CN115710825B - Electrically driven thermochromic fiber and preparation method thereof - Google Patents
Electrically driven thermochromic fiber and preparation method thereof Download PDFInfo
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- CN115710825B CN115710825B CN202211610971.9A CN202211610971A CN115710825B CN 115710825 B CN115710825 B CN 115710825B CN 202211610971 A CN202211610971 A CN 202211610971A CN 115710825 B CN115710825 B CN 115710825B
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- 239000000835 fiber Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 92
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 58
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 33
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 33
- 239000002131 composite material Substances 0.000 claims abstract description 32
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000009467 reduction Effects 0.000 claims abstract description 14
- 229920006306 polyurethane fiber Polymers 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims description 26
- 239000006185 dispersion Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 229920002635 polyurethane Polymers 0.000 claims description 18
- 239000004814 polyurethane Substances 0.000 claims description 18
- 238000002791 soaking Methods 0.000 claims description 18
- 239000002109 single walled nanotube Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 11
- 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
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 238000010981 drying operation Methods 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 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 11
- 239000000463 material Substances 0.000 abstract description 10
- 239000004753 textile Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000004020 conductor Substances 0.000 abstract description 2
- 238000001000 micrograph Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000002441 reversible effect 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
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001931 thermography Methods 0.000 description 1
Classifications
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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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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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 graphene oxide/carbon nano tube composite solution, preparing conductive fibers and preparing electrically-driven thermochromic fibers. According to the invention, polyurethane fiber is soaked in graphene oxide/carbon nano tube composite solution for weight increment, and then is subjected to reheat reduction, and finally thermochromic ink and isophorone are smeared to prepare the electro-driven thermochromic fiber. The invention combines the active control of electrochromic and thermochromic structure by utilizing the electrothermal property of the conductive material and the color-changing property of the thermochromic material, and the prepared electro-driven thermochromic fiber has the advantages of both. The electro-driven thermochromic fiber is simple in structure and convenient to prepare, and can actively control the color change, so that the intelligent textile is simpler, more intelligent and 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 textile capable of showing different colors along with the change of external environment 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 into 3 types according to the stimulation mode of the materials: photochromic, thermochromic, electrochromic. Photochromic refers to a compound whose molecular structure changes under the action of light of a certain wavelength and intensity, resulting in its corresponding reversible change in the absorption peak of light, i.e. color. Electrochromic refers to the phenomenon that the optical properties of a material change stably and reversibly under the action of an external electric field, and the appearance of the material shows reversible changes of color and transparency, and the essence of the electrochromic is that the chemical structure of the material changes under the action of the electric field, so that the absorption spectrum of the material changes. Thermochromic refers to a material whose color changes significantly with temperature over a range of temperatures. Photochromic textiles require an additional light source device or are excited by irradiation with a specific wavelength in a certain direction, and the application range is relatively limited. Electrochromic textiles can adjust the color change of materials by controlling the magnitude of current or voltage, but the requirements of flexibility and wearability of devices are difficult to meet due to the defects of complex structure, poor stretchability, high cost and the like. Thermochromic materials are relatively simple in principle and device structure, but the active control of the color change cannot be achieved by an external heat 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 aim of the invention is achieved by the following technical scheme: a method for preparing an electrically driven thermochromic fiber, comprising the steps of:
s1, preparing graphene oxide/carbon nano tube composite solution: dropwise adding carboxylated single-walled carbon nanotube dispersion liquid into graphene oxide dispersion liquid, and stirring while dropwise adding to prepare graphene oxide/carbon nanotube composite solution; wherein the mass ratio of graphene oxide to carboxylated single-walled carbon nanotubes is 0.8-3:1;
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 dripped with the aqueous polyurethane, taking out and drying after soaking, repeating the soaking and drying operations until the weight of the fibers is increased by 15-30%, and finally placing the fibers in a drying oven at 180-220 ℃ for thermal reduction;
S3, preparing the electrically-driven thermochromic fiber: dripping isophorone into the thermochromic ink, uniformly mixing the thermochromic ink and the isophorone according to the mass ratio of 12-18:1, coating the mixture on the conductive fiber prepared in the step S2, and drying to obtain the electrically-driven thermochromic fiber.
Further, the preparation method of the graphene oxide dispersion liquid in the step S1 comprises the following steps: 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 graphene oxide dispersion liquid.
Further, in the step S1, the mass ratio of the graphene oxide to the carboxylated single-walled carbon nanotubes is 1:1.
Further, the temperature of the drying 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.
The electrically driven thermochromic fiber prepared by the method.
The invention has the following advantages: according to the invention, polyurethane fiber is soaked in graphene oxide/carbon nano tube composite solution for weight increment, and then is subjected to reheat reduction, and finally thermochromic ink and isophorone are smeared to prepare the electro-driven thermochromic fiber. The invention combines the active control of electrochromic and thermochromic structure by utilizing the electrothermal property of the conductive material and the color-changing property of the thermochromic material, and the prepared electro-driven thermochromic fiber has the advantages of both. The electro-driven thermochromic fiber is simple in structure and convenient to prepare, and can actively control the color change, so that the intelligent textile is simpler, more intelligent and multifunctional.
Drawings
Fig. 1 is a graph of temperature versus time for conductive fibers at different voltages.
Fig. 2 is an infrared thermal imaging of conductive fibers under 4V (up), 5V (down) voltage stimulus.
Fig. 3 is a graph of fiber comparison before and after discoloration.
Fig. 4 is a cross-sectional electron microscope image of conductive fibers (left) and fibers as they are (right).
Fig. 5 is a cross-section (left) of a color-changing fiber and a partial magnification electron microscope (right).
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples, to which the scope of the invention is not limited:
Example 1: a method for preparing an electrically driven thermochromic fiber, comprising the steps of:
S1, preparing graphene oxide/carbon nano tube composite solution: dropwise adding carboxylated single-walled carbon nanotube dispersion liquid into graphene oxide dispersion liquid, and stirring while dropwise adding to prepare graphene oxide/carbon nanotube composite solution; wherein, the mass ratio of graphene oxide to carboxylated single-walled carbon nanotubes is 0.8:1; the preparation method of the graphene oxide dispersion liquid comprises the following steps: adding graphene oxide powder into ultrapure water, performing ultrasonic treatment for 8 min, and then dropwise adding ammonia water to adjust the pH value to 7 to obtain 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 in the graphene oxide/carbon nano tube composite solution dripped with the aqueous polyurethane, taking out and drying after soaking, wherein the drying temperature is 40 ℃, the drying time is 5min, repeating the soaking and drying operations until the weight of the fibers is increased by 15%, and finally placing the fibers in a 180 ℃ oven for thermal reduction, wherein the thermal reduction time is 12 min;
S3, preparing the electrically-driven thermochromic fiber: dripping isophorone into the thermochromic ink, uniformly mixing the thermochromic ink and the isophorone according to the mass ratio of 12:1, coating the mixture on the conductive fiber prepared in the step S2, and drying to obtain the electro-driven thermochromic fiber.
Example 2: a method for preparing an electrically driven thermochromic fiber, comprising the steps of:
S1, preparing graphene oxide/carbon nano tube composite solution: dropwise adding carboxylated single-walled carbon nanotube dispersion liquid into graphene oxide dispersion liquid, and stirring while dropwise adding to prepare graphene oxide/carbon nanotube composite solution; wherein, the mass ratio of graphene oxide to carboxylated single-walled carbon nanotubes is 3:1; the preparation method of the graphene oxide dispersion liquid comprises the following steps: adding graphene oxide powder into ultrapure water, performing ultrasonic treatment for 15 min, and then dropwise adding ammonia water to adjust the pH value to 8 to obtain 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 and drying after soaking, wherein the drying temperature is 80 ℃, the drying time is 1 min, repeating the soaking and drying operations until the weight of the fibers is increased by 30%, and finally placing the fibers into a baking oven at 220 ℃ for thermal reduction, wherein the thermal reduction time is 18: 18 min;
S3, preparing the electrically-driven thermochromic fiber: dripping isophorone into the thermochromic ink, uniformly mixing the thermochromic ink and the isophorone according to the mass ratio of 18:1, coating the mixture on the conductive fiber prepared in the step S2, and drying to obtain the electro-driven thermochromic fiber.
Example 3: a method for preparing an electrically driven thermochromic fiber, comprising the steps of:
S1, preparing graphene oxide/carbon nano tube composite solution: dropwise adding carboxylated single-walled carbon nanotube dispersion liquid into graphene oxide dispersion liquid, and stirring while dropwise adding to prepare graphene oxide/carbon nanotube composite solution; wherein, the mass ratio of graphene oxide to carboxylated single-walled carbon nanotubes is 1:1; 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 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 1:10, soaking polyurethane fibers in the graphene oxide/carbon nano tube composite solution dripped with the aqueous polyurethane, taking out and drying after soaking, wherein the drying temperature is 60 ℃, the drying time is 3min, repeating the soaking and drying operations until the weight of the fibers is increased by 25%, and finally placing the fibers in a baking oven at 200 ℃ for thermal reduction, wherein the thermal reduction time is 15min;
S3, preparing the electrically-driven thermochromic fiber: dripping isophorone into the thermochromic ink, uniformly mixing the thermochromic ink and the isophorone according to the mass ratio of 16:1, coating the mixture on the conductive fiber prepared in the step S2, and drying to obtain the electro-driven thermochromic fiber.
The beneficial effects of the invention are illustrated by the following experiments:
1. preparation of electrically driven thermochromic fibers
S1, preparing graphene oxide/carbon nano tube composite solution: dropwise adding 10 mg/mL carboxylated single-wall carbon nanotube dispersion 5mL into graphene oxide dispersion, and stirring while dropwise adding to obtain graphene oxide/carbon nanotube composite solution; the preparation method of the graphene oxide dispersion liquid comprises the following steps: adding 50 mg graphene oxide powder into 10 mL ultrapure water, performing ultrasonic treatment for 10 min, and then dropwise adding ammonia water to adjust the pH value to 7.5 to obtain graphene oxide dispersion liquid;
S2, preparing conductive fibers: dripping 10 mg aqueous polyurethane into the graphene oxide/carbon nano tube composite solution, soaking polyurethane fibers in the graphene oxide/carbon nano tube composite solution in which the aqueous polyurethane is dripped, taking out and drying 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 g, dripping 1g isophorone into the thermochromic ink, uniformly mixing, coating the mixture on the conductive fiber prepared in the step S2, and drying to obtain the electrically-driven thermochromic fiber.
2. Electrothermal property of conductive fiber
And applying 3-5V constant voltage to two ends of the conductive fiber with the length of 1cm, shooting by using an infrared thermal imager, removing the applied voltage after the temperature is stable, and measuring the electrothermal performance of the conductive fiber. The results are shown in fig. 1 and 2, and the results show that the conductive fiber can be heated to 60 ℃ under the voltage of 4V, and the temperature required by the color change of the color-changing ink is reached. The heating time of the conductive fiber is about 15 s, the cooling time is about 10 s, which shows that the conductive fiber has good heat conducting property and can realize the quick response of heat to voltage.
3. Color change properties of color-changing fibers
The color change performance of the color-changing fiber was tested, and as shown in fig. 3, 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 turns orange due to electric heat when voltage is applied.
4. Cross-section electron microscope image of conductive fiber
As a result of electron microscopic scanning of the cross section of the conductive fiber, as shown in fig. 4, it was found from a comparison of electron microscopic images of the cross section of the conductive fiber (left) and the fiber-like (right) that the conductive layer composed of reduced graphene oxide/carbon nanotubes/aqueous polyurethane was attached to the outside of the polyurethane fiber filament.
5. Cross-section electron microscope image of color-changing fiber
The section of the color-changing fiber is scanned by an electron microscope, and as shown in a result of fig. 5, the color-changing layer and the conductive layer are sequentially wrapped outside the polyurethane fiber from the cross section (left) of the color-changing fiber and the enlarged electron microscope image (right), so that the structure is compact, and meanwhile, the color-changing layer wraps the conductive layer to protect the conductive network structure.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art who is skilled in the art to which the present invention pertains will appreciate that the technical scheme and the inventive concept according to the present invention are equally substituted or changed within the scope of the present invention.
Claims (5)
1. A method for preparing an electrically driven thermochromic fiber, comprising the steps of:
s1, preparing graphene oxide/carbon nano tube composite solution: dropwise adding carboxylated single-walled carbon nanotube dispersion liquid into graphene oxide dispersion liquid, and stirring while dropwise adding to prepare graphene oxide/carbon nanotube composite solution; wherein the mass ratio of graphene oxide to carboxylated single-walled carbon nanotubes is 0.8-3:1;
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 dripped with the aqueous polyurethane, taking out and drying after soaking, repeating the soaking and drying operations 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, wherein the thermal reduction time is 12-18 min;
S3, preparing the electrically-driven thermochromic fiber: dripping isophorone into the thermochromic ink, uniformly mixing the thermochromic ink and the isophorone according to the mass ratio of 12-18:1, coating the mixture on the conductive fiber prepared in the step S2, and drying to obtain the electrically-driven thermochromic fiber.
2. The method for preparing an electrically driven thermochromic fiber according to claim 1, wherein the method for preparing the graphene oxide dispersion in step S1 comprises the following steps: 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 graphene oxide dispersion liquid.
3. The method for preparing an electrically driven thermochromic fiber according to claim 1, wherein the mass ratio of graphene oxide to carboxylated single-walled carbon nanotubes in step S1 is 1:1.
4. The method for preparing an electrically driven thermochromic fiber according to claim 1, wherein the temperature of the drying in the step S2 is 40-80 ℃ and the time of the drying is 1-5 min.
5. An electrically driven thermochromic fiber prepared according to the method of any one of claims 1-4.
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Citations (8)
| 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 |
| 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20200181811A1 (en) * | 2018-12-06 | 2020-06-11 | Lintec Of America, Inc. | Continuous production of thermochromic yarns |
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- 2022-12-15 CN CN202211610971.9A patent/CN115710825B/en active Active
Patent Citations (8)
| 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 |
| 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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