CN105401142A - Aluminum alloy sodium soap grease cured film forming solution and preparation method thereof - Google Patents
Aluminum alloy sodium soap grease cured film forming solution and preparation method thereof Download PDFInfo
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- CN105401142A CN105401142A CN201510739898.9A CN201510739898A CN105401142A CN 105401142 A CN105401142 A CN 105401142A CN 201510739898 A CN201510739898 A CN 201510739898A CN 105401142 A CN105401142 A CN 105401142A
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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
- C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
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Abstract
The invention discloses an aluminum alloy sodium soap grease cured film forming solution. The solution is composed of, by weight, 1-2 parts of myristic acid, 0.1-0.3 part of polydimethylsiloxane, 3-4 parts of sodium soap grease, 100-110 parts of bis(gamma-triethoxysilylpropyl)tetrasulfide, 10-12 parts of butyl titanate, 0.8-1 part of calcium lactobionate, 3-5 parts of multiwalled carbon nanotubes, 0.8-1 part of cerous nitrate, 0.3-1 part of trimethylolpropane, 0.08-0.1 part of polytetrafluoroethylene, 1-2 parts of sodium pyrophosphate and 0.1-0.2 part of triethanolamine borate. The sodium soap grease treated by the polydimethylsiloxane is added into a cured film, friction on the surface of aluminum alloy can be lowered, and a good lubricating effect is achieved.
Description
Technical field
The present invention relates to technical field of aluminum alloy surface treatment, particularly relate to a kind of aluminium alloy sodium base grease cured film shaping dope 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 sodium base grease cured film shaping dope and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of aluminium alloy sodium base grease cured film shaping dope, it is made up of the raw material of following weight parts:
Tetradecanoic acid 1-2, polydimethylsiloxane 0.1-0.3, sodium base grease 3-4, two (the silica-based propyl group of γ-triethoxy) tetrasulfide 100-110, butyl (tetra) titanate 10-12, calcium lactobionate 0.8-1, multi-walled carbon nano-tubes 3-5, cerous nitrate 0.8-1, TriMethylolPropane(TMP) 0.3-1, tetrafluoroethylene 0.08-0.1, trisodium phosphate 1-2, triethanolamine borate 0.1-0.2.
A preparation method for described aluminium alloy sodium base grease cured film shaping dope, comprises the following steps:
(1) above-mentioned two (the silica-based propyl group of γ-triethoxy) tetrasulfide is mixed by the volume ratio of 1-2:3-4:90-100 with deionized water, dehydrated alcohol, ultrasonic disperse 10-20 minute, add Glacial acetic acid, adjustment PH is 4-5, at 20-30 DEG C, be incubated 46-50 hour, obtain coupling agent solution;
(2) joined in 16-20 times of dehydrated alcohol by above-mentioned sodium base grease, stir, add calcium lactobionate, insulated and stirred 3-5 minute at 70-80 DEG C, add above-mentioned polydimethylsiloxane, 100-200 rev/min is stirred 10-16 minute, obtains silane lubricating grease;
(3) above-mentioned triethanolamine borate is joined in 5-10 times of dehydrated alcohol, stir, add tetradecanoic acid, raised temperature is 50-60 DEG C, adds above-mentioned coupling agent solution, drips the sulfuric acid of 96-98%, adjustment PH is 1-3, insulation reaction 40-50 minute, obtains modification coupling agent solution;
(4) above-mentioned cerous nitrate is joined its volume 200-300 doubly, in the ethanolic soln of 4-6%, ultrasonic 1-2 minute is rare earth alcohol liquid;
(5) mixed by the volume ratio of 1-2:25-30:2-3 with dehydrated alcohol, acetic acid by above-mentioned butyl (tetra) titanate, stir, drip above-mentioned rare earth alcohol liquid, add above-mentioned silane lubricating grease after dropwising, stir, ageing 20-24 hour, obtains TiO 2 sol;
(6) 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;
(7) 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 modification 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 sodium base grease cured 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.
Add the sodium base grease of polydimethylsiloxane process in cured film of the present invention, the friction of aluminum alloy surface can be reduced, there is good lubricant effect.
Embodiment
A kind of aluminium alloy sodium base grease cured film shaping dope, it is made up of the raw material of following weight parts:
Tetradecanoic acid 1, polydimethylsiloxane 0.1, sodium base grease 3, two (the silica-based propyl group of γ triethoxy) tetrasulfide 100, butyl (tetra) titanate 10, calcium lactobionate 0.8, multi-walled carbon nano-tubes 3, cerous nitrate 0.8, TriMethylolPropane(TMP) 0.3, tetrafluoroethylene 0.08, trisodium phosphate 1, triethanolamine borate 0.1.
A preparation method for described aluminium alloy sodium base grease cured film shaping dope, comprises the following steps:
(1) above-mentioned two (the silica-based propyl group of γ triethoxy) tetrasulfide is mixed by the volume ratio of 1:3:90 with deionized water, dehydrated alcohol, ultrasonic disperse 10 minutes, adds Glacial acetic acid, regulates PH to be 4, at 20 DEG C, be incubated 46 hours, obtain coupling agent solution;
(2) joined in 16 times of dehydrated alcohols by above-mentioned sodium base grease, stir, add calcium lactobionate, at 70 DEG C, insulated and stirred 3 minutes, adds above-mentioned polydimethylsiloxane, and 100 revs/min are stirred 10 minutes, obtain silane lubricating grease;
(3) above-mentioned triethanolamine borate joined in 5 times of dehydrated alcohols, stir, add tetradecanoic acid, raised temperature is 50 DEG C, adds above-mentioned coupling agent solution, drips the sulfuric acid of 96%, and regulate PH to be 1, insulation reaction 40 minutes, obtains modification coupling agent solution;
(4) above-mentioned cerous nitrate is joined its volume 200 times, 4% ethanolic soln in, ultrasonic 1 minute is rare earth alcohol liquid;
(5) mixed by the volume ratio of 1:25:2 with dehydrated alcohol, acetic acid by above-mentioned butyl (tetra) titanate, stir, drip above-mentioned rare earth alcohol liquid, add above-mentioned silane lubricating grease, stir after dropwising, ageing 20 hours, obtains TiO 2 sol;
(6) 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;
(7) 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 modification 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 sodium base grease cured 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 sodium base grease cured film shaping dope, is characterized in that what it was made up of the raw material of following weight parts:
Tetradecanoic acid 1-2, polydimethylsiloxane 0.1-0.3, sodium base grease 3-4, two (the silica-based propyl group of γ-triethoxy) tetrasulfide 100-110, butyl (tetra) titanate 10-12, calcium lactobionate 0.8-1, multi-walled carbon nano-tubes 3-5, cerous nitrate 0.8-1, TriMethylolPropane(TMP) 0.3-1, tetrafluoroethylene 0.08-0.1, trisodium phosphate 1-2, triethanolamine borate 0.1-0.2.
2. a preparation method for aluminium alloy sodium base grease cured film shaping dope as claimed in claim 1, is characterized in that comprising the following steps:
(1) above-mentioned two (the silica-based propyl group of γ-triethoxy) tetrasulfide is mixed by the volume ratio of 1-2:3-4:90-100 with deionized water, dehydrated alcohol, ultrasonic disperse 10-20 minute, add Glacial acetic acid, adjustment PH is 4-5, at 20-30 DEG C, be incubated 46-50 hour, obtain coupling agent solution;
(2) joined in 16-20 times of dehydrated alcohol by above-mentioned sodium base grease, stir, add calcium lactobionate, insulated and stirred 3-5 minute at 70-80 DEG C, add above-mentioned polydimethylsiloxane, 100-200 rev/min is stirred 10-16 minute, obtains silane lubricating grease;
(3) above-mentioned triethanolamine borate is joined in 5-10 times of dehydrated alcohol, stir, add tetradecanoic acid, raised temperature is 50-60 DEG C, adds above-mentioned coupling agent solution, drips the sulfuric acid of 96-98%, adjustment PH is 1-3, insulation reaction 40-50 minute, obtains modification coupling agent solution;
(4) above-mentioned cerous nitrate is joined its volume 200-300 doubly, in the ethanolic soln of 4-6%, ultrasonic 1-2 minute is rare earth alcohol liquid;
(5) mixed by the volume ratio of 1-2:25-30:2-3 with dehydrated alcohol, acetic acid by above-mentioned butyl (tetra) titanate, stir, drip above-mentioned rare earth alcohol liquid, add above-mentioned silane lubricating grease after dropwising, stir, ageing 20-24 hour, obtains TiO 2 sol;
(6) 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;
(7) 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 modification 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 sodium base grease cured 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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| CN102453429A (en) * | 2010-10-26 | 2012-05-16 | 浙江大学 | Preparation method for nano-TiO2/organic silicon metal anti-corrosion coating |
| WO2012101215A1 (en) * | 2011-01-28 | 2012-08-02 | Hydro Aluminium Rolled Products Gmbh | Aluminium strip with a high thermal and electrical conductivity |
| CN104630749A (en) * | 2015-02-22 | 2015-05-20 | 桂林理工大学 | Corrosion-resistant self-assembled doped film layer on aluminum alloy surface and preparation method of corrosion-resistant self-assembled doped film layer |
| CN104710555A (en) * | 2015-04-01 | 2015-06-17 | 海安索菲亚生态环境新材料科技有限公司 | Method for preparing water-based hybrid anti-corrosive emulsion with self-repairing function |
| CN104988482A (en) * | 2015-07-11 | 2015-10-21 | 合肥正浩机械科技有限公司 | Polyacid metal surface treating agent and preparation method thereof |
-
2015
- 2015-11-04 CN CN201510739898.9A patent/CN105401142A/en active Pending
Patent Citations (6)
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| CN101583739A (en) * | 2006-09-29 | 2009-11-18 | 莫门蒂夫性能材料股份有限公司 | Storage stable composition of partial and/or complete condensate of hydrolyzable organofunctional silane |
| CN102453429A (en) * | 2010-10-26 | 2012-05-16 | 浙江大学 | Preparation method for nano-TiO2/organic silicon metal anti-corrosion coating |
| WO2012101215A1 (en) * | 2011-01-28 | 2012-08-02 | Hydro Aluminium Rolled Products Gmbh | Aluminium strip with a high thermal and electrical conductivity |
| CN104630749A (en) * | 2015-02-22 | 2015-05-20 | 桂林理工大学 | Corrosion-resistant self-assembled doped film layer on aluminum alloy surface and preparation method of corrosion-resistant self-assembled doped film layer |
| CN104710555A (en) * | 2015-04-01 | 2015-06-17 | 海安索菲亚生态环境新材料科技有限公司 | Method for preparing water-based hybrid anti-corrosive emulsion with self-repairing function |
| CN104988482A (en) * | 2015-07-11 | 2015-10-21 | 合肥正浩机械科技有限公司 | Polyacid metal surface treating agent and preparation method thereof |
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Application publication date: 20160316 |