CN103031551B - A kind of metal surface silane finish that contains ethylenediamine tetramethylene fork Alendronate and preparation method thereof - Google Patents
A kind of metal surface silane finish that contains ethylenediamine tetramethylene fork Alendronate and preparation method thereof Download PDFInfo
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- CN103031551B CN103031551B CN201210550918.4A CN201210550918A CN103031551B CN 103031551 B CN103031551 B CN 103031551B CN 201210550918 A CN201210550918 A CN 201210550918A CN 103031551 B CN103031551 B CN 103031551B
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Abstract
The invention discloses a kind of metal surface silane finish that contains ethylenediamine tetramethylene fork Alendronate, 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: VTES 25-33, N-phenyl-3-TSL 8330 30-43, water nano zinc oxide material 100-190, ethylenediamine tetramethylene fork Alendronate 3-5, 1, 6-hexamethylene diamine 1-2, ethylene glycol 4-5, oxalic acid 2-4, zirconium tetrafluoride 2-3, ammonium molybdate 2-3, trimethylolpropane 1-2, citric acid 1-2, pentaerythrite 0.8-1, t-butyl hydroperoxide 0.6-0.9, remaining is water, the water nano zinc oxide material of preparing by technique of the present invention has high dispersion stability and efficient cohesive, it is evenly distributed in metal surface, makes metal have high compactness and the permeability of anti-ion, the auxiliary agents such as the zirconium tetrafluoride adding, 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 ethylenediamine tetramethylene fork Alendronate 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 ethylenediamine tetramethylene fork Alendronate, by the formulated mixed liquor of following component, the weight portion of each component in every liter of mixed liquor (gram) be:
VTES 25-33, N-phenyl-3-TSL 8330 30-43, water nano zinc oxide material 100-190, ethylenediamine tetramethylene fork Alendronate 3-5,1,6-hexamethylene diamine 1-2, ethylene glycol 4-5, oxalic acid 2-4, zirconium tetrafluoride 2-3, ammonium molybdate 2-3, trimethylolpropane 1-2, citric acid 1-2, pentaerythrite 0.8-1, t-butyl hydroperoxide 0.6-0.9, 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) by 1, two (triethoxy the is silica-based) ethane of 2-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, described nano zine oxide, glycerine, 1, the mass ratio of the water in two (triethoxy the is silica-based) ethane of 2-and step (2), the ethanol in step (3) is: two (triethoxy is silica-based) ethane of nano zine oxide: glycerine: 1,2-: 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 ethylenediamine tetramethylene fork Alendronate, comprises the following steps:
(1) VTES of above-mentioned weight portion 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 the ethylenediamine tetramethylene fork Alendronate, 1 of above-mentioned weight portion, 6-hexamethylene diamine, zirconium tetrafluoride, ammonium molybdate, trimethylolpropane, citric acid fully stir, and obtain compound B;
(3) ethylene glycol of above-mentioned weight portion and pentaerythrite are mixed with remaining water, then add the t-butyl hydroperoxide of above-mentioned weight portion, be stirred to t-butyl hydroperoxide 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 ethylenediamine tetramethylene fork Alendronate described in obtaining after fully stirring.
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 VTES 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 zirconium tetrafluoride 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 ethylenediamine tetramethylene fork Alendronate, by the formulated mixed liquor of following component, the weight portion of each component in every liter of mixed liquor (gram) be:
VTES 33, N-phenyl-3-TSL 8330 30-43, water nano zinc oxide material 170, ethylenediamine tetramethylene fork Alendronate 5,1,6-hexamethylene diamine 2, ethylene glycol 5, oxalic acid 4, zirconium tetrafluoride 3, ammonium molybdate 2, trimethylolpropane 2, citric acid 2, pentaerythrite 0.8, t-butyl hydroperoxide 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 4%, 2% anilinomethyl triethoxysilane are added in above-mentioned dispersion liquid, back flow reaction 1 hour 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) by 1, two (triethoxy the is silica-based) ethane of 2-is dissolved in ethanol, be prepared into mass concentration and be 4% 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, described nano zine oxide, glycerine, 1, the mass ratio of the water in two (triethoxy the is silica-based) ethane of 2-and step (2), the ethanol in step (3) is: two (triethoxy is silica-based) ethane of nano zine oxide: glycerine: 1,2-: water: ethanol is 15g:2g: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 ethylenediamine tetramethylene fork Alendronate, comprises the following steps:
(1) VTES of above-mentioned weight portion 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 the ethylenediamine tetramethylene fork Alendronate, 1 of above-mentioned weight portion, 6-hexamethylene diamine, zirconium tetrafluoride, ammonium molybdate, trimethylolpropane, citric acid fully stir, and obtain compound B;
(3) ethylene glycol of above-mentioned weight portion and pentaerythrite are mixed with remaining water, then add the t-butyl hydroperoxide of above-mentioned weight portion, be stirred to t-butyl hydroperoxide 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 ethylenediamine tetramethylene fork Alendronate described in obtaining after fully stirring.
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 ethylenediamine tetramethylene fork Alendronate, 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: VTES 25-33, N-phenyl-3-TSL 8330 30-43, water nano zinc oxide material 100-190, ethylenediamine tetramethylene fork Alendronate 3-5, 1, 6-hexamethylene diamine 1-2, ethylene glycol 4-5, oxalic acid 2-4, zirconium tetrafluoride 2-3, ammonium molybdate 2-3, trimethylolpropane 1-2, citric acid 1-2, pentaerythrite 0.8-1, t-butyl hydroperoxide 0.6-0.9, 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 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) by 1, two (triethoxy the is silica-based) ethane of 2-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.
2. a kind of metal surface silane finish that contains ethylenediamine tetramethylene fork Alendronate according to claim 1, it is characterized in that, in the preparation method of described water nano zinc oxide material, described nano zine oxide, glycerine, 1, the mass ratio of the water in two (triethoxy the is silica-based) ethane of 2-and step (2), the ethanol in step (3) is: two (triethoxy is silica-based) ethane of nano zine oxide: glycerine: 1,2-: water: ethanol is 10-15g:1-2g:2-4g:95-105g:95-105g.
3. a kind of metal surface silane finish that contains ethylenediamine tetramethylene fork Alendronate 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 ethylenediamine tetramethylene fork Alendronate as claimed in claim 1, is characterized in that comprising the following steps:
(1) VTES of above-mentioned weight portion 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 the ethylenediamine tetramethylene fork Alendronate, 1 of above-mentioned weight portion, 6-hexamethylene diamine, zirconium tetrafluoride, ammonium molybdate, trimethylolpropane, citric acid fully stir, and obtain compound B;
(3) ethylene glycol of above-mentioned weight portion and pentaerythrite are mixed with remaining water, then add the t-butyl hydroperoxide of above-mentioned weight portion, be stirred to t-butyl hydroperoxide 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 ethylenediamine tetramethylene fork Alendronate described in obtaining after fully stirring.
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| CN103463867A (en) * | 2013-06-20 | 2013-12-25 | 天长市天乐电器厂 | Bamboo charcoal filter element and preparation method thereof |
| CN104099601A (en) * | 2014-06-19 | 2014-10-15 | 锐展(铜陵)科技有限公司 | Surface treating agent for antioxidant aluminum alloy |
| CN104263121A (en) * | 2014-09-03 | 2015-01-07 | 天长市开林化工有限公司 | Polyvinyl acetate latex paint |
| CN112553609A (en) * | 2019-09-10 | 2021-03-26 | 天津大学 | Carbon steel surface phosphonic acid-silane composite membrane and preparation method and application thereof |
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| CN101287784A (en) * | 2005-08-26 | 2008-10-15 | Ppg工业俄亥俄公司 | Coating compositions exhibiting corrosion resistance properties, related coated substrates, and methods |
| CN101326308A (en) * | 2005-12-15 | 2008-12-17 | 日本帕卡濑精株式会社 | Surface treatment for metal materials, surface treatment process, and surface- treated metal materials |
| JP4207178B2 (en) * | 1998-03-27 | 2009-01-14 | ライプニッツ−インスティトゥート フィア ノイエ マテリアーリエン ゲマインニュッツィゲ ゲゼルシャフト ミット ベシュレンクタ ハフトゥンク | Method for protecting metal substrates against corrosion |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4207178B2 (en) * | 1998-03-27 | 2009-01-14 | ライプニッツ−インスティトゥート フィア ノイエ マテリアーリエン ゲマインニュッツィゲ ゲゼルシャフト ミット ベシュレンクタ ハフトゥンク | Method for protecting metal substrates against corrosion |
| CN101287784A (en) * | 2005-08-26 | 2008-10-15 | Ppg工业俄亥俄公司 | Coating compositions exhibiting corrosion resistance properties, related coated substrates, and methods |
| CN101326308A (en) * | 2005-12-15 | 2008-12-17 | 日本帕卡濑精株式会社 | Surface treatment for metal materials, surface treatment process, and surface- treated metal materials |
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