CN110387743A - Electrically conductive composite fibre beam and preparation method thereof - Google Patents
Electrically conductive composite fibre beam and preparation method thereof Download PDFInfo
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- CN110387743A CN110387743A CN201910647666.9A CN201910647666A CN110387743A CN 110387743 A CN110387743 A CN 110387743A CN 201910647666 A CN201910647666 A CN 201910647666A CN 110387743 A CN110387743 A CN 110387743A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G61/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G61/12—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule
- C08G61/122—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides
- C08G61/123—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds
- C08G61/126—Macromolecular compounds containing atoms other than carbon in the main chain of the macromolecule derived from five- or six-membered heterocyclic compounds, other than imides derived from five-membered heterocyclic compounds with a five-membered ring containing one sulfur atom in the ring
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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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/10—Definition of the polymer structure
- C08G2261/11—Homopolymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2261/00—Macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain of the macromolecule
- C08G2261/30—Monomer units or repeat units incorporating structural elements in the main chain
- C08G2261/32—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain
- C08G2261/322—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed
- C08G2261/3223—Monomer units or repeat units incorporating structural elements in the main chain incorporating heteroaromatic structural elements in the main chain non-condensed containing one or more sulfur atoms as the only heteroatom, e.g. thiophene
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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
- 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
Abstract
The present invention provides a kind of electrically conductive composite fibre beams and preparation method thereof, the preparation method of the electrically conductive composite fibre beam passes through reverse microemulsion process for 3, on 4- ethene dioxythiophene in-situ polymerization to fibre bundle, the linear poly- 3,4-rthylene dioxythiophene electrically conductive composite fibre beam of the uniform and fine and close nanometer of preparation.The preparation method can regulate and control poly- 3,4-rthylene dioxythiophene in the formation condition on fibre bundle surface, form the more regular nanometer linear structure for being conducive to electron-transport and migration, technical process is simple, and controllability is strong, while having good repeatability.Prepared electrically conductive composite fibre beam can be applied to the fields such as wearable electronic device, energy storage, sensor.
Description
Technical field
The present invention relates to conductive fiber material preparation fields, and in particular to a kind of electrically conductive composite fibre beam and its preparation side
Method.
Background technique
Conductive fiber causes the extensive concern of domestic and international material circle as a kind of important intellectual material, in clothes, passes
The fields such as sensor and intelligent textile have huge application prospect.
In recent years, conducting polymer has been widely used in fields such as modified electrode, electrochemistry and sensors.Its
In, presently the most environmentally friendly conductive polymer poly 3,4-rthylene dioxythiophene (PEDOT) is since molecular structure is simple, conductivity
High, the advantages that stability is good and energy gap is small, shows one's talent in numerous conducting polymers, has obtained extensive research and concern.Cause
This, PEDOT is a kind of excellent conductive carrier.Conductive material based on PEDOT shows with high surface area, high conductivity,
The various nanostructures of the swift electron rate of transform, hydrophobic interaction and good biocompatibility, as nanometer sheet, nano flower and
Nano wire etc..
Application No. is the patents of invention of CN201710128767.6 to disclose a kind of stretchable conductive material of three-dimensional and its system
Preparation Method obtains polyurethane fiber pad using the method for electrostatic spinning, and forms conduction by interfacial polymerization on it
PEDOT obtains conductive fiber pad flexible.
Application No. is the patents of invention of CN201710329153.4 to disclose a kind of flexible wearable nano fabrics biography
Sensor and preparation method thereof.It prepares continuous nano-fibre yams by being conjugated electrostatic spun yarn technology, then fine in yarn
It ties up surface aggregate and coats one layer of PEDOT, the nano fibre yarn of preparation has good electric conductivity.
However, although traditional situ aggregation method preparation PEDOT step is relatively simple, due to its uncontrollable factor compared with
More, polymerization reaction is difficult to control, and therefore, the PEDOT structure formed on fiber is mostly the particle of reunion or the block of accumulation
Shape, however, irregular structure is unfavorable for the transmission and migration of electronics.All the time, the uncontrollability limit of PEDOT nanostructure
Its development and application are made.
Currently, carrying out the method for home position polymerization reaction not yet to 3,4 ethene dioxythiophene monomers using reverse microemulsion process
See report.
Summary of the invention
Against the above deficiency, the purpose of the present invention is to provide a kind of electrically conductive composite fibre beams and preparation method thereof.This is led
The preparation method of electric bundle of composite fibers, by 3,4-rthylene dioxythiophene in-situ polymerization to fibre bundle, is made by reverse microemulsion process
The standby uniformly linear poly- 3,4-rthylene dioxythiophene electrically conductive composite fibre beam of fine and close nanometer.The preparation method can regulate and control poly- 3,
4- ethene dioxythiophene forms the regular nanometer threadiness knot for being conducive to electron-transport and migration in the formation condition on fibre bundle surface
Structure, technical process is simple, and controllability is strong, while having good repeatability.Prepared electrically conductive composite fibre beam can be applied
In fields such as wearable electronic device, energy storage, sensors.
For achieving the above object, the present invention provides a kind of preparation method of electrically conductive composite fibre beam, including it is as follows
Step:
S1, fibre single thread is subjected to surface decontamination processing, then dries to obtain fibre bundle spare；
S2, the surfactant that surfactant and organic solvent are hybridly prepared into predetermined concentration under preset temperature is had
Machine solution；
S3, the aqueous oxidizing agent solution that oxidant and deionized water are hybridly prepared into predetermined concentration at normal temperature；
S4, at room temperature, it is organic molten that the fibre bundle that step S1 is obtained is put into surfactant made from step S2
In liquid, dipping, stir process；Then solution is added than the aqueous oxidizing agent solution for preparing step S3 according to preset vol
In, stir process；Finally according to preset vol than 3,4 ethene dioxythiophene monomers, stir process, to use reverse microemulsion is added
3,4 ethene dioxythiophene home position polymerization reactions of liquid method completion fibre bundle；
S5, drying is cleaned, obtains electrically conductive composite fibre beam.
Preferably, in step s 4, the volume ratio of the aqueous oxidizing agent solution and the organic solvent be 0.017~
0.045。
Preferably, in step s 4, described 3, the volume ratio of 4 ethene dioxythiophene monomers and the organic solvent is
0.0030~0.0067.
Preferably, in step s 2, the mass concentration of the surfactant is 10wt% -20wt%；It is described organic molten
The mass concentration of agent is 80wt% -90wt%.
Preferably, the surfactant is aerosol OT.
Preferably, in step s3, the concentration of oxidant is 6mol/L~8mol/L in the aqueous oxidizing agent solution；It is described
Oxidant is one of anhydrous ferric trichloride, Iron(III) chloride hexahydrate.
Preferably, in step s 2, the organic solvent is one or both of n-hexane, paraxylene；It is described pre-
If temperature is 15 DEG C~25 DEG C.
Preferably, the fibre bundle include but is not limited to be aramid fiber, nylon fiber, polyester fiber, cotton fiber, polyamide fibre
One of fiber, silk fiber, and its fibre length is 10~20cm.
For achieving the above object, the present invention also provides it is a kind of according to the above technical scheme in any technical solution institute
State preparation method preparation electrically conductive composite fibre beam comprising fiber base material and pass through reverse microemulsion process in-situ polymerization deposition
In the linear poly- 3,4-rthylene dioxythiophene of the nanometer of the fibrous substrate surface.
Preferably, the length of the fiber base material is 10~20cm.
Reaction principle of the invention is:
Antiphase boundaries polymerization is a kind of effective ways for preparing one-dimensional PEDOT nanostructure.In Reverse Microemulsion System,
Water is mutually dissolved the aggregation for promoting the surfactant molecule in nonpolar solvent by polar group and hydrogen bond.Therefore,
Many reactants can be introduced into the conversion zone of the aqueous nano-scale in reversed phase micelle.These micellas, which play, to be received
The effect of rice reactor.
Aerosol OT (AOT) is a kind of double tail anionic surfactants, and can be dissolved in well
In solvent such as n-hexane or paraxylene, by the volume ratio, fixed stirring rate and mode, list that adjust water and organic solvent
The reaction conditions such as the molar ratio of bulk concentration, monomer and oxidant, can prepare different PEDOT nanostructures, and such as nanometer rods are received
Rice fiber and nanotube etc..
Anhydrous ferric trichloride (FeCl3) or Iron(III) chloride hexahydrate (FeCl3·6H2It O is) the most normal in EDOT oxidation polymerization
Oxidant.Work as FeCl3Or FeCl3·6H2When O aqueous solution is added in the solution of AOT, the anion and Fe on the head AOT3+
Reverse phase cylindrical micelles, therefore, Fe are formd by electrostatic attraction3+The anionic head of AOT can be absorbed in.In EDOT
In the chemical oxidising polymerisation of monomer, Fe3+Play the role of oxidant, and is centrally formed in the polarization of AOT reverse phase cylindrical micelles
Therefore aquaporin has constructed the one-dimensional water-oil interface divided by reverse phase cylindrical micelles, have and carry out boundary in nanoscale
The necessary condition of face polymerization reaction.
AOT reversed phase micelle hydrophilic radical outside, including lipophilic group, with the increase of reversed phase micelle, is added three in system
After ferric chloride solution, group forms column；After EDOT monomer is added, monomer carries out polymerization reaction on the outside of cylindrical micellar, when anti-
After answering, AOT is washed off, is left the PEDOT nanofiber in outside.
The beneficial effects of the present invention are:
1. preparation method provided by the invention carries out chemistry polymerizing in situ using reverse microemulsion process, is aoxidized by control
The volume ratio and 3 of agent aqueous solution and organic solvent, the volume ratio of 4 ethene dioxythiophenes and organic solvent, regulation PEDOT are poly-
Reaction process is closed, to form the uniform and fine and close PEDOT nanowire structure for being conducive to ion and transmitting and migrating on fibre bundle surface,
Overcome the defect of the prior art.
2. preparation method provided by the invention, simple process, controllability is strong, while having good repeatability, is suitble to
Large-scale application and popularization.
3. electrically conductive composite fibre beam prepared by the present invention can be widely applied to wearable electronic device, energy storage, sensing
Equal fields.
Detailed description of the invention
Fig. 1 is aramid fiber fibril electron microscope, scale 10um.
Fig. 2 is the electron microscope of nanometer threadiness PEDOT conduction Composite aramid fiber fiber prepared by embodiment 1, scale 1um.
Fig. 3 is nanometer threadiness PEDOT conduction Composite aramid fiber fiber local distribution electron microscope prepared by embodiment 1, and scale is
100nm。
Fig. 4 is cotton fiber fibril electron microscope, scale 10um.
Fig. 5 is the electron microscope of the conductive compound cotton fiber of nanometer threadiness PEDOT prepared by embodiment 6, scale 1um.
Fig. 6 is the conductive compound cotton fiber local distribution electron microscope of nanometer threadiness PEDOT prepared by embodiment 6, and scale is
100nm。
Fig. 7 is the resistance view of nanometer threadiness PEDOT conduction Composite aramid fiber fiber prepared by the embodiment of the present invention 1.
Fig. 8 is the resistance view of the conductive compound cotton fiber of nanometer threadiness PEDOT prepared by the embodiment of the present invention 6.
Specific embodiment
Clear, complete description is carried out below with reference to technical solution of the attached drawing to various embodiments of the present invention, it is clear that is retouched
The embodiment stated is only a part of the embodiments of the present invention, instead of all the embodiments；Based on the embodiment of the present invention, ability
Domain those of ordinary skill obtained all other embodiment without making creative work, belongs to the present invention
The range protected.
The present invention provides a kind of preparation methods of electrically conductive composite fibre beam, include the following steps:
S1, fibre single thread is subjected to surface decontamination processing, then dries to obtain fibre bundle spare；
S2, the surfactant that surfactant and organic solvent are hybridly prepared into predetermined concentration under preset temperature is had
Machine solution；
S3, the aqueous oxidizing agent solution that oxidant and deionized water are hybridly prepared into predetermined concentration at normal temperature；
S4, at room temperature, it is organic molten that the fibre bundle that step S1 is obtained is put into surfactant made from step S2
In liquid, dipping, stir process；Then solution is added than the aqueous oxidizing agent solution for preparing step S3 according to preset vol
In, stir process；Finally according to preset vol than 3,4 ethene dioxythiophene monomers, stir process, to use reverse microemulsion is added
3,4 ethene dioxythiophene home position polymerization reactions of liquid method completion fibre bundle；
S5, drying is cleaned, obtains electrically conductive composite fibre beam.
Wherein, in step sl, the surface decontamination processing includes the following steps:
S11, by fibre single thread deionized water ultrasonic cleaning 10-30min, dry at room temperature；
S12, by fibre single thread dehydrated alcohol ultrasonic cleaning 10-30min, dry at room temperature；
S13, by fibre single thread acetone ultrasonic cleaning 10-30min, dry at room temperature spare.
In step s 2, the mass concentration of the surfactant is 10wt% -20wt%；The matter of the organic solvent
Amount concentration is 80wt% -90wt%.Preferably, the surfactant is aerosol OT.In step s 2,
The organic solvent is one or both of n-hexane, paraxylene；The preset temperature is 15 DEG C~25 DEG C.
In step s3, the concentration of oxidant is 6mol/L~8mol/L in the aqueous oxidizing agent solution.The oxidant
For one of anhydrous ferric trichloride, Iron(III) chloride hexahydrate.
In step s 4, the volume ratio of the aqueous oxidizing agent solution and the organic solvent is 0.017-0.045.Described 3,
The volume ratio of 4 ethene dioxythiophene monomers and the organic solvent is 0.0030-0.0067.
The present invention also provides the electrically conductive composite fibre beams prepared according to above-mentioned preparation method comprising fiber base material and logical
Reverse microemulsion process in-situ polymerization deposition is crossed in the linear poly- 3,4-rthylene dioxythiophene of nanometer of the fibrous substrate surface.It is preferred that
Ground, the length of the fiber base material are 10-20cm.
The preparation method of electrically conductive composite fibre beam is illustrated below with reference to embodiment 1-16 and comparative example 1-5:
Embodiment 1
A. surface decontamination processing is carried out to fibre single thread:
Aramid fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
The paraxylene that the aerosol OT that quality is 15g is 100ml with volume is mixed at a temperature of 20 DEG C
It closes, is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
By quality be 3.0g anhydrous ferric trichloride and volume be 2.7ml deionized water mix at normal temperature, sufficiently stir
The anhydrous ferric trichloride solution that concentration is 7.2M is obtained after mixing uniformly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the aramid fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, anhydrous ferric trichloride solution obtained in a dropping step c dropwise；After uniform stirring 30min, the EDOT of 470ul is added dropwise dropwise,
Reaction carries out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The aramid fiber beam obtained after step d reaction is cleaned, conductive Composite aramid fiber fibre bundle is obtained after drying.
Fig. 1-3 is respectively aramid fiber fibril, nanometer threadiness PEDOT conduction Composite aramid fiber fiber and nanometer threadiness PEDOT
Conductive Composite aramid fiber fiber local distribution electron microscope compares it is found that aramid fiber fibril surface is smooth, conduction prepared by the present invention
Nanometer threadiness structure distribution is presented in the PEDOT of composite fiber surface, and interlaced, forms more uniform intensive three-dimensional network
Shape distribution, is conducive to electron-transport and migration, forms efficient conductive network.
With the increase of electrically conductive composite fibre Shu Changdu, the trend increased uniformly and quickly, electric conductivity is presented in resistivity
It significantly improves, as shown in Figure 7.
Comparative example 1
The PEDOT electrically conductive composite fibre beam of in-situ polymerization is carried out using conventional method.
Embodiment 1 and comparative example 1 are carried out to the analyzing conductivity of bundle of composite fibers, composite fibre prepared by embodiment 1
The resistance of beam is 205 Ω/cm, and the resistance of bundle of composite fibers prepared by comparative example 1 is 423 Ω/cm；Conduction prepared by comparative example 1
Composite fibre, using the conductive fiber of conventional method preparation, its pattern is uncontrollable and inhomogenous, therefore resistance is also bigger.
Embodiment 2
Difference with embodiment 1 is only that: the volume ratio of aqueous oxidizing agent solution and organic solvent is 0.017, other steps
Essentially identical, details are not described herein.
Embodiment 3
Difference with embodiment 1 is only that: the volume ratio of aqueous oxidizing agent solution and organic solvent is 0.045, other steps
Essentially identical, details are not described herein.
Comparative example 2
Difference with embodiment 1 is only that: the volume ratio of aqueous oxidizing agent solution and organic solvent is 0.010, other steps
Essentially identical, details are not described herein.
Comparative example 3
Difference with embodiment 1 is only that: the volume ratio of aqueous oxidizing agent solution and organic solvent is 0.055, other steps
Essentially identical, details are not described herein.
Table 1 is that the volume change of aqueous oxidizing agent solution and organic solvent is compound to conduction in embodiment 1-3 and comparative example 2-3
The influence of fibre bundle electric conductivity
According to table 1: in the range of the volume ratio of aqueous oxidizing agent solution and organic solvent is 0.017~0.15, with
The increase of the volume ratio of aqueous oxidizing agent solution and organic solvent, resistance the changing rule being gradually increasing is presented.
It is compound when the volume ratio of aqueous oxidizing agent solution and organic solvent is respectively 0.010 and 0.055 in comparative example 2-3
The resistance of fibre bundle is larger, although using the preparation that reverse microemulsion process carries out conductive fiber, since parameter modification is larger,
Uniform nanometer threadiness PEDOT structure cannot be formed, so its electric conductivity is good not as good as the conductive fiber of strict control parameter, electricity
Resistance is universal larger.
Embodiment 4
Difference with embodiment 1 is only that: the volume ratio of 3,4 ethene dioxythiophenes and organic solvent is 0.0030, other
Step is essentially identical, and details are not described herein.
Embodiment 5
Difference with embodiment 1 is only that: the volume ratio of 3,4 ethene dioxythiophenes and organic solvent is 0.0067, other
Step is essentially identical, and details are not described herein.
Comparative example 4
Difference with embodiment 1 is only that: the volume ratio of 3,4 ethene dioxythiophenes and organic solvent is 0.0020, other
Step is essentially identical, and details are not described herein.
Comparative example 5
Difference with embodiment 1 is only that: the volume ratio of 3,4 ethene dioxythiophenes and organic solvent is 0.0075, other
Step is essentially identical, and details are not described herein.
Table 2 is the volume ratio of 3,4 ethene dioxythiophenes and organic solvent in embodiment 1, embodiment 4-5 and comparative example 4-5
Change the influence to fibre bundle electric conductivity
According to table 2: in the range of the volume ratio of EDOT and organic solvent is 0.0030~0.0067, with 3,4
The changing rule gradually decreased is presented in the increase of the volume ratio of ethene dioxythiophene monomer and organic solvent, resistance.
In comparative example 4-5, when the volume ratio of EDOT and organic solvent are respectively 0.0020 and 0.0075, bundle of composite fibers
Resistance it is larger, although use reverse microemulsion process carry out conductive fiber preparation be unable to shape since parameter modification is larger
At uniform nanometer threadiness PEDOT structure, so its electric conductivity is good not as good as the conductive fiber of strict control parameter, resistance is universal
It is larger.
Embodiment 6
A. surface decontamination processing is carried out to fibre single thread:
Cotton fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is guaranteed
Back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, at room temperature
It dries, saves backup；
B. the preparation of surfactant organic solution:
The paraxylene that the aerosol OT that quality is 12g is 80ml with volume is mixed at a temperature of 20 DEG C
It closes, is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
By quality be 2.4g anhydrous ferric trichloride and volume be 2.2ml deionized water mix at normal temperature, sufficiently stir
The anhydrous ferric trichloride solution that concentration is 7M is obtained after mixing uniformly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the cotton fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, anhydrous ferric trichloride solution obtained in a dropping step c dropwise；After uniform stirring 30min, the EDOT of 380ul is added dropwise dropwise,
Reaction carries out at room temperature, and the reaction time is for 24 hours；
E. drying is cleaned:
The cotton fiber beam obtained after step d reaction is cleaned, conductive composite cotton fabric fibre bundle is obtained after drying.
Fig. 4-6 is respectively cotton fiber fibril, the conductive compound cotton fiber of nanometer threadiness PEDOT and nanometer threadiness PEDOT conductive
Compound cotton fiber local distribution electron microscope compares it is found that cotton fiber fibril surface is smooth, electrically conductive composite fibre prepared by the present invention
Nanometer threadiness structure distribution is presented in the PEDOT on surface, and interlaced, forms more uniform intensive three-dimensional network shape distribution,
Conducive to electron-transport and migration, efficient conductive network is formed.
With the increase of electrically conductive composite fibre Shu Changdu, the trend increased uniformly and quickly, electric conductivity is presented in resistivity
It significantly improves, as shown in Figure 8.
Embodiment 7
A. surface decontamination processing is carried out to fibre single thread:
Nylon fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
The paraxylene that the aerosol OT that quality is 18g is 120ml with volume is mixed at a temperature of 20 DEG C
It closes, is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The anhydrous ferric trichloride that quality is 3.7g is mixed at normal temperature with the deionized water that volume is 3.24ml, is sufficiently stirred
The anhydrous ferric trichloride solution that concentration is 7.5M is obtained after mixing uniformly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the nylon fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, anhydrous ferric trichloride solution obtained in a dropping step c dropwise；After uniform stirring 30min, the EDOT of 560ul is added dropwise dropwise,
Reaction carries out at room temperature, and the reaction time is for 24 hours.
E. it cleans drying: the nylon fiber beam obtained after step d reaction being cleaned, conductive composite nylon is obtained after drying
Fibre bundle.
Embodiment 8
A. surface decontamination processing is carried out to fibre single thread:
Polyester fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
By quality be 22.6g aerosol OT and volume be 150ml paraxylene at a temperature of 20 DEG C
Mixing is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The anhydrous ferric trichloride that quality is 4.6g is mixed at normal temperature with the deionized water that volume is 4ml, is sufficiently stirred
The anhydrous ferric trichloride solution that concentration is 8M is obtained after uniformly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the polyester fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, anhydrous ferric trichloride solution obtained in a dropping step c dropwise；After uniform stirring 30min, the EDOT of 705ul is added dropwise dropwise,
Reaction carries out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The polyester fiber beam obtained after step d reaction is cleaned, conductive composite terylene fibre bundle is obtained after drying.
Embodiment 9
A. surface decontamination processing is carried out to fibre single thread:
Spandex fibre monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
By quality be 27.2g aerosol OT and volume be 180ml paraxylene at a temperature of 20 DEG C
Mixing is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The Iron(III) chloride hexahydrate that quality is 5.5g is mixed at normal temperature with the deionized water that volume is 4.86ml, sufficiently
The Iron(III) chloride hexahydrate solution that concentration is 6M is obtained after mixing evenly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the spandex fibre beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, Iron(III) chloride hexahydrate solution obtained in a dropping step c dropwise；After uniform stirring 30min, it is added dropwise 850ul's dropwise
EDOT, reaction carry out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The spandex fibre beam obtained after step d reaction is cleaned, conductive compound spandex fibre beam is obtained after drying.
Embodiment 10
A. surface decontamination processing is carried out to fibre single thread:
Silk fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
By quality be 30.2g aerosol OT and volume be 200ml paraxylene at a temperature of 20 DEG C
Mixing is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The anhydrous ferric trichloride that quality is 6.1g is mixed at normal temperature with the deionized water that volume is 5.4ml, is sufficiently stirred
The anhydrous ferric trichloride solution that concentration is 6.5M is obtained after mixing uniformly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the silk fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, anhydrous ferric trichloride solution obtained in a dropping step c dropwise；After uniform stirring 30min, the EDOT of 940ul is added dropwise dropwise,
Reaction carries out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The silk fiber beam obtained after step d reaction is cleaned, conductive composite silk fibre bundle is obtained after drying.
Embodiment 11
A. surface decontamination processing is carried out to fibre single thread:
Cotton fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is guaranteed
Back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, at room temperature
It dries, saves backup；
B. the preparation of surfactant organic solution:
The aerosol OT that quality is 12g is mixed at a temperature of 20 DEG C with the n-hexane that volume is 80ml,
It is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The Iron(III) chloride hexahydrate that quality is 4.0g is mixed at normal temperature with the deionized water that volume is 2.2ml, sufficiently
The Iron(III) chloride hexahydrate solution that concentration is 7M is obtained after mixing evenly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the cotton fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, Iron(III) chloride hexahydrate solution obtained in a dropping step c dropwise；After uniform stirring 30min, it is added dropwise 380ul's dropwise
EDOT, reaction carry out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The cotton fiber beam obtained after step d reaction is cleaned, conductive composite cotton fabric fibre bundle is obtained after drying.
Embodiment 12
A. surface decontamination processing is carried out to fibre single thread:
Aramid fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
The aerosol OT that quality is 15g is mixed at a temperature of 20 DEG C with the n-hexane that volume is 100ml,
It is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The Iron(III) chloride hexahydrate that quality is 5.1g is mixed at normal temperature with the deionized water that volume is 2.7ml, sufficiently
The Iron(III) chloride hexahydrate solution that concentration is 7.5M is obtained after mixing evenly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the aramid fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, Iron(III) chloride hexahydrate solution obtained in a dropping step c dropwise；After uniform stirring 30min, it is added dropwise 470ul's dropwise
EDOT, reaction carry out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The aramid fiber beam obtained after step d reaction is cleaned, conductive Composite aramid fiber fibre bundle is obtained after drying.
Embodiment 13
A. surface decontamination processing is carried out to fibre single thread:
Nylon fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
The aerosol OT that quality is 18g is mixed at a temperature of 20 DEG C with the n-hexane that volume is 120ml,
It is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The Iron(III) chloride hexahydrate that quality is 6.1g is mixed at normal temperature with the deionized water that volume is 3.24ml, sufficiently
The Iron(III) chloride hexahydrate solution that concentration is 6.9M is obtained after mixing evenly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the nylon fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, Iron(III) chloride hexahydrate solution obtained in a dropping step c dropwise；After uniform stirring 30min, it is added dropwise 560ul's dropwise
EDOT, reaction carry out at room temperature, and the reaction time is for 24 hours.
E. it cleans drying: the nylon fiber beam obtained after step d reaction being cleaned, conductive composite nylon is obtained after drying
Fibre bundle.
Embodiment 14
A. surface decontamination processing is carried out to fibre single thread:
Polyester fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
The n-hexane that the aerosol OT that quality is 22.6g is 150ml with volume is mixed at a temperature of 20 DEG C
It closes, is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The Iron(III) chloride hexahydrate that quality is 7.7g is mixed at normal temperature with the deionized water that volume is 4.05ml, sufficiently
The Iron(III) chloride hexahydrate solution that concentration is 7M is obtained after mixing evenly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the polyester fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, Iron(III) chloride hexahydrate solution obtained in a dropping step c dropwise；After uniform stirring 30min, it is added dropwise 850ul's dropwise
EDOT, reaction carry out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The polyester fiber beam obtained after step d reaction is cleaned, conductive composite terylene fibre bundle is obtained after drying.
Embodiment 15
A. surface decontamination processing is carried out to fibre single thread:
Spandex fibre monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
The aerosol OT that quality is 27g is mixed at a temperature of 20 DEG C with the n-hexane that volume is 180ml,
It is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The Iron(III) chloride hexahydrate that quality is 9.2g is mixed at normal temperature with the deionized water that volume is 4.86ml, sufficiently
The Iron(III) chloride hexahydrate solution that concentration is 6M is obtained after mixing evenly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the spandex fibre beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, Iron(III) chloride hexahydrate solution obtained in a dropping step c dropwise；After uniform stirring 30min, it is added dropwise 850ul's dropwise
EDOT, reaction carry out at room temperature, and the reaction time is for 24 hours.
E. drying is cleaned:
The spandex fibre beam obtained after step d reaction is cleaned, conductive compound spandex fibre beam is obtained after drying.
Embodiment 16
A. surface decontamination processing is carried out to fibre single thread:
Silk fiber monofilament is sequentially placed into deionized water, dehydrated alcohol, carries out ultrasonic cleaning 15min in acetone, is protected
Card back cleans up, and room temperature carries out the cleaning of next step again after drying, after the completion of the ultrasonic cleaning of final step acetone, room temperature
Under dry, save backup；
B. the preparation of surfactant organic solution:
The aerosol OT that quality is 30g is mixed at a temperature of 20 DEG C with the n-hexane that volume is 200ml,
It is configured to the aerosol OT solution that concentration is 0.34M；
C. the preparation of aqueous oxidizing agent solution:
The Iron(III) chloride hexahydrate that quality is 10.2g is mixed at normal temperature with the deionized water that volume is 5.4ml, sufficiently
The Iron(III) chloride hexahydrate solution that concentration is 8M is obtained after mixing evenly；
D. the EDOT home position polymerization reaction of fibre bundle:
At 20 °C, the silk fiber beam that step a is obtained is put into surfactant organic solution made from step b
In, simultaneously uniform stirring 30min is impregnated, agitating mode is mechanical stirring, wherein churned mechanically revolving speed is 400rmp；30min
Afterwards, Iron(III) chloride hexahydrate solution obtained in a dropping step c dropwise；After uniform stirring 30min, it is added dropwise 940ul's dropwise
EDOT, reaction carry out at room temperature, and the reaction time is for 24 hours；
E. drying is cleaned:
The silk fiber beam obtained after step d reaction is cleaned, conductive composite silk fibre bundle is obtained after drying.
Following table is the performance comparable situation of embodiment 6-16 electrically conductive composite fibre:
Table 3 is the performance that embodiment 6-16 prepares the condition of electrically conductive composite fibre beam and the electrically conductive composite fibre beam of preparation
According to table 3: electrically conductive composite fibre beam prepared by the present invention has excellent electric conductivity.
The variation of organic solvent and oxidant species can generate certain influence to the electric conductivity of bundle of composite fibers, but
Difference is little.
Since the material of different substrate materials is different, surface institute band group is different, in reaction system different substrate materials to oxidant and
The adsorption capacity of monomer etc. is different, therefore the resistance of gained conductive fiber beam will be different, but difference will not be very big,
It is other to substantially remain in an order of magnitude, gap does not exceed 100 Ω.
It should be noted that the fibre bundle is not limited to as cotton fiber, aramid fiber, nylon fiber, polyester fiber, ammonia
Synthetic fibre fiber, silk fiber, or other fibers such as nylon fibre.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of electrically conductive composite fibre beam, which comprises the steps of:
S1, fibre single thread is subjected to surface decontamination processing, then dries to obtain fibre bundle spare；
S2, the surfactant that surfactant and organic solvent are hybridly prepared into predetermined concentration under preset temperature are organic molten
Liquid；
S3, the aqueous oxidizing agent solution that oxidant and deionized water are hybridly prepared into predetermined concentration at normal temperature；
S4, at room temperature, the fibre bundle that step S1 is obtained is put into surfactant organic solution made from step S2,
Dipping, stir process；Then it is added in solution according to preset vol than the aqueous oxidizing agent solution for preparing step S3, stirring
Processing；Finally according to preset vol than 3,4 ethene dioxythiophene monomers, stir process, with complete using reverse microemulsion process is added
At the 3 of fibre bundle, 4 ethene dioxythiophene home position polymerization reactions；
S5, drying is cleaned, obtains electrically conductive composite fibre beam.
2. the preparation method of electrically conductive composite fibre beam according to claim 1, it is characterised in that: in step s 4, described
The volume ratio of aqueous oxidizing agent solution and the organic solvent is 0.017~0.045.
3. the preparation method of electrically conductive composite fibre beam according to claim 1, it is characterised in that: in step s 4, described
The volume ratio of 3,4 ethene dioxythiophene monomers and the organic solvent is 0.0030~0.0067.
4. the preparation method of electrically conductive composite fibre beam according to claim 1, it is characterised in that: in step s 2, described
The mass concentration of surfactant is 10wt%~20wt%；The mass concentration of the organic solvent is 80wt%~90wt%.
5. the preparation method of electrically conductive composite fibre beam according to claim 4, it is characterised in that: the surfactant is
Aerosol OT.
6. the preparation method of electrically conductive composite fibre beam according to claim 1, it is characterised in that: in step s3, described
The concentration of oxidant is 6mol/L~8mol/L in aqueous oxidizing agent solution；The oxidant is anhydrous ferric trichloride, six hydrations three
One of iron chloride.
7. the preparation method of electrically conductive composite fibre beam according to claim 1, it is characterised in that: in step s 2, described
Organic solvent is one of n-hexane, paraxylene；The preset temperature is 15 DEG C~25 DEG C.
8. the preparation method of electrically conductive composite fibre beam according to claim 1, it is characterised in that: the fibre bundle include but
It is not limited to one of aramid fiber, nylon fiber, polyester fiber, cotton fiber, nylon fibre, silk fiber, and its fiber
Length is 10~20cm.
9. the electrically conductive composite fibre beam of preparation method preparation described in a kind of any one of -8 claims according to claim 1,
It is characterized by comprising fiber base material and by reverse microemulsion process in-situ polymerization deposition the fibrous substrate surface nanometer
Linear poly- 3,4-rthylene dioxythiophene.
10. electrically conductive composite fibre beam according to claim 9, it is characterised in that: the length of the fiber base material be 10~
20cm。
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| CN113026368A (en) * | 2021-03-10 | 2021-06-25 | 苏州大学 | Preparation method of flexible piezoresistive conductive material |
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