CN113089123B - Zirconium carbide/polypyrrole-polyurethane composite fiber and preparation method and application thereof - Google Patents
Zirconium carbide/polypyrrole-polyurethane composite fiber and preparation method and application thereof Download PDFInfo
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- CN113089123B CN113089123B CN202110428026.6A CN202110428026A CN113089123B CN 113089123 B CN113089123 B CN 113089123B CN 202110428026 A CN202110428026 A CN 202110428026A CN 113089123 B CN113089123 B CN 113089123B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The invention provides a zirconium carbide/polypyrrole-polyurethane composite fiber and a preparation method and application thereof, wherein the composite fiber comprises a polyurethane matrix and zirconium carbide/polypyrrole composite particles, the zirconium carbide/polypyrrole composite particles comprise zirconium carbide and polypyrrole, and the polypyrrole is doped with lithium bis (trifluoromethylsulfonyl) imide; the preparation method comprises the steps of firstly synthesizing zirconium carbide/polypyrrole composite particles, dissolving polyurethane in dimethylformamide and stirring to obtain a polyurethane solution, dispersing the zirconium carbide/polypyrrole composite particles in the polyurethane solution, and carrying out a wet spinning process; the polypyrrole provided by the invention has strong absorption capacity to near infrared light, and the zirconium carbide can absorb the near infrared light and visible light efficiently; the polypyrrole has a photo-thermal conversion function and an electric-thermal conversion function, and the zirconium carbide/polypyrrole composite particles are filled in polyurethane fibers to prepare the fiber material which has a light absorption heating function and an electrifying heating function.
Description
Technical Field
The invention belongs to the technical field of composite fibers, and particularly relates to a zirconium carbide/polypyrrole-polyurethane composite fiber as well as a preparation method and application thereof.
Background
In winter, down jackets can only maintain the basic heat for people to live. Insulation based on air conditioning and heating is another strategy for people to cope with cold climate by maintaining constant body temperature and normal activities. But the use of air-conditioner and warm air brings about serious environmental hazards such as ozone layer holes, greenhouse effect, etc. Therefore, in order to reduce the use of air conditioners and heating, the textile with the more excellent heat preservation function has certain development prospect.
Polypyrrole is a semiconductor material which has both a photothermal conversion function and an electrothermal conversion function. Although polypyrrole absorbs heat, polypyrrole absorbs light energy mainly in the near infrared band. Zirconium carbide is a carbide having an excellent photothermal conversion function, and can absorb not only light energy in the visible light band but also light energy in the near-infrared band. At present, there is little research report on combining two materials to develop composite particles having both an electrothermal function and a photothermal conversion function.
The publication No. CN111014275A discloses a preparation method of iron oxide-polypyrrole granules, firstly nano Fe 2 O 3 Ultrasonically dispersing in distilled water, wherein the solid-liquid ratio is 2 g: 1L, then adding polyvinylpyrrolidone with the mass of 0.2-0.3 times of solid phase material, and mechanically stirring. Then, 0.05% by volume of pyrrole was added thereto, and the mixture was further stirred. Then, 4.0g/L ferric chloride solution with the volume of 20-30% of the system is added dropwise, and stirring is continued for 5 h. And finally, performing centrifugal treatment and washing with deionized water and ethanol respectively, wherein the product is prepared according to a feed-liquid ratio of 1: 5-20, adding ethanol, magnetically stirring in a water bath at a constant temperature of 50 ℃, adding 0.5-0.7 times of 3-mercaptopropyltrimethoxysilane by mass of a solid phase material, reacting for 1-3h while stirring, and drying in an oven at 80 ℃ to obtain the product. In addition, publication No. CN104004186A discloses a hollow copper sulfide/polypyrrole nanocomposite, which is obtained by adding sodium sulfide cuprous oxide to cuprous oxide serving as a template, gradually forming hollow copper sulfide through the kirkendall effect, then adding a pyrrole monomer and an oxidant, performing oxidative polymerization on the pyrrole monomer to form a polypyrrole shell, and then performing freeze drying. However, few studies on polypyrrole and zirconium carbide composite particles have been reported at present.
Disclosure of Invention
Aiming at the defects in the prior art, the primary object of the invention is to provide a zirconium carbide/polypyrrole-polyurethane composite fiber. Namely, polypyrrole with photothermal conversion and electrothermal conversion functions and a zirconium carbide material with photothermal conversion efficiency are combined to obtain composite particles with photothermal conversion and electrothermal conversion functions, the composite particles are added into a polyurethane material with excellent mechanical properties and spun into fibers, and finally the zirconium carbide/polypyrrole-polyurethane composite fibers with photothermal conversion and electrothermal conversion functions are obtained.
The second purpose of the invention is to provide a preparation method of the zirconium carbide/polypyrrole-polyurethane composite fiber.
The third purpose of the invention is to provide the application of the zirconium carbide/polypyrrole-polyurethane composite fiber.
In order to achieve the above primary object, the solution of the present invention is:
the zirconium carbide/polypyrrole-polyurethane composite fiber comprises a polyurethane matrix and zirconium carbide/polypyrrole composite particles, wherein the content of polyurethane is 90-99.9 wt%, and the content of the zirconium carbide/polypyrrole composite particles is 0.1-10 wt%.
The zirconium carbide/polypyrrole composite particles comprise zirconium carbide and polypyrrole, and the polypyrrole is doped with lithium bis (trifluoromethylsulfonyl) imide.
When visible light and near infrared light irradiate the composite fiber, the polypyrrole and zirconium carbide particles absorb light energy to increase the internal energy of the polypyrrole and zirconium carbide particles, and then the energy is released. Therefore, the composite fiber has a photothermal conversion function. In addition, the polypyrrole doped with the lithium bis (trifluoromethylsulfonyl) imide has excellent conductivity, so that the zirconium carbide/polypyrrole particles have good conductivity, when the zirconium carbide/polypyrrole particles are contained in the composite fiber, the composite fiber can enable the fiber to have obvious Joule heating effect under low voltage, and the heat generated under the low voltage can be used for heating human bodies.
In order to achieve the second objective, the solution of the invention is:
the preparation method of the zirconium carbide/polypyrrole-polyurethane composite fiber comprises the following steps:
(1) sequentially adding zirconium carbide, lithium bis (trifluoromethylsulfonyl) imide, pyrrole and an oxidant into deionized water and stirring to obtain a zirconium carbide/polypyrrole solution, and then filtering and drying the zirconium carbide/polypyrrole solution to obtain zirconium carbide/polypyrrole composite particles;
(2) dissolving polyurethane in dimethylformamide and stirring to obtain a polyurethane solution;
(3) dispersing the zirconium carbide/polypyrrole composite particles in a polyurethane solution to obtain a zirconium carbide/polypyrrole-polyurethane spinning solution;
(4) and carrying out wet spinning on the zirconium carbide/polypyrrole-polyurethane spinning solution to obtain the zirconium carbide/polypyrrole-polyurethane composite fiber.
Further, in the step (1), the oxidizing agent is one or more selected from the group consisting of ferric chloride and ceric ammonium nitrate. Under the action of an oxidant, one charge neutral pyrrole monomer molecule loses one electron and is oxidized into a cation free radical, then two cation free radicals are combined to generate dication of a PPy dimer, then the charge neutral PPy dimer is generated through disproportionation, then the PPy dimer is oxidized and combined with the cation free radical, and then the PPy dimer is disproportionated to generate a trimer, and the reaction is carried out until a chain-shaped Ppy with the polymerization degree of n is generated.
Further, in the step (1), the content of zirconium carbide in water is 0.1-10 wt%, the content of lithium bis (trifluoromethylsulfonyl) imide is 0.1-10 wt%, and polypyrrole doped with lithium bis (trifluoromethylsulfonyl) imide can enhance the electron transfer of polypyrrole, so that the conductivity of polypyrrole can be enhanced. The content of pyrrole is 0.1-20 wt%, the content of oxidant is 0.1-20 wt%, the molar ratio of oxidant and pyrrole is 1:1-3:1, and the temperature of zirconium carbide/polypyrrole solution is 0-10 ℃.
In the step (1), although polypyrrole is a material having both a photothermal conversion function and an electrothermal conversion function, polypyrrole mainly absorbs light energy in a near-infrared band to generate heat energy. Zirconium carbide can absorb not only light energy in the visible light band but also light energy in the near infrared band. The zirconium carbide/polypyrrole composite particles are prepared by polymerizing polypyrrole on the surface of zirconium carbide in situ, and the composite particles have good photothermal conversion function and good electrothermal conversion function.
Further, in the step (1), the stirring speed is 5-20rpm, the stirring time is 5-10min, and the temperature is 0-10 ℃. After polymerization, filtering the composite particles through filter paper, washing the composite particles for 1 to 8 times by using deionized water, and drying the composite particles at 40 to 60 ℃.
Further, in the step (2), the content of polyurethane in the polyurethane solution is 10-25 wt%.
Further, in step (2), dimethylformamide was selected as the solvent because: when the polyurethane is added into the dimethylformamide, the small molecules of the dimethylformamide solvent can permeate into the gaps of the polyurethane macromolecules, and finally the two are mixed to form a uniform phase in one state.
Further, in the step (2), the stirring speed is 50-150rpm, the stirring time is 0.5-5h, and the temperature is 30-50 ℃.
Further, in the step (3), the content of the zirconium carbide/polypyrrole composite particles in the zirconium carbide/polypyrrole-polyurethane mixed spinning solution is 0.01 to 1.5 wt%. Adding zirconium carbide/polypyrrole granules, and uniformly dispersing the zirconium carbide/polypyrrole granules into the mixed solution by stirring to obtain the zirconium carbide/polypyrrole-polyurethane mixed spinning solution.
Further, in the step (3), stirring and ultrasonic wave are adopted for processing in a dispersing mode, the stirring speed is 10-50rpm, the stirring time is 10-30min, and the stirring temperature is 10-30 ℃; the ultrasonic treatment time is 10-30min, and the ultrasonic frequency is 12-30 KHz.
Further, in the step (4), in the wet spinning process, the propelling speed of the zirconium carbide/polypyrrole-polyurethane spinning solution is 5-20 mL/h; the coagulating bath is water at 10-30 deg.C; the drawing speed is 0.1-1 cm/s.
In order to achieve the third object, the solution of the invention is:
an application of zirconium carbide/polypyrrole-polyurethane composite fibers in autumn and winter heat-preservation clothing fabrics.
Due to the adoption of the scheme, the invention has the beneficial effects that:
firstly, the method obtains zirconium carbide/polypyrrole composite particles by polymerizing polypyrrole on the surface of zirconium carbide, the particles have both a photothermal conversion function and an electrothermal conversion function, the particles are filled in polyurethane to prepare zirconium carbide/polypyrrole-polyurethane composite fibers by adopting a wet spinning technology, and the fibers can be woven into knitted fabrics, woven fabrics and non-woven fabrics to obtain fabrics with photothermal and electrothermal conversion functions, so that the zirconium carbide/polypyrrole composite particles can provide a new choice for manufacturing warm-keeping clothes.
Secondly, the preparation method of the invention has simple steps, unique process and easy popularization.
Drawings
FIG. 1 is a process flow diagram of the zirconium carbide/polypyrrole-polyurethane composite fiber of the present invention.
Fig. 2 is an SEM image of zirconium carbide particles of an example of the present invention.
Fig. 3 is an SEM image of zirconium carbide/polypyrrole particles of an example of the invention.
FIG. 4 is a graph showing the mechanical properties of a zirconium carbide/polypyrrole-polyurethane composite fiber according to an example of the present invention.
Fig. 5 is a graph showing a photothermal conversion curve of a zirconium carbide/polypyrrole-polyurethane composite fiber according to an embodiment of the present invention.
FIG. 6 is a graph showing the electrothermal transition curves of the zirconium carbide/polypyrrole-polyurethane composite fibers according to the example of the present invention.
Detailed Description
The invention provides a zirconium carbide/polypyrrole-polyurethane composite fiber and a preparation method and application thereof.
< zirconium carbide/polypyrrole-polyurethane composite fiber >
The zirconium carbide/polypyrrole-polyurethane composite fiber comprises a polyurethane matrix and zirconium carbide/polypyrrole composite particles, wherein the content of polyurethane is 90-99.9 wt%, and the content of the zirconium carbide/polypyrrole composite particles is 0.1-10 wt%. The zirconium carbide/polypyrrole composite particles comprise zirconium carbide and polypyrrole, and the polypyrrole is doped with lithium bis (trifluoromethylsulfonyl) imide.
< preparation method of zirconium carbide/polypyrrole-polyurethane composite fiber >
As shown in fig. 1, the preparation method of the zirconium carbide/polypyrrole-polyurethane composite fiber of the present invention comprises the following steps:
(1) sequentially adding zirconium carbide particles, lithium bis (trifluoromethylsulfonyl) imide, pyrrole and an oxidant into deionized water and stirring to obtain a zirconium carbide/polypyrrole solution, and then filtering and drying the zirconium carbide/polypyrrole solution to obtain zirconium carbide/polypyrrole composite particles;
(2) dissolving polyurethane in dimethylformamide and stirring to obtain a polyurethane solution;
(3) dispersing the zirconium carbide/polypyrrole composite particles in a polyurethane solution to obtain a zirconium carbide/polypyrrole-polyurethane spinning solution;
(4) and carrying out wet spinning on the zirconium carbide/polypyrrole-polyurethane spinning solution to obtain the zirconium carbide/polypyrrole-polyurethane composite fiber.
Wherein, in the step (1), the oxidant is selected from more than one of ferric chloride and ceric ammonium nitrate.
In the step (1), the content of zirconium carbide in water is 0.1-10 wt%, the content of lithium bis (trifluoromethylsulfonyl) imide is 0.1-10 wt%, the content of pyrrole is 0.1-20 wt%, the content of oxidant is 0.1-20 wt%, the molar ratio of oxidant to pyrrole is 1:1-3:1, and the temperature of zirconium carbide/polypyrrole solution is 0-10 ℃.
In the step (1), the stirring speed is 5-20rpm, the stirring time is 5-10min, and the temperature is 0-10 ℃.
In the step (2), the content of polyurethane in the polyurethane solution is 10 to 25 wt%.
In the step (2), the stirring speed is 50-150rpm, the stirring time is 0.5-5h, and the temperature is 30-50 ℃.
In the step (3), the content of the zirconium carbide/polypyrrole composite particles in the zirconium carbide/polypyrrole-polyurethane mixed spinning solution is 0.01 to 1.5 wt%.
In the step (3), the dispersion mode adopts stirring and ultrasonic wave to process, the stirring speed is 10-50rpm, the stirring time is 10-30min, and the stirring temperature is 10-30 ℃; the ultrasonic treatment time is 10-30min, and the ultrasonic frequency is 12-30 KHz.
In the step (4), in the wet spinning process, the advancing speed of the zirconium carbide/polypyrrole-polyurethane spinning solution is 5-20 mL/h; the coagulating bath is water at 10-30 deg.C; the drawing speed is 0.1-1 cm/s.
The surface appearance of the cross section of the fiber is observed by an electronic scanning electron microscope.
A plurality of fibers are arranged in a plane and irradiated with an infrared lamp, and then the surface temperature of the fibers is measured with a thermocouple thermometer, and the surface temperature of the fibers increases as the irradiation time of the infrared light increases. When the infrared lamp was removed, the temperature of the fiber surface dropped rapidly.
A voltage of 10V is applied to two ends of a fiber (with the length of 2cm), then the temperature of the surface of the fiber is measured by a thermocouple thermometer, and the temperature of the surface of the fiber is increased and then becomes flat along with the time.
And obtaining a mechanical curve graph of the zirconium carbide/polypyrrole-polyurethane composite fiber through a mechanical property tester, wherein the fiber is stretched and then suddenly broken.
< use of zirconium carbide/polypyrrole-polyurethane composite fiber >
The zirconium carbide/polypyrrole-polyurethane composite fiber can be applied to autumn and winter thermal insulation clothing fabrics. Meanwhile, more choices are provided for selecting materials of autumn and winter warm-keeping clothes, the thermal comfort of people wearing the clothes is improved, the use of air conditioners is reduced, certain fossil energy is saved, and the pressure of the environment is reduced.
The present invention will be further described with reference to the following examples.
Example (b):
the preparation method of the zirconium carbide/polypyrrole-polyurethane composite fiber of the embodiment includes the following steps:
(1) sequentially adding zirconium carbide, lithium bis (trifluoromethylsulfonyl) imide, pyrrole and ferric chloride (serving as oxidants) into deionized water and stirring at the rotation speed of 5rpm for 10min at the temperature of 0 ℃ to obtain a zirconium carbide/polypyrrole solution, and then filtering and drying the zirconium carbide/polypyrrole solution to obtain zirconium carbide/polypyrrole composite particles; wherein the content of zirconium carbide in water is 5 wt%, the content of lithium bis (trifluoromethylsulfonyl) imide is 3 wt%, the content of pyrrole is 3 wt%, the molar ratio of oxidant to pyrrole is 2.5:1, and the temperature of zirconium carbide/polypyrrole solution is 0 ℃.
(2) Dissolving polyurethane in dimethylformamide and stirring at the rotation speed of 150rpm for 5 hours at the temperature of 30 ℃ to obtain a polyurethane solution; the polyurethane content of the polyurethane solution was 15 wt%.
(3) Dispersing the zirconium carbide/polypyrrole composite particles in a polyurethane solution to obtain a zirconium carbide/polypyrrole-polyurethane spinning solution; wherein, the content of the zirconium carbide/polypyrrole composite particles in the zirconium carbide/polypyrrole-polyurethane mixed spinning solution is 1.5 wt%; the dispersion mode adopts stirring and ultrasonic wave for treatment, the stirring speed is 10rpm, the stirring time is 10min, and the stirring temperature is 30 ℃; the ultrasonic treatment time is 15min, and the ultrasonic frequency is 30 KHz.
(4) And carrying out wet spinning on the zirconium carbide/polypyrrole-polyurethane spinning solution to obtain the zirconium carbide/polypyrrole-polyurethane composite fiber. In the wet spinning process, the advancing speed of the zirconium carbide/polypyrrole-polyurethane spinning solution is 5 mL/h; the coagulating bath is water, and the temperature is 25 ℃; the drawing speed was 1 cm/s.
The surface morphology of the zirconium carbide particles used in this example is shown in FIG. 2, the surface morphology of the zirconium carbide/polypyrrole composite particles is shown in FIG. 3. The grain diameter of zirconium carbide particles is between 50 and 1000nm, and the agglomeration condition among the particles is not obvious; the particle size of the zirconium carbide/polypyrrole composite particles is between 500-8000nm, and certain agglomeration phenomenon exists among the particles. The mechanical property curve of the zirconium carbide/polypyrrole-polyurethane composite fiber is shown in fig. 4, the breaking strength of the fiber reaches 25.9Mpa, and the breaking elongation reaches 509 percent. The photothermal conversion curve of the zirconium carbide/polypyrrole-polyurethane composite fiber is shown in fig. 5, after the infrared lamp is used for irradiating for 150s, the surface temperature of the composite fiber is increased to about 65 ℃, and when the light source is turned off, the fiber temperature is rapidly reduced. The electrothermal conversion curve of the zirconium carbide/polypyrrole-polyurethane composite fiber is shown in fig. 6, the fiber is rapidly heated to about 60 ℃ under the drive of 10V voltage, and then the temperature is basically kept unchanged.
The embodiments described above are presented to facilitate one of ordinary skill in the art to make and use the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments and the generic principles defined herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments. Those skilled in the art should appreciate that many modifications and variations are possible in light of the above teaching without departing from the scope of the invention.
Claims (10)
1. A zirconium carbide/polypyrrole-polyurethane composite fiber is characterized in that: the polyurethane/polypyrrole composite particle comprises 90-99.9 wt% of polyurethane and 0.1-10 wt% of zirconium carbide/polypyrrole composite particles;
the zirconium carbide/polypyrrole composite particles comprise zirconium carbide and polypyrrole, and the polypyrrole is doped with lithium bis (trifluoromethylsulfonyl) imide;
the preparation method of the zirconium carbide/polypyrrole-polyurethane composite fiber comprises the following steps:
(1) sequentially adding zirconium carbide, lithium bis (trifluoromethylsulfonyl) imide, pyrrole and an oxidant into deionized water and stirring to obtain a zirconium carbide/polypyrrole solution, and then filtering and drying the zirconium carbide/polypyrrole solution to obtain zirconium carbide/polypyrrole composite particles;
(2) dissolving polyurethane in dimethylformamide and stirring to obtain a polyurethane solution;
(3) dispersing the zirconium carbide/polypyrrole composite particles in a polyurethane solution to obtain a zirconium carbide/polypyrrole-polyurethane spinning solution;
(4) and carrying out a wet spinning process on the zirconium carbide/polypyrrole-polyurethane spinning solution to obtain the zirconium carbide/polypyrrole-polyurethane composite fiber.
2. A method for preparing the zirconium carbide/polypyrrole-polyurethane composite fiber according to claim 1, wherein: which comprises the following steps:
(1) sequentially adding zirconium carbide, lithium bis (trifluoromethylsulfonyl) imide, pyrrole and an oxidant into deionized water and stirring to obtain a zirconium carbide/polypyrrole solution, and then filtering and drying the zirconium carbide/polypyrrole solution to obtain zirconium carbide/polypyrrole composite particles;
(2) dissolving polyurethane in dimethylformamide and stirring to obtain a polyurethane solution;
(3) dispersing the zirconium carbide/polypyrrole composite particles in a polyurethane solution to obtain a zirconium carbide/polypyrrole-polyurethane spinning solution;
(4) and carrying out a wet spinning process on the zirconium carbide/polypyrrole-polyurethane spinning solution to obtain the zirconium carbide/polypyrrole-polyurethane composite fiber.
3. The method of claim 2, wherein: in the step (1), the oxidant is selected from more than one of ferric chloride and ammonium ceric nitrate.
4. The method of claim 2, wherein: in the step (1), the content of zirconium carbide in water is 0.1-10 wt%, the content of lithium bis (trifluoromethylsulfonyl) imide is 0.1-10 wt%, the content of pyrrole is 0.1-20 wt%, the content of oxidant is 0.1-20 wt%, the molar ratio of oxidant to pyrrole is 1:1-3:1, and the temperature of the zirconium carbide/polypyrrole solution is 0-10 ℃.
5. The method of claim 2, wherein: in the step (1), the rotation speed of the stirring is 5-20rpm, the stirring time is 5-10min, and the temperature is 0-10 ℃.
6. The method of claim 2, wherein: in the step (2), the content of polyurethane in the polyurethane solution is 10-25 wt%.
7. The method of claim 2, wherein: in the step (2), the rotating speed of the stirring is 50-150rpm, the stirring time is 0.5-5h, and the temperature is 30-50 ℃.
8. The production method according to claim 2, characterized in that: in the step (3), the content of zirconium carbide/polypyrrole composite particles in the zirconium carbide/polypyrrole-polyurethane mixed spinning solution is 0.01-1.5 wt%; and/or the presence of a gas in the gas,
in the step (3), the dispersing mode adopts stirring and ultrasonic wave to process, the stirring speed is 10-50rpm, the stirring time is 10-30min, and the stirring temperature is 10-30 ℃; the ultrasonic time is 10-30min, and the ultrasonic frequency is 12-30 KHz.
9. The method of claim 2, wherein: in the step (4), in the wet spinning process, the propelling speed of the zirconium carbide/polypyrrole-polyurethane spinning solution is 5-20 mL/h; the coagulating bath is water at 10-30 deg.C; the drawing speed is 0.1-1 cm/s.
10. Use of the zirconium carbide/polypyrrole-polyurethane composite fiber according to claim 1 in autumn and winter thermal insulation clothing fabric.
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2021
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| JPH04245910A (en) * | 1991-01-31 | 1992-09-02 | Jujo Paper Co Ltd | Photothermal converting fiber and photothermal fusible fiber |
| CN101613888A (en) * | 2009-07-31 | 2009-12-30 | 东华大学 | Polyacrylonitrile-based solar energy storage heat generating fiber and manufacture method thereof |
| WO2013182568A2 (en) * | 2012-06-06 | 2013-12-12 | Cht R. Beitlich Gmbh | Textile auxiliary agent and textile product finished therewith |
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