CN104178758A - Chromate-free passivation method for aluminum and aluminum alloy - Google Patents
Chromate-free passivation method for aluminum and aluminum alloy Download PDFInfo
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- CN104178758A CN104178758A CN201410476055.XA CN201410476055A CN104178758A CN 104178758 A CN104178758 A CN 104178758A CN 201410476055 A CN201410476055 A CN 201410476055A CN 104178758 A CN104178758 A CN 104178758A
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Abstract
The invention relates to a chromate-free passivation method for aluminum and aluminum alloy. According to the chromate-free passivation method, the surface of aluminum or aluminum alloy contacts a chromate-free passivation liquid, and the chromate-free passivation liquid comprises (a) titanate, (b) zirconate, (c) modified organic silicon resin, (d) novolac epoxy resin, (e) type-II metallic compounds and (f) citric acid. By adopting the method, a uniform converted coating can be generated on sediment of the aluminum and aluminum alloy, the coating is excellent in corrosion resistance, and the time for generating white corrosive products is delayed. The chromate-free passivation method provided by the invention is low in cost, simple to operate and relatively high in environment-friendly value.
Description
Technical field
The present invention relates to metal surface treatment technology, particularly, the present invention relates to a kind of aluminum and its alloy chromium-free deactivation method and chromium-free passivation liquid.
Background technology
Aluminium surface treatment is a professional technique that relates to a lot of fields, comprises automobile, motorcycle, space flight and aviation, household electrical appliance, electronics, building materials, universal metal processing.Wherein, chemical conversion film is a kind of technique means the most frequently used in aluminium surface treatment.Chemical conversion film has certain erosion resistance and good physical adsorption ability, can greatly improve the bonding force of aluminium matrix and coating, strengthens the resistance to corrosion of aluminum products, and its processing speed soon, does not consume electric energy, required equipment is simple, processing cost is low.At present, the method for comparatively common chemical conversion film has three kinds:
1, chromaking: this method was in mountain american chemical paint company invention in 1945, and also referred to as A Luoding oxidation style, Hou You Britain ICI Imperial Chemical Industries promotes the use of, and claims A Luo Crow nurse method.Its main component is: take chromic anhydride as oxygenant and membrane-forming agent, and the additive such as fluorochemical in addition, film forming is fine and close chromic salt, has good erosion resistance.But the formed conversion film of this method, contains sexavalent chrome, can cause serious harm to human body, also can cause severe contamination to environment.
2, phosphorus chromaking: claim again green chromaking, phosphorus chromaking was just brought into use in aluminium surface treatment as far back as 1945, so far, still in use.Phosphorus chromaking film comes from trivalent chromium, and its main component is: superphosphate, acidity or basic chromium hydrochlorate, complexing agent, fluorochemical.The difference of this method and chromaking method is that phosphoric acid salt has substituted chromic salt, has reduced pollution, and in technique, has simplified the operation of acid deoxidation effect.But in this method, phosphorus chromaking film erosion resistance, not as chromaking film, is received certain restriction so use, and, chromic pollution do not departed from completely yet.
The U.S. the 5th, 380,374,5,952,049 and 6,038, No. 309 patents disclose the acidic solution of use Han IV family's metallic compound (comprising titanium), together with oxygen anion in the situation that of floride-free compound ion for form conversion coating on aluminium and alloy, magnesium and ferrous metal.The U.S. the 6th, 059,867,5,951,747,5,728,233 and 5,584, No. 946 patents disclose the acidic solution of use Han IV family's metallic compound (comprising titanium), link and form conversion coating on aluminium and alloy thereof with phosphoric acid salt and relevant ions.The U.S. the 6th, 206, No. 982 patents disclose a kind of rare earth element that utilizes and on aluminium, have formed the method for conversion coating as cerium.These inventions are generally used for producing cementability undercoat, and it provides painting good cementability.Foregoing invention is not suitable for zinc or the zinc alloy settling electroplated conventionally, and its decorative appearance and erosion resistance are particularly importants.
The U.S. the 6th, 217,674,5,449,414 and 5,342, No. 456 patents disclose uses IV family metallic compound in water-soluble organic polymer dispersion liquid.These compositions are coated on metal objects by dipping or spraying technology.The organic polymer coating applying in this way tends to inhomogeneous, and for various commercial purposes, this is undesirable.
CN1260391C discloses a kind of composition and method that does not contain chromium, for improving the erosion resistance of zinc or zinc alloy surface.The source that said composition contains a kind of titanium ion or titanate, a kind of oxygenant and fluorochemical or complex fluorides.Said composition preferably contains a kind of organic acid and/or a kind of Ⅱ family metallic compound, is preferably Ⅱ family metallic compound.
CN102181853 A relates to a kind for the treatment of solution for aluminum alloy surface passivation, material by following mass percent forms: the mixture 20-30% of potassium titanate, sodium titanate and metatitanic acid magnesium salts, the mixture 5-15% of potassium zirconium, sodium zirconate and zirconic acid magnesium salts, modified organic silicone resin 5-15%, and urethane resin 40-50%.Novel treatment fluid for chromium-free passivation of aluminum alloy of the present invention, be specifically designed to the surface treatment of aluminium and alloy thereof, magnesium and alloy thereof, not only can improve the erosion resistance of material itself, and can strengthen the sticking power of material and its coating, there is the advantages such as operation is simple, cost is low, pollution-free.
The chromium-free deactivation method of aluminum and its alloy described in the prior art, or after passivation, effect is bad, erosion resistance can not meet application request, or because chromium-free passivation liquid cost of material is higher, cost is higher, is not easy to mass-producing application.
Summary of the invention
One of object of the present invention is to provide a kind of chromium-free deactivation method of aluminum and its alloy, strong by the aluminum and its alloy erosion resistance after described method passivation, and cost is low, is convenient to commercial applications.
In order to achieve the above object, the present invention has adopted following technical scheme:
Described aluminum and its alloy chromium-free deactivation method is by contacting described aluminum or aluminum alloy surface with a kind of chromium-free passivation liquid, described chromium-free passivation liquid contains:
A) in the titanate 10～20g/L of titanium content;
B) zirconate 1～5g/L;
C) modified organic silicone resin 5～10g/L;
D) novolac epoxy 1～5g/L;
E) the metallic compound 1～10g/L of II family;
F) citric acid 1～15g/L.
The content of described titanate is for example 10.5g/L, 11g/L, 11.5g/L, 12g/L, 12.5g/L, 13g/L, 13.5g/L, 14g/L, 14.5g/L, 15g/L, 15.5g/L, 16g/L, 16.5g/L, 17g/L, 17.5g/L, 18g/L, 18.5g/L, 19g/L or 19.5g/L.
The content of described zirconate is for example 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L or 4.5g/L.
The content of described modified organic silicone resin is for example 5.5g/L, 6g/L, 6.5g/L, 7g/L, 7.5g/L, 8g/L, 8.5g/L, 9g/L or 9.5g/L.
The content of described novolac epoxy is for example 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L or 4.5g/L.
The content of described II family metallic compound is for example 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L, 4.5g/L, 5g/L, 5.5g/L, 6g/L, 6.5g/L, 7g/L, 7.5g/L, 8g/L, 8.5g/L, 9g/L or 9.5g/L.
The content of described citric acid is for example 2g/L, 3g/L, 4g/L, 5g/L, 6g/L, 7g/L, 8g/L, 9g/L, 10g/L, 11g/L, 12g/L, 13g/L or 14g/L.
Make us finding uncannily, chromium-free deactivation method of the present invention can produce blueness or polychromatic finish on aluminum and its alloy settling, has improved the corrosion resistance nature of aluminum and its alloy.
Preferably, described chromium-free passivation liquid comprises:
A) in the titanate 12～20g/L of titanium content;
B) zirconate 1.5～5g/L;
C) modified organic silicone resin 6～10g/L;
D) novolac epoxy 1.5～5g/L;
E) the metallic compound 2～10g/L of II family;
F) citric acid 2～15g/L.
Preferably, described chromium-free passivation liquid comprises:
A) in the titanate 14～20g/L of titanium content;
B) zirconate 2～5g/L;
C) modified organic silicone resin 7～10g/L;
D) novolac epoxy 2～5g/L;
E) the metallic compound 3～10g/L of II family;
F) citric acid 4～15g/L.
Described titanate is selected from the mixture of a kind of in potassium titanate, sodium titanate, magnesium titanate or at least two kinds, described mixture is the mixture of magnesium titanate and sodium titanate for example, the mixture of potassium titanate and magnesium titanate, the mixture of sodium titanate and potassium titanate, the mixture of magnesium titanate, sodium titanate and potassium titanate, preferably potassium titanate, sodium titanate and magnesium titanate three's mixture.
Described zirconate is selected from the mixture of a kind of in potassium zirconium, magnesium zirconate, sodium zirconate or at least two kinds, described mixture is the mixture of sodium zirconate and magnesium zirconate for example, the mixture of magnesium zirconate and potassium zirconium, the mixture of sodium zirconate and potassium zirconium, the mixture of sodium zirconate, magnesium zirconate and potassium zirconium, preferably potassium zirconium, magnesium zirconate and sodium zirconate three's mixture.
Described modified organic silicone resin is selected from epoxy resin modified organosilicon resin, vibrin modified organic silicone resin, urethane resin modified organic silicone resin, acrylic resin modified organic silicone resin, the mixture of a kind of in Synolac modified organic silicone resin or at least two kinds, described mixture is the mixture of Synolac modified organic silicone resin and acrylic resin modified organic silicone resin for example, the mixture of urethane resin modified organic silicone resin and vibrin modified organic silicone resin, the mixture of epoxy resin modified organosilicon resin and Synolac modified organic silicone resin, the mixture of acrylic resin modified organic silicone resin and urethane resin modified organic silicone resin, the mixture of vibrin modified organic silicone resin and epoxy resin modified organosilicon resin, the mixture of Synolac modified organic silicone resin and urethane resin modified organic silicone resin, the mixture of acrylic resin modified organic silicone resin and vibrin modified organic silicone resin, Synolac modified organic silicone resin, the mixture of acrylic resin modified organic silicone resin and urethane resin modified organic silicone resin, vibrin modified organic silicone resin, the mixture of epoxy resin modified organosilicon resin and Synolac modified organic silicone resin, acrylic resin modified organic silicone resin, urethane resin modified organic silicone resin, the mixture of vibrin modified organic silicone resin and epoxy resin modified organosilicon resin, Synolac modified organic silicone resin, acrylic resin modified organic silicone resin, the mixture of urethane resin modified organic silicone resin and vibrin modified organic silicone resin, preferred epoxy modified organic silicone resin and/or polyurethane-modified silicone resin.Preparation method those skilled in the art of described Synolac modified organic silicone resin, acrylic resin modified organic silicone resin, urethane resin modified organic silicone resin, vibrin modified organic silicone resin and epoxy resin modified organosilicon resin can prepare with reference to the disclosed method of prior art, for example can be with reference to periodical literature (Qin Liang, Chen Qi, Ni Lizhong, silicone resin method of modifying, glass reinforced plastic, 2003,4:12-15) prepare organic-silicon-modified resin.
The present invention adopts epoxy resin to substitute urethane resin of the prior art.Epoxy resin can reach the performance identical with urethane, more but the price of epoxy resin reduces compared with the price of urethane, makes cost.Add, the toxicity of urethane is larger, therefore, selects epoxy resin environment protecting better.Concrete selection the present invention contrast of described epoxy resin is not restricted, and for example described epoxy resin can be selected epoxy resin-12, epoxy resin-13, epoxy resin-16, epoxy resin-20 and epoxy resin 6101.Above-mentioned epoxy resin is all available commercially.
Chromium-free passivation liquid of the present invention, is acidic liquid, can make aluminium workpiece slightly dissolve, owing to having consumed hydrogen ion at this dissolution process, thereby make near pH value treatment solution and aluminium workpiece interface increase, and then cause zirconium and titanyl compound to be separated out, be attached to aluminium workpiece surface; Meanwhile, by the effect of coordination compound, the modified organic silicone resin in treatment solution and epoxy resin fat are combined with above-mentioned precipitate, thereby are attached on aluminium workpiece surface, and last, the surface of aluminium workpiece has formed one deck conversion film.
The most preferred method of coating chromium-free passivation liquid is that pending parts are immersed in chromium-free passivation liquid.Yet, other contact methods as spraying or conveying belt flash also can accept.Can be the scope of approximately 10 seconds to 5 minutes the duration of contact between chromium-free passivation liquid and pending parts.Treated parts shift out from composition, and water cleans, then dry.
Can apply additional top coat if silicate, light-cured resin and combination thereof are further to improve outward appearance and/or the erosion resistance of parts.The top coat that these are additional and coating method thereof are well known in the art.
" comprising " of the present invention, mean it except described component, can also comprise other components, these other components give described chromium-free passivation liquid different characteristics.In addition, " comprising " of the present invention, can also replace with enclosed " being " or " by ... form ".
Chromium-free passivation liquid of the present invention for example can also add urethane, the content of described urethane is 1～10g/L, for example 1.5g/L, 2g/L, 2.5g/L, 3g/L, 3.5g/L, 4g/L, 4.5g/L, 5g/L, 5.5g/L, 6g/L, 6.5g/L, 7g/L, 7.5g/L, 8g/L, 8.5g/L, 9g/L or 9.5g/L.
The preparation method of chromium-free passivation liquid of the present invention is: by above-mentioned formula, each material is mixed, in erosion resistance container, stir until evenly, then filter and can obtain chromium-free passivation liquid.
The aluminum and its alloy obtaining by chromium-free deactivation method of the present invention, not only can improve the erosion resistance of material itself, and can strengthen the sticking power of material and its coating, has the advantages such as operation is simple, cost is low, pollution-free.
By being determined in neutral salt spray booth, forming the erosion resistance (according to ASTM B-117) that white abrasion product required time is evaluated conversion coating, there is white corrosion thing for 350 hours in aluminum component first.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
Fill a prescription as described below each material is mixed, in erosion resistance container, stir until evenly, then filter and can obtain chromium-free passivation liquid.
Described chromium-free passivation liquid comprises:
A) in the titanate 10g/L of titanium content;
B) zirconate 1g/L;
C) modified organic silicone resin 5g/L;
D) novolac epoxy 1g/L;
E) the metallic compound 1g/L of II family;
F) citric acid 1g/L.
First with acid or neutral scavenging solution, clean aluminum component surface, remove greasy dirt and the dust on aluminum component surface; Water cleans other impurity of aluminum component remained on surface again; Then, then carry out passivation with the passivating solution described in embodiment 1, on aluminum component surface, form one deck conversion film coating, last water and washed with de-ionized water aluminium material surface.
Embodiment 2
Fill a prescription as described below each material is mixed, in erosion resistance container, stir until evenly, then filter and can obtain chromium-free passivation liquid.
Described chromium-free passivation liquid comprises:
A) in the titanate 20g/L of titanium content;
B) zirconate 5g/L;
C) modified organic silicone resin 10g/L;
D) novolac epoxy 5g/L;
E) the metallic compound 10g/L of II family;
F) citric acid 15g/L.
First with acid or neutral scavenging solution, clean aluminum component surface, remove greasy dirt and the dust on aluminum component surface; Water cleans other impurity of aluminum component remained on surface again; Then, then carry out passivation with the passivating solution described in embodiment 2, on aluminum component surface, form one deck conversion film coating, last water and washed with de-ionized water aluminium material surface.
Embodiment 3
Fill a prescription as described below each material is mixed, in erosion resistance container, stir until evenly, then filter and can obtain chromium-free passivation liquid.
Described chromium-free passivation liquid comprises:
A) in the titanate 15g/L of titanium content;
B) zirconate 3g/L;
C) modified organic silicone resin 7g/L;
D) novolac epoxy 3g/L;
E) the metallic compound 5g/L of II family;
F) citric acid 8g/L.
First with acid or neutral scavenging solution, clean aluminum component surface, remove greasy dirt and the dust on aluminum component surface; Water cleans other impurity of aluminum component remained on surface again; Then, then carry out passivation with the passivating solution described in embodiment 3, on aluminum component surface, form one deck conversion film coating, last water and washed with de-ionized water aluminium material surface.
Embodiment 4
Fill a prescription as described below each material is mixed, in erosion resistance container, stir until evenly, then filter and can obtain chromium-free passivation liquid.
Described chromium-free passivation liquid comprises:
A) in the titanate 14g/L of titanium content;
B) zirconate 4g/L;
C) modified organic silicone resin 8g/L;
D) novolac epoxy 4g/L;
E) the metallic compound 7g/L of II family;
F) citric acid 10g/L.
First with acid or neutral scavenging solution, clean aluminum component surface, remove greasy dirt and the dust on aluminum component surface; Water cleans other impurity of aluminum component remained on surface again; Then, then carry out passivation with the passivating solution described in embodiment 4, on aluminum component surface, form one deck conversion film coating, last water and washed with de-ionized water aluminium material surface.
By being determined in neutral salt spray booth, forming the erosion resistance (according to ASTM B-117) that white abrasion product required time is evaluated conversion coating, there is white corrosion thing for 350 hours in aluminum component first.
By being determined in neutral salt spray booth, form the erosion resistance (according to ASTM B-117) that white abrasion product required time is evaluated conversion coating, embodiment 1-4 under equal conditions as above tests, and test result is as shown in table 1:
Table 1. embodiment 1-4 and comparative example 1-2 erosion resistance test result
Should be noted that and understand, in the situation that not departing from the desired the spirit and scope of the present invention of accompanying claim, can make various modifications and improvement to the present invention of foregoing detailed description.Therefore, the scope of claimed technical scheme is not subject to the restriction of given any specific exemplary teachings.
Applicant's statement, the present invention illustrates detailed method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed method, does not mean that the present invention must rely on above-mentioned detailed method and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to the selection of the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (6)
1. an aluminum and its alloy chromium-free deactivation method, is characterized in that, described method is by contacting described aluminum or aluminum alloy surface with a kind of chromium-free passivation liquid, and described chromium-free passivation liquid comprises:
A) in the titanate 10～20g/L of titanium content;
B) zirconate 1～5g/L;
C) modified organic silicone resin 5～10g/L;
D) novolac epoxy 1～5g/L;
E) the metallic compound 1～10g/L of II family;
F) citric acid 1～15g/L.
2. the method for claim 1, is characterized in that, described chromium-free passivation liquid comprises:
A) in the titanate 12～20g/L of titanium content;
B) zirconate 1.5～5g/L;
C) modified organic silicone resin 6～10g/L;
D) novolac epoxy 1.5～5g/L;
E) the metallic compound 2～10g/L of II family;
F) citric acid 2～15g/L.
3. method as claimed in claim 1 or 2, is characterized in that, described chromium-free passivation liquid comprises:
A) in the titanate 14～20g/L of titanium content;
B) zirconate 2～5g/L;
C) modified organic silicone resin 7～10g/L;
D) novolac epoxy 2～5g/L;
E) the metallic compound 3～10g/L of II family;
F) citric acid 4～15g/L.
4. the method as described in one of claim 1-3, is characterized in that, described titanate is selected from the mixture of a kind of in potassium titanate, sodium titanate, magnesium titanate or at least two kinds, preferably potassium titanate, sodium titanate and magnesium titanate three's mixture.
5. the method as described in one of claim 1-4, is characterized in that, described zirconate is selected from the mixture of a kind of in potassium zirconium, magnesium zirconate, sodium zirconate or at least two kinds, preferably potassium zirconium, magnesium zirconate and sodium zirconate three's mixture.
6. the method as described in one of claim 1-5, it is characterized in that, described modified organic silicone resin is selected from mixture, preferred epoxy modified organic silicone resin and/or the polyurethane-modified silicone resin of a kind of in epoxy resin modified organosilicon resin, vibrin modified organic silicone resin, urethane resin modified organic silicone resin, acrylic resin modified organic silicone resin, Synolac modified organic silicone resin or at least two kinds.
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| CN111575695A (en) * | 2020-05-11 | 2020-08-25 | 四川中德铝业有限公司 | Modified aluminum profile with good corrosion prevention effect and preparation method thereof |
| CN115584496A (en) * | 2022-10-25 | 2023-01-10 | 福建省长汀金龙稀土有限公司 | Surface treatment method for permanent magnet, permanent magnet and protective film thereof |
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