CN109826013B - Nano-material-reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent and preparation method and application thereof - Google Patents
Nano-material-reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a nano-material reinforced high-temperature resistant carbon fiber thermoplastic sizing agent, a preparation method and application thereof, wherein the sizing agent comprises the following components: 0-15% of nano material, 0.1-10% of PAIK and the balance of strong polar solvent in percentage by weight of the sizing agent; when in use, the carbon fiber is ultrasonically dipped in the sizing agent and then is dried. The invention solves the problem that the existing sizing agent is not suitable for preparing high-performance thermoplastic resin matrix composite materials due to low decomposition temperature, can improve the wettability of carbon fibers and high-performance thermoplastic resin, and improve the interface strength between a base material and the carbon fibers in the composite materials, and has the advantages of simple operation, convenient use, green and environment-friendly preparation process and no environmental pollution.
Description
Technical Field
The invention belongs to the technical field of carbon fiber composite materials, and particularly relates to a high-temperature-resistant carbon fiber thermoplastic sizing agent reinforced by a nano material, and a preparation method and application thereof.
Background
The carbon fiber has smooth surface and chemical inertness, which generally causes poor bonding property between the carbon fiber and a matrix material, and the sizing agent can play a role of a bridge, transfer load and exert the excellent property of the carbon fiber to the maximum. In addition, since carbon fibers are liable to have phenomena of monofilament breakage, fuzz, and the like due to their brittleness during production, spinning, and transportation, the fibers are usually subjected to sizing treatment in actual production to suppress these defects.
At present, most carbon fiber products adopt thermosetting sizing agents, and are not suitable for preparing thermoplastic resin matrix composite materials. Compared with thermosetting resin, the thermoplastic resin has more advantages such as easy recovery, low density, high toughness, convenient transportation, long storage time, short production period and the like, and is widely applied to the fields of aerospace, automobiles, medical instruments, sports instruments and the like.
Generally, the processing temperature of the high-performance thermoplastic resin is more than 300-400 ℃, the thermosetting sizing agent can be degraded when the temperature exceeds 250 ℃, and degraded substances remain on the surface of the fiber, so that the interface bonding degree between the carbon fiber and the thermoplastic resin is seriously influenced, the product is easy to have defects, and the mechanical property is reduced. The common thermoplastic sizing agent mainly aims at thermoplastic matrixes such as Polyurethane (PU), polypropylene (PP), Polyamide (PA) and the like, the degradation temperature (180-250 ℃) is far lower than the processing temperature (280-400 ℃) of high-performance thermoplastic resin, and the mechanical property of the composite material is easily reduced. The research on the high-temperature resistant sizing agent suitable for the high-performance thermoplastic resin is not reported.
Disclosure of Invention
In view of the above, the present invention provides a nanomaterial-reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent, a preparation method and an application thereof, aiming at the above defects of the existing sizing agent and the requirements of the preparation of high-performance thermoplastic resin-based composite materials, which can effectively improve the bonding performance of carbon fibers and a high-performance thermoplastic matrix, and has stable state and difficult degradation under high-temperature processing conditions.
In order to achieve the above object, the first aspect of the present invention provides a nanomaterial-reinforced refractory carbon fiber thermoplastic sizing agent, comprising: 0-15% of nano material, 0.1-10% of PAIK and the balance of strong polar solvent in percentage by weight of the sizing agent; the structural formula of PAIK is as follows:
wherein n is a positive integer.
Preferably, the nano material comprises one or more of Carbon Nano Tube (CNT) and its derivatives, Graphene Oxide (GO) and its derivatives, nano carbon black and its derivatives, and nano silicon dioxide and its derivatives.
Preferably, the strongly polar solvent comprises one or more of dimethyl sulfoxide (DMSO), methanol, Dimethylformamide (DMF), acetic acid, ethanol, and Tetrahydrofuran (THF).
The second aspect of the present invention provides a preparation method of the nanomaterial-reinforced high temperature resistant carbon fiber thermoplastic sizing agent, comprising the steps of: adding 4-hydroxyindole and 4, 4' -difluorobenzophenone in equimolar amount to the reactionAdding solvent, water-carrying agent and catalyst anhydrous K into the container2CO3Heating to 155-165 ℃ in an inert gas environment for reaction for 5.5-6.5 h, then heating to 180-190 ℃ for reaction for 7.5-8.5 h, cleaning reaction liquid after the reaction is finished, filtering and drying in vacuum to obtain PAIK; and then PAIK is dissolved in a strong polar solvent according to the proportion, and the nano material is added for ultrasonic treatment.
The third aspect of the invention provides an application of the nanomaterial-reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent, wherein the sizing agent is used for preparing a high-performance thermoplastic resin-based carbon fiber composite material, and the preparation steps comprise:
s1, putting the carbon fibers into a nano-material reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent, and carrying out ultrasonic impregnation and drying to obtain sized carbon fibers;
and S2, compounding the sized carbon fibers and a high-performance thermoplastic resin base material to obtain the composite material.
Preferably, in step S1, before the carbon fiber is sized, the carbon fiber is subjected to surface modification and then is sized; the surface modification mode comprises the following steps: introducing one or more of hydroxyl, carboxyl, sulfonic group, nitro and amino on the surface of the carbon fiber.
More preferably, in step S1, the carbon fiber is subjected to surface modification after desizing.
Further preferably, in step S1, the desizing method includes: and (3) desizing by adopting organic solvent treatment or high-temperature treatment.
Preferably, in step S2, the high performance thermoplastic resin includes one or more of Polyetheretherketone (PEEK), polyphenylene sulfide (PPS), Polysulfone (PSF), Polyimide (PI), and Polyarylate (PAR).
Preferably, in step S2, the compounding method includes the steps of: spraying high-performance thermoplastic resin on the surface of the sized carbon fiber, baking at 280-400 ℃ to obtain carbon fiber prepreg, stacking the carbon fiber prepreg, heating to 280-400 ℃, pressurizing, maintaining pressure, cooling under the action of pressure, and demolding to obtain the composite material.
Compared with the prior art, the invention has the beneficial effects that:
the high-temperature-resistant sizing agent is synthesized mainly through reaction, is suitable for a high-performance thermoplastic resin-based carbon fiber composite material, and can effectively improve the interface bonding strength of carbon fibers and a high-performance thermoplastic matrix and enhance the mechanical property of the composite material. And secondly, the degradation temperature of the sizing agent reaches more than 500 ℃, which is far higher than the processing temperature of the high-performance thermoplastic resin, so that the reduction of the performance caused by the increase of porosity due to the decomposition of the sizing agent in the processing of the thermoplastic resin can be avoided.
Drawings
FIG. 1 is a thermogravimetric analysis curve of PAIK obtained in example 1.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited to the following specific examples.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The embodiment provides a high-temperature-resistant carbon fiber thermoplastic sizing agent reinforced by a nano material and a preparation method thereof, and the obtained sizing agent is used for preparing a high-performance thermoplastic resin-based carbon fiber composite material. Specifically, in the embodiment, Graphene Oxide (GO) is used as a nano material, dimethyl sulfoxide (DMSO) is used as an organic solvent, polyether ether ketone (PEEK) is used as a high-performance thermoplastic resin base material, plain woven carbon fibers are used as a fiber fabric, and sodium sulfonate (-SO) is introduced to the carbon fibers3Na) is specifically carried out as follows:
(1) synthesis of PAIK: the reaction equation for the synthesis of PAIK is as follows:
wherein n is a positive integer.
The PAIK synthesis process comprises the following steps: adding 4-hydroxyindole, 4' -difluorobenzophenone with equal molar mass, dimethyl sulfoxide (DMSO) serving as a reaction solvent, toluene serving as a water-carrying agent and anhydrous K serving as a catalyst into a reaction kettle2CO3The solid-to-liquid ratio was 30% W/V. In N2Heating to 160 ℃ under the environment for reaction for 6h, heating to 185 ℃ for reaction for 8h, then washing the reaction liquid with deionized water and acetone for a plurality of times, filtering and drying in vacuum to obtain the needed PAIK. The obtained PAIK thermogravimetric analysis curve is shown in FIG. 1, the initial thermal decomposition temperature is 510 ℃, the processing temperature is higher than that of the high-performance thermoplastic resin, and the thermal stability is good.
(2) Preparing a sizing agent: PAIK is dissolved in dimethyl sulfoxide (DMSO) with the concentration of 1%, 10 wt% of Graphene Oxide (GO) is added, and ultrasonic treatment is adopted to fully dissolve and disperse uniformly.
(3) Sizing treatment: introducing sodium sulfonate (-SO) into the multilayer through high-temperature desizing treatment and modification3Na) is put into the sizing agent, and the plain woven carbon fiber is ultrasonically dipped for 2h and then dried.
(4) Preparing a composite material: and (3) uniformly spraying polyether ether ketone (PEEK) powder on the front surface and the back surface of the carbon fiber by adopting an electrostatic powder spraying process, and baking the carbon fiber in an oven at 380 ℃ for 5-10 min to obtain the carbon fiber prepreg. And (3) stacking the prepreg products in a hot press at a required angle, heating to 380 ℃, applying 5MPa pressure, maintaining the pressure for 20min, cooling to room temperature under the action of pressure, and demolding to obtain the high-performance thermoplastic composite material.
The prepared high-performance thermoplastic composite material is subjected to performance test, the tensile strength is 640MPa, the interlaminar shear strength can reach 90MPa, and the interlaminar shear strength is improved by 80% compared with that of the composite material without sizing.
Example 2
The embodiment provides a nano-material reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent and a preparation method thereofThe obtained sizing agent is used for preparing the high-performance thermoplastic resin-based carbon fiber composite material. Specifically, in this embodiment, Carbon Nanotubes (CNTs) are used as the nanomaterial, Dimethylformamide (DMF) is used as the organic solvent, polyphenylene sulfide (PPS) is used as the high performance thermoplastic resin substrate, plain weave carbon fibers are used as the fiber fabric, and amino groups (-NH) are introduced to the carbon fibers2) The specific process is as follows:
(1) synthesis of PAIK: adding 4-hydroxyindole, 4' -difluorobenzophenone with equal molar mass, dimethyl sulfoxide (DMSO) serving as a reaction solvent, toluene serving as a water-carrying agent and anhydrous K serving as a catalyst into a reaction kettle2CO3The solid-to-liquid ratio was 30% W/V. In N2Heating to 158 ℃ under the environment for reaction for 6.5h, heating to 180 ℃ for reaction for 8.5h, then washing the reaction liquid with deionized water and acetone for several times, filtering and drying in vacuum to obtain the needed PAIK. The PAIK has initial thermal decomposition temperature higher than the processing temperature of high-performance thermoplastic resin and good thermal stability.
(2) Preparing a sizing agent: PAIK was dissolved in DMF at a concentration of 5% and 3 wt% Carbon Nanotubes (CNT) were added and sonicated to fully dissolve and disperse uniformly.
(3) Sizing treatment: introducing amino (-NH) into the multilayer by high-temperature desizing treatment and modification2) And then placing the plain woven carbon fiber into the sizing agent, ultrasonically dipping for 2h, and drying.
(4) Preparing a composite material: and (3) uniformly spraying polyphenylene sulfide (PPS) powder on the front and back surfaces of the carbon fiber by adopting an electrostatic powder spraying process, and baking the carbon fiber in an oven at 380 ℃ for 8min to obtain the carbon fiber prepreg. And (3) stacking the prepreg products in a hot press at a required angle, heating to 380 ℃, applying 5MPa pressure, maintaining the pressure for 20min, cooling to room temperature under the action of pressure, and demolding to obtain the high-performance thermoplastic composite material. The performance test of the prepared high-performance thermoplastic composite material is improved by 81 percent compared with that of the composite material without sizing, and is basically consistent with that of the embodiment 1.
Example 3
The embodiment provides a high-temperature-resistant carbon fiber thermoplastic sizing agent reinforced by a nano material and a preparation method thereof, and the obtained sizing agent is used for preparing a high-performance thermoplastic resin-based carbon fiber composite material. Specifically, in this embodiment, the nano-silica is used as a nano-material, the organic solvent is Tetrahydrofuran (THF), the Polyimide (PI) is used as a high-performance thermoplastic resin substrate, the plain weave carbon fiber is used as a fiber fabric, and a carboxyl group (-COOH) is introduced to the carbon fiber, and the specific process is as follows:
(1) synthesis of PAIK: adding 4-hydroxyindole, 4' -difluorobenzophenone with equal molar mass, dimethyl sulfoxide (DMSO) serving as a reaction solvent, toluene serving as a water-carrying agent and anhydrous K serving as a catalyst into a reaction kettle2CO3The solid-to-liquid ratio was 30% W/V. In N2Heating to 165 ℃ in the environment for reaction for 5.5h, heating to 187 ℃ for reaction for 7.5h, then washing the reaction liquid with deionized water and acetone for a plurality of times, filtering and drying in vacuum to obtain the needed PAIK. The PAIK has initial thermal decomposition temperature higher than the processing temperature of high-performance thermoplastic resin and good thermal stability.
(2) Preparing a sizing agent: PAIK was dissolved in THF at a concentration of 2% and 12 wt% nano-silica was added and sonicated to dissolve and disperse well.
(3) Sizing treatment: and (3) placing the multilayer plain woven carbon fiber subjected to high-temperature desizing treatment and modification to introduce carboxyl (-COOH) into the sizing agent, ultrasonically dipping for 2h, and drying.
(4) Preparing a composite material: and uniformly spraying Polyimide (PI) powder on the front and back surfaces of the carbon fiber by adopting an electrostatic powder spraying process, and baking in an oven at 380 ℃ for 8min to obtain the carbon fiber prepreg. And (3) stacking the prepreg products in a hot press at a required angle, heating to 380 ℃, applying 5MPa pressure, maintaining the pressure for 20min, cooling to room temperature under the action of pressure, and demolding to obtain the high-performance thermoplastic composite material. The performance test of the prepared high-performance thermoplastic composite material is improved by 78 percent compared with that of the composite material without sizing, and the performance is basically consistent with that of the composite material in the embodiment 1.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention. It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (4)
1. A method for preparing a high-performance thermoplastic resin-based carbon fiber composite material by adopting a nano-material-reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent is characterized by comprising the following steps of: the preparation method comprises the following steps:
s1, carrying out surface modification on carbon fibers, putting the modified carbon fibers into a nano-material reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent, carrying out ultrasonic impregnation and drying to obtain sized carbon fibers; the components of the nanomaterial reinforced high-temperature-resistant carbon fiber thermoplastic sizing agent comprise: 0-15% of nano material, 0.1-10% of PAIK and the balance of strong polar solvent in percentage by weight of the sizing agent; the structural formula of PAIK is as follows:
wherein n is a positive integer, the nano-material reinforced high-temperature resistant carbon fiber thermoplastic sizing agent is prepared by adding 4-hydroxyindole and 4, 4' -difluorobenzophenone with equal molar mass into a reaction vessel, and continuously adding a solvent, a water-carrying agent and a catalyst anhydrous K2CO3Heating to 155-165 ℃ in an inert gas environment for reaction for 5.5-6.5 h, then heating to 180-190 ℃ for reaction for 7.5-8.5 h, cleaning reaction liquid after the reaction is finished, filtering and drying in vacuum to obtain PAIK; then PAIK is dissolved in a strong polar solvent according to the proportion, and nano materials are added to be processed by ultrasonic treatment; the nano material comprises one or more of carbon nano tube and derivatives thereof, graphene oxide and derivatives thereof, nano carbon black and derivatives thereof, and nano silicon dioxide and derivatives thereof, and the strong polar solvent comprises dimethyl sulfoxide, methanol, dimethyl sulfoxide, and dimethyl sulfoxideOne or more of methylformamide, acetic acid, ethanol and tetrahydrofuran;
s2, spraying high-performance thermoplastic resin on the surface of the sized carbon fiber, baking at 280-400 ℃ to obtain carbon fiber prepreg, stacking the carbon fiber prepreg, heating to 280-400 ℃, pressurizing, maintaining pressure, cooling under the action of pressure, and demolding to obtain the composite material, wherein the high-performance thermoplastic resin comprises one or more of polyether ether ketone, polyphenylene sulfide, polysulfone, polyimide and polyarylate.
2. The method of claim 1, wherein: the surface modification mode comprises the following steps: introducing one or more of hydroxyl, carboxyl, sulfonic group, nitro and amino on the surface of the carbon fiber.
3. The method of claim 1, wherein: in step S1, the carbon fibers are desized and then subjected to surface modification.
4. The method of claim 3, wherein: in step S1, the desizing method includes: and (3) desizing by adopting organic solvent treatment or high-temperature treatment.
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