CN110117406B - Method for preparing aramid fiber III nano-coated fiber reinforced composite material - Google Patents

Method for preparing aramid fiber III nano-coated fiber reinforced composite material Download PDF

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CN110117406B
CN110117406B CN201910294914.6A CN201910294914A CN110117406B CN 110117406 B CN110117406 B CN 110117406B CN 201910294914 A CN201910294914 A CN 201910294914A CN 110117406 B CN110117406 B CN 110117406B
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aramid
iii
fiber
nano
pan
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CN110117406A (en
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樊威
田荟霞
王红红
于洋
杨雪
孟雪
张涛
于希晨
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Xian Polytechnic University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/04Reinforcing macromolecular compounds with loose or coherent fibrous material
    • C08J5/046Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/34Core-skin structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/08Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyacrylonitrile as constituent
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2363/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2433/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/18Homopolymers or copolymers of nitriles
    • C08J2433/20Homopolymers or copolymers of acrylonitrile
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2477/00Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
    • C08J2477/10Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids

Abstract

The invention discloses a method for preparing aramid fiber III nano-coated fiber reinforced composite material, which comprises the steps of pretreating aramid fiber III, carrying out plasma surface treatment on the pretreated aramid fiber III, preparing a mixed solution of PAN and N-N dimethylformamide as a spinning solution, taking the aramid fiber III subjected to the plasma surface treatment as a core layer, preparing PAN-aramid fiber III nano-coated fiber by using an electrostatic spinning parallel electrode method, treating the PAN-aramid fiber III nano-coated fiber with ethanol, drying the dried PAN-aramid fiber III nano-coated fiber and curing the PAN-aramid fiber III nano-coated fiber reinforced epoxy resin composite material with an epoxy resin matrix to obtain the PAN-aramid fiber III nano-coated fiber reinforced epoxy resin composite material. The prepared nano-coated fiber with the sheath-core structure has the advantages of porous nano effect and material characteristics, has the characteristics of high porosity and specific surface area of the sheath-layer nano fiber and excellent mechanical property of the core-layer aramid fiber, and solves the problem of poor interfacial adhesion of the aramid fiber and epoxy resin composite material in the prior art.

Description

Method for preparing aramid fiber III nano-coated fiber reinforced composite material
Technical Field
The invention belongs to the technical field of fiber reinforced composite materials, and relates to a method for preparing an aramid fiber III nano-coated fiber reinforced composite material.
Background
With the continuous progress of scientific technology and the rapid development of social economy, particularly the rapid advance of advanced science and technology, more, tighter and higher requirements are put forward on the performance of materials, the traditional single-performance materials cannot meet the actual requirements in many aspects, and the textile materials with common structures cannot meet the higher requirements in the fields of aviation, aerospace, automobiles, buildings, medical appliances and the like any more. Therefore, in the recent decades, a large number of novel textile materials with complex structures have appeared, and have exerted unique advantages in various fields.
The compounding of materials is a great trend and trend of the development of modern material science and engineering, and is also an important direction of the development of new material technology. As a novel material, the composite material can greatly improve the defect problem of a single material, so that the composite material is widely applied to various fields such as aerospace, national defense and military industry, land transportation, building, civil engineering and the like. In modern composite materials, compared with other reinforced composite materials, fiber reinforced resin-based composite materials are more perfect in development and most widely applied, and have the advantages of high specific strength, large specific stiffness, good damping property, long fatigue life, designability of mechanical property, good forming process performance, multiple material varieties and the like, and are more and more highly regarded by the aerospace industry at home and abroad.
The resin-based composite material adopts various reinforcing materials, mainly comprising glass fiber, aramid fiber, carbon fiber, ultra-high molecular weight polyethylene fiber and the like. Aramid fiber reinforced resin matrix composite materials among a plurality of reinforced materials are widely applied to various fields of aerospace, military, machinery, automobiles, electronics and electricity and the like because of having various excellent properties such as high specific strength, large specific modulus, corrosion resistance, high temperature resistance and the like, and particularly show more and more important functions in structural materials in the aerospace field. However, as can be seen from the structure of the aramid fiber III, the surface of the aramid fiber III is lack of active groups, so that the interface bonding strength between the aramid fiber III and a resin matrix is low, the interlaminar shear performance is poor, and the exertion of the mechanical properties of the aramid fiber III and resin matrix composite is finally influenced, so that the application of the aramid fiber III reinforced composite is greatly limited.
Disclosure of Invention
The invention aims to provide a method for preparing an aramid III nano-coated fiber reinforced composite material, which solves the problem of poor interface adhesion of aramid III fibers and epoxy resin composite materials in the prior art.
The technical scheme adopted by the invention is that the method for preparing the aramid fiber III nano-coated fiber reinforced composite material specifically comprises the following steps:
Step 1, pretreating aramid fiber III;
step 2, placing the aramid III fiber obtained in the step 1 in a plasma surface treatment device for plasma surface treatment;
step 3, preparing a mixed solution of PAN and N-N dimethylformamide;
step 4, taking the aramid fiber III obtained in the step 2 as a core layer, taking the mixed solution obtained in the step 3 as a spinning solution, and preparing PAN-aramid fiber III nano-coated fiber by using an electrostatic spinning parallel electrode method;
step 5, rinsing the PAN-aramid III nano-coated fiber obtained in the step 4 by using an ethanol solution, and then drying for later use;
and 6, curing the PAN-aramid III nano-coated fiber obtained in the step 5 and an epoxy resin matrix to obtain the PAN-aramid III nano-coated fiber reinforced epoxy resin composite material.
The invention is also characterized in that:
the step 1 is implemented according to the following steps:
step 1.1, soaking aramid fiber III in an absolute ethyl alcohol solution for 20-28 h;
step 1.2, placing the aramid III fiber obtained in the step 1.1 in an ultrasonic cleaning instrument for treatment for 25-35 min;
step 1.3, washing the aramid III fiber obtained in the step 1.2 with deionized water for 3-5 times, and washing absolute ethyl alcohol attached to the surface of the aramid III fiber;
And step 1.4, drying the aramid III fiber obtained in the step 1.3 in an oven at the temperature of 85-95 ℃ for 3-5 hours to obtain the pretreated aramid III fiber.
The plasma surface treatment time in the step 2 is 5-14min, the discharge power of the plasma surface treatment device is 52.5-97.5W, and the discharge air pressure is 1000-2500 Pa.
In the mixed solution in the step 3, the mass fraction of PAN is 6-20%, and the mass fraction of N-N dimethylformamide is 80-94%.
And 4, in the preparation of the PAN-aramid III nano-coated fiber by using an electrostatic spinning parallel electrode method, the flow speed of the spinning solution is 0.3-1.3ml/h, the spinning voltage is 15-23kV, the spinning environment temperature is 20 +/-2 ℃, and the relative humidity is 60 +/-5%.
And 5, rinsing the absolute ethyl alcohol solution for 2-3min, drying at 85-95 ℃ for 1-2 h.
In the step 6, the curing temperature is 50-80 ℃, and the curing time is 4-6 h.
The invention has the beneficial effects that:
(1) the method for preparing the aramid III nano-coated fiber reinforced composite material can obviously improve the interface bonding property of an aramid III fiber reinforcement and a resin matrix, solves the problems of poor interface bonding property of the aramid III fiber and epoxy resin composite material and poor mechanical property of a nano-fiber material prepared by electrostatic spinning in the prior art, widens the application field of nano-fiber, and promotes wider application of the aramid fiber/epoxy resin composite material;
(2) According to the method for preparing the aramid fiber III nano-coated fiber reinforced composite material, the damage of the plasma surface modification to a fiber matrix is small, the treatment process is simple, the environmental pollution is less, and the method is a green and effective surface modification method. The electrostatic spinning method has the advantages of simple equipment, low cost, simple operation and more types of spinnable materials, and is the most effective method for preparing the continuous nano fibers. The method combining the two can be used for preparing the composite material with excellent performance, and has the advantages of short time consumption, high efficiency and less environmental pollution in the operation process;
(3) according to the method for preparing the aramid fiber III nano-coated fiber reinforced composite material, Polyacrylonitrile (PAN) has good weather resistance and sun resistance, and is also resistant to chemical reagents, so that the aramid fiber III nano-coated fiber reinforced composite material is a high polymer material with excellent performance and can be used in various complex environments. Aramid III is a high-performance organic fiber, has a plurality of excellent mechanical properties such as high strength, high modulus, low density, good heat resistance, excellent abrasion performance, good dimensional stability and the like, and is widely applied to the fields of military, aerospace and the like. The two materials are combined to play the advantages of the two materials at the same time, so that the performance of the two materials is made up for the deficiencies of the two materials, and the effect that 1+1 is more than 2 is generated;
(4) According to the method for preparing the aramid III nano-coating fiber reinforced composite material, the prepared nano-coating fiber has a skin-core structure, has the characteristics of porous nano effect and material characteristics, has the characteristics of high porosity and specific surface area of skin layer nano-fibers and excellent mechanical properties of core layer aramid fibers, can be widely applied to the field of fiber reinforced materials, and has a very wide application prospect.
Drawings
FIG. 1 is an electron micrograph of untreated aramid III fiber;
FIG. 2 is an electron microscope image of aramid III fibers treated by the method of preparing an aramid III nano-coated fiber reinforced composite of the present invention in example 1;
FIG. 3 is an electron microscope image of aramid III fibers treated by the method of preparing an aramid III nano-coated fiber reinforced composite of the present invention in example 2;
FIG. 4 is an electron microscope image of aramid III fibers treated by a method of preparing an aramid III nanocoated fiber reinforced composite of the present invention in example 3;
fig. 5 is an electron microscope image of aramid iii fiber treated by the method for preparing an aramid iii nano-coated fiber reinforced composite material of the present invention in example 4.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a method for preparing an aramid fiber III nano-coated fiber reinforced composite material, which is implemented according to the following steps:
step 1, pretreating aramid III fibers, specifically comprising the following steps:
step 1.1, soaking aramid fiber III in an absolute ethyl alcohol solution for 20-28 h;
step 1.2, placing the aramid III fiber obtained in the step 1.1 in an ultrasonic cleaning instrument for treatment for 25-35 min;
step 1.3, washing the aramid III fiber obtained in the step 1.2 with deionized water for 3-5 times, and washing absolute ethyl alcohol attached to the surface of the aramid III fiber;
step 1.4, drying the aramid III fiber obtained in the step 1.3 in an oven at the temperature of 85-95 ℃ for 3-5 hours to obtain pretreated aramid III fiber;
step 2, placing the aramid fiber III obtained in the step 1 in a plasma surface treatment device for plasma surface treatment for 5-14min, wherein the discharge power of the plasma surface treatment device is 52.5-97.5W, and the discharge air pressure is 1000-2500 Pa;
step 3, preparing a mixed solution of PAN and N-N dimethylformamide, wherein the mass fraction of the PAN is 6-20%, and the mass fraction of the N-N dimethylformamide is 80-94%;
step 4, taking the aramid III fiber obtained in the step 2 as a core layer, taking the mixed solution obtained in the step 3 as a spinning solution, and preparing the PAN-aramid III nano-coated fiber by using an electrostatic spinning parallel electrode method, wherein the flow rate of the spinning solution is 0.3-1.3ml/h, the spinning distance is 10-15cm, the spinning voltage is 15-23kV, the rotating speed of a winding roller is 25-35rpm, the distance between two parallel aluminum sheets is 2-6cm, the aramid III fiber of the core layer is 0.8-1.2mm higher than the upper edge of the parallel aluminum sheet, the electrostatic spinning environmental temperature is 20 +/-2 ℃, and the relative humidity is 60 +/-5%;
Step 5, rinsing the PAN-aramid III nano-coated fiber obtained in the step 4 for 2-3min by using an ethanol solution, and drying at the temperature of 85-95 ℃ for 1-2 h;
and 6, curing the PAN-aramid III nano-coated fiber obtained in the step 5 and an epoxy resin matrix at the temperature of 50-80 ℃ for 4-6h to obtain the PAN-aramid III nano-coated fiber reinforced epoxy resin composite material.
As shown in fig. 1, the untreated aramid iii fiber has a smooth surface, and is distributed with inconspicuous and discontinuous shallow grooves and tiny shallow pits, which are formed in the aramid iii spinning process. As shown in fig. 2-5, the number and depth of the grooves on the surface of the aramid fiber after plasma modification treatment are obviously increased, and the surface of the aramid fiber has obvious etching traces, so that the surface roughness of the aramid fiber is obviously increased. The contact area between the fibers and the resin can be increased, and the friction force and the mechanical riveting effect between the fibers and the resin are increased, so that the interface bonding strength is greatly increased, and the mechanical property of the composite material is improved.
Example 1
A method for preparing an aramid III nano-coated fiber reinforced composite material is implemented according to the following steps:
step 1, pretreating aramid III fibers to remove components such as spinning oil and the like remained on the surfaces of the aramid III fibers in the processing process. Soaking with absolute ethyl alcohol for 20h, then placing in an ultrasonic cleaning instrument for treatment for 25min, then cleaning with deionized water, placing in an oven at 85 ℃ for drying for 5h to obtain clean aramid III fiber, and packaging into a plastic packaging bag for later use;
Step 2, placing the pretreated aramid III fiber in a plasma surface treatment device for carrying out plasma surface treatment on the aramid III fiber, wherein the treatment time is 5min, the discharge power is 52.5W, and the discharge air pressure is 1000Pa, and as shown in an electron microscope image of the aramid III fiber treated under the condition shown in figure 2;
step 3, preparing a mixed solution of PAN and N-N Dimethylformamide (DMF) to obtain a spinning solution, wherein the mass fraction of PAN is 6%, and the mass fraction of N-N dimethylformamide is 94%;
step 4, extracting spinning solution by using an injector, taking the aramid fiber III treated by the plasma as a core layer, and preparing PAN-aramid fiber III nano-coated fiber by using an electrostatic spinning parallel electrode method, wherein the extrusion speed of the spinning solution is 0.3ml/h, the spinning voltage is 15kV, the ambient temperature of electrostatic spinning is 18 ℃, and the relative humidity is 55%;
step 5, rinsing the PAN-aramid III nano-coated fiber obtained in the step 4 with an ethanol solution for 2min to remove the solvent, and drying in an oven at 85 ℃ for 2h for later use;
and 6, curing the PAN-aramid III nano-coated fiber obtained in the step 5 and an epoxy resin matrix at the temperature of 50 ℃ for 6 hours to obtain the PAN-aramid III nano-coated fiber reinforced epoxy resin composite material.
Example 2
A method for preparing an aramid III nano-coated fiber reinforced composite material is implemented according to the following steps:
step 1, pretreating aramid III fibers to remove components such as spinning oil and the like remained on the surfaces of the aramid III fibers in the processing process. Soaking with absolute ethyl alcohol for 22h, then placing in an ultrasonic cleaner for treatment for 27min, then cleaning with deionized water, placing in an oven at 85 ℃ for drying for 5h to obtain clean aramid III fiber, and packaging into a plastic packaging bag for later use;
step 2, placing the pretreated aramid III fiber in a plasma surface treatment device for carrying out plasma surface treatment on the aramid III fiber, wherein the treatment time is 7min, the discharge power is 62.5W, and the discharge air pressure is 1300Pa, and as shown in an electron microscope image of the aramid III fiber treated under the condition shown in figure 3;
step 3, preparing a mixed solution of PAN and N-N Dimethylformamide (DMF) to obtain a spinning solution, wherein the mass fraction of PAN is 9%, and the mass fraction of N-N dimethylformamide is 91%;
step 4, extracting spinning solution by using an injector, taking the aramid fiber III treated by the plasma as a core layer, and preparing PAN-aramid fiber III nano-coated fiber by using an electrostatic spinning parallel electrode method, wherein the extrusion speed of the spinning solution is 0.5ml/h, the spinning voltage is 17kV, the ambient temperature of electrostatic spinning is 19 ℃, and the relative humidity is 57%;
Step 5, immersing the PAN-aramid III nano-coated fiber obtained in the step 4 in ethanol, rinsing for 2min to remove the solvent, and drying in an oven at 85 ℃ for 2h for later use;
and 6, curing the PAN-aramid III nano-coated fiber obtained in the step 5 and an epoxy resin matrix at the temperature of 55 ℃ for 6 hours to obtain the PAN-aramid III nano-coated fiber reinforced epoxy resin composite material.
Example 3
A method for preparing an aramid III nano-coated fiber reinforced composite material is implemented according to the following steps:
step 1, pretreating aramid III fibers to remove components such as spinning oil and the like remained on the surfaces of the aramid III fibers in the processing process. Soaking with absolute ethyl alcohol for 25h, then placing in an ultrasonic cleaning instrument for treatment for 27min, then cleaning with deionized water, placing in a 90 ℃ oven for 4h for drying to obtain clean aramid III fiber, and packaging into a plastic packaging bag for later use;
step 2, placing the pretreated aramid III fiber in a plasma surface treatment device for carrying out plasma surface treatment on the aramid III fiber, wherein the treatment time is 9min, the discharge power is 72.5W, and the discharge air pressure is 1600Pa, and as shown in an electron microscope image of the aramid III fiber treated under the condition shown in FIG. 4;
step 3, preparing a mixed solution of PAN and N-N Dimethylformamide (DMF) to obtain a spinning solution, wherein the mass fraction of PAN is 12%, and the mass fraction of N-N dimethylformamide is 88%;
Step 4, extracting spinning solution by using an injector, taking the aramid fiber III treated by the plasma as a core layer, and preparing PAN-aramid fiber III nano-coated fiber by using an electrostatic spinning parallel electrode method, wherein the extrusion speed of the spinning solution is 0.7ml/h, the spinning voltage is 19kV, the ambient temperature of electrostatic spinning is 20 ℃, and the relative humidity is 59%;
step 5, immersing the PAN-aramid III nano-coated fiber obtained in the step 4 in ethanol, rinsing for 2min to remove the solvent, and drying in an oven at 90 ℃ for 1.5h for later use;
and 6, curing the PAN-aramid III nano-coated fiber obtained in the step 5 and an epoxy resin matrix at the temperature of 60 ℃ for 6 hours to obtain the PAN-aramid III nano-coated fiber reinforced epoxy resin composite material.
Example 4
A method for preparing an aramid III nano-coated fiber reinforced composite material is implemented according to the following steps:
step 1, pretreating aramid III fibers to remove components such as spinning oil and the like remained on the surfaces of the aramid III fibers in the processing process. Soaking with absolute ethyl alcohol for 28h, then placing in an ultrasonic cleaner for treatment for 35min, then cleaning with deionized water, placing in a 95 ℃ oven for drying for 3h to obtain clean aramid III fiber, and packaging into a plastic packaging bag for later use;
Step 2, placing the pretreated aramid III fiber in a plasma surface treatment device to carry out plasma surface treatment on the aramid III fiber, wherein the treatment time is 14min, the discharge power is 97.5W, and the discharge air pressure is 2500Pa, and as shown in an electron microscope image of the aramid III fiber treated under the condition shown in FIG. 5;
step 3, preparing a mixed solution of PAN and N-N Dimethylformamide (DMF) to obtain a spinning solution, wherein the mass fraction of PAN is 20%, and the mass fraction of N-N dimethylformamide is 80%;
step 4, extracting spinning solution by using an injector, taking the aramid fiber III treated by the plasma as a core layer, and preparing PAN-aramid fiber III nano-coated fiber by using an electrostatic spinning parallel electrode method, wherein the extrusion speed of the spinning solution is 1.3ml/h, the spinning voltage is 23kV, the ambient temperature of electrostatic spinning is 22 ℃, and the relative humidity is 65%;
step 5, immersing the PAN-aramid III nano-coated fiber obtained in the step 4 in ethanol, rinsing for 3min to remove the solvent, and drying in an oven for 1h at 95 ℃ for later use;
and 6, curing the PAN-aramid III nano-coated fiber obtained in the step 5 and an epoxy resin matrix at the temperature of 80 ℃ for 6 hours to obtain the PAN-aramid III nano-coated fiber reinforced epoxy resin composite material.
The interfacial properties of the PAN-aramid iii nanocoated fiber reinforced epoxy resin composite under the conditions of examples 1-4 were tested by a monofilament fragmentation method, and the test results are shown in table 1.
TABLE 1 test results of interfacial properties of PAN-aramid III nano-coated fiber reinforced epoxy resin composite material under different implementation conditions
Conditions for carrying out Interfacial shear strength τ/MPa Increase rate/%)
Untreated 22.47 0
Example 1 26.83 19.40
Example 2 28.31 25.99
Example 3 30.23 34.53
Example 4 28.54 27.01
According to experimental results, compared with the untreated original aramid fiber III reinforced composite material, the PAN-aramid fiber III nano-coated fiber reinforced epoxy resin composite material prepared by the method for preparing the aramid fiber III nano-coated fiber reinforced composite material has the advantages that the interface performance is obviously improved, the improvement degrees of the interface bonding performance are different under different treatment conditions, and the interface shear strength of the composite material in the embodiment 3 is improved by 34.53%.
According to the method for preparing the aramid III nano-coated fiber reinforced composite material, the prepared nano-coated fiber with the skin-core structure has the characteristics of porous nano effect and material property, has the characteristics of high porosity and specific surface area of the skin layer nano-fiber and excellent mechanical property of the core layer aramid fiber, can exert the advantages of the two materials simultaneously, makes the properties of the two materials complementary to each other, and forms the composite material with excellent performance. The problems of poor interface adhesion of aramid fiber III and epoxy resin composite materials and poor mechanical property of nanofiber materials prepared by electrostatic spinning in the prior art are solved, the operation process is short in time consumption and high in efficiency, and the method has little environmental pollution, can be widely applied to the fields of fiber reinforced materials, filtering materials and the like, and has a very wide application prospect.

Claims (4)

1. A method for preparing an aramid III nano-coated fiber reinforced composite material is characterized by comprising the following steps:
step 1, pretreating aramid fiber III;
step 2, placing the aramid III fiber obtained in the step 1 in a plasma surface treatment device for plasma surface treatment;
step 3, preparing a mixed solution of PAN and N-N dimethylformamide;
step 4, taking the aramid fiber III obtained in the step 2 as a core layer, taking the mixed solution obtained in the step 3 as a spinning solution, and preparing PAN-aramid fiber III nano-coated fiber by using an electrostatic spinning parallel electrode method;
step 5, rinsing the PAN-aramid III nano-coated fiber obtained in the step 4 by using an ethanol solution, and then drying for later use;
step 6, curing the PAN-aramid III nano-coated fiber obtained in the step 5 and an epoxy resin matrix to obtain a PAN-aramid III nano-coated fiber reinforced epoxy resin composite material;
the step 1 is specifically implemented according to the following steps:
step 1.1, soaking aramid fiber III in an absolute ethyl alcohol solution for 20-28 h;
step 1.2, placing the aramid III fiber obtained in the step 1.1 in an ultrasonic cleaning instrument for treatment for 25-35 min;
step 1.3, washing the aramid III fiber obtained in the step 1.2 with deionized water for 3-5 times, and washing absolute ethyl alcohol attached to the surface of the aramid III fiber;
Step 1.4, drying the aramid III fiber obtained in the step 1.3 in an oven at the temperature of 85-95 ℃ for 3-5 hours to obtain pretreated aramid III fiber;
in the mixed solution in the step 3, the mass fraction of PAN is 6-20%, and the mass fraction of N-N dimethylformamide is 80-94%;
in the step 4, in the preparation of the PAN-aramid III nano-coated fiber by using an electrostatic spinning parallel electrode method, the flow speed of the spinning solution is 0.3-1.3ml/h, the spinning voltage is 15-23kV, the spinning environment temperature is 20 +/-2 ℃, and the relative humidity is 60 +/-5%.
2. The method for preparing the aramid fiber III nano-coated fiber reinforced composite material as claimed in claim 1, wherein the plasma surface treatment time in the step 2 is 5-14min, the discharge power of the plasma surface treatment device is 52.5-97.5W, and the discharge air pressure is 1000-2500 Pa.
3. The method for preparing the aramid III nano-coated fiber reinforced composite material as claimed in claim 1, wherein the rinsing time of the absolute ethyl alcohol solution in the step 5 is 2-3min, the drying temperature is 85-95 ℃, and the drying time is 1-2 h.
4. The method for preparing the aramid III nano-coated fiber reinforced composite material as claimed in claim 1, wherein the curing temperature in the step 6 is 50-80 ℃ and the curing time is 4-6 h.
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