CN105937029B - A kind of preparation method of inorganic-organic hybrid passivating solution - Google Patents
A kind of preparation method of inorganic-organic hybrid passivating solution Download PDFInfo
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- CN105937029B CN105937029B CN201610489146.6A CN201610489146A CN105937029B CN 105937029 B CN105937029 B CN 105937029B CN 201610489146 A CN201610489146 A CN 201610489146A CN 105937029 B CN105937029 B CN 105937029B
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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 present invention provides a kind of preparation methods of inorganic-organic hybrid passivating solution, are first added to the water nano silicon dioxide, and polyvinyl chloride, citric acid, sodium bicarbonate is added, aqueous hydrochloric acid solution, stirring is added dropwise in heating, it is cooled to room temperature, filters, obtains modified manometer silicon dioxide；Titanyl sulfate, sodium vanadate are added into H again2O2In, dispersion obtains complex liquid；Then sodium molybdate is added in water, adjusts pH to neutrality, modified manometer silicon dioxide, accelerating agent and film forming agent is added, obtains inorganic salts passivating solution；Finally silane coupling agent KH570 and KH858 are added in ethanol water, adjust pH, be added inorganic salts passivating solution, ultrasound to get.The inorganic-organic hybrid passivating solution of the present invention is environmental type product; heavy metal ion and volatile organic solvent without any pollution environment; passivation process is simple, at low cost, can gradually substitute traditional chromating liquid, realizes the environmentally protective metaplasia production of galvanized sheet passivation.
Description
Technical field
The invention belongs to passivating solution technical fields, and in particular to a kind of preparation method of inorganic-organic hybrid passivating solution.
Background technology
Sheet metal is immersed in the zinc slot melted, makes the sheet metal of its one layer of zinc of surface adhesion by hot-dip galvanized steel sheet, should
Galvanized steel plain sheet is continuously immersed in coiled steel plate to melt in the coating bath for having zinc mainly using continuous zinc coating technique productions, i.e., is made plating
Zinc steel plate, galvanizing have simple for process, equipment easy care, uniform, corrosion resistance and good of the sheet material coating produced etc. excellent
Point.
Currently, hot-dip galvanized steel sheet is in process of production frequently with chromium-free deactivation, it is blunt that chromium-free deactivation is broadly divided into inorganic matter
Change and organic matter is passivated, if individually using inorganic passivation, the corrosion resistance of film layer can not meet national standard, and shape after passivation
At inorganic salts film layer it is relatively thin, acid resistance, alkali resistance and puncture can etc. equally also can not meet demand of industrial production, to
Fail large-scale production application；The adhesive force of organic matter passivation is poor, and during baking and curing, film layer easy tos produce crackle and asks
Topic, welding performance are bad, it is also difficult to reach user's requirement, equally be unable to scale industrial production application.
Invention content
A kind of preparation of inorganic-organic hybrid passivating solution is provided the purpose of the present invention is overcome the deficiencies in the prior art
Method, gained passivating solution have good salt-fog resistant test, coating performance and adhesion performance.
A kind of preparation method of inorganic-organic hybrid passivating solution, includes the following steps：
Step 1, in parts by weight, 10 parts of nano silicon dioxide is added in 20 parts of water, add 3~7 parts of polyvinyl chloride,
2~5 parts of citric acid, 1~6 part of sodium bicarbonate are warming up to 40~60 DEG C, and 3~10 parts of 10v/v% aqueous hydrochloric acid solutions are added dropwise, and stir,
It is cooled to room temperature, filters, obtains modified manometer silicon dioxide；
Step 2, in parts by weight, 2~6 parts of titanyl sulfate, 2~6 parts of sodium vanadate are added into 30v/v%H2O2In 5~10 parts,
Dispersion, obtains complex liquid；
Step 3, in parts by weight, by sodium molybdate 10 parts add in 20 parts of water, adjust pH to neutrality, be added under stirring condition
2~5 parts of 5~8 parts of modified manometer silicon dioxide, 2~5 parts of accelerating agent and film forming agent, obtain inorganic salts passivating solution；
Step 4, in parts by weight, 2~6 parts of 3~7 parts of silane coupling agent KH570 and KH858 are added into ethanol water
In 10~20 parts, adjust pH to 4~5, be added inorganic salts passivating solution under stirring condition, ultrasound to get.
Further, stirring condition is 300~600rpm, 30~50min in step 1.
Further, dispersion condition is 1000~1500rpm, 20~30min in step 2.
Further, using organic acid for adjusting pH to neutrality in step 3.
Further, in step 4 ethanol water a concentration of 15~30v/v%.
Further, 10v/v%HNO is used in step 43Adjust pH to 4~5.
Further, ultrasound condition is 70~120W, 20~30min in step 4.
The inorganic-organic hybrid passivating solution of the present invention is environmental type product, the heavy metal without any pollution environment
Ion and volatile organic solvent, passivation process is simple, at low cost, can gradually substitute traditional chromating liquid,
Realize the environmentally protective metaplasia production of galvanized sheet passivation.
Specific implementation mode
Embodiment 1
A kind of preparation method of inorganic-organic hybrid passivating solution, includes the following steps：
Step 1, in parts by weight, by 10 parts of 20 parts of water of addition of nano silicon dioxide, 3 parts of polyvinyl chloride, lemon are added
Lemon acid 2 parts, 1 part of sodium bicarbonate, are warming up to 40 DEG C, and 3 parts of 10v/v% aqueous hydrochloric acid solutions are added dropwise, and stirring is cooled to room temperature, filters,
Obtain modified manometer silicon dioxide；
Step 2, in parts by weight, 2 parts of titanyl sulfate, 2 parts of sodium vanadate are added into 30v/v%H2O2 In 5 parts, dispersion obtains
Complex liquid；
Step 3, in parts by weight, by sodium molybdate 10 parts add in 20 parts of water, adjust pH to neutrality, be added under stirring condition
2 parts of 5 parts of modified manometer silicon dioxide, 2 parts of accelerating agent and film forming agent, obtain inorganic salts passivating solution；
Step 4, in parts by weight, 2 parts of 3 parts of silane coupling agent KH570 and KH858 are added into 10 parts of ethanol water
In, adjust pH to 4, be added inorganic salts passivating solution under stirring condition, ultrasound to get.
Wherein, stirring condition is 300rpm, 50min in step 1；Dispersion condition is 1000rpm, 30min in step 2；Step
Using organic acid for adjusting pH to neutrality in rapid 3；A concentration of 15v/v% of ethanol water in step 4, using 10v/v%HNO3It adjusts
Save pH to 4~5, ultrasound condition 70W, 30min.
By gained passivating solution coated on galvanized sheet, baking and curing temperature is 100 DEG C, and the organosilan of formation is composite passivated
The film drop of the resistance to copper sulphate time reaches 220s；The area that white rust occur in 96h neutral salt spray tests is only 4%, meets GB10125-1997
Standard requirement, resistance to chemical corrosion are close to chromate passivation film；Scanning electron microscope（SEM）Analysis result shows blunt
The surface for changing film is smooth, uniform, compact structure.
Embodiment 2
A kind of preparation method of inorganic-organic hybrid passivating solution, includes the following steps：
Step 1, in parts by weight, by 10 parts of 20 parts of water of addition of nano silicon dioxide, 5 parts of polyvinyl chloride, lemon are added
Lemon acid 3 parts, 3 parts of sodium bicarbonate, are warming up to 50 DEG C, and 6 parts of 10v/v% aqueous hydrochloric acid solutions are added dropwise, and stirring is cooled to room temperature, filters,
Obtain modified manometer silicon dioxide；
Step 2, in parts by weight, 5 parts of titanyl sulfate, 4 parts of sodium vanadate are added into 30v/v%H2O2 In 7 parts, dispersion obtains
Complex liquid；
Step 3, in parts by weight, by sodium molybdate 10 parts add in 20 parts of water, adjust pH to neutrality, be added under stirring condition
3 parts of 6 parts of modified manometer silicon dioxide, 4 parts of accelerating agent and film forming agent, obtain inorganic salts passivating solution；
Step 4, in parts by weight, 4 parts of 5 parts of silane coupling agent KH570 and KH858 are added into 17 parts of ethanol water
In, adjust pH to 4, be added inorganic salts passivating solution under stirring condition, ultrasound to get.
Wherein, stirring condition is 400rpm, 40min in step 1；Dispersion condition is 1200rpm, 25min in step 2；Step
Using organic acid for adjusting pH to neutrality in rapid 3；A concentration of 20v/v% of ethanol water in step 4, using 10v/v% HNO3It adjusts
Save pH to 4~5, ultrasound condition 100W, 20min.
By gained passivating solution coated on galvanized sheet, baking and curing temperature is 100 DEG C, and the organosilan of formation is composite passivated
The film drop of the resistance to copper sulphate time reaches 210s；The area that white rust occur in 96h neutral salt spray tests is only 5%, meets GB10125-1997
Standard requirement, resistance to chemical corrosion are close to chromate passivation film；Scanning electron microscope（SEM）Analysis result shows blunt
The surface for changing film is smooth, uniform, compact structure.
Embodiment 3
A kind of preparation method of inorganic-organic hybrid passivating solution, includes the following steps：
Step 1, in parts by weight, by 10 parts of 20 parts of water of addition of nano silicon dioxide, 6 parts of polyvinyl chloride, lemon are added
Lemon acid 3 parts, 2 parts of sodium bicarbonate, are warming up to 50 DEG C, and 7 parts of 10v/v% aqueous hydrochloric acid solutions are added dropwise, and stirring is cooled to room temperature, filters,
Obtain modified manometer silicon dioxide；
Step 2, in parts by weight, 5 parts of titanyl sulfate, 3 parts of sodium vanadate are added into 30v/v%H2O2 In 9 parts, dispersion obtains
Complex liquid；
Step 3, in parts by weight, by sodium molybdate 10 parts add in 20 parts of water, adjust pH to neutrality, be added under stirring condition
3 parts of 7 parts of modified manometer silicon dioxide, 4 parts of accelerating agent and film forming agent, obtain inorganic salts passivating solution；
Step 4, in parts by weight, 4 parts of 6 parts of silane coupling agent KH570 and KH858 are added into 17 parts of ethanol water
In, adjust pH to 4, be added inorganic salts passivating solution under stirring condition, ultrasound to get.
Wherein, stirring condition is 300rpm, 50min in step 1；Dispersion condition is 1000rpm, 30min in step 2；Step
Using organic acid for adjusting pH to neutrality in rapid 3；A concentration of 15v/v% of ethanol water in step 4, using 10v/v%HNO3It adjusts
Save pH to 4~5, ultrasound condition 70W, 30min.
By gained passivating solution coated on galvanized sheet, baking and curing temperature is 100 DEG C, and the organosilan of formation is composite passivated
The film drop of the resistance to copper sulphate time reaches 235s；The area that white rust occur in 96h neutral salt spray tests is only 3%, meets GB10125-1997
Standard requirement, resistance to chemical corrosion are close to chromate passivation film；Scanning electron microscope（SEM）Analysis result shows blunt
The surface for changing film is smooth, uniform, compact structure.
Embodiment 4
A kind of preparation method of inorganic-organic hybrid passivating solution, includes the following steps：
Step 1, in parts by weight, by 10 parts of 20 parts of water of addition of nano silicon dioxide, 7 parts of polyvinyl chloride, lemon are added
Lemon acid 5 parts, 6 parts of sodium bicarbonate, are warming up to 60 DEG C, and 10 parts of 10v/v% aqueous hydrochloric acid solutions are added dropwise, and stirring is cooled to room temperature, filters,
Obtain modified manometer silicon dioxide；
Step 2, in parts by weight, 6 parts of titanyl sulfate, 6 parts of sodium vanadate are added into 30v/v%H2O2 In 10 parts, dispersion obtains
To complex liquid；
Step 3, in parts by weight, by sodium molybdate 10 parts add in 20 parts of water, adjust pH to neutrality, be added under stirring condition
5 parts of 8 parts of modified manometer silicon dioxide, 5 parts of accelerating agent and film forming agent, obtain inorganic salts passivating solution；
Step 4, in parts by weight, 6 parts of 7 parts of silane coupling agent KH570 and KH858 are added into 20 parts of ethanol water
In, adjust pH to 4, be added inorganic salts passivating solution under stirring condition, ultrasound to get.
Wherein, stirring condition is 600rpm, 30min in step 1；Dispersion condition is 1500rpm, 20min in step 2；Step
Using organic acid for adjusting pH to neutrality in rapid 3；A concentration of 30v/v% of ethanol water in step 4, using 10v/v%HNO3It adjusts
Save pH to 4~5, ultrasound condition 120W, 20min.
By gained passivating solution coated on galvanized sheet, baking and curing temperature is 100 DEG C, and the organosilan of formation is composite passivated
The film drop of the resistance to copper sulphate time reaches 205s；The area that white rust occur in 96h neutral salt spray tests is only 6%, meets GB10125-1997
Standard requirement, resistance to chemical corrosion are close to chromate passivation film；Scanning electron microscope（SEM）Analysis result shows blunt
The surface for changing film is smooth, uniform, compact structure.
Claims (7)
1. a kind of preparation method of inorganic-organic hybrid passivating solution, it is characterised in that：Include the following steps：
Step 1, in parts by weight, by 10 parts of 20 parts of water of addition of nano silicon dioxide, 3~7 parts of polyvinyl chloride, lemon are added
Sour 2~5 parts, 1~6 part of sodium bicarbonate, are warming up to 40~60 DEG C, and 3~10 parts of 10v/v% aqueous hydrochloric acid solutions are added dropwise, and stir, cooling
To room temperature, filtering obtains modified manometer silicon dioxide；
Step 2, in parts by weight, 2~6 parts of titanyl sulfate, 2~6 parts of sodium vanadate are added into 30v/v%H2O2In 5~10 parts, point
It dissipates, obtains complex liquid；
Step 3, in parts by weight, by sodium molybdate 10 parts add in 20 parts of water, adjust pH to neutrality, be added and be modified under stirring condition
2~5 parts of 5~8 parts of nano silicon dioxide, 2~5 parts of accelerating agent and film forming agent, obtain inorganic salts passivating solution；
Step 4, in parts by weight, by 2~6 parts of 3~7 parts of silane coupling agent KH570 and KH858 add to ethanol water 10~
In 20 parts, adjust pH to 4~5, be added inorganic salts passivating solution under stirring condition, ultrasound to get.
2. the preparation method of inorganic-organic hybrid passivating solution according to claim 1, it is characterised in that：It is stirred in step 1
Condition is 300~600rpm, 30~50min.
3. the preparation method of inorganic-organic hybrid passivating solution according to claim 1, it is characterised in that：Disperse in step 2
Condition is 1000~1500rpm, 20~30min.
4. the preparation method of inorganic-organic hybrid passivating solution according to claim 1, it is characterised in that：It is used in step 3
Organic acid for adjusting pH is to neutrality.
5. the preparation method of inorganic-organic hybrid passivating solution according to claim 1, it is characterised in that：Ethyl alcohol in step 4
A concentration of 15~30v/v% of aqueous solution.
6. the preparation method of inorganic-organic hybrid passivating solution according to claim 1, it is characterised in that：It is used in step 4
10v/v%HNO3Adjust pH to 4~5.
7. the preparation method of inorganic-organic hybrid passivating solution according to claim 1, it is characterised in that：It is ultrasonic in step 4
Condition is 70~120W, 20~30min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN106756953A (en) * | 2016-12-30 | 2017-05-31 | 张庆 | A kind of polyvinyl alcohol Chrome-free corrosion resistant type silane passivating film |
| CN106637172A (en) * | 2016-12-30 | 2017-05-10 | 张庆 | Fluorine-containing self-lubrication environment-friendly silane passivation 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Effective date of registration: 20201231 Address after: 236214 Dingzhuang, Shili village, Nanzhao Town, Yingshang County, Fuyang City, Anhui Province Patentee after: YINGSHANG SHILI ECOLOGICAL AGRICULTURE Co.,Ltd. Address before: 325000 3 lane, Bai Lou, Shuang Yu Street, Lucheng District, Wenzhou, Zhejiang. Patentee before: Zhou Xiangzhu |