CN109207973A - A kind of preparation method for the passivating solution replacing chromic acid passivation - Google Patents
A kind of preparation method for the passivating solution replacing chromic acid passivation Download PDFInfo
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- CN109207973A CN109207973A CN201811342887.7A CN201811342887A CN109207973A CN 109207973 A CN109207973 A CN 109207973A CN 201811342887 A CN201811342887 A CN 201811342887A CN 109207973 A CN109207973 A CN 109207973A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
- C23C22/08—Orthophosphates
Abstract
The present invention provides a kind of preparation methods of passivating solution for replacing chromic acid passivation, wherein the passivating solution for passivation is composed of the following components: 10~20g/L of ammonium persulfate, 2~6g/L of phytic acid, 15~25g/L of tertiary sodium phosphate, phosphatase 11~3mL/L, 0.5~1mL/L of boric acid, four propyl alcohol 0.5~3g/L of zirconium, 0.1~1g/L of benzotriazole, 3~6g/L of complexing agent, 5~10g/L of water-soluble film-forming resin, 4~6g/L of nano silicon oxide, 0.1~3g/L of stabilizer, remaining is water；The passivating solution complies fully with the environmental protection standards such as China's electroplating wastewater discharge standard and RoHS Directive；The present invention is main deactivation matter using ammonium persulfate and tertiary sodium phosphate, phytic acid is auxiliary deactivation matter, and chelating bridge formation is played the role of by water-soluble film-forming resin and being crosslinked for complexing agent, to form the molecular compound film layer that one layer of three kinds of substance combines, so that film-formation result is good, film forming speed is fast, and film layer has preferable adhesive force, and film forming causes dense and uniform.
Description
The application is divisional application, original application application No. is 201610893934.1, the applying date is October 13 in 2016
Day, it is entitled " a kind of environment-protective process for replacing chromic acid passivation ".
Technical field
The invention belongs to field of metal surface treatment technology, and in particular to a kind of preparation for the passivating solution for replacing chromic acid passivation
Method.
Background technique
Hot-dip metal plated material, including hot-dip galvanized metal material and hot-dip aluminizing zinc metal material, corrode, all in order to prevent
One layer of metal protection coating can be applied to form protecting film on the surface of hot-dip metal plated material.The thus performance of metal protection coating
It is particularly significant for the anti-corrosion of hot-dip metal plated material.
Hexavalent chromate passivating technique due to the excellent corrosion resistance of its chemical composition coating and good self-reparing capability,
It is industrial commonly used chemical conversion process for treating surface.It is not only raw in aluminum profile but due to the high toxicity of Cr VI
Serious waste water, residue contamination are generated during producing, also generates serious secondary pollution in its use, removal process.Text at present
The Chromium-free passivating treatment method for offering report includes: zirconium-titanium system, Rare Earth, manganese salt system, cobalt salt system, molybdenum salt system and silane system etc.
Passivation system.
If 102181853 A of CN discloses a kind of novel treatment fluid for chromium-free passivation of aluminum alloy, by following mass percents
Material composition: the mixture 20-30% of potassium titanate, sodium titanate and metatitanic acid magnesium salts, the mixing of potassium zirconium, sodium zirconate and zirconic acid magnesium salts
Object 5-15%, modified organic silicone resin 5-15% and polyurethane resin 40-50%.Novel aluminum alloy Chrome-free of the present invention is blunt
Change treatment fluid, dedicated for the surface treatment of aluminium and its alloy, magnesium and its alloy.CN 101161861A discloses one kind and is used for
Handle the chromium-free passivation liquid and its application method of aluminium alloy, its component of the passivating solution and weight concentration be containing Ti (IV) 0.05~
The fluorine zirconic acid of 0.15WT%, the fluorine zirconic acid containing Zr (IV) 0.01~0.05WT% and the organic phosphoric acid containing 0.02WT% to saturated concentration
Compound.China's application 200710009302.5 discloses " a kind of chromium-free passivation liquid ", the program 35~140g organic acid, 20
~25g inorganic salts, 0.8~1g surfactant, 4~5g oxidant and inorganic acid are configured to the passivating solution that pH is 2~5, inorganic
For object in conjunction with organic matter, corrosion resistance is suitable with chromate.China application CN102002697 A discloses " chromium-free passivation liquid ",
20~35 grams of salt, 18~38 grams of the complexing agent, reductant-oxidant 0.051 that the program is formed using free element
~0.15 gram cooperates with water, and the passivating solution passivation technology is identical as chromating technique, saves worker's training of enterprise
Instruction expense.But existing non-chromium passivation treatment fluid exists, and the processing time is long, treatment temperature is high, complex treatment process, production cost
, there is a certain distance in the disadvantages of high apart from industrial production.
Summary of the invention
The object of the present invention is to provide a kind of environment-protective process for replacing chromic acid passivation, passivator used in the technique overcomes
The defect that the existing chrome-free tanning agent processing time is long, treatment temperature is high, corrosion resistance is poor, before there is preferable industrial application
Scape.
To solve the above problems, the technical solution adopted by the present invention are as follows:
A kind of environment-protective process replacing chromic acid passivation, the passivating solution for passivation are composed of the following components: ammonium persulfate 10~
20g/L, 2~6g/L of phytic acid, 15~25g/L of tertiary sodium phosphate, phosphatase 11~3mL/L, 0.5~1mL/L of boric acid, four propyl alcohol zirconiums 0.5
~3g/L, 0.1~1g/L of benzotriazole, 3~6g/L of complexing agent, 5~10g/L of water-soluble film-forming resin, nano silicon oxide 4
~6g/L, 0.1~3g/L of stabilizer, remaining is water；
Wherein, the passivating solution the preparation method comprises the following steps: (1) by above-mentioned dosage composition take a certain amount of ammonium persulfate, tertiary sodium phosphate, network
Mixture and water-soluble film-forming resin are poured into water, are stirred continuously to form solution A；(2) a certain amount of phosphoric acid is taken, is slowly added drop-wise to molten
In liquid A, while change is added to stir, solution B is formed；(3) four propyl alcohol zirconiums, benzotriazole, nano silicon oxide, side are added into solution B
Add change to stir, forms solution C；(4) a certain amount of boric acid is poured into a certain amount of water, is stirred well to boric acid and is completely dissolved, formed
Solution D, then solution C is poured into solution D, it is stirred when pouring into, forms solution E；(5) a certain amount of phytic acid and stabilizer are taken,
It is added in solution E, stirs while adding, form solution F to get the passivating solution.
Wherein, the water-soluble film-forming resin is water-soluble polyester film-forming resin, water-soluble phenylpropyl alcohol film-forming resin, water solubility
Epoxy film forming resins, soluble polyurethane film-forming resin, the third film-forming resin of water-soluble silicon, water-soluble acrylic film-forming resin and water
At least one of dissolubility fluorine carbon film-forming resin.
The average grain diameter of the nano silicon oxide is 20~25nm.
The stabilizer is one or both of ethylenediamine tetra-acetic acid, malonic acid, sodium citrate, sodium gluconate
Above mixture.
The complexing agent is that triethanolamine and four sodium of 1-hydroxy ethylidene-1,1-diphosphonic acid are formed by weight 1:1~2.
The passivating solution is acidic aqueous solution, and pH is 2~4.
The water is the deionized water of pure water or conductivity less than 6 μ S/cm.
Technical effect of the invention are as follows: the passivating solution complies fully with China's electroplating wastewater discharge standard and RoHS Directive
Equal environmental protection standards, selected is all cheap nontoxic material composition, safety and environmental protection when use；The present invention uses ammonium persulfate
It is main deactivation matter with tertiary sodium phosphate, phytic acid is auxiliary deactivation matter, and passes through the friendship of water-soluble film-forming resin and complexing agent
Connection plays the role of chelating and builds bridge, so that the molecular compound film layer that one layer of three kinds of substance combines is formed, so that film-formation result is good, at
Film speed is fast, and film layer has preferable adhesive force, and film forming cause is dense and uniform, and has preferable anti-corrosion function, middle salt air corrosion
Test display be greater than 180h, and four propyl alcohol zirconiums addition so that passivating film compactness, binding force and hardness significantly improve；Separately
Outside, passivator of the present invention is placed 360 days at room temperature, and apparent performance change does not occur.
The main performance index of passivating solution prepared by the present invention such as the following table 1:
| Physical and chemical index | Detection method | Index |
| Appearance | Range estimation | Light yellow transparent liquid |
| Solid content | Difference weight method | 14~17wt% |
| PH value | PH meter | 2~4 |
| Viscosity | Rotational viscometer | 7.0~11.0mpa.s, 25 DEG C |
| Specific gravity | Densimeter | 1.0~1.2g/cm3 |
Specific embodiment
Technical solution of the present invention is further elaborated below with reference to embodiment:
Embodiment 1
A kind of environment-protective process replacing chromic acid passivation, the passivating solution for passivation are composed of the following components: ammonium persulfate 10g/L,
Phytic acid 2g/L, tertiary sodium phosphate 15g/L, phosphatase 11 mL/L, boric acid 0.5mL/L, four propyl alcohol zirconium 0.5g/L, benzotriazole
0.1g/L, complexing agent 3g/L, water-soluble polyester film-forming resin 5g/L, nano silicon oxide 4g/L, ethylenediamine tetra-acetic acid 0.1g/L,
Yu Weishui；The complexing agent is that triethanolamine and four sodium of 1-hydroxy ethylidene-1,1-diphosphonic acid are formed by weight 1:2.
Embodiment 2
A kind of environment-protective process replacing chromic acid passivation, the passivating solution for passivation are composed of the following components: ammonium persulfate 20g/L,
Phytic acid 6g/L, tertiary sodium phosphate 25g/L, phosphoric acid 3mL/L, boric acid 1mL/L, four propyl alcohol zirconium 3g/L, benzotriazole 1g/L, network
Mixture 6g/L, water-soluble phenylpropyl alcohol film-forming resin 10g/L, nano silicon oxide 6g/L, stabilizer malonic acid 3g/L, remaining is water；Institute
Stating complexing agent is that triethanolamine and four sodium of 1-hydroxy ethylidene-1,1-diphosphonic acid are formed by weight 1:1.2.
Embodiment 3
A kind of environment-protective process replacing chromic acid passivation, the passivating solution for passivation are composed of the following components: ammonium persulfate 15g/L,
Phytic acid 4g/L, tertiary sodium phosphate 20g/L, phosphoric acid 2mL/L, boric acid 0.8mL/L, four propyl alcohol zirconium 1.5g/L, benzotriazole
0.4g/L, complexing agent 4g/L, soluble epoxide film-forming resin 8g/L, nano silicon oxide 5g/L, stabilizer sodium citrate 1.3g/L,
Remaining is water；The complexing agent is that triethanolamine and four sodium of 1-hydroxy ethylidene-1,1-diphosphonic acid are formed by weight 1:1.
Embodiment 4
A kind of environment-protective process replacing chromic acid passivation, the passivating solution for passivation are composed of the following components:
Ammonium persulfate 12g/L, phytic acid 3g/L, tertiary sodium phosphate 19g/L, phosphoric acid 2mL/L, boric acid 0.6mL/L, four propyl alcohol zirconiums
1.7g/L, benzotriazole 0.5g/L, complexing agent 4g/L, soluble polyurethane film-forming resin 7g/L, nano silicon oxide 5g/L,
Stabilizer sodium gluconate 2.0g/L, remaining is water；The complexing agent is triethanolamine and four sodium of 1-hydroxy ethylidene-1,1-diphosphonic acid by weight
Amount is formed than 1:1.5.
Embodiment 5
A kind of environment-protective process replacing chromic acid passivation, the passivating solution for passivation are composed of the following components: ammonium persulfate 18g/L,
Phytic acid 5g/L, tertiary sodium phosphate 22g/L, phosphoric acid 3mL/L, boric acid 0.8mL/L, four propyl alcohol zirconium 2.5g/L, benzotriazole
0.8g/L, complexing agent 5g/L, water-soluble acrylic film-forming resin 8g/L, nano silicon oxide 5g/L, stabilizer ethylenediamine tetra-acetic acid
2.5g/L, remaining is water；The complexing agent is that triethanolamine and four sodium of 1-hydroxy ethylidene-1,1-diphosphonic acid are formed by weight 1:1.8.
Embodiment 6
A kind of environment-protective process replacing chromic acid passivation, the passivating solution for passivation are composed of the following components:
Ammonium persulfate 16g/L, phytic acid 4g/L, tertiary sodium phosphate 17g/L, phosphoric acid 2mL/L, boric acid 0.6L/L, four propyl alcohol zirconiums
1.8g/L, benzotriazole 0.4g/L, complexing agent 6g/L, water-soluble fluorine carbon film-forming resin 7g/L, nano silicon oxide 5g/L, surely
Determine agent sodium citrate 1.5g/L, remaining is water；The complexing agent be triethanolamine and four sodium of 1-hydroxy ethylidene-1,1-diphosphonic acid by weight
1:1.7 composition.
Embodiment 7
The preparation method of passivator described in embodiment 1-6 includes the following steps: that (1) takes a certain amount of persulfuric acid by above-mentioned dosage composition
Ammonium, tertiary sodium phosphate, complexing agent and water-soluble film-forming resin are poured into water, are stirred continuously to form solution A；(2) a certain amount of phosphorus is taken
Acid is slowly added drop-wise in solution A, while change is added to stir, forms solution B；(3) four propyl alcohol zirconiums, three nitrogen of benzo are added into solution B
Azoles, nano silicon oxide form solution C while change is added to stir；(4) a certain amount of boric acid is poured into a certain amount of water, is stirred well to boron
Acid is completely dissolved, and is formed solution D, then solution C is poured into solution D, is stirred when pouring into, and solution E is formed；(5) it takes a certain amount of
Phytic acid and stabilizer, be added in solution E, stir while adding, formed solution F to get the passivating solution.
Embodiment 8
Experiment is tested for the property to the passivator of embodiment 1-6, test technology: galvanized part is taken out from electroplating bath, washed
Light is rinsed out in the dust technology of 5wt% afterwards, then is rinsed in deionized water twice, prepared passivating solution work is then placed in
In liquid, passivation time 20-60s dries 10-20min under conditions of 110 DEG C after slot out to obtain the final product.The property of zinc coat after passivation
It can be as follows:
Its test result is as follows table 2:
Passivator its corrosion resistance in hygrothermal environment as can be seen from Table 2 prepared by the present invention is preferable, salt tolerant water immersion property
Well, good film-forming property, salt-fog resistant time are long.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention, although
Present invention has been described in detail with reference to the aforementioned embodiments, for those skilled in the art, still can be right
Technical solution documented by foregoing embodiments is modified or equivalent replacement of some of the technical features.It is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in protection of the invention
Within the scope of.
Claims (7)
1. a kind of environment-protective process for replacing chromic acid passivation, which is characterized in that the passivating solution for passivation is composed of the following components: mistake
10~20g/L of ammonium sulfate, 2~6g/L of phytic acid, 15~25g/L of tertiary sodium phosphate, phosphatase 11~3mL/L, 0.5~1mL/L of boric acid,
Four propyl alcohol 0.5~3g/L of zirconium, 0.1~1g/L of benzotriazole, 3~6g/L of complexing agent, 5~10g/L of water-soluble film-forming resin,
4~6g/L of nano silicon oxide, 0.1~3g/L of stabilizer, remaining is water；
Wherein, the passivating solution the preparation method comprises the following steps: (1) by above-mentioned dosage composition take a certain amount of ammonium persulfate, tertiary sodium phosphate, network
Mixture and water-soluble film-forming resin are poured into water, are stirred continuously to form solution A；(2) a certain amount of phosphoric acid is taken, is slowly added drop-wise to molten
In liquid A, while change is added to stir, solution B is formed；(3) four propyl alcohol zirconiums, benzotriazole, nano silicon oxide, side are added into solution B
Add change to stir, forms solution C；(4) a certain amount of boric acid is poured into a certain amount of water, is stirred well to boric acid and is completely dissolved, formed
Solution D, then solution C is poured into solution D, it is stirred when pouring into, forms solution E；(5) a certain amount of phytic acid and stabilizer are taken,
It is added in solution E, stirs while adding, form solution F to get the passivating solution.
2. environment-protective process according to claim 1, which is characterized in that the water-soluble film-forming resin be water-soluble polyester at
Film resin, water-soluble phenylpropyl alcohol film-forming resin, soluble epoxide film-forming resin, soluble polyurethane film-forming resin, water-soluble silicon third
At least one of film-forming resin, water-soluble acrylic film-forming resin and water-soluble fluorine carbon film-forming resin.
3. environment-protective process according to claim 1, which is characterized in that the average grain diameter of the nano silicon oxide be 20~
25nm。
4. environment-protective process according to claim 1, which is characterized in that the stabilizer is ethylenediamine tetra-acetic acid, third
The mixture of one or more of diacid, sodium citrate, sodium gluconate.
5. environment-protective process according to claim 1, which is characterized in that the complexing agent is triethanolamine and hydroxy ethylidene two
Four sodium of phosphonic acids is formed by weight 1:1~2.
6. environment-protective process according to claim 1, which is characterized in that the passivating solution be acidic aqueous solution, pH be 2~
4。
7. environment-protective process according to claim 1, which is characterized in that the water is pure water or conductivity less than 6 μ S/
The deionized water of cm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811342887.7A CN109207973A (en) | 2016-10-13 | 2016-10-13 | A kind of preparation method for the passivating solution replacing chromic acid passivation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811342887.7A CN109207973A (en) | 2016-10-13 | 2016-10-13 | A kind of preparation method for the passivating solution replacing chromic acid passivation |
| CN201610893934.1A CN106435547B (en) | 2016-10-13 | 2016-10-13 | A kind of environment-protective process replacing chromic acid passivation |
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| CN201610893934.1A Division CN106435547B (en) | 2016-10-13 | 2016-10-13 | A kind of environment-protective process replacing chromic acid passivation |
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| CN201811342887.7A Withdrawn CN109207973A (en) | 2016-10-13 | 2016-10-13 | A kind of preparation method for the passivating solution replacing chromic acid passivation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531898A (en) * | 2018-04-11 | 2018-09-14 | 浙江康盛股份有限公司 | A kind of chromium-free passivation liquid |
| CN115613022A (en) * | 2022-09-28 | 2023-01-17 | 湖南金裕环保科技有限公司 | Chromium-free natural color passivating agent for aluminum and aluminum alloy and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115851060B (en) * | 2022-12-09 | 2023-07-04 | 浙江花园新能源股份有限公司 | Chromium-free environment-friendly ultrathin lithium electric copper foil and preparation process thereof |
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| CN101891998A (en) * | 2009-05-18 | 2010-11-24 | 攀钢集团钢铁钒钛股份有限公司 | Paint composition and galvanized passivated material |
| CN102089458A (en) * | 2008-07-16 | 2011-06-08 | 日本帕卡濑精株式会社 | Aqueous metal-surface-treating agent and surface-treated metal material |
| CN102634785A (en) * | 2012-05-07 | 2012-08-15 | 东莞市闻誉实业有限公司 | Method for passivation of zinc and zinc alloy and chromium-free passivation solution |
| CN104250766A (en) * | 2013-06-28 | 2014-12-31 | 无锡杨市表面处理科技有限公司 | Brass surface chrome-free passivation solution |
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| CN103205742A (en) * | 2013-04-09 | 2013-07-17 | 海宁市科泰克金属表面技术有限公司 | Chromate-free passivator for zinc coating |
| CN104674206A (en) * | 2013-12-03 | 2015-06-03 | 青岛惠城石化科技有限公司 | Study on environmental-friendly citric acid passivation solution formula |
| CN104651821A (en) * | 2015-02-11 | 2015-05-27 | 常州君合科技股份有限公司 | Novel aluminum and high-molecular aluminum alloy chromium-free film forming agent |
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2016
- 2016-10-13 CN CN201610893934.1A patent/CN106435547B/en active Active
- 2016-10-13 CN CN201811342887.7A patent/CN109207973A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102089458A (en) * | 2008-07-16 | 2011-06-08 | 日本帕卡濑精株式会社 | Aqueous metal-surface-treating agent and surface-treated metal material |
| CN101891998A (en) * | 2009-05-18 | 2010-11-24 | 攀钢集团钢铁钒钛股份有限公司 | Paint composition and galvanized passivated material |
| CN102634785A (en) * | 2012-05-07 | 2012-08-15 | 东莞市闻誉实业有限公司 | Method for passivation of zinc and zinc alloy and chromium-free passivation solution |
| CN104250766A (en) * | 2013-06-28 | 2014-12-31 | 无锡杨市表面处理科技有限公司 | Brass surface chrome-free passivation solution |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531898A (en) * | 2018-04-11 | 2018-09-14 | 浙江康盛股份有限公司 | A kind of chromium-free passivation liquid |
| CN115613022A (en) * | 2022-09-28 | 2023-01-17 | 湖南金裕环保科技有限公司 | Chromium-free natural color passivating agent for aluminum and aluminum alloy and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106435547A (en) | 2017-02-22 |
| CN106435547B (en) | 2019-02-19 |
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