CN113249819B - Carbon nano tube-nano Fe3O4-polyimide composite fiber and preparation method thereof - Google Patents

Carbon nano tube-nano Fe3O4-polyimide composite fiber and preparation method thereof Download PDF

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CN113249819B
CN113249819B CN202110571523.1A CN202110571523A CN113249819B CN 113249819 B CN113249819 B CN 113249819B CN 202110571523 A CN202110571523 A CN 202110571523A CN 113249819 B CN113249819 B CN 113249819B
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carbon nano
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CN113249819A (en
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牛鸿庆
姜铭
武德珍
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties

Abstract

Carbon nano tube-nano Fe3O4A method for preparing a polyimide composite fiber, comprising: by usingThe sand mill mixes the carbon nano tube and the nano Fe3O4Grinding and blending the two in a solvent and improving the dispersibility of the two in the solvent, and then grinding the powder to prepare the carbon nano tube/nano Fe with dianhydride and diamine by adopting an in-situ polymerization method3O4A/polyimide composite fiber. The method prepares the thin, light, wide and strong wave-absorbing material on the premise of not influencing the excellent performance of the polyimide fiber, and can be widely applied to the field of aerospace.

Description

Carbon nano tube-nano Fe3O4-polyimide composite fiber and preparation method thereof
Technical Field
The invention belongs to the technical field of functional preparation of polyimide fibers, and particularly relates to a wave-absorbing composite polyimide fiber and a preparation method thereof.
Background
With the development of science and technology, a large amount of electronic equipment enters daily life, electromagnetic radiation pollution is increasingly serious, the electronic equipment becomes new social public nuisance gradually, and the health of human beings is influenced. In military, the international competition of weaponry is intensified day by day, and along with the development of detection technology, the realization of target stealth in war has profound significance for improving the survival and the attack-fighting capability of weapon system. The most effective method for solving the electromagnetic radiation pollution and realizing the target stealth is to adopt wave-absorbing materials. With the continuous progress of science and technology, the electromagnetic wave absorbing material gradually develops and progresses towards the direction of 'strong quality, thin thickness, wide frequency band and strong wave absorption', and the preparation of the wave absorbing material with excellent performance becomes one of the hot research directions in the field.
The polyimide fiber is a high molecular polymer with an imide ring structure on a main chain, is generally polymerized by a dianhydride monomer and a diamine monomer, and has the excellent characteristics of higher strength and modulus, good heat resistance, low dielectric property, chemical corrosion resistance and the like; particularly as a broadband wave-transparent material: the low dielectric constant and loss make it widely used in radar, antenna and other fields.
The wave-absorbing material is a material capable of absorbing and attenuating incident electromagnetic waves and converting electromagnetic energy into heat energy to be dissipated or destructing the electromagnetic waves due to interference, and is generally formed by compounding an absorbent and a matrix material capable of transmitting the electromagnetic waves. The wave-absorbing material should satisfy two conditions, one is impedance matching: whether the electromagnetic wave incident on the material meets impedance matching or not, the electromagnetic wave entering the material system is as much as possible and is not reflected; secondly, attenuation conditions are as follows: in designing the structure of the wave-absorbing material, the attenuation conditions must be taken into account so that the electromagnetic waves can be consumed quickly after entering the interior of the material. Wave absorbers are generally classified into magnetic loss, dielectric loss, and resistance loss according to the loss mechanism. The magnetic loss mainly comprises the attenuation of electromagnetic waves by mechanisms such as eddy current loss, hysteresis loss, residual loss and the like. Ferrite is a material that typically has a dominant residual loss.
The decay of the resistively lost electromagnetic energy is caused by the electrical resistance of the material, with higher resistive losses, and materials with greater electrical conductivity are more favorable for converting electromagnetic energy into heat. Mainly comprises carbon fiber, conductive high polymer, graphite, silicon carbide, conductive carbon black and the like. Dielectric loss attenuates electromagnetic waves mainly by material polarization (dipole polarization, ion polarization, or interface polarization), and barium titanate, ferroelectric ceramics, or the like are mainly used.
Nowadays, the research of wave-absorbing agents is gradually deepened, and novel wave-absorbing agents and wave-absorbing mechanisms are being widely researched so as to obtain high-efficiency, light, thin and broadband wave-absorbing materials and meet increasingly severe use requirements. The carbon nano tube is used as a novel nano wave-absorbing material, has the advantages of excellent mechanical property, good chemical stability, high specific surface area, large length-diameter ratio and the like, has a unique one-dimensional structure, and can be better arranged along the axial direction of the fiber in the spinning drafting process; the nano ferrite wave-absorbing material is one of the wave-absorbing agents which are well researched at present, has the advantages of good wave-absorbing performance, low price and the like, and can still present better wave-absorbing performance under the harsh conditions of lower frequency and thinner thickness, thereby becoming an important component of the radar wave-absorbing material.
Carbon nanotube/Nano Fe in the invention3O4The polyimide composite fiber organically combines the wave absorbing performance of the functional body and the wave permeability of the polyimide matrix, exerts the loss capacity to electromagnetic waves to the maximum extent, and the high thermal stability and the high glass transition temperature of the PI are beneficial to stabilizing nano-sized functional body particles, so that the functional body particles are not aggregated and are very beneficial to the dispersibility of a composite material; the carbon nano tube is beneficial to the improvement of the heat resistance, the mechanical property, the size stability and the like of the fiber on the basis of realizing the wave absorbing function of the fiber.
Disclosure of Invention
The invention aims to provide a high-performance polyimide composite fiber with low matching thickness and strong wave-absorbing performance and a preparation method thereof.
Carbon nano tube/nano Fe3O4Preparation method of polyimide composite fiber, carbon nano tube and nano Fe3O4The method is used as a wave absorbing agent, takes polyimide fiber as a matrix, and comprises the following steps:
A. adopting an in-situ polymerization method to mix the ground carbon nano tube and the nano Fe3O4Dispersing in organic solvent, adding dianhydride monomer and diamine monomer to synthesize carbon nanotube/nanometer Fe3O4A polyamic acid mixed solution;
B. spinning the mixed solution to obtain polyamide acid composite fiber, and performing thermal imidization or chemical imidization treatment to obtain carbon nano tube/nano Fe3O4A/polyimide composite fiber.
Wherein, the organic solvent in the step A is one or more mixed monomers of N, N-dimethylacetamide (DMAc), N-N-Dimethylformamide (DMF), dimethyl sulfoxide (DMSO) and the like.
And B, performing surface treatment on the carbon nano tube in the step A, wherein the surface of the carbon nano tube contains hydroxyl, carboxyl and imidacloprid nitrogen.
The grinding in the step A comprises the following specific steps: mixing carbon nanotube and nano Fe3O4Respectively mixing according to the mass ratio of 8:1-1: 8; then mixing the mixed powder with an organic solvent according to the mass-volume ratio of 1g:100ml-2g:100ml, and putting the mixture into a sand mill for grinding.
The dianhydride monomer in the step A is one or a combination of more of pyromellitic dianhydride, 4,4 ' -diphenyl ether dianhydride, hexafluoro-isopropylphthalic acid, 3,3 ', 4,4 ' -biphenyl tetracarboxylic dianhydride, 2,3,3 ', 4 ' -biphenyl tetracarboxylic dianhydride, 3,3 ', 4,4 ' -benzophenone tetracarboxylic dianhydride and the like in any proportion; the diamine monomer is one or more of p-phenylenediamine, m-phenylenediamine, p-aminodiphenyl ether, 3 '-diaminobenzidine and 4, 4' -diaminodiphenyl ether in any proportion. The molar ratio of the diamine monomer to the dianhydride monomer is 1:1-1: 1.1.
Wherein the solid content of the polyamic acid in the step A is 10-30 wt%.
Wherein, the spinning process in the step B comprises the following specific steps: and transferring the prepared mixed solution into a spinning tank, spraying the mixed solution through a spinneret plate, directly entering a coagulating bath, and sequentially passing through the coagulating bath and a water washing tank under the action of axial traction force to obtain the polyamide acid composite fiber. Preferably, the coagulating bath is a mixed solution of N-N-dimethylacetamide and deionized water, the temperature of the coagulating bath is 30-50 ℃, and the volume fraction of the N-N-dimethylacetamide is 10-30%.
Wherein, in the step B, the specific process of thermal imidization is as follows: the obtained polyamide acid composite fiber is subjected to gradient heating in an oven for thermal imidization treatment to obtain the carbon nano tube/nano Fe3O4A/polyimide composite fiber.
Or in the step B, the specific chemical imidization process is as follows: soaking the obtained polyamic acid composite fiber in a chemical imidization reagent, and performing heat treatment to obtain the carbon nano tube/nano Fe3O4A polyimide composite fiber; the imidization reagent is pyridine/acetic anhydride solution with the volume ratio of 3:1-1: 3.
The invention also provides the carbon nano tube/nano Fe prepared by the preparation method3O4A/polyimide composite fiber. Preferably, when the carbon nano tube is mixed with the nano Fe3O4The mass ratio of (3) to (1) and the mass ratio of the wave absorber to the polyamic acid is 6 to 100, the lowest reflection loss of the polyimide composite fiber is-43 dB at a minimum matching thickness of 2.45 mm.
Compared with the prior art, the invention has the following beneficial effects:
the carbon nano tube/nano Fe of the invention3O4The preparation method of the polyimide composite fiber uses the carbon nano tube with the surface containing hydroxyl, carboxyl and imidacloprid nitrogen to improve the dispersibility of the carbon nano tube in the polyimide matrix, and further uses a nano dispersing sand mill to grind the carbon nano tube and the nano Fe3O4Uniform dispersion in the polyimide matrix.
Carbon nano-particles using the present inventionTube/nano Fe3O4Preparation method of polyimide composite fiber and prepared carbon nano tube/nano Fe3O4A/polyimide composite fiber. Carbon nano-tube and nano Fe in composite fiber3O4The dispersion is uniform, and the composite fiber has excellent wave-absorbing performance in an X wave band. When carbon nano tube and nano Fe3O4When the mass ratio of the wave absorbing agent to the polyamic acid is 3:1 and 6:100, the lowest reflection loss of the polyimide composite fiber can reach-43 dB when the lowest matching thickness is 2.45 mm.
Drawings
FIG. 1 shows the preparation of nano Fe-carbon nanotube in example 5 of the present invention3O4Scanning electron micrographs of polyimide composite fibers.
FIG. 2 is a carbon nanotube-nano Fe prepared according to example 13O4-reflection loss curve of polyimide composite fiber in the frequency range of X-band.
FIG. 3 is a carbon nanotube-nano Fe prepared according to example 23O4-reflection loss curve of polyimide composite fiber in the frequency range of X-band.
FIG. 4 carbon nanotube-nano Fe prepared according to example 33O4-reflection loss curve of polyimide composite fiber in the frequency range of X-band.
FIG. 5 is a carbon nanotube-nano Fe prepared according to example 43O4-reflection loss curve of polyimide composite fiber in the frequency range of X-band.
FIG. 6 is a carbon nanotube-nano Fe prepared according to example 53O4-reflection loss curve of polyimide composite fiber in the frequency range of X-band.
FIG. 7 is a carbon nanotube-nano Fe prepared according to comparative example 13O4-reflection loss curve of polyimide composite fiber in the frequency range of X-band.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited to the details of the description.
Example 1
A. Mixing carbon nano-tube and nano Fe3O4Mixing the mixture with DMAc according to a mass ratio of 5:1, wherein the mass ratio of the mixture to the DMAc is 1g:100ml of the mixture is added into a sand mill to be ground and dispersed, the rotating speed is 2000r/min, the grinding is carried out for 60min, and the carbon nano tube/nano Fe is obtained3O4a/DMAc dispersion. The carbon nanotube has an average diameter of 30nm and an average length of 25 μm, and contains a hydroxyl group, a carboxyl group and an imidacloprid nitrogen on the surface.
Adding the dispersion, BPDA and p-PDA (the molar ratio of the dispersion to the BPDA is 1:1) into DMAc, and stirring to obtain the carbon nano tube/nano Fe with the solid content of 15 wt% and the mass ratio of the wave absorbing agent to the polyamic acid of 6:1003O4Polyamic acid solution.
B. The solution is prepared into polyamide acid composite fiber through wet spinning, and the prepared fiber is heated in a drying oven in a gradient way for thermal imidization, so that the final carbon nano tube/nano Fe can be obtained3O4A/polyimide composite fiber.
The method specifically comprises the following steps: transferring the prepared mixed solution into a spinning tank, carrying out vacuum defoaming for 5 hours at 30 ℃, then uniformly and stably spraying the spinning solution through a spinneret plate under the nitrogen pressure of 0.20MPa, directly entering a coagulating bath, and sequentially passing through the coagulating bath and a rinsing bath under the action of axial traction force; then the mixture is heated in a gradient way in a drying oven for thermal imidization, and the carbon nano tube/nano Fe can be obtained3O4A/polyimide composite fiber. The coagulation bath is a mixed solution of N-N-dimethylacetamide and deionized water, the temperature of the coagulation bath is 30 ℃, and the volume fraction of the N-N-dimethylacetamide is 10%. The gradient temperature rise comprises the specific steps of preserving heat for 1 hour at 60 ℃, preserving heat for 2 hours when the temperature rises to 135 ℃, and preserving heat for 2 hours when the temperature rises to 320 ℃.
The polyimide composite fiber prepared by the method is mixed with paraffin to prepare a sample block, wherein the mass fraction of the fiber is 40%, the electromagnetic parameter test is carried out on the composite sample block by using a vector network analyzer and adopting a waveguide method, and the reflection loss curves with different thicknesses are obtained by calculation and are shown in figure 2.
Example 2
Mixing carbon nano-tube and nano Fe3O4Mixing according to the weight ratio of 3: 1. The rest is the same as in example 1.
The polyimide composite fiber prepared by the method is mixed with paraffin to prepare a sample block, wherein the mass fraction of the fiber is 40%, the composite sample block is subjected to electromagnetic parameter test by using a vector network analyzer and adopting a waveguide method, and reflection loss curves with different thicknesses are obtained by calculation and are shown in figure 3.
Example 3
Mixing carbon nano-tube and nano Fe3O4Mixing according to the weight ratio of 1:1. The rest is the same as in example 1.
The polyimide composite fiber prepared by the method is mixed with paraffin to prepare a sample block, wherein the mass fraction of the fiber is 40%, the electromagnetic parameter test is carried out on the composite sample block by using a vector network analyzer and adopting a waveguide method, and the reflection loss curves with different thicknesses are obtained by calculation and are shown in figure 4.
Example 4
Mixing carbon nano-tube and nano Fe3O4Mixing according to the weight ratio of 1: 3. The rest is the same as in example 1.
The polyimide composite fiber prepared by the method is mixed with paraffin to prepare a sample block, wherein the mass fraction of the fiber is 40%, the electromagnetic parameter test is carried out on the composite sample block by using a vector network analyzer and adopting a waveguide method, and the reflection loss curves with different thicknesses are obtained by calculation and are shown in figure 5.
Example 5
Mixing carbon nano-tube and nano Fe3O4Mixing according to the weight ratio of 1: 5. The rest is the same as in example 1.
The polyimide composite fiber prepared by the method is mixed with paraffin to prepare a sample block, wherein the mass fraction of the fiber is 40%, the electromagnetic parameter test is carried out on the composite sample block by using a vector network analyzer and adopting a waveguide method, and the reflection loss curves with different thicknesses are obtained by calculation and are shown in figure 6.
Comparative example 1
Mixing a pure carbon nanotube and DMAc according to the mass-volume ratio of 1g:100ml of the mixture is added into a sand mill to be ground and dispersed, the rotating speed is 2000r/min, and the grinding time is 60 min. The rest is the same as in example 1.
The polyimide composite fiber prepared by the method is mixed with paraffin to prepare a sample block, wherein the mass fraction of the fiber is 40%, the electromagnetic parameter test is carried out on the composite sample block by using a vector network analyzer and adopting a waveguide method, and the reflection loss curves with different thicknesses are obtained by calculation and are shown in figure 7.
The invention prepares the carbon nano tube-nano Fe by spinning by utilizing an in-situ polymerization method3O4-polyimide composite fibers. Experiments prove that compared with the polyimide composite fiber (comparative example 1) only added with the carbon nano tube, the invention simultaneously adds the carbon nano tube and the nano Fe under the condition of adding the wave absorbing agent with the same content3O4The obtained polyimide composite fiber (examples 1 to 5) has relatively better wave-absorbing performance due to the synergistic effect. This is because the electromagnetic wave loss of the composite fiber is derived from the dielectric loss only when only the carbon nanotubes are added, and the nano-Fe is added3O4Then, the electromagnetic wave loss of the composite fiber is derived from the dielectric loss of the carbon nanotube and the nano Fe3O4Magnetic loss of (2). Contrast different carbon nano tube and nano Fe3O4The composite fiber with the proportion can also find that the composite fiber prepared in the embodiment 1 has better wave-absorbing performance, the lowest reflection loss is-43 dB when the matching thickness is 2.45mm, the wave-absorbing frequency bandwidth is 3.02 GHz, and the composite fiber is the optimal embodiment, and the dielectric loss of the carbon nano tube and the nano Fe at the moment3O4The synergistic effect of the magnetic loss of (a) is the best.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. Not all embodiments are exhaustive. All obvious changes and modifications which are obvious to the technical scheme of the invention are covered by the protection scope of the invention.

Claims (1)

1. Carbon nano tube-nano Fe3O4Preparation method of-polyimide composite fiber, carbon nano tube and nano Fe3O4The wave absorbing agent takes polyimide fiber as a matrix, and is characterized by comprising the following steps:
A. mixing carbon nano-tube and nano Fe3O4Mixing the mixture with DMAc according to a mass ratio of 3:1, wherein the mass to volume ratio of the mixture to DMAc is 1g:100ml of the mixture is added into a sand mill for grinding and dispersion, the rotating speed is 2000r/min, the grinding is carried out for 60min, and the carbon nano tube/nano Fe is obtained3O4A DMAc dispersion; the carbon nano tube has the average diameter of 30nm and the average length of 25 mu m, and the surface of the carbon nano tube contains hydroxyl, carboxyl and imidacloprid nitrogen;
adding the dispersion, BPDA and p-PDA into DMAc, and stirring to obtain carbon nano tube/nano Fe with the solid content of 15 wt% and the mass ratio of the wave absorbing agent to the polyamic acid of 6:1003O4Polyamic acid solution; the molar ratio of BPDA to p-PDA is 1: 1;
B. the solution is prepared into polyamide acid composite fiber through wet spinning, and the prepared fiber is subjected to gradient heating in an oven for thermal imidization to obtain the final carbon nano tube/nano Fe3O4A polyimide composite fiber;
the method comprises the following specific steps: transferring the prepared mixed solution into a spinning tank, carrying out vacuum defoaming for 5 hours at 30 ℃, then uniformly and stably spraying the spinning solution through a spinneret plate under the nitrogen pressure of 0.20MPa, directly entering a coagulating bath, and sequentially passing through the coagulating bath and a rinsing bath under the action of axial traction force; then the mixture is heated in a gradient way in a drying oven for thermal imidization, and the carbon nano tube/nano Fe can be obtained3O4A polyimide composite fiber; wherein the coagulation bath is a mixed solution of N-N-dimethylacetamide and deionized water, the temperature of the coagulation bath is 30 ℃, and the volume fraction of the N-N-dimethylacetamide is 10%; the gradient temperature rise comprises the specific steps of preserving heat for 1 hour at 60 ℃, preserving heat for 2 hours when the temperature rises to 135 ℃, and preserving heat for 2 hours when the temperature rises to 320 ℃.
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