2 sol;
(7) be mixed to join in resistance furnace by above-mentioned tetrafluoroethylene, multi-walled carbon nano-tubes, reacting by heating 5-6 hour at 480-500 DEG C, cooling is come out of the stove, and is washed by product, dries, obtain carbon fluoride nano-tube;
(8) above-mentioned TriMethylolPropane(TMP) is joined in 80-100 times of dehydrated alcohol, stir, add carbon fluoride nano-tube, ultrasonic 17-20 minute, mix with above-mentioned coupling agent solution, TiO 2 sol, add each raw material of residue, stir, at 75-80 DEG C, distill 1-2 hour, cool and get final product.
3. a kind of aluminium alloy solidification anti-rust film shaping dope according to claim 1, is characterized in that the using method of this aluminium alloy cured film shaping dope is:
(1) after aluminium alloy being polished with carborundum paper, use the diamond paste polishing of 0.5 μm again, afterwards successively with acetone, ethanol, water three kinds of solvent supersonic cleanings, cleaned sample is processed respectively in the HNO3 solution of 1.8-2%NaOH solution and 4-5%, finally use deionized water ultrasonic cleaning, nitrogen drying is for subsequent use;
(2) the aluminium alloy pickling process pulling film forming in above-mentioned solution will handled well, sends into after film forming in loft drier, solidifies 110-120min, obtain cured film at 115-120 DEG C.
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| CN201510633017.5A CN105331964A (en) | 2015-09-29 | 2015-09-29 | Rust-protection aluminum alloy curing film and preparation method thereof |
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| CN201510633017.5A CN105331964A (en) | 2015-09-29 | 2015-09-29 | Rust-protection aluminum alloy curing film and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108060414A (en) * | 2017-12-14 | 2018-05-22 | 马鞍山新徽铝业有限公司 | A kind of aluminium sheet passivating solution |
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| JP2004232047A (en) * | 2003-01-31 | 2004-08-19 | Dipsol Chem Co Ltd | Treatment agent for forming highly corrosion resistant chromium-free chemical conversion film on aluminum and aluminum alloy, method of forming the chemical conversion film, and aluminum and aluminum alloy with the chemical conversion film formed |
| CN102873015A (en) * | 2012-10-29 | 2013-01-16 | 南京信息工程大学 | Method for treating metal surface |
| CN102912345A (en) * | 2012-10-29 | 2013-02-06 | 南京信息工程大学 | Aluminium alloy surface corrosion control method |
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- 2015-09-29 CN CN201510633017.5A patent/CN105331964A/en active Pending
Patent Citations (3)
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|---|---|---|---|---|
| JP2004232047A (en) * | 2003-01-31 | 2004-08-19 | Dipsol Chem Co Ltd | Treatment agent for forming highly corrosion resistant chromium-free chemical conversion film on aluminum and aluminum alloy, method of forming the chemical conversion film, and aluminum and aluminum alloy with the chemical conversion film formed |
| CN102873015A (en) * | 2012-10-29 | 2013-01-16 | 南京信息工程大学 | Method for treating metal surface |
| CN102912345A (en) * | 2012-10-29 | 2013-02-06 | 南京信息工程大学 | Aluminium alloy surface corrosion control method |
Non-Patent Citations (1)
| Title |
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| 王玉安: ""镀锌板有机硅烷钝化膜的研制与性能研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108060414A (en) * | 2017-12-14 | 2018-05-22 | 马鞍山新徽铝业有限公司 | A kind of aluminium sheet passivating solution |
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Application publication date: 20160217 |