High-performance polyether-ether-ketone composite material as well as preparation method and application thereof

Abstract

The invention discloses a high-performance polyether-ether-ketone composite material as well as a preparation method and application thereof, and belongs to the technical field of preparation of polyether-ether-ketone composite materials. The preparation method of the high-performance polyether-ether-ketone composite material comprises the following steps: step 1, adding 4, 4 '-dihydroxy-4, 4'-dihydroxy-4, 4 The preparation method comprises the following steps: adding 4, 4 '-difluorobenzophenone, modified diphenol, hexafluorobisphenol and anhydrous potassium carbonate into a container filled with a mixed solvent of dimethyl sulfoxide and toluene, heating for reflux reaction, then heating for continuous reaction, after the reaction is finished, adding into distilled water, separating out a solid, washing and drying to obtain a polymer; and 2, adding the polymer into N-methyl pyrrolidone, then adding a modification auxiliary agent, carrying out ultrasonic treatment, and carrying out heating curing to obtain the high-performance polyether-ether-ketone composite material. The polyether-ether-ketone composite material prepared by the method has excellent mechanical property and thermal stability.

Description

Technical Field

[0001] The present invention belongs to the technical field of polyetheretherketone composite material preparation, and in particular relates to a high-performance polyetheretherketone composite material and a preparation method and application thereof. Background Art

[0002] As a high-performance special engineering plastic, polyetheretherketone (PEEK) has shown broad application prospects in aerospace, medical equipment, automobile manufacturing and other fields due to its excellent chemical corrosion resistance and biocompatibility. However, with the continuous improvement of industrial technology's requirements for the comprehensive performance of materials, the mechanical performance limitations of pure PEEK have gradually become prominent. Although it already has high strength and modulus, under extreme working conditions, such as high temperature, high stress or complex load environments, pure PEEK's insufficient rigidity and poor creep resistance still restrict its further application. Especially in scenarios where it needs to withstand both mechanical and thermal loads, the material is prone to deformation or fatigue failure, making it difficult to meet the dual needs of lightweight and high reliability in high-end fields.

[0003] Patent CN109851989B discloses a polyetheretherketone (PEEK) composite material, its preparation method, and its application. The composite material comprises the following components, measured by weight: 60-75 parts PEEK; 5-10 parts PTFE; 5-15 parts polyimide; 5-10 parts carbon fiber; 0.1-1 part graphene; and 0.5-4 parts nano-silica. This invention uses PEEK as a matrix. By adding polyimide, PTFE, carbon fiber, graphene, and nano-silica, the composite material effectively improves its hardness, tensile strength, elongation at break, flexural strength, compressive strength, and high-temperature resistance. It also improves its friction resistance. However, there is still room for improvement in the mechanical and temperature resistance of this composite material. The reinforcing effect of carbon fiber mainly depends on its high modulus characteristics, but the randomness of fiber orientation distribution may lead to anisotropy. Although the nanosheet structure of graphene can inhibit crack propagation, its easy agglomeration characteristics limit the reinforcement efficiency. The addition of polyimide can significantly improve thermal stability, but the difference in glass transition temperature between it and polyetheretherketone may lead to interfacial stress concentration at high temperatures. Therefore, the mechanical properties and high temperature resistance of the prepared polyetheretherketone composite material used as the raw material of semiconductor separators still have room for improvement. Summary of the Invention

[0004] The purpose of the present invention is to provide a high-performance polyetheretherketone composite material and a preparation method and application thereof, so as to solve the technical problems of poor mechanical properties and high-temperature resistance of polyetheretherketone composite materials in the prior art.

[0005] In order to achieve the above object, the present invention adopts the following technical solutions: The present invention provides a method for preparing a high-performance polyetheretherketone composite material, comprising the following steps: Step 1: adding 4,4'-difluorobenzophenone, modified diphenol, hexafluorobisphenol and anhydrous potassium carbonate to a container containing a mixed solvent of dimethyl sulfoxide and toluene, heating and refluxing the mixture, then heating and continuing the reaction. After the reaction is completed, adding the mixture to distilled water, precipitating a solid, washing and drying the solid to obtain a polymer; In the above process, the synthetic reaction formula of the polymer is as follows: Step 2: Add the polymer to N-methylpyrrolidone, then add the modification agent, perform ultrasonic treatment, heat and cure, and obtain a high-performance polyetheretherketone composite material.

[0006] Preferably, the preparation method of the modified diphenol comprises the following steps: Q1: Add anthrone, thionyl chloride and N,N-dimethylformamide to a container, heat to reflux, and then rotary evaporate to obtain compound a; Q2: Add a mixed solution of phenol and xylene to compound a, heat under reflux for reaction, and after the reaction is completed, filter, wash, and recrystallize to obtain modified diphenol.

[0007] In the above process, the synthetic reaction formula of modified diphenol is as follows: The structure of compound a by mass spectrometry analysis was: m / z: 262.00 (100.0%), 263.99 (63.9%), 263.00(15.3%), 265.99 (10.2%), 265.00 (9.8%), 266.99 (1.6%), 264.00 (1.3%); the structure of modified diphenol by mass spectrometry analysis was: m / z: 378.13 (100.0%), 379.13 (28.4%), 380.13 (4.5%).

[0008] Preferably, in Q1, the usage ratio of anthrone, thionyl chloride and N,N-dimethylformamide is (19.2-19.6) g: (125-175) mL: (0.02-0.04) mL, and the reflux time is 10-15 h.

[0009] Preferably, in Q2, the usage ratio of phenol, xylene and compound a is (35.2-40.1) g: (90-110) mL: (17.5-18.2) g, the heating reflux reaction time is 10-14 h, the product is washed with dichloromethane and recrystallized with acetone.

[0010] Preferably, the preparation method of the modification aid comprises the following steps: S1: p-Trifluoromethylphenol and ethyl 4-bromobutyrate were added to acetonitrile, stirred and mixed, and then cesium carbonate was added. The mixture was heated and stirred under nitrogen protection. After the reaction was completed, the mixture was purified to obtain a yellow oil 1; S2: The yellow oil 1 was dissolved in methanol, and then sodium hydroxide aqueous solution was added and reacted at room temperature. After the reaction was completed, the mixture was dried under reduced pressure, diluted with distilled water, and the pH was adjusted. The mixture was filtered, washed, and dried to obtain a white solid 2; S3: Add white solid 2 and 2-hydrazino-1,3-benzoxazole to dichloromethane, stir, then add triethylamine, EDC hydrochloride and 1-hydroxybenzotriazole in sequence, stir at low temperature and then react at room temperature. After the reaction is completed, concentrate under reduced pressure and purify to obtain a modified auxiliary agent.

[0011] In the above process, the synthetic reaction formula of the modified additive is as follows: The results of mass spectrometry analysis of the yellow oil 1 were: m / z: 276.10 (100.0%), 277.10 (14.3%), 278.10 (1.5%); the results of mass spectrometry analysis of the white solid 2 were: m / z: 248.07 (100.0%), 249.07 (12.1%), 250.07 (1.3%); the results of mass spectrometry analysis of the modified auxiliary agent were: m / z: 379.11 (100.0%), 380.12 (19.8%), 381.12 (2.5%), 380.11 (1.1%).

[0012] Preferably, in S1, the molar ratio of trifluoromethylphenol, ethyl 4-bromobutyrate and cesium carbonate is (1-1.2): (1.5-1.8): (2-2.4), the heating and stirring reaction temperature is 50-55°C, and the reaction time is 8-10 hours; in S2, the amount ratio of the yellow oil 1, methanol and sodium hydroxide aqueous solution is (1-1.54) g: (8-12) mL: (5-8) mL, the concentration of the sodium hydroxide aqueous solution is 1.2 g / mL, the reaction time at room temperature is 2-4 hours, and the pH is adjusted to 5 with 1 mol / L hydrochloric acid.

[0013] Preferably, in S3, the molar ratio of the white solid 2,2-hydrazino-1,3-benzoxazole, triethylamine, EDC hydrochloride and 1-hydroxybenzotriazole is (1-1.2): (1-1.3): (4-4.6): (2-2.3): (2-2.5), the low-temperature stirring temperature is 0-1°C, and the room temperature stirring reaction time is 10-12h.

[0014] Preferably, in the step 1, the molar ratio of 4,4'-difluorobenzophenone, modified diphenol, hexafluorobisphenol and anhydrous potassium carbonate is (10-20): (1-2): (10-17): (20-25), the temperature of the reflux reaction is 130-140°C, the time is 3-5 hours, and the temperature of the continued reaction is 140-145°C, and the continued reaction time is 3-5 hours. In the step 2, the amount ratio of the polymer, N-methylpyrrolidone and the modification auxiliary agent is (0.25-0.32) g: (4-6) g: (0.082-0.091) g, and the temperature-raising curing process is: heating at 80°C for 120 minutes, heating at 200°C for 100 minutes, and the heating rate is 4°C / min.

[0015] The high-performance polyetheretherketone composite material is prepared by the above-mentioned preparation method.

[0016] Preferably, a high-performance polyetheretherketone composite material is used, and the prepared high-performance polyetheretherketone composite material is applied to the fields of semiconductors and 3D printing.

[0017] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are: In the process of preparing the polyetheretherketone composite material, the present invention adds modified diphenol and modification auxiliary agent, which can effectively improve the thermal stability and mechanical properties of the composite material. Using the prepared polyetheretherketone composite material as a raw material for a semiconductor separator can effectively increase the service life of the semiconductor separator.

[0018] The present invention uses the prepared modified diphenol as one of the main raw materials of the polyetheretherketone composite material, which can effectively improve the thermal stability and mechanical properties of the composite material. The steric hindrance effect of the anthracene ring contained in the modified diphenol significantly restricts the movement of the molecular chain, increases the glass transition temperature, and improves the thermal stability of the composite material. At the same time, the rigid skeleton of the anthracene ring forms a dynamic physical cross-linking network through π-π stacking, which not only serves as a physical cross-linking point to further improve the heat resistance, but also balances toughness and rigidity through a slip energy dissipation mechanism, thereby improving the mechanical properties of the material.

[0019] The present invention adds the prepared modification aid to the preparation process of the polyetheretherketone composite material, which can effectively improve its thermal stability. The rigid benzoxazole groups contained in the modification aid form π-π stacking and dipole interactions with the polyetheretherketone chain segments, and cooperate with the strong hydrogen bond anchoring effect of the hydrazide group to significantly accelerate the crystallization rate and refine the spherulite structure. At the same time, the high heat resistance of the benzoxazole group and the hydrogen bond network further enhance the thermal stability of the composite material. DETAILED DESCRIPTION

[0020] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0021] Example 1: This example discloses a method for preparing modified diphenol, comprising the following steps: Q1: 19.4 g of anthrone, 150 mL of thionyl chloride, and 0.03 mL of N,N-dimethylformamide were added to a container, heated under reflux for 14 h, and then rotary evaporated to obtain compound a; Q2: A mixed solution of 38.2 g of phenol and 100 mL of xylene was added to 17.8 g of compound a, and the mixture was heated under reflux for 12 h. After the reaction was completed, the mixture was filtered, washed with dichloromethane, and recrystallized with acetone to obtain modified diphenol.

[0022] This embodiment discloses a method for preparing a modification aid, comprising the following steps: S1: 1.78 g of p-trifluoromethylphenol and 3.22 g of ethyl 4-bromobutyrate were added to 10 mL of acetonitrile and stirred. 3.7 g of cesium carbonate was then added. The mixture was heated and stirred at 50°C under nitrogen for 8 h. After the reaction was complete, the mixture was purified to obtain a yellow oil 1. S2: Dissolve 1.27 g of the yellow oil 1 in 10 mL of methanol, then add 6.5 mL of a 1.2 g / mL sodium hydroxide solution and react at room temperature for 4 h. After the reaction is complete, evaporate to dryness under reduced pressure, dilute with distilled water, adjust the pH to 5 with 1 mol / L hydrochloric acid, filter, wash, and dry to obtain a white solid 2. S3: Add 2.77 g of white solid 2 and 1.74 g of 2-hydrazino-1,3-benzoxazole to 20 mL of dichloromethane. After stirring, add 4.32 g of triethylamine, 4.11 g of EDC hydrochloride and 3.02 g of 1-hydroxybenzotriazole in sequence. Stir at 0°C for 1 h and then at room temperature for 12 h. After the reaction is completed, concentrate under reduced pressure and purify to obtain a modification aid.

[0023] This embodiment discloses a method for preparing a high-performance polyetheretherketone composite material, comprising the following steps: Step 1: 8.65 g of 4,4'-difluorobenzophenone, 1.5 g of modified diphenol, 12 g of hexafluorobisphenol and 8.22 g of anhydrous potassium carbonate were added to a container containing a mixed solvent of 18 mL of dimethyl sulfoxide and 9 mL of toluene, and the mixture was heated to 140°C and refluxed for 4 hours, then heated to 140°C and continued to react for 5 hours. After the reaction was completed, the mixture was added to distilled water, the solid was precipitated, washed, and dried to obtain a polymer; Step 2: Add 0.27 g of polymer to 5 g of N-methylpyrrolidone, then add 0.085 g of modification agent, and after ultrasonic treatment, heat and cure. The process is: heating at 80°C for 120 min and heating at 200°C for 100 min, with a heating rate of 4°C / min, to obtain a high-performance polyetheretherketone composite material.

[0024] Example 2: This example discloses a method for preparing modified diphenol, comprising the following steps: Q1: 19.2 g of anthrone, 125 mL of thionyl chloride, and 0.04 mL of N,N-dimethylformamide were added to a container, heated under reflux for 14 h, and then rotary evaporated to obtain compound a; Q2: A mixed solution of 35.2 g of phenol and 110 mL of xylene was added to 17.5 g of compound a, and the mixture was heated under reflux for 12 h. After the reaction was completed, the mixture was filtered, washed with dichloromethane, and recrystallized with acetone to obtain modified diphenol.

[0025] This embodiment discloses a method for preparing a modification aid, comprising the following steps: S1: 1.62 g of p-trifluoromethylphenol and 2.93 g of ethyl 4-bromobutyrate were added to 10 mL of acetonitrile and stirred. 3.36 g of cesium carbonate was then added. The mixture was heated and stirred at 50°C under nitrogen for 8 h. After the reaction was complete, the mixture was purified to obtain a yellow oil 1. S2: Dissolve 1.54 g of the yellow oil 1 in 12 mL of methanol, then add 5 mL of a 1.2 g / mL sodium hydroxide solution and react at room temperature for 4 h. After the reaction is complete, evaporate to dryness under reduced pressure, dilute with distilled water, adjust the pH to 5 with 1 mol / L hydrochloric acid, filter, wash, and dry to obtain a white solid 2. S3: Add 2.48 g of white solid 2 and 1.49 g of 2-hydrazino-1,3-benzoxazole to 20 mL of dichloromethane. After stirring, add 4.04 g of triethylamine, 3.84 g of EDC hydrochloride and 2.7 g of 1-hydroxybenzotriazole in sequence. Stir at 0°C for 1 h and then at room temperature for 12 h. After the reaction is completed, concentrate under reduced pressure and purify to obtain a modification aid.

[0026] This embodiment discloses a method for preparing a high-performance polyetheretherketone composite material, comprising the following steps: Step 1: 5.77 g of 4,4'-difluorobenzophenone, 2 g of modified diphenol, 15.11 g of hexafluorobisphenol and 7.3 g of anhydrous potassium carbonate were added to a container containing a mixed solvent of 18 mL of dimethyl sulfoxide and 9 mL of toluene, and the mixture was heated to 140°C and refluxed for 4 hours, then heated to 140°C and continued to react for 5 hours. After the reaction was completed, the mixture was added to distilled water, the solid was precipitated, washed, and dried to obtain a polymer; Step 2: Add 0.25g of polymer to 6g of N-methylpyrrolidone, then add 0.082g of modification agent, and after ultrasonic treatment, heat and cure. The process is: heating at 80°C for 120min and heating at 200°C for 100min, with a heating rate of 4°C / min, to obtain a high-performance polyetheretherketone composite material.

[0027] Example 3: This example discloses a method for preparing modified diphenol, comprising the following steps: Q1: 19.6 g of anthrone, 155 mL of thionyl chloride, and 0.02 mL of N,N-dimethylformamide were added to a container, heated under reflux for 14 h, and then rotary evaporated to obtain compound a; Q2: A mixed solution of 40.1 g of phenol and 90 mL of xylene was added to 18.2 g of compound a, and the mixture was heated under reflux for 12 h. After the reaction was completed, the mixture was filtered, washed with dichloromethane, and recrystallized with acetone to obtain modified diphenol.

[0028] This embodiment discloses a method for preparing a modification aid, comprising the following steps: S1: 1.94 g of p-trifluoromethylphenol and 3.51 g of ethyl 4-bromobutyrate were added to 10 mL of acetonitrile and stirred. 4.03 g of cesium carbonate was then added. The mixture was heated and stirred at 50°C under nitrogen for 8 h. After the reaction was complete, the mixture was purified to obtain a yellow oil 1. S2: Dissolve 1 g of the yellow oil 1 in 8 mL of methanol, then add 8 mL of a 1.2 g / mL sodium hydroxide solution and react at room temperature for 4 h. After the reaction is complete, evaporate to dryness under reduced pressure, dilute with distilled water, adjust the pH to 5 with 1 mol / L hydrochloric acid, filter, wash, and dry to obtain a white solid 2. S3: Add 2.97 g of white solid 2 and 1.93 g of 2-hydrazino-1,3-benzoxazole to 20 mL of dichloromethane. After stirring, add 4.64 g of triethylamine, 4.41 g of EDC hydrochloride and 3.37 g of 1-hydroxybenzotriazole in sequence. Stir at 0°C for 1 h and then at room temperature for 12 h. After the reaction is completed, concentrate under reduced pressure and purify to obtain a modification aid.

[0029] This embodiment discloses a method for preparing a high-performance polyetheretherketone composite material, comprising the following steps: Step 1: 11.53 g of 4,4'-difluorobenzophenone, 1 g of modified diphenol, 8.89 g of hexafluorobisphenol and 9.13 g of anhydrous potassium carbonate were added to a container containing a mixed solvent of 18 mL of dimethyl sulfoxide and 9 mL of toluene, and the mixture was heated to 140°C and refluxed for 4 hours, then heated to 140°C and continued to react for 5 hours. After the reaction was completed, the mixture was added to distilled water, the solid was precipitated, washed, and dried to obtain a polymer; Step 2: Add 0.32 g of polymer to 4 g of N-methylpyrrolidone, then add 0.091 g of modification agent, and after ultrasonic treatment, heat and cure. The process is: heating at 80°C for 120 min and heating at 200°C for 100 min, with a heating rate of 4°C / min, to obtain a high-performance polyetheretherketone composite material.

[0030] Example 4: This example discloses a method for preparing modified diphenol, comprising the following steps: Q1: 19.3 g of anthrone, 142 mL of thionyl chloride, and 0.025 mL of N,N-dimethylformamide were added to a container, heated under reflux for 14 h, and then rotary evaporated to obtain compound a; Q2: A mixed solution of 37.3 g of phenol and 95 mL of xylene was added to 17.6 g of compound a, and the mixture was heated under reflux for 12 h. After the reaction was completed, the mixture was filtered, washed with dichloromethane, and recrystallized with acetone to obtain modified diphenol.

[0031] This embodiment discloses a method for preparing a modification aid, comprising the following steps: S1: 1.72 g of p-trifluoromethylphenol and 3.17 g of ethyl 4-bromobutyrate were added to 10 mL of acetonitrile and stirred. 4.52 g of cesium carbonate was then added. The mixture was heated and stirred at 50°C under nitrogen for 8 h. After the reaction was complete, the mixture was purified to obtain a yellow oil 1. S2: Dissolve 1.17 g of the yellow oil 1 in 9 mL of methanol, then add 6 mL of a 1.2 g / mL sodium hydroxide solution and react at room temperature for 4 h. After the reaction is complete, evaporate to dryness under reduced pressure, dilute with distilled water, adjust the pH to 5 with 1 mol / L hydrochloric acid, filter, wash, and dry to obtain a white solid 2. S3: Add 2.52 g of white solid 2 and 1.58 g of 2-hydrazino-1,3-benzoxazole to 20 mL of dichloromethane. After stirring, add 4.18 g of triethylamine, 4.01 g of EDC hydrochloride and 2.95 g of 1-hydroxybenzotriazole in sequence. Stir at 0°C for 1 h and then at room temperature for 12 h. After the reaction is completed, concentrate under reduced pressure and purify to obtain a modification aid.

[0032] This embodiment discloses a method for preparing a high-performance polyetheretherketone composite material, comprising the following steps: Step 1: 7.02 g of 4,4'-difluorobenzophenone, 1.1 g of modified diphenol, 10.07 g of hexafluorobisphenol and 7.87 g of anhydrous potassium carbonate were added to a container containing a mixed solvent of 18 mL of dimethyl sulfoxide and 9 mL of toluene, and the mixture was heated to 140°C and refluxed for 4 hours, then heated to 140°C and continued to react for 5 hours. After the reaction was completed, the mixture was added to distilled water, the solid was precipitated, washed, and dried to obtain a polymer; Step 2: Add 0.26 g of polymer to 4.5 g of N-methylpyrrolidone, then add 0.084 g of modification agent, and after ultrasonic treatment, heat and cure. The process is: heating at 80°C for 120 min and heating at 200°C for 100 min, with a heating rate of 4°C / min, to obtain a high-performance polyetheretherketone composite material.

[0033] Example 5: This example discloses a method for preparing modified diphenol, comprising the following steps: Q1: 19.5 g of anthrone, 168 mL of thionyl chloride, and 0.035 mL of N,N-dimethylformamide were added to a container, heated under reflux for 14 h, and then rotary evaporated to obtain compound a; Q2: A mixed solution of 39.8 g of phenol and 105 mL of xylene was added to 18.1 g of compound a, and the mixture was heated under reflux for 12 h. After the reaction was completed, the mixture was filtered, washed with dichloromethane, and recrystallized with acetone to obtain modified diphenol.

[0034] This embodiment discloses a method for preparing a modification aid, comprising the following steps: S1: 1.83 g of p-trifluoromethylphenol and 3.48 g of ethyl 4-bromobutyrate were added to 10 mL of acetonitrile and stirred. 4.27 g of cesium carbonate was then added. The mixture was heated and stirred at 50°C under nitrogen for 8 h. After the reaction was complete, the mixture was purified to obtain a yellow oil 1. S2: Dissolve 1.48 g of the yellow oil 1 in 11 mL of methanol, then add 7 mL of a 1.2 g / mL sodium hydroxide solution and react at room temperature for 4 h. After the reaction is complete, evaporate to dryness under reduced pressure, dilute with distilled water, adjust the pH to 5 with 1 mol / L hydrochloric acid, filter, wash, and dry to obtain a white solid 2. S3: Add 2.83 g of white solid 2 and 1.87 g of 2-hydrazino-1,3-benzoxazole to 20 mL of dichloromethane. After stirring, add 4.57 g of triethylamine, 4.23 g of EDC hydrochloride and 3.18 g of 1-hydroxybenzotriazole in sequence. Stir at 0°C for 1 h and then at room temperature for 12 h. After the reaction is completed, concentrate under reduced pressure and purify to obtain a modification aid.

[0035] This embodiment discloses a method for preparing a high-performance polyetheretherketone composite material, comprising the following steps: Step 1: 9.17 g of 4,4'-difluorobenzophenone, 1.8 g of modified diphenol, 14.23 g of hexafluorobisphenol and 8.57 g of anhydrous potassium carbonate were added to a container containing a mixed solvent of 18 mL of dimethyl sulfoxide and 9 mL of toluene, and the temperature was raised to 140°C for reflux reaction for 4 hours, and then the temperature was raised to 140°C for further reaction for 5 hours. After the reaction was completed, the mixture was added to distilled water, the solid was precipitated, washed, and dried to obtain a polymer; Step 2: Add 0.31 g of polymer to 5.5 g of N-methylpyrrolidone, then add 0.088 g of modification agent, and after ultrasonic treatment, heat and cure. The process is: heating at 80°C for 120 min and heating at 200°C for 100 min, with a heating rate of 4°C / min, to obtain a high-performance polyetheretherketone composite material.

[0036] Comparative Example 1: Compared with Example 1, in the process of preparing the polyetheretherketone composite material in Comparative Example 1, hydroquinone was used instead of modified diphenol, and other conditions remained unchanged.

[0037] Comparative Example 2: Compared with Example 1, in Comparative Example 2, during the preparation of the polyetheretherketone composite material, no modifying agent was added, and other conditions remained unchanged.

[0038] Performance Testing The polyetheretherketone composite materials prepared in Examples 1-5 and Comparative Examples 1-2 were subjected to performance tests. The hardness of the samples was tested according to GB / T 2411-2008, the tensile properties of the samples were tested according to GB / T 1040.2-2022, the bending properties of the samples were tested according to GB / T 9341-2008, and the thermal stability of the samples was tested according to GB / T 19466.2-2004. The test results are shown in Table 1: Table 1

[0039] The test results in Table 1 indicate that the polyetheretherketone composites prepared using the methods of Examples 1-5 exhibit excellent hardness, tensile properties, flexural strength, and thermal stability. A comparison of Comparative Example 1 with Examples 1-5 demonstrates that the use of modified diphenols effectively improves the hardness, tensile properties, flexural strength, and thermal stability of the composites; a comparison of Comparative Example 2 with Examples 1-5 demonstrates that the addition of a modifying agent effectively improves the thermal stability of the composites.

[0040] The above description is only a preferred specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any technician familiar with the technical field, within the technical scope disclosed by the present invention, who makes equivalent replacements or changes based on the technical solution and inventive concept of the present invention, should be covered by the scope of protection of the present invention.

[0041] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A method for preparing a high-performance polyetheretherketone composite material, characterized in that: The following steps are involved: Step 1: adding 4,4'-difluorobenzophenone, modified diphenol, hexafluorobisphenol and anhydrous potassium carbonate to a container containing a mixed solvent of dimethyl sulfoxide and toluene, heating and refluxing the mixture, then heating and continuing the reaction. After the reaction is completed, adding the mixture to distilled water, precipitating a solid, washing and drying the solid to obtain a polymer; Step 2: Add the polymer to N-methylpyrrolidone, then add the modification agent, perform ultrasonic treatment, heat and cure, and obtain a high-performance polyetheretherketone composite material.

2. The method for preparing a high-performance polyetheretherketone composite material according to claim 1, characterized in that: The preparation method of the modified diphenol comprises the following steps: Q1: Add anthrone, thionyl chloride and N,N-dimethylformamide to a container, heat to reflux, and then rotary evaporate to obtain compound a; Q2: Add a mixed solution of phenol and xylene to compound a, heat under reflux for reaction, and after the reaction is completed, filter, wash, and recrystallize to obtain modified diphenol.

3. The method for preparing a high-performance polyetheretherketone composite material according to claim 2, characterized in that: In the Q1, the usage ratio of anthrone, thionyl chloride and N,N-dimethylformamide is (19.2-19.6) g: (125-175) mL: (0.02-0.04) mL.

4. The method for preparing a high-performance polyetheretherketone composite material according to claim 2, characterized in that: In Q2, the usage ratio of phenol, xylene and compound a is (35.2-40.1) g: (90-110) mL: (17.5-18.2) g.

5. The method for preparing a high-performance polyetheretherketone composite material according to claim 1, characterized in that: The preparation method of the modification auxiliary agent comprises the following steps: S1: p-Trifluoromethylphenol and ethyl 4-bromobutyrate were added to acetonitrile, stirred and mixed, and then cesium carbonate was added. The mixture was heated and stirred under nitrogen protection. After the reaction was completed, the mixture was purified to obtain a yellow oil 1; S2: The yellow oil 1 was dissolved in methanol, and then sodium hydroxide aqueous solution was added and reacted at room temperature. After the reaction was completed, the mixture was dried under reduced pressure, diluted with distilled water, and the pH was adjusted. The mixture was filtered, washed, and dried to obtain a white solid 2; S3: Add white solid 2 and 2-hydrazino-1,3-benzoxazole to dichloromethane, stir, then add triethylamine, EDC hydrochloride and 1-hydroxybenzotriazole in sequence, stir at low temperature and then react at room temperature. After the reaction is completed, concentrate under reduced pressure and purify to obtain a modified auxiliary agent.

6. The method for preparing a high-performance polyetheretherketone composite material according to claim 5, characterized in that: In S1, the molar ratio of trifluoromethylphenol, ethyl 4-bromobutyrate and cesium carbonate is (1-1.2): (1.5-1.8): (2-2.4); in S2, the amount ratio of the yellow oil 1, methanol and sodium hydroxide aqueous solution is (1-1.54) g: (8-12) mL: (5-8) mL.

7. The method for preparing a high-performance polyetheretherketone composite material according to claim 5, characterized in that: In the S3, the molar ratio of the white solid 2,2-hydrazino-1,3-benzoxazole, triethylamine, EDC hydrochloride and 1-hydroxybenzotriazole is (1-1.2): (1-1.3): (4-4.6): (2-2.3): (2-2.5).

8. The method for preparing a high-performance polyetheretherketone composite material according to claim 1, characterized in that: In the step 1, the molar ratio of 4,4'-difluorobenzophenone, modified diphenol, hexafluorobisphenol and anhydrous potassium carbonate is (10-20): (1-2): (10-17): (20-25); in the step 2, the amount ratio of the polymer, N-methylpyrrolidone and the modification aid is (0.25-0.32) g: (4-6) g: (0.082-0.091) g.

9. A high-performance polyetheretherketone composite material, characterized in that: The preparation method is described in any one of claims 1 to 8.

10. An application of a high-performance polyetheretherketone composite material, characterized in that: The high-performance polyetheretherketone composite material according to claim 9 is applied in the preparation process of a semiconductor separator.

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