An anti-icing hydrophobic coating and a preparation method thereof

Abstract

The application discloses an anti-icing and hydrophobic coating and a preparation method, and belongs to the technical field of anti-icing and hydrophobic coatings; aiming at the problems of failures and safety risks caused by infrastructure icing in a cold and humid environment, a long-acting and durable anti-icing and hydrophobic coating is developed; a modified Ti3SiC2 / ZnO hybrid powder is innovatively introduced; the powder is combined with ZnO modified by CTAB through surface modification, and cooperates with other components to form a coating system; an anti-icing and hydrophobic mechanism is based on nano rough nodes constructed by the powder to reduce solid-liquid contact; fluorine-containing silane modification endows with ultra-low surface energy to weaken ice crystal adsorption; experiments show that the coating can promote water drop rolling, significantly weaken ice adhesion and promote ice shedding, improve anti-icing and hydrophobic performance, has long-term stability and strong environmental adaptability, and is suitable for severe environments such as severe cold and humidity.

Description

Technical Field

[0001] This invention belongs to the technical field of anti-icing hydrophobic coatings, specifically referring to an anti-icing hydrophobic coating and its preparation method. Technical Background

[0002] Anti-icing and hydrophobic coatings are widely used in the protection of infrastructure in the power, aviation, transportation, and energy sectors to address severe icing problems in cold and humid environments. These environments are characterized by temperatures often below -10 degrees Celsius, high humidity, and frequent rain, snow, freezing rain, or rime, which cause objects to easily absorb supercooled water droplets and condense into ice. This leads to continuous accumulation of ice, significantly increasing the structural load on facilities, and potentially causing malfunctions or safety accidents, threatening the safety of critical infrastructure.

[0003] Current mainstream anti-icing hydrophobic coatings mainly rely on superhydrophobic properties to reduce ice adhesion. Their microstructure can delay icing and promote ice shedding. However, in practical applications, this technology faces significant challenges: the coating is prone to wear and cracking under external force or drastic temperature changes, leading to a decrease in hydrophobicity; in extreme weather conditions such as freezing rain and wet snow with high water droplet content or large water droplet diameter, the anti-icing effect is significantly weakened; in addition, on-site construction is difficult and the material cost is high.

[0004] Therefore, the market urgently needs to develop a new generation of anti-icing and hydrophobic coatings that are long-lasting, durable, and more environmentally adaptable to effectively address the challenges of icing in harsh environments. Summary of the Invention

[0005] In view of the above situation and to overcome the defects of the prior art, the present invention provides an anti-icing hydrophobic coating and a preparation method, which effectively solves the problems of insufficient durability and limited environmental adaptability of anti-icing hydrophobic coatings on the market.

[0006] The technical solution adopted in this invention is as follows: This invention proposes an anti-icing hydrophobic coating and its preparation method, comprising the following raw materials in parts by weight:

[0007] Hydroxyacrylate resin 20-40 parts, hydroxyl-terminated fluorinated polysiloxane 10-30 parts, hydrophobic migration agent 2-12 parts, modified Ti3SiC2 / ZnO hybrid powder 5-14 parts, silane coupling agent 0.1-0.2 parts, dispersant 1-3 parts, curing agent 1-10 parts, polypyrrole nanowires 1-2 parts, organic solvent 25-60 parts;

[0008] The method for preparing the modified Ti3SiC2 / ZnO hybrid powder includes the following steps:

[0009] Zinc acetate was dissolved in anhydrous ethanol / ethylene glycol methyl ether mixed solvent and reacted at 0℃ for 1 h to generate ZnO crystal nuclei. After reflux for 6 h, monodisperse microspheres were formed. The ZnO microspheres were ultrasonically dispersed in CTAB-ethanol solution, and Ti3SiC2 suspension was added. The mixture was heated and stirred for 2 h, concentrated to 1 / 3 of the original volume by vacuum distillation, and then transferred to a high-pressure reactor. After cooling, the product was collected by centrifugation, and unreacted substances were washed away with ethanol solution to obtain hybrid powder. The hybrid powder was vacuum dried and then subjected to steam reaction for further curing. Finally, the cured product was dry-mixed with a silane coupling agent under certain conditions to obtain modified Ti3SiC2 / ZnO hybrid powder.

[0010] Furthermore, the concentration range of the zinc acetate is 0.05–0.2 mol / L.

[0011] Furthermore, in the Ti3SiC2 suspension, the particle size range of Ti3SiC2 is 0.1–1.0 μm.

[0012] Furthermore, the heating and stirring temperature is 25-80℃, and the heating method is gradient heating.

[0013] Furthermore, the steam reaction uses fluorinated silane steam.

[0014] Preferably, the fluorinated silane vapor is one of perfluorooctyltriethoxysilane, tridecafluorooctyltrimethoxysilane, and trifluoropropyltrichlorosilane.

[0015] Furthermore, the steam reaction time is 30-60 minutes.

[0016] Preferably, the dispersant is one of a polymeric dispersant, a nonionic surfactant, or a polyacrylic acid dispersant.

[0017] Preferably, the hydrophobic migrating agent is one of perfluorooctyltrichlorosilane and perfluorooctyltriethoxysilane.

[0018] Furthermore, the aforementioned anti-icing hydrophobic coating and its preparation method include the following preparation steps:

[0019] Dispersant and hydrophobic migration agent are added to organic solvent and mixed evenly. Then, hydroxyl acrylic resin, hydroxyl-terminated fluorinated polysiloxane, polypyrrole nanowires, hydrophobic migration agent, and modified Ti3SiC2 / ZnO hybrid powder are added and mixed evenly. Finally, curing agent is added and mixed evenly to obtain anti-icing hydrophobic coating.

[0020] The beneficial effects achieved by the present invention using the above structure are as follows:

[0021] (1) Ti3SiC2 has good lubricity. By modifying the surface of Ti3SiC2 to a superhydrophobic surface, and further functionalizing it, a structure similar to SiO2 is formed. Combined with ZnO coated with CTAB surfactant, the surface energy is reduced together. Vacuum dehydration and steam reaction steps can form a thin layer with low surface energy on the powder surface. Then, by solidifying and stabilizing these low surface energy modified groups, the surface energy is further reduced, and the anti-icing hydrophobic ability is improved. In addition, Ti3SiC2, as a ceramic material, has the characteristics of corrosion resistance and wear resistance, which meets the durability requirements of anti-icing hydrophobic coatings.

[0022] (2) The monodisperse microspheres of ZnO have a certain roughness. The hybridization process introduces Ti3SiC2, which is attached to the ZnO microspheres during ultrasonic dispersion, gradient heating and stirring. This nanoscale rough structure can effectively trap air, form an air cushion, reduce the actual contact area between water droplets and solid surfaces, increase the contact angle and reduce the roll-off angle, and achieve excellent hydrophobicity.

[0023] (3) In low-temperature environments, supercooled water droplets falling on the surface of the anti-icing hydrophobic coating will slide off before freezing due to their easy rolling characteristics. Even if the water droplets freeze, the actual contact area between the ice layer and the anti-icing hydrophobic coating is reduced due to the residual air layer. The rough micro-nano structure causes the formed ice layer to have internal stress and pores. At the same time, the low surface energy chemical surface reduces the physical adsorption force between the ice crystal and the substrate. The combined effect of these factors leads to a significant reduction in the adhesion between the ice layer and the substrate, making the ice layer more prone to breakage and detachment, further enhancing the anti-icing hydrophobic ability. Attached Figure Description

[0024] Figure 1 The figures show the test results of the contact angle and roll-off angle of the anti-icing hydrophobic coatings of Examples 1-10 and Comparative Examples 1-3 of the present invention.

[0025] Figure 2 The figures show the test results of the anti-icing effect of the anti-icing hydrophobic coatings of Examples 1-10 and Comparative Examples 1-3 of the present invention.

[0026] Figure 3 The figures show the test results of the de-icing effect of the anti-icing hydrophobic coatings of Examples 1-10 and Comparative Examples 1-3 of the present invention.

[0027] Figure 4 The static water droplet contact angle and roll-off angle test results are shown in the figure for an anti-icing hydrophobic coating prepared in Example 7 of the present invention.

[0028] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used together with the embodiments of the invention to explain the invention and do not constitute a limitation thereof. Detailed Implementation

[0029] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0030] Example 1:

[0031] An anti-icing hydrophobic coating and its preparation method

[0032] First, modified Ti3SiC2 / ZnO hybrid powder was prepared: anhydrous ethanol and ethylene glycol methyl ether were mixed in a 1:1 volume ratio to form an anhydrous ethanol-ethylene glycol methyl ether mixed solvent. Then, 0.05 mol / L zinc acetate was dissolved in 200 mL of the anhydrous ethanol-ethylene glycol methyl ether mixed solvent, wherein the volume ratio of zinc acetate to the anhydrous ethanol-ethylene glycol methyl ether mixed solvent was 1:1. The solution was placed in a 0℃ ice-water bath, and 10 mL of 0.1 M NaOH ethanol solution was added dropwise while stirring to maintain a low temperature. The reaction was carried out at a low temperature for 1 hour to generate ZnO crystal nuclei. The mixture was then heated to 75–85℃ and refluxed for 6 hours to form monodisperse ZnO microspheres. The ZnO microspheres were dispersed in 100 mL of a CTAB-ethanol solution, and sonicated for 20 min at 200 W to allow CTAB to electrostatically adsorb onto the ZnO surface, forming a cation layer. 2.0 g of 0.1 μm Ti3SiC2 powder was added to 100 mL of anhydrous ethanol and sonicated for 30 min to form a stable suspension. The suspension was added to the CTAB-modified ZnO dispersion. In the first stage, the temperature was increased from 25℃ to 50℃ and held for 30 min. In the second stage, the temperature was increased from 50℃ to 70℃ and held for 1.5 h, promoting the electrostatic attraction between Ti3SiC2 nanosheets and ZnO microspheres. The mixture was then concentrated to one-third of its original volume by vacuum distillation at 60℃, and transferred to a high-pressure reactor with a filling degree ≤70%. After sealing, the temperature was programmed to rise from 25℃ to 150℃ and held for 4 h. After cooling, the product was collected by centrifugation. The material was washed three times with 50% ethanol solution to remove unreacted substances, resulting in a hybrid powder. The hybrid powder was spread evenly in a vacuum dryer and heated to 120°C for 2 hours to remove water. Steam containing perfluorooctyltriethoxysilane was injected into a steam reactor and the steam reaction was carried out for 30 minutes. The mixture was then placed in a drying oven and cured at 120°C. The cured product was then dry-mixed with a silane coupling agent at 110°C for 30 minutes to enhance the interfacial bonding force, resulting in modified Ti3SiC2 / ZnO hybrid powder.

[0033] Hydroxy-acrylic resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent are added in a ratio of 20:10:2:5:0.1:1:1:1:25. The polyacrylic acid dispersant (polyacrylate copolymer) and perfluorooctyltrichlorosilane are added to the organic solvent and mixed evenly. Then, the hydroxy-acrylic resin, hydroxyl-terminated fluorinated polysiloxane, polypyrrole nanowires, silane coupling agent, and modified Ti3SiC2 / ZnO hybrid powder are added and stirred evenly. Finally, the curing agent is added and mixed evenly to obtain an anti-icing hydrophobic coating.

[0034] Example 2:

[0035] An anti-icing hydrophobic coating and its preparation method

[0036] First, modified Ti3SiC2 / ZnO hybrid powder was prepared: anhydrous ethanol and ethylene glycol methyl ether were mixed in a 1:1 volume ratio to form an anhydrous ethanol-ethylene glycol methyl ether mixed solvent. Then, 0.1 mol / L zinc acetate was dissolved in 200 mL of the anhydrous ethanol / ethylene glycol methyl ether mixed solvent, wherein the volume ratio of zinc acetate to the anhydrous ethanol-ethylene glycol methyl ether mixed solvent was 1:1. The solution was placed in an ice-water bath at 0°C, and 10 mL of 0.1 M NaOH ethanol solution was added dropwise while stirring, maintaining the low temperature. After reacting for 1 hour, ZnO crystal nuclei are generated. The mixture is then heated to 75–85℃ and refluxed for 6 hours to form monodisperse ZnO microspheres. The ZnO microspheres are dispersed in 100 mL of CTAB-ethanol solution, and ultrasonically treated for 30 minutes at 200 W to allow CTAB to electrostatically adsorb onto the ZnO surface, forming a cation layer. 2.0 g of 0.5 μm Ti3SiC2 powder is added to 100 mL of anhydrous ethanol and ultrasonically dispersed for 30 minutes to form a stable suspension. The Ti3SiC2 suspension is then... The flotation solution was added to the CTAB-modified ZnO dispersion. In the first stage, the temperature was increased from 30℃ to 60℃ and held for 30 min. In the second stage, the temperature was increased from 60℃ to 80℃ and held for 1.5 h, promoting the electrostatic attraction between Ti3SiC2 nanosheets and ZnO microspheres. The mixture was then concentrated to one-third of its original volume by vacuum distillation at 60℃, and transferred to a high-pressure reactor with a filling degree ≤70%. After sealing, the temperature was programmed to rise from 30℃ to 160℃ and held for 4 h. After cooling, the product was collected by centrifugation. Unreacted material was removed by washing three times with 50% ethanol solution to obtain hybrid powder. The hybrid powder was spread evenly in a vacuum dryer and heated to 120°C for 2 hours to remove water. Steam containing tridecafluorooctyltrimethoxysilane was injected into a steam reactor and the steam reaction was carried out for 45 minutes. Then, it was placed in a drying oven and the temperature was set to 135°C for curing. The cured product was dry-mixed with a silane coupling agent at 110°C for 30 minutes to enhance the interfacial bonding force and obtain modified Ti3SiC2 / ZnO hybrid powder.

[0037] Hydroxy-acrylic resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent are added in a ratio of 30:20:6:10:0.15:2:5:1.5:45. First, nonionic surfactant (succinate block copolymer and complex) and perfluorooctyltrichlorosilane are added to the organic solvent and mixed evenly. Then, hydroxy-acrylic resin, hydroxyl-terminated fluorinated polysiloxane, polypyrrole nanowires, silane coupling agent, and modified Ti3SiC2 / ZnO hybrid powder are added and stirred evenly. Finally, curing agent is added and mixed evenly to obtain an anti-icing hydrophobic coating.

[0038] Example 3:

[0039] An anti-icing hydrophobic coating and its preparation method

[0040] First, modified Ti3SiC2 / ZnO hybrid powder was prepared: anhydrous ethanol and ethylene glycol methyl ether were mixed at a volume ratio of 1:1 to form an anhydrous ethanol-ethylene glycol methyl ether mixed solvent. Then, 0.2 mol / L zinc acetate was dissolved in 200 mL of the anhydrous ethanol / ethylene glycol methyl ether mixed solvent, wherein the volume ratio of zinc acetate to the anhydrous ethanol-ethylene glycol methyl ether mixed solvent was 1:1. The solution was placed in an ice-water bath at 0℃, and 10 mL of 0.1 M NaOH ethanol solution was added dropwise while stirring to maintain a low temperature. The reaction was carried out at a low temperature for 1 hour to generate ZnO crystal nuclei. The mixture was then heated to 75–85℃ and refluxed for 6 hours to form monodisperse ZnO microspheres. The ZnO microspheres were dispersed in 100 mL of CTAB-ethanol solution, and sonicated for 30 min at 300 W to allow CTAB to electrostatically adsorb onto the ZnO surface, forming a cation layer. 2.0 g of Ti3SiC2 powder with a particle size of 1.0 μm was added to 100 mL of anhydrous ethanol and sonicated for 30 min to form a stable suspension. The Ti3SiC2 powder was then further dispersed... 2. The suspension was added to the CTAB-modified ZnO dispersion. In the first stage, the temperature was increased from 35℃ to 65℃ and held for 30 min. In the second stage, the temperature was increased from 65℃ to 75℃ and held for 1.5 h, which promoted the bonding of Ti3SiC2 nanosheets with ZnO microspheres through electrostatic attraction. The mixture was concentrated to 1 / 3 of its original volume by vacuum distillation at 60℃, and then transferred to a high-pressure reactor with a filling degree ≤70%. After sealing, the temperature was programmed to rise from 25℃ to 150℃ and held for 4 h. After cooling, the mixture was collected by centrifugation. The product was washed three times with 50% ethanol solution to remove unreacted substances, yielding a hybrid powder. The hybrid powder was spread evenly in a vacuum dryer and heated to 120°C for 2 hours to dehydrate. Steam containing trifluoropropyltrichlorosilane was injected into a steam reactor and the steam reaction was carried out for 60 minutes. The product was then placed in a drying oven and cured at 150°C. The cured product was then dry-mixed with a silane coupling agent at 110°C for 30 minutes to enhance the interfacial bonding force, resulting in modified Ti3SiC2 / ZnO hybrid powder.

[0041] Hydroxy-acrylic resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent are added in a ratio of 40:30:12:14:0.2:3:10:2:60. The polymeric dispersant (polymethacrylic acid derivative) and perfluorooctyltriethoxysilane are added to the organic solvent and mixed evenly. Then, the hydroxy-acrylic resin, hydroxyl-terminated fluorinated polysiloxane, polypyrrole nanowires, silane coupling agent, and modified Ti3SiC2 / ZnO hybrid powder are added and mixed evenly. Finally, the curing agent is added and mixed evenly to obtain an anti-icing hydrophobic coating.

[0042] Example 4:

[0043] An anti-icing hydrophobic coating and its preparation method

[0044] Hydroxyacrylate resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent were added in a ratio of 20:10:2:8:0.1:1:1:1:25. The remaining components, component contents, and preparation process steps were the same as in Example 1.

[0045] Example 5:

[0046] An anti-icing hydrophobic coating and its preparation method

[0047] Hydroxyacrylate resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent were added in a ratio of 20:10:2:10:0.1:1:1:1:25. The remaining components, component contents, and preparation process steps were the same as in Example 1.

[0048] Example 6:

[0049] An anti-icing hydrophobic coating and its preparation method

[0050] Hydroxyacrylate resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent were added in a ratio of 20:10:2:12:0.1:1:1:1:25. The remaining components, component contents, and preparation process steps were the same as in Example 1.

[0051] Example 7:

[0052] An anti-icing hydrophobic coating and its preparation method

[0053] Hydroxyacrylate resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent were added in a ratio of 20:10:2:14:0.1:1:1:1:25. The remaining components, component contents, and preparation process steps were the same as in Example 1.

[0054] Example 8:

[0055] An anti-icing hydrophobic coating and its preparation method

[0056] Hydroxyacrylate resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent were added in a ratio of 20:10:2:16:0.1:1:1:1:25. The remaining components, component contents, and preparation process steps were the same as in Example 1.

[0057] Example 9:

[0058] An anti-icing hydrophobic coating and its preparation method

[0059] Hydroxyacrylate resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent were added in a ratio of 20:10:2:18:0.1:1:1:1:25. The remaining components, component contents, and preparation process steps were the same as in Example 1.

[0060] Example 10:

[0061] An anti-icing hydrophobic coating and its preparation method

[0062] Hydroxyacrylate resin, hydroxyl-terminated fluorinated polysiloxane, hydrophobic migration agent, modified Ti3SiC2 / ZnO hybrid powder, silane coupling agent, dispersant, curing agent, polypyrrole nanowires, and organic solvent were added in a ratio of 20:10:2:20:0.1:1:1:1:25. The remaining components, component contents, and preparation process steps were the same as in Example 1.

[0063] Comparative Example 1:

[0064] An anti-icing hydrophobic coating and its preparation method

[0065] The difference from Example 1 is that the coating prepared in Comparative Example 1 does not contain modified Ti3SiC2 / ZnO hybrid powder, but uses SiO2 powder instead.

[0066] Comparative Example 2:

[0067] An anti-icing hydrophobic coating and its preparation method

[0068] The difference from Example 1 is that the coating prepared in Comparative Example 1 does not contain modified Ti3SiC2 / ZnO hybrid powder, but uses SiC powder instead.

[0069] Comparative Example 3:

[0070] An anti-icing hydrophobic coating and its preparation method

[0071] The difference from Example 1 is that the coating prepared in Comparative Example 1 does not contain modified Ti3SiC2 / ZnO hybrid powder.

[0072] Experimental Example 1:

[0073] Contact angle and roll-off angle tests were conducted on the anti-icing hydrophobic coatings provided in Examples 1-10 and Comparative Examples 1-3: Anti-icing hydrophobic coating samples were prepared according to the preparation methods in Examples 1-10 and Comparative Examples 1-3, respectively. The samples were uniformly coated onto epoxy fiberboard to form a coating, placed in a constant temperature drying oven, and after the coating solidified, a drop of ultrapure water was added to the flat surface area of ​​each sample using a micro-syringe. The contact angle and roll-off angle of the anti-icing hydrophobic coating were measured using a fully automatic contact angle analyzer and a roll-off angle analyzer.

[0074] according to Figure 1 The test results showed that the contact angle and roll-off angle fluctuated regularly with changes in the formulation. In the comparative experiments of Examples 1-3 and Comparative Examples 1-3, the contact angle and roll-off angle of Comparative Examples 1-3 were not as good as those of Examples 1-3 because no modified Ti3SiC2 / ZnO hybrid powder was added. Although Comparative Example 2 added modified SiC powder with better effect, the hydrophobicity was still not as good as that of Examples 1-10. As the content of hybrid powder increased, the contact angle of Examples 1 and 4-7 gradually increased to 156°, while the roll-off angle gradually decreased to 5°. As the powder content continued to increase, the contact angle of Examples 8-10 began to decrease, while the roll-off angle increased. This shows that the addition of modified Ti3SiC2 / ZnO hybrid powder significantly optimized the contact angle and roll-off angle of the anti-icing hydrophobic coating, and both excess and deficiency led to a decrease in effect.

[0075] Experimental Example 2:

[0076] Anti-icing performance tests were conducted on the anti-icing hydrophobic coatings provided in Examples 1-10 and Comparative Examples 1-3: Anti-icing hydrophobic coating samples were prepared according to the preparation methods in Examples 1-10 and Comparative Examples 1-3, and uniformly coated onto epoxy fiberboard to form a coating. The samples were placed in a constant temperature drying oven. After the coating solidified, the samples were placed on a cold stage at -20°C. A drop of ultrapure water was added to the flat surface area of ​​each sample using a microsyringe, and the time it took for the water droplet to completely freeze on the anti-icing hydrophobic coating and the untreated epoxy fiberboard was recorded.

[0077] according to Figure 2 Test data showed that the complete freezing time of water droplets on untreated epoxy fiberboard was 13 seconds. The freezing time of Examples 1-10 was significantly prolonged. Although Comparative Examples 1-3, lacking the key modified Ti3SiC2 / ZnO hybrid powder, showed some anti-icing ability compared to the surface of untreated epoxy fiberboard, the overall effect was significantly different from that of Examples 1-10. In Examples 1 and 4-7, the freezing time of water droplets gradually increased with the increase of the proportion of hybrid powder, with Example 7 reaching the optimal value. In Examples 8-10, the freezing time decreased when the amount of hybrid powder was further increased, indicating that the anti-icing ability of the anti-icing hydrophobic coating samples began to decline. Among the samples of Examples 1-10, the samples with a contact angle >150° and a roll-off angle <10° (Examples 3 and 7) showed the most significant delayed freezing effect. This indicates that the addition of modified Ti3SiC2 / ZnO hybrid powder significantly improved the anti-icing ability of the anti-icing hydrophobic coating, and that both excessive and insufficient amounts led to a decrease in the effect.

[0078] Experimental Example 3:

[0079] The de-icing performance of the anti-icing hydrophobic coatings provided in Examples 1-10 and Comparative Examples 1-3 was tested: Anti-icing hydrophobic coating samples were prepared according to the preparation methods in Examples 1-10 and Comparative Examples 1-3, and uniformly coated on epoxy fiberboard to form a coating. The samples were placed in a constant temperature drying oven. After the coating solidified, a drop of ultrapure water was added to the flat surface area of ​​each sample using a microsyringe. After freezing at -20°C for 2 hours, the samples were taken out and placed upright in a room temperature environment. The time for the water droplet to melt and fall off was compared.

[0080] from Figure 3The test results show significant differences. Overall, the water droplet detachment time in Examples 1-10 is significantly shorter than that in the comparative samples. The samples with smaller rolling angles in the examples have shorter detachment times, while the water droplets in Comparative Examples 1-3 have longer detachment times, indicating that the water droplets are not easy to detach after thawing and have poor de-icing performance. Although Comparative Examples 1 and 3, which contain other modified materials, have better de-icing performance than Comparative Example 2, which contains ordinary anti-icing hydrophobic coatings, the overall effect is significantly different from that of Examples 1-10. In Examples 4-10, as the proportion of modified Ti3SiC2 / ZnO increases, the detachment time first decreases and then increases in a non-linear manner. The effect of Example 7 is the best, which means that the addition of modified Ti3SiC2 / ZnO hybrid powder significantly improves the anti-icing ability of the anti-icing hydrophobic coating, and both excess and deficiency lead to a decrease in effect.

[0081] Figure 4 The static water droplet contact angle and roll-off angle of the anti-icing hydrophobic coating prepared in Example 7 are shown in the left figure, where the contact angle is 156° and the roll-off angle is 5°.

[0082] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

[0083] The present invention and its embodiments have been described above. This description is not restrictive, and the accompanying drawings are only one embodiment of the present invention; the actual structure is not limited thereto. In conclusion, if those skilled in the art are inspired by this description and design similar structures and embodiments without departing from the spirit of the invention, such designs should fall within the protection scope of the present invention.

Claims

1. An anti-icing hydrophobic coating, characterized in that: The raw materials include the following parts by weight: 20-40 parts of hydroxyl acrylic resin, 10-30 parts of hydroxyl-terminated fluorinated polysiloxane, 2-12 parts of hydrophobic migration agent, 5-14 parts of modified Ti3SiC2 / ZnO hybrid powder, 0.1-0.2 parts of silane coupling agent, 1-3 parts of dispersant, 1-10 parts of curing agent, 1-2 parts of polypyrrole nanowires, and 25-60 parts of organic solvent; The method for preparing the modified Ti3SiC2 / ZnO hybrid powder includes the following steps: Zinc acetate was dissolved in anhydrous ethanol / ethylene glycol methyl ether mixed solvent and reacted at 0℃ to generate ZnO crystal nuclei. The mixture was then heated and refluxed to form monodisperse ZnO microspheres. The ZnO microspheres were ultrasonically dispersed in a CTAB-ethanol solution, and a Ti3SiC2 suspension was added. The mixture was heated and stirred, then concentrated under reduced pressure to 1 / 3 of its original volume. The concentrate was then transferred to a high-pressure reactor, cooled, and centrifuged to collect the product. Unreacted material was washed away with ethanol solution to obtain hybrid powder. The hybrid powder was vacuum dried, then subjected to a steam reaction for further curing. Finally, the cured product was dry-mixed with a silane coupling agent to obtain modified Ti3SiC2 / ZnO hybrid powder. The steam reaction uses fluorinated silane steam. The fluorinated silane vapor is any one of perfluorooctyltriethoxysilane, tridecafluorooctyltrimethoxysilane, and trifluoropropyltrichlorosilane; The hydrophobic migrating agent is either perfluorooctyltrichlorosilane or perfluorooctyltriethoxysilane.

2. The anti-icing hydrophobic coating according to claim 1, characterized in that: The zinc acetate concentration range is: 0.05-0.2 mol / L.

3. The anti-icing hydrophobic coating according to claim 1, characterized in that: In the Ti3SiC2 suspension The particle size range of Ti3SiC2 is 0.1-1.0 μm.

4. The anti-icing hydrophobic coating according to claim 1, characterized in that: The heating and stirring temperature is 25-80℃, and the heating method is gradient heating.

5. The anti-icing hydrophobic coating according to claim 1, characterized in that: The steam reaction time is 30-60 minutes; the curing temperature range is 120-150℃.

6. The anti-icing hydrophobic coating according to claim 1, characterized in that: The dispersant is any one of polymeric dispersants, nonionic surfactants, and polyacrylic acid dispersants.

7. A method for preparing an anti-icing hydrophobic coating according to any one of claims 1-6, characterized in that: Bag The preparation steps include: adding dispersant and hydrophobic migration agent to an organic solvent and mixing them evenly, then adding hydroxyl acrylic resin, hydroxyl-terminated fluorinated polysiloxane, polypyrrole nanowires, silane coupling agent, and modified Ti3SiC. 2 / The ZnO hybrid powder is stirred and mixed evenly, and finally the curing agent is added and mixed evenly to obtain an anti-icing and hydrophobic coating.

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