CN105937029A - Method for preparing inorganic-organic composite passivation solution - Google Patents
Method for preparing inorganic-organic composite passivation solution Download PDFInfo
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- CN105937029A CN105937029A CN201610489146.6A CN201610489146A CN105937029A CN 105937029 A CN105937029 A CN 105937029A CN 201610489146 A CN201610489146 A CN 201610489146A CN 105937029 A CN105937029 A CN 105937029A
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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
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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
- 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 provides a method for preparing an inorganic-organic composite passivation solution. The method comprises the steps that nanosilicon dioxide is firstly added into water, polyvinyl chloride, citric acid and sodium bicarbonate are added, temperature is raised, a hydrochloric acid aqueous solution is added dropwise, stirring is carried out, the temperature is reduced to room temperature, filtering is carried out, and modified nanosilicon dioxide is obtained; then titanyl sulfate and sodium vanadate are added into H2O2, dispersing is carried out, and a complexing solution is obtained; then sodium molybdate is added into water, pH is adjusted to be neutral, the modified nanosilicon dioxide, accelerant and a film-forming agent are added, and an inorganic salt passivation solution is obtained; and finally a silane coupling agent KH570 and a silane coupling agent KH858 are added into ethanol water, pH is adjusted, the inorganic salt passivation solution is added, ultrasonic treatment is carried out, and the inorganic-organic composite passivation solution is obtained. The inorganic-organic composite passivation solution is an environment-friendly product and contains no heavy metal ions or volatile organic solvents polluting the environment; the passivation treatment process is simple and low in cost; and the inorganic-organic composite passivation solution can gradually replace a traditional chromate passivation solution, and environment-friendly production of galvanized plate passivation is achieved.
Description
Technical field
The invention belongs to passivating solution technical field, be specifically related to the preparation method of a kind of inorganic-organic hybrid passivating solution.
Background technology
Hot-dip galvanized steel sheet, will immerse in the zinc groove melted by sheet metal, make the sheet metal of its one layer of zinc of surface adhesion, this galvanized steel plain sheet mainly uses continuous zinc coating technique to produce, i.e. the steel plate of rolling is immersed in continuously melt to have in the coating bath of zinc and makes galvanized steel plain sheet, it is simple that galvanizing has technique, equipment easy care, the sheet material coating produced uniformly, the advantage such as corrosion resistance and good.
At present; hot-dip galvanized steel sheet is in process of production frequently with chromium-free deactivation; chromium-free deactivation is broadly divided into inorganic matter passivation and Organic substance is passivated; if individually using inorganic passivation; the decay resistance of passivation caudacoria layer can not meet Standard; and the inorganic salt film layer that formed is relatively thin, acid resistance, alkali resistance and puncture can etc. the most also can not meet demand of industrial production, thus fail large-scale production application；The adhesive force of Organic substance passivation is poor, and during baking and curing, film layer easily cracks problem, and its welding performance is the best, it is also difficult to reach user's requirement, equally can not large-scale industrial production application.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art to provide the preparation method of a kind of inorganic-organic hybrid passivating solution, gained passivating solution has good salt-fog resistant test, coating performance and adhesion performance.
The preparation method of a kind of inorganic-organic hybrid passivating solution, comprises the following steps:
Step 1, in parts by weight, nano silicon 10 parts is added in 20 parts of water, add polrvinyl chloride 3～7 parts, citric acid 2～5 parts, sodium bicarbonate 1～6 parts, be warming up to 40～60 DEG C, dropping 10v/v% aqueous hydrochloric acid solution 3～10 parts, stirring, it is cooled to room temperature, filters, obtain modified manometer silicon dioxide；
Step 2, in parts by weight, adds to 30v/v%H by titanyl sulfate 2～6 parts, vanadic acid sodium 2～6 parts2O2In 5～10 parts, dispersion, obtain complex liquid；
Step 3, in parts by weight, adds to sodium molybdate 10 parts in 20 parts of water, and regulation pH, to neutral, add modified manometer silicon dioxide 5～8 parts, accelerator 2～5 parts and film former 2～5 parts, obtains inorganic salt passivating solution under stirring condition；
Step 4, in parts by weight, by silane coupler KH570
3～7 parts and KH858
2～6 parts add to, in ethanol water 10～20 parts, regulate pH to 4～5, add inorganic salt passivating solution under stirring condition, ultrasonic, to obtain final product.
Further, in step 1, stirring condition is 300～600rpm, 30～50min.
Further, in step 2, dispersion condition is 1000～1500rpm, 20～30min.
Further, step 3 use organic acid for adjusting pH to neutral.
Further, in step 4, the concentration of ethanol water is 15～30v/v%.
Further, step 4 uses 10v/v%HNO3Regulation pH to 4～5.
Further, in step 4, ultrasound condition is 70～120W, 20～30min.
The inorganic-organic hybrid passivating solution of the present invention is environmental type product; heavy metal ion without any pollution environment and volatile organic solvent; passivation process is simple, low cost, can progressively substitute traditional chromating liquid, it is achieved the environmental protection metaplasia of galvanized sheet passivation is produced.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of inorganic-organic hybrid passivating solution, comprises the following steps:
Step 1, in parts by weight, adds nano silicon 10 parts in 20 parts of water, adds polrvinyl chloride 3 parts, citric acid 2 parts, sodium bicarbonate 1 part, it is warming up to 40 DEG C, drips 10v/v% aqueous hydrochloric acid solution 3 parts, stirring, it is cooled to room temperature, filters, obtain modified manometer silicon dioxide；
Step 2, in parts by weight, adds to 30v/v%H by titanyl sulfate 2 parts, vanadic acid sodium 2 parts2O2
In 5 parts, dispersion, obtain complex liquid；
Step 3, in parts by weight, adds to sodium molybdate 10 parts in 20 parts of water, and regulation pH, to neutral, add modified manometer silicon dioxide 5 parts, accelerator 2 parts and film former 2 parts, obtains inorganic salt passivating solution under stirring condition；
Step 4, in parts by weight, by silane coupler KH570
3 parts and KH858 2 parts add in ethanol water 10 parts, regulate pH to 4, add inorganic salt passivating solution under stirring condition, ultrasonic, to obtain final product.
Wherein, in step 1, stirring condition is 300rpm, 50min；In step 2, dispersion condition is 1000rpm, 30min；Step 3 use organic acid for adjusting pH to neutral；In step 4, the concentration of ethanol water is 15v/v%, uses 10v/v%HNO3Regulation pH to 4～5, ultrasound condition is 70W, 30min.
Being coated on galvanized sheet by gained passivating solution, baking and curing temperature is 100 DEG C, and the organosilan composite passivation film drop of the resistance to copper sulfate time of formation reaches 220s；96h neutral salt spray test occurs that the area of white rust is only 4%, meets GB10125-1997 standard-required, and its resistance to chemical corrosion can be close to chromate passivation film；Scanning electron microscope (SEM) analysis result shows that the surface of passivating film is smooth, uniform, compact structure.
Embodiment 2
The preparation method of a kind of inorganic-organic hybrid passivating solution, comprises the following steps:
Step 1, in parts by weight, adds nano silicon 10 parts in 20 parts of water, adds polrvinyl chloride 5 parts, citric acid 3 parts, sodium bicarbonate 3 parts, it is warming up to 50 DEG C, drips 10v/v% aqueous hydrochloric acid solution 6 parts, stirring, it is cooled to room temperature, filters, obtain modified manometer silicon dioxide；
Step 2, in parts by weight, adds to 30v/v%H by titanyl sulfate 5 parts, vanadic acid sodium 4 parts2O2
In 7 parts, dispersion, obtain complex liquid；
Step 3, in parts by weight, adds to sodium molybdate 10 parts in 20 parts of water, and regulation pH, to neutral, add modified manometer silicon dioxide 6 parts, accelerator 4 parts and film former 3 parts, obtains inorganic salt passivating solution under stirring condition；
Step 4, in parts by weight, by silane coupler KH570
5 parts and KH858 4 parts add in ethanol water 17 parts, regulate pH to 4, add inorganic salt passivating solution under stirring condition, ultrasonic, to obtain final product.
Wherein, in step 1, stirring condition is 400rpm, 40min；In step 2, dispersion condition is 1200rpm, 25min；Step 3 use organic acid for adjusting pH to neutral；In step 4, the concentration of ethanol water is 20v/v%, uses 10v/v% HNO3Regulation pH to 4～5, ultrasound condition is 100W, 20min.
Being coated on galvanized sheet by gained passivating solution, baking and curing temperature is 100 DEG C, and the organosilan composite passivation film drop of the resistance to copper sulfate time of formation reaches 210s；96h neutral salt spray test occurs that the area of white rust is only 5%, meets GB10125-1997 standard-required, and its resistance to chemical corrosion can be close to chromate passivation film；Scanning electron microscope (SEM) analysis result shows that the surface of passivating film is smooth, uniform, compact structure.
Embodiment 3
The preparation method of a kind of inorganic-organic hybrid passivating solution, comprises the following steps:
Step 1, in parts by weight, adds nano silicon 10 parts in 20 parts of water, adds polrvinyl chloride 6 parts, citric acid 3 parts, sodium bicarbonate 2 parts, it is warming up to 50 DEG C, drips 10v/v% aqueous hydrochloric acid solution 7 parts, stirring, it is cooled to room temperature, filters, obtain modified manometer silicon dioxide；
Step 2, in parts by weight, adds to 30v/v%H by titanyl sulfate 5 parts, vanadic acid sodium 3 parts2O2
In 9 parts, dispersion, obtain complex liquid；
Step 3, in parts by weight, adds to sodium molybdate 10 parts in 20 parts of water, and regulation pH, to neutral, add modified manometer silicon dioxide 7 parts, accelerator 4 parts and film former 3 parts, obtains inorganic salt passivating solution under stirring condition；
Step 4, in parts by weight, by silane coupler KH570
6 parts and KH858 4 parts add in ethanol water 17 parts, regulate pH to 4, add inorganic salt passivating solution under stirring condition, ultrasonic, to obtain final product.
Wherein, in step 1, stirring condition is 300rpm, 50min；In step 2, dispersion condition is 1000rpm, 30min；Step 3 use organic acid for adjusting pH to neutral；In step 4, the concentration of ethanol water is 15v/v%, uses 10v/v%HNO3Regulation pH to 4～5, ultrasound condition is 70W, 30min.
Being coated on galvanized sheet by gained passivating solution, baking and curing temperature is 100 DEG C, and the organosilan composite passivation film drop of the resistance to copper sulfate time of formation reaches 235s；96h neutral salt spray test occurs that the area of white rust is only 3%, meets GB10125-1997 standard-required, and its resistance to chemical corrosion can be close to chromate passivation film；Scanning electron microscope (SEM) analysis result shows that the surface of passivating film is smooth, uniform, compact structure.
Embodiment 4
The preparation method of a kind of inorganic-organic hybrid passivating solution, comprises the following steps:
Step 1, in parts by weight, adds nano silicon 10 parts in 20 parts of water, adds polrvinyl chloride 7 parts, citric acid 5 parts, sodium bicarbonate 6 parts, it is warming up to 60 DEG C, drips 10v/v% aqueous hydrochloric acid solution 10 parts, stirring, it is cooled to room temperature, filters, obtain modified manometer silicon dioxide；
Step 2, in parts by weight, adds to 30v/v%H by titanyl sulfate 6 parts, vanadic acid sodium 6 parts2O2
In 10 parts, dispersion, obtain complex liquid；
Step 3, in parts by weight, adds to sodium molybdate 10 parts in 20 parts of water, and regulation pH, to neutral, add modified manometer silicon dioxide 8 parts, accelerator 5 parts and film former 5 parts, obtains inorganic salt passivating solution under stirring condition；
Step 4, in parts by weight, by silane coupler KH570
7 parts and KH858 6 parts add in ethanol water 20 parts, regulate pH to 4, add inorganic salt passivating solution under stirring condition, ultrasonic, to obtain final product.
Wherein, in step 1, stirring condition is 600rpm, 30min；In step 2, dispersion condition is 1500rpm, 20min；Step 3 use organic acid for adjusting pH to neutral；In step 4, the concentration of ethanol water is 30v/v%, uses 10v/v%HNO3Regulation pH to 4～5, ultrasound condition is 120W, 20min.
Being coated on galvanized sheet by gained passivating solution, baking and curing temperature is 100 DEG C, and the organosilan composite passivation film drop of the resistance to copper sulfate time of formation reaches 205s；96h neutral salt spray test occurs that the area of white rust is only 6%, meets GB10125-1997 standard-required, and its resistance to chemical corrosion can be close to chromate passivation film；Scanning electron microscope (SEM) analysis result shows that the surface of passivating film is smooth, uniform, compact structure.
Claims (7)
1. the preparation method of an inorganic-organic hybrid passivating solution, it is characterised in that: comprise the following steps:
Step 1, in parts by weight, nano silicon 10 parts is added in 20 parts of water, add polrvinyl chloride 3～7 parts, citric acid 2～5 parts, sodium bicarbonate 1～6 parts, be warming up to 40～60 DEG C, dropping 10v/v% aqueous hydrochloric acid solution 3～10 parts, stirring, it is cooled to room temperature, filters, obtain modified manometer silicon dioxide；
Step 2, in parts by weight, adds to 30v/v%H by titanyl sulfate 2～6 parts, vanadic acid sodium 2～6 parts2O2In 5～10 parts, dispersion, obtain complex liquid；
Step 3, in parts by weight, adds to sodium molybdate 10 parts in 20 parts of water, and regulation pH, to neutral, add modified manometer silicon dioxide 5～8 parts, accelerator 2～5 parts and film former 2～5 parts, obtains inorganic salt passivating solution under stirring condition；
Step 4, in parts by weight, adds to silane coupler KH570 3～7 parts and KH858 2～6 parts, in ethanol water 10～20 parts, regulate pH to 4～5, adds inorganic salt passivating solution under stirring condition, ultrasonic, to obtain final product.
The preparation method of inorganic-organic hybrid passivating solution the most according to claim 1, it is characterised in that: in step 1, stirring condition is 300～600rpm, 30～50min.
The preparation method of inorganic-organic hybrid passivating solution the most according to claim 1, it is characterised in that: in step 2, dispersion condition is 1000～1500rpm, 20～30min.
The preparation method of inorganic-organic hybrid passivating solution the most according to claim 1, it is characterised in that: step 3 use organic acid for adjusting pH to neutral.
The preparation method of inorganic-organic hybrid passivating solution the most according to claim 1, it is characterised in that: in step 4, the concentration of ethanol water is 15～30v/v%.
The preparation method of inorganic-organic hybrid passivating solution the most according to claim 1, it is characterised in that: step 4 uses 10v/v%HNO3Regulation pH to 4～5.
The preparation method of inorganic-organic hybrid passivating solution the most according to claim 1, it is characterised in that: in step 4, ultrasound condition is 70～120W, 20～30min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106637172A (en) * | 2016-12-30 | 2017-05-10 | 张庆 | Fluorine-containing self-lubrication environment-friendly silane passivation film |
| CN106756942A (en) * | 2016-12-16 | 2017-05-31 | 安徽宝恒新材料科技有限公司 | A kind of stainless steel chromium-free passivation liquid |
| CN106756953A (en) * | 2016-12-30 | 2017-05-31 | 张庆 | A kind of polyvinyl alcohol Chrome-free corrosion resistant type silane passivating film |
| CN106835108A (en) * | 2016-12-30 | 2017-06-13 | 张庆 | A kind of environmentally friendly inorganic organic passivation film of modified graphene oxide |
| CN106835100A (en) * | 2016-12-30 | 2017-06-13 | 张庆 | A kind of polyaniline epoxy resin corrosion resistance composite passivation film |
| CN106939420A (en) * | 2017-03-23 | 2017-07-11 | 合肥协耀玻璃制品有限公司 | A kind of passivation for stainless steel liquid and its passivation technology |
| CN107893253A (en) * | 2017-11-29 | 2018-04-10 | 马鞍山市恒特重工科技有限公司 | A kind of Wear-resisting steel plate for mining machinery |
| CN112481575A (en) * | 2020-11-27 | 2021-03-12 | 广东达志化学科技有限公司 | Hot galvanizing passivation solution and preparation method thereof |
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| CN102070927A (en) * | 2011-01-22 | 2011-05-25 | 安徽工业大学 | Water-based surface treatment agent for color coating pretreatment of galvanized plates |
| CN105441920A (en) * | 2015-11-12 | 2016-03-30 | 上海耀岩化学品有限公司 | Metal surface treatment agent with silane coupling agents as main components and preparation method thereof |
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| CN102070927A (en) * | 2011-01-22 | 2011-05-25 | 安徽工业大学 | Water-based surface treatment agent for color coating pretreatment of galvanized plates |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106756942A (en) * | 2016-12-16 | 2017-05-31 | 安徽宝恒新材料科技有限公司 | A kind of stainless steel chromium-free passivation liquid |
| CN106756942B (en) * | 2016-12-16 | 2019-02-01 | 安徽宝恒新材料科技有限公司 | A kind of stainless steel chromium-free passivation liquid |
| CN106637172A (en) * | 2016-12-30 | 2017-05-10 | 张庆 | Fluorine-containing self-lubrication environment-friendly silane passivation film |
| CN106756953A (en) * | 2016-12-30 | 2017-05-31 | 张庆 | A kind of polyvinyl alcohol Chrome-free corrosion resistant type silane passivating film |
| CN106835108A (en) * | 2016-12-30 | 2017-06-13 | 张庆 | A kind of environmentally friendly inorganic organic passivation film of modified graphene oxide |
| CN106835100A (en) * | 2016-12-30 | 2017-06-13 | 张庆 | A kind of polyaniline epoxy resin corrosion resistance composite passivation film |
| CN106939420A (en) * | 2017-03-23 | 2017-07-11 | 合肥协耀玻璃制品有限公司 | A kind of passivation for stainless steel liquid and its passivation technology |
| CN107893253A (en) * | 2017-11-29 | 2018-04-10 | 马鞍山市恒特重工科技有限公司 | A kind of Wear-resisting steel plate for mining machinery |
| CN112481575A (en) * | 2020-11-27 | 2021-03-12 | 广东达志化学科技有限公司 | Hot galvanizing passivation solution and preparation method thereof |
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