CN105951078A - Chromate-free passivation liquid for surface treatment of electro-galvanized steel sheet and preparing method of chromate-free passivation liquid - Google Patents
Chromate-free passivation liquid for surface treatment of electro-galvanized steel sheet and preparing method of chromate-free passivation liquid Download PDFInfo
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- CN105951078A CN105951078A CN201610474467.9A CN201610474467A CN105951078A CN 105951078 A CN105951078 A CN 105951078A CN 201610474467 A CN201610474467 A CN 201610474467A CN 105951078 A CN105951078 A CN 105951078A
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- passivation liquid
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- free passivation
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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
- C23C22/40—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 molybdates, tungstates or vanadates
-
- 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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
The invention discloses chromate-free passivation liquid for surface treatment of an electro-galvanized steel sheet and a preparing method of the chromate-free passivation liquid. The chromate-free passivation liquid comprises, by mass, 3-8 parts of zinc vanadate, 5-15 parts of lithium vanadate, 1-6 parts of potassium metavanadate, 2-10 parts of tartaric acid, 2-6 parts of sodium benzoate, 3-10 parts of titanium chloride, 1-6 parts of diphenol propane, 2-8 parts of malonic acid, 1-6 parts of vinyl silane, 2-10 parts of a surface active agent, 3-12 parts of molybdate, 0.1-2 parts of polyvinyl alcohol and 30-50 parts of water. A passivation film formed through the passivation liquid can greatly improve the bonding force between metal and a paint film, no chromium is contained in the passivation liquid, and no harm is done to people and the environment in the producing process and the using process. Products are colorless and transparent, and the passivated electro-galvanized steel sheet is free of rust for 200 h in the neutral salt spray test.
Description
Technical field
The invention belongs to metal surface treatment chemical product technical field, be specifically related to a kind of plated steel sheet surface and process chromium-free passivation liquid and preparation method thereof.
Background technology
Corrosion of metal causes greatly loss to human society wealth, and particularly with the extremely close iron and steel of social life relation of people, zinc-plated is to improve the weather-resistant effective ways of iron and steel, is widely used in the industries such as aviation, electric power, traffic, building, machinery.The method generally used has plating, immersion plating and spraying plating three kinds.In a variety of contexts, the corrosion potential of zinc compares low phase for most metals material, and when steel substrate is corroded, zinc coating preferentially dissolves as anode, thus protects steel substrate.The chemical property of metallic zinc is the most active; although corrosion rate ratio in an atmosphere is relatively low; but in wet environment; exposed Several Thiourea Derivatives on Zinc Plate Surface is the most dimmed; the corrosion product forming white loose is referred to as white rust; and corrosion product is substantially to matrix unprotect, therefore, generally its surface is carried out corrosion protection process after zinc-plated.How anticorrosion is the main direction of Treatment of Metal Surface science.
In order to reduce the chemism of zinc, chromatedsolution is often used to carry out Passivation Treatment so that it is surface forms one layer of chromate conversion coating.The formal title of this tunic is called " chromate conversion coating ", and electroplating industry is referred to as " zinc coating passivation film ", or is called for short " Zincing passivation ".The chromate film on zinc alloy layer surface shows good corrosion resistance in erosion environment condition, and is the suitable replacement of the pot having severe toxicity.The chromating of zinc develops into the history having had upper a century today, and its membrane formation mechanism and production technology are the most ripe.The physical and chemical performance of film layer is the best, thus the application on plating piece is the most extensive.Applying most common passivation process in history is that chromating processes, and chromating liquid stable performance, with low cost, passivation technology is simple, and passivating film glossiness and etch resistant properties are good, are used widely, and therefore the research to chromate passivation film is the most most.Traditional chromating liquid is typically to be made up of hexavalent chromium compound, trivalent chromium compound, conducting salt, chelating agent etc..The dissolving of zinc, chromate reduction and the precipitation of trivalent chromium gel is there is during passivating film is formed, these reactions define the skeleton of passivating film, chromate is adsorbed on gel formation surface layer with the form of basic salt subsequently, so far generates complete Cr VI passivation layer.When passivation layer is because of external force after scratch, in malaria, hexavalent chromium compound is dissolved in water and reacts with the zinc layers exposed and be the most again passivated processing, so that passivating film is repaired, and the referred to as self-healing ability of Cr VI passivation.Owing to chromate film is relatively thin, under high intensity easily rupturable, affect corrosion stability, and Cr VI has certain harm to human body and environment, enhancing along with people's environmental consciousness, the passivating solution gradually adopting Chrome-free or low chromium to combine with Organic substance in recent years carries out galvanizing post processing, reaches good result, and the research to this passivating film is the most more.
Summary of the invention
It is an object of the invention to provide a kind of plated steel sheet surface and process chromium-free passivation liquid and preparation method thereof; the passivating film that passivating solution is formed can be greatly improved the adhesion between metal and paint film; without chromium in passivating solution; it is all harmless to human and environment during production process and use; product water white transparency; after electroplating steel plate Passivation Treatment, color change is inconspicuous; good stability; the passivating film using this passivating solution to obtain has good protective value, and in the plated steel sheet neutral salt spray test of passivation, 200h is rustless.
To achieve these goals, the technological means that the present invention uses is:
A kind of plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 3 ~ 8 parts, lithium vanadate 5 ~ 15 parts, potassium metavanadate 1 ~ 6 part, 2 ~ 10 parts of tartaric acid, sodium benzoate 2 ~ 6 parts, titanium chloride 3 ~ 10 parts, diphenol propane 1 ~ 6 part, malonic acid 2 ~ 8 parts, vinyl silanes 1 ~ 6 part, 2 ~ 10 parts of surfactant, molybdate 3 ~ 12 parts, polyvinyl alcohol 0.1 ~ 2 part, 30 ~ 50 parts of water.
Described molybdate is sodium molybdate or ammonium molybdate.
Described surfactant is tannic acid or Cetyl bromo-pyridine.
Described plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 4 ~ 7 parts, lithium vanadate 8 ~ 12 parts, potassium metavanadate 2 ~ 5 parts, 4 ~ 8 parts of tartaric acid, sodium benzoate 3 ~ 5 parts, titanium chloride 5 ~ 8 parts, diphenol propane 2 ~ 5 parts, malonic acid 4 ~ 6 parts, vinyl silanes 2 ~ 5 parts, 4 ~ 8 parts of surfactant, molybdate 6 ~ 10 parts, polyvinyl alcohol 0.5 ~ 1.5 part, 35 ~ 45 parts of water.
Described plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 5.5 parts, lithium vanadate 10 parts, potassium metavanadate 3.5 parts, 6 parts of tartaric acid, sodium benzoate 4 parts, titanium chloride 6.5 parts, diphenol propane 3.5 parts, malonic acid 5 parts, vinyl silanes 3.5 parts, 6 parts of surfactant, molybdate 8 parts, polyvinyl alcohol 1 part, 40 parts of water.
Described plated steel sheet surface processes the preparation method of chromium-free passivation liquid, is dissolved in by polyvinyl alcohol in the water of 1/4 working volume, is heated to 70 ~ 90 DEG C, adds remaining ingredient after cooling, stirs and i.e. obtains plated steel sheet surface process chromium-free passivation liquid.
It is preferably heated to 80 DEG C.
The chromium-free passivation liquid obtained is mainly used in the Passivation Treatment of galvanized steel sheet surface, and processing method is: after steel plate electro-galvanizing, rinses well with tap water immediately, and cold wind dries up, and then uses the method for roller coat that passivating solution is uniformly coated to plated steel sheet surface；4 ~ 6min is toasted at 180 ~ 250 DEG C；Natural cooling.
Beneficial effect: the plated steel sheet surface that the present invention provides processes chromium-free passivation liquid; the passivating film that passivating solution is formed can be greatly improved the adhesion between metal and paint film; without chromium in passivating solution; it is all harmless to human and environment during production process and use; product water white transparency; after electroplating steel plate Passivation Treatment, color change is inconspicuous; good stability; the passivating film using this passivating solution to obtain has good protective value, and in the plated steel sheet neutral salt spray test of passivation, 200h is rustless.Produce easily, low cost, of many uses.
Detailed description of the invention
Embodiment 1
A kind of plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 3 parts, lithium vanadate 15 parts, potassium metavanadate 1 part, 2 parts of tartaric acid, sodium benzoate 6 parts, titanium chloride 10 parts, diphenol propane 1 part, malonic acid 8 parts, vinyl silanes 6 parts, 2 parts of surfactant tannic acid, ammonium molybdate 12 parts, polyvinyl alcohol 0.1 part, 30 parts of water.
Polyvinyl alcohol is dissolved in the water of 1/4 working volume, is heated to 80 DEG C, after cooling, add remaining ingredient, stir and i.e. obtain plated steel sheet surface process chromium-free passivation liquid.
Embodiment 2
A kind of plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 8 parts, lithium vanadate 5 parts, potassium metavanadate 6 parts, 10 parts of tartaric acid, sodium benzoate 2 parts, titanium chloride 10 parts, diphenol propane 6 parts, malonic acid 2 parts, vinyl silanes 1 part, surfactant Cetyl bromo-pyridine 10 parts, sodium molybdate 3 parts, polyvinyl alcohol 2 parts, 50 parts of water.
Polyvinyl alcohol is dissolved in the water of 1/4 working volume, is heated to 80 DEG C, after cooling, add remaining ingredient, stir and i.e. obtain plated steel sheet surface process chromium-free passivation liquid.
Embodiment 3
A kind of plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 4 parts, lithium vanadate 12 parts, potassium metavanadate 2 parts, 8 parts of tartaric acid, sodium benzoate 3 parts, titanium chloride 5 parts, diphenol propane 2 parts, malonic acid 6 parts, vinyl silanes 2 parts, 4 parts of surfactant tannic acid, ammonium molybdate 6 parts, polyvinyl alcohol 1.5 parts, 35 parts of water.
Polyvinyl alcohol is dissolved in the water of 1/4 working volume, is heated to 80 DEG C, after cooling, add remaining ingredient, stir and i.e. obtain plated steel sheet surface process chromium-free passivation liquid.
Embodiment 4
A kind of plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 7 parts, lithium vanadate 8 parts, potassium metavanadate 5 parts, 4 parts of tartaric acid, sodium benzoate 5 parts, titanium chloride 8 parts, diphenol propane 5 parts, malonic acid 4 parts, vinyl silanes 5 parts, surfactant Cetyl bromo-pyridine 8 parts, sodium molybdate 10 parts, polyvinyl alcohol 0.5 part, 45 parts of water.
Polyvinyl alcohol is dissolved in the water of 1/4 working volume, is heated to 80 DEG C, after cooling, add remaining ingredient, stir and i.e. obtain plated steel sheet surface process chromium-free passivation liquid.
Embodiment 5
A kind of plated steel sheet surface processes chromium-free passivation liquid, and component and each constituent mass number are as follows: Zinc vanadate 5.5 parts, lithium vanadate 10 parts, potassium metavanadate 3.5 parts, 6 parts of tartaric acid, sodium benzoate 4 parts, titanium chloride 6.5 parts, diphenol propane 3.5 parts, malonic acid 5 parts, vinyl silanes 3.5 parts, 6 parts of surfactant tannic acid, ammonium molybdate 8 parts, polyvinyl alcohol 1 part, 40 parts of water.
Polyvinyl alcohol is dissolved in the water of 1/4 working volume, is heated to 80 DEG C, after cooling, add remaining ingredient, stir and i.e. obtain plated steel sheet surface process chromium-free passivation liquid.
Plated steel sheet DK7732 type electric spark CNC wire-cut machine is processed into the small pieces that specification is 13mm × 13mm × 5mm, polishing, until metallic luster, smooth and no marking are exposed in surface, as test sample, the plated steel sheet surface using embodiment 1 ~ 5 processes chromium-free passivation liquid and is coated passivation, 200 DEG C of dry 5min, natural cooling, the passivation film thickness obtained is 1.5g/m2, then carry out performance test, the results are shown in Table 1.
With reference to machinery industry standard JB/T 6073-1992, use immersion corrosion test determination plated steel sheet surface to process chromium-free passivation liquid and form the corrosion resisting property of coating in aluminum alloy surface: take sample and immerse immersion in 5% NaCl solution, sample plastic ties hangs, upper end is more than 2cm away from liquid level, solution pH value is 6.5, primary brine is changed every six days, uncovered placement, temperature 10 ± 2 DEG C, record each sample and the time of first red rust occurs, the anti-corrosion time, as Evaluation of Corrosion Resistance result, the results are shown in Table 1..
Neutral salt spray test:
Temperature in proof box is maintained at 25 DEG C, and compressed air to be preheating between 35 DEG C and be adjusted to enough pressure.The mass concentration of sodium chloride solution is 5% ± 1%, and after condensation, the pH value of solution is between 6.5-7.2.During salt spray test, fall mist amount should control in following scope: every 80cm2In horizontal plane, between the fall mist amount average out to 1.0 ~ 2.0ml collected per hour, the sample that embodiment 5 coats is placed in proof box and sprays salt continuously, observe pattern and the extent of corrosion of different time, the results are shown in Table 2.
Film adhesive is tested:
The film of test film is spaced 1mm and portrays the most vertical line, judge the fragility of film and the best to the adhesion property of this material according to the size of gap slight crack extension, the results are shown in Table 1.
Table 1:
| The anti-corrosion time | Adhesive force | |
| Embodiment 1 | 184h | Two grades |
| Embodiment 2 | 172h | Two grades |
| Embodiment 3 | 231h | One-level |
| Embodiment 4 | 246h | One-level |
| Embodiment 5 | 362h | One-level |
Table 2:
| Spray salt time/h | Pattern record | Extent of corrosion |
| 24 | Without white rust | Nothing |
| 48 | Without white rust | Nothing |
| 72 | Without white rust | Nothing |
| 96 | Without white rust | Nothing |
| 120 | Without white rust | Nothing |
| 144 | Without white rust | Nothing |
| 168 | Without white rust | Nothing |
| 192 | Without white rust | Nothing |
| 216 | Without white rust | Slightly |
| 240 | The a small amount of white rust in edge | Slightly |
Claims (7)
1. a plated steel sheet surface processes chromium-free passivation liquid, it is characterised in that component and each constituent mass number are as follows: Zinc vanadate 3 ~ 8 parts, lithium vanadate 5 ~ 15 parts, potassium metavanadate 1 ~ 6 part, 2 ~ 10 parts of tartaric acid, sodium benzoate 2 ~ 6 parts, titanium chloride 3 ~ 10 parts, diphenol propane 1 ~ 6 part, malonic acid 2 ~ 8 parts, vinyl silanes 1 ~ 6 part, 2 ~ 10 parts of surfactant, molybdate 3 ~ 12 parts, polyvinyl alcohol 0.1 ~ 2 part, 30 ~ 50 parts of water.
The most according to claim 1, plated steel sheet surface processes chromium-free passivation liquid, it is characterised in that: described molybdate is sodium molybdate or ammonium molybdate.
The most according to claim 1, plated steel sheet surface processes chromium-free passivation liquid, it is characterised in that: described surfactant is tannic acid or Cetyl bromo-pyridine.
The most according to claim 1, plated steel sheet surface processes chromium-free passivation liquid, it is characterised in that: component and each constituent mass number are as follows: Zinc vanadate 4 ~ 7 parts, lithium vanadate 8 ~ 12 parts, potassium metavanadate 2 ~ 5 parts, 4 ~ 8 parts of tartaric acid, sodium benzoate 3 ~ 5 parts, titanium chloride 5 ~ 8 parts, diphenol propane 2 ~ 5 parts, malonic acid 4 ~ 6 parts, vinyl silanes 2 ~ 5 parts, 4 ~ 8 parts of surfactant, molybdate 6 ~ 10 parts, polyvinyl alcohol 0.5 ~ 1.5 part, 35 ~ 45 parts of water.
The most according to claim 1, plated steel sheet surface processes chromium-free passivation liquid, it is characterised in that: component and each constituent mass number are as follows: Zinc vanadate 5.5 parts, lithium vanadate 10 parts, potassium metavanadate 3.5 parts, 6 parts of tartaric acid, sodium benzoate 4 parts, titanium chloride 6.5 parts, diphenol propane 3.5 parts, malonic acid 5 parts, vinyl silanes 3.5 parts, 6 parts of surfactant, molybdate 8 parts, polyvinyl alcohol 1 part, 40 parts of water.
6. plated steel sheet surface described in claim 1 processes the preparation method of chromium-free passivation liquid, it is characterized in that, polyvinyl alcohol is dissolved in the water of 1/4 working volume, be heated to 70 ~ 90 DEG C, add remaining ingredient after cooling, stir and i.e. obtain plated steel sheet surface process chromium-free passivation liquid.
Plated steel sheet surface the most according to claim 6 processes the preparation method of chromium-free passivation liquid, it is characterised in that: it is heated to 80 DEG C.
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|---|---|---|---|
| CN201610474467.9A CN105951078A (en) | 2016-06-27 | 2016-06-27 | Chromate-free passivation liquid for surface treatment of electro-galvanized steel sheet and preparing method of chromate-free passivation liquid |
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| CN201610474467.9A CN105951078A (en) | 2016-06-27 | 2016-06-27 | Chromate-free passivation liquid for surface treatment of electro-galvanized steel sheet and preparing method of chromate-free passivation liquid |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1598055A (en) * | 2004-08-02 | 2005-03-23 | 吉林大学 | Magnesium alloy phosphorization solution and its phosphorized technology |
| CN102234800A (en) * | 2011-07-27 | 2011-11-09 | 华南理工大学 | Aluminum alloy rare earth passivating liquid taking chlorine salt as accelerator and use method thereof |
| CN102312234A (en) * | 2011-10-20 | 2012-01-11 | 无锡伊佩克科技有限公司 | Passivating solution for plated metal |
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- 2016-06-27 CN CN201610474467.9A patent/CN105951078A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1598055A (en) * | 2004-08-02 | 2005-03-23 | 吉林大学 | Magnesium alloy phosphorization solution and its phosphorized technology |
| CN102234800A (en) * | 2011-07-27 | 2011-11-09 | 华南理工大学 | Aluminum alloy rare earth passivating liquid taking chlorine salt as accelerator and use method thereof |
| CN102312234A (en) * | 2011-10-20 | 2012-01-11 | 无锡伊佩克科技有限公司 | Passivating solution for plated metal |
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