CN1786091A - magnesium alloy non-chromium dacro solution paint and its preparation method - Google Patents
magnesium alloy non-chromium dacro solution paint and its preparation method Download PDFInfo
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Abstract
The present invention discloses a magnesium alloy chrome-free dyclo solution coating and its production method. It is characterized by that the organic silicon and nano powder body undergone the process of nano dispersing liquor treatment are dispersed in the resin made up by using several resins through the process of polymerization and cross-linking reaction to make modification, and mixed with zinc powder and aluminium powder so as to obtain the invented acid-resistant, alkali-resistant, salt fog resistant, impact-resistant and corrosion-resistant magnesium alloy chrome-free dyclo solution coating.
Description
Technical field:
The invention provides a kind of magnesium alloy non-chromium dacro solution paint, also disclose its production method simultaneously, belong to metallic surface protective system technical field.
Background technology:
The Dacroment that the present invention relates to is the antirust facture of being succeeded in developing by U.S. ocean company in a kind of metallic surface in 1972.From the sixties in last century, the Dacroment coating technology that is described as " the green plating " is since the U.S. comes out, few because of its environmental pollution, barrier propterty good, no hydrogen embrittlement, can be at iron and steel, aluminium--construct on-multiple the material, coating can stand 300 ℃ of a series of advantages such as high temperature, obtains swift and violent development in the whole world.
Usually traditional dacro solution paint coating contains Cr
6+, Cr in use
6+Stripping descends corrosion resistance of coating, and contaminate environment, the Dacroment coating water-fast, moisture-proof is warm, acidproof rain performance is unsatisfactory.The EOLVD disability regulations that European Union formulated in 1999 are just to Cr
6+Amount carried out strict restriction.Stipulate among the 2000/53/EG of Europe, from July 1st, 2003, in each automobile of European production and selling, Cr
6+Content must not surpass 2 grams.Therefore, the magnesium alloy dacro solution paint of Patent exploitation of the present invention must be the technology of Chrome-free.
At present, on the external automobile Application of Magnesium with 25% speed increment, the Application and Development of Magnesium Alloy Automobile Parts has become the focus of Hyundai Motor research every year on average.Yet, because the extremely active (E of magnesium alloy chemical character
0Serious corrosion in the atmospheric environment of humidity, can take place in=-2.73V), and therefore, the application of magnesium alloy parts must be carried out surface treatment.Because the extremely active (E of magnesium alloy chemical material
O=-2.73V) can produce serious corrosion in atmospheric environment, therefore, the magnesium alloy parts material is used must be along carrying out surface treatment.And traditional dacro solution paint is inoperative on magnesium alloy parts and material antiseptic.
Summary of the invention:
The present invention discloses a kind of magnesium alloy non-chromium dacro solution paint, has solved existing dacro solution paint and other coating are coated with the sticking power of loading onto existence, salt spray resistance, moisture-proof heat, acidproof, alkali resistance difference at the magnesium alloy parts material problem.
The present invention also provides the production method of magnesium alloy non-chromium dacro solution paint, is applicable to suitability for industrialized production.
Technical solution of the present invention is as follows: with organosilicon, the nano-powder through nano dispersion fluid was handled is distributed in the resin of various kinds of resin polymerization crosslinking, and it is carried out modification, adds zinc flake and aluminium powder in the resin after modification.
Its prescription is mainly made by following materials of weight proportions: (by ratio of weight and the number of copies)
Organosilicon: 0.5-5, nano-powder: 0.1-5, nano dispersion fluid: 0.05-15, compound resin: 60-100, organic solvent: 5-50, deionized water 5～25, zinc powder 30～80, aluminium powder 10～30.
Described nano-powder is selected from one or more in the following raw material: (1) nano level metal nickel (Ni); (2) nanometer grade silica (SiO
2); (3) nano level chromic oxide (Cr
2O
3); (4) nano-diamond/carbon composite particles.(5) Nano titanium dioxide (TiO
2); (6) Nano-class zinc oxide (ZnO); (7) alumina in Nano level (Al
2O
3).
Described solvent is selected from one or more in the following raw material:
(1) ether-ether class: as 2-Butoxyethyl acetate, propylene-glycol ethyl ether acetic ester etc.;
(2) ketone: as methyl iso-butyl ketone (MIBK), acetone, pimelinketone etc.;
(3) alcohols: as butanols, ethanol, Virahol etc.;
(4) ethers: as ethylene glycol monobutyl ether, propylene glycol monobutyl ether etc.;
Described compound resin is selected from one or more in the following raw material: amino (4) formaldehyde (5) phenolic aldehyde (6) polyester (7) fluorine carbon (8) butyral of (1) vinylformic acid (2) epoxy (3).Stir on intensification limit, limit, 60 ℃-180 ℃ of temperature, and revolution 500-1200 changes, and stirs 4-8 hour, leaves standstill 12-24 hour.Adjust pH value 7.5-12.
Described nano dispersion fluid is selected from one or more in the following raw material: (1) organo-silicon coupling agent comprises KH-550, KH-560, KH-560; (2) the organic titanium coupling agent comprises that KHT-203, KHT-301, KHT-303, KHT-305 (3) organoaluminum coupling agent comprise DL-411, XL-955.
Described organosilicon is selected from one or more in the following raw material: (1) hydroxyl polysiloxane, and (2) vinyltriethoxysilane, other contains the active organosilicon macromole of unsaturated double-bond (3).
Concrete production technique may further comprise the steps:
1, the preparation of compound resin: take by weighing resin according to the above ratio, with this ratio resin warming while stirring in reactor, 60 ℃-180 ℃ of temperature, revolution is 120-800 rev/min, be warming up to 60 ℃-180 ℃ after, the additional proportion organosilicon, constant temperature stirred 4-8 hour, left standstill 12-24 hour, and adjusted pH value 7.5-12, make compound resin.
2, nano-powder dispersion liquid preparation: take by weighing the organic salt coupling agent according to the above ratio, this ratio organic salt coupling agent liquid intensification limit in limit in reactor is stirred, 40 ℃-90 ℃ of temperature, revolution is 500-1200 rev/min, constant temperature stirs the 10-60 branch, add nano-powder again after adding organic solvent and deionized water latting drown, nano-powder must carry out heating under vacuum, the pre-treatment of drying before adding.Vacuum tightness should be at 3-6Pa, 80 ℃-150 ℃ of temperature.The nano-powder dispersion liquid of adjusting, blending is at room temperature carried out sand milling, dispersion, time 4-10 hour.
3, zinc powder 30～80,10～30 kilograms of aluminium powders and nano dispersion fluid are added in the compound resin, temperature 40-80 ℃, revolution is 600-1200 rev/min, time 2-4 hour.
4, after normal temperature leaves standstill 8-12 hour, sand milling, dispersion, filtration.Promptly becoming nano powder modified compound resin is film forming matter, and zinc flake, aluminium powder are the magnesium alloy non-chromium dacro solution paint of anti-corrosion paint.
Main effect of the present invention is: with organosilicon, nano silica fume or (with) nanometer aluminium powder or nano-nickel powder or (with) nano titanium powder or nanometer diamond powder or (with) unformed carbon dust after the coupling agent dispersion treatment, dose by a certain percentage crosslinking polymerization by a certain percentage acrylic acid and amino or (with) fluorine carbon, Resins, epoxy; Dose by a certain percentage fluorine carbon or (with) epoxy or (with) amino; Dose by a certain percentage butyral or (with) epoxy or (with) resin of phenolic aldehyde crosslinking polymerization, the synergistic effect resin of various kinds of resin polymerization crosslinking, add organosilicon and nano powder modified resin, make Chrome-free, environmental protection with zinc flake and aluminium powder, the magnesium alloy non-chromium dacro solution paint of thin, the salt spray resistance of filming, acidproof, alkaline-resisting, shock resistance, strong adhesion, good weatherability.
The present invention has not only kept original Dacroment not produce waste residue, waste gas, sewage, non-environmental-pollution, outside the characteristics such as stronger erosion resistance, thermotolerance, no hydrogen embrittlement, characteristics such as its acid-and base-resisting burn into salt spray resistance, strong adhesion, coating hardness height have been given prominence to more, be a kind of aqueous, environmental protective, energy-conservation Chrome-free system, especially it is anticorrosion to have height, the performance of low thickness.Non-chromium dacro solution paint makes magnesium alloy parts obtain practical value.
Embodiment:
By following examples the present invention is described for example further, and do not limit the present invention in any way, under the prerequisite that does not deviate from technical solution of the present invention, any change or change that those of ordinary skills that the present invention did are realized easily all will fall within the claim scope of the present invention.
Embodiment 1
Get acrylic resin 20-45 kilogram; Aminoresin 20-35 kilogram; Resins, epoxy 10-20 kilogram, with this ratio resin warming while stirring in reactor, 60 ℃-180 ℃ of humidity, revolution is 120-800 rev/min, be warming up to 60 ℃-180 ℃ after, add 0.5-5 kilogram hydroxyl polysiloxane, constant temperature stirred 4-8 hour, left standstill 12-24 hour, the adjustment pH value is 7.5-12, makes compound resin.
Embodiment 2
Get butyral resin 10-30 kilogram; Formaldehyde resin 30-50 kilogram; Resins, epoxy 10-20 kilogram; With this ratio resin warming while stirring in reactor, 60 ℃-180 ℃ of humidity, revolution is 120-800 rev/min, after being warming up to 60 ℃-180 ℃, add 0.5-5 kilogram organosilicon vinyltriethoxysilane, constant temperature stirred 4-8 hour, left standstill 12-24 hour, the adjustment pH value is 7.5-12, makes compound resin.
Embodiment 3
Get alkyd resin 10-40 kilogram; Resol 10-30 kilogram; Resins, epoxy 10-40 kilogram, with this ratio resin warming while stirring in reactor, 60 ℃-180 ℃ of humidity, revolution is 120-800 rev/min, be warming up to 60 ℃-180 ℃ after, add 0.5-5 kilogram organosilicon, constant temperature stirred 4-8 hour, left standstill 12-24 hour, the adjustment pH value is 7.5-12, makes compound resin.
Embodiment 4
With fluorocarbon resin 10-70 kilogram; Resins, epoxy 10-40 kilogram; Aminoresin 10-45 kilogram, with this ratio resin warming while stirring in reactor, 60 ℃-180 ℃ of humidity, revolution is 120-800 rev/min, be warming up to 60 ℃-180 ℃ after, add 0.5-5 kilogram organosilicon, constant temperature stirred 4-8 hour, left standstill 12-24 hour, the adjustment pH value is 7.5-12, makes compound resin.
Embodiment 5
Get 5 kilograms of propylene-glycol ethyl ether acetic esters; 15 kilograms in acetone; 10 kilograms of pimelinketone; 25 kilograms in butanols; 15 kilograms of Virahols; 12 kilograms of propylene glycol monobutyl ethers; 20 kilograms of deionized waters, at room temperature mixing and stirring is made solvent.
Embodiment 6
With 1 kilogram of organo-silicon coupling agent KH-550 and 2 kilograms of organoaluminum coupling agent DL-411, put into high speed agitator, stir on intensification limit, limit, revolution is 500-1200 rev/min, be warming up to 40 ℃-80 ℃ after, constant temperature stirs the 10-20 branch, makes the nano-powder dispersion liquid.
Embodiment 7
With 1 kilogram of organic titanium coupling agent KHT-301 and 10 kilograms of organoaluminum coupling agent DL-411, put into high speed agitator, stir on intensification limit, limit, revolution is 500-1200 rev/min, be warming up to 40 ℃-80 ℃ after, constant temperature stirs the 10-20 branch, makes the nano-powder dispersion liquid.
Embodiment 8
With 2 kilograms of organo-silicon coupling agent KH-560 and 2 kilograms of organic titanium coupling agent KHT-303, put into high speed agitator, stir on intensification limit, limit, revolution is 500-1200 rev/min, be warming up to 40 ℃-80 ℃ after, constant temperature stirs the 10-20 branch, makes the nano-powder dispersion liquid.
Embodiment 9
3 kilograms of nano silica fumes are blended into 1.5 kilograms of embodiment 6 (nano-powder dispersion liquid), in the mixed solution of 30 kilograms of embodiment 5 solvents, the nano-powder mixed solution of converting is at room temperature carried out sand milling, disperseed 4-8 hour, and it is qualified observing no nanometer agglomerated particles in opticmicroscope.Scattered nano-silicon dispersion liquid is blended among 100 kilograms of the embodiment 1 (compound resin), normal temperature high-speed stirring, dispersion, revolution is 800-1600 rev/min, stirring, jitter time are the 40-120 branch, add sheet metal aluminium powder, zinc powder 30-70 kilogram, high-speed stirring, dispersion 40-120 branch are adjusted pH value 7.5-12, promptly become magnesium alloy non-chromium dacro solution paint.The prepared magnesium alloy non-chromium dacro solution paint performance index of this Recipe are as follows:
Outward appearance: similar to conventional Dacroment coating, be silvery white.Sticking power: cross-hatching 100%
Salt spray resistance: pass through 480h; Moisture-proof heat: pass through 144h; Alkali resistance: 2%NaOH, soaking at room temperature is to begin to occur bubble time length comparative coatings
Alkaline resistance properties:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| 1min | 5min | 5min |
Acid resistance: 1%NaSO
4, soaking at room temperature, know short comparative coatings acid resistance to begin occurring bubble time length:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| Immediately | 5min | 10min |
Embodiment 10
2 kilograms of nanometer aluminium powder powder are blended into 2.5 kilograms of embodiment 7 (nano-powder dispersion liquid), in the mixed solution of 30 kilograms of embodiment 5 solvents, the nano-powder mixed solution of converting is at room temperature carried out sand milling, disperseed 4-8 hour, and it is qualified observing no nanometer agglomerated particles in opticmicroscope.Scattered nano-silicon dispersion liquid is blended among 100 kilograms of the embodiment 2 (compound resin), normal temperature high-speed stirring, dispersion, revolution is 800-1600 rev/min, stirring, jitter time are the 40-120 branch, add sheet metal aluminium powder, zinc powder 30-70 kilogram, high-speed stirring, dispersion 40-120 branch are adjusted pH value 7.5-12, promptly become magnesium alloy non-chromium dacro solution paint.The magnesium alloy non-chromium dacro coating property index that this Recipe process makes is as follows:
Outward appearance: similar to conventional Dacroment coating, be silvery white.Sticking power: cross-hatching 100%
Salt spray resistance: pass through 460h; Moisture-proof heat: pass through 124h; Alkali resistance: 2%NaOH, soaking at room temperature is to begin to occur bubble time length comparative coatings
Alkaline resistance properties:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| 1min | 5min | 6min |
Acid resistance: 1%NaSO
4, soaking at room temperature, know short comparative coatings acid resistance to begin occurring bubble time length:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| Immediately | 5min | 12min |
Embodiment 11
1 kilogram of nano-nickel powder and 1 kilogram of nano titanium powder are blended into 3.8 kilograms of embodiment 8 (nano-powder dispersion liquid), in the mixed solution of 30 kilograms of embodiment 5 solvents, the nano-powder mixed solution of converting is at room temperature carried out sand milling, disperseed 4-8 hour, and it is qualified observing no nanometer agglomerated particles in opticmicroscope.Scattered nano-silicon dispersion liquid is blended among 100 kilograms of the embodiment 3 (compound resin), normal temperature high-speed stirring, dispersion, revolution is 800-1600 rev/min, stirring, jitter time are the 40-120 branch, add sheet metal aluminium powder, zinc powder 30-70 kilogram, high-speed stirring, dispersion 40-120 branch are adjusted pH value 7.5-12, promptly become magnesium alloy non-chromium dacro solution paint.The magnesium alloy non-chromium dacro coating property index that this Recipe process makes is as follows:
Outward appearance: similar to conventional Dacroment coating, be silvery white.Sticking power: cross-hatching 100%; Salt spray resistance: pass through 450h; Moisture-proof heat: pass through 128h; Alkali resistance: 2%NaOH, soaking at room temperature is to begin to occur bubble time length comparative coatings.
Alkaline resistance properties:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| 1min | 5min | 5.5min |
Acid resistance: 1%NaSO
4, soaking at room temperature, know short comparative coatings acid resistance to begin occurring bubble time length:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| Immediately | 5min | 11min |
Embodiment 12
3 kilograms of nano silica fumes are blended into 1.5 kilograms of embodiment 6 (nano-powder dispersion liquid), in the mixed solution of 30 kilograms of embodiment 5 solvents, the nano-powder mixed solution of converting is at room temperature carried out sand milling, disperseed 4-8 hour, and it is qualified observing no nanometer agglomerated particles in opticmicroscope.Scattered nano-silicon dispersion liquid is blended among 100 kilograms of the embodiment 4 (compound resin), normal temperature high-speed stirring, dispersion, revolution is 800-1600 rev/min, stirring, jitter time are the 40-120 branch, add sheet metal aluminium powder, zinc powder 30-70 kilogram, high-speed stirring, dispersion 40-120 branch are adjusted pH value 7.5-12, promptly become magnesium alloy non-chromium dacro solution paint.
The magnesium alloy non-chromium dacro coating property index that this Recipe process makes is as follows:
Outward appearance: similar to conventional Dacroment coating, be silvery white.
Sticking power: cross-hatching 100%; Salt spray resistance: pass through 500h; Moisture-proof heat: pass through 160h
Alkali resistance: 2%NaOH, soaking at room temperature is to begin to occur bubble time length comparative coatings
Alkaline resistance properties:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| 1min | 5min | 8min |
Acid resistance: 1%NaSO
4, soaking at room temperature, know short comparative coatings acid resistance to begin occurring bubble time length:
| The conventional Dacroment coating of chromium is arranged | External Magni brand | The chromium-free Dyclo coating of research |
| Immediately | 5min | 20min |
Claims (7)
1, a kind of magnesium alloy non-chromium dacro solution paint is mainly made by following materials of weight proportions: organosilicon: 0.5-5, nano-powder: 0.1-5, nano dispersion fluid: 0.05-15, compound resin: 60-100, organic solvent: 5-50, deionized water 5～25, zinc powder 30～80, aluminium powder 10～30.
2, according to the coating of claim 1, it is characterized in that: described nano-powder is selected from one or more in the following raw material: (1) nano level metal nickel; (2) nanometer grade silica; (3) nano level chromic oxide; (4) nano-diamond/carbon composite particles; (5) Nano titanium dioxide; (6) Nano-class zinc oxide; (7) alumina in Nano level.
3, according to the coating of claim 1, it is characterized in that described nano dispersion fluid is selected from one or more in the following raw material: (1) organo-silicon coupling agent comprises KH-550, KH-560, KH-560; (2) the organic titanium coupling agent comprises that KHT-203, KHT-301, KHT-303, KHT-305 (3) organoaluminum coupling agent comprise DL-411, XL-955.
4, according to the coating of claim 1, it is characterized in that described compound resin is selected from one or more in the following raw material: amino (4) formaldehyde (5) phenolic aldehyde (6) polyester (7) fluorine carbon (8) butyral of (1) vinylformic acid (2) epoxy (3).
5,, it is characterized in that described organic solvent is selected from one or more in the following raw material according to the coating of claim 1:
(1) ether-ether class: as 2-Butoxyethyl acetate, propylene-glycol ethyl ether acetic ester etc.;
(2) ketone: as methyl iso-butyl ketone (MIBK), acetone, pimelinketone etc.;
(3) alcohols: as butanols, ethanol, Virahol etc.;
(4) ethers: as ethylene glycol monobutyl ether, propylene glycol monobutyl ether etc.
6, according to the coating of claim 1, it is characterized in that described organosilicon is selected from one or more in the following raw material: other contains the active organosilicon macromole of unsaturated double-bond (1) hydroxyl polysiloxane (2) vinyltriethoxysilane (3).
7, according to the production method of any described coating of claim 1 to 6, comprise following production craft step:
1) preparation of compound resin: take by weighing resin according to the above ratio, with this ratio resin warming while stirring in reactor, 60 ℃-180 ℃ of temperature, revolution is 120-800 rev/min, be warming up to 60 ℃-180 ℃ after, the additional proportion organosilicon, constant temperature stirred 4-8 hour, left standstill 12-24 hour, and adjusted pH value 7.5-12, make compound resin;
2) nano-powder dispersion liquid preparation: take by weighing the organic salt coupling agent according to the above ratio, this ratio organic salt coupling agent liquid intensification limit in limit in reactor is stirred, 40 ℃-90 ℃ of temperature, revolution is 500-1200 rev/min, constant temperature stirs the 10-60 branch, adds nano-powder again behind adding organic solvent and the deionized water latting drown, and nano-powder must carry out heating under vacuum, the pre-treatment of drying before adding, vacuum tightness should be at 3-6Pa, 80 ℃-150 ℃ of temperature; The nano-powder dispersion liquid of adjusting, blending is at room temperature carried out sand milling, dispersion, time 4-10 hour;
3) 30～80 kilograms of zinc powders, 10～30 kilograms of aluminium powders and nano dispersion fluid are added in the compound resin, temperature 40-80 ℃, revolution is 600-1200 rev/min, time 2-4 hour;
4) after normal temperature left standstill 8-12 hour, sand milling, dispersion, filtration promptly got coating of the present invention.
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