CN103031548B - A kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof - Google Patents
A kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof Download PDFInfo
- Publication number
- CN103031548B CN103031548B CN201210550917.XA CN201210550917A CN103031548B CN 103031548 B CN103031548 B CN 103031548B CN 201210550917 A CN201210550917 A CN 201210550917A CN 103031548 B CN103031548 B CN 103031548B
- Authority
- CN
- China
- Prior art keywords
- water
- zinc oxide
- ammonium metavanadate
- weight portion
- nano zinc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses a kind of metal surface silane finish that contains ammonium metavanadate, it is characterized in that the mixed liquor formulated by following component, the weight portion of each component in every liter of mixed liquor (gram) be: 3-(isobutene acyl-oxygen) propyl trimethoxy silicane 22-32, N-? phenyl-3-TSL 8330 27-40, water nano zinc oxide material 100-190, ethylenediamine tetramethylene fork Alendronate 3-5, propenyl 3-4, propane diols 3-4, zirconium fluoride 2-3, one hydration ammonia 2-3, diethanol amine 1-2, dimethyl sulfoxide (DMSO) 1-2, ammonium metavanadate 0.8-1, diethylene glycol butyl ether 0.7-0.9, remaining is water, the water nano zinc oxide material of preparing by technique of the present invention has high dispersion stability and efficient cohesive, the auxiliary agents such as it is evenly distributed in metal surface, makes metal have high compactness and the permeability of anti-ion, the ethylenediamine tetramethylene adding fork Alendronate, increase the density of silane adsorbed film, improved quality of forming film, made rete there is strong adhesion, without cavity, split sunken, evenly fine and close, the feature that polarized current density is little, and production process environmental protection, pollution-free.
Description
Technical field
The present invention relates generally to a kind of metal surface silane finish and preparation method thereof, relates in particular to a kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof.
Background technology
In field of metal surface treatment, although traditional phosphate conversion and chromating process for treating surface can obtain good effect, but contain zinc in the waste liquid of discharging in processing procedure, manganese, nickel, the carcinogens such as heavy metal ion and nitrite such as chromium, environmental pollution is very serious, and metallic surface silanization treatment technology is due to the material of hurm involved environment not, energy consumption in production process is low, technical applications is extensive, being considered to be expected to replace phosphate conversion processes and chromating processing, that latest development direction is protected separately in metal surface, the rete that the surface of workpiece that in existing technology, solution of silane was processed forms, Density inhomogeneity, there is cavity, split sunken, put forth effort not strong with holding up of metallic object.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, and metal surface silane finish of a kind of water nano zinc oxide material and preparation method thereof is provided.
The present invention is achieved by the following technical solutions:
A metal surface silane finish that contains ammonium metavanadate, by the formulated mixed liquor of following component, the weight portion of each component in every liter of mixed liquor (gram) be:
3-(isobutene acyl-oxygen) propyl trimethoxy silicane 22-32, N-phenyl-3-TSL 8330 27-40, water nano zinc oxide material 100-190, ethylenediamine tetramethylene fork Alendronate 3-5, propenyl 3-4, propane diols 3-4, zirconium fluoride 2-3, a hydration ammonia 2-3, diethanol amine 1-2, dimethyl sulfoxide (DMSO) 1-2, ammonium metavanadate 0.8-1, diethylene glycol butyl ether 0.7-0.9, remaining be water;
The preparation method of described water nano zinc oxide material is:
(1) be scattered in its quality 5-10 absolute ethyl alcohol doubly ultrasonic nano zine oxide, obtain dispersion liquid, then the anilinomethyl triethoxysilane of the cumyl peroxide of its quality 3-4%, 1-2% is added in above-mentioned dispersion liquid, back flow reaction 1-2 hour at 80-90 DEG C of temperature, after reaction, obtain the coupling agent modified nano zine oxide-alcohol suspension with reactive group, then filter, centrifugation filtrate, obtains modified nano zinc oxide;
(2) glycerine is water-soluble, then add above-mentioned modified nano zinc oxide, ball-milling treatment 1-2 hour in ball mill, obtains modified nano zinc oxide slurry;
(3) N-phenyl-3-TSL 8330 is dissolved in ethanol, be prepared into the solution that mass concentration is 2-4%, join in above-mentioned modified nano zinc oxide slurry, regulating pH value with acetic acid or sodium acetate is 4-5, ball-milling treatment 2-3 hour again, obtains described water nano zinc oxide material.
In the preparation method of described water nano zinc oxide material, the mass ratio of the water in described nano zine oxide, glycerine, N-phenyl-3-TSL 8330 and step (2), the ethanol in step (3) is: nano zine oxide: glycerine: N-phenyl-3-TSL 8330: water: ethanol is 10-15g:1-2g:2-4g:95-105 gram: 95-105 gram.
The granularity of described nano zine oxide is 40-50nm.
A preparation method for the metal surface silane finish that contains ammonium metavanadate, comprises the following steps:
(1) 3-of above-mentioned weight portion (isobutene acyl-oxygen) propyl trimethoxy silicane is added in the water of above-mentioned weight portion 60-70%, after fully dissolving, add again N-phenyl-3-TSL 8330 of above-mentioned weight portion, fully stir, obtain compound A;
(2) get the 50-60% that remains water, add the water nano zinc oxide material of above-mentioned weight portion, after fully stirring, add ethylenediamine tetramethylene fork Alendronate, zirconium fluoride, diethanol amine, the dimethyl sulfoxide (DMSO) of above-mentioned weight portion fully to stir, obtain compound B;
(3) propenyl of above-mentioned weight portion, diethylene glycol butyl ether, a hydration ammonia are mixed with remaining water, then add the ammonium metavanadate of above-mentioned weight portion, be stirred to ammonium metavanadate and dissolve completely, obtain compound C;
(4) compound A obtained above, B and C are mixed, then acetic acid or sodium acetate, adjusting PH is 3-5, finally adds the each raw material of residue, the metal surface silane finish that contains ammonium metavanadate described in obtaining after fully stirring.
The concentration of the hydration ammonia described in raw material is 3-5%.
Advantage of the present invention is:
Use silane surface inorganic agent of the present invention to process the silane coating forming in metal surface after metal and there is excellent decay resistance, extend the service life of metal, by the use that combines of 3-(isobutene acyl-oxygen) propyl trimethoxy silicane and N-phenyl-3-TSL 8330, can form densification in metal surface and coating firmly, and the water nano zinc oxide material of preparing by technique of the present invention has high dispersion stability and efficient cohesive, it is evenly distributed in metal surface, make metal there is high compactness and the permeability of anti-ion, the auxiliary agents such as the ethylenediamine tetramethylene fork Alendronate adding, increase the density of silane adsorbed film, improve quality of forming film, make rete there is strong adhesion, without cavity, split sunken, evenly fine and close, the feature that polarized current density is little, and production process environmental protection, pollution-free.
Detailed description of the invention
Embodiment 1
A metal surface silane finish that contains ammonium metavanadate, by the formulated mixed liquor of following component, the weight portion of each component in every liter of mixed liquor (gram) be:
3-(isobutene acyl-oxygen) propyl trimethoxy silicane 32, N-phenyl-3-TSL 8330 40, water nano zinc oxide material 190, ethylenediamine tetramethylene fork Alendronate 5, propenyl 4, propane diols 4, zirconium fluoride 3, a hydration ammonia 3, diethanol amine 1, dimethyl sulfoxide (DMSO) 1, ammonium metavanadate 0.8, diethylene glycol butyl ether 0.9, remaining be water;
The preparation method of described water nano zinc oxide material is:
(1) by the ultrasonic nano zine oxide absolute ethyl alcohol that is scattered in 10 times of its quality, obtain dispersion liquid, then the cumyl peroxide of its quality 3%, 2% anilinomethyl triethoxysilane are added in above-mentioned dispersion liquid, back flow reaction 2 hours at 90 DEG C of temperature, after reaction, obtain the coupling agent modified nano zine oxide-alcohol suspension with reactive group, then filter, centrifugation filtrate, obtains modified nano zinc oxide;
(2) glycerine is water-soluble, then add above-mentioned modified nano zinc oxide, in ball mill, ball-milling treatment 2 hours, obtains modified nano zinc oxide slurry;
(3) N-phenyl-3-TSL 8330 is dissolved in ethanol, be prepared into mass concentration and be 2% solution, join in above-mentioned modified nano zinc oxide slurry, regulating pH value with acetic acid or sodium acetate is 5, ball-milling treatment 2 hours again, obtains described water nano zinc oxide material.
In the preparation method of described water nano zinc oxide material, the mass ratio of the water in described nano zine oxide, glycerine, N-phenyl-3-TSL 8330 and step (2), the ethanol in step (3) is: nano zine oxide: glycerine: N-phenyl-3-TSL 8330: water: ethanol is 15g:1g:4g:105 gram: 105 grams.
The granularity of described nano zine oxide is 50nm.
A preparation method for the metal surface silane finish that contains ammonium metavanadate, comprises the following steps:
(1) 3-of above-mentioned weight portion (isobutene acyl-oxygen) propyl trimethoxy silicane is added in the water of above-mentioned weight portion 70%, after fully dissolving, add again N-phenyl-3-TSL 8330 of above-mentioned weight portion, fully stir, obtain compound A;
(2) get 60% of residue water, add the water nano zinc oxide material of above-mentioned weight portion, after fully stirring, add ethylenediamine tetramethylene fork Alendronate, zirconium fluoride, diethanol amine, the dimethyl sulfoxide (DMSO) of above-mentioned weight portion fully to stir, obtain compound B;
(3) propenyl of above-mentioned weight portion, diethylene glycol butyl ether, a hydration ammonia are mixed with remaining water, then add the ammonium metavanadate of above-mentioned weight portion, be stirred to ammonium metavanadate and dissolve completely, obtain compound C;
(4) compound A obtained above, B and C are mixed, then acetic acid or sodium acetate, adjusting PH is 3-5, finally adds the each raw material of residue, the metal surface silane finish that contains ammonium metavanadate described in obtaining after fully stirring.
The concentration of the hydration ammonia described in raw material is 5%.
Performance test:
Bending viscosity:
Process metal aluminium flake with silane surface inorganic agent of the present invention, by bending aluminium flake doubling 60 degree, peel off sweep 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless; Process metal aluminium flake with silane surface inorganic agent of the present invention, aluminium flake is soaked in boiling water 1 hour, at room temperature place 24 hours, then by bending aluminium flake doubling 60 degree, peel off sweep 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless;
Corrosion resistance:
Process galvanized steel plain sheet metal material with silane surface inorganic agent of the present invention, by this material lateral dissection, carry out spray test, agents useful for same is that concentration is 5% sodium chloride solution, test period 300 hours, measures the bubbling width forming in line of cut one side, and result bubbling width is 0; Process metal material with silane surface inorganic agent of the present invention, it is in 5% sodium chloride solution that this material is immersed in to concentration, soaks 300 hours, and material surface is substantially unchanged, soaks 400 hours, and minute quantity rust staining appears in edge.
Claims (4)
1. a metal surface silane finish that contains ammonium metavanadate, it is characterized in that the mixed liquor formulated by following component, by the weight portion of each component in gram every liter of mixed liquor of calculating be: 3-(isobutene acyl-oxygen) propyl trimethoxy silicane 22-32, N-phenyl-3-TSL 8330 27-40, water nano zinc oxide material 100-190, ethylenediamine tetramethylene fork Alendronate 3-5, propenyl 3-4, propane diols 3-4, zirconium fluoride 2-3, one hydration ammonia 2-3, diethanol amine 1-2, dimethyl sulfoxide (DMSO) 1-2, ammonium metavanadate 0.8-1, diethylene glycol butyl ether 0.7-0.9, remaining is water,
The preparation method of described water nano zinc oxide material is:
(1) be scattered in its quality 5-10 absolute ethyl alcohol doubly ultrasonic nano zine oxide, obtain dispersion liquid, then the anilinomethyl triethoxysilane of the cumyl peroxide of nano zine oxide quality 3-4%, 1-2% is added in above-mentioned dispersion liquid, back flow reaction 1-2 hour at 80-90 DEG C of temperature, after reaction, obtain the coupling agent modified nano zine oxide-alcohol suspension with reactive group, then filter, centrifugation filtrate, obtains modified nano zinc oxide;
(2) glycerine is water-soluble, then add above-mentioned modified nano zinc oxide, ball-milling treatment 1-2 hour in ball mill, obtains modified nano zinc oxide slurry;
(3) N-phenyl-3-TSL 8330 is dissolved in ethanol, be prepared into the solution that mass concentration is 2-4%, join in above-mentioned modified nano zinc oxide slurry, regulating pH value with acetic acid or sodium acetate is 4-5, ball-milling treatment 2-3 hour again, obtains described water nano zinc oxide material;
The concentration of the hydration ammonia described in raw material is 3-5%.
2. a kind of metal surface silane finish that contains ammonium metavanadate according to claim 1, it is characterized in that, in the preparation method of described water nano zinc oxide material, the mass ratio of the water in described nano zine oxide, glycerine, N-phenyl-3-TSL 8330 and step (2), the ethanol in step (3) is: nano zine oxide: glycerine: N-phenyl-3-TSL 8330: water: ethanol is 10-15g:1-2g:2-4g:95-105 gram: 95-105 gram.
3. a kind of metal surface silane finish that contains ammonium metavanadate according to claim 1, the granularity that it is characterized in that described nano zine oxide is 40-50nm.
4. a preparation method for the metal surface silane finish that contains ammonium metavanadate as claimed in claim 1, is characterized in that comprising the following steps:
(1) 3-of above-mentioned weight portion (isobutene acyl-oxygen) propyl trimethoxy silicane is added in the water of above-mentioned weight portion 60-70%, after fully dissolving, add again N-phenyl-3-TSL 8330 of above-mentioned weight portion, fully stir, obtain compound A;
(2) get the 50-60% that remains water, add the water nano zinc oxide material of above-mentioned weight portion, after fully stirring, add ethylenediamine tetramethylene fork Alendronate, zirconium fluoride, diethanol amine, the dimethyl sulfoxide (DMSO) of above-mentioned weight portion fully to stir, obtain compound B;
(3) propenyl of above-mentioned weight portion, diethylene glycol butyl ether, a hydration ammonia are mixed with remaining water, then add the ammonium metavanadate of above-mentioned weight portion, be stirred to ammonium metavanadate and dissolve completely, obtain compound C;
(4) compound A obtained above, B and C are mixed, then with acetic acid or sodium acetate, adjusting pH is 3-5, finally adds the each raw material of residue, the metal surface silane finish that contains ammonium metavanadate described in obtaining after fully stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210550917.XA CN103031548B (en) | 2012-12-18 | 2012-12-18 | A kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210550917.XA CN103031548B (en) | 2012-12-18 | 2012-12-18 | A kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103031548A CN103031548A (en) | 2013-04-10 |
| CN103031548B true CN103031548B (en) | 2016-05-04 |
Family
ID=48018933
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210550917.XA Active CN103031548B (en) | 2012-12-18 | 2012-12-18 | A kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103031548B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104099589A (en) * | 2014-06-19 | 2014-10-15 | 锐展(铜陵)科技有限公司 | Chromate-free surface treating agent for aluminum alloy |
| CN106280840A (en) * | 2016-08-24 | 2017-01-04 | 何国美 | Anti-corrosion of metal layer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434748A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
| CN101509131A (en) * | 2008-02-15 | 2009-08-19 | 宝山钢铁股份有限公司 | Anti-corrosion fingerprint-resistant surface treating pigment and producing method, and use method on stainless steel plate |
| CN102121104A (en) * | 2011-01-22 | 2011-07-13 | 安徽工业大学 | Aqueous chromium-free surface treatment solution for combining color coating pretreatment and base paint coating of galvanized plate |
| CN102409325A (en) * | 2011-12-06 | 2012-04-11 | 中国科学院金属研究所 | Environmentally-friendly corrosion-resistant chromium-free chemical conversion liquid and method for preparing chemical conversion film |
-
2012
- 2012-12-18 CN CN201210550917.XA patent/CN103031548B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101509131A (en) * | 2008-02-15 | 2009-08-19 | 宝山钢铁股份有限公司 | Anti-corrosion fingerprint-resistant surface treating pigment and producing method, and use method on stainless steel plate |
| CN101434748A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
| CN102121104A (en) * | 2011-01-22 | 2011-07-13 | 安徽工业大学 | Aqueous chromium-free surface treatment solution for combining color coating pretreatment and base paint coating of galvanized plate |
| CN102409325A (en) * | 2011-12-06 | 2012-04-11 | 中国科学院金属研究所 | Environmentally-friendly corrosion-resistant chromium-free chemical conversion liquid and method for preparing chemical conversion film |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103031548A (en) | 2013-04-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103031056B (en) | A kind of Metal surface silane treatment agent containing water nano zinc oxide material and preparation method thereof | |
| CN101643898B (en) | Phosphorus-free film forming agent and preparation method thereof | |
| CN103031551B (en) | A kind of metal surface silane finish that contains ethylenediamine tetramethylene fork Alendronate and preparation method thereof | |
| CN105779988A (en) | Chromate-free passivation solution for electroplated zinc and passivation technology thereof | |
| CN103966646A (en) | Electro-deposition preparation method and application of reduced and oxidized graphene/silane composite film | |
| CN104630765A (en) | Environmental-protection type metal coating pre-treatment agent and preparation method thereof | |
| CN107012453B (en) | A kind of method that green low temperature quickly prepares phosphating coat | |
| CN107475704B (en) | Metal surface silane treatment agent and preparation method thereof | |
| CN103087629A (en) | Anti-corrosion metal surface silane treatment agent and preparation method thereof | |
| CN103059721A (en) | Metal surface silicane treating agent containing polyethylene glycol and preparing method thereof | |
| CN101476120A (en) | Environment-friendly type metal surface finishing agent and preparation thereof | |
| CN103031549B (en) | A kind of metal surface silane finish that contains diethyl toluene diamine and preparation method thereof | |
| CN103088327A (en) | Metal surface silane treatment agent containing water-soluble phenolic resin and preparation method thereof | |
| CN103087627B (en) | A kind of metal aluminum alloy silane surface treatment agent and preparation method thereof | |
| CN103031548B (en) | A kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof | |
| CN103102724B (en) | A kind of containing acrylic acid Metal surface silane treatment agent and preparation method thereof | |
| CN101376970B (en) | Surface conditioning solution used before manganese series phosphating, preparation and use | |
| CN103060787B (en) | A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof | |
| CN103059728B (en) | A kind of corrosion resistant Metal surface silane treatment agent and preparation method thereof | |
| CN103045086B (en) | A kind of Metal surface silane treatment agent and preparation method thereof | |
| CN102304704A (en) | Aqueous silane treatment agent for improving metal surface protection performance | |
| CN102534596B (en) | A kind of silane agent that adopts carries out the technique of protection separately to metalwork surface | |
| CN103059727B (en) | A kind of Metal surface silane treatment agent containing HMPA and preparation method thereof | |
| CN103088328B (en) | A kind of galvanized steel sheet surface silane finish and preparation method thereof | |
| CN103031057A (en) | Metal surface silane treating agent containing plant ash and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |