CN116815494A - Aramid fiber composite conductive fiber and preparation method and application thereof - Google Patents
Aramid fiber composite conductive fiber and preparation method and application thereof Download PDFInfo
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- 239000000835 fiber Substances 0.000 title claims abstract description 189
- 239000002131 composite material Substances 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 229920006231 aramid fiber Polymers 0.000 title claims abstract description 29
- 229920003235 aromatic polyamide Polymers 0.000 claims abstract description 427
- 239000004760 aramid Substances 0.000 claims abstract description 350
- 239000011231 conductive filler Substances 0.000 claims abstract description 272
- 239000006185 dispersion Substances 0.000 claims abstract description 188
- 239000007788 liquid Substances 0.000 claims abstract description 144
- 239000000463 material Substances 0.000 claims abstract description 60
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 10
- 239000001257 hydrogen Substances 0.000 claims abstract description 10
- 238000002604 ultrasonography Methods 0.000 claims abstract description 5
- 239000002121 nanofiber Substances 0.000 claims description 184
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 140
- 239000000243 solution Substances 0.000 claims description 112
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 73
- 238000003756 stirring Methods 0.000 claims description 45
- 239000003513 alkali Substances 0.000 claims description 43
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 42
- 229910021389 graphene Inorganic materials 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- 239000000203 mixture Substances 0.000 claims description 37
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
- 238000001035 drying Methods 0.000 claims description 30
- 239000010936 titanium Substances 0.000 claims description 29
- 238000000034 method Methods 0.000 claims description 26
- 239000002041 carbon nanotube Substances 0.000 claims description 22
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 21
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 21
- 239000012043 crude product Substances 0.000 claims description 20
- 229910052799 carbon Inorganic materials 0.000 claims description 19
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims description 16
- 239000002585 base Substances 0.000 claims description 14
- 239000002109 single walled nanotube Substances 0.000 claims description 12
- 230000003993 interaction Effects 0.000 claims description 11
- 230000008961 swelling Effects 0.000 claims description 11
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910010293 ceramic material Inorganic materials 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 7
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- RPDAUEIUDPHABB-UHFFFAOYSA-N potassium ethoxide Chemical compound [K+].CC[O-] RPDAUEIUDPHABB-UHFFFAOYSA-N 0.000 claims description 4
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 2
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- 238000002791 soaking Methods 0.000 description 10
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- 239000012762 magnetic filler Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 238000009864 tensile test Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
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- 238000007790 scraping Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
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- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229920003366 poly(p-phenylene terephthalamide) Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
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- 230000003068 static effect Effects 0.000 description 1
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- MHSKRLJMQQNJNC-UHFFFAOYSA-N terephthalamide Chemical compound NC(=O)C1=CC=C(C(N)=O)C=C1 MHSKRLJMQQNJNC-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/08—Organic compounds
- D06M10/10—Macromolecular compounds
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/04—Physical treatment combined with treatment with chemical compounds or elements
- D06M10/06—Inorganic compounds or elements
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D—TEXTILES; PAPER
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
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- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to the technical field of conductive fibers, in particular to an aramid composite conductive fiber, a preparation method and application thereof, wherein the aramid composite conductive fiber takes para-aramid fiber as a base material, an aramid nanofiber-conductive filler dispersion liquid swells the para-aramid fiber under the assistance of ultrasound, so that microcracks with the width of 100-300nm are formed on the surface of the para-aramid fiber, and simultaneously, an aramid nanofiber-conductive filler combination in the aramid nanofiber-conductive filler dispersion liquid and the para-aramid fiber form hydrogen bonds, so that the aramid nanofiber-conductive filler combination is uniformly dispersed on the surface of the para-aramid fiber and inside the microcracks to form the aramid composite conductive fiber, thereby solving the problems of poor mechanical strength, lack of flexibility, low combination degree with the aramid fiber, low strength, poor flexibility and the like of a final composite conductive material in the prior art.
Description
Technical Field
The invention relates to the technical field of conductive fibers, in particular to an aramid composite conductive fiber, a preparation method and application thereof.
Background
At present, the development of electronic technology puts forward higher requirements on conductive, antistatic and electromagnetic shielding materials, and the performances of flexibility, light weight, high strength and the like become hot spot directions pursued in the field of materials. The one-dimensional conductive fiber base material is an important component part, and is widely applied to the fields of energy storage, electromagnetic shielding, sensing, intelligent wearing and the like due to the advantages of high length-diameter ratio, excellent high conductivity, strong reworkability and the like. The one-dimensional conductive fibers which are most widely used at present are mainly carbon materials, graphene and the like. However, the preparation process of the material often needs high-temperature conditions, the preparation process is complex, and high-efficiency continuity of the fiber is difficult to realize; and the material has low strength and lacks flexibility, so that the mechanical strength requirement of the one-dimensional conductive fiber in practical application cannot be ensured.
CN113235184a discloses a preparation method of an aramid nano-based composite conductive fiber, which uses an aramid nano-fiber as a high-strength skin layer of a one-dimensional composite fiber, and mixes MXene as a functional composite conductive core layer to prepare the composite conductive fiber. However, the breaking strength of the obtained product is only 1.71N, and the requirements of the fields of electromagnetic shielding, intelligent wearing and the like on the high strength of the fiber cannot be met; and the preparation process of the method is complex, and a large amount of time is required for solvent exchange.
Para-aramid fiber (PPTA) is one of high-performance fibers, and para-aramid fiber, namely paraphenylene terephthalamide fiber, has many excellent properties, such as good wear resistance, thermal stability, high temperature resistance, flame retardance, good chemical stability, good mechanical properties and the like. The Aramid Nanofiber (ANF) is a nano material with excellent performance, has excellent characteristics of high length-diameter ratio, large specific surface area, multiple active groups and the like, and recently, the technical proposal is to coat the aramid nanofiber on the aramid macroscopic fiber to improve the surface activity of the aramid fiber, so as to enhance the interface bonding strength of the aramid composite material.
As disclosed in CN115029939a, an electromagnetic shielding coating material with a multilayer structure based on aramid nanofibers and application thereof are disclosed, firstly, para-aramid fibers are added into a mixed solution of strong alkali and dimethyl sulfoxide for stripping, and after a period of time, the state that the aramid fibers are chemically split into nano-scale exists in a dimethyl sulfoxide dispersion of the aramid nanofibers. The dispersion liquid is coated on nylon mesh cloth in a scraping way, and then water is added to reproton the aramid nanofiber, so that the aramid nanofiber film taking the nylon mesh cloth as a base is obtained, and the film has certain mechanical strength and high temperature resistance. And spraying the conductive filler and the magnetic filler on the film, and then coating a layer of aramid nanofiber film. The steps are repeated to obtain the electromagnetic shielding coating material with the multilayer structure based on the aramid nanofibers. However, the electromagnetic shielding coating in the technical scheme is of a multi-layer structure, the problem of uneven dispersion of the conductive filler and the magnetic filler is easily caused by physical spraying, and the situation that the properties of the material are reduced due to layer separation and filler falling off easily occurs after the conductive filler and the magnetic filler are used for a period of time, so that the material cannot be recycled for a long time.
Based on the above-mentioned prior art, there are technical problems in the prior art that the carbon-based conductive fiber has poor mechanical strength, lacks flexibility, is difficult to continuously produce, has low bonding degree with the aramid fiber, and causes low strength and poor flexibility of the final composite conductive material.
Disclosure of Invention
In order to solve the technical problems, the invention provides an aramid composite conductive fiber, wherein an aramid nanofiber-conductive filler combination is uniformly dispersed on the surface of a para-aramid fiber with microcracks on the surface and the inside of the microcracks to form the aramid composite conductive fiber, the width of the microcracks is 100-300nm, and the mass ratio of the aramid nanofiber to the conductive filler in the aramid nanofiber-conductive filler combination is (0.02-1): (2-16), wherein the mass ratio of the aramid nanofiber-conductive filler combination to the para-aramid fiber is (2.02-17): 2, the specific resistance of the aramid composite conductive fiber is 5.6X10 2 -3.4×10 5 Omega cm, tensile strength of 17.32-18.56 cN/dtex, elongation at break of 5.91-6.34 percent and washing fastness of 2-4 grade;
the conductivity (specific resistance) of the aramid composite conductive fiber is tested by adopting a resistivity tester, wherein the resistivity tester is purchased from Nantong macro laboratory instruments Inc., and the model is HD2514N;
The mechanical properties (tensile strength and elongation at break) of the aramid composite conductive fibers were tested using an electronic universal tester available from Instron under the model number 34TM-30;
the method comprises the steps of testing the binding fastness (washing fastness) of conductive fillers in the aramid fiber composite conductive fiber by adopting a washing fastness testing machine, wherein the washing fastness testing machine is purchased from Darong textile instruments Inc., and the model is SW-12J;
the operation methods of all the instruments are operated according to the instrument instructions.
Further, the para-aramid fiber is para-aramid filament with fineness of 222-3330 dtex.
Further, the diameter of the aramid nanofiber is 12-15nm, and the length is 4-7 mu m.
Further, the aramid nanofiber is one of para-aramid chopped fiber, para-aramid fibrid and para-aramid filament.
Further, the conductive filler is one or more of graphene, carbon nano tube and graphene-like 2D structure MXene, wherein the graphene-like 2D structure MXene is a two-dimensional material researched by American university Lei Saier and is a two-dimensional transition metal carbide, nitride or carbonitride layered material.
The invention also provides a preparation method of the aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: immersing the aramid nanofibers into an alkali solution to obtain an alkali solution pretreated aramid nanofiber mixture, adding dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, and stirring to obtain an aramid nanofiber solution;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, and uniformly mixing to obtain conductive filler dispersion liquid;
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: adding the conductive filler dispersion liquid prepared in the step 2 into the aramid nanofiber solution in the step 1, and stirring to obtain an aramid nanofiber-conductive filler dispersion liquid, wherein the aramid nanofiber-conductive filler dispersion liquid comprises one or more of an aramid nanofiber-conductive filler combination, an alkaline compound and dimethyl sulfoxide, wherein the aramid nanofiber-conductive filler combination is formed by interaction between an aramid nanofiber and a conductive filler, and the interaction comprises one or more of a hydrogen bond formed between carbonyl in the aramid nanofiber and hydroxyl of the conductive filler, a hydrogen bond formed between carbonyl in the aramid nanofiber and carboxyl of the conductive filler, pi-pi interaction formed between pi electron cloud on a carbon-oxygen double bond in the conductive filler and pi electron cloud on a carbon-oxygen double bond in the aramid nanofiber, and pi-pi interaction formed between pi electron cloud on a carbon-oxygen double bond in the conductive filler and pi electron cloud on a benzene ring in the aramid nanofiber;
Step 4, preparing aramid composite conductive fibers: the method comprises the steps of taking para-aramid fiber as a base material, mixing an aramid nanofiber-conductive filler dispersion liquid with the para-aramid fiber, swelling the para-aramid fiber by the aid of ultrasound, enabling the surface of the para-aramid fiber to form microcracks with the width of 100-300nm, enabling an aramid nanofiber-conductive filler combination in the aramid nanofiber-conductive filler dispersion liquid to form hydrogen bonds with the para-aramid fiber, uniformly dispersing the aramid nanofiber-conductive filler combination on the surface of the para-aramid fiber and inside the microcracks, obtaining an aramid composite conductive fiber crude product, and drying and/or reducing the aramid composite conductive fiber crude product to obtain the aramid composite conductive fiber.
Further, the alkaline solution in the step 1 contains an alkaline compound and deionized water, and the mass ratio of the alkaline compound to the deionized water is (0.02-1): 5, the mass ratio of the aramid nanofiber to the alkaline compound is 1:1, the concentration of the aramid nanofiber in the aramid nanofiber solution is 0.0002-0.01 g/ml,
the concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers by the volume of deionized water and dimethyl sulfoxide in step 1.
Further, in the step 1, the soaking temperature is room temperature, the soaking time is 5-10min, the stirring time is 5-20min, the stirring temperature is room temperature, and the stirring speed is 500-1500r/min.
Further, in the step 2, the concentration of the conductive filler in the conductive filler dispersion is 0.04-0.16 g/ml,
the concentration of the conductive filler is calculated by dividing the mass of the conductive filler by the volume of dimethyl sulfoxide in the step 2.
Further, the conductive filler is one or more of graphene, carbon nano tubes and graphene-like 2D structure MXene.
Further, when the conductive filler is graphene, the conductive filler dispersion liquid is graphene-dimethyl sulfoxide dispersion liquid, and the preparation steps are as follows: dispersing graphene in water to prepare a graphene dispersion liquid, wherein the mass ratio of the graphene to the graphene dispersion liquid is (1-4): 50, adding the graphene dispersion liquid into dimethyl sulfoxide, performing ultrasonic dispersion for 2 hours under the condition that the ultrasonic power is 100-200W to obtain a graphene-dimethyl sulfoxide mixture, and performing spin evaporation on the graphene-dimethyl sulfoxide mixture to obtain the graphene-dimethyl sulfoxide dispersion liquid, wherein the mass ratio of the graphene dispersion liquid to the dimethyl sulfoxide is 20:11.
Further, when the conductive filler is a carbon nanotube, the conductive filler dispersion is a carbon nanotube-dimethyl sulfoxide dispersion, and the preparation steps are as follows: and (3) placing the carbon nano tube in dimethyl sulfoxide, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain the carbon nano tube-dimethyl sulfoxide dispersion liquid.
Further, when the conductive filler is a graphene-like 2D structure MXene, the conductive filler dispersion liquid is an MXene-dimethyl sulfoxide dispersion liquid, and the preparation steps are as follows: and placing the graphene-like 2D structure MXene in dimethyl sulfoxide, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain MXene-dimethyl sulfoxide dispersion liquid.
Further, when the conductive filler is a graphene-like 2D structure MXene and carbon nanotubes, the conductive filler dispersion is an MXene-carbon nanotube-dimethyl sulfoxide dispersion, and the preparation steps are as follows: placing the graphene-like 2D structure MXene in dimethyl sulfoxide, adding a carbon nano tube, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain the MXene-carbon nano tube-dimethyl sulfoxide dispersion liquid.
Further, when the conductive filler is graphene-like 2D structure MXene, carbon nanotubes and graphene, the conductive filler dispersion is MXene-carbon nanotubes-graphene-dimethyl sulfoxide dispersion, and the preparation steps are: placing the graphene-like 2D structure MXene in dimethyl sulfoxide, adding a carbon nano tube, adding graphene-dimethyl sulfoxide dispersion liquid, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain the MXene-carbon nano tube-graphene-dimethyl sulfoxide dispersion liquid.
Further, the graphene is graphene oxide.
Further, the carbon nanotubes are single-walled carbon nanotubes.
Further, the graphene-like 2D structure MXene is Ti 3 C 2 T x The preparation process of the MXene material comprises the following steps: titanium aluminum carbide (Ti 3 AlC 2 ) Adding MAX phase ceramic material and lithium fluoride into 9 mol/L hydrochloric acid solution, stirring at 35 ℃ to obtain Ti 3 C 2 T x MXene material, ti with deionized water 3 C 2 T x The MXene material is washed to be neutral and then dispersed in dimethyl sulfoxide to obtain MXene-dimethyl sulfoxide dispersion liquid;
the titanium aluminum carbide (Ti 3 AlC 2 ) The mass ratio of MAX phase ceramic material to lithium fluoride is (1-4): (1.6-6.4), and the volume of hydrochloric acid solution is titanium aluminum carbide (Ti) 3 AlC 2 ) 25 times the mass of the MAX phase ceramic material.
Further, the stirring speed in the step 3 is 1000-4500 r/min, and the reaction time is 10-60 min.
Further, the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid in the step 3 is 2-8 g/ml,
the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is calculated by dividing the mass of the conductive filler by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion liquid in the step 3.
Further, the alkaline compound in the step 3 is one of potassium hydroxide, potassium tert-butoxide and potassium ethoxide.
Further, the bath ratio of the para-aramid fiber to the aramid nanofiber-conductive filler dispersion in the step 4 is 1:50.
Further, the ultrasonic power in the step 4 is 100-200W, the ultrasonic time is 5-30 min, and the ultrasonic temperature is room temperature.
Further, the drying condition in the step 4 is that the drying is carried out for 2-4 hours at the heating temperature of 80-100 ℃.
Further, the reduction condition in the step 4 is that 5 g/L sodium hydrosulfite solution is used for reduction for 30 min at 95 ℃.
Further, sodium hydrosulfite contained in the sodium hydrosulfite solution is sodium hydrosulfite, the solvent is deionized water, and the sodium hydrosulfite is used for reducing graphene.
The invention also provides a material, which comprises the aramid composite conductive fiber.
The invention also provides an intelligent bracelet, which comprises the material.
The invention also provides a mobile phone, which comprises the material.
The invention also provides a stealth fighter, which comprises the material.
The invention has the beneficial effects that:
1. the aramid fiber composite conductive fiber prepared by the invention takes para-aramid fiber as a base material, the dispersion liquid of the aramid nanofiber and the conductive filler swells the para-aramid fiber under the assistance of ultrasound, so that microcracks with the width of 100-300nm are formed on the surface of the para-aramid fiber, meanwhile, the combination of the aramid nanofiber and the conductive filler in the dispersion liquid of the aramid nanofiber and the conductive filler forms hydrogen bonds with the para-aramid fiber, the combination of the aramid nanofiber and the conductive filler is uniformly dispersed on the surface of the para-aramid fiber and the inside of the microcracks to form the aramid fiber composite conductive fiber, and the conductive filler is led to the aramid nanofiber, thereby solving the problems of poor mechanical strength, lack of flexibility, low combination degree with the aramid fiber, low strength, poor flexibility and the like of the final composite conductive material in the prior art;
2. According to the invention, the aramid fiber composite conductive fiber is prepared by adopting an ultrasonic method, on one hand, the ultrasonic is matched with dimethyl sulfoxide, so that macroscopic para-aramid fiber can be swelled; on the other hand, the ultrasonic waves can enable the aramid nanofiber-conductive filler combination to be uniformly dispersed on the surface of the para-aramid fiber and the inside of the microcracks without aggregation;
3. the aramid nanofiber-conductive filler conjugate consists of an aramid nanofiber and a conductive filler through interaction, wherein the interaction mode comprises one or more of hydrogen bonds formed between carbonyl groups in the aramid nanofiber and hydroxyl groups and carboxyl groups of the conductive filler or pi-pi conjugation formed between carbonyl groups in the aramid nanofiber and carboxyl groups of the conductive filler, and the interaction can improve the washing stability of the aramid composite conductive fiber, namely, the washing fastness is improved from 1 level in the prior art to 2-4 levels;
4. according to the preparation method, the aramid nanofibers are immersed in the alkali solution to obtain an alkali solution pretreated aramid nanofiber mixture, dimethyl sulfoxide is added into the alkali solution pretreated aramid nanofiber mixture and then stirred, the specific alkali solution immersion treatment can greatly shorten the dissolution time of the aramid nanofibers, and the preparation method is simple and is matched with a specific process to greatly shorten the production period;
5. The aramid fiber composite conductive fiber prepared by the invention has wide application fields, such as the technical fields of intelligent wearing, electronic communication or aerospace, and the like, and particularly has good development prospect when applied to intelligent bracelets, mobile phones or stealth fighters.
Drawings
FIG. 1 is a schematic view of an aramid composite conductive fiber sample in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the swollen para-aramid fiber in example 1 of the present invention;
fig. 3 is a tensile test chart of the aramid composite conductive fiber in example 2 of the present invention.
Detailed Description
Example 1 sample one
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 0.02g of potassium hydroxide, adding 5mL of deionized water, stirring at normal temperature until the potassium hydroxide is completely dissolved to prepare an alkali solution, adding 0.02g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.0002 g/mL,
The concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (0.02 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml),
in the embodiment, the aramid nanofiber is para-aramid chopped fiber, the diameter of the aramid nanofiber is 12-15nm, and the length of the aramid nanofiber is 4-7 mu m;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
specifically, in this embodiment, the conductive filler is Ti 3 C 2 T x The preparation process of the MXene material comprises the following steps: 2g of titanium aluminum carbide (Ti 3 AlC 2 ) MAX phase ceramic material and 3.2g lithium fluoride are added into 50mL hydrochloric acid solution with the concentration of 9 mol/L, and the mixture is stirred at the constant temperature of 35 ℃ to obtain Ti 3 C 2 T x MXene material, ti with deionized water 3 C 2 T x Washing the MXene material to neutrality, taking 4g Ti 3 C 2 T x MXene material fractionDispersing in 100mL dimethyl sulfoxide, performing ultrasonic dispersion for 4h under the condition of ultrasonic power of 100W to obtain MXene-dimethyl sulfoxide dispersion liquid, namely conductive filler dispersion liquid, wherein the concentration of conductive filler in the conductive filler dispersion liquid is 0.04 g/mL,
the concentration of the conductive filler is calculated by dividing the mass (4 g) of the conductive filler by the volume (100 mL) of the dimethyl sulfoxide in the step 2;
Step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: the mechanical stirrer was set at a rotational speed of 1000 r/min, and the 50 mL conductive filler dispersion (containing 2g Ti) prepared in step 2 was added to the 50 mL aramid nanofiber solution in step 1 3 C 2 T x MXene material), stirring for 10 min to obtain aramid nanofiber-conductive filler dispersion liquid, wherein the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is 2g/ml,
the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is calculated by dividing the mass of the conductive filler (2 g) by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion in step 3 (100 ml).
Step 4, preparing aramid composite conductive fibers: the preparation method comprises the steps of taking para-aramid fiber with fineness of 222 dtex as a base material, mixing 100 mL aramid nanofiber-conductive filler dispersion liquid with 2.0g of para-aramid fiber, carrying out ultrasonic swelling for 5 min at room temperature under the ultrasonic power of 100W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, and drying the aramid composite conductive fiber crude product under the condition of drying for 2h at the heating temperature of 80 ℃ to obtain the aramid composite conductive fiber, namely a sample I.
FIG. 1 is a schematic view of a sample, aramid composite conductive fiber.
As shown in FIG. 2, a scanning electron microscope image of the para-aramid fiber after swelling is shown.
Example 2 sample two
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 0.02g of potassium hydroxide, adding 5mL of deionized water, stirring at normal temperature until the potassium hydroxide is completely dissolved to prepare an alkali solution, adding 0.02g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.0002 g/mL,
the concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (0.02 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml).
In the embodiment, the aramid nanofiber is para-aramid chopped fiber, the diameter of the aramid nanofiber is 12-15nm, and the length of the aramid nanofiber is 4-7 mu m;
Step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
specifically, in this embodiment, the conductive filler is graphene oxide, the conductive filler dispersion liquid is a graphene-dimethyl sulfoxide dispersion liquid, and the preparation steps include: dispersing 2g of graphene in 98mL of water to prepare a graphene dispersion liquid with the concentration of 2wt%, adding 100g of graphene dispersion liquid into 55g of dimethyl sulfoxide (with the volume of 50 mL), performing ultrasonic dispersion for 2 hours under the condition of the ultrasonic power of 100W to obtain a graphene-dimethyl sulfoxide mixture, performing rotary evaporation on the graphene-dimethyl sulfoxide mixture to obtain a graphene-dimethyl sulfoxide dispersion liquid, namely a conductive filler dispersion liquid, wherein the concentration of a conductive filler in the conductive filler dispersion liquid is 0.04g/mL,
the concentration of the conductive filler is calculated by dividing the mass (2 g) of the conductive filler by the volume (50 mL) of the dimethyl sulfoxide in the step 2;
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: setting the rotating speed of a mechanical stirrer to be 1000 r/min, adding the 50mL conductive filler dispersion liquid prepared in the step 2 into the 50mL aramid nanofiber solution in the step 1, and stirring for 10 min to obtain an aramid nanofiber-conductive filler dispersion liquid, wherein the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is 2wt%.
Step 4, preparing aramid composite conductive fibers: the preparation method comprises the steps of taking para-aramid fiber with fineness of 222 dtex as a base material, mixing 100 mL aramid nanofiber-conductive filler dispersion liquid with 2.0 g para-aramid fiber, carrying out ultrasonic swelling for 5min at room temperature under the ultrasonic power of 100W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, drying the aramid composite conductive fiber crude product, reducing for 30 min at 95 ℃ by using 100 mL 5g/L sodium hydrosulfite solution, taking out, washing and drying to obtain the aramid composite conductive fiber, namely a second sample, wherein the drying and drying conditions are that the drying or drying are carried out at the heating temperature of 80 ℃.
The sodium hydrosulfite contained in the sodium hydrosulfite solution is sodium hydrosulfite, and the solvent is deionized water.
The second sample was subjected to a tensile test, as shown in fig. 3, which is a tensile test graph of the aramid composite conductive fiber, and as the tensile force increases, the displacement of the aramid composite conductive fiber increases, and when the tensile force is 602.14N, the aramid composite conductive fiber breaks.
Example 3 sample three
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 0.02g of potassium hydroxide, adding 5mL of deionized water, stirring at normal temperature until the potassium hydroxide is completely dissolved to prepare an alkali solution, adding 0.02g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.0002 g/mL,
The concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (0.02 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml),
in the embodiment, the aramid nanofiber is para-aramid chopped fiber, the diameter of the aramid nanofiber is 12-15nm, and the length of the aramid nanofiber is 4-7 mu m;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
specifically, in this embodiment, the conductive filler is a single-walled carbon nanotube, the conductive filler dispersion liquid is a carbon nanotube-dimethyl sulfoxide dispersion liquid, and the preparation steps are as follows: placing 2g of single-wall carbon nano tube in 50mL of dimethyl sulfoxide, performing ultrasonic dispersion for 4 hours under the condition of ultrasonic power of 100W to obtain carbon nano tube-dimethyl sulfoxide dispersion liquid, namely conductive filler dispersion liquid, wherein the concentration of conductive filler in the conductive filler dispersion liquid is 0.04g/mL,
the concentration of the conductive filler is calculated by dividing the mass (2 g) of the conductive filler by the volume (50 mL) of the dimethyl sulfoxide in the step 2;
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: setting the rotating speed of a mechanical stirrer to be 1000 r/min, adding 50mL of the conductive filler dispersion liquid prepared in the step 2 into 50mL of the aramid nanofiber solution in the step 1, stirring for 10 min to obtain an aramid nanofiber-conductive filler dispersion liquid, wherein the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is 2g/mL,
The concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is calculated by dividing the mass of the conductive filler (2 g) by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion in step 3 (100 mL).
Step 4, preparing aramid composite conductive fibers: the preparation method comprises the steps of taking para-aramid fiber with fineness of 222 dtex as a base material, mixing 100 mL aramid nanofiber-conductive filler dispersion liquid with 2.0 g para-aramid fiber, carrying out ultrasonic swelling for 5min at room temperature under the ultrasonic power of 100W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, and drying the aramid composite conductive fiber crude product under the condition of drying at the heating temperature of 80 ℃ for 2h to obtain an aramid composite conductive fiber, namely a sample III.
Example 4 sample four
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 1g of potassium tert-butoxide, adding 5mL of deionized water, stirring at normal temperature until the potassium tert-butoxide is completely dissolved to prepare an alkali solution, adding 1g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.01 g/mL,
The concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (1 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml),
in the embodiment, the aramid nanofibers are para-aramid fibrids, the diameter of the aramid nanofibers is 12-15nm, and the length of the aramid nanofibers is 4-7 mu m;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
specifically, in this embodiment, the conductive filler is Ti 3 C 2 T x The preparation process of the MXene material comprises the following steps: 8g of titanium aluminum carbide (Ti 3 AlC 2 ) MAX phase ceramic material and 12.8g lithium fluoride are added into 200mL hydrochloric acid solution with the mol/L concentration of 9, and the mixture is stirred at the constant temperature of 35 ℃ to obtain Ti 3 C 2 T x MXene material, ti with deionized water 3 C 2 T x The MXene material is washed to be neutral, 16g of Ti is taken 3 C 2 T x Dispersing the MXene material in 100mL of dimethyl sulfoxide, carrying out ultrasonic dispersion for 4 hours under the condition of ultrasonic power of 100W to obtain MXene-dimethyl sulfoxide dispersion liquid, namely conductive filler dispersion liquid, wherein the concentration of the conductive filler in the conductive filler dispersion liquid is 0.16g/mL,
the concentration of the conductive filler is calculated by dividing the mass (16 g) of the conductive filler by the volume (100 mL) of the dimethyl sulfoxide in the step 2;
Step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: the 50 mL conductive filler dispersion (containing 8g Ti) prepared in step 2 was added to the 50 mL aramid nanofiber solution in step 1 by setting the mechanical stirrer rotation speed to 4500 r/min 3 C 2 T x MXene material), stirring for 60 min to obtain aramid nanofiber-conductive filler dispersion liquid, wherein the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is 8g/ml,
the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is calculated by dividing the mass of the conductive filler (8 g) by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion in step 3 (100 ml).
Step 4, preparing aramid composite conductive fibers: the preparation method comprises the steps of taking para-aramid fiber with fineness of 3300 dtex as a base material, mixing 100. 100 mL aramid nanofiber-conductive filler dispersion liquid with 2.0 g para-aramid fiber, carrying out ultrasonic swelling for 30min at room temperature under ultrasonic power of 200W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, and drying the aramid composite conductive fiber crude product under the condition of drying at 80 ℃ for 2h to obtain an aramid composite conductive fiber, namely a sample IV.
Example 5 sample five
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 1g of potassium ethoxide, adding 5mL of deionized water, stirring at normal temperature until the potassium ethoxide is completely dissolved to prepare an alkali solution, adding 1g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.01 g/mL,
the concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (1 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml),
in the embodiment, the aramid nanofiber is para-aramid filament, the diameter of the aramid nanofiber is 12-15nm, and the length of the aramid nanofiber is 4-7 mu m;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
Specifically, in this embodiment, the conductive filler is graphene oxide, the conductive filler dispersion liquid is a graphene-dimethyl sulfoxide dispersion liquid, and the preparation steps include: dispersing 8g of graphene in 92mL of water to prepare a graphene dispersion liquid with the concentration of 8wt%, adding 100g of graphene dispersion liquid into 55g of dimethyl sulfoxide (with the volume of 50 mL), performing ultrasonic dispersion for 2 hours under the condition of the ultrasonic power of 100W to obtain a graphene-dimethyl sulfoxide mixture, performing rotary evaporation on the graphene-dimethyl sulfoxide mixture to obtain a graphene-dimethyl sulfoxide dispersion liquid, namely a conductive filler dispersion liquid, wherein the concentration of a conductive filler in the conductive filler dispersion liquid is 0.16g/mL,
the concentration of the conductive filler is calculated by dividing the mass (8 g) of the conductive filler by the volume (50 mL) of the dimethyl sulfoxide in the step 2;
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: setting the rotating speed of a mechanical stirrer to be 4500 r/min, adding the 50mL conductive filler dispersion prepared in the step 2 into the 50mL aramid nanofiber solution in the step 1, stirring for 60 min to obtain an aramid nanofiber-conductive filler dispersion, wherein the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is 8 g/ml,
The concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is calculated by dividing the mass of the conductive filler (8 g) by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion in step 3 (100 ml).
Step 4, preparing aramid composite conductive fibers: the preparation method comprises the steps of taking para-aramid fiber with fineness of 3300 dtex as a base material, mixing 100 mL aramid nanofiber-conductive filler dispersion liquid with 2.0 g para-aramid fiber, carrying out ultrasonic swelling for 30min at room temperature under ultrasonic power of 200W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, drying the aramid composite conductive fiber crude product, reducing for 30min at 95 ℃ by using 100 mL 5g/L sodium hydrosulfite solution, taking out, washing and drying to obtain the aramid composite conductive fiber, namely a sample five, wherein the drying and drying conditions are that the aramid composite conductive fiber is dried or dried for 2h at 80 ℃.
The sodium hydrosulfite contained in the sodium hydrosulfite solution is sodium hydrosulfite, and the solvent is deionized water.
Example 6 sample six
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 1g of potassium hydroxide, adding 5mL of deionized water, stirring at normal temperature until the potassium hydroxide is completely dissolved to prepare an alkali solution, adding 1g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.1 g/mL,
The concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (1 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml),
in the embodiment, the aramid nanofiber is para-aramid chopped fiber, the diameter of the aramid nanofiber is 12-15nm, and the length of the aramid nanofiber is 4-7 mu m;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
specifically, in this embodiment, the conductive filler is a single-walled carbon nanotube, the conductive filler dispersion liquid is a carbon nanotube-dimethyl sulfoxide dispersion liquid, and the preparation steps are as follows: placing 8g single-wall carbon nano tube in 50mL dimethyl sulfoxide, and performing ultrasonic dispersion for 4h under the condition of ultrasonic power of 100W to obtain carbon nano tube-dimethyl sulfoxide dispersion liquid, namely conductive filler dispersion liquid, wherein the concentration of conductive filler in the conductive filler dispersion liquid is 0.16g/mL,
the concentration of the conductive filler is calculated by dividing the mass (8 g) of the conductive filler by the volume (50 mL) of the dimethyl sulfoxide in the step 2;
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: setting the rotating speed of a mechanical stirrer to be 4500 r/min, adding 50mL of the conductive filler dispersion liquid prepared in the step 2 into 50mL of the aramid nanofiber solution in the step 1, stirring for 10 min to obtain an aramid nanofiber-conductive filler dispersion liquid, wherein the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is 8 g/mL,
The concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is calculated by dividing the mass of the conductive filler (8 g) by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion in step 3 (100 ml).
Step 4, preparing aramid composite conductive fibers: the preparation method comprises the steps of taking para-aramid fiber with fineness of 222 dtex as a base material, mixing 100 mL aramid nanofiber-conductive filler dispersion liquid with 2.0 g para-aramid fiber, carrying out ultrasonic swelling for 5min at room temperature under the ultrasonic power of 100W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, and drying the aramid composite conductive fiber crude product under the condition of drying at the heating temperature of 80 ℃ for 2h to obtain an aramid composite conductive fiber, namely a sample six.
Example 7 sample seven
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 0.5g of potassium hydroxide, adding 5mL of deionized water, stirring at normal temperature until the potassium hydroxide is completely dissolved to prepare an alkali solution, adding 0.5g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.0005 g/mL,
The concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (0.05 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml),
in the embodiment, the aramid nanofiber is para-aramid chopped fiber, the diameter of the aramid nanofiber is 12-15nm, and the length of the aramid nanofiber is 4-7 mu m;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
specifically, in this embodiment, the conductive filler is Ti 3 C 2 T x The MXene material and the single-wall carbon nano tube,
Ti 3 C 2 T x the preparation process of the MXene material comprises the following steps: 5g of titanium aluminum carbide (Ti 3 AlC 2 ) MAX phase ceramic material and 8g lithium fluoride are added into 125mL 9 mol/L hydrochloric acid solution, and are stirred at the constant temperature of 35 ℃ to obtain Ti 3 C 2 T x MXene material, ti with deionized water 3 C 2 T x The MXene material was washed to neutrality,
taking 5g of Ti 3 C 2 T x Dispersing the MXene material in 100mL of dimethyl sulfoxide, adding 5g of single-walled carbon nanotube into the mixture, performing ultrasonic dispersion for 4 hours under the condition of ultrasonic power of 100W to obtain MXene-carbon nanotube-dimethyl sulfoxide dispersion liquid, namely conductive filler dispersion liquid, wherein the concentration of conductive filler in the conductive filler dispersion liquid is 0.1 g/mL,
The concentration of the conductive filler is calculated by dividing the total mass (10 g) of the conductive filler by the volume (100 mL) of the dimethyl sulfoxide in the step 2;
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: the mechanical stirrer was set at a rotational speed of 4500 r/min, and the 50 mL conductive filler dispersion (Ti-containing) prepared in step 2 was added to the 50 mL aramid nanofiber solution in step 1 3 C 2 T x MXene material and single-walled carbon nanotubes 5g in total) and stirring for 60 minObtaining the dispersion liquid of the aramid nanofiber and the conductive filler, wherein the concentration of the conductive filler in the dispersion liquid of the aramid nanofiber and the conductive filler is 5 g/ml,
the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is calculated by dividing the mass of the conductive filler (5 g) by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion in step 3 (100 ml).
Step 4, preparing aramid composite conductive fibers: the preparation method comprises the steps of taking para-aramid fiber with fineness of 3300 dtex as a base material, mixing 100. 100mL aramid nanofiber-conductive filler dispersion liquid with 2.0 g para-aramid fiber, carrying out ultrasonic swelling for 30min at room temperature under ultrasonic power of 200W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, and drying the aramid composite conductive fiber crude product under the condition of drying at 80 ℃ for 2h to obtain an aramid composite conductive fiber, namely a sample seven.
Example 8 sample eight
The embodiment provides a preparation method of an aramid composite conductive fiber, which comprises the following steps:
step 1, preparing an aramid nanofiber solution: weighing 0.1g of potassium hydroxide, adding 5mL of deionized water, stirring at normal temperature until the potassium hydroxide is completely dissolved to prepare an alkali solution, adding 0.1g of aramid nanofibers into the alkali solution, soaking for 5min at room temperature to obtain an alkali solution pretreated aramid nanofiber mixture, adding 95mL of dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, stirring for 20min at a stirring speed of 1000r/min to obtain an aramid nanofiber solution, wherein the concentration of the aramid nanofibers in the aramid nanofiber solution is 0.001 g/mL,
the concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers (0.1 g) by the sum of the volumes of deionized water and dimethyl sulfoxide in step 1 (100 ml),
in the embodiment, the aramid nanofiber is para-aramid chopped fiber, the diameter of the aramid nanofiber is 12-15nm, and the length of the aramid nanofiber is 4-7 mu m;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, uniformly mixing to obtain conductive filler dispersion liquid,
Specifically, in this embodiment, the conductive filler is Ti 3 C 2 T x MXene material, single-walled carbon nanotubes and graphene oxide,
Ti 3 C 2 T x the preparation process of the MXene material comprises the following steps: 4g of titanium aluminum carbide (Ti 3 AlC 2 ) MAX phase ceramic material and 6.4g lithium fluoride are added into 100mL hydrochloric acid solution with the concentration of 9 mol/L, and the mixture is stirred at the constant temperature of 35 ℃ to obtain Ti 3 C 2 T x MXene material, ti with deionized water 3 C 2 T x The MXene material was washed to neutrality,
4g of Ti 3 C 2 T x Dispersing the MXene material in 50mL of dimethyl sulfoxide, adding 4g single-walled carbon nanotubes into the mixture, dispersing the mixture in 50mL of graphene oxide-dimethyl sulfoxide dispersion liquid (containing 2g of graphene oxide) with the concentration of 0.04g/mL of graphene oxide, uniformly mixing the mixture, carrying out ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100W to obtain MXene-carbon nanotubes-graphene-dimethyl sulfoxide dispersion liquid, namely conductive filler dispersion liquid, wherein the concentration of conductive filler in the conductive filler dispersion liquid is 0.1g/mL,
the concentration of the conductive filler is calculated by dividing the total mass (10 g) of the conductive filler by the sum of the volumes of the dimethyl sulfoxide in the step 2 (100 mL);
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: setting the rotation speed of a mechanical stirrer to 2000 r/min, adding the 50mL conductive filler dispersion (containing Ti) prepared in the step 2 to the 50mL aramid nanofiber solution in the step 1 3 C 2 T x The MXene material, the single-walled carbon nanotube and the graphene oxide are 5g in total, the aramid nanofiber-conductive filler dispersion liquid is obtained after stirring for 60 min, the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is 5 g/ml,
the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion is calculated by dividing the mass of the conductive filler (5 g) by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion in step 3 (100 ml).
Step 4, preparing aramid composite conductive fibers: mixing 100 mL aramid nanofiber-conductive filler dispersion liquid with 2 g para-aramid fibers serving as a base material, carrying out ultrasonic swelling for 20min at room temperature under the ultrasonic power of 150W, obtaining an aramid composite conductive fiber crude product under the assistance of ultrasonic, drying the aramid composite conductive fiber crude product, then reducing for 30 min at 95 ℃ by using 5 g/L sodium hydrosulfite solution, taking out, washing and drying to obtain the aramid composite conductive fiber, namely a sample eight, wherein the drying and drying conditions are that the aramid composite conductive fiber is dried or dried for 2h at the heating temperature of 80 ℃.
The sodium hydrosulfite contained in the sodium hydrosulfite solution is sodium hydrosulfite, and the solvent is deionized water.
Comparative example 1 sample nine
The comparative example was different from example 1 in that step 1 and step 3 in example 1 were omitted, the para-aramid fiber in step 4 was directly put in the conductive filler dispersion in step 2 to be ultrasonically swelled, and the other conditions were the same as example 1, to obtain sample nine.
Comparative example 2 sample ten
The comparative example differs from example 8 in that step 1 and step 3 in example 8 were omitted, the para-aramid fiber in step 4 was directly put in the conductive filler dispersion in step 2 to be ultrasonically swelled, and the other conditions were the same as example 8, to obtain sample ten.
Comparative example 3 sample eleven
Compared with the Chinese patent application CN 115029939A, the nylon mesh is replaced by para-aramid chopped fibers.
Firstly, dissolving aramid nanofibers in dimethyl sulfoxide to prepare an aramid nanofiber solution with the mass concentration of 1%, wherein the aramid nanofibers are para-aramid chopped fibers, scraping the aramid nanofiber solution on para-aramid filaments to obtain aramid nanofibers @ aramid filaments, dissolving carbon nanotubes in the dimethyl sulfoxide to prepare a carbon nanotube dispersion with the mass concentration of 5%, coating the carbon nanotube dispersion on the aramid nanofibers @ aramid filaments, and obtaining a sample eleven.
For the samples in each example and comparative example:
the conductivity (specific resistance) of the samples was tested using a resistivity tester, available from Nantong macro laboratory instruments, inc., model HD2514N.
Testing the mechanical properties (tensile strength and elongation at break) of the samples using an electronic universal tester available from Instron, model 34TM-30;
the binding fastness (washing fastness) of the conductive filler in the sample was tested using a washing fastness tester purchased from grong textile instruments, inc., model SW-12J.
The operation methods of all the instruments are operated according to the instrument instructions.
The test indexes are summarized as the test index comparison results of each sample in table 1:
table 1 test index comparison results for each sample
As can be seen from the comparison, the specific resistance of the aramid composite conductive fiber prepared by the preparation method is as low as 5.6X10 2 Omega cm (example 5), and the tensile strength is 17.79 cN/dtex, and the color fastness to washing reaches 4 levels at the highest, which shows that the aramid fiber composite conductive fiber has good mechanical property and conductive property, and the conductive filler is firmly combined. Comparing the specific resistance of each embodiment, the specific resistance is reduced along with the increase of the content of the conductive filler, and the conductivity is improved; the comparison of the washing fastness shows that the increase of the concentration of the aramid nanofiber solution can improve the washing fastness of the aramid composite conductive fiber; the tensile strength comparison shows that the increase of the content of the conductive filler damages the tensile strength of the color fastness to water washing, but the damage degree is small, and the tensile strength of the aramid composite conductive fiber added with the carbon nano tube is highest for three different conductive fillers.
In summary, the aramid fiber composite conductive fiber prepared by the invention takes para-aramid fiber as a base material, the dispersion liquid of the aramid nanofiber and the conductive filler swells the para-aramid fiber under the assistance of ultrasound, so that microcracks with the width of 100-300nm are formed on the surface of the para-aramid fiber, meanwhile, the combination of the aramid nanofiber and the conductive filler in the dispersion liquid of the aramid nanofiber and the conductive filler and the para-aramid fiber form hydrogen bonds, the combination of the aramid nanofiber and the conductive filler is uniformly dispersed on the surface of the para-aramid fiber and the inside of the microcracks, the aramid fiber composite conductive fiber is formed, and the conductive filler is led to the aramid nanofiber, so that the problems of poor mechanical strength, lack of flexibility, low combination degree with the aramid fiber, low strength, poor flexibility and the like of a final composite conductive material in the prior art are solved; the prepared conductive fiber has good conductivity, mechanical strength and flexibility, and has wide application prospect in the fields of conductivity, static resistance, electromagnetic shielding, intelligent wearing and the like.
It will be understood that the invention is not limited to what has been described above and shown in the drawings, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (28)
1. The aramid fiber composite conductive fiber is characterized in that an aramid fiber nanofiber-conductive filler conjugate is uniformly dispersed on the surface of a para-aramid fiber with microcracks on the surface and the inside of the microcracks to form the aramid fiber composite conductive fiber, the width of the microcracks is 100-300nm, and the mass ratio of the aramid fiber nanofiber to the conductive filler in the aramid fiber nanofiber-conductive filler conjugate is (0.02-1): (2-16), wherein the mass ratio of the aramid nanofiber-conductive filler combination to the para-aramid fiber is (2.02-17): 2, the specific resistance of the aramid composite conductive fiber is 5.6X10 2 -3.4×10 5 Omega cm, tensile strength of 17.32-18.56 cN/dtex, elongation at break of 5.91-6.34% and washing fastness of 2-4 grade.
2. The aramid composite conductive fiber of claim 1, wherein the para-aramid fiber is para-aramid filament with a fineness of 222-3330 dtex.
3. The aramid composite conductive fiber of claim 1, wherein the aramid nanofiber has a diameter of 12-15nm and a length of 4-7 μm.
4. The aramid composite conductive fiber of claim 3, wherein the aramid nanofiber is one of para-aramid chopped fiber, para-aramid fibrid, para-aramid filament.
5. The aramid composite conductive fiber of claim 1, wherein the conductive filler is one or more of graphene, carbon nanotubes, and graphene-like 2D structures MXene.
6. A method for preparing the aramid composite conductive fiber as claimed in any one of claims 1 to 5, comprising the steps of:
step 1, preparing an aramid nanofiber solution: immersing the aramid nanofibers into an alkali solution to obtain an alkali solution pretreated aramid nanofiber mixture, adding dimethyl sulfoxide into the alkali solution pretreated aramid nanofiber mixture, and stirring to obtain an aramid nanofiber solution;
step 2, preparing conductive filler dispersion liquid: adding conductive filler into dimethyl sulfoxide, and uniformly mixing to obtain conductive filler dispersion liquid;
step 3, preparing an aramid nanofiber-conductive filler dispersion liquid: adding the conductive filler dispersion liquid prepared in the step 2 into the aramid nanofiber solution in the step 1, and stirring to obtain an aramid nanofiber-conductive filler dispersion liquid, wherein the aramid nanofiber-conductive filler dispersion liquid comprises one or more of an aramid nanofiber-conductive filler combination, an alkaline compound and dimethyl sulfoxide, wherein the aramid nanofiber-conductive filler combination is formed by interaction between an aramid nanofiber and a conductive filler, and the interaction comprises one or more of a hydrogen bond formed between carbonyl in the aramid nanofiber and hydroxyl of the conductive filler, a hydrogen bond formed between carbonyl in the aramid nanofiber and carboxyl of the conductive filler, pi-pi interaction formed between pi electron cloud on a carbon-oxygen double bond in the conductive filler and pi electron cloud on a carbon-oxygen double bond in the aramid nanofiber, and pi-pi interaction formed between pi electron cloud on a carbon-oxygen double bond in the conductive filler and pi electron cloud on a benzene ring in the aramid nanofiber;
Step 4, preparing aramid composite conductive fibers: the method comprises the steps of taking para-aramid fiber as a base material, mixing an aramid nanofiber-conductive filler dispersion liquid with the para-aramid fiber, swelling the para-aramid fiber by the aid of ultrasound, enabling the surface of the para-aramid fiber to form microcracks with the width of 100-300nm, enabling an aramid nanofiber-conductive filler combination in the aramid nanofiber-conductive filler dispersion liquid to form hydrogen bonds with the para-aramid fiber, uniformly dispersing the aramid nanofiber-conductive filler combination on the surface of the para-aramid fiber and inside the microcracks, obtaining an aramid composite conductive fiber crude product, and drying and/or reducing the aramid composite conductive fiber crude product to obtain the aramid composite conductive fiber.
7. The method for preparing the aramid composite conductive fiber according to claim 6, wherein the alkaline solution in the step 1 contains an alkaline compound and deionized water, and the mass ratio of the alkaline compound to the deionized water is (0.02-1): 5, the mass ratio of the aramid nanofiber to the alkaline compound is 1:1, the concentration of the aramid nanofiber in the aramid nanofiber solution is 0.0002-0.01 g/ml,
The concentration of the aramid nanofibers is calculated by dividing the mass of the aramid nanofibers by the volume of deionized water and dimethyl sulfoxide in step 1.
8. The method for preparing aramid fiber composite conductive fiber according to claim 7, wherein in the step 1, the dipping temperature is room temperature, the dipping time is 5-10min, the stirring temperature is room temperature, and the stirring speed is 500-1500r/min.
9. The method for preparing aramid composite conductive fiber according to claim 6, wherein in the step 2, the concentration of the conductive filler in the conductive filler dispersion is 0.04-0.16 g/ml,
the concentration of the conductive filler is calculated by dividing the mass of the conductive filler by the volume of dimethyl sulfoxide in the step 2.
10. The method for preparing the aramid fiber composite conductive fiber according to claim 6, wherein the conductive filler is one or more of graphene, carbon nano tube and graphene-like 2D structure MXene.
11. The method for preparing the aramid fiber composite conductive fiber according to claim 10, wherein when the conductive filler is graphene, the conductive filler dispersion liquid is graphene-dimethyl sulfoxide dispersion liquid, and the preparation steps are as follows: dispersing graphene in water to prepare a graphene dispersion liquid, wherein the mass ratio of the graphene to the graphene dispersion liquid is (1-4): 50, adding the graphene dispersion liquid into dimethyl sulfoxide, performing ultrasonic dispersion for 2 hours under the condition that the ultrasonic power is 100-200W to obtain a graphene-dimethyl sulfoxide mixture, and performing spin evaporation on the graphene-dimethyl sulfoxide mixture to obtain the graphene-dimethyl sulfoxide dispersion liquid, wherein the mass ratio of the graphene dispersion liquid to the dimethyl sulfoxide is 20:11.
12. The method for preparing the aramid composite conductive fiber according to claim 10, wherein when the conductive filler is a carbon nanotube, the conductive filler dispersion is a carbon nanotube-dimethyl sulfoxide dispersion, and the preparation steps are as follows: and (3) placing the carbon nano tube in dimethyl sulfoxide, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain a carbon nano tube-dimethyl sulfoxide dispersion liquid.
13. The method for preparing the aramid fiber composite conductive fiber according to claim 10, wherein when the conductive filler is a graphene-like 2D structure MXene, the conductive filler dispersion liquid is an MXene-dimethyl sulfoxide dispersion liquid, and the preparation steps are as follows: and placing the graphene-like 2D structure MXene in dimethyl sulfoxide, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain MXene-dimethyl sulfoxide dispersion liquid.
14. The method for preparing the aramid fiber composite conductive fiber according to claim 10, wherein when the conductive filler is a graphene-like 2D structure MXene and carbon nanotubes, the conductive filler dispersion is an MXene-carbon nanotube-dimethyl sulfoxide dispersion, and the preparation steps are as follows: placing the graphene-like 2D structure MXene in dimethyl sulfoxide, adding a carbon nano tube, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain the MXene-carbon nano tube-dimethyl sulfoxide dispersion liquid.
15. The preparation method of the aramid fiber composite conductive fiber according to claim 10, wherein when the conductive filler is graphene-like 2D structure MXene, carbon nanotubes and graphene, the conductive filler dispersion is MXene-carbon nanotubes-graphene-dimethyl sulfoxide dispersion, and the preparation steps are as follows: placing the graphene-like 2D structure MXene in dimethyl sulfoxide, adding a carbon nano tube, adding graphene-dimethyl sulfoxide dispersion liquid, and performing ultrasonic dispersion for 4 hours under the condition that the ultrasonic power is 100-200W to obtain the MXene-carbon nano tube-graphene-dimethyl sulfoxide dispersion liquid.
16. The method for preparing the aramid composite conductive fiber according to claim 10, wherein the graphene is graphene oxide;
the carbon nanotubes are single-walled carbon nanotubes;
the graphene-like 2D structure MXene is Ti 3 C 2 T x The preparation process of the MXene material comprises the following steps: adding titanium aluminum carbide MAX phase ceramic material and lithium fluoride into 9 mol/L hydrochloric acid solution, stirring at 35 ℃ constant temperature to obtain Ti 3 C 2 T x MXene material, ti is treated by deionized water 3 C 2 T x The MXene material is washed to be neutral and then dispersed in dimethyl sulfoxide to obtain MXene-dimethyl sulfoxide dispersion liquid;
the mass ratio of the titanium aluminum carbide MAX phase ceramic material to the lithium fluoride is (1-4) (1.6-6.4), and the volume of the hydrochloric acid solution is 25 times of the mass of the titanium aluminum carbide MAX phase ceramic material.
17. The method for preparing aramid composite conductive fiber according to claim 6, wherein the stirring speed in the step 3 is 1000-4500 r/min, and the reaction time is 10-60 min.
18. The method for preparing aramid composite conductive fiber according to claim 17, wherein the concentration of the conductive filler in the dispersion of aramid nanofiber-conductive filler in the step 3 is 2-8 g/ml,
the concentration of the conductive filler in the aramid nanofiber-conductive filler dispersion liquid is calculated by dividing the mass of the conductive filler by the sum of the volumes of the aramid nanofiber solution and the conductive filler dispersion liquid in the step 3.
19. The method for preparing aramid composite conductive fiber according to claim 6, wherein the alkaline compound in the step 3 is one of potassium hydroxide, potassium tert-butoxide and potassium ethoxide.
20. The method for preparing an aramid composite conductive fiber according to claim 6, wherein the bath ratio of para-aramid fiber to aramid nanofiber-conductive filler dispersion in the step 4 is 1:50.
21. The method for preparing aramid fiber composite conductive fiber according to claim 20, wherein the ultrasonic power in the step 4 is 100-200W, the ultrasonic time is 5-30 min, and the ultrasonic temperature is room temperature.
22. The method for preparing aramid composite conductive fiber of claim 21, wherein the drying condition in step 4 is drying at a heating temperature of 80-100 ℃ for 2-4 hours.
23. The method for preparing aramid composite conductive fiber of claim 22, wherein the reducing condition in the step 4 is to reduce with 5 g/L sodium hydrosulfite solution at 95 ℃ for 30 min.
24. The method for preparing aramid fiber composite conductive fiber of claim 23, wherein the sodium hydrosulfite contained in the sodium hydrosulfite solution is sodium hydrosulfite and the solvent is deionized water.
25. A material comprising the aramid composite conductive fiber of any one of claims 1 to 5.
26. A smart bracelet, comprising the material of claim 25.
27. A cell phone comprising the material of claim 25.
28. A stealth warplane comprising the material of claim 25.
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