CN110387743B - Conductive composite fiber bundle and preparation method thereof - Google Patents
Conductive composite fiber bundle and preparation method thereof Download PDFInfo
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- CN110387743B CN110387743B CN201910647666.9A CN201910647666A CN110387743B CN 110387743 B CN110387743 B CN 110387743B CN 201910647666 A CN201910647666 A CN 201910647666A CN 110387743 B CN110387743 B CN 110387743B
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Abstract
The invention provides a conductive composite fiber bundle and a preparation method thereof, and the preparation method of the conductive composite fiber bundle is characterized in that 3, 4-ethylenedioxythiophene is polymerized on the fiber bundle in situ by a reverse microemulsion method to prepare a uniform and compact nano linear poly 3, 4-ethylenedioxythiophene conductive composite fiber bundle. The preparation method can regulate and control the forming conditions of the poly 3, 4-ethylenedioxythiophene on the surface of the fiber bundle, form a more regular nano linear structure beneficial to electron transmission and migration, and has the advantages of simple process, strong controllability and good repeatability. The prepared conductive composite fiber bundle can be applied to the fields of wearable electronic devices, energy storage, sensors and the like.
Description
Technical Field
The invention relates to the field of preparation of conductive fiber materials, in particular to a conductive composite fiber bundle and a preparation method thereof.
Background
The conductive fiber is used as an important intelligent material, draws wide attention in the material field at home and abroad, and has great application prospect in the fields of clothing, sensors, intelligent textiles and the like.
In recent years, conductive polymers have been widely used in the fields of modified electrodes, electrochemistry, sensors, and the like. Among them, the most environmentally friendly conductive polymer, poly (3, 4-ethylenedioxythiophene) (PEDOT), is a unique one among many conductive polymers due to its advantages such as simple molecular structure, high conductivity, good stability and small energy gap, and has been widely studied and paid attention. Thus, PEDOT is an excellent conductive carrier. PEDOT-based conductive materials exhibit various nanostructures such as nanosheets, nanoflowers, nanowires, and the like, with large surface areas, high conductivity, fast electron transfer rates, hydrophobic interactions, and good biocompatibility.
The invention patent with the application number of CN201710128767.6 discloses a three-dimensional stretchable conductive material and a preparation method thereof, wherein a polyurethane fiber mat is obtained by an electrospinning method, and conductive PEDOT is formed on the polyurethane fiber mat through interfacial polymerization, so that a flexible conductive fiber mat is obtained.
The invention patent with the application number of CN201710329153.4 discloses a flexible wearable nanofiber fabric sensor and a preparation method thereof. The continuous nanofiber yarn is prepared by a conjugated electrostatic spinning yarn technology, and then a layer of PEDOT is polymerized and coated on the surface of the fiber in the yarn, so that the prepared nanofiber yarn has good conductivity.
However, although the conventional in situ polymerization method for preparing PEDOT has simple steps, the polymerization reaction is difficult to control due to more uncontrollable factors, and thus, most of the PEDOT structures formed on the fibers are agglomerated particles or stacked blocks, but the irregular structures are not favorable for electron transmission and migration. The uncontrollable nature of PEDOT nanostructures has historically limited their development and use.
At present, no report is found on a method for carrying out in-situ polymerization reaction on 3, 4 ethylene dioxythiophene monomer by adopting a reverse microemulsion method.
Disclosure of Invention
In view of the above disadvantages, the present invention is directed to a conductive composite fiber bundle and a method for preparing the same. According to the preparation method of the conductive composite fiber bundle, 3, 4-ethylenedioxythiophene is polymerized onto the fiber bundle in situ by a reverse micro-emulsion method, so that the uniform and compact nano linear poly 3, 4-ethylenedioxythiophene conductive composite fiber bundle is prepared. The preparation method can regulate and control the forming conditions of the poly 3, 4-ethylenedioxythiophene on the surface of the fiber bundle, form a regular nano linear structure beneficial to electron transmission and migration, and has the advantages of simple process, strong controllability and good repeatability. The prepared conductive composite fiber bundle can be applied to the fields of wearable electronic devices, energy storage, sensors and the like.
In order to achieve the above object, the present invention provides a method for preparing a conductive composite fiber bundle, comprising the steps of:
s1, performing surface decontamination treatment on the fiber monofilaments, and then airing to obtain fiber bundles for later use;
s2, mixing the surfactant and the organic solvent at a preset temperature to prepare a surfactant organic solution with a preset concentration;
s3, mixing an oxidant and deionized water at normal temperature to prepare an oxidant aqueous solution with a preset concentration;
s4, at room temperature, putting the fiber bundle obtained in the step S1 into the organic solution of the surfactant prepared in the step S2, and carrying out dipping and stirring treatment; then adding the oxidant aqueous solution prepared in the step S3 into the solution according to a preset volume ratio, and stirring; finally, adding 3, 4 ethylene dioxythiophene monomer according to a preset volume ratio, stirring, and completing the in-situ polymerization reaction of the 3, 4 ethylene dioxythiophene of the fiber bundle by adopting a reverse microemulsion method;
and S5, washing and drying to obtain the conductive composite fiber bundle.
Preferably, in step S4, the volume ratio of the aqueous solution of the oxidizing agent to the organic solvent is 0.017 to 0.045.
Preferably, in step S4, the volume ratio of the 3, 4-ethylenedioxythiophene monomer to the organic solvent is 0.0030 to 0.0067.
Preferably, in step S2, the surfactant has a mass concentration of 10 wt% to 20 wt%; the mass concentration of the organic solvent is 80-90 wt%.
Preferably, the surfactant is dioctyl sodium sulfosuccinate.
Preferably, in step S3, the concentration of the oxidant in the oxidant aqueous solution is 6mol/L to 8 mol/L; the oxidant is one of anhydrous ferric trichloride and ferric trichloride hexahydrate.
Preferably, in step S2, the organic solvent is one or both of n-hexane and p-xylene; the preset temperature is 15-25 ℃.
Preferably, the fiber bundle comprises but is not limited to one of aramid fiber, nylon fiber, polyester fiber, cotton fiber, polyamide fiber and silk fiber, and the fiber length of the fiber bundle is 10-20 cm.
In order to achieve the above object, the present invention further provides a conductive composite fiber bundle prepared by the preparation method according to any one of the above technical solutions, which comprises a fiber base material and nano linear poly 3, 4-ethylenedioxythiophene deposited on the surface of the fiber base material by in-situ polymerization through a reverse microemulsion method.
Preferably, the length of the fiber base material is 10-20 cm.
The reaction principle of the invention is as follows:
the reversed-phase interfacial polymerization method is an effective method for preparing the one-dimensional PEDOT nanometer structure. In the reverse microemulsion system, water promotes aggregation of surfactant molecules in the non-polar solvent through mutual dissolution of polar groups and hydrogen bonds. Thus, a number of reactants can be introduced into the aqueous, nano-sized reaction zone in the reverse phase micelle. These micelles act as nanoreactors.
Dioctyl sodium sulfosuccinate (AOT) is a double-tailed anionic surfactant, can be well dissolved in an organic solvent such as n-hexane or p-xylene, and different PEDOT nanostructures such as nanorods, nanofibers, nanotubes and the like can be prepared by adjusting reaction conditions such as the volume ratio of water to the organic solvent, the fixed stirring speed and mode, the monomer concentration, the molar ratio of the monomer to the oxidant and the like.
Anhydrous ferric trichloride (FeCl)3) Or ferric chloride hexahydrate (FeCl)3·6H2O) is the most commonly used oxidizing agent in EDOT oxidative polymerization. When FeCl is added3Or FeCl3·6H2When the O aqueous solution is added into the solution of AOT, the anion of the head of AOT is mixed with Fe3+Reversed-phase cylindrical micelles are formed by electrostatic attraction, and therefore, Fe3+Can be absorbed on the anion head of the AOT. In the chemical oxidative polymerization of EDOT monomers, Fe3+Acting as an oxidizing agent and in AOT reversed-phase cylindrical micellesThe polarization center forms a water channel, so that a one-dimensional water-oil interface divided by the reversed-phase cylindrical micelle is constructed, and the necessary condition for carrying out interfacial polymerization reaction in a nanometer scale is provided.
In the system, the hydrophilic group of the AOT reversed micelle is outside, the lipophilic group is inside, and with the increase of the reversed micelle, after the ferric trichloride solution is added, the groups form a column; after EDOT monomer is added, the monomer is polymerized outside the columnar micelle, and after the reaction is finished, AOT is washed away, and PEDOT nano-fiber on the outer side is remained.
The invention has the beneficial effects that:
1. according to the preparation method provided by the invention, chemical in-situ polymerization is carried out by using a reverse microemulsion method, and the PEDOT polymerization reaction process is regulated and controlled by controlling the volume ratio of the oxidant aqueous solution to the organic solvent and the volume ratio of the 3, 4-ethylenedioxythiophene to the organic solvent, so that a uniform and compact PEDOT nanowire structure which is beneficial to ion transmission and migration is formed on the surface of a fiber bundle, and the defects of the prior art are overcome.
2. The preparation method provided by the invention has the advantages of simple process, strong controllability and good repeatability, and is suitable for large-scale application and popularization.
3. The conductive composite fiber bundle prepared by the invention can be widely applied to the fields of wearable electronic devices, energy storage, sensing and the like.
Drawings
FIG. 1 is an electron microscope image of aramid fiber fibrils, with a scale of 10 um.
Fig. 2 is an electron microscope image of the nano linear PEDOT conductive composite aramid fiber prepared in example 1, with a scale of 1 um.
Fig. 3 is an electron microscope image of the local distribution of the nano linear PEDOT conductive composite aramid fiber prepared in example 1, with a ruler of 100 nm.
FIG. 4 is an electron micrograph of cotton fibrils with a scale of 10 um.
Fig. 5 is an electron microscope image of the nano linear PEDOT conductive conjugate cotton fiber prepared in example 6, with a scale of 1 um.
FIG. 6 is an electron microscope image of the local distribution of the nano linear PEDOT conductive composite cotton fiber prepared in example 6, with a ruler at 100 nm.
Fig. 7 is a resistance diagram of the nano linear PEDOT conductive composite aramid fiber prepared in example 1 of the present invention.
Fig. 8 is a resistance diagram of the nano wire-shaped PEDOT conductive composite cotton fiber prepared in example 6 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments; all other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
The invention provides a preparation method of a conductive composite fiber bundle, which comprises the following steps:
s1, performing surface decontamination treatment on the fiber monofilaments, and then airing to obtain fiber bundles for later use;
s2, mixing the surfactant and the organic solvent at a preset temperature to prepare a surfactant organic solution with a preset concentration;
s3, mixing an oxidant and deionized water at normal temperature to prepare an oxidant aqueous solution with a preset concentration;
s4, at room temperature, putting the fiber bundle obtained in the step S1 into the organic solution of the surfactant prepared in the step S2, and carrying out dipping and stirring treatment; then adding the oxidant aqueous solution prepared in the step S3 into the solution according to a preset volume ratio, and stirring; finally, adding 3, 4 ethylene dioxythiophene monomer according to a preset volume ratio, stirring, and completing the in-situ polymerization reaction of the 3, 4 ethylene dioxythiophene of the fiber bundle by adopting a reverse microemulsion method;
and S5, washing and drying to obtain the conductive composite fiber bundle.
Wherein, in step S1, the surface desmutting process includes the steps of:
s11, ultrasonically cleaning the fiber monofilaments for 10-30min by using deionized water, and airing at room temperature;
s12, ultrasonically cleaning the fiber monofilaments for 10-30min by using absolute ethyl alcohol, and airing at room temperature;
s13, ultrasonically cleaning the fiber monofilaments for 10-30min by using acetone, and airing at room temperature for later use.
In step S2, the mass concentration of the surfactant is 10 wt% to 20 wt%; the mass concentration of the organic solvent is 80-90 wt%. Preferably, the surfactant is dioctyl sodium sulfosuccinate. In step S2, the organic solvent is one or both of n-hexane and p-xylene; the preset temperature is 15-25 ℃.
In step S3, the concentration of the oxidizing agent in the aqueous oxidizing agent solution is 6 to 8 mol/L. The oxidant is one of anhydrous ferric trichloride and ferric trichloride hexahydrate.
In step S4, the volume ratio of the aqueous oxidant solution to the organic solvent is 0.017 to 0.045. The volume ratio of the 3, 4-ethylenedioxythiophene monomer to the organic solvent is 0.0030-0.0067.
The invention also provides the conductive composite fiber bundle prepared by the preparation method, which comprises a fiber base material and the nano linear poly 3, 4-ethylenedioxythiophene in-situ polymerized and deposited on the surface of the fiber base material by a reverse microemulsion method. Preferably, the length of the fibrous base material is 10-20 cm.
The following description will be made of a method for producing a conductive composite fiber bundle with reference to examples 1 to 16 and comparative examples 1 to 5:
example 1
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting aramid fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the aramid fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing 15g of dioctyl sodium sulfosuccinate with 100ml of p-xylene at 20 ℃ to prepare 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing anhydrous ferric trichloride with the mass of 3.0g and deionized water with the volume of 2.7ml at normal temperature, and fully and uniformly stirring to obtain an anhydrous ferric trichloride solution with the concentration of 7.2M;
d. EDOT in situ polymerization of fiber bundles:
b, putting the aramid fiber bundles obtained in the step a into the surfactant organic solution prepared in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the anhydrous ferric trichloride solution prepared in the step c; after stirring evenly for 30min, 470ul of EDOT was added dropwise and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying:
and d, washing the aramid fiber bundles obtained after the reaction in the step d, and drying to obtain the conductive composite aramid fiber bundles.
Fig. 1 to 3 are electron microscope images of local distribution of aramid fiber fibrils, nano linear PEDOT conductive composite aramid fibers and nano linear PEDOT conductive composite aramid fibers, respectively, and it can be known that the surfaces of the aramid fiber fibrils are smooth, and the PEDOT on the surfaces of the conductive composite fibers prepared by the present invention is in nano linear structure distribution and is staggered with each other to form relatively uniform and dense three-dimensional network distribution, which is beneficial to electron transmission and migration, and forms a high-efficiency conductive network.
As the length of the conductive composite fiber bundle increases, the resistivity tends to increase uniformly and rapidly, and the conductivity is significantly improved, as shown in fig. 7.
Comparative example 1
And carrying out in-situ polymerization on the PEDOT conductive composite fiber bundle by adopting a traditional method.
Conducting performance analysis of the composite fiber bundle was performed by using example 1 and comparative example 1, and the electrical resistance of the composite fiber bundle prepared in example 1 was 205 Ω/cm, and the electrical resistance of the composite fiber bundle prepared in comparative example 1 was 423 Ω/cm; the conductive composite fiber prepared in the comparative example 1 has uncontrollable and nonuniform appearance and relatively high resistance due to the adoption of the conductive fiber prepared by the traditional method.
Example 2
The only difference from example 1 is: the volume ratio of the aqueous oxidant solution to the organic solvent is 0.017, and other steps are basically the same and are not described again.
Example 3
The only difference from example 1 is: the volume ratio of the aqueous oxidant solution to the organic solvent is 0.045, and other steps are basically the same and are not repeated herein.
Comparative example 2
The only difference from example 1 is: the volume ratio of the aqueous oxidant solution to the organic solvent is 0.010, and other steps are basically the same and are not repeated.
Comparative example 3
The only difference from example 1 is: the volume ratio of the oxidant aqueous solution to the organic solvent is 0.055, and other steps are basically the same and are not repeated herein.
Table 1 shows the influence of the volume change of the aqueous solution of the oxidizing agent and the organic solvent on the electrical conductivity of the conductive composite fiber bundle in examples 1 to 3 and comparative examples 2 to 3
From table 1, it can be seen that: in the range that the volume ratio of the oxidant aqueous solution to the organic solvent is 0.017-0.15, the resistance shows a gradually rising change rule along with the increase of the volume ratio of the oxidant aqueous solution to the organic solvent.
In comparative examples 2 to 3, when the volume ratios of the aqueous oxidant solution and the organic solvent were 0.010 and 0.055, respectively, the composite fiber bundle had a large resistance, and although the conductive fiber was prepared by the reverse microemulsion method, the conductive fiber was not formed into a uniform nanowire-shaped PEDOT structure due to a large change in parameters, and therefore the conductive performance was not as good as that of the conductive fiber with strictly controlled parameters, and the resistance was generally large.
Example 4
The only difference from example 1 is: the volume ratio of the 3, 4-ethylenedioxythiophene to the organic solvent is 0.0030, and other steps are basically the same and are not repeated.
Example 5
The only difference from example 1 is: the volume ratio of the 3, 4 ethylene dioxythiophene to the organic solvent is 0.0067, and other steps are basically the same and are not repeated.
Comparative example 4
The only difference from example 1 is: the volume ratio of the 3, 4 ethylene dioxythiophene to the organic solvent is 0.0020, and other steps are basically the same and are not repeated.
Comparative example 5
The only difference from example 1 is: the volume ratio of the 3, 4 ethylenedioxythiophene to the organic solvent is 0.0075, and other steps are basically the same and are not repeated herein.
Table 2 shows the influence of the change in the volume ratio of 3, 4 ethylenedioxythiophene to the organic solvent on the electrical conductivity of the fiber bundle in examples 1, 4 to 5 and 4 to 5
From table 2, it can be seen that: in the range of the volume ratio of EDOT to the organic solvent being 0.0030-0.0067, the resistance shows a gradually decreasing change rule along with the increase of the volume ratio of the 3, 4 ethylene dioxythiophene monomer to the organic solvent.
In comparative examples 4 to 5, when the volume ratio of EDOT to the organic solvent was 0.0020 and 0.0075, respectively, the resistance of the composite fiber bundle was large, and although the conductive fiber was prepared by the reverse microemulsion method, the conductive fiber was not formed into a uniform nanowire-like PEDOT structure due to a large change in parameters, and therefore the conductive performance was not as good as that of the conductive fiber with strictly controlled parameters, and the resistance was generally large.
Example 6
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting the cotton fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the cotton fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing dioctyl sodium sulfosuccinate with a mass of 12g and paraxylene with a volume of 80ml at a temperature of 20 ℃ to prepare a dioctyl sodium sulfosuccinate solution with a concentration of 0.34M;
c. preparing an oxidant aqueous solution:
mixing anhydrous ferric trichloride with the mass of 2.4g and deionized water with the volume of 2.2ml at normal temperature, and fully and uniformly stirring to obtain an anhydrous ferric trichloride solution with the concentration of 7M;
d. EDOT in situ polymerization of fiber bundles:
b, placing the cotton fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the anhydrous ferric trichloride solution prepared in the step c; uniformly stirring for 30min, dropwise adding 380ul of EDOT, and reacting at room temperature for 24 h;
e. cleaning and drying:
and d, cleaning the cotton fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite cotton fiber bundle.
Fig. 4-6 are electron microscope images of local distribution of cotton fiber fibril, nano linear PEDOT conductive composite cotton fiber and nano linear PEDOT conductive composite cotton fiber, and it can be known that the surface of cotton fiber fibril is smooth, and the PEDOT on the surface of the conductive composite fiber prepared by the invention is in nano linear structure distribution and is staggered with each other to form uniform and dense three-dimensional network distribution, which is beneficial to electron transmission and migration and forms an efficient conductive network.
As the length of the conductive composite fiber bundle increases, the resistivity tends to increase uniformly and rapidly, and the conductivity is significantly improved, as shown in fig. 8.
Example 7
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting nylon fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the nylon fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing 18g of dioctyl sodium sulfosuccinate with 120ml of p-xylene at 20 ℃ to prepare 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing anhydrous ferric trichloride with the mass of 3.7g and deionized water with the volume of 3.24ml at normal temperature, and fully and uniformly stirring to obtain an anhydrous ferric trichloride solution with the concentration of 7.5M;
d. EDOT in situ polymerization of fiber bundles:
b, putting the nylon fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the anhydrous ferric trichloride solution prepared in the step c; after stirring evenly for 30min, 560ul of EDOT was added dropwise, and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying: and d, cleaning the nylon fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite nylon fiber bundle.
Example 8
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting polyester fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the polyester fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing sodium dioctyl sulfosuccinate with a mass of 22.6g with p-xylene with a volume of 150ml at a temperature of 20 ℃ to prepare a 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing anhydrous ferric trichloride with the mass of 4.6g and deionized water with the volume of 4ml at normal temperature, and fully and uniformly stirring to obtain an anhydrous ferric trichloride solution with the concentration of 8M;
d. EDOT in situ polymerization of fiber bundles:
b, placing the polyester fiber bundles obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the anhydrous ferric trichloride solution prepared in the step c; after stirring evenly for 30min, 705ul of EDOT was added dropwise and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying:
and d, cleaning the polyester fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite polyester fiber bundle.
Example 9
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting spandex fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the spandex fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing 27.2g of dioctyl sodium sulfosuccinate with 180ml of p-xylene at 20 ℃ to prepare 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing ferric trichloride hexahydrate with the mass of 5.5g and deionized water with the volume of 4.86ml at normal temperature, and fully and uniformly stirring to obtain a ferric trichloride hexahydrate solution with the concentration of 6M;
d. EDOT in situ polymerization of fiber bundles:
b, putting the spandex fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the ferric trichloride hexahydrate solution prepared in the step c; after stirring evenly for 30min, 850ul of EDOT was added dropwise, and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying:
and d, cleaning the spandex fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite spandex fiber bundle.
Example 10
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting silk fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the silk fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing 30.2g of dioctyl sodium sulfosuccinate with 200ml of p-xylene at 20 ℃ to prepare 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing anhydrous ferric trichloride with the mass of 6.1g and deionized water with the volume of 5.4ml at normal temperature, and fully and uniformly stirring to obtain an anhydrous ferric trichloride solution with the concentration of 6.5M;
d. EDOT in situ polymerization of fiber bundles:
b, at the temperature of 20 ℃, putting the silk fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b, soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the anhydrous ferric trichloride solution prepared in the step c; after stirring evenly for 30min, 940ul EDOT is added dropwise, the reaction is carried out at room temperature, and the reaction time is 24 h.
e. Cleaning and drying:
and d, cleaning the silk fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite silk fiber bundle.
Example 11
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting the cotton fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the cotton fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing dioctyl sodium sulfosuccinate with a mass of 12g and n-hexane with a volume of 80ml at a temperature of 20 ℃ to prepare a dioctyl sodium sulfosuccinate solution with a concentration of 0.34M;
c. preparing an oxidant aqueous solution:
mixing ferric trichloride hexahydrate with the mass of 4.0g and deionized water with the volume of 2.2ml at normal temperature, and fully and uniformly stirring to obtain a ferric trichloride hexahydrate solution with the concentration of 7M;
d. EDOT in situ polymerization of fiber bundles:
b, placing the cotton fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the ferric trichloride hexahydrate solution prepared in the step c; after stirring evenly for 30min, 380ul EDOT was added dropwise, and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying:
and d, cleaning the cotton fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite cotton fiber bundle.
Example 12
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting aramid fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the aramid fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing sodium dioctyl sulfosuccinate 15g with n-hexane 100ml at 20 deg.C to obtain 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing ferric trichloride hexahydrate with the mass of 5.1g and deionized water with the volume of 2.7ml at normal temperature, and fully and uniformly stirring to obtain a ferric trichloride hexahydrate solution with the concentration of 7.5M;
d. EDOT in situ polymerization of fiber bundles:
b, putting the aramid fiber bundles obtained in the step a into the surfactant organic solution prepared in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the ferric trichloride hexahydrate solution prepared in the step c; after stirring evenly for 30min, 470ul of EDOT was added dropwise and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying:
and d, washing the aramid fiber bundles obtained after the reaction in the step d, and drying to obtain the conductive composite aramid fiber bundles.
Example 13
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting nylon fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the nylon fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing 18g of dioctyl sodium sulfosuccinate with 120ml of n-hexane at 20 ℃ to prepare 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing ferric trichloride hexahydrate with the mass of 6.1g and deionized water with the volume of 3.24ml at normal temperature, and fully and uniformly stirring to obtain ferric trichloride hexahydrate solution with the concentration of 6.9M;
d. EDOT in situ polymerization of fiber bundles:
b, putting the nylon fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the ferric trichloride hexahydrate solution prepared in the step c; after stirring evenly for 30min, 560ul of EDOT was added dropwise, and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying: and d, cleaning the nylon fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite nylon fiber bundle.
Example 14
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting polyester fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the polyester fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing sodium dioctyl sulfosuccinate with a mass of 22.6g with n-hexane with a volume of 150ml at a temperature of 20 ℃ to prepare a sodium dioctyl sulfosuccinate solution with a concentration of 0.34M;
c. preparing an oxidant aqueous solution:
mixing ferric trichloride hexahydrate with the mass of 7.7g and deionized water with the volume of 4.05ml at normal temperature, and fully and uniformly stirring to obtain a ferric trichloride hexahydrate solution with the concentration of 7M;
d. EDOT in situ polymerization of fiber bundles:
b, placing the polyester fiber bundles obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the ferric trichloride hexahydrate solution prepared in the step c; after stirring evenly for 30min, 850ul of EDOT was added dropwise, and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying:
and d, cleaning the polyester fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite polyester fiber bundle.
Example 15
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting spandex fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the spandex fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing 27g of dioctyl sodium sulfosuccinate with 180ml of n-hexane at 20 ℃ to prepare 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing ferric trichloride hexahydrate with the mass of 9.2g and deionized water with the volume of 4.86ml at normal temperature, and fully and uniformly stirring to obtain a ferric trichloride hexahydrate solution with the concentration of 6M;
d. EDOT in situ polymerization of fiber bundles:
b, putting the spandex fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b at the temperature of 20 ℃, and soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the ferric trichloride hexahydrate solution prepared in the step c; after stirring evenly for 30min, 850ul of EDOT was added dropwise, and the reaction was carried out at room temperature for 24 h.
e. Cleaning and drying:
and d, cleaning the spandex fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite spandex fiber bundle.
Example 16
a. Carrying out surface decontamination treatment on the fiber monofilaments:
sequentially putting silk fiber monofilaments into deionized water, absolute ethyl alcohol and acetone for ultrasonic cleaning for 15min, ensuring that the silk fiber monofilaments are cleaned in the previous step, airing at room temperature, then carrying out cleaning in the next step, and airing at room temperature after the last step of acetone ultrasonic cleaning is finished, and storing for later use;
b. preparing an organic solution of a surfactant:
mixing 30g of dioctyl sodium sulfosuccinate with 200ml of n-hexane at 20 ℃ to prepare 0.34M sodium dioctyl sulfosuccinate solution;
c. preparing an oxidant aqueous solution:
mixing ferric trichloride hexahydrate with the mass of 10.2g and deionized water with the volume of 5.4ml at normal temperature, and fully and uniformly stirring to obtain ferric trichloride hexahydrate solution with the concentration of 8M;
d. EDOT in situ polymerization of fiber bundles:
b, at the temperature of 20 ℃, putting the silk fiber bundle obtained in the step a into the surfactant organic solution obtained in the step b, soaking and uniformly stirring for 30min, wherein the stirring mode is mechanical stirring, and the rotating speed of the mechanical stirring is 400 rmp; after 30min, dropwise adding the ferric trichloride hexahydrate solution prepared in the step c; after uniformly stirring for 30min, 940ul of EDOT is dropwise added, the reaction is carried out at room temperature, and the reaction time is 24 h;
e. cleaning and drying:
and d, cleaning the silk fiber bundle obtained after the reaction in the step d, and drying to obtain the conductive composite silk fiber bundle.
The following table compares the properties of the conductive composite fibers of examples 6-16:
table 3 shows the conditions for preparing the conductive composite fiber bundles and the properties of the prepared conductive composite fiber bundles of examples 6 to 16
From table 3, it can be seen that: the conductive composite fiber bundle prepared by the invention has excellent conductive performance.
The change of the organic solvent and the oxidant can have certain influence on the conductivity of the composite fiber bundle, but the difference is not great.
Because different base materials are different in material and different in surface-carried groups, and different base materials in a reaction system are different in adsorption capacity to oxidants, monomers and the like, the resistance of the obtained conductive fiber bundle is different, but the difference is not large, and is basically kept at a quantity level, and the difference does not exceed 100 omega.
The fiber bundle is not limited to cotton fiber, aramid fiber, nylon fiber, polyester fiber, spandex fiber, silk fiber, and other fibers such as nylon fiber.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (3)
1. The preparation method of the conductive composite fiber bundle is characterized by comprising the following steps of:
s1, performing surface decontamination treatment on the fiber monofilaments, and then airing to obtain fiber bundles for later use;
s2, mixing the surfactant and the organic solvent at a preset temperature to prepare a surfactant organic solution with the concentration of 0.34M;
s3, mixing an oxidant and deionized water at normal temperature to prepare an oxidant aqueous solution with the concentration of 7.2M;
s4, at room temperature, putting the fiber bundle obtained in the step S1 into the organic solution of the surfactant prepared in the step S2, and carrying out dipping and stirring treatment; then adding the oxidant aqueous solution prepared in the step S3 into the solution according to a preset volume ratio, and stirring; finally, adding 3, 4 ethylene dioxythiophene monomer according to a preset volume ratio, stirring, and completing the in-situ polymerization reaction of the 3, 4 ethylene dioxythiophene of the fiber bundle by adopting a reverse microemulsion method;
s5, washing and drying to obtain a conductive composite fiber bundle;
in step S4, the volume ratio of the aqueous oxidant solution to the organic solvent is 0.017;
in step S4, the volume ratio of the 3, 4 ethylenedioxythiophene monomer to the organic solvent is 0.0047;
the surfactant is dioctyl sodium sulfosuccinate;
the oxidant is one of anhydrous ferric trichloride and ferric trichloride hexahydrate;
the fiber bundle is one of aramid fiber, nylon fiber and polyester fiber.
2. The method for producing a conductive composite fiber bundle according to claim 1, characterized in that: in step S2, the organic solvent is one of n-hexane and p-xylene; the preset temperature is 15-25 ℃.
3. The method for producing a conductive composite fiber bundle according to claim 1, characterized in that: the fiber length of the fiber bundle is 10-20 cm.
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