CN1401718A - Process for preparing corrosion-resistant polyaniline paint - Google Patents
Process for preparing corrosion-resistant polyaniline paint Download PDFInfo
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- CN1401718A CN1401718A CN 02139434 CN02139434A CN1401718A CN 1401718 A CN1401718 A CN 1401718A CN 02139434 CN02139434 CN 02139434 CN 02139434 A CN02139434 A CN 02139434A CN 1401718 A CN1401718 A CN 1401718A
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Abstract
An anticorrosion polyphenylamine paint is prepared through surface treatment of conventional filler, e.g. SiO2, TiO2, alumina, etc, in-situ polymerization on the surface of filler particles to form PANI, and uniformly mixing with epoxy resin, solvent, defoaming agent and plasticizer. Its advantages are high hardness, high antiwear and anticorrosion effect and low cost.
Description
One, technical field
The present invention relates to a kind of protective system, particularly a kind of preparation technology of polyaniline anti-corrosive paint.
Two, background technology
Metallic corrosion brings tremendous loss to national economy, and it destroys example and spreads all over the occasion that all use metal.According to statistics, annual hardware and the material of scrapping owing to corrosion is equivalent to 1/3 of metal output, and be extremely huge to the waste of natural resources.In order to prevent and to slow down corrosion of metal, people adopt organic coating and the zinciferous organic or inorganic coating that applies inhibiter such as containing heavy metal such as chromium, lead, molybdenum more.Though these class methods are effective relatively, and are huge to environmental hazard, in case and coating have slightly and to scratch, its preservative effect will be had a greatly reduced quality.Therefore, people are also in the better anticorrosion approach of expectation.Recently the relative traditional coating of the polyaniline anti-corrosive paint of Chu Xianing is a huge advance made, polyaniline (PANI) has good antiseptic property to metal, but remain in practicability at certain obstacle: 1. the PANI solvability is very poor, PANI is except at some intensive polar solvents such as N-Methyl pyrrolidone (NMP), N, dissolving hardly in ordinary organic solvents is arranged outside certain solvability in the dinethylformamide (DMF) etc.; 2. the easy dedoping of the PANI of conductive state has limited its application in some resin; 3. cost an arm and a leg, availability is low.In corrosion-resistant field, the main path of preparation PANI corrosion protection coating has following three kinds.1. apply the solution of PANI, make solvent evaporates form the PANI coating.This method gained coating machine poor performance, and be subjected to the deliquescent restriction of PANI and be difficult for widespread use.2. PANI solution and conventional resins are compounded to form coating.As German Ormecon company is exactly by improving the solubleness of PANI, and makes the PANI protective system; The somebody is dissolved in PANI in the aliphatic polyamine, mix with auxiliary agent then, directly obtained polyaniline anti-corrosive paint through means such as stirring, grindings, but the solvability of polyaniline in polyamine is limited, most of polyaniline is filtered as insolubles, has only a spot of soluble part to be utilized, and the price of polyaniline is very high in addition, so this method is very uneconomical.
Three, summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, the polyaniline anti-corrosive paint that provide a kind of cheap, nontoxicity, can conveniently use.
The technical solution used in the present invention is in order to achieve the above object:
(1) preparation of anticorrosive polyaniline agent
1) 0.1～10 part coupling agent being joined 80～120 parts of concentration is in 5～50% the acidic solution, to stir, again to the organic or inorganic filler powder that wherein adds 1～100 part, mechanical stirring 1～20h, filter, dry under 30～120 ℃, finish surface preparation to powder material;
2) under 0～30 ℃, while stirring 8～11 parts of monomers, 10～1000 parts of above-mentioned treated fillers are added successively in 900～1300 parts the acidic solution;
3) under mechanical stirring at the uniform velocity, add 100～1000 parts of concentration gradually and be the acidic solution of 5～20% oxygenant, add the back and continue reaction 0.5～10h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 1～10wt% is handled 0.5～10h to above-mentioned dried material, and it is 7～10 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the inorganic of surface coverage polyaniline in eigenstate or organic anti-corrosive agent;
(2) preparation of protective system
1) get 10～20 parts of Resins, epoxy and mix, add 0.1～2.0 part of defoamer with 10～50 parts of organic solvents, 1～40 part softening agent, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 20～60 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 0.5～2h, filter, promptly get the A component of polyaniline anti-corrosive paint;
3) get 20～60 parts of low molecular polyamides and 40～80 parts of phenolic aldehyde amine mixing, make solidifying agent, promptly get the B component;
4) the A component of polyaniline anti-corrosive paint and B component are got final product by 10～30: 1 mixed.
Because it is inhibiter that the present invention adopts the PANI that does not contain heavy metal, form PANI by chemical oxidising polymerisation in common organic or inorganic filling surface original position, this filler that is covered by polyaniline can have been given play to the effect of pure PANI particulate.Because the content of PANI is very low in this filler, building-up process is simple and needn't dissolve direct application, and is therefore easy to use and cost is extremely cheap.
Five, embodiment
Embodiment 1,
(1) preparation of anticorrosive polyaniline agent
1) 1 part coupling agent KH-550 being joined 100 parts concentration is in 25% the hydrochloric acid soln, to stir, and to wherein adding 80 parts of titanium oxide powders, mechanical stirring 10h filters again, 40 ℃ dry down, finish surface preparation to powder material;
2) under 20 ℃, while stirring 10 parts of monomers, 700 parts of treated fillers are added successively 1000 parts of concentration and are in 25% the sulphuric acid soln, the monomer structure formula:
R is C
nH
2n+1, perhaps C
nH
2n+1O, n is between 0 and 10;
3) under mechanical stirring at the uniform velocity, add 400 parts of concentration gradually and be 8% potassium bichromate acidic solution, add the back and continue reaction 8h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 6wt% is handled 7h to above-mentioned dried material, and it is 8.5 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the inorganic corrosion inhibitor of surface coverage polyaniline in eigenstate;
(2) preparation of coating
1) get 18 parts of bisphenol A type epoxy resin E-51 and mix, add 0.6 part fatty acid alkyl ester with 21 parts of dimethylbenzene, 6 parts dibutyl phthalate, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 54.4 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 1.5h, filter, promptly get polyaniline anti-corrosive paint A component;
3) get 40 parts of low molecular polyamides and 70 parts of mixed solidifying agent, i.e. B components of getting of phenolic aldehyde amine;
4) mixed that the A component and the B component of polyaniline anti-corrosive paint are pressed 15: 1 is coated on the treated good steel plate, and control thickness is at 20～300 μ m, and curing gets final product under the room temperature.
Embodiment 2,
(1) preparation of anticorrosive polyaniline agent
1) with 0.1 part coupling agent KH-560, the concentration that joins 80 parts is in 15% the sulphuric acid soln, to stir, and to wherein adding 100 parts of cilicon oxide filler powder, mechanical stirring 6h filters again, 120 ℃ dry down, finish surface preparation to powder material;
2) under 0 ℃, the concentration that while stirring 10.5 parts of monomers, 1000 parts of above-mentioned treated fillers is added successively 1200 parts is in 8% the hydrochloric acid soln;
3) under mechanical stirring at the uniform velocity, add 830 parts of concentration gradually and be 5% potassium permanganate solution, add the back and continue reaction 10h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 4wt% is handled 3.2h to above-mentioned dried material, and it is 9 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the inorganic corrosion inhibitor of surface coverage polyaniline in eigenstate;
(2) preparation of coating
1) get 13 parts of bisphenol A type epoxy resin E-44 and mix, add 0.3 part ethylene oxide oligopolymer with 50 parts of dimethylbenzene, 40 parts dioctyl phthalate (DOP), mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 50 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 1.8h, filter, promptly get polyaniline anti-corrosive paint A component;
3) get 30 parts of low molecular polyamides and 80 parts of mixed solidifying agent, i.e. B components of getting of phenolic aldehyde amine;
4) mixed that the A component and the B component of polyaniline anti-corrosive paint are pressed 20: 1 is coated on the treated good steel plate, and control thickness is at 20～300 μ m, and curing gets final product under the room temperature.
Embodiment 3,
(1) preparation of anticorrosive polyaniline agent
1) with 5 parts coupling agent KH-560, join 90 parts of concentration and be in 19% the acetic acid solution, stir, to wherein adding 70 parts of montmorillonite filler powder, mechanical stirring 17h filters again, 50 ℃ dry down, finish surface preparation to powder material;
2) under 25 ℃, the concentration that while stirring 8 parts of monomers, 600 parts of above-mentioned treated fillers is added successively 1100 parts is in 20% the sulphuric acid soln;
3) under mechanical stirring at the uniform velocity, add 100 parts of concentration gradually and be 17% FeCl
3In the solution, add the back and continue reaction 0.5h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 3wt% is handled 10h to above-mentioned dried material, and it is 8 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the inorganic corrosion inhibitor of surface coverage polyaniline in eigenstate;
(2) preparation of coating
1) get 15 parts of bisphenol A type epoxy resin E-35 and mix with 10 parts of hexones, add 0.1 part methyl-silicone oil, 1 part tritolyl phosphate, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 60 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 0.5h, filter, promptly get polyaniline anti-corrosive paint A component;
3) get 40 parts of low molecular polyamides and 40 parts of mixed solidifying agent, i.e. B components of getting of phenolic aldehyde amine;
4) mixed that the A component and the B component of polyaniline anti-corrosive paint are pressed 13: 1 is coated on the treated good steel plate, and control thickness is at 20～300 μ m, and curing gets final product under the room temperature.
Embodiment 4,
(1) preparation of anticorrosive polyaniline agent
1) with 8 parts coupling agent KH-550, the concentration that joins 110 parts is in 50% the acetic acid solution, to stir, again to wherein add 50 parts alumina powder jointed, mechanical stirring 1h filters, 80 ℃ dry down, finish surface preparation to powder material;
2) under 16 ℃, the concentration that while stirring 9.2 parts of monomers, 300 parts of above-mentioned treated fillers is added successively 950 parts is in 31% the tosic acid solution;
3) under mechanical stirring at the uniform velocity, add 650 parts of concentration gradually and be in 10% the ammonium persulfate solution, add the back and continue reaction 3h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 8wt% is handled 0.5h to above-mentioned dried material, and it is 8 that the ammonia vol of adding makes the pH value of treatment solution, and to neutral, drying obtains the inorganic corrosion inhibitor of surface coverage polyaniline in eigenstate through rate, washing;
(2) preparation of coating
1) get 10 parts of bisphenol A type epoxy resin E-20 and mix, add 1.0 parts fatty acid alkyl ester with 19 parts of organic solvent hexones, 19 parts tritolyl phosphate, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 20 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 0.7h, filter, promptly get polyaniline anti-corrosive paint A component;
3) get 50 parts of low molecular polyamides and 60 parts of mixed solidifying agent, i.e. B components of getting of phenolic aldehyde amine;
4) mixed that the A component and the B component of polyaniline anti-corrosive paint are pressed 10: 1 is coated on the treated good steel plate, and control thickness is at 20～300 μ m, and curing gets final product under the room temperature.
Embodiment 5,
(1) preparation of anticorrosive polyaniline agent
1) 6 parts coupling agent KH-560 being joined 120 parts concentration is in 6% the hydrochloric acid soln, to stir, and to wherein adding 100 parts of polyvinyl chloride powders, mechanical stirring 20h filters again, 50 ℃ dry down, finish surface preparation to powder material;
2) under 3 ℃, the concentration that while stirring 8.5 parts of monomers, 98 parts of above-mentioned treated fillers is joined successively 1300 parts is in 50% the tosic acid acidic solution;
3) under mechanical stirring at the uniform velocity, add 360 parts of concentration gradually and be in 20% the potassium permanganate acidic solution, add the back and continue reaction 7h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 3wt% is handled 5h to above-mentioned dried material, and it is 9 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the organic anti-corrosive agent of surface coverage polyaniline in eigenstate;
(2) preparation of coating
1) get 20 parts of bisphenol A type epoxy resin E-51 and mix, add 2.0 parts ethylene oxide oligopolymer with 30 parts of pimelinketone, 25 parts dibutyl phthalate, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 33 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 1.0h, filter, promptly get polyaniline anti-corrosive paint A component;
3) get 60 parts of low molecular polyamides and 70 parts of mixed solidifying agent, i.e. B components of getting of phenolic aldehyde amine;
4) mixed that the A component and the B component of polyaniline anti-corrosive paint are pressed 25: 1 is coated on the treated good steel plate, and control thickness is at 20～300 μ m, and curing gets final product under the room temperature.
Embodiment 6,
(1) preparation of anticorrosive polyaniline agent
1) with 10 parts coupling agent KH-550, the concentration that joins 105 parts is in 35% the sulphuric acid soln, to stir, and to wherein adding 100 parts of titanium oxide powders, mechanical stirring 13h filters again, 65 ℃ dry down, finish surface preparation to powder material;
2) under 10 ℃ temperature, the concentration that while stirring 11 parts of monomers, 10 parts of above-mentioned treated fillers is joined successively 900 parts is in 16% the tosic acid acidic solution;
3) under mechanical stirring at the uniform velocity, add 1000 parts of concentration gradually and be in 12% the ammonium persulphate acidic solution, add the back and continue reaction 6h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 10wt% is handled 1h to above-mentioned dried material, and it is 8 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the organic anti-corrosive agent of surface coverage polyaniline in eigenstate;
(2) preparation of coating
1) get 17 parts of bisphenol A type epoxy resin E-35 and mix, add 1.6 parts methyl-silicone oil with 40 parts of dimethylbenzene, 37 parts tritolyl phosphate, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 46 parts of anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 2h, filter, promptly get polyaniline anti-corrosive paint A component;
3) get 40 parts of low molecular polyamides and 60 parts of mixed solidifying agent, i.e. B components of getting of phenolic aldehyde amine;
4) mixed that the A component and the B component of polyaniline anti-corrosive paint are pressed 18: 1 is coated on the treated good steel plate, and control thickness is at 20～300 μ m, and curing gets final product under the room temperature.
Claims (10)
1, a kind of preparation technology of polyaniline anti-corrosive paint is characterized in that:
(1) preparation of anticorrosive polyaniline agent
1) 0.1～10 part coupling agent being joined 80～120 parts of concentration is in 5～50% the acidic solution, to stir, again to the organic or inorganic filler powder that wherein adds 1～100 part, mechanical stirring 1～20h, filter, dry under 30～120 ℃, finish surface preparation to powder material;
2) under 0～30 ℃, while stirring 8～11 parts of monomers, 10～1000 parts of above-mentioned treated fillers are added successively in 900～1300 parts the acidic solution;
3) under mechanical stirring at the uniform velocity, add 100～1000 parts of concentration gradually and be the acidic solution of 5～20% oxygenant, add the back and continue reaction 0.5～10h, filtration, washing, drying;
4) to place concentration be that the ammoniacal liquor of 1～10wt% is handled 0.5～10h to above-mentioned dried material, and it is 7～10 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the inorganic of surface coverage polyaniline in eigenstate or organic anti-corrosive agent;
(2) preparation of protective system
1) get 10～20 parts of Resins, epoxy and mix, add 0.1～2.0 part of defoamer with 10～50 parts of organic solvents, 1～40 part softening agent, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s;
2) get 20～60 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 0.5～2h, filter, promptly get the A component of polyaniline anti-corrosive paint;
3) get 20～60 parts of low molecular polyamides and 40～80 parts of phenolic aldehyde amine mixing, make solidifying agent, promptly get the B component;
4) the A component of polyaniline anti-corrosive paint and B component are got final product by 10～30: 1 mixed.
2, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said coupling agent is KH-550 or KH-560 in the preparation of anticorrosive polyaniline agent.
3, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said acidic solution is hydrochloric acid, sulfuric acid, acetate or tosic acid in the preparation of anticorrosive polyaniline agent.
4, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said filler is that diameter is titanium oxide, silicon oxide, montmorillonite, aluminum oxide or the polyvinyl chloride of 10nm～100 μ m in the preparation of anticorrosive polyaniline agent.
5, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said oxygenant is potassium bichromate, potassium permanganate, FeCl in the preparation of anticorrosive polyaniline agent
3Or ammonium persulphate.
6, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said Resins, epoxy is E-51 in the preparation of the A of protective system component, E-44, E-35, the bisphenol A type epoxy resin of different molecular weights such as E-20.
7, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said organic solvent is hexone, pimelinketone or dimethylbenzene in the preparation of the A of protective system component.
8, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said defoamer is fatty acid alkyl ester, ethylene oxide oligopolymer or methyl-silicone oil in the preparation of the A of protective system component.
9, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that: said softening agent is dibutyl phthalate, dioctyl phthalate (DOP) or tritolyl phosphate in the preparation of the A of protective system component.
10, the preparation technology of polyaniline anti-corrosive paint according to claim 1 is characterized in that:
Said in the preparation of anticorrosive polyaniline agent: it is in 25% the acidic solution that 1 part coupling agent is joined 100 parts concentration, stirs, again to the organic or inorganic powder that wherein adds 80 parts, mechanical stirring 10h, filter, dry under 40 ℃, finish surface preparation to powder material; Under 20 ℃, the concentration that while stirring 10 parts of monomers, 700 parts of treated powdered materials is added successively 1000 parts is in 25% the acidic solution; Under mechanical stirring at the uniform velocity, add 400 parts of concentration gradually and be the acidic solution of 8% oxygenant, add the back and continue reaction 8h, filtration, washing, drying; It is that the ammoniacal liquor of 6wt% is handled 7h that above-mentioned dried material places concentration, and it is 9.0 that the ammonia vol of adding makes the pH value of treatment solution, and after filtration, washing is to neutral, drying obtains the inorganic of surface coverage polyaniline in eigenstate or organic anti-corrosive agent;
Said in the preparation of the A of protective system component: get 19 parts of Resins, epoxy and mix, add 0.6 part of defoamer with 21 parts of organic solvents, 1 part of softening agent, mechanical stirring is even, obtains the resin system that a viscosity is 10～40s; Get 58.4 parts anticorrosive polyaniline agent, add in the above resin system, in ball mill, disperse 1.5h, filter;
Said in the preparation of the B of protective system component: as to get 40 parts of low molecular polyamides and 60 parts of phenolic aldehyde amine mixing, make solidifying agent, promptly get the B component; The mixed that the A component and the B component of polyaniline anti-corrosive paint were pressed 20: 1 gets final product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021394342A CN1182213C (en) | 2002-09-20 | 2002-09-20 | Process for preparing corrosion-resistant polyaniline paint |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021394342A CN1182213C (en) | 2002-09-20 | 2002-09-20 | Process for preparing corrosion-resistant polyaniline paint |
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| CN1182213C CN1182213C (en) | 2004-12-29 |
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Application publication date: 20030312 Assignee: Hangzhou Yiwei Coating Chemistry Co., Ltd. Assignor: Xi'an Jiaotong University Contract record no.: 2010330000200 Denomination of invention: Process for prparing polyaniline corrosion-resistant paint Granted publication date: 20041229 License type: Exclusive License Record date: 20100303 |
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