CN115710825A - Electrically-driven thermochromic fiber and preparation method thereof - Google Patents
Electrically-driven thermochromic fiber and preparation method thereof Download PDFInfo
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- CN115710825A CN115710825A CN202211610971.9A CN202211610971A CN115710825A CN 115710825 A CN115710825 A CN 115710825A CN 202211610971 A CN202211610971 A CN 202211610971A CN 115710825 A CN115710825 A CN 115710825A
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- 239000000835 fiber Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 56
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 31
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 31
- 239000002131 composite material Substances 0.000 claims abstract description 30
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920006306 polyurethane fiber Polymers 0.000 claims abstract description 13
- 239000006185 dispersion Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 24
- 229920002635 polyurethane Polymers 0.000 claims description 16
- 239000004814 polyurethane Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 239000002109 single walled nanotube Substances 0.000 claims description 13
- 238000002791 soaking Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- 230000009467 reduction Effects 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
- 239000012498 ultrapure water Substances 0.000 claims description 6
- 230000008859 change Effects 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 8
- 239000004753 textile Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005485 electric heating Methods 0.000 abstract description 3
- 239000004020 conductor Substances 0.000 abstract description 2
- 230000009471 action Effects 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010981 drying operation Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 230000000638 stimulation Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses an electrically-driven thermochromic fiber and a preparation method thereof, and relates to the technical field of functional fibers. The preparation method comprises the steps of preparing a graphene oxide/carbon nano tube composite solution, preparing conductive fibers and preparing electrically-driven thermochromic fibers. According to the invention, polyurethane fibers are soaked in graphene oxide/carbon nano tube composite solution for weight increment, then heated and reduced, and finally, thermochromic ink and isophorone are coated to prepare the electrically-driven thermochromic fibers. The invention combines the active control of electrochromism and the thermochromism structure by utilizing the electric heating performance of the conductive material and the color changing performance of the thermochromism material, and the prepared electrically-driven thermochromism fiber has the advantages of both. The electrically-driven thermochromic fiber is simple in structure and convenient to prepare, and can actively control color change, so that intelligent textiles are simpler, more intelligent and more multifunctional.
Description
Technical Field
The invention relates to the technical field of functional fibers, in particular to an electrically-driven thermochromic fiber and a preparation method thereof.
Background
The intelligent color-changing textile is a textile which can show different colors along with the change of external environmental conditions (light, electricity, heat and the like), and is an intelligent product with high added value and high benefit. The color-changing textiles are divided according to the stimulation mode of the materials, and the color-changing textiles mainly have 3 types: photochromic, thermochromic, electrochromic. Photochromic refers to the fact that under the action of light with certain wavelength and intensity, the molecular structure of some compounds is changed, so that the absorption peak value of the compounds to the light, namely the corresponding reversible change of the color, is caused. The electrochromism is a phenomenon that the optical property of the material generates stable and reversible color change under the action of an external electric field, and the electrochromism represents reversible change of color and transparency in appearance, and the electrochromism is essentially that the chemical structure of the material is changed under the action of the electric field, so that the absorption spectrum of the material is changed. Thermochromic means that the color of the material changes obviously along with the change of temperature in a certain temperature range. Photochromic textiles require additional light source devices or irradiation excitation in a certain direction with specific wavelengths, and the range of application is relatively limited. The color of the electrochromic textile can be changed by controlling the current or voltage, but the requirements of flexibility and wearability of the device are difficult to meet due to the defects of complex structure, poor stretchability, high cost and the like. The principle of the thermochromic material and the structure of the device are relatively simple, but the function of actively controlling color change cannot be achieved by an external heating source.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an electrically-driven thermochromic fiber which is simple in structure, convenient to prepare and capable of being actively controlled and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme: a preparation method of electrically-driven thermochromic fibers comprises the following steps:
s1, preparing a graphene oxide/carbon nanotube composite solution: dropwise adding a carboxylated single-walled carbon nanotube dispersion liquid into the graphene oxide dispersion liquid while stirring to prepare a graphene oxide/carbon nanotube composite solution; wherein the mass ratio of the graphene oxide to the carboxylated single-walled carbon nanotube is 0.8-3;
s2, preparing conductive fibers: dripping aqueous polyurethane into the graphene oxide/carbon nano tube composite solution, wherein the mass ratio of the aqueous polyurethane to the graphene oxide/carbon nano tube composite is 1-8-12, soaking polyurethane fibers in the graphene oxide/carbon nano tube composite solution in which the aqueous polyurethane is dripped, taking out and drying the polyurethane fibers after soaking, repeating the operations of soaking and drying until the weight of the fibers is increased by 15-30%, and finally placing the fibers in an oven at 180-220 ℃ for thermal reduction;
s3, preparing the electrically-driven thermochromic fiber: and (3) dripping isophorone into the thermochromic ink, wherein the mass ratio of the thermochromic ink to the isophorone is 12-18.
Further, the preparation method of the graphene oxide dispersion liquid in the step S1 comprises: adding graphene oxide powder into ultrapure water, performing ultrasonic treatment for 8-15 min, and then dropwise adding ammonia water to adjust the pH value to 7-8, so as to obtain a graphene oxide dispersion liquid.
Further, the mass ratio of the graphene oxide to the carboxylated single-walled carbon nanotubes in the step S1 is 1.
Further, the drying temperature in the step S2 is 40-80 ℃, and the drying time is 1-5 min.
Further, the time of the thermal reduction in the step S2 is 12 to 18 min.
Electrically driven thermochromic fibers prepared by the above method.
The invention has the following advantages: according to the invention, polyurethane fibers are soaked in graphene oxide/carbon nano tube composite solution for weight increment, then heated and reduced, and finally coated with thermochromic ink and isophorone, so that the electrically-driven thermochromic fibers are prepared. The invention combines the active control of electrochromism and the thermochromism structure by utilizing the electric heating performance of the conductive material and the color changing performance of the thermochromism material, and the prepared electrically-driven thermochromism fiber has the advantages of both. The electrically-driven thermochromic fiber is simple in structure and convenient to prepare, and can actively control color change, so that intelligent textiles are simpler, more intelligent and more multifunctional.
Drawings
FIG. 1 is a graph of temperature versus time for conductive fibers at different voltages.
Fig. 2 is an infrared thermal imaging diagram of the conductive fiber under the stimulation of 4V (upper) and 5V (lower) voltages.
FIG. 3 is a graph comparing fibers before and after color change.
FIG. 4 is a cross-sectional electron micrograph of conductive fibers (left) and fiber stock (right).
FIG. 5 is a cross-sectional view (left) and a partial magnified electron micrograph (right) of a color-changing fiber.
Detailed Description
The invention is further described with reference to the following figures and examples, without limiting the scope of the invention to the following:
example 1: a preparation method of electrically-driven thermochromic fibers comprises the following steps:
s1, preparing a graphene oxide/carbon nanotube composite solution: dropwise adding a carboxylated single-walled carbon nanotube dispersion liquid into the graphene oxide dispersion liquid while stirring to prepare a graphene oxide/carbon nanotube composite solution; wherein the mass ratio of the graphene oxide to the carboxylated single-walled carbon nanotube is 0.8; the preparation method of the graphene oxide dispersion liquid comprises the following steps: adding graphene oxide powder into ultrapure water, performing ultrasonic treatment for 8 min, and then dropwise adding ammonia water to adjust the pH value to 7 to obtain a graphene oxide dispersion liquid;
s2, preparing conductive fibers: dripping aqueous polyurethane into the graphene oxide/carbon nano tube composite solution, wherein the mass ratio of the aqueous polyurethane to the graphene oxide/carbon nano tube composite is 1;
s3, preparing the electrically-driven thermochromic fiber: and (3) dropwise adding isophorone into the thermochromic ink, wherein the mass ratio of the thermochromic ink to the isophorone is 12.
Example 2: a method for preparing electrically driven thermochromic fibers, comprising the steps of:
s1, preparing a graphene oxide/carbon nano tube composite solution: dropwise adding a carboxylated single-walled carbon nanotube dispersion liquid into the graphene oxide dispersion liquid while stirring to prepare a graphene oxide/carbon nanotube composite solution; wherein the mass ratio of the graphene oxide to the carboxylated single-walled carbon nanotube is 3; the preparation method of the graphene oxide dispersion liquid comprises the following steps: adding graphene oxide powder into ultrapure water, performing ultrasonic treatment for 15 min, and then dropwise adding ammonia water to adjust the pH value to 8, so as to obtain a graphene oxide dispersion liquid;
s2, preparing conductive fibers: dripping aqueous polyurethane into the graphene oxide/carbon nano tube composite solution, wherein the mass ratio of the aqueous polyurethane to the graphene oxide/carbon nano tube composite is 1:12, soaking polyurethane fibers into the graphene oxide/carbon nano tube composite solution in which the aqueous polyurethane is dripped, taking out the polyurethane fibers after soaking, drying the polyurethane fibers at the temperature of 80 ℃ for 1 min, repeating the soaking and drying operations until the weight of the fibers is increased by 30%, and finally placing the fibers in a drying oven at the temperature of 220 ℃ for thermal reduction for 18 min;
s3, preparing the electrically-driven thermochromic fiber: and (3) dropwise adding isophorone into the thermochromic ink, wherein the mass ratio of the thermochromic ink to the isophorone is 18.
Example 3: a method for preparing electrically driven thermochromic fibers, comprising the steps of:
s1, preparing a graphene oxide/carbon nanotube composite solution: dropwise adding a carboxylated single-walled carbon nanotube dispersion liquid into the graphene oxide dispersion liquid while stirring to prepare a graphene oxide/carbon nanotube composite solution; wherein the mass ratio of the graphene oxide to the carboxylated single-walled carbon nanotube is 1; the preparation method of the graphene oxide dispersion liquid comprises the following steps: adding graphene oxide powder into ultrapure water, performing ultrasonic treatment for 12 min, and then dropwise adding ammonia water to adjust the pH value to 7.5 to obtain a graphene oxide dispersion liquid;
s2, preparing conductive fibers: dripping aqueous polyurethane into the graphene oxide/carbon nanotube composite solution, wherein the mass ratio of the aqueous polyurethane to the graphene oxide/carbon nanotube composite is 1;
s3, preparing the electrically-driven thermochromic fiber: and (3) dropwise adding isophorone into the thermochromic ink, wherein the mass ratio of the thermochromic ink to the isophorone is 16.
The following experiments illustrate the beneficial effects of the present invention:
1. preparation of electrically-driven thermochromic fibers
S1, preparing a graphene oxide/carbon nanotube composite solution: dropwise adding 5 mL of 10 mg/mL carboxylated single-walled carbon nanotube dispersion liquid into the graphene oxide dispersion liquid while stirring to prepare a graphene oxide/carbon nanotube composite solution; the preparation method of the graphene oxide dispersion liquid comprises the following steps: adding 50 mg of graphene oxide powder into 10 mL of ultrapure water, performing ultrasonic treatment for 10 min, and then dropwise adding ammonia water to adjust the pH value to 7.5 to obtain a graphene oxide dispersion liquid;
s2, preparing conductive fibers: dropwise adding 10 mg of waterborne polyurethane into the graphene oxide/carbon nano tube composite solution, soaking polyurethane fibers into the graphene oxide/carbon nano tube composite solution dropwise added with the waterborne polyurethane, taking out and drying the polyurethane fibers after soaking, wherein the drying temperature is 60 ℃, the drying time is 3 min, repeating the soaking and drying operations until the weight of the fibers is increased by 23%, and finally placing the fibers in a drying oven at 200 ℃ for thermal reduction, wherein the thermal reduction time is 15 min;
s3, preparing the electrically-driven thermochromic fiber: 15 And (3) dropwise adding 1 g of isophorone into g of thermochromic ink, uniformly mixing, smearing the mixture on the conductive fiber prepared in the step (S2), and drying to obtain the electrically-driven thermochromic fiber.
2. Electrothermal performance of conductive fiber
And applying 3-5V constant voltage to two ends of the 1cm conductive fiber, shooting by using an infrared thermal imager, and removing the applied voltage after the temperature is stable to measure the electric heating performance of the conductive fiber. The results are shown in fig. 1 and 2, and show that the conductive fiber can be heated up to 60 ℃ under the voltage of 4V, and the temperature required for the color change of the color change ink is reached. The temperature rise time of the conductive fiber is about 15 s, and the temperature drop time is about 10 s, which shows that the conductive fiber has good heat conductivity and can realize quick response of heat to voltage.
3. Color-changing performance of color-changing fiber
The result of the color-changing performance test of the color-changing fiber is shown in fig. 3, and it can be seen from the pictures before (left) and after (right) color change that the color-changing ink is brownish black at normal temperature and becomes orange due to the electric heat when a voltage is applied.
4. Sectional electron microscope image of conductive fiber
The cross section of the conductive fiber is subjected to electron microscope scanning, and the result is shown in fig. 4, and it can be seen from the comparison of the electron microscope images of the cross sections of the conductive fiber (left) and the fiber sample (right) that the conductive layer composed of reduced graphene oxide/carbon nanotube/waterborne polyurethane is attached outside the polyurethane fiber filament.
5. Section electron microscope image of color-changing fiber
The cross section of the color-changing fiber is subjected to electron microscope scanning, and as a result, as shown in fig. 5, the color-changing layer and the conductive layer are sequentially wrapped outside the polyurethane fiber, so that the structure is compact, and the color-changing layer wrapping the conductive layer also plays a role in protecting the conductive network structure.
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 can substitute or change the technical solution of the present invention and the inventive concept within the technical scope of the present invention.
Claims (6)
1. A method for preparing electrically driven thermochromic fibers is characterized by comprising the following steps of:
s1, preparing a graphene oxide/carbon nanotube composite solution: dropwise adding a carboxylated single-walled carbon nanotube dispersion liquid into the graphene oxide dispersion liquid while stirring to prepare a graphene oxide/carbon nanotube composite solution; wherein the mass ratio of the graphene oxide to the carboxylated single-walled carbon nanotube is 0.8-3;
s2, preparing conductive fibers: dripping aqueous polyurethane into the graphene oxide/carbon nano tube composite solution, wherein the mass ratio of the aqueous polyurethane to the graphene oxide/carbon nano tube composite is 1-8-12, soaking polyurethane fibers in the graphene oxide/carbon nano tube composite solution in which the aqueous polyurethane is dripped, taking out and drying the polyurethane fibers after soaking, repeating the operations of soaking and drying until the weight of the fibers is increased by 15-30%, and finally placing the fibers in an oven at 180-220 ℃ for thermal reduction;
s3, preparing the electrically-driven thermochromic fiber: and (3) dripping isophorone into the thermochromic ink, wherein the mass ratio of the thermochromic ink to the isophorone is 12-18.
2. The method for preparing an electrically driven thermochromic fiber according to claim 1, wherein the graphene oxide dispersion liquid in step S1 is prepared by: adding graphene oxide powder into ultrapure water, performing ultrasonic treatment for 8-15 min, and then dropwise adding ammonia water to adjust the pH value to 7-8, so as to obtain a graphene oxide dispersion liquid.
3. The method for preparing electrically-driven thermochromic fibers according to claim 1, wherein the mass ratio of graphene oxide to carboxylated single-walled carbon nanotubes in step S1 is 1.
4. The method of claim 1, wherein the drying temperature in step S2 is 40-80 ℃ and the drying time is 1-5 min.
5. The method for preparing an electrically driven thermochromic fiber as claimed in claim 1, wherein the thermal reduction time in step S2 is 12 to 18 min.
6. Electrically driven thermochromic fibers prepared according to the method of any of claims 1-5.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0473211A (en) * | 1990-07-13 | 1992-03-09 | Kuraray Co Ltd | Thermochromic polyvinyl alcohol fiber and production thereof |
| JP2007332478A (en) * | 2006-06-13 | 2007-12-27 | Lintec Corp | Thermochromic fiber-blended paper |
| WO2016107239A1 (en) * | 2014-12-29 | 2016-07-07 | 宁波南车新能源科技有限公司 | Hybrid supercapacitor |
| CN109610057A (en) * | 2018-10-31 | 2019-04-12 | 武汉纺织大学 | A kind of electrochromism yarn and preparation method thereof |
| CN110205705A (en) * | 2019-05-24 | 2019-09-06 | 华中科技大学 | A kind of thermochromism fiber, its preparation and application |
| CN110219082A (en) * | 2019-05-29 | 2019-09-10 | 武汉纺织大学 | A kind of electrochromism nanofiber covering yarn and preparation method thereof |
| US20200181811A1 (en) * | 2018-12-06 | 2020-06-11 | Lintec Of America, Inc. | Continuous production of thermochromic yarns |
| CN112522809A (en) * | 2020-12-08 | 2021-03-19 | 武汉纺织大学 | Elastic electrically-driven thermochromic sensing fiber with sheath-core structure and preparation method thereof |
| CN115125728A (en) * | 2022-07-07 | 2022-09-30 | 武汉纺织大学 | Preparation method of polyurethane film loaded with redox graphene and carbon nano tubes |
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- 2022-12-15 CN CN202211610971.9A patent/CN115710825B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0473211A (en) * | 1990-07-13 | 1992-03-09 | Kuraray Co Ltd | Thermochromic polyvinyl alcohol fiber and production thereof |
| JP2007332478A (en) * | 2006-06-13 | 2007-12-27 | Lintec Corp | Thermochromic fiber-blended paper |
| WO2016107239A1 (en) * | 2014-12-29 | 2016-07-07 | 宁波南车新能源科技有限公司 | Hybrid supercapacitor |
| CN109610057A (en) * | 2018-10-31 | 2019-04-12 | 武汉纺织大学 | A kind of electrochromism yarn and preparation method thereof |
| US20200181811A1 (en) * | 2018-12-06 | 2020-06-11 | Lintec Of America, Inc. | Continuous production of thermochromic yarns |
| CN110205705A (en) * | 2019-05-24 | 2019-09-06 | 华中科技大学 | A kind of thermochromism fiber, its preparation and application |
| CN110219082A (en) * | 2019-05-29 | 2019-09-10 | 武汉纺织大学 | A kind of electrochromism nanofiber covering yarn and preparation method thereof |
| CN112522809A (en) * | 2020-12-08 | 2021-03-19 | 武汉纺织大学 | Elastic electrically-driven thermochromic sensing fiber with sheath-core structure and preparation method thereof |
| CN115125728A (en) * | 2022-07-07 | 2022-09-30 | 武汉纺织大学 | Preparation method of polyurethane film loaded with redox graphene and carbon nano tubes |
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