CN103060791B - A kind of Metal surface silane treatment agent containing tetraisopropyl titanate and preparation method thereof - Google Patents
A kind of Metal surface silane treatment agent containing tetraisopropyl titanate and preparation method thereof Download PDFInfo
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- CN103060791B CN103060791B CN201210550823.2A CN201210550823A CN103060791B CN 103060791 B CN103060791 B CN 103060791B CN 201210550823 A CN201210550823 A CN 201210550823A CN 103060791 B CN103060791 B CN 103060791B
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- Prior art keywords
- tetraisopropyl titanate
- metal surface
- treatment agent
- maleic anhydride
- agent containing
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 16
- 239000002184 metal Substances 0.000 title claims abstract description 16
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 13
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 9
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 8
- -1 trihydroxyethyl isocyanuric ester Chemical class 0.000 claims abstract description 8
- KWIPUXXIFQQMKN-UHFFFAOYSA-N 2-azaniumyl-3-(4-cyanophenyl)propanoate Chemical compound OC(=O)C(N)CC1=CC=C(C#N)C=C1 KWIPUXXIFQQMKN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940090948 ammonium benzoate Drugs 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
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 claims abstract description 7
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims abstract description 4
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 4
- 235000019253 formic acid Nutrition 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 7
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 3
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 238000006884 silylation reaction Methods 0.000 claims description 3
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 7
- 239000011159 matrix material Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 229910001335 Galvanized steel Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000008397 galvanized steel Substances 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 3
- 239000012756 surface treatment agent Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229940098458 powder spray Drugs 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000002444 silanisation Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GZCWLCBFPRFLKL-UHFFFAOYSA-N 1-prop-2-ynoxypropan-2-ol Chemical compound CC(O)COCC#C GZCWLCBFPRFLKL-UHFFFAOYSA-N 0.000 description 1
- 102000013563 Acid Phosphatase Human genes 0.000 description 1
- 108010051457 Acid Phosphatase Proteins 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910000737 Duralumin Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 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
- 239000012530 fluid Substances 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000005461 lubrication Methods 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Chemical Treatment Of Metals (AREA)
- Preventing Corrosion Or Incrustation Of Metals (AREA)
Abstract
The invention discloses a kind of Metal surface silane treatment agent containing tetraisopropyl titanate, being made up of following component, in every 500 grams of mixed liquors, the weight (gram) of each component is: tetraisopropyl titanate 1-2, Ammonium benzoate 1-2, Colophonium 3-5, trihydroxyethyl isocyanuric ester 1-2, maleic anhydride 10-12, butyl 4-6, propylene glycol 5-8, formic acid 2-3, N-(�� mono-aminoethyl)-��-aminopropyl front three (second) TMOS 10-12, surplus be deionized water. The present invention adopts Colophonium as reaction raw materials, and the polymerizable raw material such as maleic anhydride, silane, can form stronger protecting film in metal surface; Enhance the decay resistance of metallic matrix.
Description
Technical field
The present invention relates to a kind of metallic surface silanization treating agent and with its metallic surface silanization process technique.
Background technology
Bonderizing is widely applied in coated metal pre-treatment, lubrication, the industry such as antirust. Particularly in Coating Pretreatment industry, bonderizing is one of the most frequently used preprocess method. Bonderizing is the process forming biphosphate ammonium salt protecting film after metal reacts in acid phosphatase ammonium dihydrogen saline solution on its surface. Phosphating coat also has good lubricity, insulating properties and corrosion resistance, thus is widely used in the manufacture field of the products such as automobile, machine-building, Aero-Space and household electrical appliance. Phosphorization treatment process is with ammonium dihydrogen phosphate, zinc, manganese, nickel for primary raw material, cause the Heavy environmental pollution such as heavy metal, phosphorus, nitrite, and in processing procedure, all more or less can produce sediment and harmful gas, what impact produced is normally carried out, and the waste water COD of discharge and heavy metal will endanger environment if do not carried out environmental protection treatment; It addition, bonderizing major part need to carry out when heating, energy consumption is relatively big, complex process, and operation is also inconvenient. The existing silane surface treatment technology that occurs in that, but silane surface treatment agent is unstable in metal surface film forming, and antiseptic property is unstable, poor effect.
Summary of the invention
It is an object of the invention to provide a kind of Metal surface silane treatment agent containing tetraisopropyl titanate and preparation method thereof; this solution need not be heated; not phosphorous, without sediment produce, without heavy metal, energy-conservation, management simplicity; forming stronger protecting film on duralumin, hard alumin ium alloy surface, anticorrosion ability is good.
Technical scheme is as follows:
A kind of Metal surface silane treatment agent containing tetraisopropyl titanate, it is characterised in that be made up of following component, in every 500 grams of mixed liquors, the weight (gram) of each component is:
Tetraisopropyl titanate 1-2, Ammonium benzoate 1-2, Colophonium 3-5, trihydroxyethyl isocyanuric ester 1-2, maleic anhydride 10-12, butyl 4-6, propylene glycol 5-8, formic acid 2-3, N-(�� mono-aminoethyl)-��-aminopropyl front three (second) TMOS 10-12, surplus be deionized water.
1, the preparation method of metal surface silylation protection treating agent according to claim 1, it is characterised in that comprise the following steps:
(1), rosin heating is melted, to 110-115 DEG C, adds butyl, N-(�� mono-aminoethyl)-��-aminopropyl front three (second) TMOS, stirring reaction 35-50 minute;
(2), it is warming up to 145-160 DEG C, adds trihydroxyethyl isocyanuric ester, maleic anhydride, propylene glycol, stirring reaction 40-50 minute;
(3), it is continuously heating to 190-205 DEG C, adds tetraisopropyl titanate, Ammonium benzoate, stirring reaction 40-50 minute;
(4), being cooled to 80-90 DEG C, add other material, stirring, insulation reaction 1-2 hour, after cooling, it was neutral for adjusting PH.
Silane surface treatment agent of the present invention, first metallic matrix can be directly entered in inorganic agent of the present invention and processes after defat, washing, after process, metal base surface can obtain one layer of coating, then can carry out washing or do not wash lower one technique-drying according to process requirements, the operations such as powder spray can be carried out after drying, technological parameter in processing procedure is: operating temperature: room temperature 25 DEG C, and pure water washes electrical conductivity < 20 �� s/cm, processes the time: the 90-250 second.
Compared to the prior art the present invention, has the advantage that
(1) present invention adopts Colophonium as reaction raw materials, and the polymerizable raw material such as maleic anhydride, silane, can form stronger protecting film in metal surface; Enhance the decay resistance of metallic matrix.
(2) containing corrosion inhibiter in raw material, the anticorrosion ability of protecting film is increased.
(3), formed protection rete dense uniform, polarized current density is less.
(4) protection thickness (< 150nm) is significantly less than traditional phosphating solutions film (10 ~ 15 ��m).
Detailed description of the invention
A kind of Metal surface silane treatment agent containing tetraisopropyl titanate, is made up of following component, and in every 500 grams of mixed liquors, the weight (gram) of each raw material components is:
Tetraisopropyl titanate 2, Ammonium benzoate 1, Colophonium 5, trihydroxyethyl isocyanuric ester 1, maleic anhydride 10, butyl 4, propylene glycol 8, formic acid 2-3, N-(�� mono-aminoethyl)-��-aminopropyl front three (second) TMOS 12, surplus be deionized water.
The preparation method of described metal surface silylation protection treating agent, comprises the following steps:
(1), rosin heating is melted, to 110-115 DEG C, adds butyl, N-(�� mono-aminoethyl)-��-aminopropyl front three (second) TMOS, stirring reaction 35-50 minute;
(2), it is warming up to 145-160 DEG C, adds trihydroxyethyl isocyanuric ester, maleic anhydride, propylene glycol, stirring reaction 40-50 minute;
(3), it is continuously heating to 190-205 DEG C, adds tetraisopropyl titanate, Ammonium benzoate, stirring reaction 40-50 minute;
(4), being cooled to 80-90 DEG C, add other material, stirring, insulation reaction 1-2 hour, after cooling, it was neutral for adjusting PH.
First galvanized steel plain sheet can be directly entered in inorganic agent of the present invention and processes after defat, washing, after process, matrix surface can obtain one layer of coating, then can carry out washing or do not wash lower one technique-drying according to process requirements, the operations such as powder spray can be carried out after drying, technological parameter in processing procedure is: operating temperature: room temperature 25 DEG C, pure water washes electrical conductivity < 20 �� s/cm, processes the time: the 90-250 second.
Galvanized steel plain sheet first adopts alkali-free degreasing fluid to carry out washing and removes oil stain, places in silane surface treatment agent of the present invention and processes, and after drying, carries out immersion test, adopts the NaCl aqueous solution of 0.1M, observes sample surfaces situation; Testing impedance carries out in 3.5 (wt) %NaCl aqueous solution. Galvanized steel plain sheet does not occur red rust for 10 days, and detection coating is 7.6Mpa, Z 10mHz value with galvanized steel plain sheet adhesion strength is 2.7E7.
Claims (1)
1. the Metal surface silane treatment agent containing tetraisopropyl titanate, it is characterized in that, being made up of following component, in every 500 grams of mixed liquors, the weight of each component is calculated as in grams: tetraisopropyl titanate 1-2, Ammonium benzoate 1-2, Colophonium 3-5, trihydroxyethyl isocyanuric ester 1-2, maleic anhydride 10-12, butyl 4-6, propylene glycol 5-8, formic acid 2-3, N-(�� mono-aminoethyl)-��-aminopropyl front three (second) TMOS 10-12, surplus be deionized water; The preparation method of described metal surface silylation protection treating agent, comprise the following steps: (1), by rosin heating melt, to 110-115 DEG C, add butyl, N-(�� mono-aminoethyl)-��-aminopropyl front three (second) TMOS, stirring reaction 35-50 minute; (2), it is warming up to 145-160 DEG C, adds trihydroxyethyl isocyanuric ester, maleic anhydride, propylene glycol, stirring reaction 40-50 minute; (3), it is continuously heating to 190-205 DEG C, adds tetraisopropyl titanate, Ammonium benzoate, stirring reaction 40-50 minute; (4), being cooled to 80-90 DEG C, add other material, stirring, insulation reaction 1-2 hour, after cooling, it was neutral for adjusting pH.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210550823.2A CN103060791B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing tetraisopropyl titanate and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210550823.2A CN103060791B (en) | 2012-12-18 | 2012-12-18 | A kind of Metal surface silane treatment agent containing tetraisopropyl titanate and preparation method thereof |
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| CN103060791A CN103060791A (en) | 2013-04-24 |
| CN103060791B true CN103060791B (en) | 2016-06-08 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| SG11201509980QA (en) * | 2013-06-06 | 2016-01-28 | Honeywell Int Inc | Liquid titanium oxide compositions, methods for forming the same, and methods for etching material layers of or overlying substrates using the same |
| 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 |
| CN104099012B (en) * | 2014-06-19 | 2016-08-24 | 锐展(铜陵)科技有限公司 | A kind of whisker type Aluminum alloy surface treatment agent |
| CN104109850A (en) * | 2014-06-19 | 2014-10-22 | 锐展(铜陵)科技有限公司 | Salt fog resistant aluminum alloy surface treating agent |
| CN105400427A (en) * | 2015-11-14 | 2016-03-16 | 合肥标兵凯基新型材料有限公司 | High-performance surfactant for pop cans |
| CN105441967A (en) * | 2015-11-14 | 2016-03-30 | 合肥标兵凯基新型材料有限公司 | Surface treating agent used for zip-top can and preparation method of surface treating agent |
| CN106756909A (en) * | 2016-05-31 | 2017-05-31 | 陈斌 | A kind of stainless steel surface protective agent for surface treatment and preparation method thereof |
| CN106811578A (en) * | 2017-02-14 | 2017-06-09 | 江苏广通管业制造有限公司 | A kind of method for forming alkali resistant layer in stainless steel surfaces |
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| JP4537377B2 (en) * | 2003-02-25 | 2010-09-01 | ヒェメタル ゲゼルシャフト ミット ベシュレンクテル ハフツング | Method for coating a metal surface with a polymer-rich composition |
| CN101643898B (en) * | 2009-09-04 | 2010-12-29 | 吴伟峰 | Phosphorus-free film forming agent and preparation method thereof |
| CN101713069B (en) * | 2009-11-16 | 2011-05-04 | 浙江大学 | Method for preparing additive homogeneous phase modified solution of silane and application thereof |
| CN102409325B (en) * | 2011-12-06 | 2014-06-11 | 中国科学院金属研究所 | Environmentally-friendly corrosion-resistant chromium-free chemical conversion liquid and method for preparing chemical conversion film |
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Effective date of registration: 20190419 Address after: Room C422, 4th Floor, 189 Xinjun Ring Road, Minhang District, Shanghai 201100 Patentee after: SHANGHAI BLUE SILANE NEW MATERIAL TECHNOLOGY Co.,Ltd. Address before: 241007 5 Yang Tian Road, Jiujiang Economic Development Zone, Wuhu, Anhui Patentee before: WUHU HENGKUN AUTO PARTS Co.,Ltd. |
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