CN115926522A - Polyaniline-carbon nitride compound, resin composite coating and preparation method thereof - Google Patents
Polyaniline-carbon nitride compound, resin composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polyaniline-carbon nitride compound, a resin composite coating and a preparation method thereof, wherein the polyaniline-carbon nitride compound takes polyaniline as a coating layer and flaky carbon nitride as a carrier, and the mass ratio of the polyaniline to the carbon nitride is 5-15; the resin composite coating is doped with polyaniline-carbon nitride compound, and the doping amount of the polyaniline-carbon nitride compound is 0.1-0.5% of the mass of the composite resin; the polyaniline modified carbon nitride effectively improves the defects of the original carbon nitride, improves the light absorption performance and improves the charge separation efficiency; the polyaniline-carbon nitride compound is introduced into the resin material, and the synergistic effect of the polyaniline-carbon nitride compound not only improves the corrosion resistance of the original resin coating, but also endows the numerical composite coating with anti-biofouling characteristic, and has extremely high application value in the aspects of corrosion resistance and anti-biofouling.
Description
Technical Field
The invention relates to a polyaniline-carbon nitride compound, and also relates to a resin composite coating containing the polyaniline-carbon nitride compound and a preparation method thereof.
Background
Carbon steel is an important metal material, is widely applied to various industries such as ship equipment and offshore infrastructure equipment, is easily attached by plankton, accelerates corrosion to influence the actual performance of the equipment, and causes a great amount of economic loss and safety problems. Epoxy (EP) coatings are widely used in marine environment for corrosion resistance studies due to their remarkable chemical inertness, electrical isolation and strong adhesion, but the micro-porosity and the defects caused by solvent evaporation during curing make the coatings unable to provide long-term protection.
The prior art has introduced two-dimensional materials into the resin to improve the corrosion resistance of the coating, wherein polymeric Carbon Nitride (CN) is a candidate material for corrosion resistance due to its ease of manufacture, low cost, non-toxicity and outstanding stability. However, its rapid carrier recombination, poor specific surface area and weak visible light absorption range, exposes active sites, is prone to reduction reactions, limits the activity of carbon nitride and its application in bonding resins for corrosion protection.
Disclosure of Invention
The purpose of the invention is as follows: one object of the present invention is to provide a polyaniline-carbon nitride composite capable of improving corrosion resistance and biofouling resistance of a resin coating, and another object of the present invention is to provide a resin composite coating containing the above polyaniline-carbon nitride composite and a method for preparing the same.
The technical scheme is as follows: according to the polyaniline-carbon nitride compound, in the polyaniline-carbon nitride compound, polyaniline is used as a coating layer, flaky carbon nitride is used as a carrier, and the mass ratio of the polyaniline to the carbon nitride is 5-15.
Wherein, the resin composite coating containing the polyaniline-carbon nitride composite is doped with the polyaniline-carbon nitride composite; the doping amount of the polyaniline-carbon nitride compound is 0.1-0.5% of the mass of the composite resin.
Preferably, the composite resin is a mixture of epoxy resin and polyamide resin, and the mass ratio of the epoxy resin to the polyamide resin is 1-4.
The preparation method of the resin composite coating comprises the following steps:
(1) Synthesizing carbon nitride by thermal polymerization: calcining urea and carrying out thermal polycondensation to obtain sheet carbon nitride;
(2) Preparing a polyaniline-carbon nitride compound: uniformly mixing the flaky carbon nitride prepared in the step (1) with polyaniline, and calcining to form a polyaniline-carbon nitride compound;
(3) Preparing the polyaniline-carbon nitride-resin composite coating: and (3) dispersing the polyaniline-carbon nitride compound prepared in the step (2) in an organic solvent, performing ultrasonic treatment to obtain a uniform dispersion, mixing epoxy resin and polyamide resin, and stirring to obtain the polyaniline-carbon nitride-resin composite coating.
Preferably, in the step (1), the calcination is carried out at a temperature rise rate of 3-5 ℃/min, a heat preservation temperature of 500-550 ℃ and a heat preservation time of 1.5-3 h.
Preferably, in the step (2), the mass ratio of the polyaniline to the carbon nitride is 5 to 15%.
Preferably, in the step (2), the calcination is carried out at a temperature rise rate of 3-5 ℃/min, a heat preservation temperature of 270-300 ℃ and a heat preservation time of 1.5-2 h.
Preferably, in the step (3), the mass ratio of the polyaniline-carbon nitride composite to the organic solvent is 1.
Preferably, in the step (3), the ultrasonic time is 0.5-1 h; the stirring speed is 800-1200 r/min, and the stirring time is 0.5-2 h.
Preferably, the polyaniline-carbon nitride-resin composite coating is coated on the surface of a carbon steel matrix by using a spin coater to form a composite coating with the thickness of 50-150 mu m.
Preferably, the coating is specifically performed by firstly performing low-speed spin coating for 1-2 min at a rotating speed of 300-600 r/min and then performing high-speed spin coating for 3-5 min at a rotating speed of 1200-1500 r/min.
The invention principle is as follows: according to the invention, the polyaniline-carbon nitride compound is obtained by low-temperature polymerization by using the flaky carbon nitride as a carrier and the polyaniline as a coating layer, the polyaniline is used as a black material, so that the polyaniline has excellent light absorption capability, the carbon nitride has a good lamellar structure, and can be effectively dispersed in the coating, so that a good shielding effect is provided, the path of corrosive ions reaching the metal matrix is prolonged, and the corrosion resistance of the metal matrix is improved. The polyaniline modified carbon nitride provides photo-generated electrons and free radicals, so that the defects of the original carbon nitride, such as weak light absorption capacity, easy recombination of photo-generated carriers and the like, are effectively improved, and the light absorption performance and the charge separation efficiency of the carbon nitride can be effectively improved by compounding the carbon nitride with the polyaniline; meanwhile, polyaniline is rich in a large amount of positive nitrogen ions, and free radicals generated by carbon nitride can promote polyaniline to be combined with negative ions in algae cell walls, so that the structure of the cell walls is damaged, the algae cells are further killed, and the purpose of resisting biological fouling is achieved.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages:
(1) The resin composite coating containing the polyaniline-carbon nitride composite has excellent corrosion resistance, and the EIS impedance radius of the coating formed by coating the coating on the surface of a carbon steel substrate is 1.62 multiplied by 10 10 Ω·cm 2 Corrosion current of 1.05X 10 -10 A·cm -2 Compared with other coatings, the EIS impedance of the coating is improved by 2 to 3 orders of magnitude; through a 60-day corrosion immersion experiment, no corrosion point still appears on the surface of the coating, and the corrosion resistance is durable and stable;
(2) The resin composite coating has extremely strong anti-biological fouling performance, and only a small amount of algae attachments exist on the surface of the coating after 60-day immersion experiments, and the attachment area is reduced by 95 percent compared with the similar coatings in the prior art.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) of PANI @ CN-10 and CN in examples and comparative examples; wherein Panel a is a PANI @ CN-10 Scanning Electron Microscope (SEM) of example 1 and Panel b is a Scanning Electron Microscope (SEM) of comparative example CN;
FIG. 2 is an X-ray diffraction (XRD) pattern of PANI @ CN-10 and PANI @ CN-5, PANI @ CN-10, CN of examples and comparative examples;
FIG. 3 is Fourier infrared transform (FT-IR) spectra of examples and comparative examples PANI @ CN-10 and PANI @ CN-5, PANI @ CN-10, CN;
FIG. 4 is X-ray photoelectron spectroscopy (XPS) spectra of PANI @ CN-10 and CN in examples and comparative examples;
FIG. 5 is a high resolution X-ray photoelectron spectroscopy (XPS) spectra of PANI @ CN-10 and CN in examples and comparative examples;
FIG. 6 is a representation of the photoelectrochemical properties of examples and comparative examples PANI @ CN-10 and PANI @ CN-5, PANI @ CN-10, CN; wherein (a) is solid ultraviolet (UV-vis) absorption spectrum, (b) is fluorescence (PL) spectrum, (c) is transient photocurrent response, and (d) is Nyquist plot of impedance;
FIG. 7 is spin-capture ESR spectra of PANI @ CN-10 and CN in examples and comparative examples; wherein (a) is hydroxyl radical trapping spectrum, and (b) is superoxide radical trapping spectrum;
FIG. 8 is an EIS profile analysis of examples and comparative examples PANI @ CN-10/EP and EP, CN/EP, PANI @ CN-5/EP, PANI @ CN-20/EP; wherein (a) is a Nyquist plot over 1-day immersion experiment, (b) is a Bode plot over 1-day immersion experiment, (c) is a Bode phase angle plot over 1-day immersion experiment, (d) is a Nyquist plot over 60-day immersion experiment, (e) is a Bode plot over 60-day immersion experiment, and (f) is a Bode phase angle plot over 60-day immersion experiment;
FIG. 9 is a Scanning Electron Microscope (SEM) of the coating surface after testing for 14 days of the anti-algae experiment for examples and comparative examples PANI @ CN-10/EP and EP; wherein (a, b, g, h) is an EP coating, (c, d, i, j) is a CN/EP coating, and (e, f, k, l) is a PANI @ CN-10/EP coating.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings.
Example 1
(1) Thermal polymerization to synthesize carbon nitride: 10g of urea was placed in a 50mL crucible, placed in a muffle furnace, heated from room temperature to 500 ℃ at a heating rate of 3 ℃/min, and then held at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as CN;
(2) Preparing a polyaniline-carbon nitride compound: 1g of CN and 100mg of polyaniline were uniformly mixed, placed in a crucible, placed in a muffle furnace, heated from room temperature to 250 ℃ at a heating rate of 3 ℃/min, and then kept at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as PANI @ CN-10;
(3) Preparing the polyaniline-carbon nitride-resin composite coating: 1g of epoxy resin and 0.6g of polyamide resin are taken and stirred uniformly by a magnetic stirrer at 800 r/min; adding 50mg PANI @ CN-10 and a drop of defoaming agent, and continuously stirring for half an hour to obtain the composite coating;
coating on the surface of carbon steel by a spin coater, drying at room temperature for 24h, and curing at 60 deg.C for 2h. The resulting coating sample was labeled PANI @ CN-10/EP and had a thickness of 67 μm.
Example 2
Compared to example 1, the content of polyaniline was changed:
(1) Thermal polymerization to synthesize carbon nitride: 10g of urea was placed in a 50mL crucible, placed in a muffle furnace, heated from room temperature to 500 ℃ at a heating rate of 3 ℃/min, and then held at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as CN;
(2) Preparing a polyaniline-carbon nitride compound: 1g of CN and 50mg of polyaniline were uniformly mixed, placed in a crucible, placed in a muffle furnace, heated from room temperature to 250 ℃ at a heating rate of 3 ℃/min, and then kept at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as PANI @ CN-5;
(3) Preparing the polyaniline-carbon nitride-resin composite coating: 1g of epoxy resin and 0.6g of polyamide resin are taken and stirred uniformly by a magnetic stirrer at 800 r/min; adding 50mg PANI @ CN-5 and a drop of defoaming agent, and continuously stirring for half an hour to obtain the composite coating;
coating on the surface of carbon steel by a spin coater, drying at room temperature for 24h, and curing at 60 deg.C for 2h. The resulting coating sample was labeled PANI @ CN-5/EP and had a thickness of 59 μm.
Example 3
Compared to example 1, the content of polyaniline was changed:
(1) Thermal polymerization to synthesize carbon nitride: 10g of urea was placed in a 50mL crucible, placed in a muffle furnace, heated from room temperature to 500 ℃ at a heating rate of 3 ℃/min, and then held at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as CN;
(2) Preparing a polyaniline-carbon nitride compound: 1g of CN and 150mg of polyaniline were uniformly mixed, placed in a crucible, placed in a muffle furnace, heated from room temperature to 250 ℃ at a heating rate of 3 ℃/min, and then kept at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as PANI @ CN-15;
(3) Preparing the polyaniline-carbon nitride-resin composite coating: 1g of epoxy resin and 0.6g of polyamide resin are taken and stirred evenly by a magnetic stirrer at 800 r/min; adding 50mg PANI @ CN-15 and a drop of defoaming agent, and continuing stirring for half an hour to obtain the composite coating;
coating on the surface of carbon steel by a spin coater, drying at room temperature for 24h, and curing at 60 deg.C for 2h. The resulting coating sample was labeled PANI @ CN-15/EP and had a thickness of 75 μm.
Comparative example 1
In comparison with example 1, a pure phase EP was prepared:
1g of epoxy resin and 0.6g of polyamide resin are taken and stirred evenly by a magnetic stirrer at 800 r/min; adding a drop of defoaming agent, and continuously stirring for half an hour to obtain pure-phase EP;
coating on the surface of carbon steel by a spin coater, drying at room temperature for 24h, and curing at 60 deg.C for 2h. The resulting coating sample was labeled EP and had a thickness of 59 μm.
Comparative example 2
In comparison with example 1, a carbon nitride-resin coating was prepared:
(1) Thermal polymerization to synthesize carbon nitride: 10g of urea was placed in a 50mL crucible, placed in a muffle furnace, heated from room temperature to 500 ℃ at a heating rate of 3 ℃/min, and then held at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as CN;
(2) Preparation of carbon nitride-resin coating: 1g of epoxy resin and 0.6g of polyamide resin are taken and stirred evenly by a magnetic stirrer at 800 r/min; adding 50mg CN and a drop of defoaming agent, and continuously stirring for half an hour to obtain the composite coating;
coating on the surface of carbon steel by a spin coater, drying at room temperature for 24h, and curing at 60 deg.C for 2h. The resulting coating sample was labeled CN/EP and had a thickness of 65 μm.
Comparative example 3
Compared with example 1, the content of polyaniline was changed:
(1) Thermal polymerization to synthesize carbon nitride: 10g of urea was placed in a 50mL crucible, placed in a muffle furnace, heated from room temperature to 500 ℃ at a heating rate of 3 ℃/min, and then held at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as CN;
(2) Preparing a polyaniline-carbon nitride compound: 1g of CN and 200mg of polyaniline were uniformly mixed, placed in a crucible, placed in a muffle furnace, heated from room temperature to 250 ℃ at a heating rate of 3 ℃/min, and then kept at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as PANI @ CN-20;
(3) Preparing the polyaniline-carbon nitride-resin composite coating: 1g of epoxy resin and 0.6g of polyamide resin are taken and stirred uniformly by a magnetic stirrer at 800 r/min; adding 50mg PANI @ CN-20 and a drop of defoaming agent, and continuously stirring for half an hour to obtain the composite coating; coating on the surface of carbon steel by a spin coater, drying at room temperature for 24h, and curing at 60 deg.C for 2h. The resulting coating sample was labeled PANI @ CN-20/EP and had a thickness of 59 μm.
Comparative example 4
Compared to example 1, the content of polyaniline was changed: (1) thermal polymerization to synthesize carbon nitride: 10g of urea was placed in a 50mL crucible, placed in a muffle furnace, and the temperature thereof was heated from room temperature to 500 ℃ at a heating rate of 3 ℃/min, and then kept at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as CN;
(2) Preparing a polyaniline-carbon nitride compound: 1g of CN and 30mg of polyaniline were uniformly mixed, placed in a crucible, placed in a muffle furnace, heated from room temperature to 250 ℃ at a heating rate of 3 ℃/min, and then kept at a constant temperature for 2 hours. Grinding the obtained sample in an agate mortar, and collecting for later use, wherein the sample is marked as PANI @ CN-3;
(3) Preparing the polyaniline-carbon nitride-resin composite coating: 1g of epoxy resin and 0.6g of polyamide resin are taken and stirred evenly by a magnetic stirrer at 800 r/min; adding 50mg PANI @ CN-3 and a drop of defoaming agent, and continuously stirring for half an hour to obtain the composite coating;
coating on the surface of carbon steel by a spin coater, drying at room temperature for 24h, and curing at 60 deg.C for 2h. The resulting coating sample was labeled PANI @ CN-3/EP and had a thickness of 58 μm.
As shown in fig. 1, scanning Electron Microscope (SEM) characterization was performed for example 1 and comparative example 2. As can be seen from the Scanning Electron Microscope (SEM), both are lamellar structures, which will help provide a shielding effect in the coating, enhancing the corrosion resistance. Under the condition that the mass ratio of the polyaniline to the carbon nitride is 5-15%, the sheet structure of the CN is not damaged.
As shown in fig. 2 to 4, the examples and comparative examples were subjected to material-related characterization of polyaniline/carbon nitride composites. The successful compounding of polyaniline carbon nitride through low-temperature thermal polymerization is shown.
As shown in FIG. 5, N1s spectra of high resolution X-ray photoelectron spectroscopy (XPS) in example 1 and comparative example 2 show that nitrogen cation free radicals of PANI are present on the surface of PANI @ CN-10, which helps to bind the negative charge of the algae cell wall, and the synergy of carbon nitride and polyaniline helps to improve the anti-algae performance of the coating.
As shown in fig. 6 to 7, the photoelectric properties of the composite materials of the examples and the comparative examples are characterized, and it is found that the composite material used in example 1 has good photoelectric chemical properties and excellent photogenerated carrier separation efficiency, which can help to improve the corrosion resistance and the anti-biofouling performance of the coating.
It is shown by FIG. 8 that the low frequency impedance modulus of example 1 is two orders of magnitude better than that of comparative example 1, y and pThe ratio 2 is one order of magnitude higher, and has excellent corrosion resistance. After 60 days of immersion, example 1 still maintained the highest resistance modulus, indicating excellent corrosion stability. FIG. 9 shows the anti-biofouling performance of example 1 and comparative examples 1,2, with only a small amount of biofouling on the surface of the examples, exhibiting relatively excellent anti-biofouling performance. When the content of polyaniline is too small, N in the coating + The ion content is too low, so that the ideal anti-biological fouling effect cannot be achieved; too much polyaniline content can cause the agglomeration of added fillers, destroy the sheet structure of carbon nitride and weaken the barrier effect of the carbon nitride in the coating.
Claims (10)
1. The polyaniline-carbon nitride compound is characterized in that polyaniline is used as a coating layer, flaky carbon nitride is used as a carrier, and the mass ratio of polyaniline to carbon nitride is 5-15.
2. A resin composite coating containing the polyaniline-carbon nitride composite according to claim 1, wherein the polyaniline-carbon nitride composite is doped in the resin composite coating, and the doping amount of the polyaniline-carbon nitride composite is 0.1 to 0.5% of the mass of the composite resin.
3. The composite coating according to claim 2, wherein the composite resin is a mixture of epoxy resin and polyamide resin, and the mass ratio of the polyamide resin to the epoxy resin is 1-4.
4. The method for producing a resin composite coating material according to claim 2, comprising the steps of:
(1) Calcining urea and carrying out thermal polycondensation to obtain flaky carbon nitride;
(2) Uniformly mixing the flaky carbon nitride and the polyaniline, and calcining to form a polyaniline-carbon nitride compound;
(3) The polyaniline-carbon nitride composite is dispersed in an organic solvent, a uniform dispersion is obtained by ultrasonic treatment, epoxy resin and polyamide resin are mixed, and the polyaniline-carbon nitride-resin composite coating is obtained by stirring.
5. The method according to claim 4, wherein in the step (1), the calcination is carried out at a temperature rise rate of 3 to 5 ℃/min, a holding temperature of 500 to 550 ℃ and a holding time of 1.5 to 3 hours.
6. The method according to claim 4, wherein in the step (2), the mass ratio of polyaniline to carbon nitride is 5 to 15%.
7. The method according to claim 4, wherein in the step (2), the calcination is carried out at a temperature rise rate of 3 to 5 ℃/min, a holding temperature of 270 to 300 ℃ and a holding time of 1.5 to 2 hours.
8. The method according to claim 4, wherein in the step (3), the mass ratio of the polyaniline-carbon nitride composite to the organic solvent is 1.
9. The method according to claim 4, wherein in the step (3), the ultrasonic time is 0.5 to 1 hour.
10. The method according to claim 4, wherein in the step (3), the stirring is performed at a speed of 800 to 1200r/min for a time of 0.5 to 2 hours.
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Non-Patent Citations (1)
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| ZUO SX, ET AL.: "Polyaniline/g-C3N4 composites as novel media for anticorrosion coatings", JOURNAL OF COATINGS TECHNOLOGY AND RESEARCH, vol. 14, no. 6, pages 1307 - 1314, XP036363988, DOI: 10.1007/s11998-017-9916-7 * |
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