CN116891667A - Regenerated carbon fiber composite electric heating anti-icing/deicing coating material and preparation method and application thereof - Google Patents
Regenerated carbon fiber composite electric heating anti-icing/deicing coating material and preparation method and application thereof Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
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- Compositions Of Macromolecular Compounds (AREA)
- Paints Or Removers (AREA)
Abstract
The invention relates to a regenerated carbon fiber composite electric heating anti-icing/deicing coating material and a preparation method thereof, comprising the following steps: 1-10 parts of regenerated carbon fiber, 1-10 parts of cellulose, 5-15 parts of adhesive, 0-275 parts of modified conductive filler and 50-350 parts of resin, and coating the prepared coating on an icing protection surface. After solidification, the electrode plate is pasted and connected with a power supply, and then the electric heating deicing/preventing function can be achieved. Compared with the prior art, the invention effectively utilizes the characteristics of clean surface and high conductivity of the regenerated carbon fiber recovered by thermal cracking, adopts the regenerated carbon fiber grading of different sizes, utilizes the auxiliary dispersion of cellulose and adhesive to cooperatively construct a conductive network, effectively solves the problems of low surface energy, disordered morphology and difficult dispersion of the regenerated carbon fiber, realizes the high-value recycling of the waste carbon fiber composite material, and has outstanding economic benefit and ecological benefit.
Description
Technical Field
The invention belongs to the technical field of material recycling, and particularly relates to a regenerated carbon fiber composite electric heating anti-icing/deicing coating material and a preparation method thereof.
Background
In recent years, the specific gravity of clean energy in the energy industry has been increasing. The wind power industry is taken as a recyclable new energy industry, and has important significance for adjusting energy structures, promoting energy production and promoting ecological civilization construction. In regions with rich wind energy resources, such as the western part and the north part of China, the fan blade can be frozen in cold seasons which can reach months. Icing not only can cause extra load fluctuation and structural vibration of the blade, influence the power generation efficiency of the fan blade and damage the fatigue life of the blade, but also can cause ice layer falling off to generate potential threat, so that the icing blade must be timely deiced.
Existing fan blade anti-icing/de-icing techniques fall broadly into three categories: 1) Mechanical deicing, breaking ice by aerodynamic force, and blowing off ice by high-speed airflow. A mechanical deicing device designed as in patent application CN202120056656.0 cleans ice chips by movement of the scraper ring during rotation of the blades. However, the method is low in efficiency, and the surface of the fan blade is damaged to some extent, so that the method is not suitable for large-scale application. 2) The super-hydrophobic coating is anti-icing, and the patent (application number CN 202211049851.6) prepares an oil-water gel coating which has super-hydrophobic and acid-alkali resistance and can adapt to multiple environments. The patent (application number CN 202210908502.9) also provides a preparation method of the fluorocarbon resin/polycaprolactone-based super-hydrophobic coating with self-healing capacity, the self-healing capacity is endowed to the fluorocarbon resin/polycaprolactone-based super-hydrophobic coating, the durability of the coating is enhanced, and the practicability is further improved. However, the coating can only delay icing, is difficult to maintain hydrophobicity for a long time in a severe environment, and does not have a deicing function. Once the icing phenomenon occurs, the anti-icing efficacy of the coating fails, and the anti-icing/deicing reliability is insufficient; 3) Electrothermal ice protection/removal. For example, patent (application number CN 202011613218.6) utilizes an in-situ polymerization method to prepare the carbon nanotube heating film, so that the carbon nanotube heating film has good heat resistance and is not easy to age. But the heating film preparation and application construction processes are complex, which is not beneficial to practical popularization and application. Patent (application number CN 201720581884.3) proposes a control device for an ice-preventing heating film and a heating film, which comprises a sealing layer and a conductive heating layer, and effectively prevents ice formation and removes ice rapidly by utilizing the protection, heat preservation and insulation functions of the sealing layer on the heating layer. But the heating film system has the advantages of more layers, more interfaces, lower energy utilization rate, more complex manufacturing process and higher cost. The patent (application number CN202110687103. X) proposes a method for preventing and removing ice by using a composite coating of a fan blade, wherein a heating coating is arranged inside the blade, an anti-icing coating is arranged outside the blade, and the advantages of an electrothermal coating and the anti-icing coating are coordinated. However, in the scheme, the electric heating layer is positioned in the blade, heat can be conducted to the surface only through a plurality of interfaces, and the thermal resistance of the interfaces can have a significant effect on the thermal efficiency; meanwhile, the electrothermal layer and the anti-icing layer of the scheme cannot be integrally formed, and the application difficulty and cost are increased.
Disclosure of Invention
The invention aims to provide a regenerated carbon fiber composite electric heating anti-icing/deicing coating material and a preparation method thereof, which provide a competitive scheme for fan anti-icing/deicing and promote green recovery and recycling of the composite material.
The aim of the invention can be achieved by the following technical scheme: the regenerated carbon fiber composite electric heating anti-icing/deicing coating material comprises the following raw materials in parts by weight:
the raw materials preferably comprise the following components in parts by weight:
further, the regenerated carbon fiber is obtained by thermal cracking, recycling, chopping and grinding of the waste carbon fiber composite material, and the diameter of the regenerated carbon fiber is 1-100 mu m, and the length of the regenerated carbon fiber is 0.1-7 cm.
Preferably, the regenerated carbon fibers are divided into three groups according to the size, wherein the size of the group A is 0.1-2cm, the size of the group B is 2-5cm, the size of the group C is 5-7cm, and the weight ratio A of the regenerated carbon fibers with the three sizes is as follows: b: c=1-3: 2-5: 1-4. And forming a passage with excellent conductive characteristics and mechanical strength by utilizing the mutual lap joint and pinning effect between the regenerated carbon fiber gradations, and regulating and controlling the proportion of the regenerated carbon fibers with different sizes, so that the microstructure of the conductive network can be regulated and controlled.
The regenerated carbon fiber is used as a conductive functional body and is directly mixed with resin used as a film forming substance to prepare conductive paint, cellulose is added during preparation, the agglomeration phenomenon of the regenerated carbon fiber is improved, the dispersibility of the regenerated carbon fiber in a resin matrix is increased, and in addition, an adhesive is added to assist in forming a three-dimensional conductive network.
Besides self grading of the regenerated carbon fiber, the regenerated carbon fiber can be matched with other conductive fillers, such as conductive carbon black/graphite/carbon nano tube modified by a silane coupling agent, and the conductivity of the regenerated carbon fiber can be regulated and controlled to meet the resistivity and power requirements in different application scenes. And placing the modified regenerated carbon fiber and the conductive filler in a resin system, and obtaining the electric heating anti-icing/deicing coating based on the regenerated carbon fiber through blending and stirring and curing at normal temperature, thereby realizing the application of the regenerated carbon fiber in the electric heating coating.
Specifically, the modified conductive filler comprises the following components in parts by weight:
the modified conductive filler is prepared by the following method: and (2) placing 1-10 parts of conductive filler in a blending system of 100-200 parts of absolute ethyl alcohol, 10-50 parts of deionized water and 0.5-5 parts of silane coupling agent, mixing and stirring for 6-12 hours, filtering and drying to obtain the modified conductive filler.
Wherein the conductive filler is one or more of conductive carbon black with the diameter of 15-35nm, multi-wall carbon nano tubes with the diameter and the length of about 5-20nm and 1-10mm respectively, and graphite with the diameter of less than 0.1 mm.
Further, the cellulose is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose or salts thereof;
the adhesive is one or more of dopamine hydrochloride and polypyrrole;
the silane coupling agent is one or more of gamma-aminopropyl triethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane gamma and (methacryloyloxy) propyl trimethoxysilane.
The resin is one or more of acrylic resin, fluorine resin, organic silicon resin, polyurethane and epoxy resin.
The invention also provides a preparation method of the regenerated carbon fiber composite electric heating anti-icing/deicing coating material, which comprises the following steps:
1) And (3) regulating and controlling regenerated carbon fibers: 1-10 parts of regenerated carbon fiber with the length of about 0.1-7cm, 1-10 parts of cellulose and 5-15 parts of adhesive are weighed according to the proportions of the regenerated carbon fibers with different A/B/C sizes, and are mixed in a deionized water system, and stirred for 12-24 hours. And filtering and drying (the drying temperature is 70-90 ℃ and the treatment is 8-10 h) to obtain the modified regenerated carbon fiber.
2) 50-350 parts of resin and the regenerated carbon fiber and/or 0-275 parts of modified conductive filler are mixed and stirred, and cured at normal temperature to obtain the regenerated carbon fiber composite electrothermal anti-icing/deicing coating material. When the material is applied, the material is coated on the icing protection surface and is connected with a power supply, so that the electric heating deicing/preventing function can be realized.
Compared with the prior art, the preparation method of the regenerated carbon fiber composite electric heating anti-icing/deicing coating provided by the invention effectively utilizes clean bright spots on the surface of the regenerated carbon fiber recovered by thermal cracking, and exerts excellent electric conductivity. The regenerated carbon fiber grading is used to form three-in-one passage with excellent conducting characteristic including large skeleton frame, fine skeleton and skeleton stuffing. The coating has low price, simple preparation process, good wear resistance and flexibility of resin, environment-friendly matched solvent and reasonable curing time. When the material is applied, the material is coated on the icing protection surface and can be integrally formed, and then the material is connected with a power supply, so that the material has an electrothermal anti-icing/deicing function, is simple to operate, is expected to realize industrialization in the future, greatly reduces the application cost of the regenerated carbon fiber/resin composite material in the field of anti-icing/deicing coatings of fan blades, aircraft blades and the like, and promotes the development of the regenerated carbon fiber composite material recovery industry. In addition, the invention realizes the high-value recycling of the waste carbon fiber composite material and has outstanding economic benefit and ecological benefit.
Compared with the prior art, the invention has the beneficial effects that:
1) The regenerated carbon fiber which is obtained by thermal cracking recovery and has high conductivity, clean surface and good mechanical property is used as a main conductive functional body to prepare the fan blade anti-icing/deicing coating material. The regenerated carbon fibers with different sizes are graded to form a three-in-one passage with excellent electrothermal characteristics of a large skeleton frame, a fine skeleton and a skeleton filler. The deicing device is applied to deicing of the fan blade, has obvious functions, is simple and convenient to apply and low in cost, and does not damage the whole structure and functions of the fan blade.
2) The invention effectively utilizes the characteristics of clean surface and high conductivity of the regenerated carbon fiber recovered by thermal cracking, adopts the grading of the regenerated carbon fiber with different sizes, utilizes the auxiliary dispersion of cellulose and adhesive to cooperatively construct a conductive network, effectively solves the problems of low surface energy, messy morphology and difficult dispersion of the regenerated carbon fiber, realizes the high-value recycling of the waste carbon fiber composite material, has outstanding economic benefit and ecological benefit, and can promote the recycling of the carbon fiber composite material with high-value green.
Drawings
FIG. 1 regenerated carbon fiber a) group A, B) group B, C) group C;
FIG. 2 regenerated carbon fiber scanning electron microscope picture (x5.00k);
FIG. 3 is a cross-sectional view of a regenerated carbon fiber resin-based composite material;
FIG. 4 is a sample of a regenerated carbon fiber composite electrothermal anti-icing/deicing coating material test.
Detailed Description
The invention is further described below in connection with specific embodiments.
The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit of the invention.
The invention provides a regenerated carbon fiber composite electric heating anti-icing/deicing coating material and a preparation method thereof. And preparing the electrothermal anti-icing/deicing coating by using the regenerated carbon fiber prepared by thermal cracking as a functional phase. In the thermal cracking process of the resin matrix of the composite material, the original performance, especially the conductivity, of the carbon fiber can be kept high by controlling the cracking atmosphere and the temperature (J. Composit. Mater.,52 (8) (2018), pp. 1033-1043). Meanwhile, the regenerated carbon fiber is removed with the surface sizing agent, so that the surface resistivity is further reduced, and the regenerated carbon fiber is suitable for being used as a conductive functional phase. The regenerated carbon fibers with different sizes are graded to form a three-in-one functional network of a large framework, a fine framework and framework filler, and the conductivity and mechanical property of the functional network are improved by utilizing the grading lap joint and pinning effects of different functional bodies. The invention not only can provide a scheme with remarkable characteristics and competitiveness for deicing the wind power blade, but also can promote green recovery and high-value recycling of the composite material.
The preparation method of the electrothermal anti-icing/deicing coating based on the regenerated carbon fiber comprises the following steps:
1) And (3) regulating and controlling regenerated carbon fibers: according to the different size ratios of the three regenerated carbon fibers A/B/C, 1-10 parts of regenerated carbon fibers with the length of about 0.1-7cm are weighed, mixed with 1-10 parts of nanocellulose and 5-15 parts of adhesive in a deionized water system, and stirred for 12-24 hours. And filtering and drying the product to obtain the modified regenerated carbon fiber.
In addition to the use of the modified recycled carbon fiber alone, it may also be used in combination with a conductive filler. Placing 1-10 parts of conductive filler in a blending system of 100-200 parts of absolute ethyl alcohol, 10-50 parts of deionized water and 0.5-5 parts of silane coupling agent, and stirring for 6-12 hours. And filtering and drying the product to obtain the modified conductive filler.
2) And (3) blending and stirring 50-350 parts of resin and the regenerated carbon fiber and/or the conductive filler, adding a curing agent, and curing at normal temperature to obtain the regenerated carbon fiber composite electric heating anti-icing/deicing coating material. When the material is applied, the material is coated on the icing protection surface and is connected with a power supply, so that the electric heating deicing/preventing function can be realized.
The technical principle of the invention is as follows:
the regenerated carbon fiber of one of the raw materials adopted by the invention is derived from thermal cracking recovery, and is specifically prepared by a large-scale novel cracking recovery technology (CN 201310595080.5, shanghai university of transportation, 26 days of 3 months of 2014) developed by Shanghai university of transportation, wherein the cracking recovery technology is a relatively mature recovery technology at present in China: placing the waste composite material in a nitrogen atmosphere with the temperature of 400-650 ℃ and the oxygen volume fraction of 3-20%, and enabling the resin to be heated to decompose and gasify, thus realizing recovery of carbon fibers and other materials. The regenerated carbon fiber used in the specific example was recovered by thermal cracking in a nitrogen atmosphere having an oxygen volume fraction of 5% at 450℃and a diameter of 50. Mu.m. The regenerated carbon fiber obtained by the method has high conductivity and clean surface. The thermal cracking atmosphere has little graphitization damage to the carbon fiber, and the reducing gas in the pyrolysis gas has high retention rate of mechanical properties for repairing the microdefect on the surface of the carbon fiber; compared with the original carbon fiber coated with the sizing agent on the surface, the regenerated carbon fiber has clean surface and improved heat conduction and electric conduction performance. And cutting the recycled regenerated carbon fibers by using a splitting machine to obtain the regenerated carbon fibers with different sizes.
The invention divides the regenerated carbon fiber into three groups according to the size, wherein the size of the group A is 0.1-2cm, the size of the group B is 2-5cm, the size of the group C is 5-7cm, as shown in figure 1, the regenerated carbon fiber with the three sizes is graded according to a certain proportion (as A: B: C=1-3: 2-5: 1-4).
The invention adopts cellulose and adhesive to carry out surface treatment on the regenerated carbon fiber. Most of regenerated carbon fibers are friable fabrics or scattered filaments with folds, so that the surface energy is low, and the regenerated carbon fibers are difficult to directly apply. When the regenerated carbon fiber is added into the cellulose solution, cellulose molecules can be coated on the surface of the regenerated carbon fiber, and the surface of the regenerated carbon fiber is saturated and adsorbed by the cellulose molecules along with continuous movement of the cellulose molecules to form a layer of dispersant cellulose protective film, and the regenerated carbon fiber is dispersed by steric hindrance to form a uniformly dispersed regenerated carbon fiber suspension. The dispersibility of the regenerated carbon fiber in the resin system can be improved by the aid of cellulose, and agglomeration is reduced. In addition, in order to strengthen the three-dimensional conductive network formed by mixing the regenerated carbon fibers in the resin matrix, a binder is added for auxiliary molding. The common adhesive such as polydopamine has broad-spectrum adhesiveness, and can be adhered to the surface of almost any substance to form a uniform nano film. The hydroxyl is connected with the regenerated carbon fiber, and the hydroxyl reacts with groups such as isocyanate groups, epoxy groups and the like in the resin, so that the activity and the solubility of the regenerated carbon fiber in the resin can be enhanced, and the formation of the regenerated carbon fiber three-dimensional conductive path is assisted.
The invention utilizes the silane coupling agent to modify the conductive filler. The conductive filler is present in an aggregate state in many cases, and is easily self-polymerized in the material. The conductive filler selected by the invention is one or more of conductive carbon black with the diameter of 15-35nm, multi-wall carbon nano tubes with the diameter and the length of about 5-20nm and 1-10mm respectively, and graphite with the diameter of less than 0.1 mm. The silane coupling agent can reduce the number of polar functional groups on the surface of the conductive filler, introduce propylamine groups to effectively combine with the resin, increase the compatibility and dispersibility with the resin, and further enhance the mechanical properties of the matrix by crosslinking with the resin polymer.
Dispersing the regulated regenerated carbon fiber and/or conductive filler into a resin system, and stirring to uniformly mix the regenerated carbon fiber and/or conductive filler. Pouring the mixed paint into a polytetrafluoroethylene mould, and adding a curing agent according to the requirement. And when the resin is solidified, the resin is subjected to a crosslinking reaction, and the regenerated carbon fiber and the conductive filler are connected in the resin to construct a conductive path.
The various raw materials adopted by the invention are all commercial products unless specified.
The following are more detailed embodiments, by which the technical solutions of the invention and the technical effects that can be obtained are further illustrated.
Example 1
1) And (3) regulating and controlling regenerated carbon fibers: firstly, placing 5kg of hydroxyethyl cellulose into a proper amount of deionized water solution, carrying out ultrasonic treatment for 30min, and then adding 1kgA group, 3kgB group and 1kgC group of mixed regenerated carbon fibers, wherein the macroscopic morphology of the regenerated carbon fibers is shown in figure 1 and is in a black thread shape; the microscopic morphology is shown in a scanning electron microscope as shown in fig. 2, is cylindrical, has a diameter of about 50 microns, and has a cleaner and smoother surface. 10kg of dopamine hydrochloride is added and stirred for 12 hours. And then placing the modified carbon fiber dispersion liquid into a suction filtration device containing a polytetrafluoroethylene filter membrane, carrying out vacuum suction filtration for 10min, washing with deionized water for 3 times, taking down a regenerated carbon fiber layer on the polytetrafluoroethylene filter membrane, and drying in an oven at 80 ℃ for 6h to obtain the modified regenerated carbon fiber.
2) Preparation of electrothermal anti-icing/deicing coating based on regenerated carbon fiber: after modifying 5kg of the regenerated carbon fiber in the step 1), adding 300kg of epoxy resin, stirring for 60min, and curing for a corresponding time at a resin calibration temperature to obtain the regenerated carbon fiber/epoxy resin-based electrothermal anti-icing coating, wherein a section view of the regenerated carbon fiber resin-based composite material is shown as a figure 3, and it can be seen from the figure that voids left on the resin after the regenerated carbon fiber is pulled out are fewer, a small amount of resin is left on the pulled-out carbon fiber, the gaps between the fiber and the resin are reduced, and the interface combination between the regenerated carbon fiber and the resin is improved.
3) The obtained material is coated on the icing protection surface and is connected with a power supply, so that the electric heating anti-icing/deicing function can be realized, the obtained electric heating anti-icing/deicing coating based on the regenerated carbon fiber is shown as a figure 4, and the graph shows that the surface of the anti-icing coating is smooth, no obvious protrusions exist, and the uniform heating deicing is realized.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
Example 2
1) And (3) regulating and controlling regenerated carbon fibers: firstly, 5kg of hydroxyethyl cellulose is placed in a proper amount of deionized water solution, after ultrasonic treatment is carried out for 30min, 3kgA groups, 3kgB groups and 4kgC groups of mixed regenerated carbon fibers are added, and then 5kg of dopamine hydrochloride is added and stirred for 12h. And then placing the modified carbon fiber dispersion liquid into a suction filtration device containing a polytetrafluoroethylene filter membrane, carrying out vacuum suction filtration for 10min, washing with deionized water for 3 times, taking down a regenerated carbon fiber layer on the polytetrafluoroethylene filter membrane, and drying in an oven at 80 ℃ for 6h to obtain the modified regenerated carbon fiber.
2) Preparation of electrothermal anti-icing/deicing coating based on regenerated carbon fiber: 5kg of conductive carbon black was weighed, 100kg of an absolute ethanol solution was mixed with 25kg of deionized water, and then 5kg of a silane coupling agent was dropwise added thereto, followed by stirring for 6 hours. And then placing the modified conductive filler dispersion liquid into a suction filtration device containing a polytetrafluoroethylene filter membrane, carrying out vacuum suction filtration for 10min, washing 3 times by deionized water and absolute ethyl alcohol respectively, scraping off a conductive filler layer on the polytetrafluoroethylene filter membrane, and drying in an oven at 80 ℃ for 6h to obtain the modified conductive filler.
3) And (2) after modifying 10kg of regenerated carbon fiber in the step (1), adding 95kg of polyurethane, stirring for 30min, adding the modified conductive filler obtained in the step (2), continuously stirring for 30min, and curing for a corresponding time at the resin calibration temperature to obtain the regenerated carbon fiber/polyurethane-based electrothermal anti-icing/deicing coating.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
Example 3
1) And (3) regulating and controlling regenerated carbon fibers: firstly, 5kg of hydroxyethyl cellulose is placed in a proper amount of deionized water solution, after ultrasonic treatment is carried out for 20min, 2kgA groups, 5kgB groups and 3kgC groups of mixed regenerated carbon fibers are added, and then 10kg of dopamine hydrochloride is added for stirring for 12h. And then placing the modified carbon fiber dispersion liquid into a suction filtration device containing a polytetrafluoroethylene filter membrane, carrying out vacuum suction filtration for 10min, washing with deionized water for 3 times, taking down a regenerated carbon fiber layer on the polytetrafluoroethylene filter membrane, and drying in an oven at 80 ℃ for 6h to obtain the modified regenerated carbon fiber.
2) Preparation of electrothermal anti-icing/deicing coating based on regenerated carbon fiber: and (3) after modifying 10kg of the regenerated carbon fiber in the step (1), adding 100kg of epoxy resin and 150kg of polyurethane, stirring for 60min, and curing for a corresponding time at a resin calibration temperature to obtain the electric heating anti-icing/deicing coating based on the regenerated carbon fiber.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
Example 4
1) And (3) regulating and controlling regenerated carbon fibers: firstly, placing 6kg of hydroxyethyl cellulose into a proper amount of deionized water solution, carrying out ultrasonic treatment for 60min, adding 3kgA groups, 2kgB groups and 3kgC groups of mixed regenerated carbon fibers, and then adding 8kg of dopamine hydrochloride and stirring for 24h. And then placing the modified carbon fiber dispersion liquid into a suction filtration device containing a polytetrafluoroethylene filter membrane, carrying out vacuum suction filtration for 20min, washing for 5 times by using deionized water, then taking down a regenerated carbon fiber layer on the polytetrafluoroethylene filter membrane, and drying in an oven at 80 ℃ for 8h to obtain the modified regenerated carbon fiber.
2) Preparation of electrothermal anti-icing/deicing coating based on regenerated carbon fiber: and (3) after 8kg of the regenerated carbon fiber obtained in the step (1) is modified, 170kg of epoxy resin is added, stirring is carried out for 60min, and the regenerated carbon fiber/epoxy resin-based electric heating anti-icing coating is obtained after curing for a corresponding time at the resin calibration temperature.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
Comparative example 1
The three different size mixed regenerated carbon fibers of example 4 were changed to only group a of them, i.e., 8kgA groups of regenerated carbon fibers were used, and the rest was the same as in example 4.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
Comparative example 2
The procedure of example 4 was followed except that the three different size blends of regenerated carbon fibers of example 4 were changed to only group B carbon fibers, i.e., group 8kgB regenerated carbon fibers were used.
Comparative example 3
The procedure of example 4 was followed except that the three different size blends of recycled carbon fibers of example 4 were changed to only group C carbon fibers, i.e., group 8kgC recycled carbon fibers were used.
Comparative example 4
The procedure of example 4 was repeated except that the regenerated carbon fibers of the three different sizes were used instead of only 5 of the regenerated carbon fibers kgA and 3 of the regenerated carbon fibers kgB.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
Comparative example 5
The procedure of example 4 was repeated except that the regenerated carbon fibers of the three different sizes were used instead of only 5 of the regenerated carbon fibers kgA and 3 of the regenerated carbon fibers kgC.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
Comparative example 6
The procedure of example 4 was repeated except that the regenerated carbon fibers of the three different sizes were used instead of only 5 of the regenerated carbon fibers kgB and 3 of the regenerated carbon fibers kgC.
The thickness of the electrothermal anti-icing/deicing coatings based on regenerated carbon fibers prepared in examples 1 to 4 and comparative examples 1 to 6 was controlled to be 1 to 5mm, and the thermal stability, temperature uniformity, electrothermal stability and electrothermal conversion efficiency thereof were investigated. The effects of the examples were tested in connection with the specific test methods as follows:
1. the test voltage was 36V and the test coating samples were sized 5cm by 10cm by 5 mm.
2. The coating was placed in an environment of-15 ℃, water droplets were dropped onto the surface of the coating, and the change in the state of the water droplets was recorded with a camera. When the water drop is changed from transparent to completely opaque, the water drop is completely frozen, and the delay icing time is recorded.
3. And (3) placing the coating in an environment of minus 30 ℃, dripping water drops on the surface of the coating, electrifying and heating the coating when the water drops are completely frozen at a certain rated power, and recording the melting time of the ice drops when the ice drops are completely opaque and transparent.
4. The coating is placed in an environment with the room temperature of 15 ℃ for being electrified and heated, and when the temperature of the coating tends to be stable, the highest temperature which can be reached by the coating is recorded.
The properties of the obtained regenerated carbon fiber composite electric heating anti-icing/deicing coating material are shown in table 1.
TABLE 1
Test item | Delay icing time/s | Time/s for melting ice beads | Maximum temperature/. Degree.C |
Example 1 | 600 | 14 | 83 |
Example 2 | 834 | 10 | 94 |
Example 3 | 725 | 12 | 89 |
Example 4 | 573 | 18 | 81 |
Comparative example 1 | 452 | 37 | 57 |
Comparative example 2 | 376 | 45 | 55 |
Comparative example 3 | 483 | 31 | 61 |
Comparative example 4 | 521 | 25 | 65 |
Comparative example 5 | 538 | 21 | 75 |
Comparative example 6 | 519 | 22 | 72 |
As can be seen from table 1, compared with comparative examples 1 to 6 (single-size or two-size regenerated carbon fiber gradations), the electric heating anti-icing/deicing coatings based on the regenerated carbon fibers prepared in examples 1 to 4 (three-size regenerated carbon fiber gradations) have better electric heating performance, can remarkably delay icing, has a stable highest temperature after the coating is electrified far greater than an icing point, can effectively prevent icing and deicing, and are suitable for being applied to the field of electric heating protection of fan blade coatings.
In the embodiment 2, the modified conductive filler is added on the basis of the modified regenerated carbon fiber, the construction of a regenerated carbon fiber conductive path is further assisted, and the obtained electrothermal ice prevention and removal coating has longer icing delay time, shorter ice bead melting time, highest temperature of over 90 ℃ when the temperature rises to a stable state, and excellent electrothermal performance and ice prevention and removal effect.
The raw materials and equipment used in the present invention are common raw materials and equipment in the art unless otherwise specified;
the experimental methods used in the present invention are conventional methods in the art unless otherwise specified. The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the simple modification, variation and equivalent transformation of the above embodiment according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (10)
1. The regenerated carbon fiber composite electric heating anti-icing/deicing coating material is characterized by comprising the following raw materials in parts by weight:
2. a regenerated carbon fiber composite electrothermal ice protection/deicing coating material according to claim 1, wherein: the raw materials comprise the following components in parts by weight:
3. a regenerated carbon fiber composite electrothermal ice protection/deicing coating material according to claim 1, wherein: the regenerated carbon fiber is obtained by thermal cracking, recycling, chopping and grinding of the waste carbon fiber composite material, and has the diameter of 1-100 mu m and the length of 0.1-7 cm.
4. A regenerated carbon fiber composite electrothermal ice protection/removal coating material according to claim 1 or 3, wherein: the regenerated carbon fibers are divided into three groups according to the size, wherein the size of the group A is 0.1-2cm, the size of the group B is 2-5cm, the size of the group C is 5-7cm, and the weight ratio A of the regenerated carbon fibers with the three sizes is as follows: b: c=1-3: 2-5: 1-4.
5. A regenerated carbon fiber composite electrothermal ice protection/deicing coating material according to claim 1, wherein: the modified conductive filler comprises the following components in parts by weight:
6. a regenerated carbon fiber composite electrothermal ice protection/removal coating material according to claim 5, wherein: the modified conductive filler is prepared by the following method: and (2) placing 1-10 parts of conductive filler in a blending system of 100-200 parts of absolute ethyl alcohol, 10-50 parts of deionized water and 0.5-5 parts of silane coupling agent, mixing and stirring for 6-12 hours, filtering and drying to obtain the modified conductive filler.
7. A regenerated carbon fiber composite electrothermal ice protection/deicing coating material according to claim 1, wherein: the cellulose is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose or salts thereof;
the adhesive is one or more of dopamine hydrochloride and polypyrrole;
the silane coupling agent is one or more of gamma-aminopropyl triethoxysilane, gamma- (2, 3-epoxypropoxy) propyl trimethoxysilane gamma and (methacryloyloxy) propyl trimethoxysilane;
the resin is one or more of acrylic resin, fluorine resin, organic silicon resin, polyurethane and epoxy resin.
8. The method for preparing the regenerated carbon fiber composite electric heating anti-icing/deicing coating material according to claim 1, wherein the regenerated carbon fiber composite electric heating anti-icing/deicing coating material is prepared by the following method:
1) And (3) regulating and controlling regenerated carbon fibers: weighing 1-10 parts of regenerated carbon fiber with the length of 0.1-7cm, blending the regenerated carbon fiber with 1-10 parts of cellulose and 5-15 parts of adhesive in a deionized water system, stirring for 12-24 hours, filtering and drying to obtain modified regenerated carbon fiber;
2) And (2) blending and stirring 50-350 parts of resin, 0-275 parts of modified regenerated carbon fiber obtained in the step (1) and modified conductive filler, and curing at normal temperature to obtain the regenerated carbon fiber composite electric heating anti-icing/deicing coating material.
9. The method for preparing the regenerated carbon fiber composite electric heating anti-icing/deicing coating material according to claim 8, wherein the drying temperature in step 1) is 70-90 ℃, and the drying treatment is performed for 8-10 hours;
and in the step 2), the drying temperature is 70-90 ℃, and the drying treatment is carried out for 8-10 hours.
10. The application of the regenerated carbon fiber composite electric heating anti-icing/deicing coating material according to claim 8, wherein the regenerated carbon fiber composite electric heating anti-icing/deicing coating material is coated on an icing protection surface and is connected with a power supply, so that the regenerated carbon fiber composite electric heating anti-icing/deicing coating material has an electric heating anti-icing/deicing function.
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