CN104060276B - A kind of metal surface silane coating corrosion inhibiter - Google Patents
A kind of metal surface silane coating corrosion inhibiter Download PDFInfo
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- CN104060276B CN104060276B CN201410311848.6A CN201410311848A CN104060276B CN 104060276 B CN104060276 B CN 104060276B CN 201410311848 A CN201410311848 A CN 201410311848A CN 104060276 B CN104060276 B CN 104060276B
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Abstract
A kind of metal surface silane coating corrosion inhibiter, including: nano-fluorine carbon cerium CeFCO3Need to be become lipophile through processing with acrylic acid trifluoro ethyl ester surface aggregate from hydrophilic, then with 1-hexyl-2,3-methylimidazole tetrafluoroborate ionic liquid is mixed to get product through sufficiently.In silane coupled prefilming agent, add the anti-corrosion reinforcing agent of the present invention, composite membrane can be made to have certain self-reparing capability.
Description
Technical field
The present invention relates to the preparation method of a kind of corrosion inhibiter, the preparation of a kind of metal surface silane coating corrosion inhibiter
Method.
Background technology
At present, corrosion inhibiter has become one of most widely used method in anticorrosion technique, in protection resource, reduces material
Loss aspect is fully developed talents.Compared with other anti-corrosion methods, corrosion inhibiter has and does not changes corrosive environment, does not increase equipment and throws
Money, is not affected by device shaped, and same formula can prevent the advantages such as various metals corrosion in different environments sometimes simultaneously.
But, due to some limitation of single corrosion inhibiter and the situation such as cause coating appearance uneven, need to add adding of trace
Add agent, in order to preferably improve the corrosion resisting property of corrosion inhibiter.Environmentally friendly Conversion Coating Technology receives significant attention.Have
Machine corrosion inhibiter chemical stability is good, not facile hydrolysis and degraded, and inhibition, scale inhibition effect are good, and using dosage is little.Containing long in some molecule
The organic acid esters corrosion inhibiter of alkyl group has and the ability of metal ion formation coordination compound, under certain concentration, and can be at metal
Surface self-organization becomes to have good corrosion mitigating effect and hydrophobic protecting film.Organosilan as the effective anticolodal of one,
The advantages such as its technical process is pollution-free, treatment conditions are gentle.
CN 103087629 discloses a kind of Anti-corrosion metal surface silane treatment agent and preparation method thereof, by following component
Formulated mixed liquor, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, film-forming resin, monoethanolamine benzoate,
Waterborne polyurethane resin, triethanolamine, propylene glycol, sodium tripolyphosphate, carboxymethyl cellulose, phytic acid, polydimethylsiloxane, ten
Dialkyl benzene sulfonic acids sodium, citric acid and isopropanol；The present invention uses N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane to make
For major ingredient, isopropanol is solvent, with low cost, adds waterborne polyurethane resin and multiple different auxiliary agent simultaneously, improve in raw material
Process time of inorganic agent and treatment temperature.
Traditional metal surface silane coating is the silane film preparing single component in metal surface, and thin film consistency is relatively
Low, it is commonly present pore and micro-crack so that the corrosion resistance of metal surface is unsatisfactory.At present, though scholars uses
Composite membrane, Modified Membrane, interpolation corrosion inhibiter or add the method such as nanoparticle in Silan-based Thin Films, improve the anti-corrosion of silane film
Property, or utilize electrochemical method to improve its corrosion resistance, but the corrosion resistance of silane film is still below phosphatization and chromate passivation film, and silicon
Alkane film itself does not possess self-reparing capability.Have impact on the using effect in commercial plant.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of metal surface silane coating corrosion inhibiter.
Nano-fluorine carbon cerium CeFCO3Oleophylic need to be become from hydrophilic through processing with acrylic acid trifluoro ethyl ester surface aggregate
Property, then with 1-hexyl-2,3-methylimidazole tetrafluoroborate ionic liquid is mixed to get product through sufficiently.
The present invention provides a kind of metal surface silane coating corrosion inhibiter, is realized by following steps:
Step 1. nano-fluorine carbon cerium CeFCO3Surface aggregate:
By a certain amount of nano-fluorine carbon cerium CeFCO3It is distributed in ethanol, adds acrylic acid trifluoro ethyl ester list in following ratio
Body, benzoyl peroxide and polyvinyl alcohol, dodecylbenzene sodium sulfonate etc., heat up, and reacts 6-15 hour at 60-80 DEG C, to obtain final product
To the nano-fluorine carbon cerium CeFCO through surface aggregate3Fine suspension.
Step 2. adds ionic liquid:
Nano-fluorine carbon cerium CeFCO3Fine suspension and 1-hexyl-2,3-methylimidazole tetrafluoroborate with mass ratio is
The proportioning of 95-99: 1-5 mixes 10-40hr in a kettle., obtains product.
Described nano-fluorine carbon cerium CeFCO3For commercially available prod, the product developed such as Panxi, Sichuan rare earth responsibility company limited
Product.
Described acrylic acid trifluoro ethyl ester is commercially available prod, the product produced such as Harbin Xue Jiafu chemistry of silicones company limited
Product.
Molecular formula: C6H7O2F3。
Described 1-hexyl-2,3-methylimidazole tetrafluoroborate ionic liquid, for commercially available prod, such as Chinese Academy of Sciences Lanzhou
Learn the ionic liquid product that physics Institute produces.
Molecular formula: C11H21N2BF4。
In silane coupled prefilming agent, add the metal surface silane coating corrosion inhibiter 1-10wt% of the present invention, can make multiple
Close film and there is certain self-reparing capability.
Described silane coupled prefilming agent refers to the metal surface prefilming agent in component containing silane coupler, for commercially available product
Product, reach, as Zhejiang is omnipotent, the product that Science and Technology Ltd. produces.
Beneficial effects of the present invention:
1) fluorine-containing rare earth ion, 1-hexyl-2,3-methylimidazole tetrafluoroborate ionic liquid can effectively suppress metal
The anode of matrix and cathode reaction, can improve the corrosion resistance of silane film.
2) in silane coupled prefilming agent, add the metal surface silane coating corrosion inhibiter of the present invention, composite membrane can be made to have
There is certain self-reparing capability.
Detailed description of the invention
Following example only further illustrate the present invention, are not to limit the scope of protection of the invention.
Embodiment 1
Step 1. nano-fluorine carbon cerium CeFCO3Surface aggregate:
In 500L reactor, add nano-fluorine carbon cerium CeFCO by following proportioning3It is distributed in ethanol, in following ratio
Add acrylic acid trifluoro ethyl ester monomer, benzoyl peroxide and polyvinyl alcohol, dodecylbenzene sodium sulfonate etc., heat up, at 80 DEG C
React 6 hours, i.e. obtain the nano-fluorine carbon cerium CeFCO through surface aggregate3Fine suspension.
Step 2. adds ionic liquid:
In 500L reactor, add nano-fluorine carbon cerium CeFCO3Fine suspension 97Kg, 1-hexyl-2,3-methylimidazole
Tetrafluoroborate ionic liquid 3Kg, mixes 20hr in a kettle., obtains product, numbered SX-1.
Embodiment 2
Step 1. nano-fluorine carbon cerium CeFCO3Surface aggregate:
In 500L reactor, add nano-fluorine carbon cerium CeFCO by following proportioning3It is distributed in ethanol, in following ratio
Add acrylic acid trifluoro ethyl ester monomer, benzoyl peroxide and polyvinyl alcohol, dodecylbenzene sodium sulfonate etc., heat up, at 70 DEG C
React 10 hours, i.e. obtain the nano-fluorine carbon cerium CeFCO through surface aggregate3Fine suspension.
Step 2. adds ionic liquid:
In 500L reactor, add nano-fluorine carbon cerium CeFCO3Fine suspension 95Kg, 1-hexyl-2,3-methylimidazole
Tetrafluoroborate ionic liquid 5Kg, mixes 40hr in a kettle., obtains product, numbered SX-2.
Embodiment 3
Step 1. nano-fluorine carbon cerium CeFCO3Surface aggregate:
In 500L reactor, add nano-fluorine carbon cerium CeFCO by following proportioning3It is distributed in ethanol, in following ratio
Add acrylic acid trifluoro ethyl ester monomer, benzoyl peroxide and polyvinyl alcohol, dodecylbenzene sodium sulfonate etc., heat up, at 60 DEG C
React 15 hours, i.e. obtain the nano-fluorine carbon cerium CeFCO through surface aggregate3Fine suspension.
Step 2. adds ionic liquid:
In 500L reactor, add nano-fluorine carbon cerium CeFCO3Fine suspension 99Kg, 1-hexyl-2,3-methylimidazole
Tetrafluoroborate ionic liquid 1Kg, mixes 10hr in a kettle., obtains product, numbered SX-3.
Comparative example 1
1-hexyl-2,3-methylimidazole tetrafluoroborate ionic liquid is added without, the other the same as in Example 1.Products obtained therefrom is compiled
Number it is SX-4.
Comparative example 2
Only using 1-hexyl-2,3-methylimidazole tetrafluoroborate ionic liquid one composition is coated with as metal surface silane
Layer corrosion inhibiter.The numbered SX-5 of products obtained therefrom.
Embodiment 4
In the container adding the silane coupled prefilming agent of 100g, obtained by being separately added into embodiment 1-3 and comparative example 1-2
Product 6g, 2000 turns per minute of mixing speed, stir, at surface of aluminum plate film, and carry out electrochemical impedance spectroscopy test.Rp
Being worth the quantitative response decay resistance of film layer, the corrosion resistance of the biggest explanation film is the best.R2For the resistance of coating surface micropore,
The biggest the most completely crued molecule of explanation composite film surface regenerates film at film fault location, and the self-reparing capability of film is the best.
Blank sample is common silane coupled prefilming agent, and the omnipotent Science and Technology Ltd. that reaches in Zhejiang produces.
(by document Cao Chunan, corrosion electrochemistry [M], Beijing: Chemical Industry Press, 1994.Electrochemical impedance spectroscopy is tested
Method measures)
| Production code member | Rp/KΩ | R2/Ω |
| SX-1 | 39021 | 1082 |
| SX-2 | 32050 | 854 |
| SX-3 | 43232 | 1158 |
| SX-4 | 12754 | 378 |
| SX-5 | 228 | 276 |
| Blank sample | 2 | 228 |
Embodiment 5
In the container adding the silane coupled prefilming agent of 100g, obtained by being separately added into embodiment 1-3 and comparative example 1-2
Product 1g, 2200 turns per minute of mixing speed, stir, at surface of aluminum plate film, and carry out electrochemical impedance spectroscopy test.Rp
Being worth the quantitative response decay resistance of film layer, the corrosion resistance of the biggest explanation film is the best.R2For the resistance of coating surface micropore,
The biggest the most completely crued molecule of explanation composite film surface regenerates film at film fault location, and the self-reparing capability of film is the best.
Blank sample is common silane coupled prefilming agent, and the omnipotent Science and Technology Ltd. that reaches in Zhejiang produces.
(by document Cao Chunan, corrosion electrochemistry [M], Beijing: Chemical Industry Press, 1994.Electrochemical impedance spectroscopy is tested
Method measures)
Embodiment 6
In the container adding the silane coupled prefilming agent of 100g, obtained by being separately added into embodiment 1-3 and comparative example 1-2
Product 10g, 2200 turns per minute of mixing speed, stir, at surface of aluminum plate film, and carry out electrochemical impedance spectroscopy test.
RpBeing worth the quantitative response decay resistance of film layer, the corrosion resistance of the biggest explanation film is the best.R2Electricity for coating surface micropore
Resistance, the biggest the most completely crued molecule of explanation composite film surface regenerates film at film fault location, and the self-reparing capability of film is more
Good.Blank sample is common silane coupled prefilming agent, and the omnipotent Science and Technology Ltd. that reaches in Zhejiang produces.
(by document Cao Chunan, corrosion electrochemistry [M], Beijing: Chemical Industry Press, 1994.Electrochemical impedance spectroscopy is tested
Method measures)
| Production code member | Rp/KΩ | R2/Ω |
| SX-1 | 44891 | 1167 |
| SX-2 | 38901 | 980 |
| SX-3 | 48022 | 1219 |
| SX-4 | 21983 | 677 |
| SX-5 | 370 | 332 |
| Blank sample | 2 | 229 |
Claims (1)
1. a metal surface silane coating corrosion inhibiter, it is characterised in that its preparation method comprises the following steps:
Step 1. nano-fluorine carbon cerium CeFCO3Surface aggregate:
By a certain amount of nano-fluorine carbon cerium CeFCO3It is distributed in ethanol, adds acrylic acid trifluoro ethyl ester, peroxidating in following ratio
Benzoyl, polyvinyl alcohol, dodecylbenzene sodium sulfonate, heat up, and reacts 6-15 hour at 60-80 DEG C, i.e. obtains through surface aggregate
Nano-fluorine carbon cerium CeFCO3Fine suspension；
Step 2. adds ionic liquid:
Nano-fluorine carbon cerium CeFCO3Fine suspension and 1-hexyl-2,3-methylimidazole tetrafluoroborate is with mass ratio as 95-99:
The proportioning of 1-5 mixes 10-40 hour in a kettle., obtains product.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4741847A (en) * | 1985-02-19 | 1988-05-03 | Hoechst Aktiengesellschaft | Aqueous anti-corrosion agent containing an ammonium salt of 2-benzthiazolythiocarboxylic acid |
| WO1997012076A1 (en) * | 1995-09-26 | 1997-04-03 | Elf Atochem Societe Anonyme | Metal surface treatments |
| CN1422984A (en) * | 2002-12-16 | 2003-06-11 | 中国石油化工集团公司 | Metal corrosion inhibitor |
| CN102787310A (en) * | 2012-08-27 | 2012-11-21 | 大连工业大学 | Metal surface treatment agent |
-
2014
- 2014-06-26 CN CN201410311848.6A patent/CN104060276B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4741847A (en) * | 1985-02-19 | 1988-05-03 | Hoechst Aktiengesellschaft | Aqueous anti-corrosion agent containing an ammonium salt of 2-benzthiazolythiocarboxylic acid |
| WO1997012076A1 (en) * | 1995-09-26 | 1997-04-03 | Elf Atochem Societe Anonyme | Metal surface treatments |
| CN1422984A (en) * | 2002-12-16 | 2003-06-11 | 中国石油化工集团公司 | Metal corrosion inhibitor |
| CN102787310A (en) * | 2012-08-27 | 2012-11-21 | 大连工业大学 | Metal surface treatment agent |
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