CN105001759A - Molybdate doped polypyrrole/epoxy resin self-healing coating, preparation method thereof and application thereof - Google Patents
Molybdate doped polypyrrole/epoxy resin self-healing coating, preparation method thereof and application thereof Download PDFInfo
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Abstract
The invention relates to a molybdate doped polypyrrole/epoxy resin self-healing coating, a preparation method thereof and an application thereof, and belongs to the field of metal anti-corrosion coatings. The coating is composed of two parts, namely a polypyrrole/epoxy resin system mother liquor, and a polyamide curing agent. The polypyrrole/epoxy resin system mother liquor comprises molybdate doped polypyrrole, epoxy resin, an anti-settling agent, an anti-foaming agent, a levelling agent and an organic solvent. The molybdate doped polypyrrole is added in the organic solvent and then the mixture is uniformly dispersed in an ultrasonic dispersion instrument. After that, the anti-settling agent, the antifoaming agent and the levelling agent are added respectively, and are stirred on a magnetic stirring apparatus. Then the epoxy resin is added to form the uniformly dispersed polypyrrole/epoxy resin system mother liquor. The polyamide curing agent is added in the prepared mother liquor, and is stirred to be uniformly dispersed. In this way, a molybdate doped polypyrrole/epoxy resin self-healing coating can be obtained. The coating is sprayed or brushed onto the 2024 type aluminum alloy after being subjected to oil-removing treatment. After the drying and curing process of the coating at the room temperature, a molybdate doped polypyrrole/epoxy resin self-healing coating can be formed.
Description
Technical field
The present invention relates to a kind of molybdate Doped polypyrrole/epoxy resin self-healing coatings and Synthesis and applications thereof, belong to anti-corrosive metal coating field.
Background technology
Metallic corrosion is the key subjects needing solution in industrial production badly for a long time always, therefore researches and develops effective corrosion protection steps and has great importance.In metal protection method, the most widely used method is at metallic surface coating protective system, because film-forming resin only has barrier properties, usually adds rust-stabilising pigment if chromic salt is to improve the antiseptic property of coating in coating.When coating occurs to destroy, the chromic salt in coating can form passive film in metallic surface, suppresses the germinating of corrosion.But chromic salt has carinogenicity, therefore research and development replace the filler of chromic salt, and the long-acting use and the coatings that realize coating become the target needed badly and will realize.
In recent years along with the further investigation to conductive polymers, investigators find that electric polypyrrole is in the process of oxypolymerization, can be doped into the electrical counteract that negatively charged ion keeps polypyrrole.And when polypyrrole obtains electronics generation reduction reaction, the negatively charged ion of doping can be discharged.Utilize this doping character of polypyrrole, using the carrier of polypyrrole as metal sustained release dosage, the polypyrrole after doping can be added in coating as filler.When coating is destroyed, there is corrosion betatopic in metal, polypyrrole obtains electronics as negative electrode and discharges sustained release dosage, thus plays the effect of selfreparing.Meanwhile, pyrrole monomer is carcinogenic, and polypyrrole synthesis is convenient, good stability.Therefore, polypyrrole is considered to one of material preparing coatings being hopeful most to replace chromic salt.
At present, the coatings about polypyrrole has been reported.The people such as G.Paliwoda-Porebska have developed the coatings being applicable to iron-based body, are joined in organic coating by phosphomolybdate Doped polypyrrole as filler.Chinese invention patent (publication number CN 103642365 A) reports a kind of marine aluminium alloy coatings, take nano silicon as core, prepare the polypyrrole of the fluorine titanium/zirconate ion doping of nucleocapsid structure, the silicon-dioxide of preparation/polypyrrole composite particles is joined in marine aluminium alloy priming paint as filler.But above-mentioned polypyrrole filler preparation technology is loaded down with trivial details, there is the simple polypyrrole coatings of a kind of preparation technology to be developed.This coatings is applicable to the protection of space flight aluminium alloy 2024, the bibliographical information that the application of polypyrrole coatings on space flight aluminium alloy is also not relevant.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of molybdate Doped polypyrrole/epoxy resin coatings, this preparation technology of coating is simple, workable, there is good physical and mechanical properties and coating self-healing properties, significantly improve erosion resistance and the service life of coating.
Technical scheme of the present invention is:
A kind of molybdate Doped polypyrrole/epoxy resin self-healing coatings, this coating is made up of following two components:
Component one is polypyrrole/epoxy-resin systems mother liquor, according to the mass fraction, comprises following component and content:
Molybdate Doped polypyrrole 8 ~ 20 parts, epoxy resin 140 ~ 160 parts, anti-settling agent 0.7 ~ 1 part, defoamer 0.7 ~ 1 part, flow agent 0.7 ~ 1 part, organic solvent 70 ~ 80 parts;
Component two is polyamide curing agent;
The mass ratio of epoxy resin and polyamide curing agent is 1:(0.8 ~ 1).
Described molybdate Doped polypyrrole/epoxy resin self-healing coatings, molybdate Doped polypyrrole used, i.e. selfreparing component accounts for 2 ~ 5% of the polypyrrole-epoxy resin coating system quality of molybdate Doped polypyrrole and epoxypaint composition.
Described molybdate Doped polypyrrole/epoxy resin self-healing coatings, in molybdate Doped polypyrrole, the doping of molybdate is 3 ~ 12wt% (being preferably 5 ~ 10wt%).
Described molybdate Doped polypyrrole/epoxy resin self-healing coatings, molybdate used is Sodium orthomolybdate.
Described molybdate Doped polypyrrole/epoxy resin self-healing coatings, epoxy resin is E-44 bisphenol A type epoxy resin, and polyamide curing agent is polyamide 6 50.
Described molybdate Doped polypyrrole/epoxy resin self-healing coatings, organic solvent is the mixed solvent of dimethylbenzene and propyl carbinol, and the mass ratio of dimethylbenzene and propyl carbinol is (5 ~ 7): (3 ~ 5).
The preparation method of described molybdate Doped polypyrrole/epoxy resin self-healing coatings, concrete steps are as follows:
(1) preparation of molybdate Doped polypyrrole: get 4 ~ 8 mass parts doping agent Sodium orthomolybdates with deionized water by 1:(45 ~ 70) mass ratio mix, and magnetic agitation forms the aqueous solution of doping agent; Keep whole temperature of reaction system at 0 ~ 2 DEG C, in reaction system, drip the pyrrole monomer of 1 ~ 3 mass parts in a nitrogen atmosphere, afterwards oxygenant ammonium persulfate aqueous solution 50 ~ 60 mass parts prepared in advance is dropwise instilled; Magnetic agitation is polymerized after 5 ~ 6 hours, stopped reaction, and filtered by products therefrom, filter cake deionized water wash is clean; Product is dried after 5 ~ 10 hours at the vacuum drying oven of 50 ~ 70 DEG C, and obtain the Sodium orthomolybdate Doped polypyrrole of black, its size range is 50nm ~ 100nm;
(2) preparation of polypyrrole/epoxy-resin systems mother liquor: get molybdate Doped polypyrrole prepared by 8 ~ 20 mass parts, be ground to powder with agate mortar, adds 70 ~ 80 mass parts organic solvents and is uniformly dispersed in ultrasonic wave separating apparatus; Get anti-settling agent, defoamer, each 0.7 ~ 1 mass parts of flow agent respectively, join in the polypyrrole dispersion soln of above-mentioned steps preparation, magnetic stirring apparatus stirs 5 ~ 15 minutes; Then add epoxy resin 140 ~ 160 mass parts, Homogeneous phase mixing in high speed ball mill, make epoxy resin by organic solvent diluting, form finely dispersed polypyrrole/epoxy-resin systems mother liquor;
In the mother liquor prepared, add polyamide curing agent, dispersed with stirring is even, both obtains molybdate Doped polypyrrole/epoxypaint.
The preparation method of described molybdate Doped polypyrrole/epoxy resin self-healing coatings, in oxygenant ammonium persulfate aqueous solution, ammonium persulphate and deionized water are with 1:(7 ~ 20) mass ratio prepare.
The application of described molybdate Doped polypyrrole/epoxy resin self-healing coatings, by paint spay-coating or brush on 2024 aluminium alloys through oil removal treatment, forms molybdate Doped polypyrrole/epoxy resin coatings after Air drying solidification.
Advantage of the present invention and beneficial effect are:
1, the present invention adopts molybdate Doped polypyrrole to join in epoxypaint as filler, and the coating of preparation has good self-healing properties to 2024 aluminium alloys.When coating occurs to destroy, alloy matrix aluminum corrodes, and the polypyrrole in coating obtains electronics as negative electrode, dedoping reaction occurs, discharges inhibitor anion molybdate, effectively can suppress the further corrosion of metal, thus play the effect of selfreparing.
2, the molybdate Doped polypyrrole preparation technology for preparing of the present invention is simple, easy to operate.Molybdate Doped polypyrrole has excellent electrochemical activity, can discharge inhibiter under reduction potential.Meanwhile, the polypyrrole of doping has good chemical compatibility and dispersiveness in the epoxy, and coating crosslinking degree is higher, and compactness is good.
3, molybdate Doped polypyrrole-epoxy coating excellent combination property of the present invention, and the sticking power between metallic matrix is 2 ~ 3 times of sticking power between epoxy resin varnish coating and metallic matrix.In neutral salt spray, polypyrrole-epoxy based coatings has good erosion resistance, and antiseptic property is greatly improved than epoxy resin varnish coating.
Accompanying drawing explanation
Fig. 1 is the photo of embodiment 1 coating after scribing cut after 720 hours salt fogs.
Fig. 2 is the photo of comparative example 1 coating after scribing cut after 720 hours salt fogs.
Fig. 3 is the photo of comparative example 2 coating after scribing cut after 720 hours salt fogs.
Embodiment
In a specific embodiment, molybdate Doped polypyrrole/epoxy resin self-healing coatings of the present invention and its preparation method and application, specific as follows:
(1) preparation (mass parts) of molybdate Doped polypyrrole: drip 1 ~ 3 part of pyrrole monomer in the aqueous solution of 4 ~ 8 parts of Sodium orthomolybdates, dropwise drip oxygenant ammonium persulfate aqueous solution 50 ~ 60 parts, in nitrogen atmosphere, 0 ~ 2 DEG C of condition lower magnetic force stirs polymerization 5 ~ 6 hours, after filtration, wash, 50 ~ 70 DEG C of vacuum-drying 5 ~ 10 hours, obtains black molybdate Doped polypyrrole.
(2) preparation (mass parts) of polypyrrole-epoxy coating: the molybdate Doped polypyrrole 8 ~ 20 parts getting preparation, (anti-settling agent, defoamer, flow agent are epoxypaint usual auxiliaries to add organic solvent 70 ~ 80 parts, anti-settling agent and defoamer and each 0.7 ~ 1 part of flow agent, as: anti-settling agent is modified hydrogenated Viscotrol C, defoamer is methyl-silicone oil or fatty acid alkyl ester, flow agent is silane or acrylate), epoxy resin 140 ~ 160 parts, form finely dispersed polypyrrole/epoxy-resin systems mother liquor.In the mother liquor prepared, add polyamide curing agent, obtain molybdate Doped polypyrrole/epoxypaint.
By paint spay-coating or brush on 2024 aluminium alloys through oil removal treatment, after Air drying solidification, form molybdate Doped polypyrrole/epoxy resin coatings.
The present invention is described in more detail by the following examples, but embodiments of the present invention are not limited thereto.
Embodiment 1
Get doping agent Sodium orthomolybdate 3.5 parts, mix by 1:45 mass ratio with deionized water, and magnetic agitation forms the aqueous solution of doping agent.Keep whole temperature of reaction system at 2 DEG C, in nitrogen atmosphere, in reaction system, drip the pyrrole monomer of 2 parts, then the aqueous solution (mass ratio of ammonium persulphate and deionized water is 1:17) 54 parts of the oxygenant ammonium persulphate prepared in advance is dropwise instilled.After magnetic agitation is polymerized 6 hours, stopped reaction, filtered by products therefrom, filter cake deionized water repeatedly washs.Product is after the vacuum drying oven of 60 DEG C dries 8 hours, and obtain the Sodium orthomolybdate Doped polypyrrole of black, the doping of the present embodiment Sodium orthomolybdate is 10wt%.
Get 8 parts of Sodium orthomolybdate Doped polypyrroles, 80 parts of organic solvents are uniformly dispersed in ultrasonic disperse instrument.Get anti-settling agent, defoamer, each 1 part of flow agent respectively, add the polypyrrole dispersion soln of above-mentioned preparation, magnetic stirring apparatus stirred after 10 minutes, adds 153 parts of epoxy resin, Homogeneous phase mixing in high speed ball mill, obtains finely dispersed polypyrrole/epoxy-resin systems mother liquor.
Be 1:0.8 by the mass ratio of epoxy resin and solidifying agent, polyamide curing agent joined in the mother liquor prepared, dispersed with stirring is even, both Sodium orthomolybdate Doped polypyrrole/epoxypaint.Paint brush is coated on 2024 aluminium alloys of oil removal treatment, after Air drying solidification, forms Sodium orthomolybdate Doped polypyrrole/epoxy coating.
Comparative example 1
Difference from Example 1 is:
Get 2 parts of Sodium orthomolybdate Doped polypyrroles, 80 parts of organic solvents are uniformly dispersed in ultrasonic disperse instrument.Get anti-settling agent, defoamer, each 1 part of flow agent respectively, add the polypyrrole dispersion soln of above-mentioned preparation, magnetic stirring apparatus stirred after 10 minutes, adds 153 parts of epoxy resin, Homogeneous phase mixing in high speed ball mill, obtains finely dispersed polypyrrole/epoxy-resin systems mother liquor.
Be 1:0.8 by the mass ratio of epoxy resin and solidifying agent, polyamide curing agent joined in the mother liquor prepared, dispersed with stirring is even, both Sodium orthomolybdate Doped polypyrrole/epoxypaint.Paint brush is coated on 2024 aluminium alloys of oil removal treatment, after Air drying solidification, forms Sodium orthomolybdate Doped polypyrrole/epoxy coating.
Comparative example 2
Difference from Example 1 is:
Get 4 parts of Sodium orthomolybdate Doped polypyrroles, 80 parts of organic solvents are uniformly dispersed in ultrasonic disperse instrument.Get anti-settling agent, defoamer, each 1 part of flow agent respectively, add the polypyrrole dispersion soln of above-mentioned preparation, magnetic stirring apparatus stirred after 10 minutes, adds 153 parts of epoxy resin, Homogeneous phase mixing in high speed ball mill, obtains finely dispersed polypyrrole/epoxy-resin systems mother liquor.
Be 1:0.8 by the mass ratio of epoxy resin and solidifying agent, polyamide curing agent joined in the mother liquor prepared, dispersed with stirring is even, both Sodium orthomolybdate Doped polypyrrole/epoxypaint.Paint brush is coated on 2024 aluminium alloys of oil removal treatment, after Air drying solidification, forms Sodium orthomolybdate Doped polypyrrole/epoxy coating.
Embodiment 2
Get doping agent Sodium orthomolybdate 3.5 parts, mix by 1:50 mass ratio with deionized water, and magnetic agitation forms the aqueous solution of doping agent.Keep whole temperature of reaction system at 2 DEG C, in nitrogen atmosphere, in reaction system, drip the pyrrole monomer of 2 parts, then the aqueous solution (mass ratio of ammonium persulphate and deionized water is 1:7) 60 parts of the oxygenant ammonium persulphate prepared in advance is dropwise instilled.After magnetic agitation is polymerized 6 hours, stopped reaction, filtered by products therefrom, filter cake deionized water repeatedly washs.Product is after the vacuum drying oven of 60 DEG C dries 8 hours, and obtain the Sodium orthomolybdate Doped polypyrrole of black, the doping of the present embodiment Sodium orthomolybdate is 12wt%.
Get 12 parts of Sodium orthomolybdate Doped polypyrroles, 70 parts of organic solvents are uniformly dispersed in ultrasonic disperse instrument.Get anti-settling agent, defoamer, each 0.8 part of flow agent respectively, add the polypyrrole dispersion soln of above-mentioned preparation, magnetic stirring apparatus stirred after 10 minutes, adds 145 parts of epoxy resin, Homogeneous phase mixing in high speed ball mill, obtains finely dispersed polypyrrole/epoxy-resin systems mother liquor.
Be 1:1 by the mass ratio of epoxy resin and solidifying agent, polyamide curing agent joined in the mother liquor prepared, dispersed with stirring is even, both Sodium orthomolybdate Doped polypyrrole/epoxypaint.Paint brush is coated on 2024 aluminium alloys of oil removal treatment, after Air drying solidification, forms Sodium orthomolybdate Doped polypyrrole/epoxy coating.
Embodiment 3
Get doping agent Sodium orthomolybdate 3.5 parts, mix by 1:55 mass ratio with deionized water, and magnetic agitation forms the aqueous solution of doping agent.Keep whole temperature of reaction system at 2 DEG C, in nitrogen atmosphere, in reaction system, drip the pyrrole monomer of 3 parts, then the aqueous solution (mass ratio of ammonium persulphate and deionized water is 1:18) 57 parts of the oxygenant ammonium persulphate prepared in advance is dropwise instilled.After magnetic agitation is polymerized 6 hours, stopped reaction, filtered by products therefrom, filter cake deionized water repeatedly washs.Product is after the vacuum drying oven of 60 DEG C dries 8 hours, and obtain the Sodium orthomolybdate Doped polypyrrole of black, the doping of the present embodiment Sodium orthomolybdate is 3wt%.
Get 16 parts of Sodium orthomolybdate Doped polypyrroles, 75 parts of organic solvents are uniformly dispersed in ultrasonic disperse instrument.Get anti-settling agent, defoamer, each 0.9 part of flow agent respectively, add the polypyrrole dispersion soln of above-mentioned preparation, magnetic stirring apparatus stirred after 10 minutes, adds 158 parts of epoxy resin, Homogeneous phase mixing in high speed ball mill, obtains finely dispersed polypyrrole/epoxy-resin systems mother liquor.
Be 1:0.8 by the mass ratio of epoxy resin and solidifying agent, polyamide curing agent joined in the mother liquor prepared, dispersed with stirring is even, both Sodium orthomolybdate Doped polypyrrole/epoxypaint.Paint brush is coated on 2024 aluminium alloys of oil removal treatment, after Air drying solidification, forms Sodium orthomolybdate Doped polypyrrole/epoxy coating.
The coating of embodiment 1, comparative example 1 and comparative example 2, under the condition scribing two vertical cuts and breakdown of coating, the coating photo after 720 hours salt-fog tests as shown in Figure 1, Figure 2 and Fig. 3.As we can see from the figure, the foaming of embodiment 1 coating and get rusty obviously than comparative example 1 and comparative example 2 coating few a lot, show excellent salt spray resistance and coating self-healing properties.Embodiment result shows, molybdate Doped polypyrrole used, i.e., when selfreparing component accounts for 2 ~ 5% of polypyrrole-epoxy resin coating system quality, preservative effect is best.
Claims (9)
1. molybdate Doped polypyrrole/epoxy resin self-healing coatings, is characterized in that, this coating is made up of following two components:
Component one is polypyrrole/epoxy-resin systems mother liquor, according to the mass fraction, comprises following component and content:
Molybdate Doped polypyrrole 8 ~ 20 parts, epoxy resin 140 ~ 160 parts, anti-settling agent 0.7 ~ 1 part, defoamer 0.7 ~ 1 part, flow agent 0.7 ~ 1 part, organic solvent 70 ~ 80 parts;
Component two is polyamide curing agent;
The mass ratio of epoxy resin and polyamide curing agent is 1:(0.8 ~ 1).
2. according to molybdate Doped polypyrrole/epoxy resin self-healing coatings according to claim 1, it is characterized in that: molybdate Doped polypyrrole used, i.e. selfreparing component accounts for 2 ~ 5% of the polypyrrole-epoxy resin coating system quality of molybdate Doped polypyrrole and epoxypaint composition.
3. according to molybdate Doped polypyrrole/epoxy resin self-healing coatings according to claim 1, it is characterized in that: in molybdate Doped polypyrrole, the doping of molybdate is 3 ~ 12wt%.
4. according to the molybdate Doped polypyrrole/epoxy resin self-healing coatings described in claim 1 or 3, it is characterized in that: molybdate used is Sodium orthomolybdate.
5. according to molybdate Doped polypyrrole/epoxy resin self-healing coatings according to claim 1, it is characterized in that: epoxy resin is E-44 bisphenol A type epoxy resin, polyamide curing agent is polyamide 6 50.
6. according to molybdate Doped polypyrrole/epoxy resin self-healing coatings according to claim 1, it is characterized in that: organic solvent is the mixed solvent of dimethylbenzene and propyl carbinol, the mass ratio of dimethylbenzene and propyl carbinol is (5 ~ 7): (3 ~ 5).
7. a preparation method for molybdate Doped polypyrrole/epoxy resin self-healing coatings according to claim 1, it is characterized in that, concrete steps are as follows:
(1) preparation of molybdate Doped polypyrrole: get 4 ~ 8 mass parts doping agent Sodium orthomolybdates with deionized water by 1:(45 ~ 70) mass ratio mix, and magnetic agitation forms the aqueous solution of doping agent; Keep whole temperature of reaction system at 0 ~ 2 DEG C, in reaction system, drip the pyrrole monomer of 1 ~ 3 mass parts in a nitrogen atmosphere, afterwards oxygenant ammonium persulfate aqueous solution 50 ~ 60 mass parts prepared in advance is dropwise instilled; Magnetic agitation is polymerized after 5 ~ 6 hours, stopped reaction, and filtered by products therefrom, filter cake deionized water wash is clean; Product is dried after 5 ~ 10 hours at the vacuum drying oven of 50 ~ 70 DEG C, and obtain the Sodium orthomolybdate Doped polypyrrole of black, its size range is 50nm ~ 100nm;
(2) preparation of polypyrrole/epoxy-resin systems mother liquor: get molybdate Doped polypyrrole prepared by 8 ~ 20 mass parts, be ground to powder with agate mortar, adds 70 ~ 80 mass parts organic solvents and is uniformly dispersed in ultrasonic wave separating apparatus; Get anti-settling agent, defoamer, each 0.7 ~ 1 mass parts of flow agent respectively, join in the polypyrrole dispersion soln of above-mentioned steps preparation, magnetic stirring apparatus stirs 5 ~ 15 minutes; Then add epoxy resin 140 ~ 160 mass parts, Homogeneous phase mixing in high speed ball mill, make epoxy resin by organic solvent diluting, form finely dispersed polypyrrole/epoxy-resin systems mother liquor;
In the mother liquor prepared, add polyamide curing agent, dispersed with stirring is even, both obtains molybdate Doped polypyrrole/epoxypaint.
8. the preparation method of molybdate Doped polypyrrole/epoxy resin self-healing coatings according to claim 7, is characterized in that, in oxygenant ammonium persulfate aqueous solution, ammonium persulphate and deionized water are with 1:(7 ~ 20) mass ratio prepare.
9. the application of molybdate Doped polypyrrole/epoxy resin self-healing coatings according to claim 1, it is characterized in that, by paint spay-coating or brush on 2024 aluminium alloys through oil removal treatment, after Air drying solidification, form molybdate Doped polypyrrole/epoxy resin coatings.
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