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CN-121975298-A - Carbon fiber reinforced polyether-ether-ketone composite material and preparation method thereof

CN121975298ACN 121975298 ACN121975298 ACN 121975298ACN-121975298-A

Abstract

The invention discloses a carbon fiber reinforced polyether-ether-ketone composite material which comprises, by weight, 58.1 parts to 78.1 parts of polyether-ether-ketone resin, 10 parts to 40 parts of surface modified carbon fibers, 0.1 part to 0.5 part of internal lubrication flow improver, 0.2 part to 0.5 part of compound antioxidant and 0.4 part to 1.2 parts of compound lubricant. The carbon fiber reinforced polyether-ether-ketone composite material has the characteristics of high mechanical property, high strength, high heat resistance and permanent antistatic property. The preparation method comprises the steps of adopting a strong oxidizing agent to treat the surface of carbon fiber, introducing polar groups such as hydroxyl, carboxyl, epoxy and the like to strengthen the surface activity, then utilizing hydrobromic acid and thiourea to carry out secondary modification to convert part of the polar groups into mercapto groups to prepare the surface modified carbon fiber with the surface rich in the mercapto groups, and finally uniformly dispersing the surface modified carbon fiber into a polyether-ether-ketone matrix by a melt blending method to prepare the carbon fiber reinforced polyether-ether-ketone composite material, wherein the heat resistance, the heat conductivity and the electric conductivity are synchronously optimized by improving the content of the surface modified carbon fiber.

Inventors

  • RAO DESHENG
  • CHEN YUNFENG
  • Chen Ruoken
  • TANG NING

Assignees

  • 广东奇德新材料股份有限公司

Dates

Publication Date
20260505
Application Date
20260317

Claims (10)

  1. 1. A carbon fiber reinforced polyether-ether-ketone composite material is characterized by comprising, by weight, 58.1 parts to 78.1 parts of polyether-ether-ketone resin, 10 parts to 40 parts of surface modified carbon fibers, 0.1 part to 0.5 part of internal lubrication flow improver, 0.2 part to 0.5 part of compound antioxidant and 0.4 part to 1.2 parts of compound lubricant; The surface modified carbon fiber is prepared through oxidation treatment and sulfhydrylation treatment steps.
  2. 2. The carbon fiber reinforced polyetheretherketone composite of claim 1, wherein the surface modified carbon fiber is prepared by: (a) Adding 80mL of concentrated sulfuric acid into a three-neck flask of an ice water bath, sequentially adding 5g of sodium nitrate and 50g of carbon fiber base material, stirring at a low speed for 10min, slowly dripping 8g of potassium permanganate into the three-neck flask within 1h, soaking in the ice water bath for 1h, removing the ice water bath, heating to 40 ℃ to continue to react for 1.5h to fully oxidize the surface of the carbon fiber, slowly dripping 500mL of deionized water to terminate the reaction, adding 16mL of 30wt% hydrogen peroxide solution and 12mL of hydrochloric acid under low-speed stirring to remove redundant potassium permanganate and manganese dioxide, and finally repeatedly washing, filtering and drying by a large amount of deionized water to obtain a modified carbon fiber intermediate product with the surface rich in carboxyl and hydroxyl groups; (b) The sulfhydrylation treatment step comprises the steps of sequentially adding 200mL of deionized water and 30mL of HBr (40%) into a 500mL three-neck flask with a condenser tube, stirring at room temperature for 5 minutes, adding a pretreated modified carbon fiber intermediate product, heating to 80 ℃, adding 15g of thiourea, reacting at constant temperature for 20 hours, adding 10g of sodium hydroxide for neutralization after the reaction is finished, and carrying out ultrasonic washing and filtering to obtain the surface modified carbon fiber with the surface rich in sulfhydryl groups.
  3. 3. The carbon fiber reinforced polyether-ether-ketone composite material according to claim 2, wherein the ultrasonic washing adopts 40kHz ultrasonic waves, the washing solvent is a mixed solution of deionized water and ethanol, and the washing times are 3-5 times.
  4. 4. The carbon fiber reinforced polyether-ether-ketone composite material according to claim 1, wherein the compound lubricant is two or more of polyethylene wax, montan wax, ester wax and silicone.
  5. 5. The carbon fiber reinforced polyether-ether-ketone composite material according to claim 4, wherein the compound lubricant is prepared by compounding polyethylene wax and silicone powder according to a mass ratio of 1:1.
  6. 6. The carbon fiber reinforced polyether-ether-ketone composite material according to claim 1, wherein the compound antioxidant is two or more of GA-80, revonox 608,608 and S-9228.
  7. 7. The carbon fiber reinforced polyether-ether-ketone composite material according to claim 6, wherein the compound antioxidant is prepared by compounding GA-80 and S-9228 according to a mass ratio of 1:1.
  8. 8. The carbon fiber reinforced polyetheretherketone composite of claim 2, wherein the carbon fiber substrate is a T400, T700 or T800 chopped fiber.
  9. 9. A method of preparing a carbon fiber reinforced polyetheretherketone composite material according to any one of claims 1 to 8, comprising the steps of: 1) Drying polyether-ether-ketone resin at 120 ℃ for 4 hours, mixing the polyether-ether-ketone resin with a compound antioxidant, a compound lubricant and an internal lubrication flow improver in a high-speed mixer at room temperature, stirring for 5-10 minutes at the rotation speed of 400-600 rpm to uniformly disperse all the components, and obtaining a premix; 2) Adding the surface modified carbon fiber into a double-screw extruder through a side feeding device, adding premix into a main feeding port, controlling extrusion conditions to be that the length-diameter ratio is 48:1, the melting temperature is 345-385 ℃, the rotating speed of the main screw is 300-500 rpm, and the rotating speed of the side feeding screw is 20-100 rpm, so as to obtain an extruded material; 3) And (3) sequentially cooling, air-drying, granulating and sieving the extruded material to obtain the finished carbon fiber reinforced polyether-ether-ketone composite material.
  10. 10. The carbon fiber reinforced polyether-ether-ketone composite material according to claim 9, wherein the cooling is water-cooled or air-cooled, the cooling water temperature is 20-30 ℃, the cooling time is 1-3 minutes, the air drying is carried out by blowing air flow to remove surface moisture, the air speed is 2-5m/s, the granulating is carried out by adopting a rotary granulating cutter, the granulating length is 2-4mm, and the sieving is carried out by adopting a 20-40 mesh screen to remove overlong or overlong particles.

Description

Carbon fiber reinforced polyether-ether-ketone composite material and preparation method thereof Technical Field The invention relates to the technical field of carbon fiber reinforced polyether-ether-ketone composite materials, in particular to a carbon fiber reinforced polyether-ether-ketone composite material and a preparation method thereof. Background Carbon Fiber (CF) is a high performance Fiber material with Carbon content over 95%, and has the dual advantages of high strength and high modulus. The microstructure is formed by arranging flaky graphite microcrystals along the axial direction of the fiber, and the graphite material with a regular microcrystal structure is finally formed through carbonization and graphitization process treatment of an organic fiber precursor. The material perfectly combines the unique properties of 'outer softness and inner rigidity', namely, the density is only about half of that of aluminum, but the strength is far superior to that of steel, the intrinsic characteristics of the carbon material, such as high temperature resistance, corrosion resistance, high modulus and the like, are reserved, and the material has soft processability of textile fibers, and is known as a new generation of high-performance reinforcing fibers. The polyether-ether-ketone-based carbon fiber reinforced material has wide application prospect in high-end fields such as aerospace, high-end medical treatment, automobile industry and the like due to the excellent high temperature resistance, corrosion resistance, high strength and excellent mechanical properties. However, the current preparation and application of this material still faces the following core bottlenecks: the interface binding force is insufficient, namely the interface compatibility between the Carbon Fiber (CF) and the polyether-ether-ketone matrix is poor, so that the stress transmission efficiency is low, and the overall performance (such as strength and toughness) of the material cannot be fully exerted. Carbon Fiber (CF) as a high performance reinforcement with carbon content >95% has the characteristics of light weight, high strength, high modulus, corrosion resistance, ultra-high temperature resistance and the like, but the compounding of the carbon fiber and PEEK still has significant challenges. Current studies indicate that sizing agents are critical to improving CF/PEEK interfacial properties. However, the high melting temperature (> 340 ℃) and high viscosity of PEEK require processing temperatures exceeding 300 ℃, whereas conventional sizing agents such as commercially available epoxy, polyurethane and the like are prone to decomposition and failure during processing due to low heat resistance temperature, and cannot form stable interfaces, and other carbon fiber reinforced materials generally have the problems of low strength, high density and the like, and cannot fully exert the light weight advantages of carbon fibers. Therefore, developing a PEEK-based carbon fiber reinforced material with high interfacial bonding strength has become an urgent need to break through the industry technical barriers. Disclosure of Invention The invention aims to provide a carbon fiber reinforced polyether-ether-ketone composite material and a preparation method thereof, and aims to solve the problems in the background technology. In order to achieve the above purpose, the present invention provides the following technical solutions: A carbon fiber reinforced polyether-ether-ketone composite material comprises, by weight, 58.1-78.1 parts of polyether-ether-ketone resin, 10-40 parts of surface modified carbon fiber, 0.1-0.5 part of internal lubrication flow improver, 0.2-0.5 part of compound antioxidant and 0.4-1.2 parts of compound lubricant; The surface modified carbon fiber is prepared through oxidation treatment and sulfhydrylation treatment steps. Further, the surface-modified carbon fiber is prepared by the steps of: (a) Adding 80mL of concentrated sulfuric acid into a three-neck flask of an ice water bath, sequentially adding 5g of sodium nitrate and 50g of carbon fiber base material, stirring at a low speed for 10min, slowly dripping 8g of potassium permanganate into the three-neck flask within 1h, soaking in the ice water bath for 1h, removing the ice water bath, heating to 40 ℃ to continue to react for 1.5h to fully oxidize the surface of the carbon fiber, slowly dripping 500mL of deionized water to terminate the reaction, adding 16mL of 30wt% hydrogen peroxide solution and 12mL of hydrochloric acid under low-speed stirring to remove redundant potassium permanganate and manganese dioxide, and finally repeatedly washing, filtering and drying by a large amount of deionized water to obtain a modified carbon fiber intermediate product with the surface rich in carboxyl and hydroxyl groups; (b) The sulfhydrylation treatment step comprises the steps of sequentially adding 200mL of deionized water and 30mL of HBr (40%) into a 500mL th