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CN-122011726-A - Glass fiber reinforced PEEK composite material and preparation method thereof

CN122011726ACN 122011726 ACN122011726 ACN 122011726ACN-122011726-A

Abstract

The invention discloses a glass fiber reinforced PEEK composite material and a preparation method thereof, wherein the material comprises, by mass, 60% -80% of PEEK resin, 20% -35% of chopped glass fibers, 1% -5% of hyperbranched polyaryletherketone copolymer, 0.5% -2% of silane coupling agent, 0.2% -1% of antioxidant and 1% -3% of lubricant. According to the invention, hyperbranched polyaryletherketone copolymer (with the number average molecular weight of 5000-20000 and the branching degree of 0.6-0.8) is added, and the silane coupling agent and the optimization process are matched, so that the prepared GF/PEEK composite material has the bending fatigue life of more than or equal to 2.1X107 times, the tensile strength of more than or equal to 158MPa, the bending modulus of more than or equal to 8.5GPa, and excellent comprehensive performance, and different functional formulas (wear resistance, high rigidity and heat conduction) can meet the requirements of specific scenes.

Inventors

  • GUO HONGWU
  • GAO ZHENXING

Assignees

  • 合肥圆燃新材料有限公司

Dates

Publication Date
20260512
Application Date
20260313

Claims (10)

  1. 1. The glass fiber reinforced PEEK composite material is characterized by comprising, by mass, 60% -80% of PEEK resin, 20% -35% of chopped glass fibers, 1% -5% of hyperbranched polyaryletherketone copolymer, 0.5% -2% of silane coupling agent, 0.2% -1% of antioxidant and 1% -3% of lubricant.
  2. 2. The glass fiber reinforced PEEK of claim 1, wherein the PEEK resin is in powder form with the particle size of 10-50 μm, and the water content is less than or equal to 0.02% after drying treatment before processing.
  3. 3. The glass fiber reinforced PEEK of claim 1, wherein the chopped glass fibers have a length of 3-5mm, and the surface is pretreated with a silane coupling agent, wherein the silane coupling agent is KH-602 or KH-550.
  4. 4. The glass fiber reinforced PEEK of claim 1, wherein the hyperbranched polyaryletherketone copolymer has a number average molecular weight ranging from 5000 to 20000 and a branching degree ranging from 0.6 to 0.8.
  5. 5. The glass fiber reinforced PEEK according to claim 1, wherein the antioxidant is a compound of antioxidants 168 and 1098 or an antioxidant S-9228, the lubricant is polytetrafluoroethylene, and when the wear resistance is required to be improved, the mass percentage of the lubricant is adjusted to 10%.
  6. 6. A method of preparing a glass fiber reinforced PEEK composite according to any one of claims 1-5, comprising the steps of: S1, raw material pretreatment, namely drying PEEK resin for 4-8 hours at 140-160 ℃, controlling the water content to be less than or equal to 0.02%, soaking chopped glass fibers in 1% by mass of aqueous solution of a silane coupling agent for 30 minutes, and drying for 2 hours at 120 ℃; s1, premixing, namely adding the dried PEEK resin, the hyperbranched polyaryletherketone copolymer, the antioxidant and the lubricant into a high-speed mixer according to a proportion, and mixing for 10-20 minutes at the temperature of 80 ℃ and the rotating speed of 700-900r/min to obtain a premix; S2, melt blending extrusion, namely adding premix through a main feeding port of a double-screw extruder, adding pretreated chopped glass fibers through a side feeding port, controlling the temperature of each region of the extruder to be 335-350 ℃, 360-390 ℃ from two regions to four regions, 360-380 ℃ from five regions to eight regions, 355-380 ℃ of a machine head, and cutting the extruded material into granules after cooling, wherein the screw speed is 180-220r/min, the melt pressure is 15-20 MPa; s3, post-treatment, namely drying the granulated particles at 110-130 ℃ for 3-5 hours to obtain the glass fiber reinforced PEEK composite particles.
  7. 7. The method for preparing the glass fiber reinforced PEEK composite material according to claim 6, wherein the drying temperature of the PEEK resin in S1 is 150 ℃, the drying time is 6 hours, and the silane coupling agent of the chopped glass fiber is KH-602.
  8. 8. The preparation method of the glass fiber reinforced PEEK composite material according to claim 6, wherein the rotating speed of the high-speed mixer in S2 is 800r/min, the mixing time is 15 minutes, and the hyperbranched polyaryletherketone copolymer is ensured to be uniformly dispersed in PEEK resin.
  9. 9. The preparation method of the glass fiber reinforced PEEK composite material according to claim 6, wherein the length-diameter ratio of the double-screw extruder in the step S3 is 40:1, the temperature fluctuation of each zone is less than or equal to +/-5 ℃, the screw rotating speed is less than or equal to 250r/min, and the retention length of glass fibers in the composite material is more than or equal to 1mm.
  10. 10. The preparation method of the glass fiber reinforced PEEK composite material according to claim 6, wherein the cooling mode of the material strips in the step S3 is water cooling, the cooling water temperature is controlled to be 20-30 ℃, the grain cutting length is 2-4mm, the post-treatment drying temperature is 120 ℃, and the drying time is 4 hours.

Description

Glass fiber reinforced PEEK composite material and preparation method thereof Technical Field The invention relates to the field of PEEK (polyether-ether-ketone) materials, in particular to a glass fiber reinforced PEEK composite material and a preparation method thereof. Background Polyether ether ketone (PEEK) is used as high-performance special engineering plastic, has excellent high-temperature resistance (the long-term use temperature is more than 250 ℃), chemical corrosion resistance, high mechanical strength and biocompatibility, and has irreplaceable value in the field of high-end manufacturing. In order to further improve the strength, rigidity and dimensional stability, glass Fiber (GF) is generally adopted in the industry for reinforcement and modification to form a glass fiber reinforced PEEK (GF/PEEK) composite material. However, the existing GF/PEEK composite material has the core technical problems that a PEEK matrix is a nonpolar semi-crystalline polymer, the surface of glass fiber contains polar hydroxyl groups, the interfacial compatibility of the PEEK matrix and the glass fiber is poor, and the binding force between the fiber and the matrix is weak. The traditional solution mainly relies on silane coupling agents (such as KH-550 and KH-602) to carry out surface treatment on glass fibers, but the coupling agents can only connect the fibers and the matrix through physical adsorption or weakening chemical action, and the interface bonding strength is limited. Under long-term dynamic load, microcracks are easy to generate at the interface, the fibers are easily debonded and pulled out, and finally, the bending fatigue performance of the composite material is insufficient, the bending fatigue life of the GF/PEEK composite material prepared by the prior art is usually less than or equal to 10 7 times under the conditions of 80MPa of bending stress and 10Hz of frequency, the tensile strength is less than or equal to 120MPa, the bending modulus is less than or equal to 6GPa, and the long-term use requirements of core components such as aeroengine brackets, medical instrument joint members and the like are difficult to be met. In addition, some prior art attempts to add common copolymer as compatilizer, but the compatilizer has low matching degree with PEEK matrix structure, poor dispersibility, easy agglomeration, not only can not effectively improve interface combination, but also can possibly degrade mechanical property of materials, meanwhile, PEEK melt has high viscosity, and the traditional formula has insufficient fluidity in the processing process, thus easily causing equipment abrasion and product forming defects (such as material shortage and air bubbles) and further limiting the application range. Disclosure of Invention The invention aims to provide a glass fiber reinforced PEEK composite material and a preparation method thereof, which are used for solving the technical problems in the background technology. The technical scheme of the invention provides a glass fiber reinforced PEEK composite material, which comprises, by mass, 60% -80% of PEEK resin, 20% -35% of chopped glass fiber, 1% -5% of hyperbranched polyaryletherketone copolymer, 0.5% -2% of silane coupling agent, 0.2% -1% of antioxidant and 1% -3% of lubricant, wherein the bending fatigue life of the composite material under the conditions of 80MPa of bending stress and 10Hz of frequency is more than or equal to 2X 10 7 times, the tensile strength is more than or equal to 150MPa, and the bending modulus is more than or equal to 8GPa. In a preferred embodiment, the PEEK resin is in the form of powder with the particle size of 10-50 μm, and the water content after drying treatment is less than or equal to 0.02%. In a preferred embodiment, the chopped glass fibers have a length of 3-5mm and the surfaces are pretreated with a silane coupling agent, which is KH-602 or KH-550. In a preferred embodiment, the hyperbranched polyaryletherketone copolymer has a number average molecular weight of 5000-20000 and a branching degree of 0.6-0.8, and the hydroxyl end groups thereof form hydrogen bonding with the PEEK matrix, and the aromatic end rings react chemically with the hydroxyl groups on the surface of the glass fiber. In a preferred embodiment, the antioxidant is a compound of antioxidants 168 and 1098 or an antioxidant S-9228, and the lubricant is polytetrafluoroethylene, and when the wear resistance is required to be improved, the mass percentage of the lubricant is adjusted to 10%. A preparation method of a glass fiber reinforced PEEK composite material comprises the following steps: S1, raw material pretreatment, namely drying PEEK resin for 4-8 hours at 140-160 ℃, controlling the water content to be less than or equal to 0.02%, soaking chopped glass fibers in 1% by mass of aqueous solution of a silane coupling agent for 30 minutes, and drying for 2 hours at 120 ℃; s1, premixing, namely adding the dried PEEK resin, the hyperbran