CN115746689A - Bionic self-repairing, antifouling and anticorrosion multifunctional coating and preparation method thereof - Google Patents
Bionic self-repairing, antifouling and anticorrosion multifunctional coating and preparation method thereof Download PDFInfo
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Abstract
The invention provides a bionic self-repairing, antifouling and anticorrosive multifunctional coating and a preparation method thereof, which mainly aim at the problem that the existing self-repairing polymer has poor mechanical properties due to high chain segment mobility and cannot be used in a complex and variable marine environment. The introduced graphene can absorb near infrared light and convert the near infrared light into heat energy, and the temperature of the composite material is increased, so that a photo-thermal self-healing function is realized, the graphene has strong barrier property, corrosion factors in the sea can be effectively prevented from permeating into the coating, and the corrosion resistance of the composite material is improved. Meanwhile, the introduced antifouling agent can be used for preparing coatings with various functions of photo-thermal self-healing, antifouling and corrosion prevention.
Description
Technical Field
The invention belongs to the technical field of bionic materials.
Background
With the wide application of large cargo ships, marine corrosion and biological pollution have become major problems restricting the development of marine resources. According to research, corrosion problems consume 4% of the global GDP annually, with microbial corrosion accounting for approximately 50%. The preparation of the comprehensive antifouling and anticorrosive paint (IAAC) is one of effective technical means for solving marine corrosion and biological pollution, and is widely concerned by numerous scholars. However, IAACs are often affected by marine sediments, causing them to be damaged. Eventually, the IAAC will lose its anti-fouling and anti-corrosion functions, affecting its service life. Inspired by dynamic chemical bonds, the introduction of the dynamic chemical bonds into the coating system can realize the self-healing of the coating, which provides possibility for designing IAACs with self-healing function. However, due to the high segment mobility of the self-repairing polymer, the mechanical properties of the self-repairing polymer are poor, and the self-repairing polymer cannot be used in a complex and variable marine environment. Animal cartilage tissue has high mechanical strength and self-healing ability after injury. Cartilage tissue of animals consists of collagen cells and intercellular collagen fibers. The side chains of proteoglycan molecules in the cartilage matrix are connected with collagen fibers through hydrogen bonds to form a net structure, and a large number of collagen fibers are interwoven into a net to bear high acting force. Thus, the layered fibrous structure with strong supramolecular interactions imparts strong mechanical strength and toughness to the cartilage tissue. Inspired by this, an effective strategy to prepare IAACs with high strength mechanical and self-healing properties is to add a layered fibrous material in the coating that is non-covalently or chemically cross-linked with the polymer molecules.
Disclosure of Invention
Aiming at the phenomena, the invention provides a bionic self-repairing, antifouling and anticorrosive multifunctional coating and a preparation method thereof. The introduced graphene can absorb near infrared light and convert the near infrared light into heat energy, and the temperature of the composite material is increased, so that a photo-thermal self-healing function is realized, the graphene has strong barrier property, corrosion factors in the sea can be effectively prevented from permeating into the coating, and the corrosion resistance of the composite material is improved. Meanwhile, the introduced anti-fouling agent can be used for preparing coatings with multiple functions of photo-thermal self-healing, anti-fouling and corrosion prevention.
The invention discloses a preparation method of a bionic self-repairing, antifouling and anticorrosive multifunctional coating, which comprises the following specific steps:
1) Adding reduced graphene oxide (rGO) into Dimethylformamide (DMF), ultrasonically mixing for 1 hour, pouring into a reaction container, adding isophorone diisocyanate (IPDI), reacting for 12 hours under a nitrogen atmosphere, and centrifuging to obtain a mixture after the reaction is finished; and ultrasonically cleaning the mixture for 3 times by using butyl acetate, and finally drying the cleaned product in a vacuum drying furnace at 60 ℃ for 24 hours to obtain the functionally reduced graphene oxide (FrGO).
The ratio of the reduced graphene oxide to the dimethylformamide is that 2mg of the reduced graphene oxide is added into every 0.5-2mL of the dimethylformamide; the mass ratio of the reduced graphene oxide to the isophorone diisocyanate is 1 (1-10).
2) Pouring isophorone diisocyanate into another reaction container, heating to 50 ℃, introducing nitrogen, adding polytetrahydrofuran ether glycol (PTMG) into the reaction container at the speed of 0.2mL per second, reacting at 50 ℃ for 30 minutes after dropwise adding is completed, then heating to 80 ℃, reacting for 3 hours to obtain a polyurethane prepolymer, bottling and sealing the polyurethane prepolymer, cooling to room temperature, and storing; the mass ratio of the isophorone diisocyanate to the polytetrahydrofuran ether glycol is 0.92
3) Weighing the polyurethane prepolymer and ethyl acetate according to the mass ratio of the polyurethane prepolymer to the ethyl acetate of 1 (0.6-2), pouring the weighed polyurethane prepolymer and the ethyl acetate into a beaker, adding the functionally reduced graphene oxide, and mixing and ultrasonically dispersing for 1 hour to obtain a polyurethane prepolymer mixed solution; adding an antifouling agent 2-methyl-4-isothiazoline-3-ketone (MIT) and a chain extender 2-hydroxyethyl disulfide (HEDS) into dimethylformamide, and completely dissolving to obtain a chain extender and antifouling agent mixed solution; adding the chain extender anti-fouling agent mixed solution into the polyurethane prepolymer mixed solution, and adding an ethyl acetate solvent for dilution to enable the solute to account for 20-50% of the solution by mass; then stirring for 2 hours at 60 ℃ to finish the reaction, and obtaining the coating for preparing the bionic self-repairing, antifouling and anticorrosive multifunctional coating;
4) And (3) after the coating is coated on the surface of a metal substrate, curing for 24 hours in a vacuum furnace at the temperature of 80 ℃ to obtain the bionic self-repairing, antifouling and anticorrosive multifunctional coating.
The mass ratio of the functional reduced graphene oxide to the polyurethane prepolymer is (0.05-0.15) to 1; the mass ratio of the polyurethane prepolymer to the chain extender 2-hydroxyethyl disulfide is (4.0-4.2) to 1; the antifouling agent 2-methyl-4-isothiazoline-3-ketone accounts for 0.1 to 10 weight percent of the mass of the whole polyurethane coating; the ratio of the total mass of 2-methyl-4-isothiazolin-3-one and 2-hydroxyethyl disulfide to the mass of DMF is 1 (0.5-1.5).
Preferably, the preparation process of the reduced graphene oxide in the invention is as follows:
1) Dispersing 1mg of Graphene Oxide (GO) in deionized water according to the proportion of adding 1mg of GO in every 0.8-1.2mL of deionized water, and carrying out ultrasonic treatment for 1h to obtain a graphene oxide dispersion liquid;
2) Adding hydrazine hydrate into the graphene oxide dispersion liquid, and stirring for 24 hours at 100 ℃; the proportion of hydrazine hydrate to graphene oxide is that 0.8-1.2mL of hydrazine hydrate is added into every 100mg of graphene;
3) Filtering the obtained mixture obtained in the step 2) and washing with ethanol and deionized water, and drying the separated black solid by freeze-drying to obtain reduced graphene oxide;
preferably, in step 2), PTMG is poured into a rotary bottle of a rotary evaporator in preparation of the polyurethane prepolymer, and then distilled under vacuum at 120 ℃ for 2 hours, and after cooling to 60 ℃, the solution is bottled and sealed for storage.
The metal substrate comprises: alloys of one or more of iron, copper, steel, magnesium, titanium, aluminum.
The invention has the beneficial effects that:
the raw materials used by the method are IPDI (isophorone diisocyanate), PTMG-850 (polytetrahydrofuran ether glycol, molecular weight 850), HEDS (2-hydroxyethyl disulfide), MIT (2-methyl-4-isothiazoline-3-ketone) and graphene oxide, and the used solvents are ethyl acetate and DMF; the raw materials are common raw materials in the market, are low in price, and the synthesis method is simple and can be synthesized on a large scale.
The coating provided by the invention has the functions of antibiosis, antifouling and self-repairing, and also has super-strong mechanical properties after cutting off and self-repairing.
Drawings
FIG. 1 is a graph showing the antibacterial ability of a coating layer measured by a plate coating method of comparative example bacteria
FIG. 2 is a graph showing the antibacterial ability of the coating layer measured by the plate coating method of bacteria according to the example
FIG. 3 is a photograph showing the area (nearly 100%) of the green algae adhered to the surface of the comparative example coating
FIG. 4 is a photograph showing the area (approximately 10%) of the adhered green algae on the surface of the coating layer of the example
FIG. 5 shows the corrosion resistance of a coating of a comparative example
FIG. 6 shows the corrosion resistance of the example coating
FIG. 7 is a photograph after fracture of comparative examples and after 5min of irradiation with near infrared light
FIG. 8 is a photograph of a mechanical property test performed after cutting-off and near-infrared illumination self-repairing performed by an embodiment of the present invention
FIG. 9 shows the tensile properties of comparative examples and examples.
Detailed Description
The technical solution of the invention is further explained and illustrated in the form of specific embodiments.
Examples
300mg GO was dispersed in 300mL deionized water and sonicated for 1h. Subsequently, 3mL of hydrazine hydrate was added to the GO dispersion and stirred at 100 ℃ for 24h. The resulting mixture was filtered and washed several times with ethanol and deionized water. Finally, the isolated black solid was dried by lyophilization to obtain reduced graphene oxide rGO.
200mg rGO and 100ml DMF were mixed by sonication for 1 hour. The mixture was then poured into a four-necked flask and 2g of IPDI was added. The reaction was carried out under a nitrogen atmosphere for 12 hours. After completion of the reaction, a mixture was obtained by centrifugation. And ultrasonically cleaning the mixture for 3 times by using butyl acetate, and finally drying the cleaned product in a vacuum drying furnace at 60 ℃ for 24 hours to obtain FrGO.
Before the prepolymer synthesis, PTMG-850 was first poured into a rotary bottle of a rotary evaporator and then distilled under vacuum at 120 ℃ for 2 hours. After cooling to 60 ℃, it is bottled and stored sealed.
60g of the IPDI solution was poured into a four-necked flask, heated to 50 ℃ and passed through nitrogen, 65g of PTMG-850 was poured into a constant pressure dropping funnel, and dropped into the four-necked flask at a rate of 0.2mL per second. The reaction was carried out at 50 ℃ for 30 minutes. The temperature was then raised to 80 ℃ and the reaction was continued for 3 hours. The prepolymer was bottled and sealed, cooled to room temperature and stored.
2.5g of prepolymer and 5g of butyl acetate solvent were poured into a beaker and 310mg of FrGO was added. The mixture was ultrasonically dispersed for 1 hour. Then, 0.155g of MIT and 0.6g of HEDS were added to 0.755g of DMF and completely dissolved, and then added to the above mixture. The mixture was stirred at 60 ℃ for 2 hours.
Then added to the mixture and 4.58g of ethyl acetate was added so that the solute accounted for approximately 30% of the solution mass. The mixture was finally cured in a vacuum oven at 80 ℃ for 24 hours.
Comparative example:
before prepolymer synthesis, PTMG was first poured into a rotary bottle of a rotary evaporator and then distilled under vacuum at 120 ℃ for 2 hours. After cooling to 60 ℃, it is bottled and stored hermetically.
60g of the IPDI solution was poured into a four-necked flask, heated to 50 ℃ and passed through nitrogen, and 65g of PTMG was poured into a constant pressure dropping funnel and dropped into the four-necked flask at a rate of 4 drops per second. The reaction was carried out at 50 ℃ for 30 minutes. The temperature was then raised to 80 ℃ and the reaction was continued for 3 hours. The prepolymer was bottled and sealed, cooled to room temperature and stored.
2.5g of the prepolymer solution and 5g of butyl acetate solvent were poured into a beaker and 310mg of FrGO was added. Then, 0.6g of HEDS was added to 0.755g of DMF and completely dissolved, followed by addition to the above mixture. The mixture was stirred at 60 ℃ for 2 hours.
Then added to the mixture and 4.58g of ethyl acetate was added so that the solute was close to 30% by mass of the solution. The mixture was finally cured in a vacuum oven at 80 ℃ for 24 hours.
Effect verification
As can be seen from the comparison between FIG. 1 and FIG. 2, the method of the present invention has good antibacterial and antifouling effects, FIG. 3 is a photograph of the green algae attached to the surface of the comparative example coating, and the experimental method is as follows: chlorella was cultured in F/2 medium at 25 ℃ for 14 h with light and dark (L/D) cycles. At the same time, all coatings should be sterilized under UV light for 2 hours before testing. When the chlorella cell count was 1000000/mL, the coating (10 mm by 10 mm) was immersed in 40mL of algae solution. After 30 days of incubation, the coating was removed and washed, and then photographed with an electron microscope. The adhesion area is close to 100%, and the adhesion area of the green algae on the surface of the coating of the embodiment (figure 4) is only close to 10%, which also proves that the invention has good antibacterial and antifouling effects.
Fig. 5 and 6 show the corrosion resistance of the coatings of the comparative example and the example, respectively. The higher the impedance modulus value in the low frequency region (0.01 Hz), the stronger the corrosion resistance of the coating. As can be seen in FIG. 5, the | Z Yof the comparative example coating 0.01Hz Decay rapidly with immersion time, from 2.78 x 10 at 1 day of immersion 8 Ω·cm 2 Decay to 5.56 x 10 at 15 days of immersion 5 Ω·cm 2 . Most excellent are example coatings with | Z tint 0.01Hz 2.18 x 10 from 1 day of soaking 9 Ω·cm 2 Reduced to 3.34 x 10 at 15 days of immersion 8 Ω·cm 2 。
FIG. 7 is a photograph of the comparative example and the example after the comparative example and the example are broken and irradiated with near infrared light for 5min, in which the crack does not disappear, indicating that the self-repairing function is not provided, and in the present invention, the crack disappears and has the self-repairing function; FIG. 8 is a photograph of a mechanical property test performed after cutting-off and near-infrared illumination self-repair performed according to an embodiment of the present invention. After cutting and self-repairing, the size of the cross section is about 10mm 0.5mm (60mm 10mm 0.5 mm), and the cross section can bear at least 3kg without fracture, which indicates that the material has super-strong mechanical properties. FIG. 9 illustrates that the invention has good tensile properties, reaching 40MPa.
Claims (6)
1. A preparation method of a bionic self-repairing, antifouling and anticorrosive multifunctional coating is characterized by comprising the following specific steps:
1) Adding reduced graphene oxide into dimethylformamide, ultrasonically mixing for 1 hour, pouring into a reaction container, adding isophorone diisocyanate, reacting for 12 hours under the nitrogen atmosphere, and centrifuging to obtain a mixture after the reaction is finished; ultrasonically cleaning the mixture for 3 times by using butyl acetate, and finally drying the cleaned product in a vacuum drying furnace at 60 ℃ for 24 hours to obtain functionally reduced graphene oxide;
the ratio of the reduced graphene oxide to the dimethylformamide is that 2mg of the reduced graphene oxide is added into every 0.5-2mL of the dimethylformamide; the mass ratio of the reduced graphene oxide to the isophorone diisocyanate is 1 (1-10);
2) Pouring isophorone diisocyanate into another reaction container, heating to 50 ℃, introducing nitrogen, adding polytetrahydrofuran ether glycol into the reaction container at the speed of 0.2mL per second, reacting at 50 ℃ for 30 minutes after dropwise addition is completed, then heating to 80 ℃, reacting for 3 hours to obtain a polyurethane prepolymer, bottling and sealing the polyurethane prepolymer, cooling to room temperature, and storing; the mass ratio of the isophorone diisocyanate to the polytetrahydrofuran ether glycol is 0.92; the molecular weight of the polytetrahydrofuran ether glycol is 850;
3) Weighing the polyurethane prepolymer and ethyl acetate according to the mass ratio of the polyurethane prepolymer to the ethyl acetate of 1 (0.6-2), pouring the weighed polyurethane prepolymer and the ethyl acetate into a beaker, adding the functionally reduced graphene oxide, and mixing and ultrasonically dispersing for 1 hour to obtain a polyurethane prepolymer mixed solution; adding an antifouling agent 2-methyl-4-isothiazoline-3-ketone and a chain extender 2-hydroxyethyl disulfide into dimethylformamide, and completely dissolving to obtain a chain extender antifouling agent mixed solution; adding the chain extender anti-fouling agent mixed solution into the polyurethane prepolymer mixed solution, and adding an ethyl acetate solvent for dilution to enable the solute to account for 20-50% of the solution by mass; then stirring for 2 hours at 60 ℃ to finish the reaction, and obtaining the multifunctional coating for preparing the bionic self-repairing, antifouling and anticorrosion coating;
the mass ratio of the functional reduced graphene oxide to the polyurethane prepolymer is (0.05-0.15) to 1; the mass ratio of the polyurethane prepolymer to the chain extender 2-hydroxyethyl disulfide is (4.0-4.2) to 1; the antifouling agent 2-methyl-4-isothiazoline-3-ketone accounts for 0.1 to 10 weight percent of the whole polyurethane coating; the ratio of the total mass of 2-methyl-4-isothiazolin-3-one and 2-hydroxyethyl disulfide to the mass of dimethylformamide is 1 (0.5-1.5).
2. The preparation method of the bionic self-repairing, antifouling and anticorrosive multifunctional coating as claimed in claim 1, wherein the preparation process of the reduced graphene oxide is as follows:
1) Dispersing GO in deionized water according to the proportion that 1mg of graphene oxide is added into every 0.8-1.2mL of deionized water, and carrying out ultrasonic treatment for 1h to obtain a graphene oxide dispersion liquid;
2) Adding hydrazine hydrate into the graphene oxide dispersion liquid, and stirring for 24 hours at 100 ℃; the ratio of hydrazine hydrate to graphene oxide is that 0.8-1.2mL of hydrazine hydrate is added into each 100mg of graphene;
3) Filtering the mixture obtained in step 2) and washing with ethanol and deionized water, and drying the separated black solid by freeze-drying to obtain reduced graphene oxide.
3. The preparation method of the bionic self-repairing, antifouling and anticorrosion multifunctional coating material as claimed in claim 1, wherein in step 2), before the preparation of the polyurethane prepolymer, PTMG is poured into a rotary bottle of a rotary evaporator, and then the PTMG is distilled under vacuum at 120 ℃ for 2 hours, and after the PTMG is cooled to 60 ℃, the PTMG is bottled and sealed for storage.
4. The bionic self-repairing, anti-fouling and anti-corrosion multifunctional coating prepared by the method according to any one of claims 1 to 3.
5. A method for preparing a bionic self-repairing, antifouling and anticorrosion multifunctional coating by using the coating as claimed in claim 4 comprises the following specific steps: after the coating is coated on the surface of a metal substrate, curing the coating for 24 hours in a vacuum furnace at the temperature of 80 ℃ to obtain the bionic self-repairing, antifouling and anticorrosive multifunctional coating; the metal substrate comprises: alloys of one or more of iron, copper, steel, magnesium, titanium, aluminum.
6. The bionic self-repairing, anti-fouling and anti-corrosion multifunctional coating prepared by the method according to claim 5.
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| CN116218345A (en) * | 2023-04-19 | 2023-06-06 | 中国海洋大学 | Preparation method and application of photo-thermal nano heterojunction and self-repairing anticorrosive paint thereof |
| CN116355514A (en) * | 2023-04-14 | 2023-06-30 | 吉林大学 | Coating with antifouling, anticorrosion and bionic self-healing functions and preparation method thereof |
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| CN116355514B (en) * | 2023-04-14 | 2024-02-02 | 吉林大学 | Coating with antifouling, anticorrosion and bionic self-healing functions and preparation method thereof |
| CN116218345A (en) * | 2023-04-19 | 2023-06-06 | 中国海洋大学 | Preparation method and application of photo-thermal nano heterojunction and self-repairing anticorrosive paint thereof |
| CN116218345B (en) * | 2023-04-19 | 2024-04-26 | 中国海洋大学 | Preparation method and application of photo-thermal nano heterojunction and self-repairing anticorrosive paint thereof |
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