CN115232532A - Preparation method of fluorinated graphene modified epoxy resin coating - Google Patents
Preparation method of fluorinated graphene modified epoxy resin coating Download PDFInfo
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- CN115232532A CN115232532A CN202210953405.1A CN202210953405A CN115232532A CN 115232532 A CN115232532 A CN 115232532A CN 202210953405 A CN202210953405 A CN 202210953405A CN 115232532 A CN115232532 A CN 115232532A
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- coating
- epoxy resin
- fluorinated graphene
- graphene
- preparing
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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
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C01B32/198—Graphene oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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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
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- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/61—Specific applications or type of materials thin films, coatings
Abstract
The invention discloses a preparation method of a fluorinated graphene modified epoxy resin coating, relates to the technical field of chemistry, and particularly relates to a preparation method of a fluorinated graphene modified epoxy resin coating, which comprises the following steps: s1: preparing experimental medicines and experimental instruments; s2: graphene oxide was prepared by an improved hummers method. According to the preparation method of the fluorinated graphene modified epoxy resin coating, hydrofluoric acid (HF) and Graphene Oxide (GO) are reacted to prepare Fluorinated Graphene (FG), the Fluorinated Graphene (FG) is added into epoxy resin to prepare a composite material, the influence of the adhesion and corrosion resistance of the Fluorinated Graphene (FG) modified epoxy resin (EP) coating is explored, the surface morphology, microstructure and corrosion protection performance of the fluorinated graphene FG are researched through detection equipment such as FTIR, XRD and SEM, and the influence of the Fluorinated Graphene (FG) on the coating compactness is researched through adhesion testing.
Description
Technical Field
The invention relates to the technical field of chemistry, in particular to a preparation method of a fluorinated graphene modified epoxy resin coating.
Background
Corrosion refers to the process of material loss and destruction by the surrounding medium, which is the change of material property. The corrosion phenomenon of materials is reflected in various fields including transportation, chemical engineering, machinery, energy sources and the like. At present, the organic protective coating is the main protective measure of the metal material in the marine environment.
The epoxy resin is a modern important organic anticorrosive paint, and has excellent physical and mechanical properties, electric insulation property, adhesion property, low cost and the like. However, epoxy resin coatings also have many defects, such as poor low temperature cracking resistance, high spatial structure porosity, low strength, poor flexibility and the like [1], epoxy resins are easy to generate increased spatial structure porosity due to curing shrinkage effect, so that corrosive media are transmitted to the interior of the coating through the pores to be contacted with a substrate, and thus the substrate is corroded. Researches show that the nano-filler added into the epoxy resin coating can effectively make up for the micropore defect [2], improve the barrier property of the coating and optimize the corrosion resistance of the coating.
Graphene (G) is a carbon nanostructure formed in an sp2 hybridization manner, and is a new material closely packed into a single-layer two-dimensional honeycomb lattice structure, and Graphene has excellent mechanical properties, electrical conductivity, thermal conductivity, self-lubricating property and excellent optical transparency. The graphene is doped in the epoxy resin, so that the strength, toughness, lubricity and barrier property of the epoxy resin are greatly improved. But due to the defects among the graphene lamellar structures and the high conductivity of the graphene, the effect of improving the corrosion resistance of the epoxy resin coating is small, the graphene coating only keeps the protective performance in a short time, and the graphene can promote the metal corrosion at the coating defects during long-term soaking [3,4].
Fluorinated Graphene (FG) is a derivative of graphene, which is a two-dimensional planar structure of carbon nanomaterial formed in an sp3 manner, and retains part of its sp2 structure and its own sp3 structure [5]. Wherein the bond between the carbon atom and the fluorine atom is between a covalent bond and an ionic bond. Because fluorine is very electronegative, fluorinated graphene has greater thermal stability and oxidation resistance than graphene. The fluorinated graphene has a two-dimensional structure and excellent performances such as low surface energy, strong hydrophobicity, mechanical property, high temperature resistance, corrosion resistance and the like, so that the fluorinated graphene can be widely applied to corrosion-resistant coatings, nano-electronics, photoelectric and thermoelectric devices.
Epoxy groups (Epoxy epoxide) are cyclic structures consisting of one oxygen atom and two carbon atoms, have high activity and are active reaction groups, and the special structures enable the curing forms of Epoxy resin to be diversified. The molecular structure of the bisphenol A epoxy resin determines the final performance of the bisphenol A epoxy resin, and the bisphenol A epoxy resin has the following characteristics when being crosslinked with an amine curing agent to form a net structure: good mechanical property, excellent adhesive force, excellent insulating property and wide application field, and the epoxy resin has many advantages but also has some disadvantages: for example, poor light stability, easy pulverization, poor low-temperature curability, brittle texture, poor fatigue resistance, poor impact resistance, and the like.
The oxygen resin and the fluorinated graphene respectively have a plurality of excellent performances, and how to combine and exert the advantages of the oxygen resin and the fluorinated graphene becomes an important content for researching the performance of the coating at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a fluorinated graphene modified epoxy resin coating, which solves the problems in the background art.
In order to realize the purpose, the invention is realized by the following technical scheme: a preparation method of a fluorinated graphene modified epoxy resin coating comprises the following steps:
s1: preparing experimental medicines and experimental instruments;
s2: preparing graphene oxide by an improved hummers method;
s2.1: preparing pre-oxidized graphite: weighing 10g of graphite powder, 4g of potassium persulfate and 10g of phosphorus pentoxide, sequentially adding the graphite powder, the potassium persulfate and the phosphorus pentoxide into a beaker filled with 24mL of sulfuric acid in a fume hood under the condition of stirring, transferring the beaker into a pre-adjusted 60 ℃ constant-temperature water bath pot after no gas is produced for reaction for 3h, transferring the beaker into a pre-adjusted 25 ℃ constant-temperature water bath pot for reaction for 5h after the reaction is finished, adding a small part of deionized water to dilute sulfuric acid, performing suction filtration, washing the sulfuric acid to be neutral while performing suction filtration by using a large amount of deionized water, and drying the sulfuric acid at normal temperature to obtain pre-oxidized graphite;
s2.2: preparing graphite oxide: weighing 1g of pre-oxidized graphite, adding the pre-oxidized graphite into a beaker filled with 25mL of sulfuric acid, immediately stirring to uniformly disperse the pre-oxidized graphite, putting the beaker into an ice water bath, adding 3g of potassium permanganate after the pre-oxidized graphite is completely dissolved, reacting for 2 hours, moving the beaker into a constant-temperature water bath kettle at 35 ℃ for reacting for 40 minutes, then adding 46mL of deionized water, finally adding 140mL of 2, continuing to react for 1 hour at 35 ℃, finally dropwise adding 30% of H2O2 until no gas is generated, enabling the solution to become bright yellow, centrifuging and filtering while hot, washing the solution to be neutral by using a large amount of 5% hydrochloric acid and deionized water, pouring the final precipitate into a culture dish after 1 hour of ultrasonic oscillation, and drying for 24 hours at 90 ℃ to obtain flaky Graphite Oxide (GO);
s3: preparing fluorinated graphene:
s3.1: weighing 50mg of graphene oxide sample, adding the graphene oxide sample into a beaker containing 40mL of deionized water, placing the beaker in an ultrasonic oscillation cleaner for ultrasonic treatment for 30min to form uniform graphene oxide dispersion liquid, then adding 10mL of hydrofluoric acid (HF) into the dispersion liquid, transferring the dispersion liquid into a hydrothermal kettle with a polytetrafluoroethylene lining, screwing the hydrothermal kettle to seal the hydrothermal kettle, then placing the hydrothermal kettle in an oven, carrying out heat treatment at 160 ℃ for 12h, naturally cooling the hydrothermal kettle to room temperature after the reaction is finished, directly evaporating the solution to obtain a solid, obtaining a fluorinated graphene sample to be tested,
s3: the preparation of the fluorinated graphene modified epoxy resin coating,
s3.2: preparing a metal matrix: the experimental metal matrix is Q235 carbon steel sheet, the size is 50mm multiplied by 25mm multiplied by 2mm, the Q235 carbon steel sheet is respectively polished by water abrasive paper with different specifications (180 #, 400#, 600#, 1000 #), ultrasonically deoiled by acetone, and dried for standby; preparation of fluorinated graphene modified epoxy resin coating [23]
S3.3: adding the FG and the epoxy resin into a beaker according to the mass ratio of 1: 200, uniformly mixing and stirring for 5min, and mixing the materials according to the weight ratio of a wetting dispersant: adhesive force dispersing agent: leveling agent =8:4:1, adding 20g of post-assistant in a mass ratio of 1, performing ultrasonic dispersion for 2 hours to uniformly disperse the fluorinated graphene and the assistant into epoxy resin, then adding a polyamide curing agent in a mass ratio of 2: 1 of the epoxy resin and the polyamide curing agent, uniformly stirring, uniformly coating the cured mixture on the surface of a pretreated carbon steel sheet, standing at room temperature for 12 hours, transferring the mixture to a drying oven at 60 ℃ for drying for 12 hours to obtain a fluorinated graphene modified epoxy resin coating, expressing FG/EP, preparing an epoxy varnish coating according to the same curing conditions, expressing EP,
s4: testing the fluorinated graphene modified epoxy resin coating;
s4.1: fourier infrared spectroscopy (FTIR): qualitative and quantitative analysis can be carried out on the sample through infrared spectroscopy, whether the prepared fluorinated graphene is successfully doped with fluorine can be proved, the spectrum scanning range is 4000cm < -1 > to 500cm < -1 >, samples are prepared by a KBr tablet pressing method,
S4.2X-ray diffraction (XRD): the method comprises the following steps of irradiating a sample with X-rays to generate diffraction peaks with different intensities at different angles, wherein each substance has a unique diffraction peak, and analyzing the diffraction spectrum to determine the specific diffraction spectrum generated by the substance, such as the composition, crystal form, molecular configuration, intramolecular bonding mode and the like of the sample substance, so as to judge whether the manufactured graphene fluoride is successful, wherein the interplanar spacing of the graphene fluoride is calculated by Bragg diffraction law (lambda =2d sin theta) to obtain a scanning range: 3 to 80 degrees,
s4.3: adhesion test of the coating: the adhesive force of the coating represents the binding capacity between the metal and the coating, the coating not only needs the hardness and compactness of the coating, but also needs to be closely attached to a substrate, when the self condensation force of the coating is reduced, a corrosion medium can contact the substrate through the coating to accelerate electrochemical corrosion reaction, the good adhesive force can prevent the corrosion medium from permeating, further the electrochemical corrosion reaction between the corrosion medium and the metal is prevented, the test adopts a cross-hatch method to test the adhesive force of the graphene oxide modified epoxy resin coating, and the test refers to the adhesive force evaluation grade of the national standard coating,
s4.4: and (3) testing the corrosion resistance of the coating: EP and FG/EP were coated on a Q235 carbon steel sheet, and immersed in 3 groups of strong acid, 3.5% NaCl electrolyte, and strong acid for 20 days, respectively, and changes in surface corrosion morphology before and after coating were observed under a Scanning Electron Microscope (SEM).
Optionally, the experimental drug comprises natural graphite powder, potassium persulfate, phosphorus pentoxide, sulfuric acid, potassium permanganate, hydrogen peroxide, hydrofluoric acid, epoxy resin E51, polyamide, an adhesion auxiliary agent, a wetting dispersant 2150, a leveling agent 310 and acetone.
Optionally, the experimental apparatus includes an electric centrifuge, an ultrasonic cleaner, an electronic balance, a coating thickness gauge, a constant temperature drying oven, a scanning electron microscope, and an X-ray diffractometer.
The invention provides a preparation method of a fluorinated graphene modified epoxy resin coating, which has the following beneficial effects:
1. according to the preparation method of the fluorinated graphene modified epoxy resin coating, hydrofluoric acid (HF) and Graphene Oxide (GO) are adopted to react to prepare Fluorinated Graphene (FG), then the Fluorinated Graphene (FG) is added into epoxy resin to prepare a composite material, the influence of the adhesion and corrosion resistance of the Fluorinated Graphene (FG) modified epoxy resin (EP) coating is explored, the surface morphology, microstructure and corrosion protection performance of the Fluorinated Graphene (FG) are researched through detection equipment such as FTIR, XRD and SEM, and the influence of the Fluorinated Graphene (FG) on the compactness of the coating is researched through adhesion testing. The result shows that the Hummers is successfully utilized to successfully prepare the Graphene Oxide (GO) and the hydrothermal method is used to prepare the Fluorinated Graphene (FG); after the Fluorinated Graphene (FG) is added into the epoxy resin, the adhesive force of the epoxy resin is improved, the compactness of the epoxy resin is improved, an electrochemical corrosion medium is blocked, the permeation process of the corrosion medium is delayed, and the corrosion resistance and the stability of the epoxy resin are enhanced.
Drawings
FIG. 1is a schematic structural view of a bisphenol A type epoxy resin of the present invention;
FIG. 2 is a FTIR plot of Graphene Oxide (GO) and graphene Fluoride (FG) according to the present invention;
FIG. 3 is an XRD pattern of FG powder of the invention;
FIG. 4 is an appearance diagram of the cross-cut method of the present invention;
FIG. 5 is a graph showing the change of the EP coating of the present invention in initial immersion in an acid solution for 1d and 20 d;
FIG. 6 is a graph showing the variation of the FG/EP coating of the present invention at the beginning of immersion in acid solution, 1d and 20 d;
FIG. 7 is a graph showing the change of immersion initiation, 1d and 20d of the EP coating of the present invention in a 3.5% NaCl solution;
FIG. 8 is a graph of the initial, 1d and 20d variation of the FG/EP coating of the invention in a 3.5% NaCl solution;
FIG. 9 is a graph showing the change of the EP coating of the present invention in initial immersion, 1d and 20d in an alkaline solution;
FIG. 10 is a graph showing the variation of the immersion initiation, 1d and 20d of the FG/EP coating of the present invention in an alkaline solution;
FIG. 11 is a SEM representation of an EP coating and FG/EP coating of the invention after immersion in a pH 13 NaOH solution for 20 days;
FIG. 12 is a schematic SEM image of an EP coating and FG/EP coating of the invention after immersion in a pH 1H 2SO4 solution for 20 d;
FIG. 13 is an SEM image of the EP coating and FG/EP coating of the invention after immersion in 3.5% NaCl solution for 20 d;
FIG. 14 is a SEM representation of the initial appearance of an EP coating and FG/EP coating of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1 to 14, the present invention provides a technical solution: a preparation method of a fluorinated graphene modified epoxy resin coating comprises the following steps:
s1: preparing experimental medicines and experimental instruments;
s2: preparing graphene oxide by an improved hummers method;
s2.1: preparing pre-oxidized graphite: weighing 10g of graphite powder, 4g of potassium persulfate and 10g of phosphorus pentoxide, sequentially adding the graphite powder, 4g of potassium persulfate and 10g of phosphorus pentoxide into a beaker filled with 24mL of sulfuric acid in a fume hood under the condition of stirring, transferring the beaker into a thermostat water bath kettle debugged in advance at 60 ℃ after no gas is produced, reacting for 3h, transferring the beaker into the thermostat water bath kettle debugged in advance at 25 ℃ after the reaction is finished for 5h, then adding a small part of deionized water to dilute sulfuric acid, performing suction filtration, washing with a large amount of deionized water while performing suction filtration to be neutral, and drying at normal temperature to obtain pre-oxidized graphite;
s2.2: preparing graphite oxide: weighing 1g of pre-oxidized graphite, adding the pre-oxidized graphite into a beaker filled with 25mL of sulfuric acid, immediately stirring to uniformly disperse the pre-oxidized graphite, putting the beaker into an ice water bath, adding 3g of potassium permanganate after the pre-oxidized graphite is completely dissolved, reacting for 2 hours, moving the beaker into a constant temperature water bath kettle at 35 ℃ for reacting for 40min, then adding 46mL of deionized water, and finally adding 140mL. The reaction was continued at 35 ℃ for 1h. Finally, 30% H2O2 was added dropwise so that the solution turned bright yellow until no more gas was formed. The mixture was filtered by centrifugation while hot and washed to neutrality with a large amount of 5% hydrochloric acid and deionized water. Pouring the final precipitate into a culture dish after 1h of ultrasonic oscillation, and drying at 90 ℃ for 24h to obtain flaky Graphite Oxide (GO);
s3: preparing fluorinated graphene:
s3.1: weighing 50mg of graphene oxide sample, adding the graphene oxide sample into a beaker containing 40mL of deionized water, and placing the beaker in an ultrasonic oscillation cleaner for ultrasonic treatment for 30min to form a uniform graphene oxide dispersion liquid. Then, 10mL of hydrofluoric acid (HF) was added to the dispersion, the dispersion was transferred to a hydrothermal reactor with a polytetrafluoroethylene liner, the hydrothermal reactor was tightly screwed and sealed, and then it was placed in an oven and heat-treated at 160 ℃ for 12 hours. After the reaction was completed, it was allowed to cool naturally to room temperature. And directly evaporating the solution to obtain a solid, so as to obtain a fluorinated graphene sample to be detected.
S3: preparing a fluorinated graphene modified epoxy resin coating,
s3.2: preparing a metal matrix: the experimental metal matrix is a Q235 carbon steel sheet with the size of 50mm25mm2 mm. Grinding the Q235 carbon steel sheet by using water-milled sand paper with different specifications (180 #, 400#, 600#, 1000 #), ultrasonically removing oil by using acetone, and drying for later use; preparation of fluorinated graphene modified epoxy resin coating [23]
S3.3: adding the FG and the epoxy resin into a beaker according to the mass ratio of 1: 200, uniformly mixing and stirring for 5min, and mixing the materials according to the weight ratio of a wetting dispersant: adhesive force dispersing agent: leveling agent =8:4:1, adding 20g of post-addition agent, and performing ultrasonic dispersion for 2 hours to uniformly disperse the fluorinated graphene and the addition agent into the epoxy resin. Then adding a polyamide curing agent according to the mass ratio of 2: 1 of the epoxy resin to the polyamide curing agent, uniformly stirring, uniformly coating the cured polyamide curing agent on the surface of the pretreated carbon steel sheet, standing at room temperature for 12 hours, and transferring the carbon steel sheet to a drying oven at 60 ℃ for drying for 12 hours. The fluorinated graphene modified epoxy resin coating is obtained and is indicated by FG/EP. Epoxy varnish coatings were prepared according to the same curing conditions and are indicated by EP.
S4: testing the fluorinated graphene modified epoxy resin coating;
s4.1: fourier infrared spectroscopy (FTIR): qualitative and quantitative analysis can be carried out on the sample through infrared spectroscopy, and whether the prepared fluorinated graphene is successfully doped with fluorine can be proved. The spectral scanning range is 4000cm < -1 > to 500cm < -1 >. The sample is prepared by KBr tablet method, and the characteristic result of observing the infrared spectrogram of 1GO and FG in figure 2 shows that 3420cm-1 is the absorption peak of O-H, and 1634cm-1 is the characteristic absorption peak of six-membered ring C = C bond. After fluorination treatment, FG has a characteristic absorption peak of a C-F bond representing a covalent bond at 1210cm-1 and a characteristic absorption peak of a semi-ionic C-F bond at 1080cm-1, which indicates that FG with a certain fluorination degree is obtained after GO is subjected to fluorination treatment.
S4.2X-ray diffraction (XRD): the method comprises the steps of irradiating a sample with X-rays to generate diffraction peaks with different intensities at different angles, and analyzing the diffraction pattern of each substance to obtain the specific diffraction pattern generated by the substance, wherein the specific diffraction pattern is determined by the composition, crystal form, molecular configuration, intramolecular bonding mode and the like of the sample substance, so as to judge whether the prepared successfully fluorinated graphene exists or not. The interplanar spacing of the fluorinated graphene is calculated from bragg diffraction law (λ =2d sin θ) to obtain the scanning range: 3-80 degrees, and observing fig. 3, the characteristic diffraction peak representing the FG (001) crystal face appears at 2 theta =15.56 degrees, and the corresponding distance between the fluorinated graphene and the fluorinated graphene is calculated to be 0.57nm through a Bragg equation; FG shows a characteristic diffraction peak representing the graphite (002) crystal plane at 2 θ =31.03 °. While the corresponding diffraction peak in natural graphite is 26.5 deg., the corresponding lamella spacing is 0.34nm. It is demonstrated that FG after the fluorination treatment exfoliated the multilayer graphite, and the larger interlayer distance was attributed to the intercalation of fluorine atoms, which reduced the interlayer forces, allowing the graphite fluoride to diffuse into fewer layers. A characteristic diffraction peak representing the FG (100) crystal plane due to fluorination appears weakly at 2 θ =40.70 °, and the above analysis shows that the graphite gives FG by the fluorination treatment.
S4.3: adhesion test of the coating: the adhesion of the coating represents the bonding capability between the metal and the coating. The coating needs not only its own hardness and compactness but also close adhesion to the substrate. When the coating self-coagulation force is reduced, the corrosion medium can contact the substrate through the coating, and the electrochemical corrosion reaction is accelerated. The good adhesive force can prevent the penetration of the corrosive medium, thereby preventing the electrochemical corrosion reaction between the corrosive medium and the metal. The adhesion of the graphene oxide modified epoxy resin coating is tested by a cross-cut method in the experiment. And the adhesion evaluation grade of the national standard coating is referred.
The adhesion evaluation rating of the coating is shown in Table 1
Table 1ISO 2409 Scoring adhesion rating
S4.4: and (3) testing the corrosion resistance of the coating: EP and FG/EP were coated on a Q235 carbon steel sheet, and immersed in 3 groups of strong acid, 3.5% NaCl electrolyte, and strong acid for 20 days, respectively, and changes in surface corrosion morphology before and after coating were observed under a Scanning Electron Microscope (SEM).
Referring to FIG. 4, the adhesion of comparative EP to FG/EP was measured by cross-hatch method in this experiment, and the cross-hatch appearance of the coating is shown in FIG. 4: there was little partial peeling at the FG/EP coating intersection, and little peeling along the edge at the EP coating intersection. The adhesion rating of the FG/EP coating obtained was 1A and that of the EP coating was 2A. The experimental results show that the FG/EP coating adhesion is greater than that of the EP coating. Therefore, the addition of the fluorinated graphene does not affect the original excellent adhesive force of the epoxy resin, and partial pore defects in the fluorinated graphene modified epoxy resin coating are filled with the added FG, so that the compactness of the coating is improved, the adhesive force between the coating and a substrate interface is increased, and the substrate is prevented from being corroded due to the permeation of corrosive media.
Corrosion resistance test referring to fig. 5, FG/EP coating and EP coating were immersed in H2SO4 solution at pH 1, nacl solution at 3.5% and NaOH solution at pH 13, respectively, and the morphology change was observed at 1d and 20d before and after immersion as shown in fig. 5-10: it can be seen from the figure that within 24h, as shown in FIGS. 5-6, the EP coating and FG/EP coating did not change significantly from solution to solution in NaOH solution at pH 13; but the edge of the surface of the coating in the H2SO4 solution with the pH value of 1 generates bubbles; as shown in FIG. 7, the coating did not change significantly in the 3.5% NaCl solution, but the back surface of the carbon steel sheet corroded and the solution rusted. After 20 days of soaking, under macroscopic observation, as shown in fig. 9, the EP coating and the FG/EP coating have no obvious change in the NaOH solution with pH 13, and the back surface of the carbon steel sheet is not corroded; as shown in FIG. 10, in the 3.5% NaCl solution, no difference between the EP coating and the FG/EP coating occurred, no apparent phenomenon was observed on the surface, and rust occurred in the solution; as shown in FIG. 9, in the H2SO4 solution with pH 1, the EP coating edge was largely peeled off and adhered to the cup wall, the rust was adhered to the coating, the FG/EP coating edge was slightly peeled off and adhered to the cup wall, and the rust was adhered to the coating. Further, it was found that the EP coating and the FG/EP coating have corrosion resistance in a 3.5% NaCl solution and a NaOH solution having a pH of 13. However, the corrosion resistance is poor in the H2SO4 solution with pH value of 1.
Scanning Electron microscope testing (SEM)
FG/EP and EP, respectively soaked in strong acid, 3.5% NaCl solution and strong base, and observed under SEM for 20d to form a pair of patterns as shown in FIGS. 11-14;
as shown in fig. 11, under alkaline conditions, the left EP coating showed extensive corrosion and blistering, wrinkling. Whereas FG/EP coatings are smoother with better integrity, but blistering also occurs;
as shown in fig. 12, the EP coating cracked under acidic conditions, resulting in extensive corrosion. FG/EP coatings delaminate and corrode to a greater extent, but to a lesser extent than EP coatings;
as shown in FIG. 13, in the 3.5% NaCl solution, the EP coating exhibited a large number of pitting, the FG/EP coating exhibited a strong resistance to corrosive media, no significant corrosion occurred smoothly, and a large amount of corrosive media could not enter the coating interior to contact the carbon steel sheet, so that electrochemical corrosion did not occur.
As shown in fig. 14, the EP coating and FG/EP coating did not undergo corrosion initial morphology, which resulted in some flatness of the coating due to the cutting of the coating as measured by SEM. However, the smoothness of FG/EP is much higher than that of EP, and the doping of fluorinated graphene is illustrated on the side face, so that the compactness of the epoxy coating is improved by one level. And FG is uniformly dispersed in EP, and large-area agglomeration does not occur.
Comparing and analyzing the SEM appearances of the EP coating and the FG/EP coating soaked for 20d in three different environments, the FG/EP coating has better corrosion appearance change degree than the EP coating due to the pore defect of the epoxy resin caused by FG modification, generates excellent barrier property on an electrochemical corrosion medium, improves the corrosion resistance of the electrochemical corrosion medium, and enhances the stability, the barrier property and the hardness of the coating.
The experimental medicine comprises natural graphite powder, potassium persulfate, phosphorus pentoxide, sulfuric acid, potassium permanganate, hydrogen peroxide, hydrofluoric acid, epoxy resin E51, polyamide, an adhesion auxiliary agent, a wetting dispersing agent 2150, a leveling agent 310 and acetone.
The experimental apparatus comprises an electric centrifuge, an ultrasonic cleaner, an electronic balance, a coating thickness gauge, a constant-temperature drying box, a scanning electron microscope and an X-ray diffractometer.
Example two: based on the first embodiment, the differences from the first embodiment are that: preparing FG (FG) by taking graphene as a raw material, and then preparing fluorinated graphene by taking N and O doped graphene aerogel as a precursor by adopting a direct fluorination method, wherein researches show that the fluorine content is increased along with the increase of the temperature in the process of increasing the temperature from 200 ℃ to 300 ℃; however, at 350 ℃, higher fluorination temperatures lead to decomposition of the C — F bond, resulting in partial recovery of the sp2 hybrid structure and loss of fluorine atoms. The by-products generated in the fluorination process reduce the electrochemical performance of the fluorinated graphene as the cathode material.
2. The single-layer graphene is grown by adopting a chemical vapor deposition method, and then FG with different fluorine contents is prepared in the environment of sulfur hexafluoride (SF 6) plasma gas. Angle-dependent NEXAFS revealed that the interaction of fluorine atoms forms covalent C — F bonds with graphene substrates, perpendicular to the plane of the substrate FG, and enhances physical absorption as measured by XPS.
3. The graphene and xenon difluoride gases are heated to 350 ℃ by increasing the temperature under an inert atmosphere and held for 1 and 5 days. The structural characteristics of the fluorographene are confirmed after characterization, and the band gap of the fluorographene is 3.8eV. Finally, the surface fluorographitic can be used for electronics, photovoltaic applications and energy harvesting applications.
4. And reacting the graphene with a fluorinating agent to prepare the fluorinated graphene. FG prepared has comparable conductivity to graphene. Research shows that the strong electronegativity of fluorine atoms increases the affinity of C to F, the FG obviously improves the stability under high voltage, and the prepared FG can be applied to lithium ion battery electrode materials as electrode materials;
5. in a nitrogen environment, KOH and graphene are uniformly mixed according to a certain proportion, the mixture is treated at 600 ℃ for 5 hours, then a product is placed in a vacuum reactor, the vacuum reactor is evacuated by nitrogen replacement, mixed gas of fluorine gas and nitrogen gas is filled, and the fluorinated graphene is obtained under a certain condition.
Example three: based on the first embodiment, the difference from the first embodiment is that: preparing fluorinated graphene by taking graphene oxide as a raw material:
1. preparing fluorinated expanded graphite with high fluorine content from expanded graphite by a high-temperature gas-phase fluorination method, stripping the fluorinated expanded graphite/organic composite material by taking an organic matter as an intercalation agent by a stripping method to obtain a fluorinated graphene dispersion solution, and finally performing centrifugal separation, washing and drying on a target product to obtain the multilayer fluorinated graphene.
2. A solid stripping method assisted by melamine is developed to synthesize fluorinated graphene nanosheets, a ball mill grinds a mixture for 6h at a speed of 80rpm under an argon atmosphere, then deionized water is used for removing the melamine in the product to obtain a centrifugal product, and the centrifugal product is washed and dried by ethanol to obtain micron-sized ultrathin fluorinated nanosheets, wherein most of the thickness of the micron-sized ultrathin fluorinated nanosheets is less than 2nm. The research shows that melamine molecules on the surface are dispersedly adsorbed on the surface of the graphite fluoride, and Van der Waals interaction between graphite fluoride layers is effectively weakened. Under the condition of proper solid ball milling, the melamine-assisted graphite fluoride stripping method is simple, convenient, feasible and efficient, has wide prospect, provides opportunities for the field-winning ultrathin graphite fluoride nanosheets,
3. mixing PvP and graphite fluoride, and adding a certain amount of isopropanol as a dispersing agent to prepare the low-layer fluorinated graphene sheet with a high thickness-diameter ratio (ratio of sheet size to sheet thickness). Compared with graphite fluoride, the graphite fluoride used as the lubricant additive can more effectively improve the wear resistance of the lubricant,
4. method for preparing fluorinated graphene by liquid phase exfoliation, and method for preparing Fluorinated Graphite (FGR), C by taking cationic surfactant Cetyl Trimethyl Ammonium Bromide (CTAB) as exfoliating agent 16 H 33 (CH 3 ) 3 N + (CTA + ) The executing group can generate strong electrostatic adsorption on the fluorine group in the FGR, and has certain electronegativity. CTA + The intercalation of cations can enlarge the interplanar spacing between adjacent FGR layers, CTAB can also reduce surface tension and surface energy, and eliminate trap states through chemical interaction forces during the preparation process. The FGS luminescence of this study covers the entire visible spectrum, indicating broad application in many areas of lighting,
5. the method comprises the following steps of (1) stripping graphite fluoride with the aid of ammonia borane, mixing the graphite fluoride with the ammonia borane, successfully stripping FG under the condition of solid ball milling, and then washing with an ethanol solution, thereby removing the ammonia borane from a generated product. Analyzing and testing NH adsorbed on the surface of graphite fluoride on the surface 3 BH 3 The molecules can weaken van der waals interactions between adjacent fluorinated graphene sheets.
The Epoxy resin has a structure that an Epoxy group (Epoxy epoxide) is a cyclic structure consisting of one oxygen atom and two carbon atoms, has high activity and is an active reaction group, and the special structure enables the curing form of the Epoxy resin to tend to diversify. The epoxy resin is formed by polycondensation of phenol and epoxy chloropropane under the action of an alkaline catalyst, and can form a three-dimensional cross-linked network cured product under appropriate reagents and environmental conditions. Epoxy resins are generally classified by their chemical structure into glycidyl ether (ester, amine) type, aliphatic and alicyclic epoxy compounds. The bisphenol a epoxy resin is the most widely used one of all epoxy resins, and is prepared by condensation polymerization of diphenol propane (bisphenol a, BPA) and Epichlorohydrin (ECH), and the structural formula of the bisphenol a epoxy resin is shown in fig. 1, and as can be seen from the above chemical structural formula, the bisphenol a epoxy resin has the following characteristics:
(1) the active epoxy groups are at both ends of the molecular structure,
(2) has a plurality of benzene ring structures in the molecular structure, endows the product with good tolerance,
(3) the molecular structure contains a large number of ether bond structures, isopropyl and methyl,
(4) when the polymerization degree n is large, a large number of secondary hydroxyl groups are present in the molecular chain.
Example four: using nitrogen trifluoride (NF) 3 ) The gas reacts with Graphene Oxide (GO) to prepare Fluorinated Graphene (FG), and then the FG is added into epoxy resin to prepare different composite materials. The surface appearance, microstructure, coating protection performance and corrosion protection performance of different FGs are researched through detection equipment such as SEM and electrochemical workstation. The results show that the corrosion resistance of the FG/EP coating is improved by 3 orders of magnitude compared with the EP coating after FG is added into the epoxy resin matrix, and the low-frequency impedance modulus of the FG/EP coating is as high as 7.27 multiplied by 10 10 Ω·cm -2， However, the corrosion resistance of FG/EP coatings shows an increase and then a decrease with increasing fluorine content. Therefore, the addition of FG obviously improves the hydrophobicity and the barrier property of the epoxy resin matrix, and is beneficial to improving the long-term corrosion resistance of the coating.
The influence of Fluorinated Graphene (FG) addition on the corrosion resistance of epoxy resin (EP) coatings was explored. Research and analysis show that the FG modified EP resin has better dispersion stability, improves the mechanical property of the coating, improves the hydrophobicity and shielding property of the coating, can form a labyrinth effect in the coating, and obviously improves the long-term protective property of the coating under the double action of the hydrophobicity and the labyrinth effect.
Researches find that the orderly filled FGO can obviously improve the thermal property and the mechanical property of the F-EP, and the modification effect is better than that of the disorderly filled FGO. When the interlayer spacing of FGO is about 9nm. The elastic modulus, glass transition temperature, thermal expansion coefficient and thermal conductivity of FGO are all improved, and the effect is best. In addition, micro parameters of different systems are calculated, the influence mechanism of ordered filling and FGO layer spacing on F-EP performance is analyzed, and FGO is considered to be capable of binding F-EP molecules on two sides of the nanosheet, so that the movement capability of the molecular chain segment of the material is reduced, and the enhancement effect is achieved. The research result can provide a new idea for the development of the high-performance epoxy nanocomposite.
Fluorinated Graphene (FG) is used as a filler in WEP to improve its barrier properties, which contributes to the improvement of corrosion resistance, and the chemical composition and microstructure of FG and FG-modified WEP are systematically analyzed and studied for corrosion resistance. The result shows that the tensile strength of the WEP coating can be obviously improved by adding the FG sheet into the WEP, the barrier property of the WEP coating can be improved, a corrosive agent is prevented from permeating into an interface between the coating and a substrate, and meanwhile, the research result also shows that the fluorine content has obvious influence on the mechanical property and long-term corrosion resistance of the FG modified WEP coating, and the performance of the coating is deteriorated along with the increase of the fluorine content.
The fluorinated graphene modified epoxy resin coating (FG/EP) is prepared by researching the improvement degree of the performance of the fluorinated graphene modified epoxy resin coating layer. Through various analyses of the method described in the literature, the preparation process of the graphene oxide is mature, low in cost and high in safety. Regarding the fluorination process, the hydrothermal method is simple to operate and low in energy consumption, and the appropriate fluorinating agent is selected for safely and controllably fluorinating the epoxy resin. Therefore, firstly, graphite is used as a raw material, an improved Hummers method is adopted to prepare graphene oxide, then the graphene oxide is used as a raw material, a hydrothermal method is adopted to fluorinate the graphene oxide to prepare fluorinated graphene, and the structure and the microstructure of the fluorinated graphene are characterized by adopting FTIR (Fourier transform infrared spectroscopy), XRD (X-ray diffraction), SEM (scanning Electron microscope) and other testing means. FG/EP was prepared and subjected to corrosion testing under different conditions.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (3)
1. A preparation method of a fluorinated graphene modified epoxy resin coating is characterized by comprising the following steps: the method comprises the following steps:
s1: preparing experimental medicines and experimental instruments;
s2: preparing graphene oxide by an improved hummers method;
s2.1: preparing pre-oxidized graphite: weighing 10g of graphite powder, 4g of potassium persulfate and 10g of phosphorus pentoxide, sequentially adding the graphite powder, 4g of potassium persulfate and 10g of phosphorus pentoxide into a beaker filled with 24mL of sulfuric acid in a fume hood under the condition of stirring, transferring the beaker into a thermostat water bath kettle debugged in advance at 60 ℃ after no gas is produced, reacting for 3h, transferring the beaker into the thermostat water bath kettle debugged in advance at 25 ℃ after the reaction is finished for 5h, then adding a small part of deionized water to dilute sulfuric acid, performing suction filtration, washing with a large amount of deionized water while performing suction filtration to be neutral, and drying at normal temperature to obtain pre-oxidized graphite;
s2.2: preparing graphite oxide: weighing 1g of pre-oxidized graphite, adding the pre-oxidized graphite into a beaker filled with 25mL of sulfuric acid, immediately stirring to uniformly disperse the pre-oxidized graphite, putting the beaker into an ice water bath, adding 3g of potassium permanganate after the pre-oxidized graphite is completely dissolved, reacting for 2 hours, moving the beaker into a constant-temperature water bath kettle at 35 ℃ for reacting for 40 minutes, then adding 46mL of deionized water, finally adding 140mL of 2, continuing to react for 1 hour at 35 ℃, finally dropwise adding 30% of H2O2 until no gas is generated, enabling the solution to become bright yellow, centrifuging and filtering while hot, washing the solution to be neutral by using a large amount of 5% hydrochloric acid and deionized water, pouring the final precipitate into a culture dish after 1 hour of ultrasonic oscillation, and drying for 24 hours at 90 ℃ to obtain flaky Graphite Oxide (GO);
s3: preparing fluorinated graphene:
s3.1: weighing 50mg of graphene oxide sample, adding the graphene oxide sample into a beaker containing 40mL of deionized water, placing the beaker in an ultrasonic oscillation cleaner for ultrasonic treatment for 30min to form uniform graphene oxide dispersion liquid, then adding 10mL of hydrofluoric acid (HF) into the dispersion liquid, transferring the dispersion liquid into a hydrothermal kettle with a polytetrafluoroethylene lining, screwing the hydrothermal kettle to seal the hydrothermal kettle, then placing the hydrothermal kettle in an oven, carrying out heat treatment at 160 ℃ for 12h, naturally cooling the hydrothermal kettle to room temperature after the reaction is finished, directly evaporating the solution to obtain a solid, obtaining a fluorinated graphene sample to be tested,
s3: preparing a fluorinated graphene modified epoxy resin coating,
s3.2: preparing a metal matrix: the experimental metal matrix is Q235 carbon steel sheet, the size is 50mm multiplied by 25mm multiplied by 2mm, the Q235 carbon steel sheet is respectively polished by water abrasive paper with different specifications (180 #, 400#, 600#, 1000 #), ultrasonically deoiled by acetone, and dried for standby; preparing a fluorinated graphene modified epoxy resin coating,
s3.3: adding the FG and the epoxy resin into a beaker according to the mass ratio of 1: 200, uniformly mixing and stirring for 5min, and mixing the materials according to the weight ratio of a wetting dispersant: adhesive force dispersing agent: leveling agent =8:4:1, adding 20g of post-assistant in a mass ratio of 1, performing ultrasonic dispersion for 2 hours to uniformly disperse the fluorinated graphene and the assistant into epoxy resin, then adding a polyamide curing agent in a mass ratio of 2: 1 of the epoxy resin and the polyamide curing agent, uniformly stirring, uniformly coating the cured mixture on the surface of a pretreated carbon steel sheet, standing at room temperature for 12 hours, transferring the mixture to a drying oven at 60 ℃ for drying for 12 hours to obtain a fluorinated graphene modified epoxy resin coating, expressing FG/EP, preparing an epoxy varnish coating according to the same curing conditions, expressing EP,
s4: testing the fluorinated graphene modified epoxy resin coating;
s4.1: fourier infrared spectroscopy (FTIR): qualitative and quantitative analysis can be carried out on the sample through infrared spectroscopy, whether the prepared fluorinated graphene is successfully doped with fluorine can be proved, the spectrum scanning range is 4000cm < -1 > to 500cm < -1 >, samples are prepared by a KBr tablet pressing method,
S4.2X-ray diffraction (XRD): the method comprises the following steps of irradiating a sample with X-rays to generate diffraction peaks with different intensities at different angles, and analyzing a diffraction pattern of each substance to obtain a unique diffraction pattern generated by the substance, wherein the unique diffraction pattern is determined by the composition, crystal form, molecular configuration, intramolecular bonding mode and the like of the sample substance, and further judging whether the prepared graphene fluoride is successfully prepared, and the crystal face spacing of the graphene fluoride is calculated by Bragg diffraction law (lambda =2d sin theta) to obtain a scanning range: 3 to 80 degrees,
s4.3: adhesion test of the coating: the adhesive force of the coating represents the binding capacity between metal and the coating, the coating not only needs the hardness and compactness of the coating, but also needs to be closely attached to a substrate, when the self condensation force of the coating is reduced, a corrosive medium can contact the substrate through the coating to accelerate electrochemical corrosion reaction, the good adhesive force can prevent the penetration of the corrosive medium, further the electrochemical corrosion reaction between the corrosive medium and the metal is prevented, the test adopts a cross-cut method to test the adhesive force of the graphene oxide modified epoxy resin coating, and refers to the adhesive force evaluation level of the national standard coating,
s4.4: and (3) testing the corrosion resistance of the coating: EP and FG/EP were coated on a Q235 carbon steel sheet, and immersed in 3 groups of strong acid, 3.5% NaCl electrolyte, and strong acid for 20 days, respectively, and changes in surface corrosion morphology before and after coating were observed under a Scanning Electron Microscope (SEM).
2. The method for preparing a fluorinated graphene modified epoxy resin coating according to claim 1, wherein the method comprises the following steps: the experimental medicine comprises natural graphite powder, potassium persulfate, phosphorus pentoxide, sulfuric acid, potassium permanganate, hydrogen peroxide, hydrofluoric acid, epoxy resin E51, polyamide, an adhesion auxiliary agent, a wetting dispersing agent 2150, a leveling agent 310 and acetone.
3. The method for preparing a fluorinated graphene modified epoxy resin coating according to claim 1, wherein the method comprises the following steps: the experimental apparatus comprises an electric centrifuge, an ultrasonic cleaner, an electronic balance, a coating thickness gauge, a constant-temperature drying box, a scanning electron microscope and an X-ray diffractometer.
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| CN115818974A (en) * | 2022-12-26 | 2023-03-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
| CN115818974B (en) * | 2022-12-26 | 2024-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
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| CN103288069A (en) * | 2013-05-10 | 2013-09-11 | 西北工业大学 | Method for preparing fluorinated graphene through microwave hydrothermal method |
| CN111451107A (en) * | 2020-04-08 | 2020-07-28 | 四川轻化工大学 | Preparation method of high-adhesion and high-corrosion-resistance fluorinated graphene coating |
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| CN103288069A (en) * | 2013-05-10 | 2013-09-11 | 西北工业大学 | Method for preparing fluorinated graphene through microwave hydrothermal method |
| CN111451107A (en) * | 2020-04-08 | 2020-07-28 | 四川轻化工大学 | Preparation method of high-adhesion and high-corrosion-resistance fluorinated graphene coating |
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| CN115818974A (en) * | 2022-12-26 | 2023-03-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
| CN115818974B (en) * | 2022-12-26 | 2024-04-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for generating graphene coating on glass surface |
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