CN103059723A - Stripping-resistant metal surface silicane treating agent and preparation method thereof - Google Patents
Stripping-resistant metal surface silicane treating agent and preparation method thereof Download PDFInfo
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- CN103059723A CN103059723A CN2012105509521A CN201210550952A CN103059723A CN 103059723 A CN103059723 A CN 103059723A CN 2012105509521 A CN2012105509521 A CN 2012105509521A CN 201210550952 A CN201210550952 A CN 201210550952A CN 103059723 A CN103059723 A CN 103059723A
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Abstract
The invention discloses a stripping-resistant metal surface silicane treating agent. The stripping-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: 32-40 g of gamma-(2,3-epoxypropoxy) propyltrimethoxysilicane, 21-26 g of 2-(3,4-epoxycyclohexyl) ethyltrimethoxysilane, 160-200 g of a water-based nanometer zinc oxide material, 3-5 g of sodium ethylenediamine tetramethylene phosphonate, 3-4 g of 1,4-cyclohexanedimethanol, 2-3 g of propylene glycol, 2-3 g of titanyl sulfate, 2-3 g of ammonium hydroxide, 1-2 g of diethylenetriamine, 1-2 g of diethanol amine, 0.8-1 g of plant ash, 0.6-0.8 g of ammonium metavanadate, 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 stripping-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 anti-metallic surface silane finish of peeling off 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 anti-metallic surface silane finish of peeling off, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
γ-(2, the 3-glycidoxy) propyl trimethoxy silicane 32-40,2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane 21-26, water nano zinc oxide material 160-200, ethylenediamine tetramethylene fork Alendronate 3-5,1,4 cyclohexane dimethanol 3-4, propylene glycol 2-3, titanyl sulfate 2-3, a hydration ammonia 2-3, Diethylenetriaminee (DETA) 1-2, diethanolamine 1-2, plant ash 0.8-1, ammonium meta-vanadate 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) with 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane 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, described nano zine oxide, glycerol, 2-(3, the 4-epoxycyclohexyl) mass ratio of the water in ethyl trimethoxy silane and the step (2), the ethanol in the step (3) is: nano zine oxide: glycerol: 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane: water: ethanol is the 10-15g:1-2g:2-4g:95-105 gram: the 95-105 gram.
The granularity of nano zine oxide is 40-50nm.
A kind of preparation method of the anti-metallic surface silane finish of peeling off may further comprise the steps:
(1) with the γ-(2 of above-mentioned weight part, the 3-glycidoxy) propyl trimethoxy silicane adds in the water of above-mentioned weight part 60-70%, fully adds 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane of above-mentioned weight part after the dissolving again, 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, adds the ethylenediamine tetramethylene fork Alendronate, 1 of above-mentioned weight part, 4-cyclohexanedimethanol, titanyl sulfate, Diethylenetriaminee (DETA), diethanolamine fully stir, and get compound B;
(3) remaining water is heated to 20-25 ℃, then adds hydration ammonia and an ammonium meta-vanadate of above-mentioned weight part, be stirred to ammonium meta-vanadate and dissolve fully, get compound C;
(4) 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 D;
(5) compound A obtained above, B, C and D are mixed, then add acetic acid or sodium-acetate, adjusting PH is 3-5, adds at last each raw material of residue, namely gets the described anti-metallic surface silane finish of peeling off after fully stirring.
A kind of anti-metallic surface silane finish of peeling off, the concentration of the hydration ammonia described in the raw material is 3-5%.
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 γ-(2, the 3-glycidoxy) propyl trimethoxy silicane and 2-(3, the 4-epoxycyclohexyl) the ethyl trimethoxy silane use that combines, 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 anti-metallic surface silane finish of peeling off, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
γ-(2, the 3-glycidoxy) propyl trimethoxy silicane 40,2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane 26, water nano zinc oxide material 200, ethylenediamine tetramethylene fork Alendronate 5,1,4 cyclohexane dimethanol 4, propylene glycol 3, titanyl sulfate 3, a hydration ammonia 3, Diethylenetriaminee (DETA) 2, diethanolamine 2, plant ash 0.8, ammonium meta-vanadate 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) with 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane 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 3 hours again, obtains described water nano zinc oxide material.
Among the preparation method of described water nano zinc oxide material, described nano zine oxide, glycerol, 2-(3, the 4-epoxycyclohexyl) mass ratio of the water in ethyl trimethoxy silane and the step (2), the ethanol in the step (3) is: nano zine oxide: glycerol: 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane: water: ethanol is the 15g:2g:4g:105 gram: 105 grams.
The granularity of described nano zine oxide is 50nm.
A kind of preparation method of the anti-metallic surface silane finish of peeling off may further comprise the steps:
(1) with the γ-(2 of above-mentioned weight part, the 3-glycidoxy) propyl trimethoxy silicane adds in the water of above-mentioned weight part 60%, fully adds 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane of above-mentioned weight part after the dissolving again, 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 the ethylenediamine tetramethylene fork Alendronate, 1 of above-mentioned weight part, 4-cyclohexanedimethanol, titanyl sulfate, Diethylenetriaminee (DETA), diethanolamine fully stir, and get compound B;
(3) remaining water is heated to 25 ℃, then adds hydration ammonia and an ammonium meta-vanadate of above-mentioned weight part, be stirred to ammonium meta-vanadate and dissolve fully, get compound C;
(4) with the plant ash of above-mentioned weight part with 15% salt acid soak 3 hours, deionized water wash soaked 4 hours with 10% sodium hydroxide solution again, again with deionized water wash to neutral, oven dry is ground into ultrafine powder, gets compound D;
(5) compound A obtained above, B, C and D are mixed, then add acetic acid or sodium-acetate, regulating PH is 5, adds at last each raw material of residue, namely gets the described anti-metallic surface silane finish of peeling off after fully stirring.
The concentration of the hydration ammonia described in the raw material is 5%.
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 material 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 (5)
1. an anti-metallic surface silane finish of peeling off 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:
γ-(2, the 3-glycidoxy) propyl trimethoxy silicane 32-40,2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane 21-26, water nano zinc oxide material 160-200, ethylenediamine tetramethylene fork Alendronate 3-5,1,4 cyclohexane dimethanol 3-4, propylene glycol 2-3, titanyl sulfate 2-3, a hydration ammonia 2-3, Diethylenetriaminee (DETA) 1-2, diethanolamine 1-2, plant ash 0.8-1, ammonium meta-vanadate 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) with 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane 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 anti-metallic surface silane finish of peeling off according to claim 1, it is characterized in that, among the preparation method of described water nano zinc oxide material, described nano zine oxide, glycerol, 2-(3, the 4-epoxycyclohexyl) mass ratio of the water in ethyl trimethoxy silane and the step (2), the ethanol in the step (3) is: nano zine oxide: glycerol: 2-(3,4-epoxycyclohexyl) ethyl trimethoxy silane: water: ethanol is the 10-15g:1-2g:2-4g:95-105 gram: the 95-105 gram.
3. a kind of anti-metallic surface silane finish of peeling off according to claim 1, the granularity that it is characterized in that described nano zine oxide is 40-50nm.
4. the preparation method of an anti-metallic surface silane finish of peeling off as claimed in claim 1 is characterized in that may further comprise the steps:
(1) with the γ-(2 of above-mentioned weight part, the 3-glycidoxy) propyl trimethoxy silicane adds in the water of above-mentioned weight part 60-70%, fully adds 2-(3, the 4-epoxycyclohexyl) ethyl trimethoxy silane of above-mentioned weight part after the dissolving again, 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, adds the ethylenediamine tetramethylene fork Alendronate, 1 of above-mentioned weight part, 4-cyclohexanedimethanol, titanyl sulfate, Diethylenetriaminee (DETA), diethanolamine fully stir, and get compound B;
(3) remaining water is heated to 20-25 ℃, then adds hydration ammonia and an ammonium meta-vanadate of above-mentioned weight part, be stirred to ammonium meta-vanadate and dissolve fully, get compound C;
(4) 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 D;
(5) compound A obtained above, B, C and D are mixed, then add acetic acid or sodium-acetate, adjusting PH is 3-5, adds at last each raw material of residue, namely gets the described anti-metallic surface silane finish of peeling off after fully stirring.
5. an anti-metallic surface silane finish of peeling off is characterized in that, the concentration of the hydration ammonia described in the raw material is 3-5%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280840A (en) * | 2016-08-24 | 2017-01-04 | 何国美 | Anti-corrosion of metal layer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101693811A (en) * | 2009-09-28 | 2010-04-14 | 常州捷迈特表面工程技术有限公司 | Chromium-free waterborne corrosion resistant coating used for surface of metal and preparation method thereof |
| CN101939388A (en) * | 2007-12-07 | 2011-01-05 | 迪普索尔化学株式会社 | Surface-treating aqueous solution and treatment methods for forming corrosion-resistant coating film over zinc or zinc alloy deposit |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101939388A (en) * | 2007-12-07 | 2011-01-05 | 迪普索尔化学株式会社 | Surface-treating aqueous solution and treatment methods for forming corrosion-resistant coating film over zinc or zinc alloy deposit |
| CN101693811A (en) * | 2009-09-28 | 2010-04-14 | 常州捷迈特表面工程技术有限公司 | Chromium-free waterborne corrosion resistant coating used for surface of metal and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280840A (en) * | 2016-08-24 | 2017-01-04 | 何国美 | Anti-corrosion of metal layer |
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