CN103059727A - Metal surface silicane treating agent containing hexamethylphosphoric triamide and preparing method thereof - Google Patents
Metal surface silicane treating agent containing hexamethylphosphoric triamide and preparing method thereof Download PDFInfo
- Publication number
- CN103059727A CN103059727A CN2012105507329A CN201210550732A CN103059727A CN 103059727 A CN103059727 A CN 103059727A CN 2012105507329 A CN2012105507329 A CN 2012105507329A CN 201210550732 A CN201210550732 A CN 201210550732A CN 103059727 A CN103059727 A CN 103059727A
- Authority
- CN
- China
- Prior art keywords
- water
- zinc oxide
- weight part
- silicane
- hmpa
- 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.)
- Granted
Links
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 37
- GNOIPBMMFNIUFM-UHFFFAOYSA-N hexamethylphosphoric triamide Chemical compound CN(C)P(=O)(N(C)C)N(C)C GNOIPBMMFNIUFM-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910052751 metal Inorganic materials 0.000 title abstract description 14
- 239000002184 metal Substances 0.000 title abstract description 14
- 238000000034 method Methods 0.000 title description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 54
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000011787 zinc oxide Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims abstract description 10
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 claims abstract description 8
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 229910000077 silane Inorganic materials 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 235000011187 glycerol Nutrition 0.000 claims description 15
- 238000002360 preparation method Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 12
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 claims description 10
- KOVKEDGZABFDPF-UHFFFAOYSA-N n-(triethoxysilylmethyl)aniline Chemical compound CCO[Si](OCC)(OCC)CNC1=CC=CC=C1 KOVKEDGZABFDPF-UHFFFAOYSA-N 0.000 claims description 10
- 229960004756 ethanol Drugs 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 238000012545 processing 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
- 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
- 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
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- -1 N-(beta- aminoethyl)-gamma-aminopropyl Chemical group 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N N-phenyl amine Natural products NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 abstract 2
- 239000012964 benzotriazole Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 239000012756 surface treatment agent Substances 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 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
- 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
- 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
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000000280 densification Methods 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
- 230000003245 working effect Effects 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)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a metal surface silicane treating agent containing hexamethylphosphoric triamide. The metal surface silicane treating agent containing the hexamethylphosphoric triamide is characterized by being a mixed solution which is prepared from following compositions of, by weight in every liter of the mixed solution, 35-45g of aniline methyl triethoxy silicane, 35-45g of N-(beta- aminoethyl)-gamma-aminopropyl trimethoxy silicane, 100-180g of aqueous nanometer zinc oxide material, 3-4g of glycerol, 2-3g of diethylene glycol, 2-4g of ethylene glycol monobutyl ether, 2-3g of titanium tetrafluoride, 2-3g of hexamethylphosphoric triamide, 2-3g of urea, 1-2g of citric acid, 0.3-0.6g of benzotriazole, and the balance water. The metal surface silicane treating agent containing the hexamethylphosphoric triamide 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 aniline methyl triethoxy silicane and the N-(beta- aminoethyl)-gamma-aminopropyl trimethoxy 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 HMPA 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 HMPA, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
Anilinomethyl triethoxysilane 35-45, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 35-45, water nano zinc oxide material 100-180, glycerine 3-4, glycol ether 2-3, ethylene glycol monobutyl ether 2-4, titanium tetrafluoride 2-3, HMPA 2-3, urea 2-3, citric acid 1-2, azimidobenzene 0.3-0.6, 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) N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 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.
A kind of metallic surface silane finish that contains HMPA, among the preparation method of described water nano zinc oxide material, the water in described nano zine oxide, glycerol, vinyl three ('beta '-methoxy oxyethyl group) silane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: N-(β-aminoethyl)-γ-aminopropyl trimethoxy silicon: 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 HMPA may further comprise the steps:
(1) anilinomethyl triethoxysilane with above-mentioned weight part adds in the water of above-mentioned weight part 60-70%, fully adds the N-(β-aminoethyl) of above-mentioned weight part-γ-aminopropyltrimethoxysilane after the dissolving again, fully stirs, and gets compound A;
(2) get the 60-70% that remains water, add the water nano zinc oxide material of above-mentioned weight part, after fully stirring, the titanium tetrafluoride, HMPA, urea, the citric acid that add above-mentioned weight part fully stir, and get compound B;
(3) glycerine and the glycol ether with above-mentioned weight part mixes with remaining water, is heated to 40-50 ℃, then adds the azimidobenzene of above-mentioned weight part, is stirred to azimidobenzene 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 ethylene glycol monobutyl ether of above-mentioned weight part, fully namely gets the described metallic surface silane finish that contains HMPA 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 the use that combines of anilinomethyl triethoxysilane and N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, 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 titanium tetrafluoride that add, 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 metallic surface silane finish that contains HMPA, by the formulated mixed solution of following component, the weight part (gram) of each component is in every liter of mixed solution:
Anilinomethyl triethoxysilane 45, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 45, water nano zinc oxide material 140, glycerine 4, glycol ether 3, ethylene glycol monobutyl ether 4, titanium tetrafluoride 3, HMPA 3, urea 3, citric acid 1, azimidobenzene 0.6, 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 3%, 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) N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 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 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, vinyl three ('beta '-methoxy oxyethyl group) silane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: N-(β-aminoethyl)-γ-aminopropyl trimethoxy silicon: 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 HMPA may further comprise the steps:
(1) anilinomethyl triethoxysilane with above-mentioned weight part adds in the water of above-mentioned weight part 60-70%, fully adds the N-(β-aminoethyl) of above-mentioned weight part-γ-aminopropyltrimethoxysilane after the dissolving again, fully stirs, and gets compound A;
(2) get the 60-70% that remains water, add the water nano zinc oxide material of above-mentioned weight part, after fully stirring, the titanium tetrafluoride, HMPA, urea, the citric acid that add above-mentioned weight part fully stir, and get compound B;
(3) glycerine and the glycol ether with above-mentioned weight part mixes with remaining water, is heated to 40-50 ℃, then adds the azimidobenzene of above-mentioned weight part, is stirred to azimidobenzene 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 ethylene glycol monobutyl ether of above-mentioned weight part, fully namely gets the described metallic surface silane finish that contains HMPA after the 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 HMPA 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:
Anilinomethyl triethoxysilane 35-45, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 35-45, water nano zinc oxide material 100-180, glycerine 3-4, glycol ether 2-3, ethylene glycol monobutyl ether 2-4, titanium tetrafluoride 2-3, stablizer HMPA 2-3, urea 2-3, citric acid 1-2, azimidobenzene 0.3-0.6, 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) N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane 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 HMPA 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, vinyl three ('beta '-methoxy oxyethyl group) silane and the step (2), the mass ratio of the ethanol in the step (3) are: nano zine oxide: glycerol: N-(β-aminoethyl)-γ-aminopropyl trimethoxy silicon: 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 HMPA 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 HMPA as claimed in claim 1 is characterized in that may further comprise the steps:
(1) anilinomethyl triethoxysilane with above-mentioned weight part adds in the water of above-mentioned weight part 60-70%, fully adds the N-(β-aminoethyl) of above-mentioned weight part-γ-aminopropyltrimethoxysilane after the dissolving again, fully stirs, and gets compound A;
(2) get the 60-70% that remains water, add the water nano zinc oxide material of above-mentioned weight part, after fully stirring, the titanium tetrafluoride, HMPA, urea, the citric acid that add above-mentioned weight part fully stir, and get compound B;
(3) glycerine and the glycol ether with above-mentioned weight part mixes with remaining water, is heated to 40-50 ℃, then adds the azimidobenzene of above-mentioned weight part, is stirred to azimidobenzene 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 ethylene glycol monobutyl ether of above-mentioned weight part, fully namely gets the described metallic surface silane finish that contains HMPA after the stirring.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210550732.9A CN103059727B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing HMPA and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210550732.9A CN103059727B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing HMPA and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103059727A true CN103059727A (en) | 2013-04-24 |
| CN103059727B CN103059727B (en) | 2016-03-02 |
Family
ID=48102637
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210550732.9A Active CN103059727B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing HMPA and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103059727B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2624076A (en) * | 2022-11-02 | 2024-05-08 | Hitachi Ltd | Metal surface treatment agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008062618A1 (en) * | 2006-11-21 | 2008-05-29 | Nihon Parkerizing Co., Ltd. | Aqueous surface treatment for environment-friendly precoated metal materials, surface-treated metal materials, and environment-friendly precoated metal materials |
| CN101857755A (en) * | 2010-06-30 | 2010-10-13 | 张俊锋 | Emulsion paint coating surface water-repellent coating agent and preparation method thereof |
-
2012
- 2012-12-18 CN CN201210550732.9A patent/CN103059727B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008062618A1 (en) * | 2006-11-21 | 2008-05-29 | Nihon Parkerizing Co., Ltd. | Aqueous surface treatment for environment-friendly precoated metal materials, surface-treated metal materials, and environment-friendly precoated metal materials |
| CN101857755A (en) * | 2010-06-30 | 2010-10-13 | 张俊锋 | Emulsion paint coating surface water-repellent coating agent and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2624076A (en) * | 2022-11-02 | 2024-05-08 | Hitachi Ltd | Metal surface treatment agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103059727B (en) | 2016-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103031056B (en) | A kind of Metal surface silane treatment agent containing water nano zinc oxide material and preparation method thereof | |
| CN101643898B (en) | Phosphorus-free film forming agent and preparation method thereof | |
| CN106906462B (en) | A kind of metal surface pretreating reagent and preparation method thereof, application | |
| CN102560469B (en) | Metal surface silylation protection treating agent | |
| CN104630765A (en) | Environmental-protection type metal coating pre-treatment agent and preparation method thereof | |
| CN107012456B (en) | Modified metal surface pretreating reagent of a kind of alkoxyl silicone ethyl Polyhedral Oligomeric silsesquioxane and preparation method thereof, application | |
| 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 | |
| CN103059721A (en) | Metal surface silicane treating agent containing polyethylene glycol and preparing method thereof | |
| CN102732869A (en) | Chromium-free passivating agent for galvanized plate with organosilane as main component and preparation process thereof | |
| CN106894009B (en) | A kind of epoxy group POSS modified metal surface pretreating reagent and preparation method thereof, application | |
| CN104278260B (en) | A kind of silanization treating agent for aluminum alloy surface and preparation method thereof | |
| CN106085089A (en) | A kind of aeroge metallic copper corrosion-inhibiting coating and preparation method thereof | |
| CN103088327A (en) | Metal surface silane treatment agent containing water-soluble phenolic resin and preparation method thereof | |
| CN103060787B (en) | A kind of Metal surface silane treatment agent containing diethanolamine and preparation method thereof | |
| CN103087627B (en) | A kind of metal aluminum alloy silane surface treatment agent and preparation method thereof | |
| CN109181525B (en) | Polyaniline-silane-nano ceramic composite surface treating agent | |
| CN103102724B (en) | A kind of containing acrylic acid Metal surface silane treatment agent and preparation method thereof | |
| CN106835093A (en) | A kind of Q types POSS modified metal surface pretreating reagent and preparation method thereof, application | |
| CN103045086B (en) | A kind of 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 | |
| CN103059727A (en) | Metal surface silicane treating agent containing hexamethylphosphoric triamide and preparing method thereof | |
| CN107868544A (en) | A kind of metal surface filming agent and preparation method thereof | |
| CN103059728B (en) | A kind of corrosion resistant Metal surface silane treatment agent and preparation method thereof | |
| CN114164423B (en) | Chromium-free passivation solution and preparation method and application thereof |
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 hexamethylphosphoramide 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 |