A mxene-based deicing superhydrophobic coating, coating and preparation method and coating application

Abstract

The application relates to an MXene-based deicing super-hydrophobic coating, a coating layer and a preparation method and coating application, the coating comprising the following components in percentage by mass: 2-5% of super-hydrophobic modified MXene photothermal material, 2-5% of epoxy resin, 0.5-1.5% of an epoxy resin curing agent, 0.5-1.5% of PDMS, 0.05-0.15% of a PDMS curing agent and 80-90% of a diluent; wherein the super-hydrophobic modified MXene photothermal material is a MXene powder treated by fluorine-free long-chain silane; the application uses MXene with excellent light-heat conversion performance as a photothermal material, carries out low-surface-energy hydrophobic modification on the MXene material by using fluorine-free long-chain silane, avoids environmental pollution caused by perfluoro or polyfluoro organic compounds, integrates the advantages of the super-hydrophobic coating and the photothermal coating, and realizes passive ice prevention and active photothermal deicing of the MXene-based deicing super-hydrophobic coating.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of super-hydrophobic coating anti-icing and de-icing, and particularly relates to a de-icing super-hydrophobic coating based on MXene, a coating, and a preparation method and application thereof. BACKGROUND

[0002] Ice formation is a ubiquitous and inevitable phenomenon in nature. However, for outdoor equipment or devices such as highways, power lines and wind power equipment, surface icing can bring major safety challenges and economic losses. In the past few decades, many anti-icing / de-icing strategies have been tried, such as electric or steam heating to melt ice, chemical de-icing and mechanical vibration de-icing. However, these methods are usually high in energy consumption, low in cost-effectiveness or harmful to the environment, and cannot meet the growing requirements of low carbon emissions and ecosystem protection.

[0003] In recent years, passive anti-icing technology has received increasing attention as an effective anti-icing strategy. Passive anti-icing technology aims to reduce surface ice, relying only on the super-hydrophobic or anti-icing properties of the material inside to reduce external intervention and save costs. For example, super-hydrophobic coatings (SHC) inspired by lotus leaves and slippery liquid-infused porous surfaces (SLIPS) inspired by pitcher plants, both of which not only have good ice delay and anti-icing properties, but also are low in energy consumption and friendly to the environment. However, the lubricant in SLIPS can be lost over time, causing SLIPS to lose its anti-icing properties and making it unsuitable for long-term practical applications. Super-hydrophobic coatings mainly rely on the synergistic effect of micro-nano structures and low surface energy to reduce the contact area and contact time of water droplets with the surface, greatly extending the ice formation time, thus having excellent passive anti-icing ability. However, the micro-nano structure of the super-hydrophobic surface is very fragile and can cause the surface to lose its long-lasting anti-icing ability. More importantly, the ice formation behavior in a low-temperature and high-humidity environment can cause mechanical interlocking between the ice and the surface micro-nano structure and a significant increase in ice adhesion strength, thus causing the surface to lose its anti-icing ability. Therefore, there is an urgent need to find a more efficient and more durable de-icing strategy.

[0004] Therefore, the present application provides a de-icing super-hydrophobic coating based on MXene that can both passively prevent ice and actively remove ice by photothermal de-icing, as well as a preparation method and application thereof. SUMMARY

[0005] In view of the problems of difficult de-icing, low efficiency and high cost of outdoor devices in the prior art, the present application provides a de-icing super-hydrophobic coating based on MXene that can both passively prevent ice and actively remove ice by photothermal de-icing, as well as a preparation method and application thereof.

[0006] Firstly, the application provides a deicing super-hydrophobic coating based on MXene, comprising the following components in mass percentage: super-hydrophobic modified MXene photothermal material 2-5%, epoxy resin 2-5%, epoxy resin curing agent 0.5-1.5%, PDMS 0.5-1.5%, PDMS curing agent 0.05-0.15%, diluent 80-90%;

[0007] The super-hydrophobic modified MXene photothermal material is a fluorine-free long-chain silane treated MXene powder.

[0008] The epoxy resin is one of epoxy resins E-44, E-51, E-20 and E-42.

[0009] The epoxy resin curing agent is one of 593 curing agent, polyether amine 230 curing agent and T-31 curing agent.

[0010] The PDMS and the PDMS curing agent are Dow Corning DC184 main agent and corresponding curing agent.

[0011] The diluent is one or more of ethyl acetate, butyl acetate, toluene, acetone and n-hexane.

[0012] The fluorine-free long-chain silane includes hexadecyl trimethoxysilane, octadecyl trimethoxysilane or dodecyl trimethoxysilane.

[0013] Secondly, the application further provides a preparation method of the deicing super-hydrophobic coating based on MXene, comprising the following steps:

[0014] S1 preparation of MXene

[0015] After mixing concentrated HCl and water into a hydrochloric acid solution, LiF is added into the hydrochloric acid solution and stirred and mixed, and then Ti3AlC2 is slowly added into the above mixture, the container is sealed and placed in a water bath at 35-45 DEG C and stirred for 18-36 h.

[0016] The above reaction mixture is centrifuged and washed with ultrapure water until the supernatant pH is greater than or equal to 6, the precipitate is collected and dispersed in ultrapure water, and then ultrasonic is performed under the condition of ice water bath for 1-2 h to obtain a MXene suspension,

[0017] The above suspension is centrifuged to obtain a MXene colloid, which is vacuum freeze-dried for 24-48 h to obtain a MXene powder.

[0018] S2 preparation of super-hydrophobic modified MXene photothermal material

[0019] The MXene powder prepared in S1 is added to a fluorine-free long-chain silane-containing ethanol solution, and stirred at room temperature for 12-24 h, and after centrifugal treatment, the supernatant is removed and vacuum freeze-dried for 24-48 h to obtain the super-hydrophobic modified MXene photothermal material;

[0020] S3 Preparation of a MXene-based deicing super-hydrophobic coating

[0021] The diluent is divided into two portions, the super-hydrophobic modified MXene photothermal material prepared in S2 is added to one portion of the diluent, and stirred until uniformly dispersed; the epoxy resin and PDMS are added to the other portion of the diluent, and stirred until uniformly dispersed; the two portions of the diluent are mixed, and the epoxy resin curing agent and PDMS curing agent are added, and stirred again until uniformly dispersed, to obtain the MXene-based deicing super-hydrophobic coating.

[0022] The mass percentage of each component is: super-hydrophobic modified MXene photothermal material 2-5%, epoxy resin 2-5%, epoxy resin curing agent 0.5-1.5%, PDMS 0.5-1.5%, PDMS curing agent 0.05-0.15%, and diluent 80-90%.

[0023] In S1, the concentration of the hydrochloric acid solution is 9 mol / L, and the mass ratio of LiF to Ti3AlC2 is (1-1.6):1.

[0024] In S2, the mass ratio among the MXene powder, long-chain silane and diluent is (1-2):(1-2):50.

[0025] The epoxy resin is one of epoxy resins E-44, E-51, E-20 and E-42;

[0026] The epoxy resin curing agent is one of 593 curing agent, polyether amine 230 curing agent and T-31 curing agent;

[0027] The PDMS and the PDMS curing agent are Dow Corning DC184 main agent and corresponding curing agent;

[0028] The diluent is one or more of ethyl acetate, butyl acetate, toluene, acetone and n-hexane.

[0029] The fluorine-free long-chain silane includes hexadecyl trimethoxysilane, octadecyl trimethoxysilane or dodecyl trimethoxysilane.

[0030] Further, the present application also provides a MXene-based deicing super-hydrophobic coating prepared by using the MXene-based deicing super-hydrophobic coating as described above.

[0031] Furthermore, the present invention also provides a method for preparing an MXene-based de-icing superhydrophobic coating, wherein the prepared superhydrophobic coating is sprayed onto a substrate by a spraying method, and after constant temperature curing, an MXene-based de-icing superhydrophobic coating with passive anti-icing and active photothermal de-icing is obtained.

[0032] Pre-treat the substrate before spraying: sand the substrate with sandpaper, and then ultrasonically clean it with ethanol and ultrapure water; during spraying, the spraying pressure of the spray gun is 2 bar to 4 bar, the nozzle diameter of the spray gun is 0.3 to 0.8 mm, and the distance between the nozzle and the substrate is 15 to 20 cm.

[0033] Finally, the present invention provides an application of an MXene-based de-icing superhydrophobic coating, which applies the MXene-based de-icing superhydrophobic coating described above to the aerospace field, wind power generation, wires and cables, or other power facilities.

[0034] The technical solution of this invention has the following advantages:

[0035] 1. In this invention, MXene is used as a photothermal material, which has excellent photothermal conversion performance. The MXene material is modified with low surface energy hydrophobicity using fluorine-free long-chain silanes, avoiding the pollution of the environment by perfluorinated or polyfluorinated organic compounds. At the same time, the photothermal performance and superhydrophobic performance are integrated, simplifying the process and integrating the advantages of superhydrophobic coating and photothermal coating. It is also more energy-saving and environmentally friendly than traditional de-icing technology.

[0036] 2. This invention uses epoxy resin as an adhesive to firmly adhere the superhydrophobic modified MXene photothermal material to the substrate. PDMS is used as an auxiliary adhesive to reduce the surface energy of the coating, achieving long-term maintenance of superhydrophobicity and forming an epoxy-PDMS dynamic bonding network, avoiding the functional limitations of a single adhesive. During use, uniform coating is achieved by controlling particle size and adjusting spraying parameters. The operation is simple and suitable for various substrates such as metals, glass, and composite materials.

[0037] 3. The MXene-based superhydrophobic coating prepared in this invention exhibits excellent passive anti-icing and photothermal active de-icing performance. It effectively delays icing time in low-temperature, light-free environments of -10℃ and -20℃, and further extends icing time under illumination. Photothermal heating and de-icing experiments show that under a solar irradiance of 100 mW / cm², the coating can effectively delay icing time. 2 Under these conditions, the surface temperature of the coating rises rapidly, and the frost and ice on the coating surface melt quickly. Even under lower ambient temperatures and weaker light intensity, the coating still has good anti-icing and de-icing properties.

[0038] 4. The MXene-based de-icing superhydrophobic coating prepared by this invention has excellent chemical stability and mechanical durability. It can still maintain superhydrophobic properties under conditions such as repeated tape peeling, cyclic sandpaper abrasion, water jet impact, sand and gravel impact, and strong acid and alkali / corrosion, and is suitable for application in harsh environments.

[0039] 5. The method for preparing an MXene-based de-icing superhydrophobic coating provided by the present invention uses fluorine-free long-chain silane to modify MXene, thereby achieving integrated photothermal and superhydrophobic properties. The method is simple, controllable, and low-cost, laying a technical foundation for large-scale industrial production and commercial promotion. Attached Figure Description

[0040] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are one application of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0041] Figure 1 The diagrams show the water contact angles of the MXene-based de-icing superhydrophobic coating described in Embodiment 1 of the present invention and the blank aluminum plate in Comparative Example 1, where (a) is the water contact angle of the blank aluminum plate and (b) is the water contact angle of the MXene-based de-icing superhydrophobic coating.

[0042] Figure 2 The de-icing superhydrophobic coating based on MXene described in Example 1 of this invention, as well as Examples 8, 9, and the blank aluminum plate in Comparative Example 1, were tested at 100 mW / cm². 2 Temperature rise curve under illumination intensity conditions;

[0043] Figure 3 The temperature rise and fall curves of the MXene-based de-icing superhydrophobic coating described in Embodiment 1 of the present invention during 10 photothermal heating / cooling cycle tests;

[0044] Figure 4 The images show a comparison of the icing start and end of the MXene-based de-icing superhydrophobic coating described in Example 1 of the present invention and the blank aluminum plate in Comparative Example 1 under -20℃ conditions.

[0045] Figure 5 The de-icing superhydrophobic coating based on MXene described in Example 1 of this invention and the blank aluminum plate in Comparative Example 1 are compared at -20℃ and 100 mW / cm². 2 Comparison of the start and end of ice droplet melting under light intensity conditions;

[0046] Figure 6The de-icing superhydrophobic coating based on MXene described in Example 1 of this invention and the blank aluminum plate in Comparative Example 1 are compared at -20℃ and 100 mW / cm². 2 Comparison of the start and end of ice melting under light intensity conditions;

[0047] Figure 7 The de-icing superhydrophobic coating based on MXene described in Example 1 of this invention and the blank aluminum plate in Comparative Example 1 are compared at -20℃ and 100 mW / cm². 2 Comparison of the start and end of frost melting under light intensity conditions;

[0048] Figure 8 The image shows the contact angle change on 800-grit sandpaper used for the MXene-based de-icing superhydrophobic coating obtained in Example 1 of this invention during 200 wear tests (each wear distance was 10 cm) under a 50 g load.

[0049] Figure 9 The MXene-based de-icing superhydrophobic coated cable and blank cable described in this invention operate at -20℃ and 100 mW / cm. 2 Comparison of the start and end of surface ice melting under light intensity conditions over 10 minutes. Detailed Implementation

[0050] To further illustrate the objectives, technical solutions, and advantages of the embodiments of the present invention, the technical solutions in the embodiments of the present invention will be described in detail below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Based on these embodiments of the present invention, all other embodiments obtained without creative effort are within the protection scope of the present invention.

[0051] Unless otherwise specified, all materials and reagents used in this invention are considered to be commercially available.

[0052] First, the present invention provides an MXene-based de-icing superhydrophobic coating comprising the following components by weight percentage: 2%–5% superhydrophobic modified MXene photothermal material, 2%–5% epoxy resin, 0.5%–1.5% epoxy resin curing agent, 0.5%–1.5% PDMS, 0.05%–0.15% PDMS curing agent, and 80%–90% diluent;

[0053] The superhydrophobic modified MXene photothermal material is MXene powder treated with fluorine-free long-chain silane;

[0054] The epoxy resin is one of epoxy resins E-44, E-51, E-20, and E-42;

[0055] The epoxy resin curing agent is one of 593 curing agent, polyetheramine 230 curing agent, and T-31 curing agent;

[0056] The PDMS and the PDMS curing agent are Dow Corning DC184 main agent and corresponding curing agent;

[0057] The diluent is one or more of ethyl acetate, butyl acetate, toluene, acetone, and n-hexane.

[0058] The fluorine-free long-chain silanes include hexadecyltrimethoxysilane, octadecyltrimethoxysilane, or dodecyltrimethoxysilane.

[0059] Secondly, this invention also provides a method for preparing an MXene-based de-icing superhydrophobic coating, comprising the following steps:

[0060] S1 Preparation of MXene

[0061] After mixing concentrated HCl with water to form a hydrochloric acid solution, LiF was added to the hydrochloric acid solution and stirred for 30 min. Then, Ti3AlC2 was slowly added to the above mixture. The container was sealed and placed in a 35℃ water bath and stirred for 18-36 h.

[0062] The above reaction mixture was washed by centrifugation with ultrapure water at 3500 rpm until the pH of the supernatant was ≥6. The precipitate was collected, dispersed in ultrapure water, and then sonicated in an ice-water bath for 1 h to obtain an MXene suspension.

[0063] The above suspension was centrifuged at 5000 r / min for 30 min to obtain MXene colloid, which was then freeze-dried under vacuum for 48 h to obtain MXene powder.

[0064] S2 Preparation of Superhydrophobic Modified MXene Photothermal Material

[0065] The MXene powder obtained by S1 was added to an ethanol solution containing fluorine-free long-chain silane, and the mixture was stirred at room temperature for 24 h. After centrifugation at 5000 r / min for 10 min, the supernatant was removed and the mixture was freeze-dried under vacuum for 24 h to obtain superhydrophobic modified MXene photothermal material.

[0066] S3 prepares MXene-based de-icing superhydrophobic coatings

[0067] Diluent was divided into two equal parts. The superhydrophobic modified MXene photothermal material prepared by S2 was added to one part of the diluent and stirred for 30 minutes until it was evenly dispersed. Epoxy resin and PDMS were added to the other part of the diluent and stirred for 10 minutes until it was evenly dispersed. After mixing the two parts of the diluent, epoxy resin curing agent and PDMS curing agent were added and stirred evenly again to obtain an MXene-based de-icing superhydrophobic coating.

[0068] The mass percentages of each component are as follows: superhydrophobic modified MXene photothermal material 2%–5%, epoxy resin 2%–5%, epoxy resin curing agent 0.5%–1.5%, PDMS 0.5%–1.5%, PDMS curing agent 0.05%–0.15%, and diluent 80%–90%.

[0069] In S1, the concentration of the hydrochloric acid solution is 9 mol / L, and the mass ratio of LiF to Ti3AlC2 is (1-1.6):1.

[0070] In S2, the mass ratio of the MXene powder, long-chain silane and diluent is (1-2):(1-2):50.

[0071] The epoxy resin is one of epoxy resins E-44, E-51, E-20, and E-42;

[0072] The epoxy resin curing agent is one of 593 curing agent, polyetheramine 230 curing agent, and T-31 curing agent;

[0073] The PDMS and the PDMS curing agent are Dow Corning DC184 main agent and corresponding curing agent;

[0074] The diluent is one or more selected from ethyl acetate, butyl acetate, toluene, acetone, and n-hexane.

[0075] The fluorine-free long-chain silanes include hexadecyltrimethoxysilane, octadecyltrimethoxysilane, or dodecyltrimethoxysilane.

[0076] Furthermore, the present invention also provides an MXene-based de-icing superhydrophobic coating, which is prepared using the MXene-based de-icing superhydrophobic coating described above.

[0077] Furthermore, the present invention also provides a method for preparing an MXene-based de-icing superhydrophobic coating, wherein the prepared superhydrophobic coating is sprayed onto a substrate by a spraying method, and the MXene-based de-icing superhydrophobic coating is obtained after curing in an oven at 60°C for 3 hours.

[0078] Pre-treat the substrate before spraying: sand the substrate with sandpaper, and then clean it ultrasonically with ethanol and ultrapure water; during spraying, the spraying pressure of the spray gun is 2 bar to 4 bar, the nozzle diameter of the spray gun is 0.5 mm, and the distance between the nozzle and the substrate is 15 to 20 cm.

[0079] Finally, the present invention provides an application of an MXene-based de-icing superhydrophobic coating, which applies the MXene-based de-icing superhydrophobic coating described above to the aerospace field, wind power generation, wires and cables, or other power facilities.

[0080] Example 1: This example relates to the specific preparation process of an MXene-based de-icing superhydrophobic coating, as follows:

[0081] S1: Mix 45 ml of concentrated HCl with 12 mol / L and 15 ml of ultrapure water to make a 9 mol / L hydrochloric acid solution, then add 4.8 g of LiF to the hydrochloric acid solution and stir for 30 min;

[0082] Then, slowly add 3.0 g of Ti3AlC2 to the above etching solution at a rate of 1.0 g / min; then seal the container and place it in a 35°C water bath and stir for 24 h.

[0083] The above reaction mixture was centrifuged and washed with ultrapure water until the pH of the supernatant was ≥6; the precipitate was collected and dispersed in ultrapure water, and then sonicated for 1 h under ice-water bath conditions to obtain MXene suspension; the above suspension was then centrifuged at 3500 r / min for 30 min to obtain MXene colloid, and further freeze-dried under vacuum for 48 h to obtain MXene powder.

[0084] S2: 2.0 g of MXene powder prepared by S1 was added to 50 ml of ethanol solution containing 1.0 g of hexadecyltrimethoxysilane. After stirring and reacting at room temperature for 24 h, the mixture was centrifuged at 5000 r / min for 10 min, the supernatant was removed and the mixture was freeze-dried under vacuum for 24 h to obtain superhydrophobic modified MXene photothermal material.

[0085] S3: Add 0.4 g of the superhydrophobic modified MXene photothermal material prepared in S2 to 5 ml of ethyl acetate and stir for 30 min until uniformly dispersed. Then add 0.4 g of epoxy resin and 0.1 g of PDMS to another 5 ml of ethyl acetate and stir for 10 min until uniformly dispersed. Then mix the two diluted solutions, add 0.1 g of 593 epoxy resin curing agent and 0.01 g of PDMS curing agent, and stir for 10 min until uniform to obtain an MXene-based de-icing superhydrophobic coating.

[0086] S4: The MXene-based de-icing superhydrophobic coating obtained in S3 was sprayed onto an aluminum plate and cured in a 60°C oven for 3 hours to obtain the MXene-based de-icing superhydrophobic coating.

[0087] Example 2: This example provides a coating, which differs from Example 1 in that the amount of LiF added in S2 is 3.0 g, while the other components and amounts are the same as in Example 1.

[0088] Example 3: This example provides a coating, which differs from Example 1 in that the amount of LiF added in S2 is 3.9 g, while the other components and amounts are the same as in Example 1.

[0089] Example 4: This example provides a coating, which differs from Example 1 in that the fluorine-free long-chain silane mentioned in S2 is octadecyltrimethoxysilane, while the other components and amounts are the same as in Example 1.

[0090] Example 5: This example provides a coating, which differs from Example 1 in that the fluorine-free long-chain silane mentioned in S2 is dodecyltrimethoxysilane, while the other components and amounts are the same as in Example 1.

[0091] Example 6: This example provides a coating, which differs from Example 1 in that the amount of hexadecyltrimethoxysilane added in S2 is 0.5 g, while the other components and amounts are the same as in Example 1.

[0092] Example 7: This example provides a coating that differs from Example 1 in that the amount of hexadecyltrimethoxysilane added in S2 is 2.0 g, while the other components and amounts are the same as in Example 1.

[0093] Example 8: This example provides a coating, which differs from Example 1 in that the amount of superhydrophobic modified MXene photothermal material added in S3 is 0.2 g, while the other components and amounts are the same as in Example 1.

[0094] Example 9: This example provides a coating, which differs from Example 1 in that the amount of superhydrophobic modified MXene photothermal material added in S3 is 0.6 g, while the other components and amounts are the same as in Example 1.

[0095] Comparative Example 1: This comparative example is a blank comparative example. The blank aluminum plate substrate was pretreated by sanding it with 800-grit sandpaper, then ultrasonically cleaning it with ethanol and ultrapure water for 5 minutes, and then drying it. This serves as the blank comparative example.

[0096] Comparative Example 2: This comparative example provides a coating that differs from Example 1 in that: S2 is missing, and the photothermal material used in S3 is unmodified MXene; the other components and amounts are the same as in Example 1.

[0097] Comparative Example 3: This comparative example provides a coating that differs from Example 1 in that the amount of epoxy resin and PDMS and their corresponding curing agents in S3 is doubled, while the other components and amounts are the same as in Example 1.

[0098] Experimental Example 1: Hydrophobicity Test: The water contact angles of the MXene-based de-icing superhydrophobic coatings prepared in each example and the comparative example were measured using a water contact angle meter (MIC-100S, optical contact angle meter). The results are shown in Table 1.

[0099] Table 1 Initial contact angle of coatings in each embodiment and comparative example

[0100]

[0101] Based on the data analysis in Table 1, we can conclude that:

[0102] The MXene-based de-icing superhydrophobic coatings prepared in Examples 1-5 all exhibit contact angles exceeding 150°, demonstrating excellent superhydrophobic properties. Figure 1 (For a direct comparison between Example 1 and a blank aluminum plate).

[0103] Effect of modifier dosage: In Example 6, the contact angle was only 138° due to insufficient addition of long-chain silane; In Example 7, although the amount of silane was increased, the improvement in hydrophobicity was limited, indicating that there was modification saturation.

[0104] Material ratio control: In Example 8, the contact angle dropped to 121° due to the low amount of MXene added (over-coating by resin / PDMS); In Example 9, the excessive addition of MXene did not significantly change the hydrophobicity, revealing the material dispersion threshold;

[0105] Key components of the system are missing: In Comparative Example 2, the unmodified MXene resulted in a contact angle of only 90°, while in Comparative Example 3, the contact angle remained at 120° due to the suppression of hydrophobic groups by excessive resin / PDMS.

[0106] Table 1 shows the results: the degree of silane grafting on the MXene surface and the material-binder ratio are crucial to the superhydrophobic performance of the coating; the MXene-based de-icing superhydrophobic coating provided by this invention has good superhydrophobic performance.

[0107] Experimental Example 2: Chemical Stability Test: The MXene-based de-icing superhydrophobic coatings prepared in each example and each comparative example were immersed in strong acid (pH=1), strong alkali (pH=13) and sodium chloride solutions, respectively. The hydrophobicity of each coating was measured after 24 h.

[0108] Table 2. Contact angles of coatings from various embodiments and comparative examples after 24 hours of immersion in acids, alkalis, and salts.

[0109]

[0110] Analysis of the data in Table 2 shows that:

[0111] The MXene-based de-icing superhydrophobic coatings prepared in Examples 1-5 maintained a contact angle of approximately 150° after being exposed to acid, alkali, and salt solutions for 24 hours.

[0112] After chemical immersion treatment, the contact angles of Examples 6 and 7 remained at 135-137° and 152-155°, respectively. In Example 8, due to insufficient MXene addition, the contact angle remained at 118-121° after chemical immersion treatment.

[0113] In Example 9, due to excessive MXene, the unfixed modified MXene structure in the coating was destroyed by acid and alkali solutions after chemical immersion treatment, resulting in the loss of superhydrophobicity and a decrease in contact angle to 141-142°.

[0114] Comparative Example 2 showed that the contact angle remained basically unchanged after chemical immersion treatment, while Comparative Example 3, due to the excessive addition of resin, had a stronger tolerance to chemical immersion treatment, and the contact angle remained at 119-121°.

[0115] The above chemical stability tests reflect that the MXene-based de-icing superhydrophobic coating described in this application has excellent chemical stability.

[0116] Experimental Example 3: Mechanical stability test: The MXene-based de-icing superhydrophobic coatings prepared in each example and each comparative example were subjected to 200 friction tests in the horizontal direction under a 50 g weight load (the friction distance was 10 cm each time).

[0117] Table 3 Contact angles after friction with coated sandpaper in each embodiment and comparative example

[0118]

[0119] Analysis of the data in Table 3 shows that:

[0120] The MXene-based de-icing superhydrophobic coatings prepared in Examples 1-5 maintained a contact angle of approximately 150° even after being abraded with sandpaper. Figure 8(This refers to the change in surface water contact angle during the sandpaper rubbing process in Example 1).

[0121] The hydrophobicity of Examples 6 and 7 decreased slightly after sandpaper abrasion, decreasing to 132° and 151° respectively;

[0122] In Example 8, due to insufficient MXene addition, the contact angle only decreased by 1° to 149° after sandpaper abrasion; while in Example 9, due to excessive MXene, most of the MXene in the coating was worn away after sandpaper abrasion, resulting in a significant decrease in the contact angle and loss of superhydrophobicity.

[0123] In Comparative Example 2, the contact angle decreased to 86° after sandpaper abrasion, while in Comparative Example 3, the surface roughness increased after sandpaper abrasion, thus increasing the contact angle to 124°.

[0124] The above sandpaper friction test reflects that the MXene-based de-icing superhydrophobic coating described in this invention has excellent mechanical stability.

[0125] Experiment Example 4: Photothermal Performance Test: Photothermal heating experiments were conducted on the MXene-based de-icing superhydrophobic coatings prepared in each example and on each comparative example; specifically, a light power meter (PL-MW 2000) was used to adjust the xenon lamp source (PLS-SXE300+) to one solar irradiance (100 mW / cm²). 2 The coating was vertically irradiated for 360 seconds, and the temperature change of the coating surface during the irradiation was measured using an infrared thermal imager (HIKMICROH21ProS+). The distance between the xenon lamp and the coating was 20 cm, and the ambient temperature was room temperature (16℃).

[0126] Table 4. Maximum Temperature of Photothermal Performance Tests for Coatings in Each Example and Comparative Example

[0127]

[0128] Analysis of the data in Table 4 shows that:

[0129] The MXene-based de-icing superhydrophobic coatings prepared in Examples 1-7 and Comparative Examples 2 and 3 showed a temperature increase from 16°C to 77.6-78.4°C after 360 s of irradiation with a xenon lamp simulating the intensity of sunlight, while the temperature of Comparative Example 1 only increased to 30.8°C.

[0130] In Example 8, due to insufficient MXene addition, the highest temperature after light exposure remained at 75.5°C, while in Example 9, due to excessive MXene, the highest temperature after light exposure reached 81.5°C. This indicates that the amount of MXene added is positively correlated with the photothermal performance of the coating, but excessive MXene does not produce a significant difference.

[0131] like Figure 2As shown, it is a temperature rise curve for photothermal performance testing of Examples 1, 8, 9 and Comparative Example 1; it can be seen from the figure that the MXene-based de-icing superhydrophobic coating of the present invention has excellent photothermal performance.

[0132] like Figure 3 As shown, the MXene-based de-icing superhydrophobic coating prepared in Example 1 still exhibits excellent photothermal performance after 10 photothermal heating / cooling cycles.

[0133] The above demonstrates that the MXene-based de-icing superhydrophobic coating of this invention exhibits excellent photothermal stability.

[0134] Experiment 5: Icing and Photothermal De-icing Performance Tests: Icing and photothermal de-icing performance tests were conducted on the MXene-based de-icing superhydrophobic coatings prepared in each example and the comparative examples using a cooling platform, a xenon lamp light source, and a power meter. Specifically, the cooling platform temperature was set to -20℃. The coating sample was placed on the cooling platform, and 10 μL of deionized water was dropped onto the coating surface. The freezing process and time were recorded under no-light conditions. The freezing time was defined as the time from the moment the water droplet came into contact with the surface until a small tip appeared on the top of the water droplet. Then, the xenon lamp light source was turned on, and the power meter was used to adjust the xenon lamp light source to one solar irradiance (100 mW / cm²). 2 Record the melting process and time. The de-icing time is defined as the time from when the xenon lamp light source irradiates the coating surface until the ice completely melts into a liquid state.

[0135] Table 5. Icing and defrosting times of coatings in each embodiment and comparative example.

[0136]

[0137] Table 5 shows the icing and solar-thermal de-icing performance tests:

[0138] The MXene-based de-icing superhydrophobic coatings prepared in Examples 1-5 exhibited an icing time of 523-553 s at -20℃ (compared to only 16 s for the blank aluminum plate) and a de-icing time of 271-295 s under illumination. The icing time was longer than the de-icing time, and no ice formed on the surface under illumination. Figure 4 , Figure 5 (The figures show a comparison of the icing process and the de-icing process for Example 1 and Comparative Example 1, respectively).

[0139] Example 6 (insufficient hydrophobic modification): freezing / de-icing times were 322 s / 310 s, indicating weakened performance; Example 7 (excess silane): freezing time was 544 s / de-icing time was 297 s, confirming that there is a modification threshold for hydrophobic modification.

[0140] Example 8 (insufficient MXene) showed a sharp drop in freezing time to 100 s (334 s for de-icing), exposing surface structural defects in the coating. Example 9 (excessive MXene) showed an extended freezing time to 584 s (237 s for de-icing), resulting in a small contact area between the coating and water droplets.

[0141] Comparative Example 2 (unmodified) iced for 27 s / de-iced for 303 s, and Comparative Example 3 (excess resin) iced for 39 s / de-iced for 270 s, demonstrating that the lack of the MXene-hydrophobic synergistic system cannot achieve effective anti-icing and de-icing.

[0142] The above icing and photothermal de-icing performance tests reflect that the MXene-based de-icing superhydrophobic coating described in this invention has excellent passive anti-icing and photothermal active de-icing performance.

[0143] Experiment Example 6: Photothermal De-icing and Defrosting Tests: Photothermal de-icing and defrosting tests were conducted on the MXene-based superhydrophobic coatings prepared in each example and on each comparative example using a cooling platform, a xenon lamp light source, and a power meter. Specifically, the cooling platform temperature was set to -20°C. The coating samples were placed on the cooling platform, and a 2 mm thick layer of ice / naturally formed frost was placed on top of the coating. Then, the xenon lamp light source was turned on, and the power meter was used to adjust the xenon lamp light source to one solar irradiance (100 mW / cm²). 2 Record the melting process and time of ice / frost layers.

[0144] Table 6. Icing and defrosting times of coatings in each embodiment and comparative example.

[0145]

[0146] Analysis of the data in Table 6 shows that:

[0147] The de-icing time of the MXene-based superhydrophobic coatings prepared in Examples 1-5 was between 536-559 s, and the defrosting time was between 88-98 s. Figure 6 , Figure 7 (The figures show a comparison of the icing process and the de-icing process for Example 1 and Comparative Example 1, respectively).

[0148] Although the silane content was changed in Examples 6 and 7, it had virtually no effect on the photothermal properties of MXene. Therefore, the difference in defrosting and de-icing times compared to Example 1 was small.

[0149] In Example 8, due to insufficient MXene addition, the de-icing time was significantly extended to 1549 s, and the defrosting time was also extended to 114 s;

[0150] Although an excessive amount of MXene was added in Example 9, the defrosting time and the de-icing time were only slightly reduced, to 510 s and 86 s, respectively.

[0151] Comparative Example 1 was a blank aluminum plate, which could not defrost and de-ice on its own under light conditions; Comparative Example 2 did not undergo hydrophobic modification of MXene, resulting in better contact between the water after the ice and frost melted and the coating, extending the freezing time to 987 s and the frosting time to 187 s, respectively; Comparative Example 3, due to the addition of excessive resin, caused the water after the ice melted to remain on the surface, extending the freezing time to 1335 s and the frosting time to only 100 s.

[0152] The above photothermal de-icing and defrosting test results demonstrate that the MXene-based de-icing superhydrophobic coating of this invention has excellent photothermal de-icing and defrosting performance.

[0153] Experimental Example 7: Cable De-icing Test: The substrate in Example 1 was replaced with a 2×1.5mm² cable, and the MXene-based de-icing superhydrophobic coating described in this invention was sprayed onto the surface of the cable. A blank cable was used for comparison.

[0154] Photothermal de-icing tests were conducted on coated and blank cables using a cooling platform, a xenon lamp source, and a power meter. Specifically, the cables were placed in centrifuge tubes filled with water, frozen in a refrigerator, and then placed on a cooling platform set to -20°C. The xenon lamp source was then turned on, and the power meter was used to adjust the xenon lamp source to one solar irradiance (100 mW / cm²). 2 Record the melting process of ice on the cable surface within 10 minutes.

[0155] like Figure 9 As shown, both coated and blank cables had ice layers on their surfaces before light exposure; however, after 10 minutes of light exposure, only a corner of the ice layer on the blank cable melted, while the ice layer on the coated cable surface melted almost completely, and the supercooled water on the surface slid off almost completely, indicating that the cable surface had good photothermal de-icing performance.

[0156] The above cable de-icing test results demonstrate that the MXene-based de-icing superhydrophobic coating described in this invention has good practical application effects and prospects.

[0157] Obviously, the above description is a preferred embodiment of this application, but it should not be construed as limiting the scope of this application. It should be noted that those skilled in the art can make several improvements and modifications without departing from the principles of this application, and these improvements and modifications are also considered to be within the scope of protection of this application.

Claims

1. A de-icing superhydrophobic coating based on MXene, characterized in that, It is composed of the following components by weight percentage: 2%–5% superhydrophobic modified MXene photothermal material, 2%–5% epoxy resin, 0.5%–1.5% epoxy resin curing agent, 0.5%–1.5% PDMS, 0.05%–0.15% PDMS curing agent, and 80%–90% diluent; The superhydrophobic modified MXene photothermal material is MXene powder treated with fluorine-free long-chain silane; The epoxy resin is one of epoxy resins E-44, E-51, E-20, and E-42; The epoxy resin curing agent is one of 593 curing agent, polyetheramine 230 curing agent, and T-31 curing agent; The PDMS and the PDMS curing agent are Dow Corning DC184 main agent and corresponding curing agent; The diluent is one or more selected from ethyl acetate, butyl acetate, toluene, acetone, and n-hexane; The fluorine-free long-chain silanes include hexadecyltrimethoxysilane, octadecyltrimethoxysilane, or dodecyltrimethoxysilane.

2. A method for preparing an MXene-based de-icing superhydrophobic coating, characterized in that, Includes the following steps: S1 Preparation of MXene After mixing concentrated HCl with water to prepare a hydrochloric acid solution, LiF was added to the hydrochloric acid solution and stirred. Then, Ti3AlC2 was slowly added to the above mixture. The container was sealed and placed in a water bath at 35-45°C and stirred for 18-36 hours. The above reaction mixture was centrifuged and washed with ultrapure water until the pH of the supernatant was ≥6. The precipitate was collected, dispersed in ultrapure water, and then sonicated in an ice-water bath for 1–2 hours to obtain an MXene suspension. The above suspension was centrifuged to obtain MXene colloid, which was then freeze-dried under vacuum for 24–48 h to obtain MXene powder. S2 Preparation of Superhydrophobic Modified MXene Photothermal Material The MXene powder obtained by S1 was added to an ethanol solution containing fluorine-free long-chain silane, and the mixture was stirred at room temperature for 12-24 h. After centrifugation, the supernatant was removed and the mixture was freeze-dried under vacuum for 24-48 h to obtain superhydrophobic modified MXene photothermal material. S3 prepares MXene-based de-icing superhydrophobic coatings Diluent was divided into two equal parts. The superhydrophobic modified MXene photothermal material prepared by S2 was added to one part of the diluent and stirred until it was evenly dispersed. Epoxy resin and PDMS were added to the other part of the diluent and stirred until it was evenly dispersed. After the two parts of the diluent were mixed, epoxy resin curing agent and PDMS curing agent were added and stirred evenly again to obtain an MXene-based de-icing superhydrophobic coating. The mass percentages of each component are as follows: superhydrophobic modified MXene photothermal material 2%–5%, epoxy resin 2%–5%, epoxy resin curing agent 0.5%–1.5%, PDMS 0.5%–1.5%, PDMS curing agent 0.05%–0.15%, and diluent 80%–90%; the fluorine-free long-chain silane includes hexadecyltrimethoxysilane, octadecyltrimethoxysilane, or dodecyltrimethoxysilane.

3. The method for preparing an MXene-based de-icing superhydrophobic coating according to claim 2, characterized in that, In S1, the concentration of the hydrochloric acid solution is 9 mol / L, and the mass ratio of LiF to Ti3AlC2 is (1-1.6):

1.

4. The method for preparing an MXene-based de-icing superhydrophobic coating according to claim 2, characterized in that, In S2, the mass ratio of the MXene powder, long-chain silane and diluent is (1-2):(1-2):

50.

5. The method for preparing an MXene-based de-icing superhydrophobic coating according to claim 2, characterized in that, The epoxy resin is one of epoxy resins E-44, E-51, E-20, and E-42; The epoxy resin curing agent is one of 593 curing agent, polyetheramine 230 curing agent, and T-31 curing agent; The PDMS and the PDMS curing agent are Dow Corning DC184 main agent and corresponding curing agent; The diluent is one or more of ethyl acetate, butyl acetate, toluene, acetone, and n-hexane.

6. A de-icing superhydrophobic coating based on MXene, characterized in that: It is prepared using the MXene-based de-icing superhydrophobic coating described in claim 1.

7. A method for preparing an MXene-based de-icing superhydrophobic coating, characterized in that: The superhydrophobic coating described in claim 1 is sprayed onto a substrate using a spraying method. After curing at a constant temperature, an MXene-based de-icing superhydrophobic coating with passive anti-icing and active photothermal de-icing is obtained.

8. The method for preparing an MXene-based de-icing superhydrophobic coating according to claim 7, characterized in that, Pre-treat the substrate before spraying: sand the substrate with sandpaper, and then ultrasonically clean it with ethanol and ultrapure water; during spraying, the spraying pressure of the spray gun is 2 bar to 4 bar, the nozzle diameter of the spray gun is 0.3 to 0.8 mm, and the distance between the nozzle and the substrate is 15 to 20 cm.

9. An application of an MXene-based de-icing superhydrophobic coating, characterized in that: The MXene-based de-icing superhydrophobic coating as described in claim 6 or the MXene-based de-icing superhydrophobic coating as described in claim 7 or 8 can be applied to aerospace, wind power generation, wire and cable or other power facilities.

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