CN111592809A - Graphene-polypyrrole composite heavy-duty anticorrosive paint and preparation method thereof - Google Patents
Graphene-polypyrrole composite heavy-duty anticorrosive paint and preparation method thereof Download PDFInfo
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- CN111592809A CN111592809A CN201910749936.7A CN201910749936A CN111592809A CN 111592809 A CN111592809 A CN 111592809A CN 201910749936 A CN201910749936 A CN 201910749936A CN 111592809 A CN111592809 A CN 111592809A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
- C09D5/106—Anti-corrosive paints containing metal dust containing Zn
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0893—Zinc
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Abstract
The invention provides a graphene-polypyrrole zinc-rich heavy-duty anticorrosive paint and a preparation method thereof, wherein the paint comprises the following components: cured epoxy resin, a graphene-polypyrrole composite material and zinc powder; wherein the mass ratio of the graphene-polypyrrole composite material to the cured epoxy resin is (0.3-0.8): 100, respectively; the mass ratio of the graphene-polypyrrole composite material to the zinc powder is (0.0075-0.03): 4. according to the invention, the utilization rate of zinc and the service life of the primer are improved through the graphene-polypyrrole; the problems of low utilization rate of zinc, pollution, waste and the like of the existing zinc-rich primer are solved; the preparation method is simple and easy to realize industrial production.
Description
Technical Field
The invention relates to a heavy-duty anticorrosive coating, and in particular relates to a graphene-polypyrrole composite heavy-duty anticorrosive coating and a preparation method thereof.
Background
The marine corrosion is a common subject in the world at present, which is invading marine engineering facilities in China at an astonishing speed, and threatens the safety of the marine engineering facilities all the time and greatly hinders the step of marine economic development in China. Heavy-duty anticorrosive coatings refer to anticorrosive coatings that can be applied in a relatively harsh corrosive environment compared to conventional anticorrosive coatings and have a longer protection period than conventional anticorrosive coatings.
The epoxy zinc-rich primer has the advantages of quick natural drying, strong adhesive force, strong corrosion resistance, high zinc powder content in a paint film, cathodic protection, excellent water resistance and the like, and is widely applied to marine corrosion prevention.
The document search of the prior art finds that Chinese patent documents CN107141969A, CN103483983A and CN107345110A provide a preparation method of a zinc-rich primer, and the method has the following defects: the utilization rate of zinc is low, and pollution and waste are caused.
No report on the use of graphene-polypyrrole to prepare epoxy zinc rich primer coatings was found by searching existing patents and literature.
Disclosure of Invention
The invention aims to provide a graphene-polypyrrole composite heavy-duty anticorrosive coating and a preparation method thereof, so as to solve the problems of low utilization rate of zinc of a zinc-rich primer, pollution and waste and the like in the prior art, improve the utilization rate and the service life of zinc in an epoxy zinc-rich primer, resist salt spray for 2000 hours, and meet performance indexes required in a severe marine corrosion environment.
The invention discloses a graphene-polypyrrole composite heavy-duty anticorrosive paint which is characterized by comprising the following components: cured epoxy resin, a graphene-polypyrrole composite material and zinc powder; wherein the mass ratio of the graphene-polypyrrole composite material to the cured epoxy resin is (0.3-0.8): 100, respectively; the mass ratio of the graphene-polypyrrole composite material to the zinc powder is (0.0075-0.03): 4.
the graphene-polypyrrole composite material is characterized in that the mass ratio of graphene to polypyrrole in the graphene-polypyrrole composite material is (0.5-5) to 1, and the preferable mass ratio is (0.5-2): 1; the graphene is 1-10 layers of graphene, and is preferably single-layer graphene; the conductivity of the polypyrrole is 1-15S/cm, and is preferably 13-15S/cm;
the cured epoxy resin is bisphenol A epoxy resin and a polyamine curing agent, wherein the molar ratio of epoxy groups to amino groups is 1: (1-1.2) to complete curing.
The invention also provides a preparation method of the graphene-polypyrrole composite heavy-duty anticorrosive paint, which is characterized by comprising the following steps of:
(1) mixing the graphene-polypyrrole composite material with a solvent to obtain a suspension; (2) adding the suspension into the cured epoxy resin, and uniformly stirring to obtain a mixture; (3) adding zinc powder into the mixture, and stirring to uniformly mix the zinc powder and the mixture to obtain the graphene-polypyrrole composite heavy-duty anticorrosive paint;
the solvent is an organic solvent, and the organic solvent comprises: one or a mixture of more than two of ethanol, acetone, toluene, xylene or N-methyl pyrrolidone; preferably, the solvent is xylene; the addition amount of the solvent is 0.1-2 ml: 10g of epoxy resin.
Further, the preparation method of the graphene-polypyrrole composite heavy-duty anticorrosive coating also comprises the preparation method of the graphene-polypyrrole composite material, and comprises the following steps: uniformly mixing graphene and sodium dodecyl benzene sulfonate to obtain a solid mixture; adding pyrrole and hydrochloric acid into the solid mixture, and keeping the temperature at-5 to 10 ℃ to react for 0.5 to 5 hours; adding ammonium persulfate into the reactant, and keeping the temperature of between 5 ℃ below zero and 10 ℃ for continuous reaction for 5 to 24 hours to obtain the graphene-polypyrrole composite material;
the mass ratio of the graphene to the sodium dodecyl benzene sulfonate is (0.5-5) to 1, preferably (0.5-2) to 1; the volume ratio of the pyrrole to the hydrochloric acid is 0.1:5, and the concentration of the hydrochloric acid is 0.1-5 mol/L, preferably 1 mol/L; the ratio of the mass of the graphene to the volume of the pyrrole is (0.5 g-2 g): 5mL, preferably 1 g: 5 mL; the mass ratio of the ammonium persulfate to the volume of the pyrrole is (0.5 g-5 g): 1mL, preferably 1.2 g: 1 mL.
Further, in the step (1), the graphene and the sodium dodecyl benzene sulfonate are uniformly mixed in pure water by ultrasonic waves, then a solid mixture is obtained by filtering, and the mixture is dried at the temperature of 60-75 ℃.
The graphene-polypyrrole composite heavy-duty anticorrosive coating improves the utilization rate of zinc (by 30 percent compared with the prior art) and prolongs the service life of a primer (for example, the salt spray resistant exposure time is prolonged by more than 1000 hours) through the graphene-polypyrrole; the problems of low utilization rate of zinc, pollution, waste and the like of the existing zinc-rich primer are solved; the preparation method is simple and easy to realize industrial production, and the salt spray resistance of the prepared graphene-polypyrrole composite heavy-duty anticorrosive coating reaches 2000h, so that the performance index required in a severe corrosion environment in the ocean is met.
Drawings
Fig. 1 is a fourier transform infrared spectrum of graphene and the graphene-polypyrrole composite material of the present invention.
FIG. 2 shows the salt spray test results of the heavy duty anticorrosive coatings of examples 1 to 3 of the present invention.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings and examples. It should be recognized that the present embodiments are not to be considered as limiting, and that numerous modifications and alterations of the present invention will become apparent to those skilled in the art upon a reading of the present embodiments.
Example 1
(1) Taking 0.1g of graphene and 0.1g of sodium dodecyl benzene sulfonate, mixing, putting into 200mL of pure water, performing ultrasonic treatment for 2 hours, filtering, and drying at 70 ℃ for 4 hours to obtain a powdery solid mixture; adding 0.5mL of pyrrole and 25mL of hydrochloric acid with the concentration of 0.5mol/L into the solid mixture, and stirring and reacting for 1h at the temperature of 5 ℃; then 0.6g of ammonium persulfate is added into the reactants, and the mixture is stirred and reacted for 10 hours at the temperature of 5 ℃; carrying out suction filtration on the reaction mixture to obtain a solid, and then washing and drying to obtain the graphene-polypyrrole composite material;
(2) taking 0.0075g of the graphene-polypyrrole composite material, adding into 1.5mL of dimethylbenzene, and carrying out ultrasonic mixing for 30min to obtain a graphene-polypyrrole-dimethylbenzene solution for later use;
(3) taking 3g E51 epoxy resin and 1g D-230 polyether amine curing agent, and fully and uniformly stirring to obtain cured epoxy resin;
(4) pouring the cured epoxy resin obtained in the step (3) into the graphene-polypyrrole-xylene solution obtained in the step (2), and continuously stirring for 3min until the mixture is uniform; adding 4g of zinc powder, fully stirring for 3min, and standing for 2min to obtain the graphene-polypyrrole composite heavy-duty anticorrosive coating.
The coating was applied to a 10X 1mm iron block (the surface of the iron block was polished smooth with 800# sandpaper) and allowed to dry for 48 hours to complete the preparation of test samples.
Example 2
(1) Taking 0.1g of graphene and 0.2g of sodium dodecyl benzene sulfonate, mixing, putting into 200mL of pure water, performing ultrasonic treatment for 2 hours, filtering, and drying at 70 ℃ for 3 hours to obtain a powdery solid mixture; adding 1mL of pyrrole and 25mL of hydrochloric acid with the concentration of 1.0mol/L into the solid mixture, and stirring and reacting for 1.2h at the temperature of 2 ℃; adding 1.2g of ammonium persulfate into the reactant, and stirring and reacting for 12 hours at the temperature of 3 ℃; carrying out suction filtration on the reaction mixture to obtain a solid, and then washing and drying to obtain the graphene-polypyrrole composite material;
(2) adding 0.015g of the graphene-polypyrrole composite material into 1.5mL of dimethylbenzene, and carrying out ultrasonic mixing for 30min to obtain a standby graphene-polypyrrole-dimethylbenzene solution;
(3) taking 4g E44 epoxy resin and 1g T31 epoxy curing agent, and fully and uniformly stirring to obtain cured epoxy resin;
(4) pouring the cured epoxy resin obtained in the step (3) into the graphene-polypyrrole-xylene solution obtained in the step (2), and continuously stirring for 2min until the mixture is uniform; adding 4g of zinc powder, fully stirring for 5min, and standing for 2min to obtain the graphene-polypyrrole composite heavy-duty anticorrosive coating.
The coating was applied to a 10X 1mm iron block (the surface of the iron block was polished smooth with 800# sandpaper) and allowed to dry for 48 hours to complete the preparation of test samples.
Example 3
(1) Taking 0.2g of graphene and 0.1g of sodium dodecyl benzene sulfonate, mixing, putting into 200mL of pure water, performing ultrasonic treatment for 2 hours, filtering, and drying at 60 ℃ for 5 hours to obtain a powdery solid mixture; adding 0.5mL of pyrrole and 25mL of hydrochloric acid with the concentration of 2.0mol/L into the solid mixture, and stirring and reacting for 2h at the temperature of 0 ℃; then 2g of ammonium persulfate is added into the reactant, and the reaction is carried out for 24 hours under the condition of keeping the temperature at 0 ℃ with stirring; carrying out suction filtration on the reaction mixture to obtain a solid, and then washing and drying to obtain the graphene-polypyrrole composite material;
(2) adding 0.03g of the graphene-polypyrrole composite material into 2mL of dimethylbenzene, and carrying out ultrasonic mixing for 30min to obtain a standby graphene-polypyrrole-dimethylbenzene solution;
(3) taking 4g E44 epoxy resin and 1g T31 epoxy curing agent, and fully and uniformly stirring to obtain cured epoxy resin;
(4) pouring the cured epoxy resin obtained in the step (3) into the graphene-polypyrrole-xylene solution obtained in the step (2), and continuously stirring for 3min until the mixture is uniform; adding 4g of zinc powder, fully stirring for 3min, and standing for 2min to obtain the graphene-polypyrrole composite heavy-duty anticorrosive coating.
The coating was applied to a 10X 1mm iron block (the surface of the iron block was polished smooth with 800# sandpaper) and allowed to dry for 48 hours to complete the preparation of test samples.
Fig. 1 is a comparison graph of fourier transform infrared spectra of graphene and the graphene-polypyrrole composite material of the present invention, which confirms the presence of a functional group on the surface of graphene after polypyrrole grafting, and indicates that in-situ polymerization on the surface of graphene is successful.
FIG. 2 shows salt spray test results of heavy duty anticorrosive coatings of examples 1-3 of the present invention, in examples 1 and 3, rust spots appear at 1000h, wherein the rust spots of example 3 are small, and in example 2, only a small rust spot appears at the end of a scratch after 2000h exposure, which fully satisfies the requirements of heavy duty anticorrosion.
In conclusion, the graphene-polypyrrole composite heavy-duty anticorrosive coating and the preparation method thereof have the advantages that the preparation method of the heavy-duty anticorrosive coating is simple, the industrial production is easy to realize, the salt mist resistance effect of the prepared graphene-polypyrrole composite heavy-duty anticorrosive coating is good, and the heavy-duty anticorrosive use condition under the marine environment can be met.
Claims (11)
1. The graphene-polypyrrole composite heavy-duty anticorrosive paint is characterized by comprising the following components: cured epoxy resin, a graphene-polypyrrole composite material and zinc powder; wherein the mass ratio of the graphene-polypyrrole composite material to the cured epoxy resin is (0.3-0.8): 100, respectively; the mass ratio of the graphene-polypyrrole composite material to the zinc powder is (0.0075-0.03): 4.
2. the graphene-polypyrrole composite heavy-duty anticorrosive coating according to claim 1, wherein the mass ratio of graphene to polypyrrole in the graphene-polypyrrole composite material is (0.5-5): 1; the graphene is 1-10 layers of graphene; the conductivity of the polypyrrole is 1-15S/cm.
3. The graphene-polypyrrole composite heavy-duty anticorrosive coating according to claim 1, wherein the mass ratio of graphene to polypyrrole in the graphene-polypyrrole composite material is (0.5-2): 1; the graphene is single-layer graphene; the conductivity of the polypyrrole is 13-15S/cm.
4. The graphene-polypyrrole composite heavy-duty anticorrosive coating according to claim 1, wherein the cured epoxy resin is bisphenol a epoxy resin and polyamine curing agent, and the molar ratio of epoxy group to amino group is 1: (1-1.2) to complete curing.
5. The preparation method of the graphene-polypyrrole composite heavy-duty anticorrosive paint according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) mixing the graphene-polypyrrole composite material with a solvent to obtain a suspension; (2) adding the suspension into the cured epoxy resin, and uniformly stirring to obtain a mixture; (3) and adding zinc powder into the mixture, and stirring to uniformly mix the zinc powder and the mixture to obtain the graphene-polypyrrole composite heavy-duty anticorrosive paint.
6. The method according to claim 5, wherein the solvent is an organic solvent comprising: one or a mixture of more than two of ethanol, acetone, toluene, xylene or N-methyl pyrrolidone; the addition amount of the solvent is 0.1-2 ml: 10g of epoxy resin.
7. The method of claim 6, wherein the solvent is xylene.
8. The preparation method of claim 5, further comprising a preparation method of the graphene-polypyrrole composite material, comprising the following steps: uniformly mixing graphene and sodium dodecyl benzene sulfonate to obtain a solid mixture; adding pyrrole and hydrochloric acid into the solid mixture, and keeping the temperature at-5 to 10 ℃ to react for 0.5 to 5 hours; and adding ammonium persulfate into the reactant, and keeping the temperature of between 5 ℃ below zero and 10 ℃ for continuous reaction for 5 to 24 hours to obtain the graphene-polypyrrole composite material.
9. The preparation method according to claim 8, wherein the mass ratio of the graphene to the sodium dodecyl benzene sulfonate is (0.5-5): 1; the volume ratio of the pyrrole to the hydrochloric acid is 0.1:5, the concentration of the hydrochloric acid is 0.1-5 mol/L; the ratio of the mass of the graphene to the volume of the pyrrole is (0.5 g-2 g): 5 mL; the mass ratio of the ammonium persulfate to the volume of the pyrrole is (0.5 g-5 g): 1 mL.
10. The preparation method according to claim 8, wherein the mass ratio of the graphene to the sodium dodecyl benzene sulfonate is (0.5-2): 1; the volume ratio of the pyrrole to the hydrochloric acid is 0.1:5, the concentration of the hydrochloric acid is 1 mol/L; the ratio of the mass of the graphene to the volume of the pyrrole is 1 g: 5 mL; the mass ratio of the ammonium persulfate to the volume of the pyrrole is 1.2 g: 1 mL.
11. The preparation method according to claim 8, wherein in the step (1), the graphene and the sodium dodecyl benzene sulfonate are ultrasonically mixed in pure water, then the mixture is filtered to obtain a solid mixture, and the solid mixture is dried at 60-75 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112175478A (en) * | 2020-09-18 | 2021-01-05 | 上海船舶工艺研究所(中国船舶工业集团公司第十一研究所) | Trititanium dicarbonide-polypyrrole modified anticorrosive coating and preparation method thereof |
| CN114561118A (en) * | 2022-03-31 | 2022-05-31 | 哈尔滨工程大学 | Polypyrrole-coated graphene corrosion inhibitor container and preparation method thereof, and composite coating and application thereof |
| CN116676011A (en) * | 2023-06-01 | 2023-09-01 | 上海船舶工艺研究所(中国船舶集团有限公司第十一研究所) | Sustained-release cellulose-cuprous oxide antifouling agent and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112175478A (en) * | 2020-09-18 | 2021-01-05 | 上海船舶工艺研究所(中国船舶工业集团公司第十一研究所) | Trititanium dicarbonide-polypyrrole modified anticorrosive coating and preparation method thereof |
| CN112175478B (en) * | 2020-09-18 | 2022-03-15 | 上海船舶工艺研究所(中国船舶工业集团公司第十一研究所) | Trititanium dicarbonide-polypyrrole modified anticorrosive coating and preparation method thereof |
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Application publication date: 20200828 |