CN112662270A - Preparation method of modified graphene oxide epoxy composite anticorrosive paint - Google Patents
Preparation method of modified graphene oxide epoxy composite anticorrosive paint Download PDFInfo
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Abstract
The invention discloses a preparation method of a modified graphene oxide epoxy composite anticorrosive paint, which comprises the following specific steps: the method comprises the following steps: preparing graphite flakes, sodium nitrate, potassium permanganate, sulfuric acid, hydrochloric acid and hydrogen peroxide to prepare uniformly dispersed graphene oxide nanosheets; step two: adding graphene oxide nanosheets into ethanol, performing ultrasonic treatment to obtain a dispersion liquid, adding a small amount of chlorinated 1-butyl-3 methylimidazole solution, fully stirring, and filtering and washing to obtain a modified graphene oxide nanosheet dispersion; step three: adding the modified graphene oxide nanosheet dispersoid into epoxy resin, removing ethanol in an oven, adding a polyamine curing agent, and fully and uniformly stirring to obtain the modified graphene oxide epoxy composite anticorrosive paint. The modified graphene oxide epoxy composite anticorrosive paint prepared by the method has good corrosion resistance and strong adhesive force, and can be used for surface corrosion prevention of underground pipelines, military equipment, storage tanks and marine equipment.
Description
Technical Field
The invention provides a preparation method of a modified graphene oxide epoxy composite anticorrosive paint, and belongs to the technical field of anticorrosive paint preparation.
Background
Organic coatings are widely used on metal substrates and are one of the most practical and effective methods for protecting metal structures from corrosion. In various organic coatings, epoxy resin is used as an anticorrosive coating due to stable chemical properties, good corrosion resistance, strong adhesion, low curing shrinkage, high tensile strength and high bending strength, and is widely applied to the fields of underground pipelines, military equipment, storage tanks, marine equipment and the like. In addition to good corrosion resistance, the epoxy resin coating has a crack or micropore in the coating structure, and the barrier performance of the coating gradually decreases under the action of a long-term corrosive electrolyte, so that the metal surface is locally corroded. In addition, the presence of pores in the cured epoxy coating causes water and the like to penetrate into the epoxy metal interface, which causes corrosion of the metal substrate and delamination of the coating.
The graphene oxide nanosheet is a novel nano material developed in recent years, is composed of a quasi-two-dimensional honeycomb lattice of carbon atoms, has hydroxyl and epoxy functional groups on a basal plane and carbonyl and carboxyl on the edge, and has the advantages of sheet structure, high specific surface area, electrical insulation, excellent mechanical strength, barrier property to oxygen, water and corrosive ions and the like. The addition of the epoxy resin can enhance the barrier property of the epoxy coating, lead to the reduction of the porosity of the coating and improve the corrosion resistance of the epoxy resin coating.
The performance of epoxy coatings is improved by adding graphene oxide nanoplatelets, which must increase their interaction and compatibility with the polymer matrix, but due to strong van der waals forces between the flakes and their hydrophilicity, graphene oxide flakes tend to form large-sized aggregates in the polymer matrix.
Therefore, it is required to improve the interaction and compatibility of graphene oxide and polymer aggregate, reduce the agglomeration of graphene oxide in polymer, improve the dispersibility of graphene oxide, and enhance the corrosion resistance of epoxy coating.
Disclosure of Invention
1. In order to reduce the agglomeration of the graphene oxide in the polymer, improve the dispersibility of the graphene oxide and enhance the corrosion resistance of the epoxy coating. The invention provides a preparation method of a modified graphene oxide epoxy composite anticorrosive paint, which realizes the dispersion state of graphene oxide and the interface interaction between graphene oxide and an epoxy matrix and improves the anticorrosive performance of an epoxy coating.
2. The technical scheme of the invention is as follows:
firstly, preparing graphite flakes, sodium nitrate, potassium permanganate, sulfuric acid, hydrochloric acid and hydrogen peroxide to prepare uniformly dispersed graphene oxide nanosheets; secondly, adding graphene oxide nanosheets into ethanol, performing ultrasonic treatment to obtain a dispersion liquid, adding a small amount of 1-butyl-3 methylimidazole chloride solution, fully stirring, and filtering and washing to obtain a modified graphene oxide nanosheet dispersion; and finally, adding the modified graphene oxide nanosheet dispersoid into epoxy resin, removing ethanol in an oven, adding a polyamine curing agent, and fully and uniformly stirring to obtain the graphene oxide epoxy composite anticorrosive paint. The method comprises the following specific steps:
(1) preparing a graphene oxide nanosheet: placing 1g of graphite flakes and 1g of sodium nitrate into 20ml of 98% concentrated sulfuric acid, stirring for 1 hour in an ice bath, slowly adding 3g of potassium permanganate, controlling the temperature at 12 ℃, continuously stirring at 30 ℃ to form brown paste, then adding water for dilution, continuously stirring, adding 12ml of hydrogen peroxide solution for reaction until the color becomes yellow, finally rinsing with dilute hydrochloric acid for centrifugation, and then washing with deionized water to obtain the graphene oxide nanosheet.
(2) Preparing a modified graphene oxide nanosheet: weighing 10-20mg of the graphene oxide nanosheet prepared in the step (1), placing the graphene oxide nanosheet into 50ml of ethanol for ultrasonic dispersion for 30min, then adding 0-5ml of 1-butyl-3 methylimidazole chloride solution, fully stirring for 20h, filtering the solution, and washing with ethanol and deionized water to obtain the 1-butyl-3 methylimidazole chloride modified graphene oxide nanosheet.
(3) The preparation method of the modified graphene oxide epoxy composite anticorrosive paint comprises the following steps: adding the chlorinated 1-butyl-3 methylimidazole modified graphene oxide nanosheet prepared in the step (2) into epoxy resin, uniformly stirring, drying in an oven at 80 ℃ for 1h, taking out, adding a polyamine curing agent, fully stirring for 2h to obtain the modified graphene oxide epoxy composite anticorrosive paint, wherein the mass ratio of the epoxy resin to the polyamine curing agent is 2:1, and the total volume is 100 ml.
Advantageous effects
1. According to the invention, chlorinated 1-butyl-3 methylimidazole is used as a surfactant to improve graphene oxide nanosheets in the epoxy coating, and chlorinated 1-butyl-3 methylimidazole molecules can reduce the surface hydrophilicity of graphene oxide through the interaction of an ionic part and a hydrophobic part with the surface of the graphene oxide, so that the nanosheets and epoxy resin have better compatibility.
2. According to the invention, the positive charge part of chlorinated 1-butyl-3 methylimidazole can interact with the negative charge sites of graphene oxide nanosheets, and adsorption of chlorinated 1-butyl-3 methylimidazole on graphene oxide sheets is carried out through electrostatic attraction. The chlorinated 1-butyl-3 methylimidazole molecules on the graphene oxide flakes can prevent the graphene oxide flakes from agglomerating in the resin matrix, and the dispersion effect is promoted.
3. The graphene oxide epoxy composite anticorrosive coating prepared by the invention has a good application effect, the hydrophobicity of the graphene oxide modified by chlorinated 1-butyl-3 methylimidazole molecules is improved, the water-resisting effect of an epoxy coating can be further improved, the penetration of corrosive substances such as acid, alkali and salt is inhibited, and the corrosion resistance and the adhesive force of the coating are improved.
Drawings
FIG. 1 shows the results of the iron plate sprayed in example 1 after being left standing for 480 hours under the salt spray test conditions;
FIG. 2 shows the results of the iron pieces sprayed in example 2 after being left standing for 480 hours under the salt spray test conditions.
Detailed Description
The present invention is further illustrated by the following specific examples, which should not be construed as limiting the scope of the invention.
Example 1
Placing 1g of graphite flakes and 1g of sodium nitrate into 20ml of 98% concentrated sulfuric acid, stirring for 1 hour in an ice bath, slowly adding 3g of potassium permanganate, controlling the temperature at 12 ℃, continuously stirring at 30 ℃ to form brown paste, then adding water for dilution, continuously stirring, adding 12ml of hydrogen peroxide solution for reaction until the color becomes yellow, finally rinsing with dilute hydrochloric acid for centrifugation, and then washing with deionized water to obtain the graphene oxide nanosheet.
Weighing 10mg of the prepared graphene oxide nanosheet, placing the graphene oxide nanosheet into 50ml of ethanol for ultrasonic dispersion for 30min, then adding 1ml of 1-butyl-3-methylimidazole chloride solution, fully stirring for 20h, filtering the solution, and washing with ethanol and deionized water to obtain the 1-butyl-3-methylimidazole chloride modified graphene oxide nanosheet.
Adding the prepared chlorinated 1-butyl-3 methylimidazole modified graphene oxide nanosheet into epoxy resin, uniformly stirring, drying in an oven at 80 ℃ for 1h, taking out, adding a polyamine curing agent, fully stirring for 2h, wherein the mass ratio of the epoxy resin to the polyamine curing agent is 2:1, the total volume is 100ml, and obtaining the modified graphene oxide epoxy composite anticorrosive paint, and testing physical properties and electrochemical properties.
The anticorrosive paint obtained in example 1 was sprayed on an iron plate, and a salt spray test was performed using a 5% sodium chloride solution for 480 hours, and fig. 1 shows the result of the iron plate sprayed in example 1 after being left to stand for 480 hours under the salt spray test conditions. It can be seen from the figure that the iron sheet has no corrosion trace and coating peeling phenomenon, which indicates that the graphene oxide epoxy composite anticorrosive coating modified by 1-butyl-3 methylimidazole prepared in example 1 has good anticorrosive effect and adhesion.
EXAMPLE 2
Placing 1g of graphite flakes and 1g of sodium nitrate into 20ml of 98% concentrated sulfuric acid, stirring for 1 hour in an ice bath, slowly adding 3g of potassium permanganate, controlling the temperature at 12 ℃, continuously stirring at 30 ℃ to form brown paste, then adding water for dilution, continuously stirring, adding 12ml of hydrogen peroxide solution for reaction until the color becomes yellow, finally rinsing with dilute hydrochloric acid for centrifugation, and then washing with deionized water to obtain the graphene oxide nanosheet.
Weighing 15mg of the prepared graphene oxide nanosheet, placing the weighed graphene oxide nanosheet into 50ml of ethanol for ultrasonic dispersion for 30min, then adding 3ml of 1-butyl-3 methylimidazole chloride solution, fully stirring for 20h, filtering the solution, and washing with ethanol and deionized water to obtain the 1-butyl-3 methylimidazole chloride modified graphene oxide nanosheet.
Adding the prepared chlorinated 1-butyl-3 methylimidazole modified graphene oxide nanosheet into epoxy resin, uniformly stirring, drying in an oven at 80 ℃ for 1h, taking out, adding a polyamine curing agent, fully stirring for 2h, wherein the mass ratio of the epoxy resin to the polyamine curing agent is 2:1, the total volume is 100ml, and obtaining the modified graphene oxide epoxy composite anticorrosive paint, and testing physical properties and electrochemical properties.
Example 3
Placing 1g of graphite flakes and 1g of sodium nitrate into 20ml of 98% concentrated sulfuric acid, stirring for 1 hour in an ice bath, slowly adding 3g of potassium permanganate, controlling the temperature at 12 ℃, continuously stirring at 30 ℃ to form brown paste, then adding water for dilution, continuously stirring, adding 12ml of hydrogen peroxide solution for reaction until the color becomes yellow, finally rinsing with dilute hydrochloric acid for centrifugation, and then washing with deionized water to obtain the graphene oxide nanosheet.
Weighing 20mg of the prepared graphene oxide nanosheet, placing the weighed graphene oxide nanosheet into 50ml of ethanol for ultrasonic dispersion for 30min, then adding 5ml of 1-butyl-3 methylimidazole chloride solution, fully stirring for 20h, filtering the solution, and washing the solution with ethanol and deionized water to obtain the 1-butyl-3 methylimidazole chloride modified graphene oxide nanosheet.
Adding the prepared chlorinated 1-butyl-3 methylimidazole modified graphene oxide nanosheet into epoxy resin, uniformly stirring, drying in an oven at 80 ℃ for 1h, taking out, adding a polyamine curing agent, fully stirring for 2h, wherein the mass ratio of the epoxy resin to the polyamine curing agent is 2:1, the total volume is 100ml, and obtaining the modified graphene oxide epoxy composite anticorrosive paint, and testing physical properties and electrochemical properties.
Comparative example 1
In order to further illustrate the beneficial effects produced by the present invention, in this embodiment, graphene oxide is modified without adding chlorinated 1-butyl-3 methylimidazole, and the prepared graphene oxide nanosheet is directly added to epoxy resin and a polyamine curing agent, and the specific steps are as follows:
placing 1g of graphite flakes and 1g of sodium nitrate into 20ml of 98% concentrated sulfuric acid, stirring for 1 hour in an ice bath, slowly adding 3g of potassium permanganate, controlling the temperature at 12 ℃, continuously stirring at 30 ℃ to form brown paste, then adding water for dilution, continuously stirring, adding 12ml of hydrogen peroxide solution for reaction until the color becomes yellow, finally rinsing with dilute hydrochloric acid for centrifugation, and then washing with deionized water to obtain the graphene oxide nanosheet.
Adding the prepared graphene oxide nanosheets into epoxy resin, uniformly stirring, drying in an oven at 80 ℃ for 1h, taking out, adding a polyamine curing agent, wherein the mass ratio of the epoxy resin to the polyamine curing agent is 2:1, the total volume is 100ml, and fully stirring for 2h to obtain the graphene oxide epoxy composite anticorrosive paint and testing the physical properties and the electrochemical properties of the graphene oxide epoxy composite anticorrosive paint.
The anticorrosive paint obtained in the comparative example 1 was sprayed on an iron plate, a salt spray test was performed using a 5% sodium chloride solution for 480 hours, and fig. 2 shows the results of the iron plate sprayed in the comparative example 1 after being left to stand for 480 hours under the salt spray test conditions. From the figure, it can be seen that the iron sheet sprayed in comparative example 1 has corrosion traces and coating peeling phenomena, which indicates that the prepared graphene oxide epoxy composite anticorrosive coating without 1-butyl-3 methylimidazole has poor anticorrosive performance and adhesion.
Table 1 shows the physical properties and electrochemical properties of examples 1 to 3 and comparative example 1, and it can be seen that the anticorrosive coating prepared by the present invention has good mechanical properties, corrosion resistance and electrochemical properties, and can prolong the coating life and better protect the coated equipment.
Table 1 shows the physical and electrochemical properties of examples 1 to 3 and comparative example 1
Claims (5)
1. A preparation method of a modified graphene oxide epoxy composite anticorrosive paint is characterized in that the prepared graphene oxide epoxy composite anticorrosive paint has good corrosion resistance, and comprises the following specific steps:
the method comprises the following steps: preparing graphite flakes, sodium nitrate, potassium permanganate, sulfuric acid, hydrochloric acid and hydrogen peroxide to prepare uniformly dispersed graphene oxide nanosheets;
step two: adding graphene oxide nanosheets into ethanol, performing ultrasonic treatment to obtain a dispersion liquid, adding a small amount of chlorinated 1-butyl-3 methylimidazole solution, fully stirring, and filtering and washing to obtain a modified graphene oxide nanosheet dispersion;
step three: adding the modified graphene oxide nanosheet dispersoid into epoxy resin, removing ethanol in an oven, adding a polyamine curing agent, and fully and uniformly stirring to obtain the modified graphene oxide epoxy composite anticorrosive paint.
2. The preparation method of the modified graphene oxide epoxy composite anticorrosive paint as claimed in claim 1, wherein in the first step, 1g of graphite flakes and 1g of sodium nitrate are placed into 20ml of 98% concentrated sulfuric acid to be stirred for 1 hour in an ice bath, then 3g of potassium permanganate is slowly added, the temperature is controlled at 12 ℃, then the mixture is continuously stirred at 30 ℃ to form brown paste, then water is added to dilute the mixture and the mixture is continuously stirred, 12ml of hydrogen peroxide solution is added to react until the mixture becomes yellow, finally diluted hydrochloric acid is used for rinsing and centrifuging, and the mixture is washed by deionized water to obtain the graphene oxide nanosheets.
3. The preparation method of the modified graphene oxide epoxy composite anticorrosive paint according to claim 1, characterized in that, in the second step, 10-20mg of the prepared graphene oxide nanosheets are weighed and placed into 50ml of ethanol for ultrasonic dispersion for 30min, then 1-5 ml of 1-butyl-3 methylimidazole chloride solution is added and fully stirred for 20h, and then the solution is filtered and washed with ethanol and deionized water to obtain 1-butyl-3 methylimidazole chloride modified graphene oxide nanosheets.
4. The preparation method of the modified graphene oxide epoxy composite anticorrosive paint according to claim 1, characterized in that in the third step, 1-butyl-3 methylimidazole chloride modified graphene oxide nanosheets are added into epoxy resin, uniformly stirred and placed into an oven at 80 ℃ for drying for 1 hour, then taken out and added with polyamine curing agent, the mass ratio of the epoxy resin to the polyamine curing agent is 2:1, the total volume is 100ml, and then fully stirred for 2 hours, so as to obtain the modified graphene oxide epoxy composite anticorrosive paint.
5. The modified graphene oxide epoxy composite anticorrosive paint prepared by the preparation method according to claim 1 is characterized by being used for surface anticorrosion of underground pipelines, military equipment, storage tanks and marine equipment.
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| ES2893957A1 (en) * | 2021-06-14 | 2022-02-10 | Centro De Investig Energeticas Medioambientales Y Tecnologicas Ciemat | Procedure for obtaining anti-corrosion coatings of reduced graphene oxide and use of these (Machine-translation by Google Translate, not legally binding) |
| CN116200067A (en) * | 2023-02-13 | 2023-06-02 | 山东京博装备制造安装有限公司 | Graphene filler for anti-corrosion coating of earthing storage tank and preparation process |
| CN117186519A (en) * | 2023-10-08 | 2023-12-08 | 江门市格雷亚特流体密封技术有限公司 | Sealing rubber material for petroleum casing pipe and preparation method thereof |
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Application publication date: 20210416 |