CN115678380A - Preparation method of super-hydrophobic photo-thermal coating with heat insulation function - Google Patents
Preparation method of super-hydrophobic photo-thermal coating with heat insulation function Download PDFInfo
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Abstract
The invention discloses a preparation method of a super-hydrophobic photo-thermal coating with a heat insulation function. Adding polydimethylsiloxane, carbon nano tubes, copper sulfide nano particles and PDMS curing agent into ethyl acetate solvent to prepare mixed slurry; preparing a polyvinylidene fluoride-ammonium bicarbonate mixed solution; the slurry and the solution are mixed and stirred to obtain a mixed slurry. And (3) coating the surface of the substrate with the prepared epoxy resin-ammonium bicarbonate colloid mixed solution by adopting a blade coating method, coating the epoxy resin coating with larger holes with the mixed slurry, and baking and drying to obtain the super-hydrophobic photo-thermal coating with the heat insulation function. The super-hydrophobic photo-thermal coating has good heat insulation, super-hydrophobic and photo-thermal conversion characteristics, excellent corrosion resistance, wear resistance and acid and alkali resistance, and good adhesion on the surface of most substrates.
Description
Technical Field
The invention belongs to the technical field of preparation of photo-thermal super-hydrophobic coating materials, and particularly relates to a super-hydrophobic photo-thermal coating with a heat insulation function and a preparation method thereof.
Background
Icing is an objective natural phenomenon, and brings great inconvenience and harm to production and life of people in the fields of aerospace, transportation, electric power communication and the like, so that how to prevent icing on the surface of outdoor equipment is an urgent problem to be solved when the outdoor equipment is in permanent stable operation in winter. The traditional deicing method, such as mechanical deicing, thermal energy deicing, chemical reagent deicing and the like, has the limitations of operation danger, high cost, low efficiency, environmental friendliness and the like, and is difficult to fundamentally and effectively solve the icing problem. The deicing by using the anti-icing material has the advantages of low energy consumption, wide application range and the like, and becomes a hot spot concerned by a plurality of scholars. The super-hydrophobic material prepared by the lotus leaf self-cleaning effect has excellent hydrophobic performance, so that liquid drops are separated from the wall surface before freezing, and certain anti-freezing performance is achieved. In addition, the existence of the inner cavity of the super-hydrophobic material micro-nano composite structure can block heat transfer, and the icing delaying effect is achieved. Meanwhile, the micro-nano composite structure can reduce the adhesion force between ice and the wall surface, so that the adhesion force of the ice coating is reduced, and accumulated ice is easy to remove under the action of gravity, wind and vibration, so that the super-hydrophobic material is considered as an ideal anti-icing material. However, the icing condition of the nature is complex, the super-hydrophobic surface can frost in the microstructure under the extreme environmental condition, and finally large-area icing is carried out. Icing in the super-hydrophobic microstructure increases the adhesion between ice and the wall surface, and the surface microstructure is damaged after icing and deicing for multiple times, so that the super-hydrophobic performance is lost. Even so, the super-hydrophobic surface still has certain anti-icing performance because of low icing adhesion and long icing delay time. In recent years, scholars propose that a new generation of anti-icing material should have excellent anti-icing and deicing performances. Therefore, the development of a surface capable of preventing ice and actively melting ice is receiving wide attention, and people try to embed materials with a photo-thermal effect, such as metal semiconductor materials, carbon-based materials, plasma nano materials and the like, on a super-hydrophobic surface to realize the rapid removal of ice crystals under the irradiation of sunlight.
In recent years, a plurality of scholars develop research work related to photothermal deicing, but common photothermal super-hydrophobic materials have the defects of weak mechanical property, limited application range, poor substrate adhesion and the like. The anti-icing surface developed in recent years can relieve surface icing to a certain extent, but the surface has the defects of poor durability, environmental pollution and the like, and once the surface is iced, a larger icing phenomenon can be caused, and the surface structure of the photo-thermal super-hydrophobic coating is damaged. Therefore, in order to ensure that outdoor equipment can be normally used in a low-temperature environment, the photo-thermal hydrophobic coating which can be permanently and stably used outdoors, has the functions of anti-icing and deicing and has the function of heat insulation needs to be developed. The super-hydrophobic photo-thermal coating with the heat insulation function disclosed by the invention not only has excellent super-hydrophobic, self-cleaning and photo-thermal properties, but also has excellent heat insulation performance.
Disclosure of Invention
The invention aims to provide a super-hydrophobic photo-thermal coating with heat insulation function and a preparation method thereof for solving the problem of icing on the surface of outdoor equipment.
The invention is technically characterized in that the generated gas generates cavity structures with different sizes in the coating and on the surface of the coating by decomposing ammonium bicarbonate at high temperature. According to the difference of drying and heating temperature and time, the first epoxy resin coating layer can have larger holes, the large holes can enable the epoxy resin coating layer to have better heat insulation performance, and a mechanical interlocking structure can be generated between the epoxy resin coating layer and the super-hydrophobic photo-thermal coating layer, so that the adhesion between the photo-thermal coating layer and the substrate is improved. On the other hand, also can make the super hydrophobic light and heat coating of upper strata heat-insulating and inside and the surface produce less hole through setting up different stoving temperature and stoving time, inside little hole can make it possess good heat-proof quality equally, and the little hole that the surface formed still can make its surface roughness more complicated, can pin more air, promotes its super hydrophobic performance. The coating has excellent super-hydrophobic and photo-thermal conversion performances, and also has excellent corrosion resistance, wear resistance and acid and alkali resistance. The coating and the preparation method thereof have good potential in solving the problem of equipment surface icing in the aspects of aerospace, transportation, electric power communication and the like.
The super-hydrophobic photothermal coating with the heat insulation function can be used for preparing heat insulation super-hydrophobic photothermal coatings with excellent adhesion characteristics on various substrates by a blade coating method, and the method comprises the following steps:
(1) According to the weight ratio of 0.9 to 1.0: adding epoxy resin with the model number of E-44 into acetone at the mass ratio of 9.0 to 10.0, carrying out ultrasonic treatment for 10 to 15 minutes at room temperature, and then carrying out magnetic stirring for 25 to 35 minutes to obtain an epoxy resin A solution with the mass concentration of 9 to 12 percent;
(2) According to the weight ratio of 1.5 to 2.0: dissolving ammonium bicarbonate in a DMF solution at room temperature according to a mass ratio of 4.5 to 5.0, and magnetically stirring the solution for 25 to 30 minutes to obtain an ammonium bicarbonate B solution with the mass concentration of 30 to 45 percent;
(3) Mixing the epoxy resin A solution prepared in the step (1), the ammonium bicarbonate B solution prepared in the step (2) and an epoxy resin curing agent according to the ratio of 8.0-10.0: 2.0 to 2.5: mixing the materials according to the mass ratio of 0.2 to 0.3, carrying out ultrasonic treatment on the mixture for 15 to 20 minutes at room temperature, and carrying out magnetic stirring on the mixture for 50 to 60 minutes to obtain an epoxy resin-ammonium bicarbonate colloid mixed solution C, wherein the solution C is used as a bottom layer slurry for later use.
(4) According to the weight ratio of 0.6 to 0.8:0.1 to 0.15:0.3 to 0.4: adding PDMS, a carbon nano tube, copper sulfide nano particles and a PDMS curing agent into an ethyl acetate solvent according to a mass ratio of 0.06 to 0.08, carrying out ultrasonic treatment for 25 to 30 minutes, and then magnetically stirring for 55 to 60 minutes to obtain mixed slurry D (wherein the size of the copper sulfide nano particles is 200 to 500 nanometers); ethyl acetate as a solvent was added in a slight excess amount relative to the starting material in order to form a homogeneous mixture.
(5) According to the weight ratio of 0.5 to 0.8: PVDF and ammonium bicarbonate are added into a DMF solvent according to the mass ratio of 1.0 to 1.5, and are uniformly mixed to prepare a PVDF-ammonium bicarbonate mixed solution E, the DMF is used as the solvent to form a uniformly mixed state, and the addition amount of the DMF is slightly excessive relative to the raw materials.
(6) According to the weight ratio of 9.0 to 10.0: mixing the D slurry and the E solution according to the mass ratio of 5.0 to 6.0, and stirring to prepare a mixed slurry F of PDMS, carbon nano tubes, copper sulfide nano particles, PVDF and ammonium bicarbonate; the mixed slurry F is used as upper slurry for standby.
(7) And (3) uniformly coating the solution C on a substrate by a scraper with the height of 2.0-2.5 mm, standing for 5-10 minutes at room temperature, and then putting into an oven heated to 110-120 ℃ for drying for 3-4 minutes, thereby obtaining the epoxy resin coating with large holes inside and on the surface of the substrate.
(8) And (3) setting a scraper with the height of 2.5-3.0 mm, uniformly scraping the mixed slurry F on the epoxy resin bottom layer with the large holes inside and on the surface in the step (8), standing for 5-10 minutes at room temperature, putting the mixture into an oven, setting the temperature of the oven to be 120-130 ℃, and drying the mixture for 120-150 minutes.
The above substances have the same mass unit.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained.
According to the invention, firstly, ammonium bicarbonate with a large mass ratio is added into an epoxy resin solution, the epoxy resin solution is directly dried at a high temperature for a short time to enable holes with large sizes to be generated in the bottom epoxy resin coating and on the surface of the bottom epoxy resin coating, then photo-thermal super-hydrophobic colloid slurry containing a small amount of ammonium bicarbonate is uniformly coated on the bottom epoxy resin coating in a blade-coating manner, the epoxy resin coating with the lower layer of large holes is obtained after the drying is finished, the super-hydrophobic coating with the upper layer of small holes is obtained, and the two coatings form a mechanical interlocking structure at an interface through heating and drying and are fused into a whole, so that the super-hydrophobic photo-thermal coating with a heat insulation function is finally formed.
It is further explained that the larger holes generated inside the bottom epoxy resin coating layer play a role of heat insulation on one hand, and on the other hand, the larger holes can enable the upper super-hydrophobic photo-thermal coating layer and the bottom epoxy resin coating layer to form a mechanical interlocking structure through the combination of the big holes and the small holes, so that the adhesion force between the upper photo-thermal coating layer and the bottom layer is enhanced; the small holes of the photo-thermal super-hydrophobic coating of the upper coating further play a role in heat insulation in the coating, the deicing and anti-icing performances of the coating are improved, and on the other hand, the fine holes generated on the surface of the coating form a more complex rough structure for the surface of the coating, so that the hydrophobicity of the coating is further improved, and the performances of the coating in the aspects of anti-icing and deicing are enhanced. Due to the fact that the super-hydrophobic property of the upper photo-thermal super-hydrophobic coating is reduced due to too large holes and the coating is not flat, and due to the fact that the generated holes are too small, the super-hydrophobic property and the mechanical property of the photo-thermal super-hydrophobic coating are reduced, under the same preparation process condition, the linearity of the holes of the bottom layer of the epoxy resin and the linearity of the holes of the upper photo-thermal super-hydrophobic coating are adjusted and controlled through the optimized selected ammonium bicarbonate, heating and drying time and temperature to enable the sizes to be in the range of 5-100 micrometers and 30-200 nanometers respectively, and finally the heat insulation property, the mechanical property and the super-hydrophobic property of the prepared coating are improved obviously. In contrast, the absence, low use, or excess of ammonium bicarbonate and the heating temperature and time are not optimally selected, which results in a superhydrophobic photothermal coating that either has superhydrophobic properties but poor thermal insulation and mechanical properties, or that does not have superhydrophobic properties.
Drawings
FIG. 1 shows that the super-hydrophobic photo-thermal coating with heat insulation function prepared in example 1 is 1kW/m 2 Irradiating the film for 30 minutes under power sunlight, and stopping irradiating for 2 minutes to obtain an infrared thermal imaging graph.
Fig. 2 is a water drop contact angle test chart of the superhydrophobic photothermal coating with the heat insulation function prepared in example 1.
FIG. 3 shows that the super-hydrophobic photo-thermal coating with heat insulation function prepared in example 2 is 1kW/m 2 And (3) irradiating the power sunlight for 30 minutes, and then stopping irradiating for 2 minutes to obtain an infrared thermal imaging graph.
Fig. 4 is a water drop contact angle test chart of the superhydrophobic photothermal coating with the thermal insulation function prepared in example 2.
FIG. 5 shows a coating having a superhydrophobic photothermal property at 1kW/M prepared in comparative example 5 2 And (3) irradiating the power sunlight for 30 minutes, and then stopping irradiating for 2 minutes to obtain an infrared thermal imaging graph.
FIG. 6 is a contact angle test chart of a water drop with a coating having super-hydrophobic photothermal properties prepared in comparative example 5.
Detailed Description
To further illustrate the super-hydrophobic photothermal coating with thermal insulation function and the preparation method thereof, the following embodiments are used to illustrate the present invention, but not to limit the present invention.
Example 1
(1) According to the weight ratio of 1.0:9.0, adding the epoxy resin E-44 in acetone at room temperature, carrying out ultrasonic treatment for 15 minutes, and then carrying out magnetic stirring for 35 minutes to obtain an epoxy resin A solution with the mass concentration of 12%;
(2) According to the weight ratio of 2.0:5.0, dissolving ammonium bicarbonate in the DMF solution at room temperature, and magnetically stirring for 30 minutes to obtain an ammonium bicarbonate B solution with the mass concentration of 40 percent;
(3) Mixing the epoxy resin A solution prepared in the step (1), the ammonium bicarbonate B solution prepared in the step (2) and an epoxy resin curing agent according to a ratio of 8.0:2.5:0.2, and subjecting the mixture to ultrasonic treatment at room temperature for 20 minutes, and then magnetically stirring the mixture for 60 minutes, thereby obtaining an epoxy resin-ammonium bicarbonate colloid mixed solution C. The solution C is used as bottom layer slurry for standby;
(4) According to the weight ratio of 0.8:0.15:0.4: adding PDMS, carbon nanotubes, copper sulfide nanoparticles and a PDMS curing agent into an ethyl acetate solution with the mass ratio of 1.5 to the total mass of the substances being 1.0, carrying out ultrasonic treatment for 30 minutes, and then magnetically stirring for 60 minutes to obtain a mixed slurry D;
(5) According to the weight ratio of 0.8:1.0: PVDF, ammonium bicarbonate and DMF are prepared into a PVDF-ammonium bicarbonate mixed solution E according to the mass ratio of 10.0.
(6) According to the weight ratio of 10.0:6.0 mass ratio the D slurry and the E solution were mixed and stirred, thereby preparing PDMS, carbon nanotubes, copper sulfide nanoparticles, PVDF and ammonium bicarbonate mixed slurry F. Taking the mixed slurry F as upper slurry for later use;
(7) And uniformly scraping the solution C on the substrate by a scraper with the height of 2.5mm, standing for 5 minutes at room temperature, and drying in an oven heated to 120 ℃ for 4 minutes, thereby obtaining the epoxy resin coating with large holes in the inner part and on the surface of the substrate.
(8) And (5) arranging a scraper with the height of 3.0mm to uniformly scrape the mixed slurry F on the epoxy resin bottom layer with the large holes in the inner part and the surface in the step (8), standing for 10 minutes at room temperature, then putting into an oven, setting the temperature of the oven to be 130 ℃, and drying the oven for 150 minutes.
The above substances have the same mass unit.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained. By optimizing the selection of ammonium bicarbonate andthe heating and drying time and the temperature are regulated, the average diameter of the holes of the prepared bottom epoxy resin is about 90 micrometers, and the average diameter of the holes of the prepared upper photo-thermal super-hydrophobic coating is about 50 nanometers. The product performance is shown in figures 1 and 2, and it can be seen from figure 1 that the prepared super-hydrophobic photo-thermal coating with the heat insulation function has good heat insulation performance at 1kW/m 2 After the power sunlight irradiates for 30 minutes, the highest temperature of 94.2 ℃ is still remained after the power sunlight stops irradiating for 2 minutes; from FIG. 2, it can be seen that the surface of the coating has a hydrophobic angle of 156.23 degrees, and the super-hydrophobic requirement is met.
Example 2
(1) According to the weight ratio of 0.9:10.0, adding the epoxy resin E-44 in acetone at room temperature, carrying out ultrasonic treatment for 10 minutes, and then carrying out magnetic stirring for 25 minutes to obtain an epoxy resin A solution with the mass concentration of 9%;
(2) According to the proportion of 1.5:5.0, dissolving ammonium bicarbonate in a DMF solution at room temperature, and magnetically stirring for 25 minutes to obtain an ammonium bicarbonate B solution with the mass concentration of 30%;
(3) Mixing the epoxy resin A solution prepared in the step (1), the ammonium bicarbonate B solution prepared in the step (2) and the epoxy resin curing agent according to the mass ratio of 10.0. The solution C is used as bottom slurry for standby;
(4) According to the weight ratio of 0.6:0.1:0.3: adding PDMS, carbon nanotubes, copper sulfide nanoparticles and a PDMS curing agent into an ethyl acetate solution with the mass ratio of 1.0 to the total mass of the substances being 1.0;
(5) According to the weight ratio of 0.5:1.0: PVDF, ammonium bicarbonate and DMF are prepared into a PVDF-ammonium bicarbonate mixed solution E according to the mass ratio of 10.0.
(6) According to the weight ratio of 10.0:5.0 mass ratio the D slurry and the E solution were mixed and stirred, thereby preparing PDMS, carbon nanotube, copper sulfide nanoparticle, PVDF, and ammonium bicarbonate mixed slurry F. Taking the mixed slurry F as upper slurry for later use;
(7) And uniformly coating the solution C on the substrate by arranging a scraper with the height of 2mm, standing for 5 minutes at room temperature, and drying in an oven heated to 110 ℃ for 3 minutes, thereby obtaining the epoxy resin coating with large holes in the inner part and on the surface of the substrate.
(8) And (3) setting a scraper with the height of 2.5mm to uniformly scrape the mixed slurry F on the epoxy resin bottom layer with the large holes inside and on the surface in the step (8), standing for 10 minutes at room temperature, putting the mixture into an oven, setting the temperature of the oven to be 120 ℃, and drying the mixture for 120 minutes.
The above substances have the same mass unit.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained. By optimizing the selected ammonium bicarbonate and regulating the heating and drying time and temperature, the average diameter of the pores of the prepared lower epoxy resin layer is about 20 micrometers, and the average diameter of the pores of the upper photo-thermal super-hydrophobic coating layer is about 90 nanometers. The product performance is shown in figures 3 and 4, and it can be seen from figure 3 that the prepared super-hydrophobic photo-thermal coating with the heat insulation function has good heat insulation performance at 1kW/m 2 After the power sunlight irradiates for 30 minutes, the temperature of the maximum 93.6 ℃ is still kept after the power sunlight stops irradiating for 2 minutes; from fig. 4, it can be seen that the surface hydrophobicity angle of the coating reaches 155.10 degrees, and the super-hydrophobicity requirement is met.
Example 3
(1) According to the weight ratio of 1.0:10.0, adding the epoxy resin E-44 into acetone at room temperature, carrying out ultrasonic treatment for 15 minutes, and then carrying out magnetic stirring for 35 minutes to obtain an epoxy resin A solution with the mass concentration of 10%;
(2) According to the weight ratio of 1.8:4.8, dissolving ammonium bicarbonate in the DMF solution at room temperature, and magnetically stirring for 30 minutes to obtain an ammonium bicarbonate B solution with the mass concentration of 37.5 percent;
(3) Mixing the epoxy resin A solution prepared in the step (1), the ammonium bicarbonate B solution prepared in the step (2) and the epoxy resin curing agent according to a mass ratio of 9.0. The solution C is used as bottom slurry for standby;
(4) According to the weight ratio of 0.7:0.15:0.4: adding PDMS, carbon nanotubes, copper sulfide nanoparticles and a PDMS curing agent into an ethyl acetate solution with the mass ratio of 1.3 to 8.0 to the total mass of the substances in a mass ratio of 0.07, carrying out ultrasonic treatment for 30 minutes, and then magnetically stirring for 60 minutes to obtain a mixed slurry D;
(5) According to the weight ratio of 0.7:1.5: and 9.0, preparing PVDF-ammonium bicarbonate mixed solution E from PVDF, ammonium bicarbonate and DMF.
(6) According to the weight ratio of 10.0:6.0 mass ratio the D slurry and the E solution were mixed and stirred, thereby preparing PDMS, carbon nanotubes, copper sulfide nanoparticles, PVDF and ammonium bicarbonate mixed slurry F. Taking the mixed slurry F as upper slurry for later use;
(7) And uniformly scraping the solution C on the substrate by a scraper with the height of 2.5mm, standing for 8 minutes at room temperature, and drying in an oven heated to 120 ℃ for 4 minutes, thereby obtaining the epoxy resin coating with large holes in the inner part and on the surface of the substrate.
(8) And (3) setting a scraper with the height of 3.0mm to uniformly scrape the mixed slurry F on the epoxy resin bottom layer with the large holes inside and on the surface in the step (8), standing for 8 minutes at room temperature, putting the mixture into an oven, setting the temperature of the oven to 125 ℃, and drying the mixture for 135 minutes.
The above substances have the same mass unit.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained. By optimizing the selected ammonium bicarbonate and regulating the heating and drying time and temperature, the diameter of the pores of the prepared lower epoxy resin layer is about 70 micrometers, and the average diameter of the pores of the upper photo-thermal super-hydrophobic coating layer is about 170 nanometers. The prepared super-hydrophobic photo-thermal coating with the heat insulation function has good heat insulation performanceAt 1kW/m 2 After the irradiation of the power sunlight for 30 minutes, the temperature of 93.8 ℃ at the maximum is reached after the irradiation of the power sunlight is stopped for 2 minutes, the hydrophobic angle reaches 155.80 degrees, and the hydrophobic angle on the surface of the coating reaches the super-hydrophobic requirement.
Example 4
A preparation method of a super-hydrophobic photo-thermal coating with heat insulation function is disclosed, and the method and the steps are the same as example 1, but ammonium bicarbonate is not added in the step (2). Through the steps, the prepared lower epoxy resin is not provided with holes, and the average diameter of the holes of the upper photo-thermal super-hydrophobic coating is about 165 nanometers. The prepared coating has super-hydrophobic performance, and the hydrophobic angle is measured to reach 155.82 degrees and is close to that of the coating in the embodiment 1; but because the hole structure of the lower epoxy resin is lacked, the heat insulation performance of the lower epoxy resin coating is lost, so the photo-thermal performance is reduced to 1kW/m 2 After 30 minutes of irradiation with power sunlight, the temperature of 78.8 ℃ maximum is reached after 2 minutes of cessation of irradiation. In addition, because holes are not prepared in the lower epoxy resin coating, the coating loses a mechanical interlocking structure, the mechanical property of the coating is also reduced, the combination between the film layers is not tight enough, and the requirement is not met.
Example 5
A preparation method of a super-hydrophobic photothermal coating with a heat insulation function is the same as that of example 1, but ammonium bicarbonate is not added in the step (5). Through the steps, the average diameter of the holes of the prepared lower epoxy resin layer is about 90 micrometers, and the holes are not prepared in the upper photo-thermal super-hydrophobic coating. The prepared coating has good mechanical property, but the complex rough structure on the surface of the coating loses part due to the lack of small pores generated by decomposing ammonium bicarbonate, the hydrophobicity is slightly reduced, and the heat insulation property is also reduced. The product performances are shown in FIGS. 5 and 6, and it can be seen from FIG. 5 that the prepared super-hydrophobic photothermal coating with heat insulation function has much reduced heat insulation performance compared with the heat insulation performance of the super-hydrophobic photothermal coatings of examples 1 and 2, and the heat insulation performance is reduced at 1kW/m 2 After the power sunlight irradiates for 30 minutes, the temperature of 69.8 ℃ is only obtained after the irradiation is stopped for 2 minutes; it can be seen from FIG. 6 that the hydrophobic angle of the coating surface reached 154.49 degrees, which meets the superhydrophobic requirement, but compares with example 1 and the implementationExample 2 the hydrophobic angle still decreased.
Example 6
A preparation method of a super-hydrophobic photothermal coating with a heat insulation function is the same as that of example 1, but ammonium bicarbonate is not added in the steps (2) and (5). Through the steps, the prepared coating lower epoxy resin is partially lack of large holes generated by decomposing ammonium bicarbonate, loses a mechanical interlocking structure and loses good mechanical properties. The upper photo-thermal hydrophobic coating lacks small holes generated by decomposing ammonium bicarbonate, so that the heat insulation property is lost, and the complex rough structure on the surface of the coating is lost. At 1kW/m 2 After 30 minutes of irradiation under the power sunlight, the temperature of 62.4 ℃ is only obtained after 2 minutes of stopping the irradiation. The angle of hydrophobicity was measured to reach 155.91 deg., which was slightly lower than that of example 1, and the contact angle of the water droplet was close to that of example 4. But the mechanical interlocking structure is lost, the mechanical property of the coating is greatly reduced, and the combination between film layers is not tight enough and does not meet the requirement.
Example 7
The process parameters of the embodiment are the same as the steps of the embodiment 1, except that the mass ratio of the ammonium bicarbonate particles added into the DMF solution in the step (2) is reduced from 2.0 to 1.0, so that the mass ratio is smaller than the mass ratio range of the ammonium bicarbonate in the invention, namely 1.5 to 2.0.
Through the steps, the diameter of the prepared lower-layer epoxy resin hole is about 2 micrometers, and the diameter range of the prepared lower-layer epoxy resin hole is not satisfied, wherein the diameter range of the prepared lower-layer epoxy resin hole is 5-100 micrometers; the average diameter of the holes of the upper photo-thermal super-hydrophobic coating is about 165 nanometers. Although a super-hydrophobic photothermal coating with heat insulation function can be obtained, the hydrophobic angle is measured to reach 155.85 degrees, and the contact angle of the obtained coating water drop is close to that of the example 1, the heat insulation performance of the coating is reduced at 1kW/m 2 After the power sunlight irradiates for 30 minutes, the temperature of 78.6 ℃ is only obtained after the power sunlight stops irradiating for 2 minutes, the mechanical property is also reduced, and the requirement is not met.
Example 8
The process parameters of the embodiment are the same as the steps of the embodiment 1, except that the mass ratio of the ammonium bicarbonate particles added into the DMF solution in the step (5) is increased from 1.0 to 2.0, so that the mass ratio of the ammonium bicarbonate particles is 1.0 to 1.5 beyond the mass ratio of the ammonium bicarbonate in the invention.
Through the steps, the average diameter of the holes of the prepared lower epoxy resin layer is about 90 micrometers, and a plurality of macroscopic millimeter-scale holes are generated on the coating surface of the upper photo-thermal super-hydrophobic coating, so that the appearance and the hydrophobicity of the coating are influenced, the measured hydrophobic angle is only 144.31 degrees, and the super-hydrophobic requirement is not met. Furthermore, the heat insulation performance of the coating is reduced to 1kW/m 2 After the power sunlight irradiates for 30 minutes, the temperature of 72.5 ℃ is only obtained after the power sunlight stops irradiating for 2 minutes, the mechanical property is also reduced, and the requirement is not met.
Example 9
The process parameters of this example are the same as those of example 1 except that steps (1), (2), (3) and (7) are eliminated and the resulting coating lacks the underlying epoxy resin coating.
Through the steps, the coating with the super-hydrophobic photo-thermal performance can be obtained, compared with the coating of the lower epoxy resin layer in the embodiment 1, the surface hydrophobic performance of the coating is hardly influenced, the hydrophobic angle is measured to reach 156.12 degrees, but the thermal insulation performance is reduced, and the content is 1kW/m 2 After the power sun light irradiates for 30 minutes, the temperature of 77.2 ℃ is only obtained after the power sun light stops irradiating for 2 minutes, and the mechanical property is reduced, so that the film layer can not be tightly combined with the substrate, and the requirement is not met.
Example 10
The process parameters of this example are the same as those of example 1 except that steps (4), (5), (6) and (8) are eliminated and the resulting coating lacks the topcoat photothermal superhydrophobic coating.
Through the steps, the epoxy resin coating with fine holes on the surface can be obtained, and compared with the photo-thermal super-hydrophobic coating which is lack of the upper layer in the embodiment 1, the hydrophobic property of the epoxy resin coating is completely lost and is 1kW/m 2 After the irradiation of the power sunlight for 30 minutes, the temperature of only 33.6 ℃ is obtained after the irradiation of the power sunlight is stopped for 2 minutes, so the requirement is not met.
The preferred embodiments and comparative examples of the present invention have been described above, but the present invention should not be limited to the disclosure of the embodiments. Therefore, it is intended that all equivalents and modifications which do not depart from the spirit of the invention disclosed herein are deemed to be within the scope of the invention.
Claims (9)
1. A preparation method of a super-hydrophobic photo-thermal coating with a heat insulation function is characterized by comprising the following steps:
(1) Dissolving epoxy resin in acetone to form an epoxy resin solution A;
(2) Dissolving ammonium bicarbonate in a Dimethylformamide (DMF) solvent to form an ammonium bicarbonate solution B;
(3) Mixing the epoxy resin solution A and the ammonium bicarbonate solution B, adding an epoxy resin curing agent, and stirring until the solution is uniform, thereby obtaining an epoxy resin-ammonium bicarbonate colloid mixed solution C;
(4) Adding Polydimethylsiloxane (PDMS), carbon nano tubes, copper sulfide nano particles and a PDMS curing agent into an ethyl acetate solvent according to a certain mass ratio to prepare a mixed slurry D;
(5) Adding polyvinylidene fluoride and ammonium bicarbonate with certain mass into a DMF solvent to prepare a PVDF-ammonium bicarbonate mixed solution E;
(6) Mixing and stirring the mixed slurry D and the solution E, thereby preparing a PDMS, a carbon nanotube, a copper sulfide nanoparticle, a PVDF, and an ammonium bicarbonate mixed slurry F;
(7) Coating the surface of the substrate with the epoxy resin-ammonium bicarbonate colloid mixed solution C prepared in the step (3) by adopting a blade coating method, then putting the blade-coated substrate into an oven for baking and drying, and obtaining an epoxy resin coating with holes inside and on the surface after baking;
(8) And (5) coating the epoxy resin coating with holes inside and on the surface, which is prepared in the step (7), with the mixed slurry F prepared in the step (6), then putting the mixed slurry F into a drying oven for baking and drying, and obtaining the super-hydrophobic photo-thermal coating with the heat insulation function after baking.
2. The preparation method of the superhydrophobic photothermal coating with the heat insulation function according to claim 1, wherein in the step (1), epoxy resin E-44 is added into acetone at room temperature, ultrasonic processing is performed for 10-15 minutes, and then magnetic stirring is performed for 25-35 minutes to obtain an epoxy resin A solution, wherein the mass concentration of the epoxy resin is 9-12%.
3. The method for preparing the superhydrophobic photothermal coating with the heat insulation function according to claim 1, wherein in the step (2), ammonium bicarbonate is dissolved in the DMF solution at room temperature, and the solution is magnetically stirred for 25 to 30 minutes to obtain an ammonium bicarbonate B solution, wherein the mass concentration of the ammonium bicarbonate is 30 to 45%.
4. The preparation method of the super-hydrophobic photothermal coating with the heat insulation function according to claim 1, wherein in the step (3), the epoxy resin solution A, the ammonium bicarbonate solution B and the epoxy resin curing agent are mixed according to the ratio of 8.0 to 10.0:2.0 to 2.5: mixing the components in a mass ratio of 0.2 to 0.3, and carrying out ultrasonic treatment and uniform stirring on the mixture at room temperature to obtain an epoxy resin-ammonium bicarbonate colloid mixed solution C.
5. The preparation method of the super-hydrophobic photothermal coating with the heat insulation function according to claim 1, wherein in the step (4), the mass ratio of the PDMS, the carbon nanotube, the copper sulfide nanoparticle and the PDMS curing agent is 0.6 to 0.8:0.1 to 0.15:0.3 to 0.4:0.06 to 0.08, wherein the size of the copper sulfide nano-particles is 200 to 500 nanometers.
6. The preparation method of the super-hydrophobic photothermal coating with the heat insulation function according to claim 1, wherein the mass ratio of PVDF to ammonium bicarbonate in the step (5) is 0.5 to 0.8:1.0 to 1.5.
7. The preparation method of the super-hydrophobic photothermal coating with the heat insulation function according to claim 1, wherein the mass ratio of the mixed slurry D to the solution E in the step (6) is 9.0 to 10.0:5.0 to 6.0.
8. The preparation method of the super-hydrophobic photothermal coating with the heat insulation function according to claim 1, wherein in the step (7), a scraper with the height of 2-2.5 mm is arranged to uniformly scrape the solution C on the substrate, the substrate is kept stand for 5-10 minutes at room temperature, and then the substrate is heated to 110-120 ℃ and dried for 3-4 minutes.
9. The preparation method of the super-hydrophobic photothermal coating with the heat insulation function according to claim 1, wherein in the step (8), a scraper with the height of 2.5-3.0 mm is arranged, the mixed slurry F is uniformly coated on the epoxy resin bottom layer with the large holes in the inner part and the surface in the step (8), the mixture is placed in an oven after standing for 5-10 minutes at room temperature, the temperature of the oven is set to 120-130 ℃, and the drying is carried out for 120-150 minutes.
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