CN115011225A - Bionic frost-preventing and removing material and preparation method and application thereof - Google Patents
Bionic frost-preventing and removing material and preparation method and application thereof Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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Abstract
The invention provides a bionic anti-icing and frost-removing material and a preparation method and application thereof.A microcapsule phase change material is used for effectively preventing the leakage of the phase change material and the volume change caused by phase change, and the stability of temperature control and heat release in the bionic anti-icing and frost-removing material is improved by compounding the microcapsule phase change material with a first polymer resin; the hydrophobic modified photo-thermal composite fiber material and the second polymer resin are utilized to construct the super-hydrophobic photo-thermal layer of the micro-nano hierarchical porous network, so that high absorption of light in a broad spectrum and high light-heat conversion capability are realized. By utilizing the multi-element synergistic effect of the super-hydrophobic photothermal layer and the phase change energy release layer, the solar energy heat dissipation layer has the function of preventing and removing ice and frost in all weather (at night and in the daytime), effectively solves the problem of unbalance of solar energy supply, and has higher recycling value.
Description
Technical Field
The invention belongs to the technical field of chemistry and materials, and particularly relates to a bionic frost prevention and removal material, a preparation method thereof and application thereof in the field of outdoor engineering such as electric power communication, fan blades, locomotives, aviation and the like.
Background
Icing and frosting are ubiquitous natural phenomena, but for the fields of electric power communication, aerospace, transportation and the like, ice adhesion and accumulation often bring serious safety hazards and great economic loss. Power failure accidents caused by icing of transmission lines; the service life loss of the unit caused by the icing of the fan blade; safety accidents caused by icing of the vehicle chassis and flight accidents caused by frosting of the airplane.
The icing on the surface of the material is mostly caused by the collision of the supercooled water with the surface, and depends on a plurality of factors such as ice adhesion, hydrodynamic conditions, a water film structure on the surface, and the surface energy of the surface. At present, ice control technologies are mainly divided into two types, the first type is an active deicing method, including a mechanical deicing method, an electrothermal deicing method, a chemical deicing method and the like, and the defects of low efficiency, high energy consumption, environmental pollution and difficulty in meeting social requirements are overcome. The second method is a passive anti-icing method, which is to coat or construct an anti-icing coating on the surface of the material to reduce the adhesion amount of ice on the surface of the material, and the ice is typically a lubricated surface represented by nepenthes and a super-hydrophobic surface represented by lotus leaves. For lubricated surfaces, the difficulty of large area preparation, as well as the consumption of lubricating fluids and environmental pollution, have limited the development and widespread use of such surfaces. The super-hydrophobic surface can slow down the icing of the surface to a certain extent, but researches find that the super-hydrophobic surface has stronger dependence on temperature, the anti-icing time is shorter, and the super-hydrophobic surface is easy to lose efficacy in a high-humidity environment. Once frozen, ice adheres to the surface of the material in a "pinning" manner, creating greater deicing challenges. Meanwhile, after the surface is subjected to a plurality of icing and deicing cycles, the surface micro-nano structure can be damaged, and the ice adhesion strength is obviously increased. Recently, some new solar photo-thermal surfaces have demonstrated the potential for environmentally friendly and energy efficient deicing protection. Current design strategies focus more on photothermal conversion efficiency and ignore effective management of thermal energy. Resulting in excellent defrosting effect during the day and complete failure at night. In addition, the existing anti-icing frost technology generally has the problems of short frost control time, poor frost control effect after multiple use, poor mechanical damage resistance, limitation by an external light source and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a bionic frost control material and a preparation method and application thereof. The bionic anti-icing material has the characteristics of cyclic utilization, high efficiency and energy saving while achieving the aim of preventing icing and defrosting in all weather.
The invention aims to realize the following technical scheme:
a bionic frost prevention material comprises a phase change energy release layer and a super-hydrophobic photothermal layer; the phase change energy release layer comprises a microcapsule phase change material and first high polymer resin; the super-hydrophobic photo-thermal layer comprises a hydrophobic modified photo-thermal composite fiber material and second high polymer resin, and is coated on the surface of the phase-change energy release layer.
In the present invention, the term "frost control material" refers to a material having both active and passive frost control capabilities.
According to the invention, the microcapsule phase change material is used for effectively preventing the leakage of the phase change material and the volume change caused by phase change, and the stability of temperature control and heat release in the bionic anti-icing and deicing material is improved by compounding the microcapsule phase change material with the first polymer resin; a hydrophobic modified photo-thermal composite fiber material and second polymer resin are utilized to construct a super-hydrophobic photo-thermal layer of a micro-nano hierarchical porous network, so that high absorption of light in a broad spectrum and high light-heat conversion capability are realized. By utilizing the multi-element synergistic effect of the super-hydrophobic photothermal layer and the phase change energy release layer, the coating has the function of preventing and removing frost in all weather (at night and in daytime).
According to the invention, the thickness of the phase change energy release layer is 1-200mm, such as 1mm, 5mm, 10mm, 15mm, 20mm, 30mm, 40mm, 50mm, 60mm, 70mm, 80mm, 90mm, 100mm, 110mm, 120mm, 130mm, 150mm, 170mm, 180mm, 190mm or 200mm, and specifically, coatings or sample blocks with different shapes and thicknesses can be made according to the requirements of working conditions.
According to the invention, the phase change latent heat released by the phase change energy release layer in a severe cold environment (below 0 ℃) is more than 70kJ/kg, and the phase change point migration does not exceed 1 ℃ after repeated heat absorption and heat release through thermal cycle stability measurement.
According to the invention, the raw materials for preparing the phase change energy release layer comprise a microcapsule phase change material, a first high polymer resin, a first curing agent and a solvent.
According to the invention, the raw materials for preparing the phase change energy release layer comprise the following components in percentage by weight:
25-75 parts of microcapsule phase change material; 15-75 parts of first high polymer resin; 1-35 parts of a first curing agent; 10-50 parts of solvent.
Preferably, the raw materials for preparing the phase change energy release layer comprise the following components in percentage by weight:
50-66 parts of microcapsule phase change material; 23-50 parts of first high polymer resin; 5-11 parts of a first curing agent; 20-40 parts of solvent.
According to the invention, the phase-change energy release layer is prepared by the following method:
uniformly mixing the microcapsule phase change material, the first polymer resin, the first curing agent and the solvent, and curing to prepare the phase change energy release layer.
Wherein the curing temperature is room temperature, and the curing time is 8-24 hours.
According to the invention, the microcapsule phase change material has a core-shell structure and comprises a core and a shell, wherein the core is a phase change material, and the shell is a film forming material.
Wherein the phase change material is at least one of inorganic phase change material, organic phase change material or mixed phase change material (phase change material formed by mixing inorganic phase change material and organic phase change material), solid-liquid phase change temperature region is-30 deg.C-20 deg.C, such as straight chain alkane (C) 8-20 ) Paraffin, fatty acids, polyhydric alcohols, and the like. In the embodiment of the invention, the phase-change material is preferably one or a combination of dodecane, tridecane, methyl laurate, n-decanol, tetradecane, pentadecane, hexadecane and the like.
Wherein the film-forming material is a high molecular material or an inorganic material, such as at least one of polyethylene, polybutadiene, polystyrene, polyether, polypropylene, polyacrylamide, polysiloxane, polymethyl methacrylate, polyurea, polyamide, isocyanate, urea-formaldehyde polymer, melamine-formaldehyde polymer, silica, calcium carbonate, titanium dioxide, calcium silicate, and the like.
According to the invention, the microcapsule phase change material can be prepared by adopting an in-situ polymerization method, an interfacial polycondensation method or a sol-gel method known in the field.
According to the invention, the particle size of the microcapsule phase change material is 5-150 μm. The microcapsule phase change material comprises a phase change material and a film forming material, wherein the mass ratio of the phase change material to the film forming material is 3: 7-7: 3. The enthalpy value of the microcapsule phase change material is more than 100 kJ/kg. The enthalpy retention rate of the microcapsule phase change material is more than 65%.
According to the present invention, the first polymer resin is at least one selected from epoxy resin, polyurethane, hydroxyacrylic resin, and the like. The first polymer resin has a setting function, and preferably has a room temperature curing and bonding function.
According to the present invention, the first curing agent is selected from ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, polyethylenepolyamine, isophoronediamine, diaminodicyclohexylmethane, methylcyclopentadiene, diaminomethylcyclohexanediamine, m-xylylenediamine, diaminodiphenylmethane, 650 low molecular polyamide, 651 low molecular polyamide, T31 curing agent, 593 curing agent, amino resin, Toluene Diisocyanate (TDI), isophorone diisocyanate (IPDI) diphenylmethane diisocyanate (MDI), Hexamethylene Diisocyanate (HDI), and the like.
According to the present invention, the solvent is selected from acetone, absolute ethanol, toluene, xylene, styrene, ethyl acetate, butyl acetate, dimethylformamide, polyhydric alcohol, benzyl alcohol, butyl glycidyl ether, 1, 4-butanediol diglycidyl ether, ethylene glycol diglycidyl ether, neopentyl glycol diglycidyl ether, polypropylene glycol diglycidyl ether, 1, 6-hexanediol diglycidyl ether, and the like.
According to the invention, the thickness of the super-hydrophobic smooth thermal layer is 50-250 μm, such as 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm, 120 μm, 130 μm, 140 μm, 150 μm, 160 μm, 180 μm, 200 μm, 220 μm, 230 μm, 240 μm and 250 μm, and specifically, coatings or sample blocks with different shapes and thicknesses can be made according to the requirements of working conditions.
According to the invention, the contact angle of the super-hydrophobic smooth thermal layer is more than or equal to 154 degrees; the rolling angle is less than or equal to 3 degrees; the adhesive force is more than 1-2 grade, and the coating hardness is more than 2H.
According to the invention, the hydrophobic modified photothermal composite fiber material is selected from composite materials of hydrophobic modified nanoparticles and carbon-based photothermal fibers.
Wherein the carbon-based photothermal fibers are selected from carbon nanotubes, carbon nanofibers, fullerene nanofibers, black silicon carbide fibers, carbonized carboxymethyl cellulose, and the like.
The nano particles are selected from any one or two of nano silicon dioxide, nano titanium dioxide, nano copper sulfide, nano copper phosphide, nano titanium dioxide, nano black phosphorus and the like.
Wherein, carbon back light and heat fibrous surface's functional group includes the combination of any one or more than two kinds in carbonyl, carboxyl and the hydroxyl, can graft the nanoparticle through above-mentioned functional group to carbon back light and heat fibrous surface effectively increases fibre surface roughness to do benefit to further hydrophobic modification.
Among them, the method of hydrophobic modification is known in the art, such as reaction with monosilane, siloxane or silazane to achieve hydrophobic modification.
According to the invention, the hydrophobic modified photo-thermal composite fiber material is preferably a hydrophobic modified silicon dioxide-multi-walled carbon nanotube.
Wherein the silica-multi-walled carbon nanotube is a silica-loaded multi-walled carbon nanotube, and the hydrophobically modified silica-multi-walled carbon nanotube is obtained by hydrophobically modifying the surface of the silica-loaded multi-walled carbon nanotube, for example, by reacting the silica-multi-walled carbon nanotube with silane, siloxane or silazane.
Wherein the monosilane is, for example, trimethylchlorosilane.
Wherein the siloxane may be Si (C) 1-10 Alkyl) (OC 1-10 Alkyl radical) 3 Such as n-octyltriethoxysilane.
Among them, the silazanes such as hexamethyldisilazane.
According to the invention, the raw materials for preparing the super-hydrophobic photo-thermal layer comprise a hydrophobic modified photo-thermal composite fiber material, a diluent, a second polymer resin and a second curing agent.
According to the invention, the raw materials for preparing the super-hydrophobic smooth thermal layer comprise the following components in percentage by mass:
10-30 parts of a hydrophobic modified photo-thermal composite fiber material; 70-90 parts of second high polymer resin; 5-15 parts of a second curing agent; diluent, 400 portions and 800 portions.
The second polymer resin is selected from one or a mixture of more of fluorocarbon resin, fluorosilicone resin and organic silicon modified acrylic resin. Preferably, the surface energy of the super-hydrophobic photothermal layer prepared after the second polymer resin is cured is lower than 25J/m 2 Has better antifouling effect.
Wherein the second curing agent is selected from aliphatic isocyanate, alicyclic isocyanate, aromatic isocyanate and derivatives thereof, such as commercially available products N75, N3390, N3375 and the like.
Wherein the diluent is selected from one or a mixture of more of xylene, toluene, butanol, ethyl acetate, n-hexane, cyclohexanone, n-butanol, isopropyl acetate, butyl acetate, isopropanol, propylene glycol methyl ether, propylene glycol ethyl ether, ethylene glycol methyl ether, propylene glycol methyl ether acetate and ethyl lactate.
According to the invention, the super-hydrophobic smooth thermal layer is prepared by the following method:
1) mixing the hydrophobic modified photo-thermal composite fiber material and a diluent to prepare a uniform dispersion liquid;
2) mixing the dispersion liquid prepared in the step 1), a second polymer resin and a second curing agent, and curing to prepare the super-hydrophobic photo-thermal layer coating.
According to the invention, the super-hydrophobic smooth thermal layer is prepared by the following method:
1) mixing the hydrophobic modified photo-thermal composite fiber material and a diluent, performing ultrasonic treatment for 0.5h, and stirring for 15min to fully mix the materials to prepare a uniform dispersion liquid;
2) mixing the dispersion liquid prepared in the step 1), a second polymer resin and a second curing agent, and curing to prepare the super-hydrophobic photo-thermal layer coating.
The invention also provides a preparation method of the bionic anti-icing and deicing material, which comprises the following steps:
1) preparing a phase change energy release layer and preparing a coating of the super-hydrophobic light and heat layer;
2) and coating the paint for preparing the super-hydrophobic smooth and hot layer on the surface of the phase change energy release layer, and curing and drying to form the bionic anti-icing and frost-removing material.
According to the invention, in step 2), the curing temperature is room temperature, and the curing time is 8-24 hours.
According to the invention, in step 2), the coating comprises at least one of spraying, brushing, rolling and the like.
According to the invention, the bionic anti-icing material can be applied to anti-icing treatment in the outdoor engineering fields of power communication, fan blades, locomotives, airplane aviation and the like.
In the invention, the aim of deicing can be achieved without an additional light source and device when the bionic deicing material is used, and the limit of the bionic deicing material on low-temperature deicing can be greatly widened.
In the invention, the development process of the bionic anti-icing and frost-removing material is mainly inspired by the synergistic thermal management of polar bear ternary (hair-hydrophobic and black skin-light energy is converted into heat energy and fat-stored and released heat energy), and a novel multi-element synergistic bionic anti-icing and frost-removing material is designed by applying a bionic synergistic idea and comprises a super-hydrophobic photothermal layer and a phase change energy release layer.
The bionic deicing and deicing material has the humidity of 20 percent at the temperature of between 15 ℃ below zero and 18 ℃ below zero, can not freeze under the condition of illumination, and can effectively delay the freezing for more than 8 hours under the condition of no illumination.
The surface layer of the bionic anti-fouling/anti-fouling material has excellent super-hydrophobic property and photo-thermal property, the contact angle is larger than or equal to 154 degrees, and the rolling angle is smaller than or equal to 3 degrees; after being polished by 800-sand-1000-mesh sand paper for 40 times, the contact angle still reaches 147 degrees, the rolling angle is 11.5 degrees, and the anti-icing and deicing performances can be continuously provided. The phase change energy release layer has stable and reversible phase change process and large latent heat, and effectively realizes the stability of controlling the temperature in the frost prevention and control material.
The invention has the beneficial effects that:
the bionic anti-icing and deicing material disclosed by the invention can realize the combination of super-hydrophobic anti-icing and photo-thermal deicing, and is cooperated with the phase change energy release layer, so that the ice control efficiency of the super-hydrophobic photo-thermal layer is further improved, and the optimal anti-icing and deicing effect is achieved. In the daytime, sunlight irradiates the super-hydrophobic photothermal layer, light energy is quickly converted into heat energy, the surface temperature of the material is improved, and surface liquid drops are automatically separated from the surface before freezing by utilizing the self-cleaning performance of the super-hydrophobic surface; meanwhile, the microcapsule phase change agent in the phase change layer continuously absorbs heat. At night, the ambient temperature is reduced, and the phase change energy release layer begins to release heat, so that the whole material is maintained above the icing temperature of the super-hydrophobic layer, the anti-icing performance of the super-hydrophobic structure is continuously exerted, and the icing time is prolonged. Even if a small amount of ice is coated, the heat generated by illumination can melt the ice layer on the surface of the material.
The microcapsule phase change material is used for effectively preventing the leakage of the phase change material and the volume change caused by phase change, and the stability of temperature control and heat release in the bionic frost prevention and removal material is improved by compounding the microcapsule phase change material with the first high polymer resin; a hydrophobic modified photo-thermal composite fiber material and second polymer resin are used for constructing a super-hydrophobic photo-thermal layer of a micro-nano hierarchical porous network, so that high absorption of light and high light-heat conversion capability in a broad spectrum are realized. By utilizing the multi-element synergistic effect of the super-hydrophobic photothermal layer and the phase change energy release layer, the solar energy heat dissipation layer has the function of preventing and removing ice and frost in all weather (at night and in the daytime), effectively solves the problem of unbalance of solar energy supply, and has higher recycling value.
The preparation method has the advantages of simple process, convenient operation, normal-temperature curing, easy industrial production and the like, can be used for preparing the anti-icing and anti-frosting material in a large scale, and is beneficial to industrial application.
The bionic deicing and deicing material disclosed by the invention can be widely applied to deicing and deicing treatment of engineering components such as vehicles, airplanes, blades and the like, and has the advantages of no energy consumption, low cost and no pollution to the environment.
Drawings
FIG. 1 is a schematic diagram of the bionic frost control material prepared in example 2 of the present invention.
Fig. 2 is a transmission electrogram of hydrophobically modified silica-multiwall carbon nanotubes prepared in example 2 of the present invention.
Fig. 3 is a scanning electron microscope image and a contact angle image of the superhydrophobic photothermal layer with different amounts of hydrophobically modified silica-multi-walled carbon nanotubes added in example 2 of the present invention.
Fig. 4 shows the photothermal effect of the test pieces of comparative examples 2 to 3 and example 2 according to the present invention.
FIG. 5 is a graph showing the control performance at-20 ℃ in example 2 of the present invention, comparative example 1 and comparative example 3.
FIG. 6 is a graph showing the change in the amount of surface frost formed by six cycles of heating and cooling at-30 ℃ in example 2 of the present invention and comparative example 3.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
Example 1
With dodecane as core, silicon dioxide (SiO) 2 ) For film-forming material, the microencapsulated dodecane phase change agent is prepared by adopting an in-situ interfacial polycondensation method.
75 parts of microencapsulated dodecane phase change agent, 18 parts of hydroxy acrylic resin, 7 parts of hexamethylene diisocyanate and 40 parts of dimethylbenzene are uniformly mixed, placed in a cylindrical polytetrafluoroethylene mold, applied pressure is 6mPa, cured at room temperature for 12 hours, and demolded to obtain a phase change energy release layer with the thickness of 3 mm.
Dispersing 120mg of carboxyl-based multi-wall carbon nanotube powder in 150mL of mixed solution of ethanol and water (the volume ratio of the ethanol to the water is 145:5) and performing ultrasonic action for 0.5h to obtain black suspension. Then, 2.4mL of ethyl orthosilicate was added to the black suspension to adjust the pH to 9-10, thereby obtaining a mixture. The mixture was placed in a 250mL Teflon autoclave and heated to 110 ℃ for 10 h. And after the hydrothermal reaction, performing centrifugal separation at 10000r/min for 10min, washing with methanol for at least three times, and drying to prepare the silicon dioxide-multi-walled carbon nanotube.
2.0g of the prepared silica-multiwall carbon nanotube was added to 50mL of ethanol and 3mL of n-octyltriethoxysilane, and the pH was adjusted to 9-10 to obtain a mixed solution. The mixed solution was stirred at 60 ℃ for 6 to 8 hours and left at room temperature for 24 hours. And then washing the fiber with ethanol for three times, and drying the fiber at 150 ℃ for 5min to obtain the n-octyltriethoxysilane-modified silicon dioxide-multi-walled carbon nanotube composite fiber.
20 parts by weight of n-octyltriethoxysilane-modified silica-multiwalled carbon nanotube composite fiber and 600 parts by weight of mixed solvent (the volume ratio of xylene to butyl acetate is 7:3) are subjected to ultrasonic treatment for 0.5 hour, and then are subjected to electric stirring and dispersion for 15 minutes to be fully mixed, so that uniform dispersion liquid is prepared. Adding 85 parts by weight of fluorocarbon resin and 9 parts by weight of curing agent N75, and stirring for 15 minutes to obtain the super-hydrophobic photo-thermal layer coating.
And spraying the prepared paint of the super-hydrophobic smooth thermal layer on the surface of the dried phase change energy release layer, wherein the thickness of a dry film of the coating is 150 mu m.
Example 2
With tetradecane as core and silicon dioxide (SiO) 2 ) The microencapsulated tetradecane phase-change agent is prepared by adopting an in-situ interface polycondensation method as a film-forming material.
Uniformly mixing 66 parts of microencapsulated tetradecane phase change agent, 23 parts of epoxy resin, 11 parts of isophorone diamine and 40 parts of xylene, putting the mixture into a cylindrical polytetrafluoroethylene mold, applying pressure of 4mPa, curing at room temperature for 12 hours, and demolding to obtain a phase change energy release layer with the thickness of 5 mm.
The preparation method of the silica-multiwall carbon nanotube is the same as that of example 1.
2.0g of the silica-multiwalled carbon nanotube prepared above was added to 50mL of ethanol and 4mL of hexamethyldisilazane, and the pH was adjusted to 9-10 to obtain a mixed solution. The mixed solution was stirred at 60 ℃ for 6 to 8 hours and left at room temperature for 24 hours. And then washing the fiber with ethanol for three times, and drying the fiber at 150 ℃ for 5min to obtain the hexamethyldisilazane-modified silicon dioxide-multiwalled carbon nanotube composite fiber.
The preparation method comprises the following steps of carrying out ultrasonic treatment on 15 parts by weight of hexamethyldisilazane-modified silicon dioxide-multiwalled carbon nanotube composite fiber and 600 parts by weight of mixed solvent (the volume ratio of ethyl acetate to butyl acetate is 1:1) for 0.5 hour, and then carrying out electric stirring and dispersion for 15 minutes to fully mix the materials to prepare uniformly dispersed dispersion liquid. Adding 90 parts by weight of fluorosilicone resin and 10 parts by weight of N3390, and stirring for 15 minutes to obtain the super-hydrophobic photo-thermal layer coating.
And spraying the prepared paint for forming the super-hydrophobic smooth thermal layer on the surface of the dried phase-change energy-release layer, wherein the thickness of a dry film of the paint is 100 mu m.
The superhydrophobic smooth-thermal layer added with the silicon dioxide-multi-walled carbon nanotube composite fiber content modified by hexamethyldisilazane with different contents is prepared according to the method in the example 2. The hexamethyldisilazane-modified silicon dioxide-multiwalled carbon nanotube composite fiber comprises, by weight, 5 parts, 10 parts, 15 parts, 20 parts and 30 parts of the hexamethyldisilazane-modified silicon dioxide-multiwalled carbon nanotube composite fiber, 90 parts of fluorosilicone resin and 10 parts of N3390, wherein the hexamethyldisilazane-modified silicon dioxide-multiwalled carbon nanotube composite fiber accounts for 5%, 10%, 15%, 20% and 30% of the total weight of the fluorosilicone resin and the N3390. The scanning electron microscope image and the contact angle image are shown in fig. 3, and it can be seen from the images that the size of the formed network pores is gradually reduced, the number of the pores is gradually increased, and the hydrophobicity is gradually enhanced with the increase of the content of the hexamethyldisilazane modified silica-multi-walled carbon nanotube composite fiber.
The photothermal properties of the biomimetic anti-icing material prepared according to example 2 at low temperature are shown in FIG. 4. The light source is simulated sunlight (xenon lamp), and the illumination intensity is 1kw/m 2 And starting to illuminate the sample block at the temperature of-21 ℃, turning off the light source when the temperature is raised to 30 ℃, and detecting the change of the temperature along with the time by using infrared imaging. Example 2 contains a super-hydrophobic photo-thermal layer and a phase change energy release layer, and the temperature is rapidly increased under the illumination condition; turning off the light source, a delay time plateau occurs during the cooling process. Comparative example 2 is an epoxy resin sample block of the same size, and the temperature rise and decrease speed is relatively slow at-21 DEG C(ii) a Comparative example 3 because the super-hydrophobic smooth thermal layer was sprayed, under the illumination condition, the temperature was rapidly raised, the light source was turned off, and the temperature was rapidly lowered.
Example 3
Tridecane/hexadecane (mass ratio 1:1) is used as an inner core, urea formaldehyde resin is used as a film forming material, and an in-situ polymerization method is adopted to prepare the microencapsulated tridecane/hexadecane phase change agent.
50 parts of microencapsulated tridecane/hexadecane phase change agent, 40 parts of polyurethane, 10 parts of TDI and 10 parts of dimethylformamide are spread on tinplate, and cured for 8-12 hours at room temperature to obtain a phase change energy release layer with the thickness of 2 mm.
The preparation method of the silica-multiwall carbon nanotube is the same as that of example 1.
2.0g of the silica-multiwall carbon nanotube prepared above was added to 50mL of ethanol and 6mL of trimethylchlorosilane, and the pH was adjusted to 9-10 to obtain a mixed solution. And (3) placing the mixed solution at 60 ℃, stirring for 6-8 hours, placing for 24 hours, then washing with ethanol for three times, and drying at 150 ℃ for 5min to obtain the trimethylchlorosilane modified silicon dioxide-multi-walled carbon nanotube composite fiber.
20 parts by weight of trimethylchlorosilane modified silicon dioxide-multi-walled carbon nanotube composite fiber and 600 parts by weight of mixed solvent (the volume ratio of xylene to ethyl acetate is 7:3) are subjected to ultrasonic treatment for 0.5 hour, and then are stirred and dispersed for 15 minutes in an electric mode to be mixed fully, so that uniform dispersion liquid is prepared. And adding 90 parts by weight of organic silicon modified acrylic resin and 10 parts by weight of HDI, and stirring for 15 minutes to obtain the super-hydrophobic photo-thermal coating.
And spraying the prepared paint of the super-hydrophobic smooth thermal layer on the surface of the dried phase-change energy-release layer, wherein the thickness of a dry film of the paint is 150 mu m.
Comparative example 1
Tinplate of the same size.
Comparative example 2
Epoxy cured swatches of the same size. And (3) uniformly mixing 66 parts of epoxy resin, 33 parts of isophorone diamine and 10 parts of dimethylbenzene, putting the mixture into a cylindrical polytetrafluoroethylene mold, applying pressure of 4mPa, curing at room temperature for 12 hours, and demolding to obtain a phase change energy release layer with the thickness of 5 mm.
Comparative example 3
The other operation is the same as that of example 2, except that the phase change energy release layer does not contain the microencapsulated tetradecane phase change agent.
Comparative example 4
Microencapsulated dodecane and hydroxy acrylic resin with the same size are used for curing the phase change layer sample block.
Uniformly mixing 75 parts by weight of microencapsulated dodecane phase change agent, 18 parts by weight of hydroxyl acrylic resin, 7 parts by weight of hexamethylene diisocyanate and 40 parts by weight of dimethylbenzene, putting the mixture into a cylindrical polytetrafluoroethylene mold, applying pressure of 6mPa, curing at room temperature for 12 hours, and demolding to obtain a phase change energy release layer with the thickness of 3 mm.
The test sample blocks prepared in the embodiment 1 and the comparative example 4 of the invention are placed in an environment with the temperature of-20 ℃ for testing the frosting and defrosting performances, the comparative example 4 contains the phase-change material, the heat can be released in the environment with the temperature below 0 ℃, and the frosting phenomenon can occur after the test sample blocks are placed for 30 minutes, but the comparative example 4 does not have a photo-thermal layer, the temperature rise is slow, the energy storage efficiency is slow, and the frost can not be melted. Example 1 had no frosting after 30 minutes of standing due to the presence of the photothermal layer and the phase change layer.
The test pieces prepared in example 2 of the present invention and comparative examples 1 and 3 were photographed by being placed at-20 c, as shown in fig. 5, wherein the first behavior is comparative example 1, the second behavior is comparative example 3, and the third behavior is example 2, and it can be seen that the test pieces prepared in comparative examples 1 and 3 were frosted after being placed at-20 c for 5min in a dark environment, and the test pieces prepared in example 2 were not frosted after being placed at-20 c for 30min due to the photo-thermal layer and the phase change layer. When the test piece prepared in comparative example 1 was irradiated with a light source for 8min, the frost was not melted; in comparative example 3, icing phenomenon starts to occur after the glass is placed at-20 ℃ for 5min, and due to the super-hydrophobic photo-thermal layer, the frost starts to melt after being irradiated by a light source for 5min, and the frost completely melts after being irradiated for 8 min. When the lamp-off time was extended to 60 minutes, a small amount of frosting occurred in example 2, while more frosting occurred in comparative example 3, as shown in FIG. 6, at-20 deg.C, 0.7kw/m 2 The condition was that the lamp was turned on and off for 6 cycles (60 minutes for off and 60 minutes for on for 1 cycle).
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made without departing from the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A bionic anti-icing material comprises a phase change energy release layer and a super-hydrophobic photothermal layer; the phase change energy release layer comprises a microcapsule phase change material and a first high polymer resin; the super-hydrophobic photo-thermal layer comprises a hydrophobic modified photo-thermal composite fiber material and second high polymer resin, and is coated on the surface of the phase-change energy release layer.
2. The material of claim 1, wherein the phase change release layer has a thickness of 1-200 mm.
3. The material of claim 1 or 2, wherein the phase change energy release layer is prepared from raw materials comprising a microcapsule phase change material, a first polymer resin, a first curing agent and a solvent; preferably, the raw materials for preparing the phase-change energy-release layer comprise the following components in percentage by mass:
25-75 parts of microcapsule phase change material; 15-75 parts of first high polymer resin; 1-35 parts of a first curing agent; 10-50 parts of solvent.
4. The material according to any one of claims 1-3, wherein the first polymeric resin is selected from at least one of epoxy, polyurethane, hydroxy acrylic resin, and the like;
preferably, the microcapsule phase change material has a core-shell structure and comprises a core and a shell, wherein the core is a phase change material, and the shell is a film forming material.
5. The material of any one of claims 1-4, wherein the super-hydrophobic smooth thermal layer has a thickness of 50-250 μm.
Preferably, the contact angle of the super-hydrophobic glossy and thermal layer is greater than or equal to 154 degrees; the rolling angle is less than or equal to 3 degrees; the adhesive force is more than 1-2 grade, and the coating hardness is more than 2H.
6. The material of any one of claims 1-5, wherein the hydrophobically modified photothermal composite fiber material is selected from composites of hydrophobically modified nanoparticles and carbon-based photothermal fibers.
Preferably, the carbon-based photothermal fibers are selected from carbon nanotubes, carbon nanofibers, fullerene nanofibers, black silicon carbide fibers, carbonized carboxymethyl cellulose, and the like.
Preferably, the photo-thermal nanoparticles are selected from any one or two of nano-silica, nano-titanium dioxide, nano-copper sulfide, nano-copper phosphide, nano-titanium dioxide, nano-black phosphorus and the like.
Preferably, the hydrophobic modified photo-thermal composite fiber material is preferably hydrophobic modified silica-multi-walled carbon nanotubes.
7. The material of any one of claims 1-6, wherein the raw materials for preparing the super-hydrophobic photothermal composite layer comprise the hydrophobically modified photothermal composite fiber material, a diluent, a second polymer resin and a second curing agent.
Preferably, the raw materials for preparing the super-hydrophobic smooth thermal layer comprise the following components in percentage by mass:
10-30 parts of a hydrophobic modified photo-thermal composite fiber material; 70-90 parts of second high polymer resin; 5-15 parts of a second curing agent; diluent, 400 portions and 800 portions.
8. The material according to any one of claims 1 to 7, wherein the second polymer resin is selected from one or a mixture of fluorocarbon resin, fluorosilicone resin and organosilicon modified acrylic resin.
9. A method of preparing a biomimetic anti-icing material according to any of claims 1-8, the method comprising the steps of:
1) preparing a phase change energy release layer and preparing a coating of the super-hydrophobic smooth and hot layer;
2) and coating the coating for preparing the super-hydrophobic smooth thermal layer on the surface of the phase change energy release layer, and curing and drying to form the bionic anti-icing and frost-removing material.
10. Use of the biomimetic anti-icing material according to any of claims 1-8 in an anti-icing process in the field of outdoor engineering such as electrical communications, wind turbine blades, locomotives, aircraft aviation, and the like.
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