CN113969434A - An electro/thermochromic fluorescent fiber and its preparation method and application - Google Patents
An electro/thermochromic fluorescent fiber and its preparation method and application Download PDFInfo
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- CN113969434A CN113969434A CN202111284195.3A CN202111284195A CN113969434A CN 113969434 A CN113969434 A CN 113969434A CN 202111284195 A CN202111284195 A CN 202111284195A CN 113969434 A CN113969434 A CN 113969434A
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K9/00—Tenebrescent materials, i.e. materials for which the range of wavelengths for energy absorption is changed as a result of excitation by some form of energy
- C09K9/02—Organic tenebrescent materials
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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
- D01F1/06—Dyes
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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
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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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1088—Heterocyclic compounds characterised by ligands containing oxygen as the only heteroatom
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Abstract
本发明涉及一种电/热致变色荧光纤维及其制备方法和应用。该纤维包括成纤聚合物、荧光染料和相变材料。该制备方法包括：将荧光染料和熔融态的相变材料混合，加入到含有表面活性剂的水溶液中，得到乳液，然后与成纤聚合物水溶液混合，得到纺丝液，湿法纺丝。该纤维具有良好、稳定的变色性能。
The invention relates to an electro/thermochromic fluorescent fiber and its preparation method and application. The fibers include fiber-forming polymers, fluorescent dyes, and phase-change materials. The preparation method includes: mixing the fluorescent dye and the molten phase change material, adding it into an aqueous solution containing a surfactant to obtain an emulsion, then mixing with the aqueous solution of a fiber-forming polymer to obtain a spinning solution, and wet spinning. The fiber has good and stable discoloration properties.
Description
Technical Field
The invention belongs to the field of intelligent fibers and preparation and application thereof, and particularly relates to an electrochromic/thermochromic fluorescent fiber and a preparation method and application thereof.
Background
On the basis of possessing the wearability and the appearance style of common textile materials, the intelligent textile material can also sense the external environment, and can make corresponding feedback by changing one or more performance parameters of the intelligent textile material, thereby responding to the external environment and realizing a novel textile material which is adaptive to the external environment. The intelligent textile with the tunable luminescence characteristic has great application potential in the fields of sensing, image display, optical recording, anti-counterfeiting, environment monitoring, camouflage and the like by sensing the change of an external environment so as to adjust the color change of the intelligent textile, and is paid more and more attention. The one-dimensional intelligent fiber serving as a basic unit of the textile material has good application adaptability and becomes a core hotspot of a plurality of researches. The intelligent color-changing fiber capable of tunable luminescence is based on luminescent materials responding to external stimuli such as electricity, heat, light, humidity, pH value and ions. Among these controllable methods, electricity can be considered as the most accurate operation method of the optical device. Considerable pioneering work has been done to develop electrochromic devices. However, the electrochromic device is usually based on electrically controlled oxidation-reduction reaction, which results in complex fiber composition and complicated preparation process, and greatly hinders the practical application and commercialization thereof. In contrast, the thermochromic luminescent material has attracted much attention due to its characteristics of simple preparation, low cost, wide applicability, and the like. In combination with an electrically heated material, an electro/thermochromic material containing one-dimensional fibers can be easily obtained.
Disclosure of Invention
The invention aims to solve the technical problem of providing an electrochromic/thermochromic fluorescent fiber and a preparation method and application thereof so as to fill the blank in the prior art.
The invention provides an electro/thermochromic fluorescent fiber, which comprises a fiber-forming polymer, a fluorescent dye and a phase-change material.
The electrochromic fluorescent fiber further comprises a metal wire, and the metal wire is wrapped by the mixture of the fiber-forming polymer, the fluorescent dye and the phase-change material to form a core-wrapping structure.
The mass ratio of the fiber-forming polymer to the fluorescent dye to the phase-change material is 1000-3000: 1-10: 1000-3000.
The fiber-forming polymer comprises one or more of sodium alginate SA, polyvinyl alcohol PVA and polyacrylonitrile PAN.
The fluorescent dye comprises one or more of coumarin organic matters, methylene blue and nile red.
The phase change material comprises one or more of fatty acid FA, paraffin PWs, polyethylene glycol PEG and polycaprolactone PCL.
The invention also provides a preparation method of the electric/thermochromic fluorescent fiber, which comprises the following steps:
(1) mixing a fluorescent dye and a molten phase-change material, and adding the mixture into an aqueous solution containing a surfactant to obtain an emulsion; (2) mixing the emulsion obtained in the step (1) with a fiber-forming polymer aqueous solution to obtain a spinning solution;
(3) extruding the spinning solution obtained in the step (1) from a single-axis spinneret orifice, entering a coagulating bath for coagulation and drafting to form nascent fibers, and drying to obtain thermochromic fluorescent fibers;
or extruding the spinning solution in the step (1) from a coaxial spinneret orifice along with the metal wire, enabling the spinning solution to wrap the metal wire to form a core-wrapping structure, entering a coagulating bath for coagulation and drafting to form a nascent fiber, and drying to obtain the electrochromic fluorescent fiber.
The mass ratio of the fluorescent dye, the molten phase-change material and the surfactant in the step (1) is 1-10: 1000-3000: 300 to 1200.
The mass ratio of the mixture of the fluorescent dye and the molten phase-change material in the emulsion in the step (1) to the water is 1: 20-1: 100.
the mass ratio of the mixture of the fluorescent dye and the molten phase-change material in the emulsion in the step (1) to the water is 1: 30.
the surfactant in the step (1) comprises one or more of cetyl trimethyl ammonium bromide CTAB, sodium dodecyl benzene sulfonate SDBS and monolauryl phosphate MAP.
The mass ratio of the emulsion to the fiber-forming polymer aqueous solution in the step (2) is 2: 1-2: 4.
and (3) the mass fraction of the fiber-forming polymer in the spinning solution in the step (2) is 1.5-20%.
When the fiber forming polymer in the step (2) is sodium alginate, the mass fraction of the sodium alginate in the spinning solution is 1.5-4%, and the preferable mass fraction is 2%.
When the fiber forming polymer in the step (2) is polyvinyl alcohol, the mass fraction of the polyvinyl alcohol in the spinning solution is 10-20%, and the preferred mass fraction is 15%.
The diameter of the needle eye of the single-axis spinneret orifice in the step (3) is 0.5-2.0 mm.
The diameter of the outer hole of the coaxial spinneret hole in the step (3) is 1.5-3.0 mm, and the diameter of the inner hole is 0.3-1.0 mm.
The drafting multiple in the step (3) is 1.1-3.0 times.
And (3) the coagulating bath is an aqueous solution or a supersaturated inorganic salt aqueous solution containing polyvalent metal ions with the mass fraction of 0.3-2.0%.
When the fiber-forming polymer is sodium alginate, the coagulating bath is an aqueous solution containing polyvalent metal ions with the mass fraction of 0.3-2.0%.
The aqueous solution containing 0.3-2.0% by mass of polyvalent metal ions comprises Ca2+、Ba2+、Al3+The preferable mass fraction of one or more of the aqueous solutions is 0.5%.
When the fiber-forming polymer is polyvinyl alcohol, the coagulation bath is a supersaturated aqueous solution of an inorganic salt.
The supersaturated aqueous solution of inorganic salt comprises Na2SO4、ZnSO4One or two of them.
The invention also provides an application of the electrochromic/thermochromic fluorescent fiber in intelligent textiles.
The invention adopts the phase-change material as the disperse matrix of the fluorescent dye, and can induce the transition between the crystalline state and the molten state thereof through the temperature, thereby realizing the regulation and control of the disperse state of the fluorophore and developing the ideal thermochromic luminescent material. Specifically, in the molten state of the phase-change material, the fluorescent dye and the phase-change material molecules have good interaction, and a dispersed state is presented. When the temperature is below the phase transition point, the phase change material undergoes self-crystallization behavior, phase separation from the fluorescent dye, causing the fluorophore to be forced to exist in an aggregated state. The strategy for realizing the fluorescent color change regulation and control through the self-crystallization phase change has no special structural requirements on the fluorescent dye, and the method is simple and easy to implement. The self-crystallized phase-change thermal fluorescent photochromic material can be mixed with spinning solution, and the fluorescent photochromic fiber with thermal induction can be spun by the traditional spinning technology. In addition, the thermochromic fluorescent system can realize electrically triggered fluorescent color change through a heat-resistant material, namely the electrochromic fluorescent fiber is prepared.
The invention realizes the electric/thermal driven fluorescent color changing function by utilizing the self-crystallization phase change material through regulating and controlling the dispersion state of the fluorescent group by temperature. The phase-change material as the matrix can realize the transformation between a crystalline state and a molten state before and after the phase-change point, thereby controlling the dispersion state of the fluorescent dye filled in the phase-change material and realizing the purpose of electro/thermal fluorescence color change.
Advantageous effects
The fiber-forming high polymer and the color-changing fluorescent emulsion are uniformly mixed together by physical blending, and the thermochromic fluorescent fiber is prepared by utilizing a wet spinning technology and can show different fluorescent colors at normal temperature and high temperature (higher than the temperature of a phase change point). The fluorescence color change of the fiber is kept consistent in 100 temperature rise-temperature fall cycles, which proves that the color-changing fluorescence fiber based on the self-crystallization phase change has good stability. In addition, the electric/thermochromic fluorescent fiber formed by compounding the spinning solution and the metal wire can utilize joule heat of an electric heating material to realize voltage regulation and control of fluorescent change of the metal wire composite fiber.
Drawings
FIG. 1 is a graph showing the change of fluorescence color of the color-changing fluorescent emulsion prepared in example 1 by mixing 7- (diethylamino) coumarin-3-methyl and hexadecanoic acid before and after heating.
FIG. 2 is an SEM topography of emulsion droplet particles in the color-changing fluorescent emulsion prepared in example 1.
FIG. 3 is a photograph of the thermochromic fluorescent fiber of example 1 taken at room temperature and high temperature (75 ℃) with ultraviolet light (365 nm).
FIG. 4 shows the fluorescence colors of the thermochromic fluorescent fibers of example 1 in the crystalline state (room temperature) and the molten state (75 deg.C) respectively after the fibers undergo 100 heating/cooling cycles.
FIG. 5 is a photograph taken under visible light and under UV lamp irradiation of the electro-thermochromic fluorescent fibers prepared in example 1.
FIG. 6 shows that the fluorescence color conversion of the electro-thermochromic fluorescent fiber prepared in example 1 is controlled by applying a voltage across the fiber.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
And (3) reagent sources:
7- (diethylamino) coumarin-3-methyl: saen chemical technology (shanghai) ltd;
palmitic acid, sodium alginate: shanghai Aladdin Biotechnology GmbH;
anhydrous calcium chloride: shanghai Tankou Technique, Inc.;
polyvinyl alcohol, sodium sulfate, cetyltrimethylammonium bromide, sodium dodecylbenzenesulfonate: chemical agents of the national drug group, ltd.
Example 1
A preparation method of electrochromic fluorescent fibers based on hexadecanoic acid phase-change materials comprises the following steps:
(1) preparation of color-changing fluorescent emulsion based on hexadecanoic acid phase-change material
Weighing 7.0mg of 7- (diethylamino) coumarin-3-methyl powder and 1.5g of palmitic acid powder, heating in a water bath at 80 ℃ to completely dissolve coumarin and palmitic acid, and magnetically stirring for 10min until the solution is clear and transparent to obtain a phase-change mixture. Meanwhile, 0.5g of CTAB powder and 50mL of deionized water are added into a beaker, and the mixture is stirred and heated in a water bath kettle at 80 ℃ by magnetic force, and the phase-change mixture is poured into the CTAB aqueous solution quickly and is stirred and heated by magnetic force for 10min, so that the coumarin/palmitic acid emulsion is obtained.
(2) Preparation of fluorescent color-changing sodium alginate spinning solution
Weighing 2.0g of sodium alginate powder in a beaker, adding 50mL of deionized water, and magnetically stirring the solution for 6 hours until the sodium alginate is fully dissolved, and the solution is uniform and has no bubbles. And (3) cooling the color-changing fluorescent emulsion prepared in the step (1), pouring the cooled color-changing fluorescent emulsion into a sodium alginate solution, and uniformly stirring.
(3) Preparation of electrochromic fluorescent fiber
Feeding the sodium alginate spinning solution into a metering pump, wherein the outer aperture of a spinneret orifice needle is 3.0mm, and the inner aperture is 0.6 mm. Leading copper wires out of the inner hole to be wrapped in spinning solution extruded from the outer hole, and directly feeding the spinning solution into a coagulating bath (CaCl with the mass ratio of 0.5%) after being sprayed out by a spinneret2Solution), and drawn and wound to form a nascent fiber, the draw ratio of which is set to 1.5 times. And naturally airing the primary silk fiber to obtain the electrochromic fluorescent fiber.
FIG. 1 shows that: the fluorescence of the coumarin/palmitic acid mixture is orange at normal temperature (left picture), and the fluorescence is converted into blue when the coumarin/palmitic acid mixture is heated to be above the phase transition point (right picture), which shows that the fluorescence color of the coumarin/palmitic acid mixture is converted between orange and blue before and after the phase transition temperature, and the change is reversible.
FIG. 2 shows that: in the coumarin/palmitic acid emulsion, emulsion droplets are ellipsoidal, and the diameter is about 100 nm.
FIG. 3 shows: the thermochromic fluorescent fibers show yellow fluorescence at normal temperature (25 ℃ C.) (left panel), and blue fluorescence at high temperature (75 ℃ C.) (right panel).
FIG. 4 shows that: the thermochromic fluorescent fiber stably shows yellow fluorescence at normal temperature (25 ℃) and blue fluorescence at high temperature (75 ℃) after going through 100 heating-cooling cycles (left panel).
FIG. 5 shows that: the fiber is light yellow under visible light (left picture), and generates orange-yellow fluorescence under ultraviolet light (right picture), which illustrates that the electrochromic fluorescent fiber prepared in example 1 is yellow under normal temperature, and shows orange-yellow fluorescence under ultraviolet lamp irradiation.
FIG. 6 shows that: the left graph shows blue fluorescence in the power-on state, and the right graph shows yellow fluorescence in the power-off state, which shows that the fluorescence color of the fiber can be regulated and controlled by joule heat to be changed by applying voltage to two ends of the copper wire, and the change is also reversible.
Example 2
A preparation method of a thermochromic fluorescent fiber based on a myristic acid phase change material comprises the following steps:
(1) preparation of color-changing fluorescent emulsion based on myristic acid phase-change material
Weighing 5.0mg of 7- (diethylamino) coumarin-3-methyl powder and 1.5g of myristic acid powder, heating in a water bath at 70 ℃ to completely dissolve coumarin and myristic acid, and magnetically stirring for 10min until the solution is clear and transparent to obtain a phase-change mixture. Meanwhile, 0.6g of SDBS powder and 50mL of deionized water are added into a beaker, magnetic stirring and heating are carried out in a 70 ℃ water bath kettle, the phase-change mixture is rapidly poured into the SDBS aqueous solution, and magnetic stirring and heating are carried out for 10min, so as to obtain the coumarin/myristic acid color-change fluorescent emulsion.
(2) Preparation of fluorescent color-changing polyvinyl alcohol spinning solution
Weighing 15.0g of polyvinyl alcohol powder in a beaker, adding 50mL of deionized water, and dissolving at 95 ℃ for 6h until the polyvinyl alcohol is fully dissolved, the solution is uniform and has no bubbles. And after the original spinning solution is cooled, mixing the cooled original spinning solution with the color-changing fluorescent emulsion, and uniformly stirring.
(3) Preparation of thermochromic fluorescent fibers
Feeding the polyvinyl alcohol spinning solution into a metering pump, wherein the aperture of a spinneret orifice needle is 1.2 mm. The spinning solution is sprayed out by a spinneret and directly enters a coagulating bath (supersaturated sodium sulfate solution), and is drafted and wound to form primary filaments, wherein the drafting multiple is 1.5 times. And taking out the fibers, and performing thermal drying treatment to obtain the thermochromic fluorescent fibers.
Comparative example 1
In a comparison patent of 'fluorescent fiber based on rare earth doping up-conversion nano material and a preparation method thereof', the fluorescent fiber based on the rare earth doping up-conversion nano material is disclosed, poly dopamine modified fiber is firstly soaked in GPTMS modified YF3: Yb and Er nano crystal colloidal solution for 30-60min, is repeatedly washed by ethanol after being taken out, and is soaked in PEI modified YF3: Yb and Er nano crystal colloidal solution for 30-60 min; and repeating the assembling process to prepare the fluorescent fiber based on the rare earth doped up-conversion nano material. The invention endows the fiber with upconversion fluorescence performance, and has important application value in the field of anti-counterfeiting textiles.
Compared with the prior art, the preparation method of the fluorescent fiber adopts the completely different processes: according to the contrast patent, the rare earth doped fluorescent nanocrystalline is modified on the surface of the polydopamine modified fiber in a surface assembly mode; in the invention, the fluorescent dye, the phase-change material and the fiber-forming polymer are mixed to prepare the color-changing fluorescent spinning solution, and then the color-changing fluorescent fiber which can be woven is directly prepared by adopting a wet spinning process. Compared with the nano fluorescent fiber of the comparative example, the fiber prepared by the invention has strong spinnability and wide application.
The fluorescent material of the present invention is different from the comparative patents: the comparative patent is to perform fluorescence emission through a rare earth doped fluorescent nanocrystal; the invention aims at one or more of organic fluorescent dyes including coumarin organic matters, methylene blue and nile red.
The luminescent properties of the fluorescent fibers of the present invention are quite different from the comparative patents: compared with the fluorescent fiber in the patent, the color of the fluorescent fiber is single, and the conversion of the fluorescent color to the external stimulus cannot be generated; the dispersion state of the fluorescent group can be regulated and controlled by the state of the dispersed matrix phase-change material, so that the electric/thermal fluorescence color-changing behavior is realized.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115019626A (en) * | 2022-07-07 | 2022-09-06 | 吉林大学 | Application of thermosensitive fluorescent material in anti-counterfeiting trademark |
| CN115074863A (en) * | 2022-06-29 | 2022-09-20 | 华中科技大学 | A kind of electrochromic fiber and fabric, and preparation method thereof |
| CN116103786A (en) * | 2023-02-20 | 2023-05-12 | 江南大学 | A preparation method of bistable multi-stimuli-responsive Janus discoloration fiber |
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Application publication date: 20220125 |
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