CN103060787A - Metal surface silicane treating agent containing diethanol amine and preparing method thereof - Google Patents
Metal surface silicane treating agent containing diethanol amine and preparing method thereof Download PDFInfo
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- CN103060787A CN103060787A CN2012105507901A CN201210550790A CN103060787A CN 103060787 A CN103060787 A CN 103060787A CN 2012105507901 A CN2012105507901 A CN 2012105507901A CN 201210550790 A CN201210550790 A CN 201210550790A CN 103060787 A CN103060787 A CN 103060787A
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Abstract
The invention discloses a metal surface silicane treating agent containing diethanol amine. The metal surface silicane treating agent containing the diethanol amine is characterized by being a mixed solution which is prepared from following compositions of, by weight part ratio in every liter of the mixed solution, 28-35 parts of 1,2-bis (triethoxy silicon) ethane, 32-40 parts of gamma-aminopropyl triethoxy silicane, 100-160 parts of aqueous nanometer zinc oxide material, 2-3 parts of allyl alcohol, 1-2 parts of ethylene glycol, 2-3 parts of sodium tripolyphosphate, 2-4 parts of propylene glycol, 2-3 parts of zirconium tetrafluoride, 2-3 parts of diethanol amine, 2-3 parts of ammonium chloride, 1-2 parts of diethylene glycol monobutyl ether, 1-2 parts of trimethylolpropane, 0.3-0.5 part of sodium dodecyl benzene sulfonate, and the balance water. The metal surface silicane treating agent containing the diethanol amine has the advantages that, a silicane coating formed on the surface of metal after the metal is processed by using the surface silicane treating agent has good decay resistance, service life of the metal is prolonged, and a compact and firm coating is formed on the surface of the metal by combining the 1,2-bis (triethoxy silicon) ethane and the gamma-aminopropyl triethoxy silicane for use.
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 diethanolamine 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 diethanolamine, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
1,2-two (triethoxy is silica-based) ethane 28-35, γ-aminopropyl triethoxysilane 32-40, water nano zinc oxide material 100-160, vinylcarbinol 2-3, ethylene glycol 1-2, tripoly phosphate sodium STPP 2-3, propylene glycol 2-4, zirconium tetrafluoride 2-3, diethanolamine 2-3, ammonium chloride 2-3, Diethylene Glycol butyl ether 1-2, TriMethylolPropane(TMP) 1-2, Sodium dodecylbenzene sulfonate 0.3-0.5, 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 1, two (triethoxy the is silica-based) ethane of 2-are 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, 1, water in two (triethoxy the is silica-based) ethane of 2-and the step (2), the mass ratio of the ethanol in the step (3) are: two (triethoxy is silica-based) ethane of nano zine oxide: glycerol: 1,2-: 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.
A kind of preparation method who contains the metallic surface silane finish of diethanolamine 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 γ-aminopropyl triethoxysilane of above-mentioned weight part after the dissolving again, fully stir, and get compound A;
(2) get the 60-70% that remains water, the water nano zinc oxide material that adds above-mentioned weight part, after fully stirring, the tripoly phosphate sodium STPP, zirconium tetrafluoride, diethanolamine, ammonium chloride, Diethylene Glycol butyl ether, the TriMethylolPropane(TMP) that add above-mentioned weight part fully stir, and get compound B;
(3) vinylcarbinol and the ethylene glycol with above-mentioned weight part mixes with remaining water, is heated to 40-50 ℃, then adds the Sodium dodecylbenzene sulfonate of above-mentioned weight part, is stirred to Sodium dodecylbenzene sulfonate and dissolves fully, gets compound C;
(4) compound A obtained above, B and C are mixed, then acetic acid or sodium-acetate, adjustings PH is 3-5, adds at last the propylene glycol of above-mentioned weight part, fully namely gets the described metallic surface silane finish that contains diethanolamine after the 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 1, the use that combines of two (triethoxy the is silica-based) ethane of 2-and γ-aminopropyl triethoxysilane, 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 zirconium tetrafluoride that add have increased the density of silane adsorption film, have 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 diethanolamine, 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 35 of 1,2-, γ-aminopropyl triethoxysilane 40, water nano zinc oxide material 160, vinylcarbinol 3, ethylene glycol 2, tripoly phosphate sodium STPP 3, propylene glycol 4, zirconium tetrafluoride 3, diethanolamine 3, ammonium chloride 3, Diethylene Glycol butyl ether 2, TriMethylolPropane(TMP) 2, Sodium dodecylbenzene sulfonate 0.5, 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 5 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 2 hours 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 1, two (triethoxy the is silica-based) ethane of 2-are dissolved in the ethanol, be prepared into mass concentration and be 2% solution, 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, 1, water in two (triethoxy the is silica-based) ethane of 2-and the step (2), the mass ratio of the ethanol in the step (3) are: two (triethoxy is silica-based) ethane of nano zine oxide: glycerol: 1,2-: 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 who contains the metallic surface silane finish of diethanolamine 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 γ-aminopropyl triethoxysilane of above-mentioned weight part after the dissolving again, fully stir, and get compound A;
(2) get 70% of residue water, the water nano zinc oxide material that adds above-mentioned weight part, after fully stirring, the tripoly phosphate sodium STPP, zirconium tetrafluoride, diethanolamine, ammonium chloride, Diethylene Glycol butyl ether, the TriMethylolPropane(TMP) that add above-mentioned weight part fully stir, and get compound B;
(3) vinylcarbinol and the ethylene glycol with above-mentioned weight part mixes with remaining water, is heated to 50 ℃, then adds the Sodium dodecylbenzene sulfonate of above-mentioned weight part, is stirred to Sodium dodecylbenzene sulfonate and dissolves fully, gets compound C;
(4) compound A obtained above, B and C are mixed, then acetic acid or sodium-acetate, regulating PH is 5, adds at last the propylene glycol of above-mentioned weight part, namely gets the described metallic surface silane finish that contains diethanolamine 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 metallic surface silane finish that contains diethanolamine 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:
1,2-two (triethoxy is silica-based) ethane 28-35, γ-aminopropyl triethoxysilane 32-40, water nano zinc oxide material 100-160, vinylcarbinol 2-3, ethylene glycol 1-2, tripoly phosphate sodium STPP 2-3, propylene glycol 2-4, zirconium tetrafluoride 2-3, diethanolamine 2-3, ammonium chloride 2-3, Diethylene Glycol butyl ether 1-2, TriMethylolPropane(TMP) 1-2, Sodium dodecylbenzene sulfonate 0.3-0.5, 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 1, two (triethoxy the is silica-based) ethane of 2-are 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 diethanolamine 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, 1, water in two (triethoxy the is silica-based) ethane of 2-and the step (2), the mass ratio of the ethanol in the step (3) are: two (triethoxy is silica-based) ethane of nano zine oxide: glycerol: 1,2-: 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 diethanolamine 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 diethanolamine 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 γ-aminopropyl triethoxysilane of above-mentioned weight part after the dissolving again, fully stir, and get compound A;
(2) get the 60-70% that remains water, the water nano zinc oxide material that adds above-mentioned weight part, after fully stirring, the tripoly phosphate sodium STPP, zirconium tetrafluoride, diethanolamine, ammonium chloride, Diethylene Glycol butyl ether, the TriMethylolPropane(TMP) that add above-mentioned weight part fully stir, and get compound B;
(3) vinylcarbinol and the ethylene glycol with above-mentioned weight part mixes with remaining water, is heated to 40-50 ℃, then adds the Sodium dodecylbenzene sulfonate of above-mentioned weight part, is stirred to Sodium dodecylbenzene sulfonate and dissolves fully, gets compound C;
(4) compound A obtained above, B and C are mixed, then acetic acid or sodium-acetate, adjustings PH is 3-5, adds at last the propylene glycol of above-mentioned weight part, fully namely gets the described metallic surface silane finish that contains diethanolamine after the stirring.
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Cited By (3)
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| CN104099003A (en) * | 2014-06-17 | 2014-10-15 | 安徽省六安市朝晖机械制造有限公司 | Environment-friendly aluminum alloy surface treatment agent |
| CN109468009A (en) * | 2018-10-29 | 2019-03-15 | 重庆炫吉科技有限公司 | A kind of environment-friendly type metal surface Coating Pretreatment agent and preparation method |
| 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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| US20060099429A1 (en) * | 2003-02-23 | 2006-05-11 | Heribert Domes | Method for coating metallic surfaces with a composition that is rich in polymers |
| JP2007051365A (en) * | 2005-07-22 | 2007-03-01 | Nippon Steel Corp | Chromate-free surface-treated metal material excellent in corrosion resistance, heat resistance, fingerprint resistance, conductivity, coatability and black-dreg resistance at processing |
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| CN109468009A (en) * | 2018-10-29 | 2019-03-15 | 重庆炫吉科技有限公司 | A kind of environment-friendly type metal surface Coating Pretreatment agent and preparation method |
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