CN115678380B - 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 were 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. Besides good heat insulation, super-hydrophobic and photo-thermal conversion characteristics, the super-hydrophobic photo-thermal coating also has excellent corrosion resistance, wear resistance and acid and alkali resistance, and has good adhesive force on most substrate surfaces.
Description
Technical Field
The invention belongs to the technical field of preparation of photothermal super-hydrophobic coating materials, and particularly relates to a super-hydrophobic photothermal coating with a heat insulation function and a preparation method thereof.
Background
Icing is an objective natural phenomenon, and brings numerous inconvenience and harm to human production and life in the fields of aerospace, transportation, power communication and the like, so that how to prevent icing and icing on the surface of outdoor equipment is a problem which needs to be solved in the winter for durable and stable operation of the outdoor equipment. The traditional deicing method, such as mechanical deicing, thermal deicing, chemical agent deicing and the like, has various limitations of operation danger, high cost, low efficiency, unfriendly environment and the like, and is difficult to radically and effectively solve the icing problem. Deicing by using the anti-icing material has the advantages of low energy consumption, wide application range and the like, and has become a focus of attention of a plurality of students. The super-hydrophobic material prepared by the lotus leaf self-cleaning effect has excellent hydrophobic property, so that liquid drops are separated from the wall surface before icing, and the super-hydrophobic material has certain anti-icing property. In addition, the existence of the hollow inside the super-hydrophobic material micro-nano composite structure can obstruct heat transfer, and the effect of delaying icing is achieved. Meanwhile, the micro-nano composite structure can reduce the adhesion force between ice and the wall surface, so that the ice-coating adhesion force is reduced, and the accumulated ice is easy to remove under the action of gravity, wind and vibration, so that the super-hydrophobic material is considered to be an ideal anti-icing material. However, due to the fact that the natural icing condition is complex, the superhydrophobic surface can frost in the microstructure under the extreme environmental condition, and finally ice in a large area. Icing in the superhydrophobic microstructure increases the adhesion between ice and the wall surface, and the surface microstructure is damaged after multiple icing and deicing, so that the superhydrophobic 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 have proposed that new generation anti-icing materials should have excellent anti-icing and deicing properties. Therefore, development of a surface capable of preventing ice and actively melting ice has been widely focused, and attempts have been made to embed materials with photo-thermal effects, such as metal semiconductor materials, carbon-based materials, plasma nanomaterials, etc., on a superhydrophobic surface to achieve rapid removal of ice crystals under irradiation of sunlight.
Recently, a plurality of students develop related research work of photo-thermal deicing, but common photo-thermal super-hydrophobic materials have a plurality of defects of weak mechanical properties, limited application range, poor substrate adhesion and the like. The anti-icing surface developed in recent years can alleviate the 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 frozen, the surface icing phenomenon is larger, and the surface structure of the photothermal super-hydrophobic coating is damaged. Therefore, in order to ensure that the outdoor equipment can be normally used in a low-temperature environment, a photo-thermal hydrophobic coating which can be permanently and stably used outdoors, has anti-icing and deicing functions and has a heat insulation function 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 a heat insulation function and a preparation method thereof for solving the problem of icing on the surface of outdoor equipment.
The key and main technical features of the invention are that the generated gas generates hollow structures with different sizes inside the coating and on the surface of the coating by decomposing ammonium bicarbonate at high temperature. According to the different drying and heating temperatures and times, the first layer of epoxy resin coating has larger holes, and the larger holes not only enable the epoxy resin coating to have better heat insulation performance, but also enable the epoxy resin coating and the super-hydrophobic photo-thermal coating to generate a mechanical interlocking structure, thereby improving the adhesion between the photo-thermal coating and the substrate. On the other hand, through setting up different stoving temperatures and stoving time also can make the inside and surface of upper heat-insulating super-hydrophobic photo-thermal coating produce less hole, inside little hole can make it possess good heat insulation performance equally, and the little hole that the surface formed can also make its surface roughness structure more complicated, can lock more air, promotes its super-hydrophobic performance. The coating has excellent super-hydrophobic and photo-thermal conversion performance, and also has excellent corrosion resistance, wear resistance and acid-base resistance. The coating and the preparation method thereof have good potential for solving the problem of icing on the surface of equipment in the aspects of aerospace, transportation, power communication and the like.
The super-hydrophobic photo-thermal coating with the heat insulation function can be used for preparing the heat insulation super-hydrophobic photo-thermal coating with excellent adhesion characteristics on various substrates by a knife coating method, and the method comprises the following steps of:
(1) According to 0.9-1.0: 9.0-10.0 mass percent, adding the type E-44 epoxy resin into acetone at room temperature, performing ultrasonic treatment for 10-15 minutes, and then magnetically stirring for 25-35 minutes to obtain an epoxy resin A solution with the mass concentration of 9-12%;
(2) According to 1.5-2.0: 4.5-5.0 mass ratio, dissolving ammonium bicarbonate in DMF solution at room temperature, and magnetically stirring for 25-30 minutes to obtain ammonium bicarbonate B solution with mass concentration of 30-45%;
(3) 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 are mixed according to the proportion of 8.0-10.0: 2.0 to 2.5: mixing the materials according to the mass ratio of 0.2-0.3, carrying out ultrasonic treatment on the mixture for 15-20 minutes at room temperature, and then carrying out magnetic stirring on the mixture for 50-60 minutes, thereby obtaining an epoxy resin-ammonium bicarbonate colloid mixed C solution which is used as bottom layer slurry for standby.
(4) According to 0.6-0.8: 0.1 to 0.15:0.3 to 0.4: adding PDMS, carbon nano tubes, copper sulfide nano particles and a PDMS curing agent into an ethyl acetate solvent according to the mass ratio of 0.06-0.08, performing ultrasonic treatment for 25-30 minutes, and magnetically stirring for 55-60 minutes to obtain mixed slurry D (wherein the size of the copper sulfide nano particles is 200-500 nanometers); ethyl acetate was used as a solvent to form a uniform state, and the amount thereof was added in a slight excess relative to the raw materials.
(5) According to 0.5-0.8: and adding PVDF and ammonium bicarbonate into DMF solvent according to the mass ratio of 1.0-1.5, uniformly mixing to prepare PVDF-ammonium bicarbonate mixed solution E, wherein DMF is used as solvent to form a uniform mixing state, and the adding amount of the DMF is slightly excessive relative to the raw materials.
(6) According to 9.0-10.0: mixing and stirring the slurry D and the solution E according to the mass ratio of 5.0-6.0, thereby preparing mixed slurry F of PDMS, carbon nanotubes, copper sulfide nano particles, PVDF and ammonium bicarbonate; the mixed slurry F is used as upper slurry for standby.
(7) And (3) uniformly scraping and coating the C solution on the substrate by a scraper with the height of 2.0-2.5 mm, standing for 5-10 minutes at room temperature, and then placing the substrate into a baking oven which is heated to 110-120 ℃ for baking for 3-4 minutes, so that an epoxy resin coating with larger holes in the interior and the surface of the substrate can be obtained.
(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 larger holes in the inner part and the surface of the mixed slurry F in the step (8), standing for 5-10 minutes at room temperature, putting the mixed slurry F into a baking oven, setting the temperature of the baking oven to 120-130 ℃, and drying the mixed slurry F for 120-150 minutes.
The mass units of the above materials are consistent.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained.
According to the invention, ammonium bicarbonate with a larger 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 the inside and the surface of a bottom epoxy resin coating to generate holes with a larger size, then photo-thermal super-hydrophobic colloid slurry containing a small amount of ammonium bicarbonate is uniformly scraped on the epoxy resin bottom layer, after drying, an epoxy resin coating with a lower layer of larger holes is obtained, and a super-hydrophobic coating with a lower layer of smaller holes is obtained, and the two layers of coatings are heated and dried to form a mechanical interlocking structure at an interface 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 larger holes are formed in the bottom epoxy resin coating to play a role in heat insulation, and on the other hand, the larger holes can enable the super-hydrophobic photo-thermal coating on the upper layer to be combined with the epoxy resin coating on the bottom layer to form a mechanical interlocking structure through the large holes, so that the adhesion between the photo-thermal coating on the upper layer and the bottom layer is enhanced; the small holes of the photo-thermal super-hydrophobic coating of the upper coating layer further play a role in heat insulation in the coating layer, so that the deicing and anti-icing performances of the coating layer are improved, on the other hand, the tiny holes generated on the surface of the coating layer construct a more complex coarse structure for the surface of the coating layer, so that the hydrophobicity of the coating layer is further improved, and the performance of the coating layer in the aspects of anti-icing and deicing is enhanced. The super-hydrophobic characteristic of the upper photo-thermal super-hydrophobic coating is reduced due to overlarge holes, the coating is uneven, and the super-hydrophobic and mechanical properties of the photo-thermal super-hydrophobic coating are reduced due to overlarge generated holes, so that under the same preparation process conditions, the hole linearity of the bottom layer holes and the upper photo-thermal super-hydrophobic coating of the epoxy resin is regulated and controlled by optimizing and selecting ammonium bicarbonate, heating and drying time and temperature, and the hole linearity is respectively in the range of 5-100 micrometers and 30-200 nanometers, and finally the thermal insulation characteristic, mechanical properties and super-hydrophobic properties of the prepared coating are obviously improved. In contrast, the absence, use of little or use of excess ammonium bicarbonate and the heating temperature and time cannot be optimally selected, which results in superhydrophobic photothermal coatings that have either superhydrophobic properties but poor thermal and mechanical properties or no superhydrophobic properties.
Drawings
FIG. 1 shows a super-hydrophobic photo-thermal coating with heat insulation function prepared in example 1 at 1kW/m 2 And irradiating under the power sunlight for 30 minutes, and stopping irradiating for 2 minutes to obtain an infrared thermal imaging graph.
Fig. 2 is a graph for testing the contact angle of water drops of the super-hydrophobic photo-thermal coating with heat insulation function prepared in example 1.
FIG. 3 shows a super-hydrophobic photo-thermal coating with heat insulation function prepared in example 2 at 1kW/m 2 And irradiating under the power sunlight for 30 minutes, and stopping irradiating for 2 minutes to obtain an infrared thermal imaging graph.
Fig. 4 is a graph for testing the contact angle of water drops of the super-hydrophobic photo-thermal coating with heat insulation function prepared in example 2.
FIG. 5 is a coating of 1kW/M with super-hydrophobic photo-thermal properties prepared in comparative example 5 2 And irradiating under the power sunlight for 30 minutes, and stopping irradiating for 2 minutes to obtain an infrared thermal imaging graph.
Fig. 6 is a graph of a water drop contact angle test with a coating having superhydrophobic photo-thermal properties prepared in comparative example 5.
Detailed Description
In order to further illustrate the super-hydrophobic photo-thermal coating with heat insulation function and the preparation method thereof, the following embodiments are used for illustrating the invention, but are not used for limiting the invention.
Example 1
(1) According to 1.0:9.0, adding the model E-44 epoxy resin into acetone at room temperature, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 35 minutes to obtain an epoxy resin A solution with the mass concentration of 12%;
(2) According to 2.0:5.0, dissolving ammonium bicarbonate in DMF solution at room temperature, and magnetically stirring for 30 minutes to obtain ammonium bicarbonate B solution with the mass concentration of 40%;
(3) 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 are mixed according to the following ratio of 8.0:2.5: mixing the components in a mass ratio of 0.2, carrying out ultrasonic treatment on the mixture for 20 minutes at room temperature, and then carrying out magnetic stirring on the mixture for 60 minutes to obtain an epoxy resin-ammonium bicarbonate colloid mixed C solution. Taking the solution C as bottom layer slurry for standby;
(4) According to 0.8:0.15:0.4: adding PDMS, carbon nano-tubes, copper sulfide nano-particles and a PDMS curing agent into an ethyl acetate solution with the mass ratio of 1.5:8.0 to the total mass of the materials, carrying out ultrasonic treatment for 30 minutes, and magnetically stirring for 60 minutes to obtain a mixed slurry D;
(5) According to 0.8:1.0:10.0 mass ratio PVDF, ammonium bicarbonate and DMF were formulated into PVDF-ammonium bicarbonate mixed solution E.
(6) According to 10.0:6.0 mass ratio the D slurry and the E solution were mixed and stirred, thereby preparing a mixed slurry F of PDMS, carbon nanotubes, copper sulfide nanoparticles, PVDF, and ammonium bicarbonate. The mixed slurry F is used as upper slurry for standby;
(7) A doctor blade with the height of 2.5 and mm is arranged to uniformly scrape the solution C on the substrate, the substrate is placed for 5 minutes at room temperature and then put into an oven which is heated to 120 ℃ for drying for 4 minutes, and thus an epoxy resin coating with larger holes inside and on the surface is obtained on the substrate.
(8) And (3) uniformly scraping the mixed slurry F on the epoxy resin bottom layer with larger holes in the inner part and the surface in the step (8) by a scraper with the height of 3.0mm, standing for 10 minutes at room temperature, putting the mixture into a baking oven, setting the temperature of the baking oven to 130 ℃, and drying the mixture for 150 minutes.
The mass units of the above materials are consistent.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained. The average diameter of the holes of the prepared bottom epoxy resin is about 90 micrometers through the optimal selection of ammonium bicarbonate, heating and drying time and temperature regulation, 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 the super-hydrophobic photo-thermal coating with heat insulation function prepared in figure 1 has good heat insulation performance and is 1kW/m 2 After irradiation for 30 minutes under power sunlight, the highest temperature of 94.2 ℃ is still obtained after the irradiation is stopped for 2 minutes; from fig. 2, it can be seen that the hydrophobic angle of the surface of the coating reaches 156.23 degrees, and the super-hydrophobic requirement is met.
Example 2
(1) According to 0.9:10.0, adding the model E-44 epoxy resin into acetone at room temperature, performing ultrasonic treatment for 10 minutes, and magnetically stirring for 25 minutes to obtain an epoxy resin A solution with the mass concentration of 9%;
(2) According to 1.5:5.0, dissolving ammonium bicarbonate in DMF solution at room temperature, and magnetically stirring for 25 minutes to obtain 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 10.0:2.0:0.3, carrying out ultrasonic treatment on the mixture for 20 minutes at room temperature, and then carrying out magnetic stirring on the mixture for 60 minutes, thereby obtaining the epoxy resin-ammonium bicarbonate colloid mixed C solution. Taking the solution C as bottom layer slurry for standby;
(4) According to 0.6:0.1:0.3: adding PDMS, carbon nano-tubes, copper sulfide nano-particles and a PDMS curing agent into an ethyl acetate solution with the mass ratio of 1.0:8.0 to the total mass of the materials, performing ultrasonic treatment for 25 minutes, and magnetically stirring for 55 minutes to obtain mixed slurry D;
(5) According to 0.5:1.0:10.0 mass ratio PVDF, ammonium bicarbonate and DMF were formulated into PVDF-ammonium bicarbonate mixed solution E.
(6) According to 10.0:5.0 mass ratio the D slurry and the E solution were mixed and stirred, thereby preparing a mixed slurry F of PDMS, carbon nanotubes, copper sulfide nanoparticles, PVDF, and ammonium bicarbonate. The mixed slurry F is used as upper slurry for standby;
(7) A doctor blade with the height of 2mm is arranged to uniformly scrape the solution C on the substrate, the substrate is placed for 5 minutes at room temperature and then put into an oven which is heated to 110 ℃ for drying for 3 minutes, and thus an epoxy resin coating with larger holes inside and on the surface is obtained on the substrate.
(8) And (3) setting a scraper with the height of 2.5mm, uniformly scraping the mixed slurry F on the epoxy resin bottom layer with larger holes in the inner part and the surface in the step (8), standing for 10 minutes at room temperature, putting the mixture into a baking oven, setting the temperature of the baking oven to 120 ℃, and drying the mixture for 120 minutes.
The mass units of the above materials are consistent.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained. By optimizing the selected ammonium bicarbonate and heating and drying time and temperatureAnd the average diameter of the holes of the prepared lower epoxy resin layer is about 20 micrometers, and the average diameter of the holes of the upper photo-thermal super-hydrophobic coating layer is about 90 nanometers. The product performance is shown in figures 3 and 4, and the super-hydrophobic photo-thermal coating with heat insulation function prepared in figure 3 has good heat insulation performance and is 1kW/m 2 After irradiation for 30 minutes under power sunlight, the highest temperature of 93.6 ℃ still exists after the irradiation is stopped for 2 minutes; from fig. 4, it can be seen that the hydrophobic angle of the surface of the coating reaches 155.10 degrees, and the super-hydrophobic requirement is met.
Example 3
(1) According to 1.0:10.0, adding the model E-44 epoxy resin into acetone at room temperature, performing ultrasonic treatment for 15 minutes, and magnetically stirring for 35 minutes to obtain an epoxy resin A solution with the mass concentration of 10%;
(2) According to 1.8:4.8, dissolving ammonium bicarbonate in DMF solution at room temperature, and magnetically stirring for 30 minutes to obtain ammonium bicarbonate B solution with the mass concentration of 37.5%;
(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 9.0:2.4:0.25, carrying out ultrasonic treatment on the mixture for 20 minutes at room temperature, and then carrying out magnetic stirring on the mixture for 60 minutes, thereby obtaining the epoxy resin-ammonium bicarbonate colloid mixed C solution. Taking the solution C as bottom layer slurry for standby;
(4) According to 0.7:0.15:0.4:0.07 mass ratio of PDMS, carbon nano-tubes, copper sulfide nano-particles and PDMS curing agent are added into ethyl acetate solution with the mass ratio of 1.3:8.0 to the total mass of the materials, and the mixture is subjected to ultrasonic treatment for 30 minutes, and then is magnetically stirred for 60 minutes to obtain mixed slurry D;
(5) According to 0.7:1.5:9.0 the PVDF, ammonium bicarbonate and DMF were formulated as PVDF-ammonium bicarbonate mixed solution E.
(6) According to 10.0:6.0 mass ratio the D slurry and the E solution were mixed and stirred, thereby preparing a mixed slurry F of PDMS, carbon nanotubes, copper sulfide nanoparticles, PVDF, and ammonium bicarbonate. The mixed slurry F is used as upper slurry for standby;
(7) A doctor blade with the height of 2.5 and mm is arranged to uniformly scrape the solution C on the substrate, the substrate is placed for 8 minutes at room temperature and then put into an oven which is heated to 120 ℃ for drying for 4 minutes, and thus an epoxy resin coating with larger holes inside and on the surface is obtained on the substrate.
(8) And (3) uniformly scraping the mixed slurry F on the epoxy resin bottom layer with larger holes in the inner part and the surface in the step (8) by a scraper with the height of 3.0 and mm, standing for 8 minutes at room temperature, putting the mixture into a baking oven, setting the temperature of the baking oven to 125 ℃, and drying the mixture for 135 minutes.
The mass units of the above materials are consistent.
Through the steps, the super-hydrophobic photo-thermal coating with the heat insulation function can be obtained. The diameter of the holes of the prepared lower layer epoxy resin is about 70 micrometers, and the average diameter of the holes of the upper layer photo-thermal super-hydrophobic coating is about 170 nanometers by optimizing and selecting ammonium bicarbonate, heating and drying time and temperature. The prepared super-hydrophobic photo-thermal coating with the heat insulation function has good heat insulation performance and is 1kW/m in size 2 After the irradiation under the power sunlight for 30 minutes, the highest temperature of 93.8 ℃ exists after the irradiation is stopped for 2 minutes, the hydrophobic angle reaches 155.80 degrees, and the hydrophobic angle of the surface of the coating meets the super-hydrophobic requirement.
Example 4
A preparation method of a super-hydrophobic photo-thermal coating with a heat insulation function is the same as that of example 1, but ammonium bicarbonate is not added in step (2). Through the steps, the prepared lower layer epoxy resin is not provided with holes, and the average diameter of the holes of the upper layer photo-thermal super-hydrophobic coating is about 165 nanometers. The prepared coating has super-hydrophobic performance, and the measured hydrophobic angle is 155.82 degrees and is close to that of the example 1; however, due to the lack of the hole structure of the lower epoxy resin, the lower epoxy resin coating loses the heat insulation performance, so that the photo-thermal performance is reduced by 1kW/m 2 After 30 minutes of irradiation under power sunlight, the irradiation was stopped for 2 minutes with a maximum temperature of 78.8 ℃. Furthermore, byHoles are not prepared in the lower epoxy resin coating, so that the coating loses a mechanical interlocking structure, the mechanical properties of the coating are reduced greatly, and the bonding between the film layers is not tight enough, so that the requirements are not met.
Example 5
A preparation method of a super-hydrophobic photo-thermal coating with a heat insulation function is the same as that of example 1, but ammonium bicarbonate is not added in step (5). Through the steps, the average diameter of the holes of the prepared lower epoxy resin layer is about 90 microns, and the holes are not prepared in the upper photo-thermal super-hydrophobic coating layer. The prepared coating has good mechanical properties, but the complex coarse structure on the surface of the coating loses part due to the lack of small holes generated by decomposing ammonium bicarbonate, the hydrophobicity is slightly reduced, and the heat insulation property is also reduced. The product performance is shown in fig. 5 and 6, and it can be seen from fig. 5 that the super-hydrophobic photo-thermal coating with heat insulation function prepared by the method has a much reduced heat insulation performance of 1kW/m compared with the heat insulation performance of the examples 1 and 2 2 After irradiation for 30 minutes under power sunlight, the irradiation is stopped for 2 minutes, and the temperature is only 69.8 ℃; it can be seen from fig. 6 that the hydrophobic angle of the coating surface reaches 154.49 °, and the superhydrophobic requirement is achieved, but the hydrophobic angle is still reduced compared to examples 1 and 2.
Example 6
A preparation method of a super-hydrophobic photo-thermal coating with a heat insulation function is the same as that of example 1, but ammonium bicarbonate is not added in step (2) and step (5). Through the steps, the prepared coating lower layer epoxy resin part lacks large holes generated by decomposing ammonium bicarbonate, loses a mechanical interlocking structure and loses good mechanical properties. The photo-thermal hydrophobic coating on the upper layer is lost in heat insulation due to the lack of small holes generated by decomposing ammonium bicarbonate, and the complex rough structure on the surface of the coating is lost. At 1kW/m 2 After irradiation for 30 minutes under power sunlight, the irradiation was stopped for 2 minutes at a temperature of only 62.4 ℃. The water repellency was measured to be 155.91 °, and was slightly reduced compared to example 1, and the water drop contact angle was similar to example 4. But the mechanical interlocking structure is lost, the mechanical property of the coating is also reduced greatly, and the film layerThe combination is not tight enough, and the requirement is not satisfied.
Example 7
The process parameters and steps of the embodiment are the same as those of the embodiment 1, except that the mass ratio of ammonium bicarbonate particles added into DMF solution in the step (2) is reduced from 2.0 to 1.0, so that the mass ratio of ammonium bicarbonate is smaller than the mass ratio range of 1.5-2.0 in the invention.
The diameter of the prepared lower epoxy resin hole is about 2 microns, and the diameter range of the prepared lower epoxy resin hole is not satisfied by 5-100 microns; the pores of the upper photothermal superhydrophobic coating have an average diameter of about 165 nm. Although a superhydrophobic photo-thermal coating having a heat-insulating function was obtained, the water drop contact angle of the obtained coating was close to that of example 1 when the water-repellent angle was measured to 155.85 °, but the heat-insulating property of the coating was lowered at 1kW/m 2 After the irradiation under the power sunlight for 30 minutes, the irradiation is stopped for 2 minutes, the temperature of 78.6 ℃ is only reached, the mechanical property is also reduced, and the requirement is not met.
Example 8
The process parameters and steps of the embodiment are the same as those 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 exceeds the mass ratio range of 1.0-1.5 in the invention.
Through the steps, the average diameter of the holes of the prepared lower epoxy resin layer is about 90 micrometers, a plurality of macroscopic millimeter holes are formed on the surface of the coating of the upper photo-thermal super-hydrophobic coating layer, the appearance and the hydrophobicity of the coating are affected, the measured hydrophobic angle is 144.31 degrees, and the super-hydrophobic requirement is not met. Furthermore, the heat-insulating property of the coating is reduced by 1kW/m 2 After the irradiation under the power sunlight for 30 minutes, the irradiation is stopped for 2 minutes, the temperature of 72.5 ℃ is only reached, the mechanical property is also reduced, and the requirement is not met.
Example 9
The process parameters of this example are substantially the same as those of example 1, except that steps (1), (2), (3) and (7) are omitted, so that the resulting coating lacks an underlying coating epoxy resin coating.
Through the steps, the toilet bowl is convenientA coating having superhydrophobic photo-thermal properties was obtained, which was hardly affected in the surface hydrophobicity as compared with example 1 in which the underlying epoxy resin coating was absent, and the hydrophobicity was measured to be 156.12 ℃but the heat insulation property was lowered at 1kW/m 2 After the irradiation for 30 minutes under the power sunlight, the irradiation is stopped for 2 minutes, and the temperature is only 77.2 ℃, so that the mechanical property is reduced, and the film layer cannot be tightly combined with the substrate, so that the requirements are not met.
Example 10
The process parameters and steps of the embodiment are approximately the same as those of the embodiment 1, except that the steps (4), (5), (6) and (8) are omitted, so that the prepared coating lacks the photothermal super-hydrophobic coating of the upper coating.
By the above steps, an epoxy resin coating with fine holes on the surface can be obtained, which has completely lost the hydrophobic property at 1kW/m compared with the coating of example 1 lacking the upper photo-thermal super-hydrophobic coating 2 After the irradiation for 30 minutes under the power sunlight, the irradiation is stopped for 2 minutes, and the temperature is only 33.6 ℃, so that the requirements are not met.
The foregoing is a preferred embodiment of the present invention and a comparative example, but the present invention should not be limited to the disclosure of this embodiment. So that equivalents and modifications will fall within the scope of the invention, all within the spirit and scope of the invention as disclosed.
Claims (5)
1. The preparation method of the super-hydrophobic photo-thermal coating with the heat insulation function is characterized by comprising the following steps of:
(1) Dissolving epoxy resin in acetone to form an epoxy resin solution A;
(2) Dissolving ammonium bicarbonate in a dimethylformamide solvent to form ammonium bicarbonate solution B;
(3) Epoxy resin solution A, ammonium bicarbonate solution B and epoxy resin curing agent are mixed according to the proportion of 8.0-10.0: 2.0 to 2.5: mixing the components according to the mass ratio of 0.2-0.3, and carrying out ultrasonic treatment and uniform stirring at room temperature to obtain an epoxy resin-ammonium bicarbonate colloid mixed solution C;
(4) Polydimethyl siloxane, carbon nano tubes, copper sulfide nano particles and PDMS curing agent according to the proportion of 0.6 to 0.8:0.1 to 0.15:0.3 to 0.4: adding 0.06-0.08 mass ratio into ethyl acetate solvent to prepare mixed slurry D, wherein the size of copper sulfide nano particles is 200-500 nanometers;
(5) Adding polyvinylidene fluoride and ammonium bicarbonate with the mass ratio of 0.5-0.8:1.0-1.5 into a DMF solvent to prepare PVDF-ammonium bicarbonate mixed solution E;
(6) Mixing and stirring the mixed slurry D and the solution E according to the mass ratio of 9.0-10.0:5.0-6.0, thereby preparing mixed slurry F of PDMS, carbon nano-tubes, copper sulfide nano-particles, PVDF and ammonium bicarbonate;
(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 substrate coated with a film in a baking oven for baking and drying, and obtaining an epoxy resin coating with holes in the interior and the surface after baking;
(8) And (3) coating the mixed slurry F prepared in the step (6) with the epoxy resin coating with holes inside and on the surface prepared in the step (7), and then placing the mixed slurry F in an oven for baking and drying to obtain the super-hydrophobic photo-thermal coating with the heat insulation function after baking.
2. The preparation method of the super-hydrophobic photo-thermal coating with the heat insulation function according to claim 1, wherein in the step (1), the model E-44 epoxy resin is added into acetone at room temperature and subjected to ultrasonic treatment for 10-15 minutes, and then magnetically stirred for 25-35 minutes to obtain an epoxy resin solution A; wherein the mass concentration of the epoxy resin is 9-12%.
3. The preparation method of the super-hydrophobic photo-thermal coating with the heat insulation function according to claim 1, wherein in the step (2), ammonium bicarbonate is dissolved in DMF (dimethyl formamide) solution at room temperature, and is magnetically stirred for 25-30 minutes to obtain ammonium bicarbonate solution B, wherein the mass concentration of the ammonium bicarbonate is 30-45%.
4. The preparation method of the super-hydrophobic photo-thermal coating with the heat insulation function according to claim 1, wherein a scraper with the height of 2-2.5 mm is arranged in the step (7) to uniformly scrape the solution C on a 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.
5. The preparation method of the super-hydrophobic photo-thermal 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 to uniformly scrape the mixed slurry F on the epoxy resin bottom layer with larger holes in the inner part and the surface of the mixed slurry F in the step (7), the mixed slurry F is placed into an oven after being kept stand for 5-10 minutes at room temperature, the temperature of the oven is set to 120-130 ℃, and the mixed slurry F is dried for 120-150 minutes.
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