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Method for performing surface modification on reinforcing fiber by using crystalline polyaryletherketone sizing agent

A polyaryletherketone and reinforced fiber technology, which is applied in the direction of carbon fiber, fiber treatment, fiber type, etc., can solve the problems of powder and fiber bundles not having adhesive force, PEEK melt viscosity is high, and thermal decomposition temperature is low, etc., to achieve Meet the needs of different composite materials, mild post-treatment means, and the effect of a large molecular weight range

Active Publication Date: 2020-03-27
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The PEEK powder in the patent does not have the two functions of shaping the fiber bundles and protecting the fiber sizing agent, and the powder and the fiber bundles do not have cohesive force, which will easily cause the powder to fall off, pollute the environment and fail, and because of the high viscosity of the PEEK melt , the powder has limited wettability to fibers during processing
In addition, the alkylphenol polyvinyl ether used is not suitable for the PEEK composite material system because the thermal decomposition temperature is lower than the processing temperature of the PEEK composite material

Method used

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  • Method for performing surface modification on reinforcing fiber by using crystalline polyaryletherketone sizing agent
  • Method for performing surface modification on reinforcing fiber by using crystalline polyaryletherketone sizing agent
  • Method for performing surface modification on reinforcing fiber by using crystalline polyaryletherketone sizing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Dissolve 2.5g of ketimine polyetheretherketone (number-average molecular weight: 2000g / mol) in 997.5mL of NMP, and place it in a sizing tank with an effective stroke of 1m after it is completely dissolved. The carbon fiber bundles are subjected to sizing treatment; the carbon fibers after preliminary sizing are dried in NMP at 230°C in a resistance wire evaporator; the fiber bundles from which the solvent has been removed are introduced into a hydrolysis tank with 0.1mol / L dilute sulfuric acid for acidification treatment for 2 hours, and obtained after hydrolysis Carbon fiber bundles sized with crystalline polyether ether ketone, the carbon fiber bundles are dried at 150° C. and then wound up to obtain carbon fibers sized with crystalline polyether ether ketone. The surface morphology of carbon fiber before and after sizing is as follows: figure 1 As shown, its IFSS with PEEK is 60MPa, which is 100% higher than that of unsized carbon fiber (30MPa) (IFSS test curve see ...

Embodiment 2

[0042] Dissolve 10g of ketimine polyetheretherketoneketone (number-average molecular weight 4000g / mol) in 1040mL of DMF, slowly add 0.25g of carbon nanotubes under ultrasonic vibration conditions after complete dissolution, and place them in an effective stroke of 10mm after fully dispersed In the sizing tank, sizing treatment is performed on the carbon fiber bundles that have been washed off the sizing agent (the method of removing the sizing agent is ultrasonic washing with acetone for 48 hours) at a rate of 1 mm / min; the carbon fibers after preliminary sizing are heated in a resistance wire evaporator at 200 ° C Dry the DMF; the fiber bundles from which the solvent has been removed are introduced into a hydrolysis tank equipped with 0.9mol / L dilute sulfuric acid for acidification treatment for 2 hours, and after hydrolysis, crystalline polyetheretherketoneketone sized carbon fiber bundles are obtained. Winding after drying to obtain crystalline polyether ether ketone sized c...

Embodiment 3

[0044] Dissolve 10g of ketimine polyetherketone (number-average molecular weight 6000g / mol) in 1060mL of DMF, slowly add 0.5g of acidified carbon nanotubes under ultrasonic conditions after it is completely dissolved, and place it in a sizing machine with an effective stroke of 1m In the tank, the unsized basalt fiber was sized at a rate of 100 mm / min; the basalt fiber after preliminary sizing was dried in an infrared heating evaporator at 210 ° C; Acidification treatment in a hydrolysis tank with L dilute hydrochloric acid for 2 hours, after hydrolysis, basalt fiber bundles sized with crystalline polyetherketone were obtained, and the basalt fiber bundles were dried at 150°C and rolled up to obtain basalt fibers sized with crystalline polyetherketone . Its IFSS with PEEK is 78MPa, a 160% increase compared to unsized basalt fiber (31MPa).

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Abstract

The invention discloses a method for performing surface modification on a reinforcing fiber by using a crystalline polyaryletherketone sizing agent, and belongs to the technical field of reinforcing fiber surface treatment. A soluble polyaryletherketone precursor is configured as a solution, an interface reinforcing filler is added under the ultrasonic oscillation condition to prepare the solublepolyaryletherketone sizing agent, and the soluble polyaryletherketone sizing agent is placed in a sizing tank; after the sizing agent is used for sizing the reinforcing fiber, a solvent is dried by evaporation to enable the soluble polyarylether precursor to be uniformly adhered to the surface of the reinforcing fiber, and then the precursor on the surface of the reinforcing fiber generates a hydrolysis reaction under the acidic condition and is converted into polyaryletherketone with the crystallinity, the heat resistance and the insolubility in the organic solvent; and finally, water is evaporated to obtain the reinforcing fiber modified by the crystalline polyaryletherketone sizing agent. When the modified reinforcing fiber is used for reinforcing PEEK resin, the interfacial shear strength (IFSS) of a composite material is remarkably improved (267%) compared with an unsized carbon fiber, and the modified reinforcing fiber is solvent-resistant and can be used at the high temperature.

Description

technical field [0001] The invention belongs to the technical field of reinforcement fiber surface treatment, and in particular relates to a method for surface modification of reinforcement fibers by using a crystalline polyaryletherketone sizing agent. Background technique [0002] Resin-based composites are widely used in various fields due to their light weight, excellent mechanical properties and designability. With the development of aerospace and national defense, traditional resin-based composite materials have been difficult to meet the requirements of high-temperature, high-strength and corrosive environments. Therefore, special engineering plastic-based composite materials represented by polyether ether ketone (PEEK) resin The application is more and more extensive. However, due to the molecular structure characteristics of polyetheretherketone, it is difficult to produce a strong interaction with the reinforcing fiber, resulting in a lower interfacial shear stren...

Claims

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Application Information

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IPC IPC(8): D06M15/41C08L61/16C08J5/06C08J5/08C03C25/32D06M101/40D06M101/36
CPCC03C25/32C08J5/06C08J5/08C08J2361/16D06M15/41D06M2101/36D06M2101/40D06M2200/40
Inventor 王贵宾陈卓奇杨砚超栾加双王天娇王晟道丛鑫张淑玲
Owner JILIN UNIV
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