CN102108241A - 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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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 phosphoric acid ester doped polyaniline protective system and preparation method thereof.
Background technology
The metallic corrosion problem spreads all over national economy all departments, every profession and trade, and the national economic development, people's lives and social environment are produced significant damage.In order to prevent corrosion, great amount of manpower, 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 that has now specific function, and a large amount of test-results prove that polyaniline paint has excellent antiseptic power to metal.The 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 this method is not suitable for the rotproofing of site operation and large-scale metal parts, therefore uses limited; (2) adopt the chemical process synthesized polyaniline as anticorrosive additive, be prepared into composite coating with film-forming resin blend commonly used.This method has overcome the deficiency of electrochemical polymerization, is present main research field.
Patent ZL 03121402.9,200810051457.X, 200810051576.5 have reported by polyaniline and Resins, epoxy, urethane resin, solidifying agent and various additive preparation polyaniline anti-corrosive paint.Yet polyaniline has very strong conjugacy because of its molecular chain, and to be considered to a kind of insoluble infusible polymkeric substance and general polymerization thing consistency relatively poor always; And with traditional anticorrosive additive ratio, polyaniline does not also have advantage on Costco Wholesale.Therefore electrically conductive polyaniline is dispersed or dissolved in resins for universal use and organic solvent, make a small amount of polyaniline of its adding can reach the ideal preservative effect is the direction that scientist makes great efforts always.Though have been found that at present and adopt some special intensive polar solvents, can make the polyaniline dissolving as N-Methyl pyrrolidone, meta-cresol etc., these solvents generally exist boiling point higher, and toxic, therefore are difficult in the protective system to be applied.
Summary of the invention
In order to solve the problem that prior art exists, the present invention adopts the doping agent of a kind of special phosphoric acid ester as polyaniline, utilize " gegenion is induced processibility ", polyaniline is well disperseed in organic solvent, the very a spot of electrically conductive polyaniline of adding just obtains good preservative effect in anticorrosion paint formulation thereby make, and has reduced the cost of polyaniline anti-corrosive paint greatly.Adopt Resins, epoxy and polyaniline anti-corrosive paint system, coating damage resistant experiment 1000h corrosion is not expanded, and the plate face is non-foaming.Make it that wide application be arranged in actual engineering.
A kind of phosphoric acid ester doped polyaniline protective system provided by the invention, it is a two-component coating, the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy 120～200;
Phosphoric acid ester doped polyaniline 10～50;
Pigment 300～500;
Filler 50～160;
Thinner 200～300;
Auxiliary agent 10～30;
The B component:
Solidifying agent 60～150;
Described Resins, epoxy 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 a 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 phosphoric acid ester doped polyaniline is prepared by following method: press the mol ratio, polyaniline in eigenstate: phosphoric acid ester: water=1: 0.1～0.5: 40～50, phosphoric acid ester and polyaniline in eigenstate be mixed in mix 2～6 hours in the water, filter, be washed with water to filtrate neutrality, filter cake obtains the phosphoric acid ester doped polyaniline in oven for drying; Polyaniline in eigenstate is unadulterated intermediate oxidation attitude polyaniline.
The structural formula of described polyaniline in eigenstate is:
In the 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, k=1～20 wherein;
Described phosphoric acid ester is any one of following structural formula:
In the formula, m=0～20.
The preparation method's of a kind of phosphoric acid ester doped polyaniline protective system provided by the invention step and condition are as follows:
By proportioning take by weighing Resins, epoxy, thinner is put into the sand mill jar, put into phosphoric acid ester doped polyaniline powder under stirring, stirred 0.5～2 hour, stir and add auxiliary agent, pigment and filler down more respectively, stirred 0.5～3 hour with 2500 rev/mins speed, sand milling 1～5 hour filters with 200 order filter clothes, obtains the A component;
By proportioning component B and component A are stirred in the machine at height and to stir 3～5 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1200～1500 rev/mins.
A kind of usage of phosphoric acid ester doped polyaniline protective system is as follows: phosphoric acid ester doped polyaniline protective system is sprayed on the surface of the metallic substance of polishing, oil removing, processing of rust removing, and self-vulcanizing gets final product.
Beneficial effect: the phosphoric acid ester doped polyaniline protective system that the present invention makes has medium and atmospheric environment corrosion such as stronger salt spray resistance, acid, alkali.
The phosphoric acid ester doped polyaniline protective system that the present invention prepares all has good preservative effect for different metal such as iron and steel, copper, aluminium etc.
Phosphoric acid ester doped polyaniline synthesis technique of the present invention is simple, and preparation cost is low.
Phosphoric acid ester doped polyaniline protective system of the present invention is compared the addition that has reduced polyaniline with traditional polyaniline anti-corrosive paint, has reduced use cost, has enlarged its range of application.
Phosphoric acid ester doped polyaniline protective system of the present invention can reach damage resistant experiment 1000h corrosion and not expand, the plate face is non-foaming, reaching such technical indicator is more than 2 times of traditional polyaniline anti-corrosive paint, has solved defectives such as the easy foaming of traditional polyaniline anti-corrosive paint damage resistant experiment.
Embodiment
Comparative Examples 1: take by weighing 100 gram Resins, epoxy E51 respectively, dimethylbenzene 240 grams are put into the sand mill jar, stir to add 5 gram dispersant B YK163, aluminium dihydrogen tripolyphosphate 150 grams down respectively, zinc phosphate 150 grams, iron mica 100 grams, talcum powder 80 grams, zinc oxide 70 grams, process white 50 grams, flow agent BYK371:5 gram stirred 2 hours sand milling 3 hours with 2500 rev/mins speed, filter with 200 order filter clothes, obtain the A component.
The B component is: 50 gram solidifying agent NX-2015;
Component A and component B stirred in the machine at height stirred 5 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1200 rev/mins.It is sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, and self-vulcanizing gets final product.Treat to test its salt mist experiment scratch resistant performance after the paint film completely solidified.
Gained the results are shown in Table 1
Embodiment 1: take by weighing 150 gram Resins, epoxy E51 respectively, dimethylbenzene 200 grams are put into the sand mill jar, stir down, put into by phosphoric acid ester doped polyaniline powder 10 grams of structural formula for the phosphoric acid ester preparation of (1), stirred 2 hours, stir down, add 15 gram dispersant B YK163 more respectively, aluminium dihydrogen tripolyphosphate 150 grams, zinc phosphate 150 grams, iron mica 70 grams, talcum powder 60 grams, zinc oxide 50 grams, process white 40 grams, 5 gram flow agent BYK371 stirred 1 hour sand milling 2 hours with 2500 rev/mins speed, filter with 200 order filter clothes, obtain the A component.
The B component is: 100 gram solidifying agent NX-2040;
Component A and component B stirred in the machine at height stirred 5 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1200 rev/mins.
It is sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, and self-vulcanizing gets final product.Treat to test its salt mist experiment scratch resistant performance after the paint film completely solidified.Gained the results are shown in Table 1.
Embodiment 2: take by weighing 120 gram Resins, epoxy E44 respectively, dimethylbenzene 220 grams are put into the sand mill jar, stir down, put into by phosphoric acid ester doped polyaniline powder 20 grams of phosphate ester structure formula for the phosphoric acid ester preparation of (3), stirred 1 hour, stir and add 10 gram dispersant B YK163 down more respectively, aluminium dihydrogen tripolyphosphate 200 grams, zinc phosphate 200 grams, iron mica 100 grams, talcum powder 30 grams, zinc oxide 20 grams, process white 10 grams, 10 gram flow agent BYK371, stirred 0.5 hour with 2500 rev/mins speed, sand milling 3 hours filters with 200 order filter clothes, obtains the A component.
The B component is: 60 gram solidifying agent NX-2041;
Component A and component B stirred in the machine at height stirred 3 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1500 rev/mins.
It is sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, and self-vulcanizing gets final product.Treat to test its salt mist experiment scratch resistant performance after the paint film completely solidified.Gained the results are shown in Table 1.
Embodiment 3: take by weighing 200 gram Resins, epoxy E44 respectively, dimethylbenzene 240 grams are put into the sand mill jar, stir down, put into by phosphoric acid ester doped polyaniline powder 30 grams of phosphate ester structure formula for the phosphoric acid ester preparation of (2), stirred 0.5 hour, stir and add 5 gram dispersant B YK163 down more respectively, aluminium dihydrogen tripolyphosphate 130 grams, zinc phosphate 130 grams, iron mica 60 grams, talcum powder 20 grams, zinc oxide 20 grams, process white 10 grams, 5 gram flow agent BYK371, stirred 3 hours with 2500 rev/mins speed, sand milling 1 hour filters with 200 order filter clothes, obtains the A component.
The B component is: 150 gram solidifying agent ZY-650;
Component A and component B stirred in the machine at height stirred 4 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1300 rev/mins.
It is sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, and self-vulcanizing gets final product.Treat to test its salt mist experiment scratch resistant performance after the paint film completely solidified.Gained the results are shown in Table 1.
Embodiment 4: take by weighing 160 gram Resins, epoxy E20 respectively, dimethylbenzene 260 grams are put into the sand mill jar, stir down, put into by phosphoric acid ester doped polyaniline powder 40 grams of phosphate ester structure formula for the phosphoric acid ester preparation of (4), stirred 1 hour, stir and add 15 gram dispersant B YK163 down more respectively, aluminium dihydrogen tripolyphosphate 120 grams, zinc phosphate 120 grams, iron mica 80 grams, talcum powder 50 grams, zinc oxide 40 grams, process white 50 grams, 15 gram flow agent BYK371, stirred 2 hours with 2500 rev/mins speed, sand milling 5 hours filters with 200 order filter clothes, obtains the A component.
The B component is: 72 gram solidifying agent NX-2045;
Component A and component B stirred in the machine at height stirred 4 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1200 rev/mins.
It is sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, and self-vulcanizing gets final product.Treat to test its salt mist experiment scratch resistant performance after the paint film completely solidified.Gained the results are shown in Table 1.
Embodiment 5: take by weighing 140 gram Resins, epoxy E20 respectively, dimethylbenzene 300 grams are put into the sand mill jar, stir down, put into by phosphoric acid ester doped polyaniline powder 50 grams of phosphate ester structure formula for the phosphoric acid ester preparation of (5), stirred 2 hours, stir and add 10 gram dispersant B YK163 down more respectively, aluminium dihydrogen tripolyphosphate 150 grams, zinc phosphate 130 grams, iron mica 70 grams, talcum powder 20 grams, zinc oxide 30 grams, process white 30 grams, 10 gram flow agent BYK371, stirred 1 hour with 2500 rev/mins speed, sand milling 2 hours filters with 200 order filter clothes, obtains the A component.
The B component is: 60 gram solidifying agent ZY-3115;
Component A and component B stirred in the machine at height stirred 5 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1400 rev/mins.
It is sprayed on through the surface of the steel of polishing, oil removing, processing of rust removing, and self-vulcanizing gets final product.Treat to test its salt mist experiment scratch resistant performance after the paint film completely solidified.Gained the results are shown in Table 1.
Table 1.
Annotate: Comparative Examples, the used solidifying agent NX-2015 of embodiment 1-5, NX-2040, NX-2041, NX-2045 are the phenolic aldehyde amine curing agent of Ka Delai; ZY-650, ZY-3115 grind scientific and technological polyamide-based solidifying agent in being.
Claims (8)
1. a phosphoric acid ester doped polyaniline protective system is characterized in that, it is a two-component coating, and the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy is 120～200;
The phosphoric acid ester doped polyaniline is 10～50;
Pigment is 300～500;
Filler is 50～160;
Thinner is 200～300;
Auxiliary agent is 10～30;
The B component: solidifying agent is 60～150;
Described Resins, epoxy 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 a 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 phosphoric acid ester doped polyaniline is prepared by following method: press the mol ratio, polyaniline in eigenstate: phosphoric acid ester: water=1: 0.1～0.5: 40～50, phosphoric acid ester and polyaniline in eigenstate be mixed in mix 2～6 hours in the water, filter, be washed with water to filtrate neutrality, filter cake obtains the phosphoric acid ester doped polyaniline in oven for drying; Described polyaniline in eigenstate is unadulterated intermediate oxidation attitude polyaniline;
The structural formula of described polyaniline in eigenstate is:
In the 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, k=1～20 wherein;
Described phosphoric acid ester is any one of following structural formula:
In the formula, m=0～20.
2. a kind of phosphoric acid ester doped polyaniline protective system as claimed in claim 1 is characterized in that the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy is 150;
Phosphoric acid ester doped polyaniline 10;
Pigment is 370, wherein, and aluminium dihydrogen tripolyphosphate; Zinc phosphate: iron mica is 150: 150 grams: iron mica 70;
Filler is 150, and wherein, 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;
The B component: solidifying agent is 100.
3. a kind of phosphoric acid ester doped polyaniline protective system as claimed in claim 1 is characterized in that the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy is 120;
Phosphoric acid ester doped polyaniline 20;
Pigment is 500, wherein, and aluminium dihydrogen tripolyphosphate; Zinc phosphate: iron mica is 200: 200: 100;
Filler is 60, and wherein, 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;
The B component: solidifying agent is 60.
4. a kind of phosphoric acid ester doped polyaniline protective system as claimed in claim 1 is characterized in that the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy is 200;
The phosphoric acid ester doped polyaniline is 30;
Pigment is 320, wherein, and aluminium dihydrogen tripolyphosphate; Zinc phosphate: iron mica is 130: 130: 60;
Filler is 50, and wherein, talcum powder: zinc oxide: process white is 20: 20: 10;
Thinner is 240;
The auxiliary agent dispersion agent is 10, dispersant B YK163: flow agent BYK371 is 5: 5;
The B component: solidifying agent is 150.
5. a kind of phosphoric acid ester doped polyaniline protective system as claimed in claim 1 is characterized in that the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy is 200;
The phosphoric acid ester doped polyaniline is 30;
Pigment is 320, wherein, and aluminium dihydrogen tripolyphosphate; Zinc phosphate: iron mica is 130: 130: 60;
Filler is 50, and wherein, talcum powder: zinc oxide: process white is 20: 20: 10;
Thinner is 240;
Auxiliary agent is 10, and wherein, dispersant B YK163: flow agent BYK371 is 5: 5;
The B component: solidifying agent is 150.
6. a kind of phosphoric acid ester doped polyaniline protective system as claimed in claim 1 is characterized in that the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy is 160;
The phosphoric acid ester doped polyaniline is 40;
Pigment is 320, wherein, and aluminium dihydrogen tripolyphosphate; Zinc phosphate: iron mica is 120: 120: 80;
Filler is 140, and wherein, talcum powder: zinc oxide: process white is 50: 40: 50;
Thinner is 260; Auxiliary agent is 30, and wherein, dispersant B YK163: flow agent BYK371 is 15: 15;
The B component: solidifying agent is 72.
7. a kind of phosphoric acid ester doped polyaniline protective system as claimed in claim 1 is characterized in that the component of its prescription and weight part proportioning are:
The A component:
Resins, epoxy is 140;
The phosphoric acid ester doped polyaniline is 50;
Pigment is 350, wherein, and aluminium dihydrogen tripolyphosphate; Zinc phosphate: iron mica is 150: 130: 70;
Filler is 80, and wherein, talcum powder: zinc oxide: process white is 20: 30: 30;
Thinner is 300;
Auxiliary agent is 20, and wherein, dispersant B YK163: flow agent BYK371 is 10: 10;
The B component: solidifying agent is 60.
8. the method for making of a kind of phosphoric acid ester doped polyaniline protective system as claimed in claim 1 is characterized in that step is as follows:
By proportioning take by weighing Resins, epoxy, thinner is put into the sand mill jar, put into phosphoric acid ester doped polyaniline powder under stirring, stirred 0.5～2 hour, stir and add auxiliary agent, pigment and filler down more respectively, stirred 0.5～3 hour with 2500 rev/mins speed, sand milling 1～5 hour filters with 200 order filter clothes, obtains component A;
By proportioning component B and component A are stirred in the machine at height and to stir 3～5 minutes, obtain phosphoric acid ester doped polyaniline protective system with 1200～1500 rev/mins.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834265A (en) * | 2014-03-24 | 2014-06-04 | 中国科学院长春应用化学研究所 | 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 |
| CN117567018A (en) * | 2024-01-16 | 2024-02-20 | 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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| CN101368058A (en) * | 2008-10-09 | 2009-02-18 | 同济大学 | Process for producing polyaniline corrosion protection conducting coating |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103834265A (en) * | 2014-03-24 | 2014-06-04 | 中国科学院长春应用化学研究所 | Polyaniline anti-corrosive paint |
| 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 |
| CN117567018A (en) * | 2024-01-16 | 2024-02-20 | 山东民烨耐火纤维有限公司 | Preparation method of ceramic fiber antistatic heat insulation plate |
| 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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|---|---|
| CN102108241B (en) | 2014-04-16 |
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