CN108831752B - A kind of aramid fiber electrochemical capacitor and preparation method thereof - Google Patents

A kind of aramid fiber electrochemical capacitor and preparation method thereof Download PDF

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CN108831752B
CN108831752B CN201810639595.3A CN201810639595A CN108831752B CN 108831752 B CN108831752 B CN 108831752B CN 201810639595 A CN201810639595 A CN 201810639595A CN 108831752 B CN108831752 B CN 108831752B
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aramid fiber
nano silver
silver grain
fiber beam
cladding
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CN108831752A (en
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顾嫒娟
方浩
梁国正
袁莉
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Suzhou University
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Suzhou University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/48—Conductive polymers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention discloses a kind of aramid fiber electrochemical capacitors and preparation method thereof.Nano silver grain, carbon nanotube, polypyrrole are successively coated on to the surface of aramid fiber in a manner of being chemically bonded, prepare aramid fiber electrode.Two beam aramid fiber electrodes and electrolyte are wound, aramid fiber electrochemical capacitor is obtained.Compared with the polymer fiber electrochemical capacitor of prior art preparation, the features such as aramid fiber electrochemical capacitor provided by the invention has both high specific capacitance, high-energy density, high-mechanical property, high stability, good flexible and wearable property；Preparation method technique is controllable, is suitble to large-scale application.

Description

A kind of aramid fiber electrochemical capacitor and preparation method thereof
Technical field
The present invention relates to fiber electrodes, electrochemical capacitor and preparation method thereof, and in particular to a kind of aramid fiber electrification Learn capacitor and preparation method thereof.
Background technique
Fast development with wearable smart machine and the urgent need to sustainable energy, high-energy density fiber Electrochemical capacitor is small-sized with its, lightweight, flexibility, efficiently, the advantages that being easily integrated, show huge application prospect.Fiber Electrochemical capacitor is constituted by fiber electrode with electrolyte with parallel, winding, coaxial structure, therefore its performance largely takes Certainly in fiber electrode material.In order to make wearable fiber electrochemical capacitor move towards application from concept, it is badly in need of exploitation and has both well The high-performance fiber electrode of flexible, wearable property and excellent chemical property.
So far, multiple fiber be used to prepare the electrode of fiber capacitor.Wherein, carbon fiber is frangible, cannot be frequent It is bent and is not easy to weave；For metallic fiber (such as stainless steel fibre, nickel fiber) though having ductility, matter is hard, has plasticity； Graphene fiber and carbon nano-tube fibre are not suitable for large-scale production due to higher cost.Polymer fiber is flexible due to having, It is the ideal material for preparing wearable fiber electrode.
However, there are three bottlenecks for existing polymer fiber electrode and its capacitor.First, the conductivity of electrode is low, Lead to low energy densities.Polymer fiber generally passes through coated with carbon material (such as carbon nanotube, graphene), conducting polymer Object (such as polyaniline, polypyrrole) or transition metal oxide (such as manganese dioxide, zinc oxide) obtain capacitive property.Although packet Covered capacitance material, but polymer fiber does not contribute capacitive property, thus the specific capacitance of polymer fiber electrode and its The energy density of capacitor is generally relatively low.Second, it is bonded poor between inorganic coating and fibrous matrix, is repeatedly deforming Or clad may fall off performance is caused to deteriorate after electrochemistry circulation, cause the wearable property of fiber capacitor poor.Third, The mechanical performance of existing polymer fiber capacitor can't reach requirement.Currently, usually fine with polyester fiber, polyamide The matrix as polymer fiber capacitor such as dimension, polyurethane fiber, cotton fiber, their tensile property is usually very low, mainly Meet the application in daily life, and is not suitable for the field that ballistic resistant products etc. have high requirements to mechanical performance.
Therefore, preparation has both the polymer fiber capacitor of excellent chemical property and good flexible, wearable property It is still a challenge.In polymer fiber, aramid fiber is due to outstanding mechanical performance, hot property and chemical resistance Can, huge concern has just been received since birth.But, aramid fiber electricity identical as other polymers fiber capacitor The problem of capacitive property of container and cementability between inorganic coating object, still has to be solved.Development has both excellent electricity The aramid fiber capacitor of chemical property, mechanical performance and good flexible, wearable property has significant application value.
Summary of the invention
In order to overcome the shortcomings of the prior art, the purpose of the present invention is to provide having both, high specific capacitance, high-energy are close Degree, high-mechanical property, high stability, good flexible and wearable property aramid fiber electrode and electrochemical capacitor, system Preparation Method is suitble to large-scale application.
Realizing the technical solution of the object of the invention is:
A kind of preparation method of aramid fiber electrochemical capacitor, comprises the following steps:
(1) aramid fiber beam is immersed in the aqueous solution containing Dopamine hydrochloride and Tri(Hydroxymethyl) Amino Methane Hydrochloride In, reaction obtains the aramid fiber beam of poly-dopamine cladding；
(2) polyvinylpyrrolidone is added in silver ammino solution, obtains solution C；The aramid fiber that poly-dopamine is coated Beam is added in solution C, then glucose solution is added dropwise, and reaction obtains the aramid fiber beam of Nano silver grain cladding；
(3) the aramid fiber beam of Nano silver grain cladding is added and contains γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy In the aqueous solution of silane, reaction obtains the aramid fiber beam that Nano silver grain of the surface with epoxy group coats；
(4) the aramid fiber beam that the Nano silver grain by surface with epoxy group coats is added containing band carboxyl carbon nanotube Ethanol solution in, reaction obtain the aramid fiber beam of carbon nanotube and Nano silver grain double-coating；
(5) the aramid fiber beam of carbon nanotube and Nano silver grain double-coating is added in the aqueous solution containing pyrroles, Silver nitrate aqueous solution is added dropwise again, reaction obtains the aramid fiber beam of polypyrrole, carbon nanotube and three layers of Nano silver grain cladding；
(6) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene It in alcogel, then takes out and is intertwined, solidify at room temperature, obtain aramid fiber electrochemical capacitor；By polyethylene Alcohol, acid and water heat 1~10h at 50~100 DEG C, obtain polyvinyl alcohol gel after cooling.
The invention also discloses the aramid fiber electrochemical capacitors prepared according to above-mentioned preparation method.
The invention also discloses the aramid fiber beams of polypyrrole, carbon nanotube and three layers of Nano silver grain cladding in preparation virtue Application in synthetic fibre fiber electrochemical capacitor.
In the application, the preparation for the aramid fiber beam that the polypyrrole, carbon nanotube and three layers of Nano silver grain coat Method comprises the following steps:
(1) aramid fiber beam is immersed in the aqueous solution containing Dopamine hydrochloride and Tri(Hydroxymethyl) Amino Methane Hydrochloride In, reaction obtains the aramid fiber beam of poly-dopamine cladding；
(2) polyvinylpyrrolidone is added in silver ammino solution, obtains solution C；The aramid fiber that poly-dopamine is coated Beam is added in solution C, then glucose solution is added dropwise, and reaction obtains the aramid fiber beam of Nano silver grain cladding；
(3) the aramid fiber beam of Nano silver grain cladding is added and contains γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy In the aqueous solution of silane, reaction obtains the aramid fiber beam that Nano silver grain of the surface with epoxy group coats；
(4) the aramid fiber beam that the Nano silver grain by surface with epoxy group coats is added containing band carboxyl carbon nanotube Ethanol solution in, reaction obtain the aramid fiber beam of carbon nanotube and Nano silver grain double-coating；
(5) the aramid fiber beam of carbon nanotube and Nano silver grain double-coating is added in the aqueous solution containing pyrroles, Silver nitrate aqueous solution is added dropwise again, reaction obtains the aramid fiber beam of polypyrrole, carbon nanotube and three layers of Nano silver grain cladding.
In above-mentioned technical proposal, in step (1), the aramid fiber includes Fanglun 1414, gathers One or more of mpd-i fiber, poly fiber；Contain Dopamine hydrochloride and three hydroxyl first The pH value of the aqueous solution of base aminomethane hydrochloride is 8.5, reacts and reacts 5~48h for shaken at room temperature；After reaction by fiber Taking-up washes and dries, and obtains the aramid fiber beam of poly-dopamine cladding；Dopamine hydrochloride, trishydroxymethylaminomethane hydrochloric acid Salt, aramid fiber beam mass ratio be (0.1~1): (0.05~0.5): (0.1~1).
In above-mentioned technical proposal, in step (2), react for 10~60min of oscillating reactions at room temperature；It after reaction will be fine Dimension is taken out and is washed and dried, and the aramid fiber beam of Nano silver grain cladding is obtained；Silver nitrate, polyvinylpyrrolidone, glucose, The mass ratio of the aramid fiber beam of poly-dopamine cladding is (0.5~5): (0.05~0.5): (1~10): (0.1~1)；Step (3) in, the mass ratio for the aramid fiber beam that γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane, Nano silver grain coat is (0.5~5): (0.1~1)；In step (4), the virtue of the Nano silver grain cladding with carboxyl carbon nanotube, surface with epoxy group The mass ratio of synthetic fibre fibre bundle is (0.5~5): (0.1~1).
In above-mentioned technical proposal, in step (3), react in 50~100 DEG C of 1~10h of oscillating reactions；After reaction will Fiber taking-up washes and dries, and obtains the aramid fiber beam that Nano silver grain of the surface with epoxy group coats；γ-(2,3- ring The third oxygen of oxygen) propyl trimethoxy silicane, Nano silver grain cladding aramid fiber beam mass ratio be (0.5~5): (0.1~ 1).
In above-mentioned technical proposal, in step (4), react in 50~80 DEG C of oscillating reactions 5~for 24 hours；After reaction will Fiber taking-up washes and dries, and obtains the aramid fiber band carboxyl carbon nanometer of carbon nanotube and Nano silver grain double-coating The mass ratio for the aramid fiber beam that the Nano silver grain of pipe, surface with epoxy group coats is (0.5~5): (0.1~1).
In above-mentioned technical proposal, in step (5), the carbon nanotube includes multi-walled carbon nanotube, single-walled carbon nanotube, carbon One or more of nanotube bundle；Silver nitrate, pyrroles, carbon nanotube and Nano silver grain double-coating aramid fiber beam Mass ratio is (0.2~4): (0.1~2): (0.1~1)；Reaction is 5~48h of oscillating reactions at room temperature；It after reaction will be fine Dimension is taken out and is washed and dried, and aramid fiber electrode is obtained.
In above-mentioned technical proposal, in step (6), the acid is phosphoric acid, sulfuric acid or combinations thereof；The matter of polyvinyl alcohol, acid, water Amount is than being (1~20): (1~20): 100.
Aramid fiber electrochemical capacitor disclosed by the invention and preparation method thereof can carry out as follows, in mass ratio:
(1) 0.1~1 part of Dopamine hydrochloride and 0.05~0.5 part of Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100 parts In water, solution A is obtained；0.1~10 part of sodium hydroxide is dissolved in 100 parts of water, sodium hydrate aqueous solution is obtained；Use hydroxide Sodium water solution adjusts the pH value of solution A to 8.5, obtains solution B；0.1~1 part of aramid fiber beam is immersed in solution B, in room Temperature is lower to vibrate 5~48h；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained；
(2) 0.5~5 part of silver nitrate is dissolved in 50 parts of water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.05~0.5 part of polyvinylpyrrolidone, obtains solution C；1~10 part of glucose is dissolved in 50 parts of water, glucose is obtained Aqueous solution；The aramid fiber beam of 0.1~1 part of poly-dopamine cladding is added into solution C, vibrates at room temperature, while adding dropwise Enter glucose solution, continues to vibrate 10~60min at room temperature；Fiber is taken out after reaction, is washed and dried, is obtained The aramid fiber beam of Nano silver grain cladding；
(3) 0.5~5 part of γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100 parts of water, adds 0.1 The aramid fiber beam of~1 part of poly-dopamine and Nano silver grain cladding, in 50~100 DEG C of 1~10h of oscillation；After reaction will Fiber takes out, washes and dries, and obtains the aramid fiber beam that Nano silver grain of the surface with epoxy group coats；
(4) 0.5~5 part of carbon nanotube with carboxyl is added in 80 parts of ethyl alcohol, adds 0.1~1 part of surface and has Epoxy group Nano silver grain cladding aramid fiber beam, in 50~80 DEG C vibrate 5~for 24 hours；Fiber is taken out after reaction, It washes and dries, obtains the aramid fiber beam of carbon nanotube and Nano silver grain double-coating；
(5) 0.2~4 part of silver nitrate is dissolved in 50 parts of water, obtains silver nitrate aqueous solution；0.1~2 part of pyrroles is added In 50 parts of water, the aramid fiber beam of 0.1~1 part of carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, Silver nitrate aqueous solution is added dropwise simultaneously, continues to vibrate 5~48h at room temperature；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam of polypyrrole, carbon nanotube and three layers of Nano silver grain cladding；
(6) 1~20 part of polyvinyl alcohol, 1~20 part of acid and 100 parts of water are heated into 1~10h at 50~100 DEG C, after cooling Obtain polyvinyl alcohol gel；
(7) by two strands of polypyrroles of step (5) preparation, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding It is immersed in polyvinyl alcohol gel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrification Learn capacitor.
Compared with prior art, the beneficial effect that the present invention obtains is:
1, the present invention devises the compound coating layer of silver, carbon nanotube and polypyrrole, by the high capacitance of polypyrrole and silver, carbon The high conductivity of nanotube combines, simultaneously because there are synergistic effect, the electrochemical capacitors of acquisition between silver and carbon nanotube Device has the outstanding chemical properties such as high specific capacitance, high-energy density.
2, the present invention generates clad in aramid fiber surface by hydridization and complex technique, clad and fibrous matrix it Between there are chemical action, the presence of silver and carbon nanotube can prevent the structure of polypyrrole from destroying, and the electrochemistry of acquisition is electric Container has high stability and good wearable property.
3, the present invention uses aramid fiber to obtain as the matrix of fiber electrochemical capacitor and have both good flexibility, height The fiber electrochemical capacitor of tensile strength and modulus.
Detailed description of the invention
Fig. 1 is the poly- paraphenylene terephthalamide of the Fanglun 1414 of the offer of embodiment 3, poly-dopamine cladding Poly- pair of Fanglun 1414, multi-walled carbon nanotube cladding that p-phenylenediamine fiber, Nano silver grain coat The stereoscan photograph of the Fanglun 1414 of phenylene terepthalamide's fiber and polypyrrole cladding；
Fig. 2 is the poly- paraphenylene terephthalamide of the Fanglun 1414 of the offer of embodiment 3, poly-dopamine cladding P-phenylenediamine fiber, the Fanglun 1414 of Nano silver grain cladding, γ-(the third oxygen of 2,3- epoxy) propyl three The poly- paraphenylene terephthalamide that the Fanglun 1414 of methoxy silane cladding, multi-walled carbon nanotube coat is to benzene two The infrared spectroscopy of the Fanglun 1414 of amine fiber and polypyrrole cladding；
Fig. 3 is Fanglun 1414 and the polypyrrole for the multi-walled carbon nanotube cladding that embodiment 3 provides The Raman spectrum of the Fanglun 1414 of cladding；
Fig. 4 is the poly- paraphenylene terephthalamide of the Fanglun 1414 of the offer of embodiment 3, poly-dopamine cladding Poly- pair of Fanglun 1414, multi-walled carbon nanotube cladding that p-phenylenediamine fiber, Nano silver grain coat The X-ray diffractogram of the Fanglun 1414 of phenylene terepthalamide's fiber and polypyrrole cladding；
Fig. 5 is the length for the aramid fiber electrochemical capacitor that comparative example 1, comparative example 2, comparative example 3 and embodiment 3 provide Specific capacitance, volumetric capacitance and quality are than capacitor histogram；
Fig. 6 is the length for the aramid fiber electrochemical capacitor that comparative example 1, comparative example 2, comparative example 3 and embodiment 3 provide Energy density, volume energy density and mass energy density histogram；
Fig. 7 is capacitor and initial electricity of the aramid fiber electrochemical capacitor of the offer of embodiment 3 under differently curved angle The ratio of appearance；
Fig. 8 is that the aramid fiber electrochemical capacitor that comparative example 1, comparative example 2, comparative example 3 and embodiment 3 provide is carrying out The conservation rate of capacitor after 90 ° of bendings of different numbers；
Fig. 9 is that the stress-strain of the Fanglun 1414 for the polypyrrole cladding that embodiment 3 provides is bent Line.
Specific embodiment
With reference to the accompanying drawing, embodiment and comparative example, technical solution of the present invention will be further described.
The preparation of the aramid fiber and its capacitor of 1 polypyrrole of comparative example cladding
(1) 0.85g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.67g pyrroles In, 0.5g Fanglun 1414's beam is added, is vibrated at room temperature, while it is water-soluble that silver nitrate is added dropwise Liquid, continuation are vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, the aramid fiber for obtaining polypyrrole cladding is fine Tie up beam；
(2) 10g polyvinyl alcohol, 10g phosphoric acid and 100mL water are heated at 90 DEG C 5h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue；
(3) the aramid fiber beam that two strands of polypyrroles coat is immersed in polyvinyl alcohol gel, fiber is taken out and wound Together, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.Its length specific capacitance, volumetric capacitance and matter Specific capacitance histogram is measured, after length energy density, volume energy density and mass energy density histogram and differently curved number Capacity retention see attached drawing 5,6,8 respectively.
The preparation of 2 polypyrrole of comparative example and the aramid fiber and its capacitor of Nano silver grain double-coating
(1) 0.2g Dopamine hydrochloride and 0.16g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；2g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution is adjusted with sodium hydrate aqueous solution The pH value of A obtains solution B to 8.5；0.5g Fanglun 1414's beam is immersed in solution B, at room temperature Oscillation is for 24 hours；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained；
(2) 1.5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.25g polyvinylpyrrolidone, obtains solution C；3g glucose is dissolved in 50mL water, glucose solution is obtained；Xiang Rong The aramid fiber beam of 0.5g poly-dopamine cladding is added in liquid C, vibrates at room temperature, while glucose solution is added dropwise, 30min is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, the virtue of Nano silver grain cladding is obtained Synthetic fibre fibre bundle；
(3) 0.85g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.67g pyrroles In, the aramid fiber beam of 0.5g Nano silver grain cladding is added, is vibrated at room temperature, while it is water-soluble that silver nitrate is added dropwise Liquid, continuation are vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, polypyrrole and Nano silver grain are obtained The aramid fiber beam of double-coating；
(4) 10g polyvinyl alcohol, 10g phosphoric acid and 100mL water are heated at 90 DEG C 5h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue；
(5) the aramid fiber beam of two strands of polypyrroles and Nano silver grain double-coating is immersed in polyvinyl alcohol gel, Fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.Its length is than electricity Hold, volumetric capacitance and quality are than capacitor histogram, length energy density, volume energy density and mass energy density histogram Attached drawing 5,6,8 is seen respectively with the capacity retention after differently curved number.
The preparation of 3 polypyrrole of comparative example and the aramid fiber and its capacitor of carbon nanotube double-coating
(1) 0.2g Dopamine hydrochloride and 0.16g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；2g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution is adjusted with sodium hydrate aqueous solution The pH value of A obtains solution B to 8.5；0.5g Fanglun 1414's beam is immersed in solution B, at room temperature Oscillation is for 24 hours；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained；
(2) 2.5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- adds 0.5g The aramid fiber beam of dopamine cladding, in 65 DEG C of oscillation 5h；Fiber is taken out after reaction, is washed and dried, surface is obtained Aramid fiber beam with epoxy group；
(3) multi-walled carbon nanotube of the 1g with carboxyl is added in 100mL ethyl alcohol, adds the surface 0.5g with epoxy group Nano silver grain cladding aramid fiber beam, in 70 DEG C of oscillation 12h；Fiber is taken out after reaction, is washed and dried, is obtained The aramid fiber beam coated to carbon nanotube；
(4) 0.85g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.67g pyrroles In, the aramid fiber beam of 0.5g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, continuation is vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, polypyrrole is obtained With the aramid fiber beam of carbon nanotube double-coating；
(5) 10g polyvinyl alcohol, 10g phosphoric acid and 100mL water are heated at 90 DEG C 5h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue；
(6) the aramid fiber beam of two strands of polypyrroles and carbon nanotube double-coating is immersed in polyvinyl alcohol gel, it will Fiber takes out and is intertwined, and gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.Its length specific capacitance, Volumetric capacitance and quality than capacitor histogram, length energy density, volume energy density and mass energy density histogram and Capacity retention after differently curved number is shown in attached drawing 5,6,8 respectively.
Embodiment 1
(1) 0.1g Dopamine hydrochloride and 0.05g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；0.1g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；It is adjusted with sodium hydrate aqueous solution molten The pH value of liquid A obtains solution B to 8.5；0.1g Fanglun 1414's beam is immersed in solution B, in room temperature Lower oscillation 5h；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained；
(2) 0.5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.05g polyvinylpyrrolidone, obtains solution C；1g glucose is dissolved in 50mL water, glucose solution is obtained；Xiang Rong The aramid fiber beam of 0.1g poly-dopamine cladding is added in liquid C, vibrates at room temperature, while glucose solution is added dropwise, 10min is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, the virtue of Nano silver grain cladding is obtained Synthetic fibre fibre bundle；
(3) 0.5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- adds 0.1g The aramid fiber beam of dopamine and Nano silver grain cladding, in 50 DEG C of oscillation 1h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats；
(4) multi-walled carbon nanotube of the 0.5g with carboxyl is added in 100mL ethyl alcohol, adds the surface 0.1g with epoxy The aramid fiber beam of the Nano silver grain cladding of base, in 50 DEG C of oscillation 5h；Fiber is taken out after reaction, is washed and dried, Obtain the aramid fiber beam of carbon nanotube and Nano silver grain double-coating；
(5) 0.2g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.1g pyrroles In, the aramid fiber beam of 0.1g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, 5h is vibrated in continuation at room temperature；After reaction by fiber take out, wash and dry, obtain polypyrrole, The aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding；
(6) 1g polyvinyl alcohol, 1g phosphoric acid and 100mL water are heated at 50 DEG C 1h, obtains polyvinyl alcohol gel after cooling；
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.
Embodiment 2
(1) 0.2g Dopamine hydrochloride and 0.16g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；2g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution is adjusted with sodium hydrate aqueous solution The pH value of A obtains solution B to 8.5；0.5g Fanglun 1414's beam is immersed in solution B, at room temperature Oscillation is for 24 hours；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained；
(2) 1.5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.25g polyvinylpyrrolidone, obtains solution C；3g glucose is dissolved in 50mL water, glucose solution is obtained；Xiang Rong The aramid fiber beam of 0.5g poly-dopamine cladding is added in liquid C, vibrates at room temperature, while glucose solution is added dropwise, 30min is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, the virtue of Nano silver grain cladding is obtained Synthetic fibre fibre bundle；
(3) 2.5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- adds 0.5g The aramid fiber beam of dopamine and Nano silver grain cladding, in 65 DEG C of oscillation 5h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats；
(4) multi-walled carbon nanotube of the 1g with carboxyl is added in 100mL ethyl alcohol, adds the surface 0.5g with epoxy group Nano silver grain cladding aramid fiber beam, in 70 DEG C of oscillation 12h；Fiber is taken out after reaction, is washed and dried, is obtained To the aramid fiber beam of carbon nanotube and Nano silver grain double-coating；
(5) 0.42g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.34g pyrroles In, the aramid fiber beam of 0.5g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, continuation is vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, poly- pyrrole is obtained It coughs up, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding；
(6) 10g polyvinyl alcohol, 10g phosphoric acid and 100mL water are heated at 90 DEG C 5h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue；
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.
Embodiment 3
(1)~(4) and embodiment 2 are consistent；
(5) 0.85g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.67g pyrroles In, the aramid fiber beam of 0.5g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, continuation is vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, poly- pyrrole is obtained It coughs up, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding.
(6)~(7) and embodiment 2 are consistent, obtain aramid fiber electrochemical capacitor.
Referring to attached drawing 1, it is the Fanglun 1414 that the embodiment of the present invention 3 provides, poly-dopamine packet The aramid fiber covered, the aramid fiber of Nano silver grain cladding, the aramid fiber of carbon nanotube and Nano silver grain double-coating With the stereoscan photograph of polypyrrole, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding.Poly- paraphenylene terephthalamide P-phenylenediamine fiber surface is bright and clean；The aramid fiber surface of poly-dopamine cladding is coarse, there is uniform clad；Nano silver grain The aramid fiber beam surface of cladding is dispersed with the silver particles that diameter is about 30nm；Carbon nanotube and Nano silver grain double-coating Aramid fiber surface has silver particles and carbon nanotube；The aramid fiber of polypyrrole, carbon nanotube and three layers of Nano silver grain cladding Surface coats the polypyrrole particle that diameter is about 1 μm.
Referring to attached drawing 2, it is Fanglun 1414's beam that the embodiment of the present invention 3 provides, poly-dopamine The aramid fiber beam of cladding, the aramid fiber beam of Nano silver grain cladding, Nano silver grain of the surface with epoxy group coat The aramid fiber beam and polypyrrole, carbon nanotube and silver nanoparticle of aramid fiber beam, carbon nanotube and Nano silver grain double-coating The infrared spectroscopy of the aramid fiber beam of three layers of particle cladding.Compared with Fanglun 1414's beam, poly-dopamine There is the asymmetric stretching vibration (2929cm of methylene in the map of the aramid fiber beam of cladding-1) and symmetrical stretching vibration (2851cm-1) characteristic peak, this comes from poly-dopamine.Compared with the aramid fiber beam of Nano silver grain cladding, surface band There is the spectrogram of the aramid fiber beam of the Nano silver grain cladding of epoxy group epoxy group asymmetric stretching vibration peak (845cm occur-1 And 908cm-1), Si-O-C stretching vibration peak (1034cm-1), Si-O stretching vibration peak (1110cm-1) and Si-CH2- R stretches Contracting vibration peak (1200cm-1), this comes from γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane.And in carbon nanotube and The characteristic peak of epoxy group is not observed in the spectrogram of the aramid fiber beam of Nano silver grain double-coating.Polypyrrole, carbon nanometer Occur in the spectrogram of pipe and the aramid fiber beam of three layers of Nano silver grain cladding from the C-H in plane vibration peak of polypyrrole (1033cm-1), C-C stretching vibration peak (1533cm-1) and pyrrole ring stretching vibration peak (1430cm-1), in 1385cm-1Occur Strong absorption peak is attributed to the interaction between polypyrrole and silver.
Referring to attached drawing 3, it is the aramid fiber fibre of the carbon nanotube that the embodiment of the present invention 3 provides and Nano silver grain double-coating Tie up the Raman spectrum for the aramid fiber beam that beam and polypyrrole, carbon nanotube and three layers of Nano silver grain coat.Carbon nanotube and silver There are the characteristic peaks of carbon material in the spectrogram of the aramid fiber beam of nanoparticle double-coating, are D absorption band (1329cm respectively-1) With G absorption band (1583cm-1), this comes from the carbon nanotube of fiber surface；Polypyrrole, carbon nanotube and Nano silver grain three There are C-H in-plane deformation peak (1000~1150cm in the spectrogram of the aramid fiber beam of layer cladding-1), pyrrole ring stretch peak (1300 ~1410cm-1) and the flexible peak (1600cm of C=C skeleton-1), these are all the characteristic peaks of polypyrrole, and it is poly- to show that fiber surface has Pyrroles's cladding.
Referring to attached drawing 4, it is Fanglun 1414's beam that the embodiment of the present invention 3 provides, poly-dopamine The aramid fiber beam of cladding, the aramid fiber beam of Nano silver grain cladding, the virtue of carbon nanotube and Nano silver grain double-coating The X-ray diffractogram for the aramid fiber beam that synthetic fibre fibre bundle and polypyrrole, carbon nanotube and three layers of Nano silver grain coat.All It can observe that the diffraction maximum of Fanglun 1414 (110) and (200) is superimposed the broad peak to be formed in spectrogram, Show that the structure of cladding front and back fiber is not destroyed；The virtue coated with Fanglun 1414's beam and poly-dopamine Synthetic fibre fibre bundle is compared, the aramid fiber beam of Nano silver grain cladding, and the aramid fiber of carbon nanotube and Nano silver grain double-coating is fine Occur respectively corresponding in the spectrogram for the aramid fiber beam that dimension beam is coated with polypyrrole, carbon nanotube and three layers of Nano silver grain (111), the diffraction maximum of (200), (220), (311) and (222) crystal face, this is the diffraction of face-centred cubic silver, it was demonstrated that fiber table There is silver-colored cladding in face.
Referring to attached drawing 5, it be aramid fiber electrochemical capacitor prepared by the embodiment of the present invention 3 with comparative example 1, compared with Length specific capacitance, volumetric capacitance and the quality specific capacitance of aramid fiber electrochemical capacitor prepared by example 2, comparative example 3.It is real Aramid fiber electrochemical capacitor prepared by example 3 is applied with optimal capacitive property, length, volume, quality specific capacitance point It Wei not 100.1mF/cm, 84.3F/cm3And 24.8F/g；And three kinds of specific capacitances of measuring be above its theoretical value (C Comparative example 2+C Comparative example 3- 2 ×C Comparative example 1, whereinCFor the specific capacitance of measuring), show between silver and carbon nanotube there are synergistic effect, this It may be better conductive network to be formd, to improve electrode since carbon nanotube has filled up the gap between silver particles Conductivity.
Referring to attached drawing 6, it be aramid fiber electrochemical capacitor prepared by the embodiment of the present invention 3 with comparative example 1, compared with Length energy density, volume energy density and the mass-energy of aramid fiber electrochemical capacitor prepared by example 2, comparative example 3 Density.Since energy density is directly proportional to specific capacitance, there is similar rule with specific capacitance, i.e., prepared by embodiment 3 Aramid fiber electrochemical capacitor has highest energy density, and length, volume, mass energy density are respectively 8.9 μ Wh/ cm、7.49mWh/cm3And 2.21mWh/g.
Referring to table 1, it is aramid fiber electrochemical capacitor prepared by the embodiment of the present invention 3 and comparative example 1, comparative example 2, capacity retention of the aramid fiber electrochemical capacitor after 1000 cyclic voltammetrics prepared by comparative example 3.Comparative example 1 Capacitor maintain minimum, the cycle performance of comparative example 2 and comparative example 3 slightly improves, and the cycle performance of embodiment 3 is best.This It is because in cyclic process, swelling and contraction occur in the electrolyte for polypyrrole, and the presence of silver particles, carbon nanotube can be with Prevent the structure of polypyrrole from destroying, to improve cycle performance.Polymer in existing report containing conducting polymer is fine Capacity retention is generally 92% hereinafter, and aramid fiber prepared by the embodiment of the present invention 3 after dimension capacitor is recycled at 1000 times Electrochemical capacitor capacity retention after 1000 circulations reaches 95.2%.
The capacity retention of table 1 embodiment 3 and comparative example 1~3
Comparative example 1 Comparative example 2 Comparative example 3 Embodiment 3
Capacity retention (%) 88.1 90.8 91.0 95.2
Referring to attached drawing 7, it is the aramid fiber electrochemical capacitor of the offer of the embodiment of the present invention 3 under differently curved angle Capacitor and initial capacitance ratio.Even if the bending angle of aramid fiber capacitor reaches 180 °, capacitor also only occurs Small variation shows that aramid fiber electrochemical capacitor has good flexibility.
Referring to attached drawing 8, it be the aramid fiber electrochemical capacitor that the embodiment of the present invention 3 provides and with comparative example 1, ratio Compared with the conservation rate of capacitor after 90 ° of bendings that the aramid fiber electrochemical capacitor that example 2, comparative example 3 provide carries out different numbers.When When number of bends reaches 500 times, the capacity retention of aramid fiber capacitor is 94.5%, higher than comparative example 1(78.8%), is compared Example 2(82.2%) and comparative example 3(87.1%), show that there are good cementabilities between each clad.
Referring to attached drawing 9, it is polypyrrole, carbon nanotube and three layers of the Nano silver grain cladding that the embodiment of the present invention 3 provides Aramid fiber load-deformation curve.The fracture for the aramid fiber that polypyrrole, carbon nanotube and three layers of Nano silver grain coat Elongation is 3.1%, and tensile strength and modulus are up to 2521MPa and 95.4GPa, shows there is good mechanical performance, comparative example The 3 aramid fiber tensile strengths provided and modulus are 2232MPa and 81.9GPa, and comparative example 1, comparative example 2 are lower.
Embodiment 4
(1) 0.2g Dopamine hydrochloride and 0.16g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；2g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution is adjusted with sodium hydrate aqueous solution The pH value of A obtains solution B to 8.5；0.5g Fanglun 1414's beam is immersed in solution B, at room temperature Oscillation is for 24 hours；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained.
(2) 1.5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.25g polyvinylpyrrolidone, obtains solution C；3g glucose is dissolved in 50mL water, glucose solution is obtained；Xiang Rong The aramid fiber beam of 0.5g poly-dopamine cladding is added in liquid C, vibrates at room temperature, while glucose solution is added dropwise, 30min is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, the virtue of Nano silver grain cladding is obtained Synthetic fibre fibre bundle.
(3) 2.5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- adds 0.5g The aramid fiber beam of dopamine and Nano silver grain cladding, in 65 DEG C of oscillation 5h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats.
(4) multi-walled carbon nanotube of the 1g with carboxyl is added in 100mL ethyl alcohol, adds the surface 0.5g with epoxy group Nano silver grain cladding aramid fiber beam, in 70 DEG C of oscillation 12h；Fiber is taken out after reaction, is washed and dried, is obtained To the aramid fiber beam of carbon nanotube and Nano silver grain double-coating.
(5) 1.27g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 1.01g pyrroles In, the aramid fiber beam of 0.5g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, continuation is vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, poly- pyrrole is obtained It coughs up, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding.
(6) 10g polyvinyl alcohol, 10g phosphoric acid and 100mL water are heated at 90 DEG C 5h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue.
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor, In Capacity retention reaches 95.1% after 1000 circulations, and when number of bends reaches 500 times, the capacitor of aramid fiber capacitor is protected Holdup is 94.1%.
Embodiment 5
(1) 1g Dopamine hydrochloride and 0.5g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, obtain solution A；10g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution A is adjusted with sodium hydrate aqueous solution PH value obtains solution B to 8.5；1g Fanglun 1414's beam is immersed in solution B, is vibrated at room temperature 48h；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained.
(2) 5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise, and to silver ammino solution, secondary clearing, addition 0.5g are poly- again Vinylpyrrolidone obtains solution C；10g glucose is dissolved in 50mL water, glucose solution is obtained；Add into solution C The aramid fiber beam for entering 1g poly-dopamine cladding, vibrates, while glucose solution is added dropwise at room temperature, continues in room temperature Lower oscillation 60min；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of Nano silver grain cladding is obtained.
(3) 5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, adds the poly- DOPA of 1g The aramid fiber beam of amine and Nano silver grain cladding, in 100 DEG C of oscillation 10h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats.
(4) multi-walled carbon nanotube of the 5g with carboxyl is added in 100mL ethyl alcohol, adds the surface 1g with epoxy group The aramid fiber beam of Nano silver grain cladding, for 24 hours in 80 DEG C of oscillations；Fiber is taken out after reaction, is washed and dried, is obtained The aramid fiber beam of carbon nanotube and Nano silver grain double-coating.
(5) 4g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；2g pyrroles is added in 50mL water, then The aramid fiber beam of 1g carbon nanotube and Nano silver grain double-coating is added, vibrates at room temperature, while nitric acid is added dropwise 48h is vibrated in silver-colored aqueous solution, continuation at room temperature；Fiber is taken out after reaction, is washed and dried, obtains polypyrrole, carbon is received The aramid fiber beam of mitron and three layers of Nano silver grain cladding.
(6) 20g polyvinyl alcohol, 20g phosphoric acid and 100mL water are heated at 100 DEG C 10h, obtains polyvinyl alcohol after cooling Gel.
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor, In Capacity retention reaches 95.0% after 1000 circulations, and when number of bends reaches 500 times, the capacitor of aramid fiber capacitor is protected Holdup is 94.2%.
Embodiment 6
(1) 0.1g Dopamine hydrochloride and 0.05g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；0.1g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；It is adjusted with sodium hydrate aqueous solution molten The pH value of liquid A obtains solution B to 8.5；0.1g Fanglun 1313 beam is immersed in solution B, in room temperature Lower oscillation 5h；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained.
(2) 0.5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.05g polyvinylpyrrolidone, obtains solution C；1g glucose is dissolved in 50mL water, glucose solution is obtained；Xiang Rong The aramid fiber beam of 0.1g poly-dopamine cladding is added in liquid C, vibrates at room temperature, while glucose solution is added dropwise, 10min is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, the virtue of Nano silver grain cladding is obtained Synthetic fibre fibre bundle.
(3) 0.5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- adds 0.1g The aramid fiber beam of dopamine and Nano silver grain cladding, in 50 DEG C of oscillation 1h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats.
(4) single-walled carbon nanotube of the 0.5g with carboxyl is added in 100mL ethyl alcohol, adds the surface 0.1g with epoxy The aramid fiber beam of the Nano silver grain cladding of base, in 50 DEG C of oscillation 5h；Fiber is taken out after reaction, is washed and dried, Obtain the aramid fiber beam of carbon nanotube and Nano silver grain double-coating.
(5) 0.2g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.1g pyrroles In, the aramid fiber beam of 0.1g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, 5h is vibrated in continuation at room temperature；After reaction by fiber take out, wash and dry, obtain polypyrrole, The aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding.
(6) 1g polyvinyl alcohol, 1g sulfuric acid and 100mL water are heated at 50 DEG C 1h, obtains polyvinyl alcohol gel after cooling.
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.
Embodiment 7
(1) 0.2g Dopamine hydrochloride and 0.16g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；5g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution is adjusted with sodium hydrate aqueous solution The pH value of A obtains solution B to 8.5；0.5g poly fiber's beam is immersed in solution B, is vibrated at room temperature for 24 hours； Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of poly-dopamine cladding is obtained.
(2) 1.5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.25g polyvinylpyrrolidone, obtains solution C；3g glucose is dissolved in 50mL water, glucose solution is obtained；Xiang Rong The aramid fiber beam of 0.5g poly-dopamine cladding is added in liquid C, vibrates at room temperature, while glucose solution is added dropwise, 30min is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, the virtue of Nano silver grain cladding is obtained Synthetic fibre fibre bundle.
(3) 2.5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- adds 0.5g The aramid fiber beam of dopamine and Nano silver grain cladding, in 65 DEG C of oscillation 5h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats.
(4) carbon nano-tube bundle of the 1g with carboxyl is added in 100mL ethyl alcohol, adds the surface 0.5g with epoxy group The aramid fiber beam of Nano silver grain cladding, in 70 DEG C of oscillation 12h；Fiber is taken out after reaction, is washed and dried, is obtained The aramid fiber beam of carbon nanotube and Nano silver grain double-coating.
(5) 0.42g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.34g pyrroles In, the aramid fiber beam of 0.5g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, continuation is vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, poly- pyrrole is obtained It coughs up, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding.
(6) 10g polyvinyl alcohol, 10g phosphoric acid and 100mL water are heated at 90 DEG C 5h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue.
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.
Embodiment 8
(1) 0.2g Dopamine hydrochloride and 0.16g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained Solution A；5g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution is adjusted with sodium hydrate aqueous solution The pH value of A obtains solution B to 8.5；By 0.25g poly(p-phenylene terephthalamide) and 0.25g poly Composite fibre beam is immersed in solution B, is vibrated at room temperature for 24 hours；Fiber is taken out after reaction, is washed and dried, is obtained The aramid fiber beam of poly-dopamine cladding.
(2) 1.5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, is added 0.25g polyvinylpyrrolidone, obtains solution C；3g glucose is dissolved in 50mL water, glucose solution is obtained；Xiang Rong The aramid fiber beam of 0.5g poly-dopamine cladding is added in liquid C, vibrates at room temperature, while glucose solution is added dropwise, 30min is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, the virtue of Nano silver grain cladding is obtained Synthetic fibre fibre bundle.
(3) 2.5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- adds 0.5g The aramid fiber beam of dopamine and Nano silver grain cladding, in 65 DEG C of oscillation 5h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats.
(4) mixture of the single-walled carbon nanotube of the multi-walled carbon nanotube by 0.5g with carboxyl and 0.5g with carboxyl adds Enter in 100mL ethyl alcohol, adds the aramid fiber beam that Nano silver grain of the surface 0.5g with epoxy group coats, vibrated in 70 DEG C 12h；Fiber is taken out after reaction, is washed and dried, the aramid fiber for obtaining carbon nanotube and Nano silver grain double-coating is fine Tie up beam.
(5) 0.85g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 0.67g pyrroles In, the aramid fiber beam of 0.5g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, continuation is vibrated for 24 hours at room temperature；Fiber is taken out after reaction, is washed and dried, poly- pyrrole is obtained It coughs up, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding.
(6) 10g polyvinyl alcohol, 10g sulfuric acid and 100mL water are heated at 90 DEG C 5h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue.
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.
Embodiment 9
(1) 0.6g Dopamine hydrochloride and 0.3g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, are obtained molten Liquid A；8g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution A is adjusted with sodium hydrate aqueous solution PH value to 8.5, obtain solution B；By 0.25g poly(p-phenylene terephthalamide) and 0.25g poly(p-benzamide) composite fibre Beam is immersed in solution B, vibrates 36h at room temperature；Fiber is taken out after reaction, is washed and dried, poly-dopamine is obtained The aramid fiber beam of cladding.
(2) 3g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise to silver ammino solution secondary clearing again, 0.35g is added Polyvinylpyrrolidone obtains solution C；6g glucose is dissolved in 50mL water, glucose solution is obtained；Into solution C The aramid fiber beam of 0.5g poly-dopamine cladding is added, vibrates at room temperature, while glucose solution is added dropwise, continues 45min is vibrated at room temperature；Fiber is taken out after reaction, is washed and dried, the aramid fiber of Nano silver grain cladding is obtained Beam.
(3) 4g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, it is poly- more adds 0.5g The aramid fiber beam of bar amine and Nano silver grain cladding, in 70 DEG C of oscillation 8h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats.
(4) mixture of the carbon nano-tube bundle of the multi-walled carbon nanotube by 1.5g with carboxyl and 1.5g with carboxyl is added In 100mL ethyl alcohol, the aramid fiber beam that Nano silver grain of the surface 0.5g with epoxy group coats is added, is vibrated in 60 DEG C 18h；Fiber is taken out after reaction, is washed and dried, the aramid fiber for obtaining carbon nanotube and Nano silver grain double-coating is fine Tie up beam.
(5) 1.27g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；50mL water is added in 1.01g pyrroles In, the aramid fiber beam of 0.5g carbon nanotube and Nano silver grain double-coating is added, is vibrated at room temperature, while being added dropwise Enter silver nitrate aqueous solution, 36h is vibrated in continuation at room temperature；Fiber is taken out after reaction, is washed and dried, poly- pyrrole is obtained It coughs up, the aramid fiber beam of carbon nanotube and three layers of Nano silver grain cladding.
(6) 15g polyvinyl alcohol, 15g phosphoric acid and 100mL water are heated at 70 DEG C 7h, it is solidifying that polyvinyl alcohol is obtained after cooling Glue.
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.
Embodiment 10
(1) 1g Dopamine hydrochloride and 0.5g Tri(Hydroxymethyl) Amino Methane Hydrochloride are dissolved in 100mL water, obtain solution A；10g sodium hydroxide is dissolved in 100mL water, sodium hydrate aqueous solution is obtained；Solution A is adjusted with sodium hydrate aqueous solution PH value obtains solution B to 8.5；By 0.33g poly(p-phenylene terephthalamide), 0.33g poly and 0.34g poly(p-benzamide) composite fibre beam is immersed in solution B, vibrates 48h at room temperature；Fiber is taken after reaction Out, it washes and dries, obtains the aramid fiber beam of poly-dopamine cladding.
(2) 5g silver nitrate is dissolved in 50mL water, ammonium hydroxide is added dropwise, and to silver ammino solution, secondary clearing, addition 0.5g are poly- again Vinylpyrrolidone obtains solution C；10g glucose is dissolved in 50mL water, glucose solution is obtained；Add into solution C The aramid fiber beam for entering 1g poly-dopamine cladding, vibrates, while glucose solution is added dropwise at room temperature, continues in room temperature Lower oscillation 60min；Fiber is taken out after reaction, is washed and dried, the aramid fiber beam of Nano silver grain cladding is obtained.
(3) 5g γ-(2,3- the third oxygen of epoxy) propyl trimethoxy silicane is added in 100mL water, adds the poly- DOPA of 1g The aramid fiber beam of amine and Nano silver grain cladding, in 100 DEG C of oscillation 10h；Fiber is taken out, cleaned and done after reaction It is dry, obtain the aramid fiber beam that Nano silver grain of the surface with epoxy group coats.
(4) single-walled carbon nanotube and 1g with carboxyl of the multi-walled carbon nanotube by 1g with carboxyl, 1g are with carboxyl The mixture of carbon nano-tube bundle is added in 100mL ethyl alcohol, adds the virtue that Nano silver grain of the surface 1g with epoxy group coats Synthetic fibre fibre bundle, for 24 hours in 80 DEG C of oscillations；Fiber is taken out after reaction, is washed and dried, carbon nanotube and nano grain of silver are obtained The aramid fiber beam of sub- double-coating.
(5) 4g silver nitrate is dissolved in 50mL water, obtains silver nitrate aqueous solution；2g pyrroles is added in 50mL water, then The aramid fiber beam of 1g carbon nanotube and Nano silver grain double-coating is added, vibrates at room temperature, while nitric acid is added dropwise 48h is vibrated in silver-colored aqueous solution, continuation at room temperature；Fiber is taken out after reaction, is washed and dried, obtains polypyrrole, carbon is received The aramid fiber beam of mitron and three layers of Nano silver grain cladding.
(6) 20g polyvinyl alcohol, 10g sulfuric acid, 10g phosphoric acid and 100mL water are heated at 100 DEG C 10h, is obtained after cooling Polyvinyl alcohol gel.
(7) the aramid fiber beam of two strands of polypyrroles, carbon nanotube and three layers of Nano silver grain cladding is immersed in polyethylene In alcogel, fiber is taken out and is intertwined, gel solidifies at room temperature, obtains aramid fiber electrochemical capacitor.

Claims (7)

1. a kind of preparation method of aramid fiber electrochemical capacitor, characterized by comprising the steps of:
(1) aramid fiber beam is immersed in the aqueous solution containing Dopamine hydrochloride and Tri(Hydroxymethyl) Amino Methane Hydrochloride, instead It should obtain the aramid fiber beam of poly-dopamine cladding；
(2) polyvinylpyrrolidone is added in silver ammino solution, obtains solution C；The aramid fiber beam that poly-dopamine coats is added Enter in solution C, then glucose solution is added dropwise, reaction obtains the aramid fiber beam of Nano silver grain cladding；
(3) the aramid fiber beam of Nano silver grain cladding is added and contains γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane Aqueous solution in, reaction obtain surface with epoxy group Nano silver grain coat aramid fiber beam；
(4) by surface with epoxy group Nano silver grain coat aramid fiber beam be added containing band carboxyl carbon nanotube or Containing in the ethanol solution with carboxyl carbon nano-tube bundle, reaction obtains carbon nanotube and the aramid fiber of Nano silver grain double-coating is fine Tie up the aramid fiber beam of beam or carbon nano-tube bundle and Nano silver grain double-coating；
(5) by the aramid fiber beam or carbon nano-tube bundle and Nano silver grain of carbon nanotube and Nano silver grain double-coating bilayer The aramid fiber beam of cladding is added in the aqueous solution containing pyrroles, then silver nitrate aqueous solution is added dropwise, and reaction obtains polypyrrole, carbon is received What mitron and three layers of the Nano silver grain aramid fiber beam coated or polypyrrole, carbon nano-tube bundle and three layers of Nano silver grain coated Aramid fiber beam；
(6) by two strands of polypyrroles, the aramid fiber beam or polypyrrole, carbon nanotube of carbon nanotube and three layers of Nano silver grain cladding Beam and the aramid fiber beam of three layers of Nano silver grain cladding are immersed in polyvinyl alcohol gel, are then taken out and are intertwined, It solidifies at room temperature, obtains aramid fiber electrochemical capacitor；Polyvinyl alcohol, acid and water heats to 1 at 50~100 DEG C~ 10h obtains polyvinyl alcohol gel after cooling.
2. preparation method according to claim 1, which is characterized in that in step (1), the aramid fiber includes poly- to benzene One or more of two formyl p-phenylenediamine fibers, Fanglun 1313, poly fiber；Contain Have the aqueous solution of Dopamine hydrochloride and Tri(Hydroxymethyl) Amino Methane Hydrochloride pH value be 8.5, react for shaken at room temperature reaction 5~ 48h；Fiber taking-up is washed and dried after reaction, obtains the aramid fiber beam of poly-dopamine cladding；Dopamine hydrochloride, three Hydroxymethyl aminomethane hydrochloride, aramid fiber beam mass ratio be (0.1~1): (0.05~0.5): (0.1~1).
3. preparation method according to claim 1, which is characterized in that in step (2), react for oscillating reactions 10 at room temperature ~60min；Fiber taking-up is washed and dried after reaction, obtains the aramid fiber beam of Nano silver grain cladding；Silver nitrate, The mass ratio for the aramid fiber beam that polyvinylpyrrolidone, glucose, poly-dopamine coat is (0.5~5): (0.05~0.5): (1~10): (0.1~1).
4. preparation method according to claim 1, which is characterized in that in step (3), react to be vibrated in 50~100 DEG C React 1~10h；Fiber taking-up is washed and dried after reaction, Nano silver grain of the surface with epoxy group is obtained and coats Aramid fiber beam；The matter for the aramid fiber beam that γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane, Nano silver grain coat Amount is than being (0.5~5): (0.1~1).
5. preparation method according to claim 1, which is characterized in that in step (4), it is anti-in 50~80 DEG C of oscillations for reacting Answer 5~for 24 hours；Fiber taking-up is washed and dried after reaction, obtains the virtue of carbon nanotube and Nano silver grain double-coating The aramid fiber beam of synthetic fibre fibre bundle or carbon nano-tube bundle and Nano silver grain double-coating；With carboxyl carbon nanotube or with carboxyl The mass ratio for the aramid fiber beam that the Nano silver grain of carbon nano-tube bundle, surface with epoxy group coats is (0.5~5): (0.1 ~1).
6. preparation method according to claim 1, which is characterized in that in step (5), the carbon nanotube includes multi wall carbon One or more of nanotube, single-walled carbon nanotube；Silver nitrate, pyrroles, carbon nanotube and Nano silver grain double-coating The mass ratio of aramid fiber beam is (0.2~4): (0.1~2): (0.1~1)；Reaction is 5~48h of oscillating reactions at room temperature；Instead Fiber taking-up is washed and dried after answering, obtains aramid fiber electrode.
7. preparation method according to claim 1, which is characterized in that in step (6), it is described acid be phosphoric acid, sulfuric acid or its Combination；Polyvinyl alcohol, acid, water mass ratio be (1~20): (1~20): 100.
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