An insulating high-thermal-conductivity anti-icing coating material for wind power blades and a preparation method thereof

Abstract

The application discloses an insulating high-thermal-conductivity anti-icing coating for a wind power blade and a preparation method thereof, and belongs to the technical field of wind power generation. The main material of the coating is hydrated salt / SiC composite phase change filler micro powder and polyurethane prepolymer. The hydrated salt / SiC composite phase change filler micro powder is composed of eutectic hydrated salt and silicon carbide. The eutectic hydrated salt selects dipotassium hydrogen phosphate hexahydrate as a phase change matrix, dipotassium hydrogen phosphate dodecahydrate as a nucleating agent, and silicon carbide as a thermal conductor and a supporting material. The coating has excellent heat absorption and storage performance and thermal conductivity, can prevent the wind power blade from icing, and can also prevent lightning strikes.

Description

Technical Field

[0001] This invention belongs to the field of wind power generation technology, specifically relating to an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades and its preparation method. Background Technology

[0002] Wind power is a clean and renewable energy source, with the wind turbine as its core equipment. A wind turbine mainly consists of a tower, blades, a generator, and a control system. Among these, the blades are one of the most critical components, their design and material selection directly affecting the turbine's performance and lifespan. However, wind turbines are typically located in mountainous or border regions where there are significant diurnal temperature variations, making them prone to freezing. These areas often experience extreme weather events such as thunderstorms. During the day, these regions have ample sunlight and relatively high temperatures, but at night, temperatures drop below freezing, making the blade surfaces of wind turbines extremely susceptible to icing. Icing not only affects the aerodynamic performance of the blades and reduces the turbine's power generation efficiency, but in severely iced areas, it can cause a power generation loss of approximately 20% to 50%. Furthermore, lightning strikes can damage the blades, affecting the normal operation of the wind turbine and potentially leading to serious safety accidents.

[0003] Therefore, how to reduce the impact of large temperature variations during service on the blades, while preventing damage to the blades from lightning and ultraviolet light, and improving the safety of wind turbines, is an urgent problem to be solved in the field of wind power generation technology. Summary of the Invention

[0004] The purpose of this invention is to overcome the shortcomings of the prior art and provide an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades and its preparation method, so as to solve the problem that wind turbine blades are subject to large temperature variations and damage from lightning and ultraviolet light during service.

[0005] To achieve the above objectives, the present invention employs the following technical solution:

[0006] A method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades includes the following steps:

[0007] Step 1: Mix dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate, and heat in a water bath until a transparent liquid is obtained to obtain a eutectic hydrated salt;

[0008] Step 2: Add silicon carbide to the eutectic hydrated salt, add aluminum dihydrogen phosphate after mechanical stirring to obtain process mixture A, dry process mixture A and sinter it, and ball mill the sintered product to obtain hydrated salt / SiC composite phase change filler.

[0009] Step 3: Weigh the polyurethane base material, which includes diisocyanate, polyether glycol, hydrophilic chain extender, catalyst, neutralizer, post-chain extender and solvent.

[0010] Step 4: Prepare polyurethane prepolymer by using diisocyanate, polyether glycol, hydrophilic chain extender, catalyst and neutralizer in polyurethane base material;

[0011] Step 5: Mix the hydrated salt / SiC composite phase change filler and silane coupling agent KH550, add toluene, react in an oil bath, and then vacuum filter the reaction product. Mix the vacuum filtered product with water and then sonicate it. The sonicated product is then vacuum filtered. The vacuum filtered product is washed with N,N-dimethylformamide and then dried to obtain the modified hydrated salt / SiC composite phase change filler micro powder.

[0012] Step 6: Mix the modified hydrated salt / SiC composite phase change filler micro powder, polyurethane prepolymer, post-chain extender and solvent, and stir to obtain an insulating, high thermal conductivity and anti-icing coating.

[0013] A further improvement of the present invention is that:

[0014] Preferably, in step 1, the mixing mass ratio of dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate is 176.67:13.86, and the water bath heating temperature is 55°C.

[0015] Preferably, in step 2, the amount of silicon carbide added is 50% to 80% of the mass of the eutectic hydrate salt;

[0016] The amount of aluminum dihydrogen phosphate added is 3 to 4.5% of the mass of the mixture of eutectic hydrate salt and silicon carbide.

[0017] Preferably, in step 2, the drying temperature is 120°C and the drying time is 4 to 6 hours.

[0018] Preferably, the sintering process in step 2 is as follows: heating at 25-50℃ for 40 min and holding for 20 min; heating at 50-75℃ for 40 min and holding for 20 min; heating at 75-100℃ for 30 min and holding for 30 min; and holding at 100℃ for 1 h.

[0019] Preferably, in step 3, the polyurethane base material comprises, by mass fraction, 20-25% diisocyanate, 15-20% polyether glycol, 2.5-7.5% post-chain extender, 1-2% hydrophilic chain extender, 1-3.5% catalyst, 0.5-2% neutralizer, and 50% solvent.

[0020] Preferably, in step 4, the preparation process of the polyurethane prepolymer is as follows:

[0021] (1) Dry the polyether glycol at 110°C for 5 hours;

[0022] (2) Place the dried polyether glycol in a three-necked round-bottom flask, introduce nitrogen gas into the flask, and stir;

[0023] (3) Add the catalyst and diisocyanate to the flask in step (2) and stir;

[0024] (4) Add the hydrophilic chain extender to the flask in step (3), stir the reaction, and obtain the reaction product;

[0025] (5) Cool the reaction product of step (4) to 50°C, add a neutralizing agent to carry out a neutralization reaction, and obtain polyurethane prepolymer.

[0026] Preferably, in step 5, the molar ratio of hydrated salt / SiC composite phase change filler to silane coupling agent KH550 is 25:1, the oil bath reaction temperature is 90℃, and the oil bath reaction time is 6h.

[0027] Preferably, in step 5, the amount of hydrated salt / SiC composite phase change filler powder added is 30-60% of the polyurethane prepolymer.

[0028] An insulating, high thermal conductivity, and anti-icing coating prepared by any of the above methods comprises hydrated salt / SiC composite phase change filler micropowder and polyurethane prepolymer. The hydrated salt / SiC composite phase change filler micropowder is composed of eutectic hydrated salt and silicon carbide. The eutectic hydrated salt is composed of dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate.

[0029] Compared with the prior art, the present invention has the following beneficial effects:

[0030] This invention discloses a method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades. This method selects hydrated salts as the phase change component, which can undergo a phase change under temperature variations, thereby absorbing or releasing a large amount of latent heat. It possesses advantages such as high phase change enthalpy, high energy storage density, high thermal conductivity, and low cost, improving the heat storage performance of the coating and more effectively absorbing and storing daytime solar heat within the coating, preventing wind turbine blades from icing and causing damage after nighttime temperature drops. Simultaneously, the selection of this material should consider its impact on blade performance and weight to ensure that it does not affect blade performance and weight, thereby improving the efficiency of the wind turbine unit. Silicon carbide is used as a thermal conductive agent and supporting material, featuring high thermal conductivity, electrical insulation, and low cost. Silicon carbide has a thermal conductivity greater than 300 W / mK and a resistivity of 10⁵–10¹² Ω·cm at room temperature. It is not easily conductive, classifying it as an insulating material. Furthermore, it does not chemically react with hydrated salts, exhibiting some corrosion resistance. Its melting or decomposition temperature is higher than that of the phase change component, ensuring the shape stability and processability of the phase change component, guaranteeing the adhesion and reliability of the coating, and allowing the entire coating to maintain good heat absorption and release effects even in harsh environments. Using a silane coupling agent as a binder, it can undergo a covalent reaction with the surface of silicon carbide under certain conditions to form covalent bonds, thus firmly existing on the surface of the inorganic material. The amino groups on the other side can also undergo a covalent reaction with the polymer matrix, enhancing the bond between the supporting material and the polymer matrix, thereby improving the overall thermal conductivity of the coating. This invention optimizes the formulation of the thermal storage coating to reduce its manufacturing cost. This can be achieved by selecting lower-priced raw materials, simplifying the production process, and improving production efficiency. Simultaneously, it improves the safety and reliability of wind turbine units.

[0031] The second aspect of this invention discloses an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades. This coating possesses excellent heat absorption and storage properties, effectively absorbing and storing solar heat within the coating layer. This prevents the blades from being scorched by strong sunlight during the day, and simultaneously prevents icing of the wind turbine blades after the temperature drops at night, thus more effectively protecting the blades from damage and improving the safety of the wind turbine unit. The coating also has high thermal conductivity, allowing the stored heat to be quickly released to the blade surface when the temperature drops at night, ensuring the blade's thermal stability and preventing icing. Furthermore, the coating is uniform and stable in texture, without agglomeration or other issues, and does not increase the weight of the blades, thereby not affecting the efficiency of the wind turbine unit. The heat storage coating of this invention is lighter and more suitable for use on wind turbine blades. The coating has a lower heat storage cost, which can reduce the cost of blade anti-icing and lightning protection in areas with large diurnal temperature differences, thus improving the economic efficiency of wind power generation. Compared to existing technologies, the heat storage coating of this invention is more economically valuable. The heat storage coating of this invention can also provide additional protective functions, such as corrosion resistance, which can further improve the service life and performance of the blades, and indirectly improve the economic efficiency of wind power generation. Attached Figure Description

[0032] Figure 1 This is a flowchart illustrating the preparation process of the insulating, high thermal conductivity, and anti-icing coating for wind turbine blades according to the present invention. Detailed Implementation

[0033] To enable those skilled in the art to understand the features and effects of the present invention, the terms and expressions used in the specification and claims are explained and defined in general below. Unless otherwise specified, all technical and scientific terms used herein have the ordinary meaning understood by those skilled in the art regarding the present invention, and in case of conflict, the definitions in this specification shall prevail.

[0034] In this article, unless otherwise specified, “contains,” “includes,” “containing,” “has,” or similar terms cover the meanings of “composed of” and “mainly composed of,” for example, “A contains a” covers the meanings of “A contains a and others” and “A contains only a.”

[0035] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0036] The following examples use instruments and equipment conventional in the art. Experimental methods in the following examples, unless otherwise specified, are generally performed under conventional conditions or as recommended by the manufacturer. All raw materials used in the following examples are conventional commercially available products with specifications conventional in the art. In this specification and the following examples, unless otherwise specified, "%" refers to weight percentage, "parts" refers to parts by weight, and "ratio" refers to weight proportion.

[0037] Wind turbine blades operate in harsh environments. Key challenges include: how to utilize solar thermal energy storage materials to improve the anti-icing performance of wind turbine blade coatings, allowing the coating to quickly release heat after nighttime temperature drops, preventing blade surface icing and damage; how to embed high thermal conductivity materials into the composite matrix to improve the coating's thermal conductivity and stability, ensuring anti-icing while protecting the blades from daytime sun damage without affecting performance or weight, thus improving wind turbine efficiency and stability; and how to ensure strong insulation through the addition of silicon carbide without increasing weight, providing lightning protection and improving the economic benefits of wind power generation.

[0038] To address the aforementioned problems, the first aspect of this invention discloses a method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades, the method specifically comprising the following steps:

[0039] Step 1, Preparation of hydrated salt phase change materials

[0040] Dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate were mixed in a beaker at a mass ratio of 176.67:13.86. The mixture was then heated and stirred in a water bath at 55°C until it melted into a transparent liquid, thus obtaining a eutectic hydrated salt.

[0041] Step 2, Preparation of hydrated salt / SiC composite phase change thermal storage material

[0042] (1) Add insulating and thermally conductive silicon carbide filler to the molten eutectic hydrated salt obtained in step 1. After mechanical stirring for 10-15 min, a eutectic hydrated salt / SiC mixture is obtained. The stirring speed is 60-110 r / min, and the silicon carbide particle size is 2-5 μm.

[0043] The mass fraction of silicon carbide is 50% to 80% of the mass of the eutectic hydrate salt.

[0044] (2) The eutectic hydrated salt / SiC mixture after being thoroughly and uniformly mixed is loaded into a crucible, and an appropriate amount of aluminum dihydrogen phosphate binder is added to obtain process mixture A.

[0045] The aluminum dihydrogen phosphate content is 3-4.5% of the mass of the eutectic hydrate salt / SiC mixture. As a binder, aluminum dihydrogen phosphate can bind SiC and eutectic salt particles together.

[0046] (3) Place the process mixture A obtained in step (3) into a crucible, put the crucible into a drying oven at 120°C and dry for 4 to 6 hours. Then close the drying oven and let it cool naturally to room temperature before taking it out to obtain process mixture B.

[0047] (4) Take out the cooled process mixture B, sinter it with a specific heating program, evaporate and remove moisture to obtain process mixture C;

[0048] The heating program is as follows: heating from 0 to 25°C for 40 minutes and holding for 20 minutes; within 40 minutes, heating from 25°C to 50°C and holding at 50°C for 20 minutes; within 40 minutes, heating from 50°C to 75°C and holding at 75°C for 20 minutes; within 30 minutes, heating from 75°C to 100°C and holding at 100°C for 30 minutes; and holding at the highest sintering temperature of 100°C for 1 hour.

[0049] It should be noted that during the heating process described above, if the temperature of process mixture B itself is high after it is removed, there is no need to perform a heating process from 0 to 25°C; the temperature can be increased directly within the subsequent temperature range.

[0050] (5) After the heat preservation process in step (4) is completed, take out the process mixture C in the crucible and put it into a planetary ball mill. Dry grind the mixture at a ball-to-material ratio of 1:1 and a speed of 100r / min until the particle size of the mixture is 10-20μm to obtain the hydrated salt / SiC composite phase change filler.

[0051] Step 3: Weigh the base material of the waterborne polyaspartic acid ester resin.

[0052] The polyurethane prepolymer is composed of a portion of the polyurethane base material, which includes: diisocyanate, polyether glycol, post-chain extender, hydrophilic chain extender, catalyst, neutralizer and solvent.

[0053] Specifically, the diisocyanate is any one or a mixture of isoflurone diisocyanate, hexamethylene diisocyanate, and 4,4'-dicyclohexylmethane diisocyanate, and its mass content is 20-25% of the polyurethane prepolymer.

[0054] Specifically, the polyether glycol is one or a mixture of polytetrahydrofuran glycol (PTMG), polyethylene glycol, and polypropylene glycol, and its mass content is 15-20% of the polyurethane base material.

[0055] Specifically, the chain extender is 1,5-pentanediol, and its mass content is 2.5% to 7.5% of the polyurethane base material.

[0056] Specifically, the hydrophilic chain extender is one or a mixture of two of 2,2-dimethylolpropionic acid and dimethylolbutyric acid, and its mass content is 1 to 2% of the polyurethane base material.

[0057] Specifically, the catalyst is one or more of dibutyltin dilaurate, stannous octoate, and dibutyltin oxide, and its mass content is 1 to 3.5% of the polyurethane base material.

[0058] Specifically, the neutralizing agent is one or more of triethylamine, tripropylamine, formic acid, acetic acid, and triethanolamine, and its mass content is 0.5% to 2% of the polyurethane base material.

[0059] Specifically, the solvent is N,N-dimethylformamide, and its mass content is 50% of the polyurethane base material.

[0060] It should be understood that the polyurethane base material mentioned above is the composition and corresponding material of the final waterborne polyaspartic ester resin. A portion of it is used in the next step to prepare the polyurethane prepolymer, and a portion is added in the final preparation step.

[0061] Step 4: Prepare polyurethane prepolymer

[0062] (1) Weigh the diisocyanate, polyether glycol, post-chain extender, hydrophilic chain extender, catalyst, neutralizer and solvent according to the set mass ratio;

[0063] (2) Dry the weighed polyether glycol at 110°C for 5 hours.

[0064] (3) Take out the dried polyether glycol from step (2) and put it into a three-necked round bottom flask. Pour nitrogen into the flask and start stirring. The stirring conditions are: 350 r / min, 20 min.

[0065] (4) Add the weighed catalyst and diisocyanate to the flask in step (3), and start stirring. The stirring conditions are: 350 r / min, 88℃, 30-60 min.

[0066] (5) Add the weighed hydrophilic chain extender to the flask in step (4), turn on the stirrer, and the stirring conditions are: 350 r / min, 80℃, 2-3 h;

[0067] (6) Cool the reaction product of step (5) to 50°C, add the weighed neutralizing agent to carry out the neutralization reaction for 30 to 40 minutes to obtain polyurethane prepolymer.

[0068] Step 5: Prepare modified hydrated salt / SiC composite phase change filler micro powder

[0069] (1) Add the hydrated salt / SiC composite phase change filler and silane coupling agent KH550 to a three-necked flask at a molar ratio of 25:1, and add toluene as a solvent for the reaction environment.

[0070] Silicon carbide tends to aggregate during composite material processing, necessitating the addition of surface modifiers. These modifiers serve two purposes: firstly, to ensure uniform dispersion of the silicon carbide, and secondly, to act as binders to connect thermally conductive ions to the polymer matrix.

[0071] (2) Place the three-necked flask in a constant temperature oil bath, heat it to 90°C, introduce nitrogen gas and maintain the nitrogen atmosphere, start stirring and react for 6 hours at a stirring speed of 100-150 r / min.

[0072] (3) After the reaction is complete, the mixed solution in (2) is vacuum filtered.

[0073] (4) Pour the vacuum-filtered hydrated salt / SiC composite phase change filler powder into a beaker, add deionized water, and sonicate for 30-60 minutes. After sonication, filter again.

[0074] (5) Add N,N-dimethylformamide to the hydrated salt / SiC composite phase change filler powder after filtration in (4) and wash it twice.

[0075] (6) Place the cleaned hydrated salt / SiC composite phase change filler powder from (5) into a vacuum drying oven; the drying oven needs to be preheated to 105℃ and kept at a constant temperature for 12 hours. The modified hydrated salt / SiC composite phase change filler powder is obtained.

[0076] Step 6: Prepare an insulating, high thermal conductivity, and anti-icing coating.

[0077] (1) Cool the reaction product of step 4 to 35°C and add it to the polyurethane prepolymer at 30-60% of the mass content of the polyurethane prepolymer.

[0078] (2) Add the weighed chain extender and solvent to (7) and start stirring. The stirring conditions are 900-2000 r / min for 30-60 min. Finally, an insulating, high thermal conductivity, and anti-icing coating is obtained.

[0079] The second invention discloses an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades prepared by the above-described method. The main materials of this coating are a hydrated salt / SiC composite phase change filler and a polyurethane prepolymer. The hydrated salt / SiC composite phase change filler is composed of a eutectic hydrated salt and silicon carbide. The eutectic hydrated salt uses dipotassium hydrogen phosphate hexahydrate as the phase change matrix, disodium hydrogen phosphate dodecahydrate as the nucleating agent, and silicon carbide as the thermal conductive agent and supporting material. The polyurethane prepolymer is a water-based polyaspartic acid ester resin. Specifically, dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate are used to prepare the eutectic hydrated salt. The hydrated eutectic salt / SiC phase change filler is prepared using a mixed sintering method. This phase change filler is cross-linked with the water-based polyaspartic acid ester resin using a binder to form a thermal storage coating.

[0080] The following description, in conjunction with specific embodiments, provides further details.

[0081] Example 1

[0082] Step 1, Preparation of hydrated salt phase change materials

[0083] Dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate were mixed in a beaker at a mass ratio of 176.67:13.86, and heated and stirred in a water bath at 55°C until they melted into a transparent liquid to obtain a eutectic hydrated salt.

[0084] Step 2, Preparation of hydrated salt / SiC composite phase change thermal storage material

[0085] (1) Add insulating and thermally conductive silicon carbide filler to the molten eutectic hydrated salt obtained in step 1. After mechanical stirring for 12 min, a eutectic hydrated salt / SiC mixture is obtained. The stirring speed is 80 r / min, and the silicon carbide particle size is 2-5 μm.

[0086] The mass fraction of silicon carbide is 60% of the mass of the eutectic hydrate salt.

[0087] (2) The eutectic hydrated salt / SiC mixture after being thoroughly and uniformly mixed is loaded into a crucible, and an appropriate amount of aluminum dihydrogen phosphate binder is added to obtain process mixture A.

[0088] The aluminum dihydrogen phosphate content is 4% of the mass of the eutectic hydrate salt / SiC mixture.

[0089] (3) Place the process mixture A obtained in step (3) into a crucible, put the crucible into a drying oven at 120°C and dry for 5 hours. Then close the drying oven and let it cool naturally to room temperature before taking it out to obtain process mixture B.

[0090] (4) Take out the cooled process mixture B and sinter it with a specific heating program to obtain process mixture C;

[0091] The heating process is as follows: heat from room temperature to 30°C for 40 minutes and hold for 20 minutes; heat to 60°C for 40 minutes and hold for 20 minutes; heat to 90°C for 30 minutes and hold for 30 minutes; and hold at the highest sintering temperature of 100°C for 1 hour.

[0092] (5) After the heat preservation process in step (4) is completed, take out the process mixture C in the crucible and put it into a planetary ball mill. Dry grind the mixture at a ball-to-material ratio of 1:1 and a speed of 100r / min until the particle size of the mixture is 10-20μm to obtain the hydrated salt / SiC composite phase change filler.

[0093] Step 3, weigh the polyurethane base material

[0094] Specifically, the diisocyanate is isoflurone diisocyanate, and its mass content is 22% of the polyurethane base material;

[0095] Specifically, the polyether diol is polytetrahydrofuran diol, and its mass content is 18% of the polyurethane prepolymer;

[0096] Specifically, the chain extender is 1,5-pentanediol, and its mass content is 5% of the polyurethane prepolymer;

[0097] Specifically, the hydrophilic chain extender is 2,2-dimethylolpropionic acid, and its mass content is 1.5% of the polyurethane prepolymer;

[0098] Specifically, the catalyst is dibutyltin dilaurate, and its mass content is 2% of the polyurethane prepolymer;

[0099] Specifically, the neutralizing agent is a type of triethylamine, and its mass content is 1.5% of the polyurethane prepolymer.

[0100] Specifically, the solvent is N,N-dimethylformamide, and its mass content is 50% of that of the polyurethane prepolymer.

[0101] Step 4: Prepare polyurethane prepolymer

[0102] (1) Weigh the diisocyanate, polyether glycol, post-chain extender, hydrophilic chain extender, catalyst, neutralizer and solvent according to the set mass ratio;

[0103] (2) Dry the weighed polyether glycol at 110°C for 5 hours.

[0104] (3) Take out the dried polyether diol from step (2) and put it into a three-necked round bottom flask. Pour nitrogen into the flask and start stirring. The stirring speed is 350 r / min and the stirring time is 20 min.

[0105] (4) Add the weighed catalyst and diisocyanate to the flask in step (3), start stirring, the stirring speed is 350 r / min, the stirring temperature is 88℃, and the stirring time is 50 min.

[0106] (5) Add the weighed hydrophilic chain extender to the flask in step (4), turn on the stirrer, the stirring speed is 350 r / min, the stirring temperature is 80℃, and the stirring time is 2.5 h.

[0107] (6) Cool the reaction product of step (5) to 50°C, add the weighed neutralizing agent to carry out the neutralization reaction for 35 minutes to obtain polyurethane prepolymer.

[0108] Step 5, Preparation of modified hydrated salt / SiC composite phase change filler micro powder

[0109] (1) Add the hydrated salt / SiC composite phase change filler and silane coupling agent KH550 to a three-necked flask in a ratio of 25:1, and add toluene as a solvent for the reaction environment.

[0110] (2) Place the three-necked flask in a constant temperature oil bath, heat it to 90°C, introduce nitrogen gas and maintain the nitrogen atmosphere, start stirring and react for 6 hours at a stirring speed of 120 r / min.

[0111] (3) After the reaction is complete, the mixed solution in (2) is vacuum filtered.

[0112] (4) After vacuum filtration, pour the hydrated salt / SiC composite phase change filler powder into a beaker, add deionized water, and sonicate for 40 minutes. After sonication, filter again.

[0113] (5) Add N,N-dimethylformamide to the hydrated salt / SiC composite phase change filler powder after filtration in (4) and wash it twice.

[0114] (6) Place the cleaned hydrated salt / SiC composite phase change filler powder from (5) into a vacuum drying oven; the drying oven needs to be preheated to 105℃ and kept at a constant temperature for 12 hours. The modified hydrated salt / SiC composite phase change filler powder is obtained.

[0115] Step 6: Prepare an insulating, high thermal conductivity, and anti-icing coating.

[0116] (1) Cool the reaction product of step 4 to 35°C and add it to the polyurethane prepolymer at 40% of the mass content of the polyurethane prepolymer.

[0117] (2) Add the weighed chain extender and solvent to (7) and start stirring. The stirring conditions are 1500 r / min for 40 min to finally obtain an insulating, high thermal conductivity, and anti-icing coating.

[0118] Example 2

[0119] Step 1, Preparation of hydrated salt phase change materials

[0120] Dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate were mixed in a beaker at a mass ratio of 176.67:13.86, and heated and stirred in a water bath at 55°C until they melted into a transparent liquid to obtain a eutectic hydrated salt.

[0121] Step 2, Preparation of hydrated salt / SiC composite phase change thermal storage material

[0122] (1) Add insulating and thermally conductive silicon carbide filler to the molten eutectic hydrated salt obtained in step 1. After mechanical stirring for 10 min, a eutectic hydrated salt / SiC mixture is obtained. The stirring speed is 110 r / min, and the silicon carbide particle size is 2-5 μm.

[0123] The mass fraction of silicon carbide is 50% of the mass of the eutectic hydrate salt.

[0124] (2) The eutectic hydrated salt / SiC mixture after being thoroughly and uniformly mixed is loaded into a crucible, and an appropriate amount of aluminum dihydrogen phosphate binder is added to obtain process mixture A.

[0125] The aluminum dihydrogen phosphate content is 3% of the mass of the eutectic hydrated salt / SiC mixture.

[0126] (3) Place the process mixture A obtained in step (3) into a crucible, put the crucible into a drying oven at 120°C and dry for 4 hours. Then close the drying oven and let it cool naturally to room temperature before taking it out to obtain process mixture B.

[0127] (4) Take out the cooled process mixture B and sinter it with a specific heating program to obtain process mixture C;

[0128] The heating process is as follows: heat from room temperature to 25°C for 40 minutes and hold for 20 minutes; heat to 50°C for 40 minutes and hold for 20 minutes; heat to 75°C for 30 minutes and hold for 30 minutes; and hold at the highest sintering temperature of 100°C for 1 hour.

[0129] Step (5): After the heat preservation process in step (4) is completed, take out the process mixture C in the crucible and put it into a planetary ball mill. Dry grind the mixture at a ball-to-material ratio of 1:1 and a speed of 100 r / min until the particle size of the mixture is 10-20 μm to obtain the hydrated salt / SiC composite phase change filler.

[0130] Step 3, weigh the polyurethane base material

[0131] Specifically, the diisocyanate is hexamethylene diisocyanate, and its mass content is 20% of the polyurethane base material;

[0132] Specifically, the polyether glycol is polyethylene glycol, and its mass content is 20% of the polyurethane prepolymer;

[0133] Specifically, the chain extender is 1,5-pentanediol, and its mass content is 4% of the polyurethane prepolymer;

[0134] Specifically, the hydrophilic chain extender is dimethylolbutyric acid, and its mass content is 2% of the polyurethane prepolymer;

[0135] Specifically, the catalyst is stannous octoate, and its mass content is 2% of the polyurethane prepolymer;

[0136] Specifically, the neutralizing agent is formic acid, and its mass content is 2% of the polyurethane prepolymer.

[0137] Specifically, the solvent is N,N-dimethylformamide, and its mass content is 50% of that of the polyurethane prepolymer.

[0138] Step 4: Prepare polyurethane prepolymer

[0139] (1) Weigh the diisocyanate, polyether glycol, post-chain extender, hydrophilic chain extender, catalyst, neutralizer and solvent according to the set mass ratio;

[0140] (2) Dry the weighed polyether glycol at 110°C for 5 hours.

[0141] (3) Take out the dried polyether diol from step (2) and put it into a three-necked round bottom flask. Pour nitrogen into the flask and start stirring. The stirring speed is 350 r / min and the stirring time is 20 min.

[0142] (4) Add the weighed catalyst and diisocyanate to the flask in step (3), start stirring, the stirring speed is 350 r / min, the stirring temperature is 88℃, and the stirring time is 30 min.

[0143] (5) Add the weighed hydrophilic chain extender to the flask in step (4), turn on the stirrer, the stirring speed is 350 r / min, the stirring temperature is 80℃, and the stirring time is 2h.

[0144] (6) Cool the reaction product of step (5) to 50°C, add the weighed neutralizing agent to carry out the neutralization reaction for 30 minutes to obtain polyurethane prepolymer.

[0145] Step 5, Preparation of modified hydrated salt / SiC composite phase change filler micro powder

[0146] (1) Add the hydrated salt / SiC composite phase change filler and silane coupling agent KH550 to a three-necked flask in a ratio of 25:1, and add toluene as a solvent for the reaction environment.

[0147] (2) Place the three-necked flask in a constant temperature oil bath, heat it to 90°C, introduce nitrogen gas and maintain the nitrogen atmosphere, start stirring and react for 6 hours at a stirring speed of 100 r / min.

[0148] (3) After the reaction is complete, the mixed solution in (2) is vacuum filtered.

[0149] (4) After vacuum filtration, pour the hydrated salt / SiC composite phase change filler powder into a beaker, add deionized water, and sonicate for 30 minutes. After sonication, filter again.

[0150] (5) Add N,N-dimethylformamide to the hydrated salt / SiC composite phase change filler powder after filtration in (4) and wash it twice.

[0151] (6) Place the cleaned hydrated salt / SiC composite phase change filler powder from (5) into a vacuum drying oven; the drying oven needs to be preheated to 105℃ and kept at a constant temperature for 12 hours. The modified hydrated salt / SiC composite phase change filler powder is obtained.

[0152] Step 6: Prepare an insulating, high thermal conductivity, and anti-icing coating.

[0153] (1) Cool the reaction product of step 4 to 35°C and add it to the polyurethane prepolymer at 40% of the mass content of the polyurethane prepolymer.

[0154] (2) Add the weighed chain extender and solvent to (7) and start stirring. The stirring conditions are 900 r / min and 60 min. Finally, the insulating, high thermal conductivity and anti-icing coating is obtained.

[0155] Example 3

[0156] Step 1, Preparation of hydrated salt phase change materials

[0157] Dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate were mixed in a beaker at a mass ratio of 176.67:13.86, and heated and stirred in a water bath at 55°C until they melted into a transparent liquid to obtain a eutectic hydrated salt.

[0158] Step 2, Preparation of hydrated salt / SiC composite phase change thermal storage material

[0159] (1) Add insulating and thermally conductive silicon carbide filler to the molten eutectic hydrated salt obtained in step 1. After mechanical stirring for 15 min, a eutectic hydrated salt / SiC mixture is obtained. The stirring speed is 60 r / min, and the silicon carbide particle size is 2-5 μm.

[0160] The mass fraction of silicon carbide is 80% of the mass of the eutectic hydrate salt.

[0161] (2) The eutectic hydrated salt / SiC mixture after being thoroughly and uniformly mixed is loaded into a crucible, and an appropriate amount of aluminum dihydrogen phosphate binder is added to obtain process mixture A.

[0162] The aluminum dihydrogen phosphate content is 4.5% of the mass of the eutectic hydrate salt / SiC mixture.

[0163] (3) Place the process mixture A obtained in step (3) into a crucible, put the crucible into a drying oven at 120°C and dry for 6 hours. Then close the drying oven and let it cool naturally to room temperature before taking it out to obtain process mixture B.

[0164] (4) Take out the cooled process mixture B and sinter it with a specific heating program to obtain process mixture C;

[0165] The heating process is as follows: heat from room temperature to 50°C for 40 minutes and hold for 20 minutes; heat to 75°C for 40 minutes and hold for 20 minutes; heat to 100°C for 30 minutes and hold for 30 minutes; and hold at the highest sintering temperature of 100°C for 1 hour.

[0166] (5) After the heat preservation process in step (4) is completed, take out the process mixture C in the crucible and put it into a planetary ball mill. Dry grind the mixture at a ball-to-material ratio of 1:1 and a speed of 100r / min until the particle size of the mixture is 10-20μm to obtain the hydrated salt / SiC composite phase change filler.

[0167] Step 3, weigh the polyurethane base material

[0168] Specifically, the diisocyanate is 4,4'-dicyclohexylmethane diisocyanate, which accounts for 25% of the mass of the polyurethane base material;

[0169] Specifically, the polyether glycol is polypropylene glycol, and its mass content is 15% of the polyurethane prepolymer;

[0170] Specifically, the chain extender is 1,5-pentanediol, and its mass content is 2.5% of the polyurethane prepolymer;

[0171] Specifically, the hydrophilic chain extender is 2,2-dimethylolpropionic acid, and its mass content is 2% of the polyurethane prepolymer;

[0172] Specifically, the catalyst is dibutyltin oxide, and its mass content is 3.5% of the polyurethane prepolymer;

[0173] Specifically, the neutralizing agent is triethanolamine, and its mass content is 2% of the polyurethane prepolymer.

[0174] Specifically, the solvent is N,N-dimethylformamide, and its mass content is 50% of that of the polyurethane prepolymer.

[0175] Step 4: Prepare polyurethane prepolymer

[0176] (1) Weigh the diisocyanate, polyether glycol, post-chain extender, hydrophilic chain extender, catalyst, neutralizer and solvent according to the set mass ratio;

[0177] (2) Dry the weighed polyether glycol at 110°C for 5 hours.

[0178] (3) Take out the dried polyether diol from step (2) and put it into a three-necked round bottom flask. Pour nitrogen into the flask and start stirring. The stirring speed is 350 r / min and the stirring time is 20 min.

[0179] (4) Add the weighed catalyst and diisocyanate to the flask in step (3), start stirring, the stirring speed is 350 r / min, the stirring temperature is 88℃, and the stirring time is 60 min.

[0180] (5) Add the weighed hydrophilic chain extender to the flask in step (4), turn on the stirrer, the stirring speed is 350 r / min, the stirring temperature is 80℃, and the stirring time is 3h.

[0181] (6) Cool the reaction product of step (5) to 50°C, add the weighed neutralizing agent to carry out the neutralization reaction for 40 minutes to obtain polyurethane prepolymer.

[0182] Step 5, Preparation of modified hydrated salt / SiC composite phase change filler micro powder

[0183] (1) Add the hydrated salt / SiC composite phase change filler and silane coupling agent KH550 to a three-necked flask in a ratio of 25:1, and add toluene as a solvent for the reaction environment.

[0184] (2) Place the three-necked flask in a constant temperature oil bath, heat it to 90°C, introduce nitrogen gas and maintain the nitrogen atmosphere, start stirring and react for 6 hours at a stirring speed of 150 r / min.

[0185] (3) After the reaction is complete, the mixed solution in step (2) is vacuum filtered.

[0186] (4) After vacuum filtration, pour the hydrated salt / SiC composite phase change filler powder into a beaker, add deionized water, and sonicate for 60 minutes. After sonication, filter again.

[0187] (5) Add N,N-dimethylformamide to the hydrated salt / SiC composite phase change filler powder after filtration in step (4) and wash it twice.

[0188] (6) Place the cleaned hydrated salt / SiC composite phase change filler powder from step (5) into a vacuum drying oven; the drying oven needs to be preheated to 105℃ and kept at a constant temperature for 12 hours. The modified hydrated salt / SiC composite phase change filler powder is obtained.

[0189] Step 6: Prepare an insulating, high thermal conductivity, and anti-icing coating.

[0190] (1) Cool the reaction product of step 4 to 35°C and add it to the polyurethane prepolymer at 40% of the mass content of the polyurethane prepolymer.

[0191] (2) Add the weighed chain extender and solvent to the product obtained in step (1), and start stirring. The stirring speed is 2000 r / min and the stirring temperature is 30 min. Finally, the insulating, high thermal conductivity and anti-icing coating is obtained.

[0192] Example 4

[0193] Step 1, Preparation of hydrated salt phase change materials

[0194] Dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate were mixed in a beaker at a mass ratio of 176.67:13.86, and heated and stirred in a water bath at 55°C until they melted into a transparent liquid to obtain a eutectic hydrated salt.

[0195] Step 2, Preparation of hydrated salt / SiC composite phase change thermal storage material

[0196] (1) Add insulating and thermally conductive silicon carbide filler to the molten eutectic hydrated salt obtained in step 1. After mechanical stirring for 13 min, a eutectic hydrated salt / SiC mixture is obtained. The stirring speed is 100 r / min, and the silicon carbide particle size is 2-5 μm.

[0197] The mass fraction of silicon carbide is 70% of the mass of the eutectic hydrate salt.

[0198] (2) The eutectic hydrated salt / SiC mixture after being thoroughly and uniformly mixed is loaded into a crucible, and an appropriate amount of aluminum dihydrogen phosphate binder is added to obtain process mixture A.

[0199] The aluminum dihydrogen phosphate content is 3.5% of the mass of the eutectic hydrate salt / SiC mixture.

[0200] (3) Place the process mixture A obtained in step (2) into a crucible, put the crucible into a drying oven at 120°C and dry for 6 hours. Then close the drying oven and let it cool naturally to room temperature before taking it out to obtain process mixture B.

[0201] (4) Take out the cooled process mixture B and sinter it with a specific heating program to obtain process mixture C;

[0202] The heating process is as follows: heat from room temperature to 40°C for 40 minutes and hold for 20 minutes; heat to 70°C for 40 minutes and hold for 20 minutes; heat to 80°C for 30 minutes and hold for 30 minutes; and hold at the highest sintering temperature of 100°C for 1 hour.

[0203] (5) After the heat preservation process in step (4) is completed, take out the process mixture C in the crucible and put it into a planetary ball mill. Dry grind the mixture at a ball-to-material ratio of 1:1 and a speed of 100r / min until the particle size of the mixture is 10-20μm to obtain the hydrated salt / SiC composite phase change filler.

[0204] Step 3, weigh the polyurethane prebase material

[0205] Specifically, the diisocyanate is isoflurone diisocyanate, and its mass content is 23% of the polyurethane base material;

[0206] Specifically, the polyether diol is polytetrahydrofuran diol, and its mass content is 17% of the polyurethane prepolymer;

[0207] Specifically, the chain extender is 1,5-pentanediol, and its mass content is 7.5% of the polyurethane prepolymer;

[0208] Specifically, the hydrophilic chain extender is 2,2-dimethylolpropionic acid, and its mass content is 1% of the polyurethane prepolymer;

[0209] Specifically, the catalyst is dibutyltin dilaurate, and its mass content is 1% of the polyurethane prepolymer;

[0210] Specifically, the neutralizing agent is tripropylamine, and its mass content is 0.5% of the polyurethane prepolymer.

[0211] Specifically, the solvent is N,N-dimethylformamide, and its mass content is 50% of that of the polyurethane prepolymer.

[0212] Step 4: Prepare polyurethane prepolymer

[0213] (1) Weigh the diisocyanate, polyether glycol, post-chain extender, hydrophilic chain extender, catalyst, neutralizer and solvent according to the set mass ratio;

[0214] (2) Dry the weighed polyether glycol at 110°C for 5 hours.

[0215] (3) Take out the dried polyether diol from step (2) and put it into a three-necked round bottom flask. Pour nitrogen into the flask and start stirring. The stirring speed is 350 r / min and the stirring time is 20 min.

[0216] (4) Add the weighed catalyst and diisocyanate to the flask in step (3), start stirring, the stirring speed is 350 r / min, the stirring temperature is 88℃, and the stirring time is 40 min.

[0217] (5) Add the weighed hydrophilic chain extender to the flask in step (4), turn on the stirrer, the stirring speed is 350 r / min, the stirring temperature is 80℃, and the stirring time is 3h.

[0218] (6) Cool the reaction product of step (5) to 50°C, add the weighed neutralizing agent to carry out the neutralization reaction for 30 minutes to obtain polyurethane prepolymer.

[0219] Step 5, Preparation of modified hydrated salt / SiC composite phase change filler micro powder

[0220] (1) Add the hydrated salt / SiC composite phase change filler and silane coupling agent KH550 to a three-necked flask in a ratio of 25:1, and add toluene as a solvent for the reaction environment.

[0221] (2) Place the three-necked flask in a constant temperature oil bath, heat it to 90°C, introduce nitrogen gas and maintain the nitrogen atmosphere, start stirring and react for 6 hours at a stirring speed of 110 r / min.

[0222] (3) After the reaction is complete, the mixed solution in step (2) is vacuum filtered.

[0223] (4) After vacuum filtration, pour the hydrated salt / SiC composite phase change filler powder into a beaker, add deionized water, and sonicate for 50 minutes. After sonication, filter again.

[0224] (5) Add N,N-dimethylformamide to the hydrated salt / SiC composite phase change filler powder after filtration in step (4) and wash it twice.

[0225] (6) Place the cleaned hydrated salt / SiC composite phase change filler powder from step (5) into a vacuum drying oven; the drying oven needs to be preheated to 105℃ and kept at a constant temperature for 12 hours. The modified hydrated salt / SiC composite phase change filler powder is obtained.

[0226] Step 6: Prepare an insulating, high thermal conductivity, and anti-icing coating.

[0227] (1) Cool the reaction product of step 4 to 35°C and add it to the polyurethane prepolymer at 40% of the mass content of the polyurethane prepolymer.

[0228] (2) Add the weighed chain extender and solvent to (7) and start stirring. The stirring conditions are 1500 r / min for 40 min to finally obtain an insulating, high thermal conductivity, and anti-icing coating.

[0229] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades, characterized in that, Includes the following steps: Step 1: Mix dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate, and heat in a water bath until a transparent liquid is obtained to obtain a eutectic hydrated salt; Step 2: Add silicon carbide to the eutectic hydrated salt, mechanically stir, and then add aluminum dihydrogen phosphate to obtain process mixture A. Dry process mixture A and sinter it. Ball mill the sintered product to obtain hydrated salt / SiC composite phase change filler. Aluminum dihydrogen phosphate acts as a binder to bond SiC and eutectic salt particles together. The amount of silicon carbide added is 50% to 80% of the mass of the eutectic hydrate salt; The amount of aluminum dihydrogen phosphate added is 3-4.5% of the mass of the mixture of eutectic hydrate salt and silicon carbide; The sintering process in step 2 is as follows: heat at 25~50℃ for 40 min, hold for 20 min; heat at 50~75℃ for 40 min, hold for 20 min; heat at 75~100℃ for 30 min, hold for 30 min; and hold at 100℃ for 1 h. Step 3: Weigh the polyurethane base material, which includes diisocyanate, polyether glycol, hydrophilic chain extender, catalyst, neutralizer, post-chain extender and solvent. Step 4: Prepare polyurethane prepolymer by using diisocyanate, polyether glycol, hydrophilic chain extender, catalyst and neutralizer in polyurethane base material; Step 5: Mix the hydrated salt / SiC composite phase change filler and silane coupling agent KH550, add toluene, react in an oil bath, and then vacuum filter the reaction product. Mix the vacuum filtered product with water and then sonicate it. The sonicated product is then vacuum filtered. The vacuum filtered product is washed with N,N-dimethylformamide and then dried to obtain the modified hydrated salt / SiC composite phase change filler micro powder. Step 6: Mix the modified hydrated salt / SiC composite phase change filler micro powder, polyurethane prepolymer, post-chain extender and solvent, and stir to obtain an insulating, high thermal conductivity and anti-icing coating.

2. The method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades according to claim 1, characterized in that, In step 1, the mixing mass ratio of dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate is 176.67:13.86, and the water bath heating temperature is 55℃.

3. The method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades according to claim 1, characterized in that, In step 2, the drying temperature is 120℃ and the drying time is 4~6h.

4. The method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades according to claim 1, characterized in that, In step 3, the polyurethane base material is composed of, by mass fraction, 20-25% diisocyanate, 15-20% polyether glycol, 2.5-7.5% post-chain extender, 1-2% hydrophilic chain extender, 1-3.5% catalyst, 0.5-2% neutralizer and 50% solvent.

5. The method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades according to claim 1, characterized in that, In step 4, the preparation process of the polyurethane prepolymer is as follows: (1) Dry the polyether glycol at 110°C for 5 hours; (2) Place the dried polyether glycol in a three-necked round-bottom flask, introduce nitrogen gas into the flask, and stir; (3) Add the catalyst and diisocyanate to the flask in step (2) and stir; (4) Add the hydrophilic chain extender to the flask in step (3), stir the reaction, and obtain the reaction product; (5) Cool the reaction product of step (4) to 50°C, add a neutralizing agent to carry out a neutralization reaction, and obtain polyurethane prepolymer.

6. The method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades according to claim 1, characterized in that, In step 5, the molar ratio of hydrated salt / SiC composite phase change filler to silane coupling agent KH550 is 25:1, the oil bath reaction temperature is 90℃, and the oil bath reaction time is 6h.

7. The method for preparing an insulating, high thermal conductivity, and anti-icing coating for wind turbine blades according to claim 1, characterized in that, In step 5, the amount of hydrated salt / SiC composite phase change filler powder added is 30-60% of that of the polyurethane prepolymer.

8. An insulating, high thermal conductivity, and anti-icing coating prepared by any one of claims 1-7, characterized in that, It includes hydrated salt / SiC composite phase change filler micro powder and polyurethane prepolymer. The hydrated salt / SiC composite phase change filler micro powder is composed of eutectic hydrated salt and silicon carbide. The eutectic hydrated salt is composed of dipotassium hydrogen phosphate hexahydrate and disodium hydrogen phosphate dodecahydrate.

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