CN101161861A - Non-chromium deactivation liquid for processing aluminium alloy and method of use thereof - Google Patents

Non-chromium deactivation liquid for processing aluminium alloy and method of use thereof Download PDF

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CN101161861A
CN101161861A CNA2007101584698A CN200710158469A CN101161861A CN 101161861 A CN101161861 A CN 101161861A CN A2007101584698 A CNA2007101584698 A CN A2007101584698A CN 200710158469 A CN200710158469 A CN 200710158469A CN 101161861 A CN101161861 A CN 101161861A
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chromium
aluminium alloy
acid
handle
free passivation
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CN100545308C (en
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刘常升
王双红
陈岁元
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Northeastern University China
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Northeastern University China
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Abstract

The present invention relates to a chrome-free passivating liquid for treating aluminum alloy and a method for using the same; the components of the passivating liquid and the weight concentration of the elements thereof consist of fluorin titanate comprising Ti (IV) between 0.05 wt percent and 0.15 wt percent, fluorin zirconate comprising Zr (IV) 0.01 wt percent and 0.05 wt percent and organic phosphate compound comprising 0.02 wt percent to saturated concentration. The use method of the passivating liquid of the invention has the following procedures: after grease on the surface of the aluminum alloy is removed, the aluminum alloy is treated by alkali cleaning, deoxidation and activation; when the temperature is between 25 DEG C and 60 DEG C and the PH value is between 3 and 3.5, the aluminum alloy is treated by impregnating or spraying for 2 min to 5 min. In the passivating liquid of the invention, organic phosphoric acid is directly added to a titanium zirconium system; the formed zirconium phosphate composite structure can obviously improve the corrosion resisting property of a passivating film and the adhesive capactiy of polymer coating (primer) on the surface of aluminum alloy.

Description

A kind of chromium-free passivation liquid and using method thereof that is used to handle aluminium alloy
Technical field
The present invention relates to a kind of chromium-free passivation liquid and using method thereof that is used to handle aluminium alloy, be specifically related to a kind of chromium-free passivation liquid and using method thereof that contains organic phosphoric acid, titanium zirconium composition.
Background technology
Traditionally, the protective treatment of aluminum alloy surface mainly is a chromating.Because of chromic salt toxicity height, environmental pollution and easily make the people carcinogenic.Along with the enhancing of environmental consciousness, the use of WEES and the strict restriction of ROHS instruction chromic salt.
In recent years, have use prospect and effect preferably chromium-free passivation liquid mainly be trivalent chromium, molybdate, rare earth cerium salt, zirconium titanium system and organosilane system.
Chromic toxicity has only about chromic 1wt%, and passivating solution is based on chromic salt.Trivalent chromium even film layer, tack are good, and its corrosion resisting property is near low chromate passivation film.But trivalent chromium is difficult to the not oxidized one-tenth sexavalent chrome of control in the passivating solution, and in use also is difficult to detect chromic concentration.So trivalent chromium is the passivating solution of main body, finally also exist the problem that contains chromium, the harm that can not fundamentally solve chromium, its use is withdrawn from the market just gradually.
Molybdenum and chromium are of the same clan, and the molybdate low toxicity, have certain advantage aspect the alternative chromate treating.Contain molybdic acid or molybdate in the passivating solution, be used with other mineral acid or salt, as phosphoric acid or salt, high violent acid or salt etc., the corrosion resisting property of passive film is better.But molybdate passive film solidity to corrosion is not as good as chromate passivation film.
Contain the oxide compound and the oxyhydroxide of cerium in the cerium salt passive film, have good solidity to corrosion, and near low chromate passivation film.But exist the treatment time long, the treatment temp height, comparatively shortcoming such as complexity also has certain distance apart from actual production.
Organosilane is to utilize Si-O-Al chemical bond and Si-O-Si network structure that aluminium alloy is played sealing process, stops and isolate corrosive medium, as Cl -Deng, improved resistance to corrosion.Simultaneously, the strong adhesive ability that has strengthened film and surface aggregate thing coating (priming paint) of Si-OH.But most of silane need alcohol as solvent, and passivating solution exists hydrolysis incomplete, poor stability and can not the vast scale dilution etc. problem.The salt spray corrosion resistance of naked film is relatively poor, and not as good as chromate passivation film, behind the coated surfaces polymeric coating, corrosion resisting property and chromic salt are suitable.
Zirconium titanium system is studied early, and is reliable, uses wider chromium-free treating liquid.The acid of the main titanium zirconium of passivating solution or salt, fluorochemical, phosphoric acid or adding organic polymer, as polyacrylic acid or fat, polyvinyl alcohol, polyethylene pyrrole Lip river alkane ketone etc.This technology can form the anti-corrosion passive film of one deck in aluminum alloy surface.Its anti-corrosion capability is approaching with chromic salt, is extensive use of on market.But also exist the passivating solution poor stability and with defective such as the sticking power of surface aggregate thing coating (priming paint) is undesirable.
In recent years, organic phosphoric acid can and generate P-O-Me chemical combination strong (Me is a metal) and can generate the P-O-C covalent linkage with the reaction of surface aggregate thing coating (priming paint) with metal chelating, became a kind of new chromium-free treatment technology.Organic phosphoric acid can more closely combine metallic matrix and surface aggregate thing coating (priming paint), strengthened the sticking power of coating to metal, the covalent linkage of phosphoric acid salt and organism formation simultaneously can play the chromic salt sealing process of conventional phosphatizing technology aftertreatment, makes coating have better corrosion resisting property.Azusa in the self-assembly of aluminium alloy AL1100 surface 1, the two phosphonic acids bonded multilayer zirconium phosphate films of 12-dodecyl, salt mist experiment reaches 48h.US 6436475 B1 of U.S. Chemetall house journal handle aluminum alloy surface with organic phosphoric acid, have obtained the phosphoric acid film of corrosion resisting property and adhesion performance preferably, but must use simultaneously with polymeric coating (priming paint).Another patent US 6488990 B1 of Chemetall company carry out sealing treatment with organic phosphoric acid to titanium zirconium film, have improved the sticking power of aluminium alloy and polymeric coating widely, but adopt for two steps handled respectively, have increased treatment step.
Summary of the invention
The objective of the invention is the problem at the prior art existence, a kind of chromium-free passivation liquid is provided, can form uniform passive film in aluminum alloy surface, this passive film has good corrosion resistance energy and the good sticking power of surface aggregate thing coating (priming paint).On using method, provide a kind of operation easy in short-term, energy-saving and cost-reducing environment-friendly type technique, to satisfy the industrial production requirement.
The technical solution used in the present invention is: its component of chromium-free passivation liquid is made up of the fluorine zirconic acid and the organic phosphoric acid compound of the hydrofluotitanic acid that contains Ti (IV) element, Zr (IV) element; Feature is that composition weight concentration content Ti (IV) is 0.05~0.15wt%, and Zr (IV) is 0.01~0.05wt%, and the organic phosphoric acid compound is that 0.02wt% is to saturation concentration.The passivating solution pH value is 3~3.5.
Above-mentioned organic phosphoric acid compound is selected Amino Trimethylene Phosphonic Acid, 2-phosphonic acids butane-1,2 for use, 4 tricarboxylic acid, 1,12-dodecyl bisphosphate, 2-hydroxyethylidene diphosphonic acid guanidine-acetic acid.Use 1 the branchiess alkylphosphonic acid carboxylic acid of long linear on a selective basis to twelve carbon atom.
The adjusting of passivating solution pH value, to select ammonium hydroxide for use be ammoniacal liquor, as conditioning agent.
The chromium-free passivation liquid of above-mentioned composition is used to handle the using method of aluminium alloy, carries out as follows:
(1) removes the grease of aluminum alloy surface;
(2) with aluminum alloy surface alkali cleaning, deoxidation activation;
(3) with the chromium-free passivation liquid for preparing aluminium alloy is flooded or spray processing, controlled temperature is 25~60 ℃, and the time is 2~5 minutes;
(4) be under 90~150 ℃ in temperature at last, dry 10~30 minutes.
The aluminum alloy surface alkali cleaning is to handle 2~5 minutes down at 25~60 ℃, uses the tap water rinsing at last.Alkaline wash is selected sodium hydroxide or the 2wt% sodium salt compositional liquor that contains 2wt% for use.The sodium salt compositional liquor is by 7wt% yellow soda ash, the 40wt% sodium pyrophosphate, and 23wt% sodium sulfate, the 15wt% sodium laurylsulfonate, the 13wt% water glass, 2wt% dodecyl phenol polyethenoxy ether is formed.
The deoxidation activation is the nonionogenic tenside that adopts sulfuric acid (concentration 98wt%), 0.01wt% hydrogen fluoride (concentration 40wt%) and the 0.2wt% of 1wt%, at room temperature handles 1~2 minute, then with distilled water or rinsed with deionized water.Nonionogenic tenside is made up of 1: 1 fatty alcohol-polyoxyethylene ether of mass ratio and polyoxyethylene nonylphenol ether.
The present invention is with respect to prior art, and its advantage and significant benefit are as follows: passivating solution of the present invention has not only alleviated environmental pollution greatly owing to do not contain chromic salt, satisfies the requirement of WEES and ROHS instruction.
The cost of material that passivating solution of the present invention adopts is cheap, and treatment process is simple.
Passivating solution of the present invention is the titanium zirconium system that directly organic phosphoric acid joined.Organic phosphoric acid elder generation and Zr 4+Reaction forms the zirconium phosphate composite structure, utilizes to generate P-O-Me chemical combination key and matrix bond, forms Al-P-Zr-P structure and Al in aluminum alloy surface at last 2O 3-TiO 2Composite membrane.The zirconium phosphate composite structure that forms can improve significantly passive film corrosion resisting property and with the adhesive ability of surface aggregate thing coating (priming paint).
The passive film corrosion resisting property that is formed by passivating solution of the present invention is good, and is good with surface aggregate thing coating (priming paint) sticking power.
Specific examples
Embodiment 1
The configuration of passivating solution:
Select commercially available hydrofluotitanic acid (40wt%) and fluorine zirconic acid (45wt%) and Amino Trimethylene Phosphonic Acid (50wt%) preparation passivating solution for use.Take by weighing hydrofluotitanic acid 5.6 gram, fluorine zirconic acid 1.2 grams, Amino Trimethylene Phosphonic Acid 0.4 gram is dissolved in 1 liter of distilled water or the deionized water, and to regulate pH value with ammoniacal liquor be 3~3.5, and at room temperature natural reaction used after 1 day.Contain Ti in this passivating solution 4+Concentration is 0.065wt%, Zr 4+Concentration is 0.024wt%, and Amino Trimethylene Phosphonic Acid concentration is 0.02wt%.
Treatment process:
(1) the AA6061 aluminium alloy is removed surperficial grease with acetone, clean with the tap water rinsing;
(2) alkali cleaning is to handle 5 minutes down in 25 ℃ with the 2wt% sodium hydroxide solution, and is clean with the tap water rinsing;
(3) in acid liquid, contain 1wt% sulfuric acid, 0.01wt% hydrogen fluoride and 2wt% nonionogenic tenside (fatty alcohol-polyoxyethylene ether of 1: 1 mass ratio and polyoxyethylene nonylphenol ether) deoxidation activation treatment 1.5 minutes under room temperature, use rinsed with deionized water;
(4) aluminium alloy be impregnated in 60 ℃ the passivating solution 2 minutes, rinsed with deionized water;
Drying is 15 minutes under (5) 150 ℃.
Can form the passive film of pearl opal in aluminum alloy surface by above-mentioned processing, carry out corrosion-resistant test according to GB/T10125-97 " artificial atmosphere corrosion test-salt-fog test ", neutral salt spray test can reach 72 hours.At room temperature spray commercially available priming paint (Ai Erfu ES400).Carry out the paint film adhesion test according to GB1720-79 " paint film adhesion assay method ", sticking power can reach 1 grade.
Embodiment 2
The configuration of passivating solution:
Select commercially available hydrofluotitanic acid (40wt%) and fluorine zirconic acid (45wt%) and Amino Trimethylene Phosphonic Acid (50wt%) preparation passivating solution for use.Take by weighing hydrofluotitanic acid 8.56 gram, fluorine zirconic acid 2.52 grams, Amino Trimethylene Phosphonic Acid 1 gram is dissolved in 1 liter of distilled water or the deionized water, and to regulate pH value with ammoniacal liquor be 3~3.5, and at room temperature natural reaction used after 1 day.Contain Ti in this passivating solution 4+Concentration is 0.1wt%, Zr 4+Concentration is that the concentration of 0.05wt%, Amino Trimethylene Phosphonic Acid is 0.1wt%.
Its treatment process is with embodiment 1, and difference is that 2wt% sodium salt compositional liquor (7wt% yellow soda ash, 40wt% sodium pyrophosphate are adopted in alkali cleaning, 23wt% sodium sulfate, 15wt% sodium laurylsulfonate, 13wt% water glass, 2wt% dodecyl phenol polyethenoxy ether), handled 2 minutes down at 60 ℃.The deoxidation activation treatment is 2 minutes after the alkali cleaning.The passivating solution for preparing was sprayed 5 minutes aluminium alloy under 25 ℃, and drying is 30 minutes under 90 ℃.
The anti-neutral salt spray test of passive film can reach 72 hours.Sticking power can reach 1 grade.
Embodiment 3
The configuration of passivating solution:
Select commercially available hydrofluotitanic acid (40wt%) and fluorine zirconic acid (45wt%) and 2-phosphonic acid butane-1,2 for use, 4-tricarboxylic acid (50wt%) preparation passivating solution.Take by weighing hydrofluotitanic acid 11.2 gram, fluorine zirconic acid 2.4 grams, 2-phosphonic acid butane-1,2,4-tricarboxylic acid 0.8 gram is dissolved in 1 liter of distilled water or the deionized water, and to regulate pH value with ammoniacal liquor be 3~3.5, and at room temperature natural reaction used after 1 day.Contain Ti in this passivating solution 4+Concentration is 0.13%, Zr 4+Concentration is 0.048%, 2-phosphonic acid butane-1,2, and 4-tricarboxylic acid concentration is 0.04%.
Other treatment process is with embodiment 1, and difference is that alkali cleaning was handled 3 minutes down at 40 ℃; The passivating solution for preparing was flooded 3 minutes aluminium alloy under 40 ℃, and drying is 20 minutes under 130 ℃.
The anti-neutral salt spray test of passive film can reach 72 hours.Sticking power can reach 1 grade.
Embodiment 4
The configuration of passivating solution:
Select commercially available hydrofluotitanic acid (40wt%) and fluorine zirconic acid (45wt%) and 1 for use, 12-dodecyl bisphosphate preparation passivating solution.Take by weighing 40% hydrofluotitanic acid, 5.6 grams, 45% fluorine zirconic acid 1.2 grams, 1,12-dodecyl bisphosphate 0.4 gram is dissolved in 1 liter of distilled water or the deionized water, and to regulate pH value with ammoniacal liquor be 3~3.5, and at room temperature natural reaction used after 1 day.Contain Ti in this passivating solution 4+Concentration is 0.065wt%, Zr 4+Concentration is 0.024wt%, 1, and the concentration of 12-dodecyl bisphosphate is 0.04wt%.
Treatment process is with embodiment 1.
The anti-neutral salt spray test of passive film can reach 72 hours.Sticking power can reach 1 grade.
Embodiment 5
The configuration of passivating solution:
Select commercially available hydrofluotitanic acid (40wt%) and fluorine zirconic acid (45wt%) and 2-hydroxyethylidene diphosphonic acid guanidine-acetic acid (50wt%) preparation passivating solution for use.Take by weighing hydrofluotitanic acid 8.56 gram, fluorine zirconic acid 2.52 grams, 2-hydroxyethylidene diphosphonic acid guanidine-acetic acid 0.4 gram is dissolved in 1 liter of distilled water or the deionized water, and to regulate pH value with ammoniacal liquor be 3~3.5, and at room temperature natural reaction used after 1 day.Contain Ti in this passivating solution 4+Concentration is 0.1wt%, Zr 4+Concentration is that the concentration of 0.05wt%, 2-hydroxyethylidene diphosphonic acid guanidine-acetic acid is 0.04wt%.
Treatment process is with embodiment 1.
The anti-neutral salt spray test of passive film can reach 72 hours.Sticking power can reach 1 grade.

Claims (10)

1. chromium-free passivation liquid that is used to handle aluminium alloy, its component is made up of the fluorine zirconic acid and the organic phosphoric acid compound of the hydrofluotitanic acid that contains Ti (IV) element, Zr (IV) element, it is characterized in that composition weight concentration content Ti (IV) is 0.05~0.15wt%, Zr (IV) is 0.01~0.05wt%, the organic phosphoric acid compound be 0.02wt% to saturation concentration, the passivating solution pH value is 3~3.5.
2. according to the described chromium-free passivation liquid that is used to handle aluminium alloy of claim 1, it is characterized in that the organic phosphoric acid compound selects Amino Trimethylene Phosphonic Acid, 2-phosphonic acids butane-1,2 for use, 4 tricarboxylic acid, 1,12-dodecyl bisphosphate, 2-hydroxyethylidene diphosphonic acid guanidine-acetic acid.
3. according to claim 1 or the 2 described chromium-free passivation liquids that are used to handle aluminium alloy, it is characterized in that the organic phosphoric acid compound is selected to select 1 the branchiess alkylphosphonic acid carboxylic acid of long linear earlier for use to twelve carbon atom.
4. according to the described chromium-free passivation liquid that is used to handle aluminium alloy of claim 1, it is characterized in that the adjusting of passivating solution pH value selects for use ammonium hydroxide as conditioning agent.
5. using method that is used to handle the chromium-free passivation liquid of aluminium alloy is characterized in that carrying out as follows:
(1) removes the grease of aluminum alloy surface;
(2) with aluminum alloy surface alkali cleaning, deoxidation activation;
(3) with the chromium-free passivation liquid for preparing aluminium alloy is flooded or spray processing, controlled temperature is 25~60 ℃, and the time is 2~5 minutes;
(4) be under 90~150 ℃ in temperature at last, dry 10~30 minutes.
6. the using method that is used to handle the chromium-free passivation liquid of aluminium alloy according to claim 5, it is characterized in that its component of chromium-free passivation liquid and the weight concentration that prepare are the hydrofluotitanic acids that contains Ti (IV) 0.05~0.15wt%, contain the fluorine zirconic acid of Zr (IV) 0.01~0.05wt% and contain the organic phosphoric acid compound of 0.02wt% to saturation concentration.
7. the using method that is used to handle the chromium-free passivation liquid of aluminium alloy according to claim 5 is characterized in that alkali cleaning is to handle 2~5 minutes down at 25~60 ℃, uses the tap water rinsing at last; Alkaline wash is selected the sodium hydroxide that contains 2wt% or the sodium salt compositional liquor of 2wt% for use.
8. the using method that is used to handle the chromium-free passivation liquid of aluminium alloy according to claim 7, it is characterized in that the sodium salt compositional liquor is by 7wt% yellow soda ash, the 40wt% sodium pyrophosphate, 23wt% sodium sulfate, the 15wt% sodium laurylsulfonate, the 13wt% water glass, 2wt% dodecyl phenol polyethenoxy ether is formed.
9. the using method that is used to handle the chromium-free passivation liquid of aluminium alloy according to claim 5, it is characterized in that deoxygenated adopts by sulfuric acid 0.01wt% hydrogen fluoride that contains 1wt% and the nonionogenic tenside of 0.2wt%, at room temperature handled 1~2 minute, then with distilled water or rinsed with deionized water.
10. the using method that is used to handle the chromium-free passivation liquid of aluminium alloy according to claim 9 is characterized in that described non-ionic surface activator is made up of fatty alcohol-polyoxyethylene ether and polyoxyethylene nonylphenol ether, and its mass ratio is 1: 1.
CNB2007101584698A 2007-11-22 2007-11-22 A kind of chromium-free passivation liquid and using method thereof that is used to handle aluminium alloy Expired - Fee Related CN100545308C (en)

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