CN102108241B - Phosphate doped polyaniline anticorrosive paint and preparation method thereof - Google Patents
Phosphate doped polyaniline anticorrosive paint and preparation method thereof Download PDFInfo
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- CN102108241B CN102108241B CN201010526285.4A CN201010526285A CN102108241B CN 102108241 B CN102108241 B CN 102108241B CN 201010526285 A CN201010526285 A CN 201010526285A CN 102108241 B CN102108241 B CN 102108241B
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Abstract
The invention provides a phosphate doped polyaniline anticorrosive paint and a preparation method thereof. In the preparation method, polyaniline is well dispersed in an organic solvent on the basis of 'countra-ion induction workability' in the presence of special phosphate used as a doping agent of the polyaniline, so that a good anticorrosive effect can be obtained by adding little conductive polyaniline in the formula of the anticorrosive paint, thereby greatly reducing the cost of polyaniline anticorrosive paint. The anticorrosive paint has strong resistance to corrosion of media (salt mist, acid, alkali and the like) and atmosphere environment, and has good anticorrosive effect on different metals such as steel, copper, aluminum and the like, thereby widening the application range of the anticorrosive paint. The synthesis process is simple with low preparation cost. After a 1000-hour scratch-resistant experiment, the anticorrosive paint can reach the technical indexes of non-propagating rusting and no blister on a board surface, which is twice more than that of the traditional polyaniline anticorrosive paint, thereby solving the defects such as blistering, happening commonly when the traditional polyaniline anticorrosive paint is subjected to scratch-resistant experiment.
Description
Technical field
The present invention relates to a kind of phosphate doped polyaniline anticorrosive paint and preparation method thereof.
Background technology
Metallic corrosion problem spreads all over each department of national economy, every profession and trade, and the national economic development, people's lives and social environment are produced to significant damage.In order to prevent corrosion, a large amount of manpowers, financial resources are all dropped in countries in the world, adopt various means to carry out corrosion prevention.
Polyaniline is one of high-tech novel material having now specific function, and many experimental results proves, polyaniline paint has excellent antiseptic power to metal.Exploitation polyaniline anti-corrosive paint becomes a new focus of coating research field at present.Existing polyaniline anti-corrosive paint mainly contains following two types: (1) electrochemical polymerization forms polyaniline coating, but the method is not suitable for the rotproofing of site operation and large-scale metal parts, therefore applies limited; (2) adopt chemical process synthesized polyaniline as anticorrosive additive, be prepared into composite coating with conventional film-forming resin blend.The method has overcome the deficiency of electrochemical polymerization, is current main research field.
Patent ZL 03121402.9,200810051457.X, 200810051576.5 have reported by polyaniline and epoxy resin, urethane resin, solidifying agent and various additive and have prepared polyaniline anti-corrosive paint.But polyaniline, because its molecular chain has very strong conjugacy, be considered to a kind of insoluble not molten polymkeric substance, and general polymerization thing consistency is poor always; And with traditional anticorrosive additive ratio, polyaniline does not also have advantage in Costco Wholesale.Therefore electrically conductive polyaniline is dispersed or dissolved in resins for universal use and organic solvent, make it add small amount polyaniline can reach desirable preservative effect is the direction that scientist makes great efforts always.Although have been found that at present and adopt some special intensive polar solvents, as N-Methyl pyrrolidone, meta-cresol etc. can make polyaniline, dissolve, these solvents generally exist boiling point higher, and toxic, are therefore difficult to be applied in protective system.
Summary of the invention
The problem existing in order to solve prior art, the present invention adopts the doping agent of a kind of special phosphoric acid ester as polyaniline, utilize " gegenion induction processibility ", polyaniline is well disperseed in organic solvent, thereby make to add the electrically conductive polyaniline of little amount just to obtain good preservative effect in anticorrosion paint formulation, reduced greatly the cost of polyaniline anti-corrosive paint.Adopt epoxy resin and polyaniline anti-corrosive paint system, coating damage resistant experiment 1000h corrosion is not expanded, and plate face is non-foaming.Make it in Practical Project, have wide application.
A kind of phosphate doped polyaniline anticorrosive paint provided by the invention, it is two-component coating, the component of its formula and weight part proportioning are:
A component:
Epoxy resin 120～200;
Phosphate doped polyaniline 10～50;
Pigment 300～500;
Filler 50～160;
Thinner 200～300;
Auxiliary agent 10～30;
B component:
Solidifying agent 60～150;
Described epoxy resin is E51, E44 or E20;
Described pigment is aluminium dihydrogen tripolyphosphate, zinc phosphate and iron mica; Aluminium dihydrogen tripolyphosphate: zinc phosphate: the weight ratio of iron mica is 120～200: 120～200: 60～100;
Described filler is zinc oxide, talcum powder and process white; Talcum powder: zinc oxide: the weight ratio of process white is 20～60: 20～50: 10～50;
Described thinner is dimethylbenzene;
Described auxiliary agent is dispersant B YK163 and flow agent BYK371; Dispersant B YK163: the weight part ratio of flow agent BYK371 is 5～15: 5～15;
Described solidifying agent is solidifying agent NX-2015, solidifying agent NX-2040, solidifying agent NX-2041, solidifying agent NX-2045, solidifying agent ZY-650 or solidifying agent ZY-3115;
Described phosphate doped polyaniline is prepared by the following method: by mol ratio, polyaniline in eigenstate: phosphoric acid ester: water=1: 0.1～0.5: 40～50, phosphoric acid ester and polyaniline in eigenstate are mixed in water and are mixed 2～6 hours, filter, be washed with water to filtrate neutrality, filter cake, in oven for drying, obtains phosphate doped polyaniline; Polyaniline in eigenstate is unadulterated intermediate oxidation state polyaniline.
The structural formula of described polyaniline in eigenstate is:
In formula, 0 < y < 1, n=1～500, R
1, R
2, R
1' and R
2' be H, C
kh
2k+1or OC
kh
2k+1, wherein k=1～20;
Described phosphoric acid ester is any one of following structural formula:
In formula, m=0～20.
The preparation method's of a kind of phosphate doped polyaniline anticorrosive paint provided by the invention step and condition are as follows:
By proportioning take epoxy resin, thinner is put into sand mill tank, under stirring, put into phosphate doped polyaniline powder, stir 0.5～2 hour, under stirring, add respectively again auxiliary agent, pigment and filler, with the speed of 2500 revs/min, stir 0.5～3 hour, sand milling 1～5 hour, with 200 order filter-cloth filterings, obtains A component;
By proportioning, component B and component A are stirred in machine and stirred 3～5 minutes with 1200～1500 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.
A kind of usage of phosphate doped polyaniline anticorrosive paint is as follows: phosphate doped polyaniline anticorrosive paint is sprayed on the surface of the metallic substance of polishing, oil removing, processing of rust removing to self-vulcanizing.
Beneficial effect: the phosphate doped polyaniline anticorrosive paint that the present invention makes has the media such as stronger salt spray resistance, acid, alkali and atmospheric environment corrosion.
The phosphate doped polyaniline anticorrosive paint that the present invention prepares all has good preservative effect for different metal as iron and steel, copper, aluminium etc.
Phosphate doped polyaniline synthesis technique of the present invention is simple, and preparation cost is low.
Phosphate doped polyaniline anticorrosive paint of the present invention has reduced the addition of polyaniline compared with traditional polyaniline anti-corrosive paint, has reduced use cost, has expanded its range of application.
Phosphate doped polyaniline anticorrosive paint of the present invention can reach damage resistant experiment 1000h corrosion and not expand, plate face is non-foaming, reaching such technical indicator is more than 2 times of traditional polyaniline anti-corrosive paint, has solved traditional polyaniline anti-corrosive paint damage resistant and has tested the defects such as easy to foaming.
Embodiment
Comparative example 1: take respectively 240 grams of 100 grams of epoxy resin E51, dimethylbenzene and put into sand mill tank, add respectively 5 grams of dispersant B YK163 under stirring, 150 grams of aluminium dihydrogen tripolyphosphates, 150 grams of zinc phosphates, 100 grams of iron micas, 80 grams of talcum powder, 70 grams, zinc oxide, 50 grams of process whites, flow agent BYK371:5 gram, stirs 2 hours sand milling 3 hours with the speed of 2500 revs/min, with 200 order filter-cloth filterings, obtain A component.
B component is: 50 grams of solidifying agent NX-2015;
Component A and component B are stirred in machine and stirred 5 minutes with 1200 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.Be sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, self-vulcanizing.After solidifying completely, paint film tests its salt mist experiment scratch resistant performance.
Acquired results is in Table 1
Embodiment 1: take respectively 150 grams of epoxy resin E51, 200 grams of dimethylbenzene are put into sand mill tank, under stirring, put into 10 grams, the phosphate doped polyaniline powder prepared for the phosphoric acid ester of (1) by structural formula, stir 2 hours, under stirring, add respectively again 15 grams of dispersant B YK163, 150 grams of aluminium dihydrogen tripolyphosphates, 150 grams of zinc phosphates, 70 grams of iron micas, 60 grams of talcum powder, 50 grams, zinc oxide, 40 grams of process whites, 5 grams of flow agent BYK371, with the speed of 2500 revs/min, stir 1 hour, sand milling 2 hours, with 200 order filter-cloth filterings, obtain A component.
B component is: 100 grams of solidifying agent NX-2040;
Component A and component B are stirred in machine and stirred 5 minutes with 1200 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.
Be sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, self-vulcanizing.After solidifying completely, paint film tests its salt mist experiment scratch resistant performance.Acquired results is in Table 1.
Embodiment 2: take respectively 120 grams of epoxy resin E44, 220 grams of dimethylbenzene are put into sand mill tank, under stirring, put into 20 grams, the phosphate doped polyaniline powder prepared for the phosphoric acid ester of (3) by phosphate ester structure formula, stir 1 hour, under stirring, add respectively again 10 grams of dispersant B YK163, 200 grams of aluminium dihydrogen tripolyphosphates, 200 grams of zinc phosphates, 100 grams of iron micas, 30 grams of talcum powder, 20 grams, zinc oxide, 10 grams of process whites, 10 grams of flow agent BYK371, with the speed of 2500 revs/min, stir 0.5 hour, sand milling 3 hours, with 200 order filter-cloth filterings, obtain A component.
B component is: 60 grams of solidifying agent NX-2041;
Component A and component B are stirred in machine and stirred 3 minutes with 1500 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.
Be sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, self-vulcanizing.After solidifying completely, paint film tests its salt mist experiment scratch resistant performance.Acquired results is in Table 1.
Embodiment 3: take respectively 200 grams of epoxy resin E44, 240 grams of dimethylbenzene are put into sand mill tank, under stirring, put into 30 grams, the phosphate doped polyaniline powder prepared for the phosphoric acid ester of (2) by phosphate ester structure formula, stir 0.5 hour, under stirring, add respectively again 5 grams of dispersant B YK163, 130 grams of aluminium dihydrogen tripolyphosphates, 130 grams of zinc phosphates, 60 grams of iron micas, 20 grams of talcum powder, 20 grams, zinc oxide, 10 grams of process whites, 5 grams of flow agent BYK371, with the speed of 2500 revs/min, stir 3 hours, sand milling 1 hour, with 200 order filter-cloth filterings, obtain A component.
B component is: 150 grams of solidifying agent ZY-650;
Component A and component B are stirred in machine and stirred 4 minutes with 1300 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.
Be sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, self-vulcanizing.After solidifying completely, paint film tests its salt mist experiment scratch resistant performance.Acquired results is in Table 1.
Embodiment 4: take respectively 160 grams of epoxy resin E20, 260 grams of dimethylbenzene are put into sand mill tank, under stirring, put into 40 grams, the phosphate doped polyaniline powder prepared for the phosphoric acid ester of (4) by phosphate ester structure formula, stir 1 hour, under stirring, add respectively again 15 grams of dispersant B YK163, 120 grams of aluminium dihydrogen tripolyphosphates, 120 grams of zinc phosphates, 80 grams of iron micas, 50 grams of talcum powder, 40 grams, zinc oxide, 50 grams of process whites, 15 grams of flow agent BYK371, with the speed of 2500 revs/min, stir 2 hours, sand milling 5 hours, with 200 order filter-cloth filterings, obtain A component.
B component is: 72 grams of solidifying agent NX-2045;
Component A and component B are stirred in machine and stirred 4 minutes with 1200 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.
Be sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, self-vulcanizing.After solidifying completely, paint film tests its salt mist experiment scratch resistant performance.Acquired results is in Table 1.
Embodiment 5: take respectively 140 grams of epoxy resin E20, 300 grams of dimethylbenzene are put into sand mill tank, under stirring, put into 50 grams, the phosphate doped polyaniline powder prepared for the phosphoric acid ester of (5) by phosphate ester structure formula, stir 2 hours, under stirring, add respectively again 10 grams of dispersant B YK163, 150 grams of aluminium dihydrogen tripolyphosphates, 130 grams of zinc phosphates, 70 grams of iron micas, 20 grams of talcum powder, 30 grams, zinc oxide, 30 grams of process whites, 10 grams of flow agent BYK371, with the speed of 2500 revs/min, stir 1 hour, sand milling 2 hours, with 200 order filter-cloth filterings, obtain A component.
B component is: 60 grams of solidifying agent ZY-3115;
Component A and component B are stirred in machine and stirred 5 minutes with 1400 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.
Be sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, self-vulcanizing.After solidifying completely, paint film tests its salt mist experiment scratch resistant performance.Acquired results is in Table 1.
Table 1.
Note: comparative example, embodiment 1-5 solidifying agent NX-2015 used, NX-2040, NX-2041, NX-2045 is the phenolic aldehyde amine curing agent of Ka Delai; ZY-650, ZY-3115 grinds the polyamide-based solidifying agent of science and technology in being.
Claims (8)
1. a phosphate doped polyaniline anticorrosive paint, is characterized in that, it is dual-component coating, and its component and weight part proportioning are:
A component:
Described epoxy resin is E51, E44 or E20;
Described pigment is aluminium dihydrogen tripolyphosphate, zinc phosphate and iron mica; Wherein, aluminium dihydrogen tripolyphosphate: zinc phosphate: the weight ratio of iron mica is 120～200:120～200:60～100;
Described filler is zinc oxide, talcum powder and process white; Wherein, talcum powder: zinc oxide: the weight ratio of process white is 20～60:20～50:10～50;
Described thinner is dimethylbenzene;
Described auxiliary agent is dispersant B YK163 and flow agent BYK371; Wherein, dispersant B YK163: the weight part ratio of flow agent BYK371 is 5～15:5～15;
Described solidifying agent is solidifying agent NX-2015, solidifying agent NX-2040, solidifying agent NX-2041, solidifying agent NX-2045, solidifying agent ZY-650 or solidifying agent ZY-3115;
Described phosphate doped polyaniline is prepared by the following method: by mol ratio, polyaniline in eigenstate: phosphoric acid ester: water=1:0.1～0.5:40～50, phosphoric acid ester and polyaniline in eigenstate are mixed in water and are mixed 2～6 hours, filter, be washed with water to filtrate neutrality, filter cake, in oven for drying, obtains phosphate doped polyaniline; Described polyaniline in eigenstate is unadulterated intermediate oxidation state polyaniline;
The structural formula of described polyaniline in eigenstate is:
In formula, 0 < y < 1, n=1-500, R
1, R
2, R
1' and R
2' be H, C
kh
2k+1or OC
kh
2k+1, wherein k=1-20;
Described phosphoric acid ester is any one of following structural formula:
2. a kind of phosphate doped polyaniline anticorrosive paint as claimed in claim 1, is characterized in that, its component and weight part proportioning are:
A component:
Epoxy resin is 150;
Phosphate doped polyaniline 10;
Pigment is 370, wherein, and aluminium dihydrogen tripolyphosphate: zinc phosphate: iron mica is 150:150:70;
Filler is 150, wherein, and talcum powder: zinc oxide: process white is 60:50:40;
Thinner is 200;
Auxiliary agent is 20; Wherein, dispersant B YK163: flow agent BYK371 is 15:5;
B component: solidifying agent is 100.
3. a kind of phosphate doped polyaniline anticorrosive paint as claimed in claim 1, is characterized in that, its component and weight part proportioning are:
A component:
Epoxy resin is 120;
Phosphate doped polyaniline 20;
Pigment is 500, wherein, and aluminium dihydrogen tripolyphosphate: zinc phosphate: iron mica is 200:200:100;
Filler is 60, wherein, and talcum powder: zinc oxide: process white is 30:20:10;
Thinner is 220;
Auxiliary agent is 20, wherein, and dispersant B YK163: flow agent BYK371 is 10:10;
B component: solidifying agent is 60.
4. a kind of phosphate doped polyaniline anticorrosive paint as claimed in claim 1, is characterized in that, its component and weight part proportioning are:
A component:
Epoxy resin is 200;
Phosphate doped polyaniline is 30:
Pigment is 320, wherein, and aluminium dihydrogen tripolyphosphate: zinc phosphate: iron mica is 130:130:60;
Filler is 50, wherein, and talcum powder: zinc oxide: process white is 20:20:10;
Thinner is 240;
Auxiliary agent dispersion agent is 10, dispersant B YK163: flow agent BYK371 is 5:5;
B component: solidifying agent is 150.
5. a kind of phosphate doped polyaniline anticorrosive paint as claimed in claim 1, is characterized in that, its component and weight part proportioning are:
A component:
Epoxy resin is 200;
Phosphate doped polyaniline is 30;
Pigment is 320, wherein, and aluminium dihydrogen tripolyphosphate: zinc phosphate: iron mica is 130:130:60;
Filler is 50, wherein, and talcum powder: zinc oxide: process white is 20:20:10;
Thinner is 240;
Auxiliary agent is 10, wherein, and dispersant B YK163: flow agent BYK371 is 5:5;
B component: solidifying agent is 150.
6. a kind of phosphate doped polyaniline anticorrosive paint as claimed in claim 1, is characterized in that, its component and weight part proportioning are:
A component:
Epoxy resin is 160;
Phosphate doped polyaniline is 40;
Pigment is 320, wherein, and aluminium dihydrogen tripolyphosphate: zinc phosphate: iron mica is 120:120:80;
Filler is 140, wherein, and talcum powder: zinc oxide: process white is 50:40:50;
Thinner is 260;
Auxiliary agent is 30, wherein, and dispersant B YK163: flow agent BYK371 is 15:15;
B component: solidifying agent is 72.
7. a kind of phosphate doped polyaniline anticorrosive paint as claimed in claim 1, is characterized in that, its component and weight part proportioning are:
A component:
Epoxy resin is 140;
Phosphate doped polyaniline is 50;
Pigment is 350, wherein, and aluminium dihydrogen tripolyphosphate: zinc phosphate: iron mica is 150:130:70:
Filler is 80, wherein, and talcum powder: zinc oxide: process white is 20:30:30;
Thinner is 300;
Auxiliary agent is 20, wherein, and dispersant B YK163: flow agent BYK371 is 10:10;
B component: solidifying agent is 60.
8. the method for making of a kind of phosphate doped polyaniline anticorrosive paint as claimed in claim 1, is characterized in that step is as follows:
By proportioning take epoxy resin, thinner is put into sand mill tank, under stirring, put into phosphate doped polyaniline powder, stir 0.5～2 hour, under stirring, add respectively again auxiliary agent, pigment and filler, with the speed of 2500 revs/min, stir 0.5～3 hour, sand milling 1～5 hour, with 200 order filter-cloth filterings, obtains component A;
By proportioning, component B and component A are stirred in machine and stirred 3～5 minutes with 1200～1500 revs/min at height, obtain phosphate doped polyaniline anticorrosive paint.
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| CN103834265B (en) * | 2014-03-24 | 2015-12-09 | 中国科学院长春应用化学研究所 | A kind of polyaniline anti-corrosive paint |
| CN104845492A (en) * | 2015-05-13 | 2015-08-19 | 贵州师范学院 | Sulfuric acid/aluminum triphosphate doped poly-o-toluidine anticorrosive coating |
| CN105176378A (en) * | 2015-10-21 | 2015-12-23 | 苏州赛斯德工程设备有限公司 | Waterborne polyaniline anticorrosive static-conductive coating and preparation method thereof |
| CN107163835A (en) * | 2017-06-15 | 2017-09-15 | 苏州莱特复合材料有限公司 | A kind of preparation method of metal fire resistant anticorrosive paint |
| CN117567018B (en) * | 2024-01-16 | 2024-03-15 | 山东民烨耐火纤维有限公司 | Preparation method of ceramic fiber antistatic heat insulation plate |
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| CN1215744A (en) * | 1997-10-25 | 1999-05-05 | 中国科学院长春应用化学研究所 | Method for preparing conductive antifouling corrosion-resistant poly-aniline paint |
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