CN102199871A - Composite conductive fiber with coaxial three-element, and preparation method thereof. - Google Patents
Composite conductive fiber with coaxial three-element, and preparation method thereof. Download PDFInfo
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- CN102199871A CN102199871A CN 201110075961 CN201110075961A CN102199871A CN 102199871 A CN102199871 A CN 102199871A CN 201110075961 CN201110075961 CN 201110075961 CN 201110075961 A CN201110075961 A CN 201110075961A CN 102199871 A CN102199871 A CN 102199871A
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Abstract
The present invention relates to a composite conductive fiber with coaxial three-element, and a preparation method thereof. The composite conductive fiber comprises a core layer of polyurethane fiber, an intermediate layer of carbon nano-tube, and an outer layer of intrinsic conducting polymer, wherein the three layers of the composite conductive fiber are coaxial. The preparation method comprises comprises: (1) preparing pretreated polyurethane fiber; (2) immersing the pretreated polyurethane fiber in a organic solvent reaction bath containing the carbon nano-tube to carry out a process to obtain a two-element composite fiber of carbon nano-tube/polyurethane; (3) immersing the two-element composite fiber of carbon nano-tube/polyurethane in a intrinsic conductive polymer monomer solution, then adding an oxidizing agent solution in a dropwise manner, carrying out a washing and drying for the resulting solution after complete reacting to obtain the composite conductive fiber with coaxial three-element. The composite conductive fiber provided by the present invention has advantages of good conductive effect, high elasticity, soft hand feeling, simple preparation technology and low input cost of equipment, and is applicable for large scale production and large scale application.
Description
Technical field
The invention belongs to composite conducting fiber and preparation field thereof, particularly relate to coaxial composite conducting fiber of a kind of ternary and preparation method thereof.
Background technology
Conductive fiber is a kind of serious difference chemical fibre dimension kind, and its electrical conductivity is greater than 10
-8Ω
-1Cm
-1, purposes is very extensive, and except that being generally used for antistatic textile, the textiles of conductive fiber high-load also has explosion-proof and characteristic shield microwaves, also is the potential new material that is used for flexible super capacitor of a kind of energy.Very a spot of conductive fiber is sneaked into the electrostatic problem that can solve in the synthetic fiber in the weaving processing; Conductive fiber also can be used as dustproof, the antistatic Work Clothes or the multifunctional sensing device in fields such as semi-conductor industry, precise electronic industry, medical science, bioscience.The anti-static fabric made from conductive fiber can reduce chemical fibre with the static safety in production of bringing for special occasions such as gas station, oil depot threaten, reduce the adverse effect that the chemical fibre clothes bring health.
The preparation of conductive fiber is adopted usually and add conductive component in polymeric matrix, as: metal, metal oxide, carbon-based material and intrinsic conduction macromolecule are realized.As: additive process, promptly in polymeric matrix, add conductive component, conductive fiber is made in spinning again; Post treatment method (or surface-coated method) promptly in the fiber last handling process, utilizes means such as swelling or coating, and with conductive component, or the slurries that contain conductive component adhere to fiber surface.The intrinsic conduction macromolecule can give conductive fiber more interesting function, as electromagnetic shielding, anticorrosion, energy storage, absorption etc.Publication number be CN 1450210A patent disclosure soluble polyaniline and polyacrylonitrile that organic sulfonic acid is mixed be dissolved in jointly in the mixed solvent, employing wet spinning technology is with the mixed solution spinning moulding; Publication number is that the patent of CN 1316554A adopts the wet spinning technology that polyaniline and polyamide and adulterant blend solution are clamp-oned in the coagulating bath, makes conductive fiber behind the drawn; Publication number be CN 1749476A patent report polyester, viscose glue or wool are carried out preliminary treatment with oxidant, apply continuously the intrinsic conduction monomer methods on its surface again; Publication number be CN 1155167A patent disclosure the synthetic polythiophene film of a kind of electrochemical deposition method that contains the conductive fiber that is arranged in parallel, this laminated film can be used as the positive pole of charged lithium cells.Publication number is that the patent of CN 1161980A has been described by the polypyrrole coating and presented the conductive cellulose fento, and with the preparation method of colloid discrete form, and it is mixed the polymer latex Ruzhong to generate composite; Publication number be CN 101070672A patent disclosure a kind of super-hydrophobic conductive fiber, process for making such fabric, be included in and utilize conducting polymer chemical oxidation in-situ polymerization at fiber or fabric face coated with conductive polymeric layer, the existence of this conductive polymer coating makes fiber or fabric possess super-hydrophobic character, has had the automatically cleaning ability.Publication number be CN 101250742A patent disclosure a kind of electrical potential difference of utilizing at conductive fiber fabric face absorption CNT, and utilize CNT to improve the method for interface performance of conductive fiber composite material.
For containing the high molecular conductive fiber of intrinsic conduction, in the blend direct spinning, conducting polymer particle addition is higher, cause co-blended spinning process difficulty, descending significantly appears in the mechanical property of fiber, in dispersion and spinning process, adopt strong shearing force also can destroy the structure of conducting polymer simultaneously, the composite fibre electric conductivity is reduced significantly.The conductive coating of the composite fibre that the post processing cladding process obtains comes off in washing and friction easily, also can make general fibre lose original excellent mechanical performances, be difficult to further be woven into fabric, and its electrical conductivity on the low side has limited its range of application, particularly make it lose its distinctive electric property to the high molecular embedding of intrinsic conduction meeting at polymeric matrix, as: energy storage characteristic, adsorption capacity.Intrinsic conduction macromolecule and synthetic fiber are acted synergistically, make the conductive fiber system of gained can obtain high conductance, can keep the original excellent mechanical performances of fiber again, and can make compound intrinsic conducting polymer bring into play its distinctive energy storage characteristic simultaneously, be the technical problem that the researcher needs to be resolved hurrily always.
Summary of the invention
Technical problem to be solved by this invention provides coaxial composite conducting fiber of a kind of ternary and preparation method thereof, and conductive fiber conductive effect of the present invention is good, elasticity is high, soft; This preparation technology is simple, and the equipment input cost is cheap, is suitable for large-scale production and application.
The coaxial composite conducting fiber of a kind of ternary of the present invention, the sandwich layer of this fiber is a polyurethane fiber, and the intermediate layer is a CNT, and skin is an intrinsic conducting polymer, and has coaxial configuration; Wherein each composition weight proportioning is 70～98 parts of polyurethane fibers, 1～10 part of CNT, 1～20 part of intrinsic conducting polymer.
The preparation method of the coaxial composite conducting fiber of a kind of ternary of the present invention comprises:
(1) preliminary treatment of polyurethane fiber: adopt ether at ambient temperature polyurethane fiber to be carried out preliminary treatment, the processing time is 5～30 minutes, takes out back cleaning, drying, gets pretreated polyurethane fiber;
(2) prepare carbon nano-tube/poly ammonia ester binary composite fibre: above-mentioned pretreated polyurethane fiber is immersed in the organic solvent reactive bath technique that contains CNT handled 1～10 minute, utilize the open structure that forms after the fiber swelling, make CNT be embedded into the polyurethane fiber top layer, form the CNT intermediate layer, obtain carbon nano-tube/poly ammonia ester binary composite fibre;
(3) preparation intrinsic conducting polymer/coaxial composite conducting fiber of carbon nano-tube/poly ammonia ester ternary: above-mentioned carbon nano-tube/poly ammonia ester binary composite fibre is immersed in the intrinsic conduction polymerization single polymerization monomer solution, infiltrating time is 1～2 hour, drip the oxidizing agent solution that contains adulterant again, rate of addition is 0.5～1.5mL/min, system was reacted in ice-water bath 5～7 hours, take out cleaning, drying after 3～5 hours in reaction under 2～10 ℃ again, promptly get the coaxial composite conducting fiber of ternary.
CNT described in the above-mentioned steps (2) is one or more of Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, and diameter is 0.4～60nm, and length is 1～15 μ m.
Organic solvent described in the above-mentioned steps (2) is meant one or more in oxolane, dimethyl formamide, dimethylacetylamide, the dimethyl sulfoxide (DMSO).
Intrinsic conducting polymer monomer described in the above-mentioned steps (3) is aniline or pyrroles, and adulterant is hydrochloric acid solution or sodium chloride solution, and oxidant is ammonium persulfate or six hydration ferric oxides.
When the intrinsic conducting polymer monomer described in the above-mentioned steps (3) is aniline, the hydrochloric acid solution of the preferred aniline of monomer solution, wherein monomer concentration is 0.1～1mol/L, the concentration of hydrochloric acid is 1mol/L.
When the intrinsic conducting polymer monomer described in the above-mentioned steps (3) is aniline, the hydrochloric acid solution of oxidant initiator system of ammonium persulfate, the hydrochloric acid solution of the preferred 1mol/L of adulterant, oxidant concentration are 0.1～1.25mol/L.
When the intrinsic conducting polymer monomer described in the above-mentioned steps (3) is the pyrroles, the preferred pyrroles's of monomer solution sodium chloride solution, wherein monomer concentration is 0.1～1mol/L, the concentration of sodium chloride is 0.3mol/L.
When the intrinsic conducting polymer monomer described in the above-mentioned steps (3) is the pyrroles, the preferred Iron(III) chloride hexahydrate (FeCl of oxidant
36H
2O) sodium chloride solution, the sodium chloride solution of the preferred 0.3mol/L of adulterant, oxidant concentration are 0.2～3mol/L.
The coaxial composite conducting fiber volume conductance of the ternary scope of gained is 10 in the above-mentioned steps (3)
-4～10
2Ω
-1Cm
-1
The coaxial composite conducting fiber of ternary of the present invention comprises conducting particles clad and elastomeric polymer fiber sandwich layer, and the intermediate layer is a CNT, and CNT can increase the interaction force between outer intrinsic conducting polymer and polyurethane fiber matrix.This ternary composite conducting fiber can be effectively as antistatic, electromagnetic shielding and the flexible sorbing material that can weave, super capacitor material etc.
Beneficial effect
(1) the electrically conductive composite fibre conductive effect of gained of the present invention is good, elasticity is high, soft;
(2) preparation technology of the present invention is simple, and the equipment input cost is cheap, is suitable for large-scale production and application;
(3) the coaxial composite conducting fiber of ternary disclosed by the invention is antistatic except that can be used for, and outside the electromagnetic shielding material, also is applicable to other a plurality of special dimensions such as flexible super capacitor material that can weave.
Description of drawings
The sem photograph on the pretreated polyurethane fiber of Fig. 1 surface.
The sem photograph on Fig. 2 carbon nano-tube/poly ammonia ester binary composite fibre surface.
The sem photograph on Fig. 3 polyaniline/coaxial composite fibre of carbon nano-tube/poly ammonia ester ternary surface.
Fig. 4 intrinsic conducting polymer/coaxial composite fibre the schematic diagram of carbon nano-tube/poly ammonia ester ternary.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Polyurethane fiber was handled in ether 5 minutes, and dry, this polyurethane fiber was handled 1 minute in the oxolane treatment fluid of carbon nanotubes (Single Walled Carbon Nanotube, diameter 0.4nm, length 1 μ m); Place the hydrochloric acid solution (concentration of hydrochloric acid is 1M) of aniline to soak into 1h the fiber after handling, aniline concentration is 0.1mol/L; In this solution, drip ammonium persulfate hydrochloric acid solution (ammonium persulfate concentration is 0.1mol/L) again, rate of addition is 0.5ml/min, system is reacted 5h in ice-water bath after, continue reaction 5h down at 2 ℃, fiber is taken out cleaning, promptly get polyaniline/carbon nano-tube/poly ammonia ester ternary composite fibre, wherein the weight proportion of each component is 1 part of a polyaniline, 1 part of CNT, 98 parts of polyurethane; This polyaniline/carbon nano-tube/poly ammonia ester ternary composite fibre conductance is 10
-4Ω
-1Cm
-1
Embodiment 2
Polyurethane fiber was handled in ether 30 minutes, and dry, this polyurethane fiber was handled 10 minutes in the methyl-sulfoxide treatment fluid of carbon nanotubes (multi-walled carbon nano-tubes, diameter 60nm, length 15 μ m); Place the hydrochloric acid solution (concentration of hydrochloric acid is 1M) of aniline to soak into 2h the fiber after handling, aniline concentration is 1mol/L; In this solution, drip ammonium persulfate hydrochloric acid solution (ammonium persulfate concentration is 1.25mol/L) again, rate of addition is 1ml/min, system is reacted 6h in ice-water bath after, continue reaction 4h down at 4 ℃, fiber is taken out cleaning, promptly get polyaniline/carbon nano-tube/poly ammonia ester ternary composite fibre, wherein the weight proportion of each component is 20 parts of polyanilines, 10 parts of CNTs, 70 parts of polyurethane; This polyaniline/carbon nano-tube/poly ammonia ester ternary composite fibre conductance is 10
2Ω
-1Cm
-1
Embodiment 3
Polyurethane fiber was handled 5 minutes in ether successively, and dry, this polyurethane fiber was handled 1 minute in the dimethylacetylamide treatment fluid of carbon nanotubes (Single Walled Carbon Nanotube, diameter 20nm, length 5 μ m); Place pyrroles's sodium chloride solution (concentration of sodium chloride solution is 0.3M) to soak into 1h the fiber after handling, pyrroles's concentration is 0.1mol/L; In this solution, drip ferric trichloride sodium chloride solution (ferric trichloride concentration is 0.2mol/L) again, rate of addition is 1.5ml/min, system is reacted 7h in ice-water bath after, continue reaction 3h down at 10 ℃, fiber is taken out cleaning, promptly get polypyrrole carbon nano-tube/poly ammonia ester ternary composite fibre, wherein the weight proportion of each component is 5 parts of polypyrroles, 5 parts of CNTs, 80 parts of polyurethane; This polypyrrole/carbon nano-tube/poly ammonia ester ternary composite fibre conductance is 10
-4Ω
-1Cm
-1
Embodiment 4
Polyurethane fiber was handled in ether 30 minutes, and dry, this polyurethane fiber was handled 10 minutes in the dimethyl formamide treatment fluid of carbon nanotubes (multi-walled carbon nano-tubes, diameter 40nm, length 8 μ m); Place pyrroles's sodium chloride solution (concentration of sodium chloride solution is 0.3 M) to soak into 2h the fiber after handling, pyrroles's concentration is 1mol/L; In this solution, drip the sodium chloride solution (ferric trichloride concentration is 3mol/L) of Iron(III) chloride hexahydrate again, rate of addition is 1ml/min, system is reacted 6h in ice-water bath after, continue reaction 4h down at 4 ℃, fiber is taken out cleaning, promptly get polypyrrole carbon nano-tube/poly ammonia ester ternary composite fibre, wherein the weight proportion of each component is 20 parts of polypyrroles, 10 parts of CNTs, 70 parts of polyurethane; This polypyrrole/carbon nano-tube/poly ammonia ester ternary composite fibre conductance is 10
2Ω
-1Cm
-1
Claims (8)
1. coaxial composite conducting fiber of ternary, the sandwich layer of this fiber is a polyurethane fiber, and the intermediate layer is a CNT, and skin is an intrinsic conducting polymer, and has coaxial configuration; Wherein each composition weight proportioning is 70～98 parts of polyurethane fibers, 1～10 part of CNT, 1～20 part of intrinsic conducting polymer.
2. the preparation method of the coaxial composite conducting fiber of ternary comprises:
(1) at ambient temperature polyurethane fiber is carried out preliminary treatment with ether, the processing time is 5～30 minutes, takes out back cleaning, drying, gets pretreated polyurethane fiber;
(2) above-mentioned pretreated polyurethane fiber is immersed in the organic solvent reactive bath technique that contains CNT handled 1～10 minute, make CNT be embedded into the polyurethane fiber top layer and form the CNT intermediate layer, obtain carbon nano-tube/poly ammonia ester binary composite fibre;
(3) above-mentioned carbon nano-tube/poly ammonia ester binary composite fibre is immersed in the intrinsic conduction polymerization single polymerization monomer solution, infiltrating time is 1～2 hour, drip the oxidizing agent solution that contains adulterant again, rate of addition is 0.5～1.5mL/min, system was reacted in ice-water bath 5～7 hours, take out cleaning, drying after 3～5 hours in reaction under 2～10 ℃ again, promptly get the coaxial composite conducting fiber of ternary.
3. the preparation method of the coaxial composite conducting fiber of a kind of ternary according to claim 2, it is characterized in that: the CNT described in the step (2) is one or more of Single Walled Carbon Nanotube or multi-walled carbon nano-tubes, diameter is 0.4～60nm, and length is 1～15 μ m.
4. the preparation method of the coaxial composite conducting fiber of a kind of ternary according to claim 2 is characterized in that: the organic solvent described in the step (2) is meant one or more in oxolane, dimethyl formamide, dimethylacetylamide, the dimethyl sulfoxide (DMSO).
5. the preparation method of the coaxial composite conducting fiber of a kind of ternary according to claim 2, it is characterized in that: the intrinsic conducting polymer monomer described in the step (3) is aniline or pyrroles, adulterant is hydrochloric acid solution or sodium chloride solution, and oxidant is ammonium persulfate or six hydration ferric oxides.
6. according to the preparation method of claim 2 or the coaxial composite conducting fiber of 5 described a kind of ternarys, it is characterized in that: when the intrinsic conducting polymer monomer described in the step (3) is aniline, monomer solution is the hydrochloric acid solution of aniline, wherein monomer concentration is 0.1～1mol/L, and the concentration of hydrochloric acid is 1mol/L; When the intrinsic conducting polymer monomer was the pyrroles, monomer solution was pyrroles's a sodium chloride solution, and wherein monomer concentration is 0.1～1mol/L, and the concentration of sodium chloride is 0.3mol/L.
7. according to the preparation method of claim 2 or the coaxial composite conducting fiber of 5 described a kind of ternarys, it is characterized in that: when the intrinsic conducting polymer monomer described in the step (3) is aniline, oxidant is the hydrochloric acid solution of ammonium persulfate, adulterant is the hydrochloric acid solution of 1mol/L, and oxidant concentration is 0.1～1.25mol/L; When the intrinsic conducting polymer monomer was the pyrroles, oxidant was Iron(III) chloride hexahydrate FeCl
36H
2The sodium chloride solution of O, adulterant are the sodium chloride solution of 0.3mol/L, and oxidant concentration is 0.2～3mol/L.
8. the preparation method of the coaxial composite conducting fiber of a kind of ternary according to claim 2 is characterized in that: the coaxial composite conducting fiber volume conductance of the ternary scope of gained is 10 in the step (3)
-4～10
2Ω
-1Cm
-1
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| CN109338727A (en) * | 2018-09-26 | 2019-02-15 | 嘉兴学院 | A kind of preparation method of flexible wearable strain transducer |
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