CN103059728B - A kind of corrosion resistant Metal surface silane treatment agent and preparation method thereof - Google Patents
A kind of corrosion resistant Metal surface silane treatment agent and preparation method thereof Download PDFInfo
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- CN103059728B CN103059728B CN201210550876.4A CN201210550876A CN103059728B CN 103059728 B CN103059728 B CN 103059728B CN 201210550876 A CN201210550876 A CN 201210550876A CN 103059728 B CN103059728 B CN 103059728B
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Abstract
The invention discloses a kind of corrosion resistant Metal surface silane treatment agent, it is characterized in that by the formulated mixed solution of following component, in often liter of mixed solution, the weight part (gram) of each component is: N-phenyl-3-TSL 8330 23-30, ureidopropyltriethoxysilane 21-26, water nano zinc oxide material 180-210, ethylenediamine tetramethylene fork Alendronate 3-5, 2-methyl isophthalic acid, ammediol 3-4, ethylene glycol monobutyl ether 2-3, oxalic acid 2-3, sodium monoflurophosphate 2-3, tetrahydrofuran (THF) 1-2, vanadium oxytrichloride 1-2, plant ash 0.8-1, t-butyl hydroperoxide 0.6-0.8, remaining is water, the water nano zinc oxide material prepared by technique of the present invention has high dispersion stability and efficient binding property, it is evenly distributed in metallic surface, metal is made to have the perviousness of high compactness and anti-ion, the auxiliary agents such as the ethylenediamine tetramethylene fork Alendronate added, add the density of silane adsorption film, improve quality of forming film, environmental protection, pollution-free.
Description
Technical field
The present invention relates generally to a kind of Metal surface silane treatment agent and preparation method thereof, particularly relates to a kind of corrosion resistant Metal surface silane treatment agent 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 containing zinc in the waste liquid of discharging in treating processes, manganese, nickel, the carcinogenic substances 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 not hurm involved environment, energy consumption in production process is low, technical applications is extensive, be considered to be expected to replace phosphate conversion process and chromating process, that recent development direction is protected separately in metallic surface, the rete of the surface of workpiece formation of solution of silane process in existing technology, Density inhomogeneity, there is cavity, split sunken, with metallic object hold up put forth effort not strong.
Summary of the invention
The object of the invention is exactly the defect in order to make up prior art, provides Metal surface silane treatment agent of a kind of water nano zinc oxide material and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of corrosion resistant Metal surface silane treatment agent, the mixed solution formulated by following component, in often liter of mixed solution, the weight part (gram) of each component is:
N-phenyl-3-TSL 8330 23-30, ureidopropyltriethoxysilane 21-26, water nano zinc oxide material 180-210, ethylenediamine tetramethylene fork Alendronate 3-5,2-methyl isophthalic acid, ammediol 3-4, ethylene glycol monobutyl ether 2-3, oxalic acid 2-3, sodium monoflurophosphate 2-3, tetrahydrofuran (THF) 1-2, vanadium oxytrichloride 1-2, plant ash 0.8-1, t-butyl hydroperoxide 0.6-0.8, remaining be water;
The preparation method of described water nano zinc oxide material is:
(1) by nano zine oxide ultrasonic disperse in its quality 5-10 dehydrated alcohol doubly, obtain dispersion liquid, then the dicumyl peroxide of its quality 3-4%, the anilinomethyl triethoxysilane of 1-2% are added in above-mentioned dispersion liquid, back flow reaction 1-2 hour at 80-90 DEG C of temperature, coupling agent modified nano zine oxide-the alcohol suspension with reactive group is obtained after reaction, then filter, centrifugation filtrate, obtains modified nano zinc oxide;
(2) glycerol is water-soluble, then add above-mentioned modified nano zinc oxide, ball-milling processing 1-2 hour in ball mill, obtain modified nano zinc oxide slurry;
(3) ureidopropyltriethoxysilane is dissolved in ethanol, be prepared into the solution that mass concentration is 2-4%, joining in above-mentioned modified nano zinc oxide slurry, is 4-5 by acetic acid or sodium-acetate adjust ph, ball-milling processing 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, glycerol, ureidopropyltriethoxysilane and step (2), the ethanol in step (3) is: nano zine oxide: glycerol: ureidopropyltriethoxysilane: 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 corrosion resistant Metal surface silane treatment agent, comprises the following steps:
(1) the N-phenyl-3-TSL 8330 of above-mentioned weight part is added in the water of above-mentioned weight part 60-70%, add the ureidopropyltriethoxysilane of above-mentioned weight part after fully dissolving again, fully stir, obtain compound A;
(2) 50-60% of residue water is got, add the water nano zinc oxide material of above-mentioned weight part, after abundant stirring, add ethylenediamine tetramethylene fork Alendronate, the 2-methyl isophthalic acid of above-mentioned weight part, ammediol, oxalic acid, sodium monoflurophosphate, tetrahydrofuran (THF), vanadium oxytrichloride fully stir, and obtain compound B;
(3) by the plant ash 12-15% salt acid soak 3-4 hour of above-mentioned weight part, deionized water wash, then soak 3-4 hour with 10-12% sodium hydroxide solution, then with deionized water wash to neutral, dry, be ground into ultrafine powder, obtain compound C;
(4) by compound A, B and C mixing obtained above, then add acetic acid or sodium-acetate, adjustment PH is 3-5, finally adds each raw material of residue, namely obtains described corrosion resistant Metal surface silane treatment agent after fully stirring.
Advantage of the present invention is:
The silane coating formed in metallic surface after using silane surface treatment agent process metal of the present invention has excellent corrosion resistance nature, extend the work-ing life of metal, to be combined use by N-phenyl-3-TSL 8330 and ureidopropyltriethoxysilane, densification can be formed and firmly coating in metallic surface, and with water nano zinc oxide material prepared by technique of the present invention, there is high dispersion stability and efficient binding property, it is evenly distributed in metallic surface, metal is made to have the perviousness of high compactness and anti-ion, the auxiliary agents such as the ethylenediamine tetramethylene fork Alendronate added, add the density of silane adsorption film, improve quality of forming film, rete is made to have strong adhesion, without cavity, split sunken, dense uniform, the feature that polarized current density is little, and production process environmental protection, pollution-free.
Embodiment
Embodiment 1
A kind of corrosion resistant Metal surface silane treatment agent, the mixed solution formulated by following component, in often liter of mixed solution, the weight part (gram) of each component is:
N-phenyl-3-TSL 8330 30, ureidopropyltriethoxysilane 26, water nano zinc oxide material 210, ethylenediamine tetramethylene fork Alendronate 3,2-methyl isophthalic acid, ammediol 4, ethylene glycol monobutyl ether 3, oxalic acid 3, sodium monoflurophosphate 3, tetrahydrofuran (THF) 1-2, vanadium oxytrichloride 2, plant ash 0.8, t-butyl hydroperoxide 0.8, remaining be water;
The preparation method of described water nano zinc oxide material is:
(1) by nano zine oxide ultrasonic disperse in the dehydrated alcohol of its quality 10 times, obtain dispersion liquid, then the dicumyl peroxide of its quality 4%, the anilinomethyl triethoxysilane of 2% are added in above-mentioned dispersion liquid, back flow reaction 1 hour at 90 DEG C of temperature, coupling agent modified nano zine oxide-the alcohol suspension with reactive group is obtained after reaction, then filter, centrifugation filtrate, obtains modified nano zinc oxide;
(2) glycerol is water-soluble, then add above-mentioned modified nano zinc oxide, in ball mill, ball-milling processing 1 hour, obtains modified nano zinc oxide slurry;
(3) ureidopropyltriethoxysilane is dissolved in ethanol, be prepared into the solution that mass concentration is 4%, joining in above-mentioned modified nano zinc oxide slurry, is 5 by acetic acid or sodium-acetate adjust ph, ball-milling processing 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, glycerol, ureidopropyltriethoxysilane and step (2), the ethanol in step (3) is: nano zine oxide: glycerol: ureidopropyltriethoxysilane: water: ethanol is 10g:1g:2g:105 gram: 105 grams.
The granularity of described nano zine oxide is 50nm.
A preparation method for corrosion resistant Metal surface silane treatment agent, comprises the following steps:
(1) the N-phenyl-3-TSL 8330 of above-mentioned weight part is added in the water of above-mentioned weight part 70%, add the ureidopropyltriethoxysilane of above-mentioned weight part after fully dissolving again, fully stir, obtain compound A;
(2) 60% of residue water is got, add the water nano zinc oxide material of above-mentioned weight part, after fully stirring, add ethylenediamine tetramethylene fork Alendronate, the 2-methyl isophthalic acid of above-mentioned weight part, ammediol, oxalic acid, sodium monoflurophosphate, tetrahydrofuran (THF), vanadium oxytrichloride fully stir, and obtain compound B;
(3) by the plant ash of above-mentioned weight part 15% salt acid soak 3-4 hour, deionized water wash, then soak 4 hours with 12% sodium hydroxide solution, then with deionized water wash to neutral, dry, be ground into ultrafine powder, obtain compound C;
(4) by compound A, B and C mixing obtained above, then add acetic acid or sodium-acetate, regulate PH to be 5, finally add each raw material of residue, after fully stirring, namely obtain described corrosion resistant Metal surface silane treatment agent.
Performance test:
Bending viscosity:
With silane surface treatment agent process metal aluminium flake of the present invention, by bending 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless; With silane surface treatment agent process metal aluminium flake of the present invention, aluminium flake is soaked 1 hour in boiling water, at room temperature place 24 hours, then by bending 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under X20 magnifying glass, detect extent of exfoliation, result flawless;
Erosion resistance:
With silane surface treatment agent process steel plate galvanized metallic substance of the present invention, by this material lateral dissection, carry out spray test, agents useful for same to be concentration be 5% sodium chloride solution, test period 300 hours, measure the bubbling width formed in line of cut side, result bubbling width is 0; With silane surface treatment agent process metallic substance of the present invention, this material being immersed in concentration is in the sodium chloride solution of 5%, and soak 300 hours, material surface is substantially unchanged, and soak 400 hours, minute quantity rust staining appears in edge.
Claims (4)
1. a corrosion resistant Metal surface silane treatment agent, is characterized in that by the formulated mixed solution of following component, by the weight part of each component in gram calculating often liter of mixed solution is:
N-phenyl-3-TSL 8330 23-30, ureidopropyltriethoxysilane 21-26, water nano zinc oxide material 180-210, ethylenediamine tetramethylene fork Alendronate 3-5,2-methyl isophthalic acid, ammediol 3-4, ethylene glycol monobutyl ether 2-3, oxalic acid 2-3, sodium monoflurophosphate 2-3, tetrahydrofuran (THF) 1-2, vanadium oxytrichloride 1-2, plant ash 0.8-1, t-butyl hydroperoxide 0.6-0.8, remaining be water;
The preparation method of described water nano zinc oxide material is:
(1) by nano zine oxide ultrasonic disperse in its quality 5-10 dehydrated alcohol doubly, obtain dispersion liquid, then the dicumyl peroxide of its quality 3-4%, the anilinomethyl triethoxysilane of 1-2% are added in above-mentioned dispersion liquid, back flow reaction 1-2 hour at 80-90 DEG C of temperature, coupling agent modified nano zine oxide-the alcohol suspension with reactive group is obtained after reaction, then filter, centrifugation filtrate, obtains modified nano zinc oxide;
(2) glycerol is water-soluble, then add above-mentioned modified nano zinc oxide, ball-milling processing 1-2 hour in ball mill, obtain modified nano zinc oxide slurry;
(3) ureidopropyltriethoxysilane is dissolved in ethanol, be prepared into the solution that mass concentration is 2-4%, joining in above-mentioned modified nano zinc oxide slurry, is 4-5 by acetic acid or sodium-acetate adjust ph, ball-milling processing 2-3 hour again, obtains described water nano zinc oxide material.
2. the corrosion resistant Metal surface silane treatment agent of one 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, glycerol, ureidopropyltriethoxysilane and step (2), the ethanol in step (3) is: nano zine oxide: glycerol: ureidopropyltriethoxysilane: water: ethanol is 10-15g:1-2g:2-4g:95-105g:95-105g.
3. the corrosion resistant Metal surface silane treatment agent of one according to claim 1, is characterized in that the granularity of described nano zine oxide is 40-50nm.
4. a preparation method for corrosion resistant Metal surface silane treatment agent as claimed in claim 1, is characterized in that comprising the following steps:
(1) the N-phenyl-3-TSL 8330 of above-mentioned weight part is added in the water of above-mentioned weight part 60-70%, add the ureidopropyltriethoxysilane of above-mentioned weight part after fully dissolving again, fully stir, obtain compound A;
(2) 50-60% of residue water is got, add the water nano zinc oxide material of above-mentioned weight part, after abundant stirring, add ethylenediamine tetramethylene fork Alendronate, the 2-methyl isophthalic acid of above-mentioned weight part, ammediol, oxalic acid, sodium monoflurophosphate, tetrahydrofuran (THF), vanadium oxytrichloride fully stir, and obtain compound B;
(3) by the plant ash 12-15% salt acid soak 3-4 hour of above-mentioned weight part, deionized water wash, then soak 3-4 hour with 10-12% sodium hydroxide solution, then with deionized water wash to neutral, dry, be ground into ultrafine powder, obtain compound C;
(4) by compound A, B and C mixing obtained above, then add acetic acid or sodium-acetate, adjustment pH is 3-5, finally adds each raw material of residue, namely obtains described corrosion resistant Metal surface silane treatment agent after fully stirring.
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| CN101193992A (en) * | 2005-04-22 | 2008-06-04 | 道康宁东丽株式会社 | Solution or dispersion for treating surface of base material, containing titanium oxide doped with metal element, method for treating surface of base material by using the liquid, and surface-treated |
| CN101978430A (en) * | 2008-03-19 | 2011-02-16 | 大日本涂料株式会社 | Dispersion, composition for transparent electroconductive film formation, transparent electroconductive film, and display |
| CN102618133A (en) * | 2012-03-31 | 2012-08-01 | 广州集泰化工有限公司 | High-temperature resistant and strong corrosive resistant water-based baking varnish for metal and preparation method for baking varnish |
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| CN101193992A (en) * | 2005-04-22 | 2008-06-04 | 道康宁东丽株式会社 | Solution or dispersion for treating surface of base material, containing titanium oxide doped with metal element, method for treating surface of base material by using the liquid, and surface-treated |
| CN101978430A (en) * | 2008-03-19 | 2011-02-16 | 大日本涂料株式会社 | Dispersion, composition for transparent electroconductive film formation, transparent electroconductive film, and display |
| CN102618133A (en) * | 2012-03-31 | 2012-08-01 | 广州集泰化工有限公司 | High-temperature resistant and strong corrosive resistant water-based baking varnish for metal and preparation method for baking varnish |
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