CN103031057A - Metal surface silane treating agent containing plant ash and preparation method thereof - Google Patents
Metal surface silane treating agent containing plant ash and preparation method thereof Download PDFInfo
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- CN103031057A CN103031057A CN2012105509517A CN201210550951A CN103031057A CN 103031057 A CN103031057 A CN 103031057A CN 2012105509517 A CN2012105509517 A CN 2012105509517A CN 201210550951 A CN201210550951 A CN 201210550951A CN 103031057 A CN103031057 A CN 103031057A
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Abstract
The invention discloses a metal surface silane treating agent containing plant ash. The metal surface silane treating agent is characterized by being a mixture solution prepared from the following ingredients in parts by weight (gram) in each liter of the mixture 20-30 parts of 1,2-bi(triethoxy silicon base) ethane, 25-35 parts of 3-glycidyl ether oxygen propyl trimethoxy silane, 150-180 parts of aqueous nano-zinc oxide, 3-5 parts of ethylene diamine tetramethylene risedremate sodium, 3-4 parts of glycerol, 3-4 parts of ethanol, 2-3 parts of N-methyl pyrrolidone, 2-3 parts of ammonia water, 1-2 parts of plant ash, 1-2 parts of sodium tripolyphosphate, 0.8-1 part of ammonium metavanadate, 0.7-0.9 parts ofHexamethyl phosphoramide and the balance of water. The aqueous nano-zinc oxide prepared by using the process provided by the invention has high dispersion stability and efficient adhesiveness, and is uniformly distributed on the surface of a metal, so that the metal has high compactness and anti-ion permeability; and due to the added assistant such as the ethylene diamine tetramethylene risedremate sodium and the like, the compactness of a silane absorbing film is increased, and the filming quality is improved with friendliness and pollution freeness.
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 metallic surface silane finish that contains plant ash 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 metallic surface silane finish that contains plant ash, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
Two (triethoxy is silica-based) ethane 20-30 of 1,2-, 3-glycidyl ether oxygen base propyl trimethoxy silicane 25-35, water nano zinc oxide material 150-180, ethylenediamine tetramethylene fork Alendronate 3-5, glycerol 3-4, ethanol 3-4, N-Methyl pyrrolidone 2-3, ammoniacal liquor 2-3, plant ash 1-2, tripoly phosphate sodium STPP 1-2, ammonium meta-vanadate 0.8-1, HMPA 0.7-0.9, 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) 3-glycidyl ether oxygen base propyl trimethoxy silicane 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, 3-glycidyl ether oxygen base propyl trimethoxy silicane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: 3-glycidyl ether oxygen base propyl trimethoxy silicane: 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 who contains the metallic surface silane finish of plant ash may further comprise the steps:
(1) with 1 of above-mentioned weight part, two (triethoxy the is silica-based) ethane of 2-add in the water of above-mentioned weight part 60-70%, fully add the 3-glycidyl ether oxygen base propyl trimethoxy silicane of above-mentioned weight part after the dissolving again, fully stir, and 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, N-Methyl pyrrolidone, tripoly phosphate sodium STPP 1-2, ammonium meta-vanadate 0.8-1, the HMPA that add above-mentioned weight part fully stir, and get compound B;
(3) remaining water is heated to 20-25 ℃, then adds ammoniacal liquor and the 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 metallic surface silane finish that contains plant ash after fully stirring.
The concentration of the ammoniacal liquor 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 1, the use that combines of two (triethoxy the is silica-based) ethane of 2-and 3-glycidyl ether oxygen base propyl trimethoxy silicane, 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, fine and close evenly, the characteristics that polarized current density is little, and the production process environmental protection, pollution-free.
Embodiment
Embodiment 1
A kind of metallic surface silane finish that contains plant ash, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
Two (triethoxy the is silica-based) ethane 30 of 1,2-, 3-glycidyl ether oxygen base propyl trimethoxy silicane 35, water nano zinc oxide material 180, ethylenediamine tetramethylene fork Alendronate 5, glycerol 4, ethanol 4, N-Methyl pyrrolidone 3, ammoniacal liquor 3, plant ash 2, tripoly phosphate sodium STPP 2, ammonium meta-vanadate 0.8, HMPA 0.9, 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) 3-glycidyl ether oxygen base propyl trimethoxy silicane 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, 3-glycidyl ether oxygen base propyl trimethoxy silicane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: 3-glycidyl ether oxygen base propyl trimethoxy silicane: water: ethanol is the 10g:2g:4g:105 gram: 105 grams.
The granularity of nano zine oxide is 50nm.
A kind of preparation method who contains the metallic surface silane finish of plant ash may further comprise the steps:
(1) with 1 of above-mentioned weight part, two (triethoxy the is silica-based) ethane of 2-add in the water of above-mentioned weight part 70%, fully add the 3-glycidyl ether oxygen base propyl trimethoxy silicane of above-mentioned weight part after the dissolving again, fully stir, and 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, N-Methyl pyrrolidone, tripoly phosphate sodium STPP 2, ammonium meta-vanadate 0.8, the HMPA that add above-mentioned weight part fully stir, and get compound B;
(3) remaining water is heated to 25 ℃, then adds ammoniacal liquor and the 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 12% sodium hydroxide solution again, and extremely neutral with deionized water wash again, 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 metallic surface silane finish that contains plant ash after fully stirring.
The concentration of the ammoniacal liquor 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 steel plate galvanized 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. a metallic surface silane finish that contains plant ash 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:
Two (triethoxy is silica-based) ethane 20-30 of 1,2-, 3-glycidyl ether oxygen base propyl trimethoxy silicane 25-35, water nano zinc oxide material 150-180, ethylenediamine tetramethylene fork Alendronate 3-5, glycerol 3-4, ethanol 3-4, N-Methyl pyrrolidone 2-3, ammoniacal liquor 2-3, plant ash 1-2, tripoly phosphate sodium STPP 1-2, ammonium meta-vanadate 0.8-1, HMPA 0.7-0.9, 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) 3-glycidyl ether oxygen base propyl trimethoxy silicane 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 metallic surface silane finish that contains plant ash according to claim 1, it is characterized in that, among the preparation method of described water nano zinc oxide material, the water in described nano zine oxide, glycerol, 3-glycidyl ether oxygen base propyl trimethoxy silicane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: 3-glycidyl ether oxygen base propyl trimethoxy silicane: water: ethanol is the 10-15g:1-2g:2-4g:95-105 gram: the 95-105 gram.
3. a kind of metallic surface silane finish that contains plant ash according to claim 1, the granularity that it is characterized in that described nano zine oxide is 40-50nm.
4. preparation method who contains the metallic surface silane finish of plant ash as claimed in claim 1 is characterized in that may further comprise the steps:
(1) with 1 of above-mentioned weight part, two (triethoxy the is silica-based) ethane of 2-add in the water of above-mentioned weight part 60-70%, fully add the 3-glycidyl ether oxygen base propyl trimethoxy silicane of above-mentioned weight part after the dissolving again, fully stir, and 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, N-Methyl pyrrolidone, tripoly phosphate sodium STPP, ammonium meta-vanadate, the HMPA that add above-mentioned weight part fully stir, and get compound B;
(3) remaining water is heated to 20-25 ℃, then adds ammoniacal liquor and the 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 metallic surface silane finish that contains plant ash after fully stirring.
5. a metallic surface silane finish that contains plant ash is characterized in that, the concentration of the ammoniacal liquor described in the raw material is 3-5%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109485087A (en) * | 2018-12-18 | 2019-03-19 | 兴化市万润锌业有限公司 | A kind of processing method of modified nano zinc oxide |
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| 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 |
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| CN109485087A (en) * | 2018-12-18 | 2019-03-19 | 兴化市万润锌业有限公司 | A kind of processing method of modified nano zinc oxide |
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