CN103060787B - A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof - Google Patents
A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof Download PDFInfo
- Publication number
- CN103060787B CN103060787B CN201210550790.1A CN201210550790A CN103060787B CN 103060787 B CN103060787 B CN 103060787B CN 201210550790 A CN201210550790 A CN 201210550790A CN 103060787 B CN103060787 B CN 103060787B
- Authority
- CN
- China
- Prior art keywords
- water
- weight part
- zinc oxide
- treatment agent
- nano zinc
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 25
- 239000002184 metal Substances 0.000 title claims abstract description 25
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000011787 zinc oxide Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 22
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 21
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 14
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000019832 sodium triphosphate Nutrition 0.000 claims abstract description 14
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims abstract description 10
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical compound F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 claims abstract description 8
- 101710194948 Protein phosphatase PhpP Proteins 0.000 claims abstract description 7
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 7
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 7
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 claims abstract description 7
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 7
- 239000011734 sodium Substances 0.000 claims abstract description 7
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 claims abstract description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 12
- 229960004756 ethanol Drugs 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 229940126062 Compound A Drugs 0.000 claims description 6
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 229960004249 sodium acetate Drugs 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 0.000 claims description 3
- LVTJOONKWUXEFR-FZRMHRINSA-N protoneodioscin Natural products O(C[C@@H](CC[C@]1(O)[C@H](C)[C@@H]2[C@]3(C)[C@H]([C@H]4[C@@H]([C@]5(C)C(=CC4)C[C@@H](O[C@@H]4[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@@H](O)[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@H](CO)O4)CC5)CC3)C[C@@H]2O1)C)[C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1 LVTJOONKWUXEFR-FZRMHRINSA-N 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 12
- 239000012756 surface treatment agent Substances 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- HXJZEGBVQCRLOD-UHFFFAOYSA-N 1-triethoxysilylpropan-2-amine Chemical compound CCO[Si](CC(C)N)(OCC)OCC HXJZEGBVQCRLOD-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 238000000280 densification Methods 0.000 abstract description 2
- 230000003245 working effect Effects 0.000 abstract description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000005452 bending Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 238000004532 chromating Methods 0.000 description 2
- 238000004299 exfoliation Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- LYCAIKOWRPUZTN-NMQOAUCRSA-N 1,2-dideuteriooxyethane Chemical compound [2H]OCCO[2H] LYCAIKOWRPUZTN-NMQOAUCRSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- -1 chromium Chemical compound 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002224 dissection Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Landscapes
- Chemical Treatment Of Metals (AREA)
Abstract
The invention discloses a kind of Metal surface silane treatment agent containing diethanolamine, 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: 1, two (triethoxy is silica-based) ethane 28-35 of 2-, 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, butyl 1-2, TriMethylolPropane(TMP) 1-2, Sodium dodecylbenzene sulfonate 0.3-0.5, remaining is water, 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, by 1, two (triethoxy the is silica-based) ethane of 2-and γ-aminopropyl triethoxysilane combine use, can form densification and firmly coating in metallic surface.
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 Metal surface silane treatment agent containing 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 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 Metal surface silane treatment agent containing diethanolamine, the mixed solution formulated by following component, in often liter of mixed solution, the weight part (gram) of each component is:
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, butyl 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) 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) by 1, two (triethoxy the is silica-based) ethane of 2-dissolves in ethanol, be prepared into the solution that mass concentration is 2-4%, join in above-mentioned modified nano zinc oxide slurry, be 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, described nano zine oxide, glycerol, 1, the mass ratio of the water in two (triethoxy the is silica-based) ethane of 2-and step (2), the ethanol in step (3) is: two (triethoxy is silica-based) ethane of nano zine oxide: glycerol: 1,2-: 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 Metal surface silane treatment agent containing diethanolamine, comprises the following steps:
(1) 1,2-of above-mentioned weight part two (triethoxy is silica-based) ethane is added in the water of above-mentioned weight part 60-70%, add the γ-aminopropyl triethoxysilane of above-mentioned weight part after fully dissolving again, fully stir, obtain compound A;
(2) 60-70% of residue water is got, add the water nano zinc oxide material of above-mentioned weight part, after abundant stirring, add the tripoly phosphate sodium STPP of above-mentioned weight part, zirconium tetrafluoride, diethanolamine, ammonium chloride, butyl, TriMethylolPropane(TMP) fully stir, obtain compound B;
(3) vinylcarbinol of above-mentioned weight part and ethylene glycol are mixed with remaining water, be heated to 40-50 DEG C, then add the Sodium dodecylbenzene sulfonate of above-mentioned weight part, be stirred to Sodium dodecylbenzene sulfonate and dissolve completely, obtain compound C;
(4) by compound A, B and C mixing obtained above, then acetic acid or sodium-acetate, adjustment PH is 3-5, finally adds the propylene glycol of above-mentioned weight part, namely obtains the described Metal surface silane treatment agent containing diethanolamine 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, by 1, two (triethoxy the is silica-based) ethane of 2-and γ-aminopropyl triethoxysilane combine use, 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 zirconium tetrafluoride 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 Metal surface silane treatment agent containing diethanolamine, the mixed solution formulated by following component, in often liter of mixed solution, the weight part (gram) of each component is:
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, butyl 2, TriMethylolPropane(TMP) 2, Sodium dodecylbenzene sulfonate 0.5, 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 5 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 2 hours 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) by 1, two (triethoxy the is silica-based) ethane of 2-dissolves in ethanol, be prepared into the solution that mass concentration is 2%, join in above-mentioned modified nano zinc oxide slurry, be 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, described nano zine oxide, glycerol, 1, the mass ratio of the water in two (triethoxy the is silica-based) ethane of 2-and step (2), the ethanol in step (3) is: two (triethoxy is silica-based) ethane of nano zine oxide: glycerol: 1,2-: water: ethanol is 15g:2g:4g:105 gram: 105 grams.
The granularity of described nano zine oxide is 50nm.
A preparation method for Metal surface silane treatment agent containing diethanolamine, comprises the following steps:
(1) 1,2-of above-mentioned weight part two (triethoxy is silica-based) ethane is added in the water of above-mentioned weight part 70%, add the γ-aminopropyl triethoxysilane of above-mentioned weight part after fully dissolving again, fully stir, obtain compound A;
(2) 70% of residue water is got, add the water nano zinc oxide material of above-mentioned weight part, after abundant stirring, add the tripoly phosphate sodium STPP of above-mentioned weight part, zirconium tetrafluoride, diethanolamine, ammonium chloride, butyl, TriMethylolPropane(TMP) fully stir, obtain compound B;
(3) vinylcarbinol of above-mentioned weight part and ethylene glycol are mixed with remaining water, be heated to 50 DEG C, then add the Sodium dodecylbenzene sulfonate of above-mentioned weight part, be stirred to Sodium dodecylbenzene sulfonate and dissolve completely, obtain compound C;
(4) by compound A, B and C mixing obtained above, then acetic acid or sodium-acetate, regulates PH to be 5, finally adds the propylene glycol of above-mentioned weight part, namely obtains the described Metal surface silane treatment agent containing diethanolamine after fully stirring.
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. the Metal surface silane treatment agent containing diethanolamine, it is characterized in that by the formulated mixed solution of following component, in often liter of mixed solution, the weight part of each component is: 1, two (triethoxy is silica-based) ethane 28-35g of 2-, γ-aminopropyl triethoxysilane 32-40g, water nano zinc oxide material 100-160g, vinylcarbinol 2-3g, ethylene glycol 1-2g, tripoly phosphate sodium STPP 2-3g, propylene glycol 2-4g, zirconium tetrafluoride 2-3g, diethanolamine 2-3g, ammonium chloride 2-3g, butyl 1-2g, TriMethylolPropane(TMP) 1-2g, Sodium dodecylbenzene sulfonate 0.3-0.5g, remaining is 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) by 1, two (triethoxy the is silica-based) ethane of 2-dissolves in ethanol, be prepared into the solution that mass concentration is 2-4%, join in above-mentioned modified nano zinc oxide slurry, be 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. a kind of Metal surface silane treatment agent containing diethanolamine according to claim 1, it is characterized in that, in the preparation method of described water nano zinc oxide material, described nano zine oxide, glycerol, 1, the mass ratio of the water in two (triethoxy the is silica-based) ethane of 2-and step (2), the ethanol in step (3) is: two (triethoxy is silica-based) ethane of nano zine oxide: glycerol: 1,2-: water: ethanol is 10-15g:1-2g:2-4g:95-105g:95-105g.
3. a kind of Metal surface silane treatment agent containing diethanolamine according to claim 1, is characterized in that the granularity of described nano zine oxide is 40-50nm.
4. a preparation method for the Metal surface silane treatment agent containing diethanolamine as claimed in claim 1, is characterized in that comprising the following steps:
(1) 1,2-of above-mentioned weight part two (triethoxy is silica-based) ethane is added in the water of above-mentioned weight part 60-70%, add the γ-aminopropyl triethoxysilane of above-mentioned weight part after fully dissolving again, fully stir, obtain compound A;
(2) 60-70% of residue water is got, add the water nano zinc oxide material of above-mentioned weight part, after abundant stirring, add the tripoly phosphate sodium STPP of above-mentioned weight part, zirconium tetrafluoride, diethanolamine, ammonium chloride, butyl, TriMethylolPropane(TMP) fully stir, obtain compound B;
(3) vinylcarbinol of above-mentioned weight part and ethylene glycol are mixed with remaining water, be heated to 40-50 DEG C, then add the Sodium dodecylbenzene sulfonate of above-mentioned weight part, be stirred to Sodium dodecylbenzene sulfonate and dissolve completely, 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 the propylene glycol of above-mentioned weight part, namely obtains the described Metal surface silane treatment agent containing diethanolamine after fully stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210550790.1A CN103060787B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210550790.1A CN103060787B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103060787A CN103060787A (en) | 2013-04-24 |
| CN103060787B true CN103060787B (en) | 2016-03-02 |
Family
ID=48103674
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210550790.1A Active CN103060787B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103060787B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109468009B (en) * | 2018-10-29 | 2020-12-18 | 重庆炫吉科技有限公司 | Environment-friendly metal surface coating pretreatment agent and preparation method thereof |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101287784A (en) * | 2005-08-26 | 2008-10-15 | Ppg工业俄亥俄公司 | Coating compositions exhibiting corrosion resistance properties, related coated substrates, and methods |
| CN101434748A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
| CN102121104A (en) * | 2011-01-22 | 2011-07-13 | 安徽工业大学 | Aqueous chromium-free surface treatment solution for combining color coating pretreatment and base paint coating of galvanized plate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060193988A1 (en) * | 2003-02-25 | 2006-08-31 | Manfred Walter | Method for coating metallic surfaces with a mixture containing at least two silanes |
| JP4776458B2 (en) * | 2005-07-22 | 2011-09-21 | 新日本製鐵株式会社 | Chromate-free surface-treated metal material with excellent corrosion resistance, heat resistance, fingerprint resistance, conductivity, paintability, and black residue resistance during processing |
-
2012
- 2012-12-18 CN CN201210550790.1A patent/CN103060787B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101287784A (en) * | 2005-08-26 | 2008-10-15 | Ppg工业俄亥俄公司 | Coating compositions exhibiting corrosion resistance properties, related coated substrates, and methods |
| CN101434748A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Preparation of nano zinc oxide modified organosilicon encapsulation adhesive |
| CN102121104A (en) * | 2011-01-22 | 2011-07-13 | 安徽工业大学 | Aqueous chromium-free surface treatment solution for combining color coating pretreatment and base paint coating of galvanized plate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103060787A (en) | 2013-04-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102560469B (en) | Metal surface silylation protection treating agent | |
| CN103183989B (en) | Water-borne rust-based anticorrosion coating and preparation method thereof | |
| CN103031056A (en) | Metal surface silane treating agent containing aqueous nano-zinc oxide and preparation method thereof | |
| CN102140667B (en) | Rear earth polyoxometallate silanization process for metal cathode before electrophoresis | |
| CN115261839B (en) | Passivating solution for passivating high corrosion-resistant alloy | |
| CN103183990B (en) | Environment-friendly water-based anticorrosive paint and preparation method thereof | |
| CN103060787B (en) | A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof | |
| CN107012453B (en) | A kind of method that green low temperature quickly prepares phosphating coat | |
| CN103183991B (en) | Antirust coating with high acid resistance and preparation method thereof | |
| CN107475704B (en) | Metal surface silane treatment agent and preparation method thereof | |
| CN103031551B (en) | A kind of metal surface silane finish that contains ethylenediamine tetramethylene fork Alendronate and preparation method thereof | |
| CN103031549B (en) | A kind of metal surface silane finish that contains diethyl toluene diamine and preparation method thereof | |
| CN103088327A (en) | Metal surface silane treatment agent containing water-soluble phenolic resin and preparation method thereof | |
| CN103087627B (en) | A kind of metal aluminum alloy silane surface treatment agent and preparation method thereof | |
| CN103045086B (en) | A kind of Metal surface silane treatment agent and preparation method thereof | |
| CN103102724A (en) | Metal surface silane treating agent containing acrylic acid and preparation method of metal surface silane treating agent | |
| CN103059728B (en) | A kind of corrosion resistant Metal surface silane treatment agent and preparation method thereof | |
| CN103031548B (en) | A kind of metal surface silane finish that contains ammonium metavanadate and preparation method thereof | |
| CN103059727B (en) | A kind of Metal surface silane treatment agent containing HMPA and preparation method thereof | |
| CN103088328A (en) | Silane finishing agent at surface of galvanized steel sheet and preparation method thereof | |
| CN103031057A (en) | Metal surface silane treating agent containing plant ash and preparation method thereof | |
| CN104099595A (en) | Surface treating agent for wipe resistant aluminum alloy | |
| CN103059723A (en) | Stripping-resistant metal surface silicane treating agent and preparation method thereof | |
| CN103059722B (en) | A kind of Metal surface silane treatment agent containing carboxymethyl cellulose and preparation method thereof | |
| CN104099597B (en) | A kind of volcanic ash Aluminum alloy surface treatment agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A metal surface silane treatment agent containing diethanolamine and its preparation method Granted publication date: 20160302 Pledgee: Wuhu Yangzi rural commercial bank Limited by Share Ltd. Pledgor: ANHUI LIUFANG ZHONGLIAN MECHANICAL SHARE Co.,Ltd. Registration number: Y2024980033735 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |