CN103059728A - Corrosion-resistant metal surface silicane treating agent and preparation method - Google Patents
Corrosion-resistant metal surface silicane treating agent and preparation method Download PDFInfo
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- CN103059728A CN103059728A CN2012105508764A CN201210550876A CN103059728A CN 103059728 A CN103059728 A CN 103059728A CN 2012105508764 A CN2012105508764 A CN 2012105508764A CN 201210550876 A CN201210550876 A CN 201210550876A CN 103059728 A CN103059728 A CN 103059728A
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Abstract
The invention discloses a corrosion-resistant metal surface silicane treating agent. The corrosion-resistant metal surface silicane treating agent is characterized in that: each liter of a mixed solution which is prepared from the following components comprises the components in parts by weight (gram) of: 23-30 g of N-phenyl-3-aminopropyl trimethoxysilane, 21-26 g of carbamido propyl triethoxysilane, 180-210 g of a water-based nanometer zinc oxide material, 3-5 parts of sodium ethylenediamine teramethylene phosphonate, 3-4 g of 2-methyl-1,3-propylene glycol, 2-3 g of ethylene glycol monobutyl ether, 2-3 g of oxalic acid, 2-3 g of sodium monofluorophosphate, 1-2 g of tetrahydrofuran, 1-2 g of vanadium oxytrichloride, 0.8-1 g of plant ash, 0.6-0.8 g of tert-butyl hydroperoxide, and the balance of water. The water-based nanometer zinc oxide material prepared by the technology of the invention has high dispersion stability and efficient adhesiveness, and is uniformly coated on the metal surface to enable the metal to have high compactness and anti-ion permeability; and due to the addition of the auxiliary agents such as the sodium ethylenediamine teramethylene phosphonate, the corrosion-resistant metal surface silicane treating agent adds the compactness of a silciane absorption film, improves film forming quality, and is environment-friendly and free from pollution.
Description
Technical field
The present invention relates generally to a kind of metallic surface silane finish and preparation method thereof, relates in particular to a kind of corrosion resistant metallic surface silane finish 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 the treating processes, manganese, nickel, the carcinogenic substances such as the heavy metal ion such as chromium and nitrite, environmental pollution is very serious, and the metallic surface silanization treatment technology is because the material of hurm involved environment not, energy consumption in production process is low, technical applications is extensive, be considered to be expected to replace phosphate conversion processing and chromating processing, that the recent development direction is protected separately in the metallic surface, the rete that the surface of workpiece that solution of silane was processed in the existing technology forms, Density inhomogeneity, the cavity is arranged, split sunken, put forth effort not strong with holding up of metallic object.
Summary of the invention
The object of the invention is exactly in order to remedy the defective of prior art, metallic surface silane finish of a kind of water nano zinc oxide material and preparation method thereof to be provided.
The present invention is achieved by the following technical solutions:
A kind of corrosion resistant metallic surface silane finish, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
N-phenyl-3-TSL 8330 23-30, urea groups propyl-triethoxysilicane 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) with the nano zine oxide ultra-sonic dispersion 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 the above-mentioned dispersion liquid, under 80-90 ℃ of temperature back flow reaction 1-2 hour, obtain the coupling agent modified nano zine oxide-alcohol suspension with reactive group after the 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 1-2 hour, obtain the modified nano zinc oxide slurry;
(3) the urea groups propyl-triethoxysilicane is dissolved in the ethanol, be prepared into the solution that mass concentration is 2-4%, join in the above-mentioned modified nano zinc oxide slurry, regulating the pH value with acetic acid or sodium-acetate is 4-5, ball-milling processing 2-3 hour again, obtain described water nano zinc oxide material.
Among the preparation method of described water nano zinc oxide material, the water in described nano zine oxide, glycerol, urea groups propyl-triethoxysilicane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: urea groups propyl-triethoxysilicane: water: ethanol is the 10-15g:1-2g:2-4g:95-105 gram: the 95-105 gram.
The granularity of described nano zine oxide is 40-50nm.
The preparation method of a kind of corrosion resistant metallic surface silane finish may further comprise the steps:
(1) the N-phenyl of above-mentioned weight part-3-TSL 8330 is added in the water of above-mentioned weight part 60-70%, fully add again the urea groups propyl-triethoxysilicane of above-mentioned weight part after the dissolving, fully stir, get compound A;
(2) get the 50-60% that remains water, the water nano zinc oxide material that adds above-mentioned weight part, after fully stirring, the ethylenediamine tetramethylene fork Alendronate, the 2-methyl isophthalic acid that add above-mentioned weight part, ammediol, oxalic acid, sodium monoflurophosphate, tetrahydrofuran (THF), vanadium oxytrichloride fully stir, and get compound B;
(3) plant ash of above-mentioned weight part is used 12-15% salt acid soak 3-4 hour, deionized water wash soaked 3-4 hour with the 10-12% sodium hydroxide solution again, and is extremely neutral with deionized water wash again, dries, and is ground into ultrafine powder, gets compound C;
(4) compound A obtained above, B and C are mixed, then add acetic acid or sodium-acetate, adjusting PH is 3-5, adds at last each raw material of residue, namely gets described corrosion resistant metallic surface silane finish after fully stirring.
Advantage of the present invention is:
Use silane surface treatment agent of the present invention to process the silane coating that forms in the metallic surface behind the metal and have excellent corrosion resistance nature, prolonged the work-ing life of metal, by the use that combines of N-phenyl-3-TSL 8330 and urea groups propyl-triethoxysilicane, can form densification in the metallic surface and coating firmly, and have high dispersion stability and efficient binding property with the water nano zinc oxide material of technique preparation of the present invention, it is evenly distributed in the metallic surface, so that metal has high compactness and the perviousness of anti-ion, the auxiliary agents such as the ethylenediamine tetramethylene fork Alendronate that adds, increased the density of silane adsorption film, improved quality of forming film, so that rete has strong adhesion, without the cavity, split sunken, evenly fine and close, the characteristics that polarized current density is little, and production process environmental protection, pollution-free.
Embodiment
Embodiment 1
A kind of corrosion resistant metallic surface silane finish, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
N-phenyl-3-TSL 8330 30, urea groups propyl-triethoxysilicane 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) with the nano zine oxide ultra-sonic dispersion in the dehydrated alcohol of 10 times of its quality, obtain dispersion liquid, then the dicumyl peroxide of its quality 4%, 2% anilinomethyl triethoxysilane are added in the above-mentioned dispersion liquid, back flow reaction is 1 hour under 90 ℃ of temperature, obtain the coupling agent modified nano zine oxide-alcohol suspension with reactive group after the 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 is 1 hour in ball mill, obtains the modified nano zinc oxide slurry;
(3) the urea groups propyl-triethoxysilicane is dissolved in the ethanol, be prepared into mass concentration and be 4% solution, join in the above-mentioned modified nano zinc oxide slurry, regulating the pH value with acetic acid or sodium-acetate is 5, ball-milling processing is 2 hours again, obtains described water nano zinc oxide material.
Among the preparation method of described water nano zinc oxide material, the water in described nano zine oxide, glycerol, urea groups propyl-triethoxysilicane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: urea groups propyl-triethoxysilicane: water: ethanol is the 10g:1g:2g:105 gram: 105 grams.
The granularity of described nano zine oxide is 50nm.
The preparation method of a kind of corrosion resistant metallic surface silane finish may further comprise the steps:
(1) the N-phenyl of above-mentioned weight part-3-TSL 8330 is added in the water of above-mentioned weight part 70%, fully add again the urea groups propyl-triethoxysilicane of above-mentioned weight part after the dissolving, fully stir, get compound A;
(2) get 60% of residue water, the water nano zinc oxide material that adds above-mentioned weight part after fully stirring, adds 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 get compound B;
(3) with the plant ash of above-mentioned weight part with 15% salt acid soak 3-4 hour, deionized water wash soaked 4 hours with 12% sodium hydroxide solution again, again with deionized water wash to neutral, oven dry is ground into ultrafine powder, gets compound C;
(4) compound A obtained above, B and C are mixed, then add acetic acid or sodium-acetate, regulating PH is 5, adds at last each raw material of residue, namely gets described corrosion resistant metallic surface silane finish after fully stirring.
Performance test:
Crooked viscosity:
Process the metal aluminium flake with silane surface treatment agent of the present invention, with crooked 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under the X20 magnifying glass, detect extent of exfoliation, as a result flawless; Process the metal aluminium flake with silane surface treatment agent of the present invention, aluminium flake was soaked in boiling water 1 hour, at room temperature placed 24 hours, then with crooked 60 degree of aluminium flake doubling, peel off curved part 3 times with adhesive tape, under the X20 magnifying glass, detect extent of exfoliation, as a result flawless;
Erosion resistance:
Process the steel plate galvanized metallic substance with silane surface treatment agent of the present invention, with this material lateral dissection, carry out spray test, agents useful for same is that concentration is 5% sodium chloride solution, test period 300 hours is measured the bubbling width that forms in line of cut one side, and the bubbling width is 0 as a result; Process metallic substance with silane surface treatment agent of the present invention, it is in 5% the sodium chloride solution that this material is immersed in concentration, soaks 300 hours, and material surface is substantially unchanged, soaks 400 hours, and the minute quantity rust staining appears in the edge.
Claims (4)
1. a corrosion resistant metallic surface silane finish is characterized in that by the formulated mixed solution of following component, and the weight part (gram) of each component is in every liter of mixed solution:
N-phenyl-3-TSL 8330 23-30, urea groups propyl-triethoxysilicane 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) with the nano zine oxide ultra-sonic dispersion 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 the above-mentioned dispersion liquid, under 80-90 ℃ of temperature back flow reaction 1-2 hour, obtain the coupling agent modified nano zine oxide-alcohol suspension with reactive group after the 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 1-2 hour, obtain the modified nano zinc oxide slurry;
(3) the urea groups propyl-triethoxysilicane is dissolved in the ethanol, be prepared into the solution that mass concentration is 2-4%, join in the above-mentioned modified nano zinc oxide slurry, regulating the pH value with acetic acid or sodium-acetate is 4-5, ball-milling processing 2-3 hour again, obtain described water nano zinc oxide material.
2. a kind of corrosion resistant metallic surface according to claim 1 silane finish, it is characterized in that, among the preparation method of described water nano zinc oxide material, the water in described nano zine oxide, glycerol, urea groups propyl-triethoxysilicane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: urea groups propyl-triethoxysilicane: water: ethanol is the 10-15g:1-2g:2-4g:95-105 gram: the 95-105 gram.
3. a kind of corrosion resistant metallic surface according to claim 1 silane finish, the granularity that it is characterized in that described nano zine oxide is 40-50nm.
4. the preparation method of a corrosion resistant metallic surface as claimed in claim 1 silane finish is characterized in that may further comprise the steps:
(1) the N-phenyl of above-mentioned weight part-3-TSL 8330 is added in the water of above-mentioned weight part 60-70%, fully add again the urea groups propyl-triethoxysilicane of above-mentioned weight part after the dissolving, fully stir, get compound A;
(2) get the 50-60% that remains water, the water nano zinc oxide material that adds above-mentioned weight part, after fully stirring, the ethylenediamine tetramethylene fork Alendronate, the 2-methyl isophthalic acid that add above-mentioned weight part, ammediol, oxalic acid, sodium monoflurophosphate, tetrahydrofuran (THF), vanadium oxytrichloride fully stir, and get compound B;
(3) plant ash of above-mentioned weight part is used 12-15% salt acid soak 3-4 hour, deionized water wash soaked 3-4 hour with the 10-12% sodium hydroxide solution again, and is extremely neutral with deionized water wash again, dries, and is ground into ultrafine powder, gets compound C;
(4) compound A obtained above, B and C are mixed, then add acetic acid or sodium-acetate, adjusting PH is 3-5, adds at last each raw material of residue, namely gets described corrosion resistant metallic surface silane finish after fully stirring.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106280840A (en) * | 2016-08-24 | 2017-01-04 | 何国美 | Anti-corrosion of metal layer |
| CN111001388A (en) * | 2019-12-30 | 2020-04-14 | 中国科学院城市环境研究所 | Preparation method and application of bamboo-based biochar phosphorus removal adsorbent |
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| 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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Patent Citations (3)
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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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106280840A (en) * | 2016-08-24 | 2017-01-04 | 何国美 | Anti-corrosion of metal layer |
| CN111001388A (en) * | 2019-12-30 | 2020-04-14 | 中国科学院城市环境研究所 | Preparation method and application of bamboo-based biochar phosphorus removal adsorbent |
| CN111001388B (en) * | 2019-12-30 | 2022-05-03 | 中国科学院城市环境研究所 | Preparation method and application of bamboo-based biochar phosphorus removal adsorbent |
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