CN102312234A - Passivating solution for plated metal - Google Patents
Passivating solution for plated metal Download PDFInfo
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- CN102312234A CN102312234A CN201110319734A CN201110319734A CN102312234A CN 102312234 A CN102312234 A CN 102312234A CN 201110319734 A CN201110319734 A CN 201110319734A CN 201110319734 A CN201110319734 A CN 201110319734A CN 102312234 A CN102312234 A CN 102312234A
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- molybdate
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Abstract
The invention relates to a chromium-free passivating solution for plated metal and a plating method thereof. The passivating solution comprises 0.001 to 30 g/L of vanadate and 0.01 to 30 g/L of molybdate, and can further comprise an aqueous solution of one or more selected from the group consisting of 1 to 300 g/L of phytic acid, 0.01 to 30 g/L of silane and 1 to 500 g/L of a resin. The passivating solution can be used for plated metal through immersion, spraying, roller coating or brush painting and forms a replacing layer and/or a covering layer on the surface of treated metal, which enables surface anti-corrosion performance of treated metal to be effectively enhanced; in addition, the passivating solution provided in the invention does not contain environment-polluting chromium of any valence state, which is beneficial for environmental protection.
Description
Technical field
The present invention relates to protection liquid and method of use thereof after plate the metallic surface, more specifically, the present invention relates to is a kind of metal-plated post-passivation liquid and method of use thereof that does not contain chromium.
Background technology
After the metal-plated (present surface treatment has plating, hot dip process etc.), be exposed in the air in the middle of the storage transportation or when using, because atmospheric moisture and variation of temperature; Can form dewfall at coating surface; Cause metal to get rusty or variable color, influence the rustless property of product appearance, in order to prevent this corrosion of coating; Behind the coating of metallic surface, need carry out Passivation Treatment to its overlay coating.
Traditional Passivation Treatment adopts sexavalence or tervalent chromic salt to form one deck passive film at coating surface usually; This film has good isolation performance and self-repair function; Have good corrosion-resisting function, have technology simple, fast, cost is low, passivation can onlinely be carried out; Advantages such as the adhesion property that the passivation product paints in the later stage application course of processing is good are conventional at present passivating methods.But its contained chromium ion all has great harm to environment and human body, and use is restricted.European Union on January 27th, 2003 through ROHS instruction, regulation exports to the steel plate galvanized that bans use of chromating in the electric equipment products of European Union.Other countries and regions are also imitated one after another and have been put into effect corresponding decree, rules.Therefore, each state is divided into three major types: inorganic passivation, organic passivation and inorganic organic mixing passivation basically all at the product of research substitute chromium hydrochlorate in the world at present.
High-valency metal salt such as molybdate, tungstate, silicate etc. are mainly adopted in inorganic passivation; CN101886259A discloses a kind of Zinc coat environmental-friendly passivation solution that is used for; Raw materials such as Sodium orthomolybdate, sodium wolframate, titanyl sulfate have wherein just been adopted; Its advantage is high temperature resistant, anti-fingerprint, but its erosion resistance is relatively poor.
Organic passivation is main with water soluble organic substance mainly, and like phytic acid, Weibull, organic huge legendary turtle compound, vinyl resin and epoxy resin etc., its advantage is that erosion resistance improves, but high thermal resistance and anti-finger printing are relatively poor.
Inorganic organic mixing passivation mainly is to add dissolved organic matter in the inorganic salt salt, to reach high corrosion resistance.A kind of chromium-free passivation liquid that is used for galvanized steel sheet surface is disclosed like CN 101235498A; Its component and compound method: molybdate: 80～160g/L, tungstate: 16～32g/L, vinylformic acid: 15～50g/L; Ydrogen peroxide 50: 20～40g/L; Phytic acid: 5～10g/L, all the other are water, the pH value is: 1.5～2.5; Use the phosphorus acid for adjusting pH value.
On substitute chromium hydrochlorate Study on passivation, direction is different at present, and scheme is numerous, but still fails to provide a kind of high corrosion resistance that provides, the product of anti-finger printing and high thermal resistance.
Summary of the invention
To the deficiency of prior art, one of the object of the invention is to provide a kind of metal-plated post-passivation liquid of high temperature resistant, corrosion-resistant and anti-fingerprint, and said passivating solution has environmental protection and the high characteristics of over-all properties.
Said metal-plated post-passivation liquid is the aqueous solution, comprises following composition:
Vannadate 0.001～30g/L
Molybdate 0.01～30g/L
Preferred said metal-plated post-passivation liquid, said passivating solution is grouped into by following one-tenth:
Vannadate 0.001～30g/L
Molybdate 0.01～30g/L
All the other are water.
Further preferred, said metal-plated post-passivation liquid is grouped into by following one-tenth:
Vannadate 0.001～30g/L
Molybdate 0.01～30g/L
Phytic acid 1～300g/L
All the other are water.
Contain resin or/and silane in the preferred especially said metal-plated post-passivation liquid.
Said metal can be metal simple-substance or alloy.
Said passivating solution pH value is 1.5～7.5, is preferably 3～6, and its pH value can be regulated through soda acid.
Said vannadate concentration is preferably 0.01～30g/L, further is preferably 0.1～20g/L, and more preferably 0.5～10g/L is preferably 1-5g/L especially;
Said molybdate concentration is preferably 0.1～30g/L, further is preferably 0.1～20g/L, and more preferably 1～10g/L is preferably 5～8g/L especially;
Said silane concentration is preferably 0.01～30g/L, further is preferably 1～20g/L, and more preferably 1～15g/L is preferably 2～9g/L especially;
Said phytic acid concentration is preferably 1～200g/L, further is preferably 1～100g/L, is preferably 30～60g/L especially.
Said resin concentration is preferably 1～500g/L, further is preferably 1～300g/L, further is preferably 1～200g/L again, and more preferably 1～100g/L is preferably 1～50g/L especially.
Said vannadate can be single vannadate, also can be the mixture of vannadate more than 2 kinds or 2 kinds, is preferably sodium salt, ammonium salt, sylvite or its mixture.
Said molybdate can be single molybdate, also can be the mixture of molybdate more than 2 kinds or 2 kinds, sodium salt, ammonium salt, sylvite or its mixture.
Silane according to the invention is preferably liquid silane; Can be in R-aminopropyl-triethoxy, tetraethoxysilane, methyltrimethoxy silane, Union carbide A-162, N-(2-amino-ethyl)-3-aminopropyl methyl dimethoxysilane, 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, 3-glycidyl ether propyl group methyl dimethoxysilane, 3-glycidyl ether propyl trimethoxy silicane, the 3-aminopropyltriethoxywerene werene one or more.
It is the plant acid solution more than 30% that said phytic acid is preferably mass concentration.Said phytic acid (Phytic acid), chemical name: phytinic acid, molecular formula: C
6H
18O
24P
6, be a kind of organic phosphoric acid compounds that from plant seed, extracts.Because therefore its huge chelating potential energy have good erosion resistance, has the excellent adhesion between corrosion stability and metal and polymeric coating in the phytate coating on metal and the alloy surface.
Said resin is preferably water-base resin or its emulsion, can be in acrylic acid aqueous resin, amino water-base resin, phenolic aldehyde water-base resin, epoxy water-base resin, polyurethane aqueous resin, the organosilicon water-base resin one or more.Said water-base resin is the tailored version performance resins of metals such as iron and steel, stainless steel, copper aluminium, and metals such as iron and steel, stainless steel, copper aluminium are had superpower sticking power and salt spray resistance, is applicable to the protection and the decoration of metal products, antirust, anti-impression of the hand;
Said water is tap water, zero(ppm) water, deionized water etc. or its mixture.
Vannadate of the present invention, molybdate, silane, phytic acid, resin are known product, can commercially availablely obtain, and also can obtain according to the preparation method of prior art/new technology, and the present invention no longer gives unnecessary details with regard to its source.
Metal-plated post-passivation liquid of the present invention does not contain the chromium of any valence state.
The person of ordinary skill in the field can add other compositions according to the specialized technical knowledge of its grasp in the metal-plated post-passivation liquid that the present invention relates to.
Metal-plated post-passivation liquid of the present invention is the method preparation according to the prior art record, for example obtains through simple hybrid technique.
One of the object of the invention also is to provide the method for use of said metal-plated post-passivation liquid.
Use metal-plated post-passivation liquid according to the invention to plating the method that the back metal carries out passivation, may further comprise the steps:
(1) carries out surface treatment to plating the back metal;
(2) in room temperature～99 ℃, the metallic surface of handling through step (1) contacts at least 5 seconds, drying fully with passivating solution.
The said surface treatment of step (1) is affiliated technical field conventional treatment method, can handle for single method, also can be that multiple processing combines.
Contact described in the step (2) can be immersion, spraying, roller coat, brushing or its combination.
Preferably be no more than 3 minutes duration of contact described in the step (2), further preferably is no more than 2 minutes, is preferably 5～60 seconds especially.
Drying described in the step (2) can be Air drying or oven dry.
Preferably at least 12 hours said Air drying time, further preferably at least 24 hours, preferred especially 48 hours.
Said bake out temperature is preferably 40 ℃～200 ℃, further is preferably 60 ℃～150 ℃.
With the metal-plated post-passivation liquid phase ratio of prior art, metal-plated post-passivation liquid involved in the present invention has the following advantages:
(1) is raw material with vannadate, molybdate, silane and phytic acid and resin etc., do not contain the compound of contaminate environment such as chromium, fundamentally solved and contain of the pollution problem of chromium passivating technology, help environmental protection environment;
(2) be used for passivation after the metal-plated, can make that corrosion resistance nature, resistance to elevated temperatures and the anti-finger printing of product surface can be enhanced after the metal-plated;
(3) preparation is simple, and easy to use, cost is lower, is with a wide range of applications.
Embodiment
For ease of understanding the present invention, it is following that the present invention enumerates embodiment.Those skilled in the art should understand, and said embodiment helps to understand the present invention, should not be regarded as concrete restriction of the present invention.
Embodiment one
Use deionized water preparation ammonium vanadate concentration to be 15g/L, the phytic acid concentration passivating solution as 60g/L as 0.01g/L, ammonium molybdate concentration as 5g/L, 3-aminopropyltriethoxywerene werene concentration, regulating its pH value is 3, obtains passivating solution 1.
Embodiment two
Use deionized water preparation vanadium sodium salt concentration to be 9g/L, the phytic acid concentration passivating solution as 30g/L as 0.5g/L, ammonium molybdate concentration as 5g/L, butyl-aminopropyl triethoxysilane concentration, regulating its pH value is 6, obtains passivating solution 2.
Embodiment three
Use deionized water preparation ammonium vanadate concentration to be 2g/L, the epoxy water-base resin concentration passivating solution as 50g/L as 5g/L, Sodium orthomolybdate concentration as 8g/L, 3-glycidyl ether propyl trimethoxy silicane concentration, its pH value is 6, obtains passivating solution 3.
Embodiment four
Use tap water preparation ammonium vanadate concentration to be 0.001g/L, the ammonium molybdate concentration passivating solution as 30g/L, its pH value is 1.5, obtains passivating solution 4.
Embodiment five
Use tap water preparation potassium vanadate concentration to be 0.01g/L, the phytic acid concentration passivating solution as 300g/L as 30g/L, Sodium orthomolybdate concentration, its pH value is 7.5, obtains passivating solution 5.
Embodiment six
Use deionized water preparation ammonium vanadate concentration to be 1g/L, the polyurethane aqueous resin concentration passivating solution as 200g/L as 10g/L, Potassium orthomolybdate concentration as 10g/L, phytic acid concentration, its pH value is 5, obtains passivating solution 6.
Embodiment seven
Use deionized water preparation vanadic acid sodium concentration to be 200g/L, phenolic aldehyde water-base resin concentration passivating solution as 1g/L, N-(2-amino-ethyl)-3-aminopropyl methyl dimethoxysilane concentration as 0.01g/L, phytic acid concentration as 1g/L as 1g/L, ammonium molybdate concentration; Its pH value is 4, obtains passivating solution 7.
Embodiment eight
Use deionized water preparation ammonium vanadate concentration to be 0.1g/L, the 3-aminopropyltriethoxywerene werene concentration passivating solution as 30g/L as 20g/L, ammonium molybdate concentration, its pH value is 7, obtains passivating solution 8.
Embodiment nine
Use deionized water preparation ammonium vanadate concentration to be 30g/L, the organosilicon water-base resin concentration passivating solution as 500g/L as 0.1g/L, Sodium orthomolybdate concentration, its pH value is 2, obtains passivating solution 9.
In order to prove the performance of the embodiment of the invention, the foregoing description is carried out neutral salt spray corrosion test (NSS), experimental procedure is following:
Adopt 1～9 pair of sample of passivating solution to carry out passivation; The sample that passivation is intact is placed in the salt fog cabinet; With reference to the standard of ISO3768, adopt that concentration is 5%, pH value is 6.5～7.2, temperature is that 35 ± 2 ℃ NaCl solution is sprayed continuously, the area of white rust appears in specimen surface during the observation experiment end; Calculate the per-cent of specimen surface white rust, estimate the corrosion resistance nature of sample.
As sample, test result is as follows with the metal after pot galvanize:
Metal sheet sample to accomplishing in the electro-galvanizing 2 minutes is tested, and the result is following:
In addition, will put into constant temperature roaster baking taking-up after 20 minutes continuously of 300 ℃ through the sample after passivating solution 1～9 passivation, specimen surface does not have red rust, be full of cracks, explains to have the good temperature resistance ability.
To sum up, experimental data can show that the plating article that adopt the embodiment of the invention to carry out passivation have excellent corrosion resisting performance and resistance to elevated temperatures, and in addition, through facts have proved, embodiments of the invention also have excellent anti-finger printing ability.Because metal-plated post-passivation liquid of the present invention does not contain toxic compounds such as chromium cpd, and is environmentally friendly, and preparation is simple, and application prospect is extensive.
Applicant's statement; The present invention explains detailed process equipment of the present invention and technical process through the foregoing description; But the present invention is not limited to above-mentioned detailed process equipment and technical process, does not mean that promptly the present invention must rely on above-mentioned detailed process equipment and technical process could be implemented.The person of ordinary skill in the field should understand, and to any improvement of the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., all drops within protection scope of the present invention and the open scope.
Claims (10)
1. a metal-plated post-passivation liquid is characterized in that said passivating solution is the aqueous solution, comprises following composition:
Vannadate 0.001～30g/L
Molybdate 0.01～30g/L
2. passivating solution as claimed in claim 1 is characterized in that, said passivating solution is grouped into by following one-tenth:
Vannadate 0.001～30g/L
Molybdate 0.01～30g/L
All the other are water.
3. like each described passivating solution of claim 1-2, it is characterized in that said passivating solution is grouped into by following one-tenth:
Vannadate 0.001～30g/L
Molybdate 0.01～30g/L
Phytic acid 1～300g/L
All the other are water.
4. like each described passivating solution of claim 1-3, it is characterized in that, contain resin or/and silane in the said passivating solution.
5. like each described passivating solution of claim 1-4, it is characterized in that said passivating solution pH value is 1.5～7.5, is preferably 3～6, its pH value can be regulated through soda acid.
6. like each described passivating solution of claim 1-4, it is characterized in that described metal-plated post-passivation liquid does not contain the chromium of any valence state.
7. like each described passivating solution of claim 1-4, it is characterized in that said vannadate concentration is preferably 0.01～30g/L, further is preferably 0.1～20g/L, more preferably 0.5～10g/L is preferably 1-5g/L especially;
Said molybdate concentration is preferably 0.1～30g/L, further is preferably 0.1～20g/L, and more preferably 1～10g/L is preferably 5～8g/L especially;
Said silane concentration is 0.01～30g/L, is preferably 1～20g/L, and more preferably 1～15g/L is preferably 2～9g/L especially;
Said phytic acid concentration is preferably 1～200g/L, further is preferably 1～100g/L, is preferably 30～60g/L especially.
Said resin concentration is 1～500g/L, is preferably 1～300g/L, further is preferably 1～200g/L, and more preferably 1～100g/L is preferably 1～50g/L especially.
8. like each described passivating solution of claim 1-4, it is characterized in that said vannadate is single vannadate, or be the mixture of vannadate more than 2 kinds or 2 kinds;
Said molybdate is single molybdate, or is the mixture of molybdate more than 2 kinds or 2 kinds;
Said silane is liquid silane; Be in R-aminopropyl triethoxysilane, tetraethoxysilane, methyltrimethoxy silane, Union carbide A-162, N-(2-amino-ethyl)-3-aminopropyl methyl dimethoxysilane, 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane, 3-glycidyl ether propyl group methyl dimethoxysilane, 3-glycidyl ether propyl trimethoxy silicane, the 3-aminopropyltriethoxywerene werene one or more;
It is the plant acid solution more than 30% that said phytic acid is preferably mass concentration;
Said resin is water-base resin and emulsion thereof, is in acrylic acid aqueous resin, amino water-base resin, phenolic aldehyde water-base resin, epoxy water-base resin, polyurethane aqueous resin, the organosilicon water-base resin one or more.
9. one kind is used each described passivating solution of claim 1-8 to plating the method that the back metal carries out passivation, may further comprise the steps:
(1) carries out surface treatment to plating the back metal;
(2) in room temperature～99 ℃, the metallic surface of handling through step (1) contacts at least 5 seconds, drying fully with passivating solution.
10. method as claimed in claim 9 is characterized in that, the said surface treatment of step (1) is affiliated technical field conventional treatment method, and for single method is handled, or multiple processing combines.
Contact described in the step (2) is immersion, spraying, roller coat, brushing or its combination;
Preferred 50～70 ℃ of passivation temperature described in the step (2);
Preferably be no more than 3 minutes duration of contact described in the step (2), further preferably is no more than 2 minutes, is preferably 5～60 seconds especially;
Drying is Air drying or oven dry described in the step (2);
Preferably at least 12 hours said Air drying time, further preferably at least 24 hours, preferred especially 48 hours;
Said bake out temperature is preferably 40 ℃～200 ℃, further is preferably 60 ℃～150 ℃.
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| CN201110319734.2A CN102312234B (en) | 2011-10-20 | 2011-10-20 | Passivating solution for plated metal |
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| CN201110319734.2A CN102312234B (en) | 2011-10-20 | 2011-10-20 | Passivating solution for plated metal |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103805981A (en) * | 2012-11-13 | 2014-05-21 | 比亚迪股份有限公司 | Nickel passivation solution, preparation method thereof and method for passivating nickel surface |
| CN103910271A (en) * | 2014-04-10 | 2014-07-09 | 苏州德奥电梯有限公司 | Car roof of lift car |
| CN104357820A (en) * | 2014-11-14 | 2015-02-18 | 无锡伊佩克科技有限公司 | Chromium-free passivator for nickel-plated sheets and preparation method thereof |
| CN104451637A (en) * | 2014-11-14 | 2015-03-25 | 无锡伊佩克科技有限公司 | Metal surface chromium-free passivation solution and preparation method thereof |
| CN104561974A (en) * | 2014-11-14 | 2015-04-29 | 无锡伊佩克科技有限公司 | Chromium-free passivation solution for electro-galvanized steel plate and preparation method of passivation solution |
| CN105951078A (en) * | 2016-06-27 | 2016-09-21 | 无锡伊佩克科技有限公司 | Chromate-free passivation liquid for surface treatment of electro-galvanized steel sheet and preparing method of chromate-free passivation liquid |
| CN106011831A (en) * | 2016-05-31 | 2016-10-12 | 无锡伊佩克科技有限公司 | Environment-friendly water-based rust inhibitor and preparation method thereof |
| CN107881493A (en) * | 2017-11-09 | 2018-04-06 | 四川工程职业技术学院 | Improve the chromium-free deactivation membrane preparation method of Electroless Plating Ni P layer oxidative resistances |
| CN110983321A (en) * | 2019-11-29 | 2020-04-10 | 吉祥铝业（长兴）有限公司 | Novel aluminum single-plate surface chromium-free conversion treatment process |
| CN114807812A (en) * | 2022-04-24 | 2022-07-29 | 上海聚丰热镀锌有限公司 | Hot-dip galvanizing process for metal plated part |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103805981B (en) * | 2012-11-13 | 2017-05-31 | 比亚迪股份有限公司 | A kind of nickel passivating solution and preparation method thereof and the method for nickel surface passivation |
| CN103805981A (en) * | 2012-11-13 | 2014-05-21 | 比亚迪股份有限公司 | Nickel passivation solution, preparation method thereof and method for passivating nickel surface |
| CN103910271A (en) * | 2014-04-10 | 2014-07-09 | 苏州德奥电梯有限公司 | Car roof of lift car |
| CN104561974B (en) * | 2014-11-14 | 2017-04-19 | 无锡伊佩克科技有限公司 | Chromium-free passivation solution for electro-galvanized steel plate and preparation method of passivation solution |
| CN104357820A (en) * | 2014-11-14 | 2015-02-18 | 无锡伊佩克科技有限公司 | Chromium-free passivator for nickel-plated sheets and preparation method thereof |
| CN104451637A (en) * | 2014-11-14 | 2015-03-25 | 无锡伊佩克科技有限公司 | Metal surface chromium-free passivation solution and preparation method thereof |
| CN104561974A (en) * | 2014-11-14 | 2015-04-29 | 无锡伊佩克科技有限公司 | Chromium-free passivation solution for electro-galvanized steel plate and preparation method of passivation solution |
| CN106011831A (en) * | 2016-05-31 | 2016-10-12 | 无锡伊佩克科技有限公司 | Environment-friendly water-based rust inhibitor and preparation method thereof |
| CN105951078A (en) * | 2016-06-27 | 2016-09-21 | 无锡伊佩克科技有限公司 | Chromate-free passivation liquid for surface treatment of electro-galvanized steel sheet and preparing method of chromate-free passivation liquid |
| CN107881493A (en) * | 2017-11-09 | 2018-04-06 | 四川工程职业技术学院 | Improve the chromium-free deactivation membrane preparation method of Electroless Plating Ni P layer oxidative resistances |
| CN110983321A (en) * | 2019-11-29 | 2020-04-10 | 吉祥铝业（长兴）有限公司 | Novel aluminum single-plate surface chromium-free conversion treatment process |
| CN110983321B (en) * | 2019-11-29 | 2022-04-29 | 吉祥铝业（长兴）有限公司 | Chromium-free conversion treatment process for surface of aluminum veneer |
| CN114807812A (en) * | 2022-04-24 | 2022-07-29 | 上海聚丰热镀锌有限公司 | Hot-dip galvanizing process for metal plated part |
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