CN113652859A - Continuous electrochromism fiber based on polyester filament and preparation method thereof - Google Patents
Continuous electrochromism fiber based on polyester filament and preparation method thereof Download PDFInfo
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- CN113652859A CN113652859A CN202110950919.7A CN202110950919A CN113652859A CN 113652859 A CN113652859 A CN 113652859A CN 202110950919 A CN202110950919 A CN 202110950919A CN 113652859 A CN113652859 A CN 113652859A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 55
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- 239000010949 copper Substances 0.000 claims abstract description 55
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- 239000006084 composite stabilizer Substances 0.000 claims abstract description 9
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- 150000002500 ions Chemical class 0.000 claims description 8
- RRHXZLALVWBDKH-UHFFFAOYSA-M trimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)C RRHXZLALVWBDKH-UHFFFAOYSA-M 0.000 claims description 8
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- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 5
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- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical group [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
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- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical group [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
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- OGKAGKFVPCOHQW-UHFFFAOYSA-L nickel sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O OGKAGKFVPCOHQW-UHFFFAOYSA-L 0.000 description 2
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
- D06M13/5135—Unsaturated compounds containing silicon atoms
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
- D06M15/267—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof of unsaturated carboxylic esters having amino or quaternary ammonium groups
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- Chemically Coating (AREA)
Abstract
The invention discloses a preparation method of a continuous electrochromism fiber based on polyester filaments, which comprises the following steps: s1, winding polyester filament yarns into a ring shape, and removing grease and impurities on the surface; s2, depositing a metal copper coating on the surface of the polyester filament yarn through an electroless deposition process; s3, annealing the polyester filament yarns to obtain polyester conductive filament yarns; s4, enabling the polyester conductive filaments to pass through a groove filled with thermochromic ink, drying the polyester conductive filaments by a heating device, and winding the polyester conductive filaments onto a rolling shaft to obtain continuous thermochromic fibers; in step S2, a composite stabilizer is added to the electroless copper plating solution, the composite stabilizer is composed of potassium ferrocyanide and 2,2 '-bipyridine, the concentration of potassium ferrocyanide is 5-10mg/L, and the concentration of 2, 2' -bipyridine is 5-10 mg/L. The preparation method can realize continuous production of the electrothermal allochroic fiber, has low production cost and controllable fiber diameter, and the obtained fiber has high conductivity.
Description
Technical Field
The invention relates to the technical field of electrochromic fibers, in particular to an electrothermal electrochromic fiber based on polyester filaments and a preparation method thereof.
Background
With the wider application of intelligent textiles, the color-changing fiber technology is rapidly developed, but the color-changing fiber is not highly wearable, has high cost and cannot be produced in a large scale, so that the color-changing fiber is not complete in practical application, and the industrial development of the color-changing fiber is greatly limited. Therefore, the continuous intelligent color-changing fiber with excellent performance produced by the low-cost process has very important scientific research value.
By an electrothermal color-changing fiber is meant that the fiber reversibly changes color, exhibiting an adjustable visual change, upon application of a voltage. The structure process is relatively simple, the preparation process of the microcapsule serving as the thermochromic material is relatively perfect, the technology for preparing the traditional fiber material into the conductive fiber by using an electroless deposition (ELD) technology is relatively mature, the raw materials are easily available, the process is simple, more importantly, the conductive fiber can be prepared by using the common traditional fiber (such as polyester filament) on the market as a substrate, and the conductive fiber obtained by the method has good conductivity, low cost and possibility of large-scale production. Therefore, the polyester monofilaments are continuously prepared into the electrothermal allochroic fibers by the ELD technology, and the electrothermal allochroic fibers have great application value and research significance in the aspects of exploring and developing novel wearable devices, and preventing counterfeiting and hiding.
The electrochromic fiber is one of the popular researches in recent years, and related reports are carried out by a plurality of research teams, but the use of the electrochromic fiber is limited due to the problems of high cost, thick fiber diameter, incapability of continuous production and the like.
As shown in FIG. 1, a research institute of Burkeley information 2016 developed an electrochromic fiber fabric display system Ebb 1, in which thermochromic dyes were applied to conductive wires to form electrochromic fibers, and the fibers were woven into a fabric, the color or pattern of which was changed when different currents were applied thereto. However, this method has a significant disadvantage in that since the selected conductive fiber is prepared by winding an ultra-fine metal wire on a cotton yarn and then the thermochromic fiber is prepared by using the thermochromic ink, the diameter of the fiber is large and the flexibility thereof has a certain defect.
In 2020, Wuhan university of textile team developed a durable core-sheath type nanocomposite yarn [2], as shown in FIG. 2, the composite yarn uses carbon nanotube/Cotton Composite Yarn (CCY) as core and nanofiber polyurethane/thermal ink as sheath, and due to its novel core-sheath nanocomposite structure, the prepared electro-thermochromic composite yarn (ECCY) has excellent mechanical and electrical heating properties and electrochromic properties. However, the method has the disadvantages that the mixed yarn of cotton yarn and carbon nano tube is selected as the substrate material, so the diameter is too large, the response time is long, the local temperature is too high, and the continuous production is difficult.
The voltage-driven sensitive electrothermal allochroic Janus fabric was prepared by the King Korea team at university in south of the Yangtze river in 2020 [3 ]. The conductive layer is formed by graphene, and after the conductive layer is electrified, heat resources are provided for the electrothermal color changing behavior of the polyester fabric due to Joule heating. Thermochromic dyes having reversible color changing properties are coated on opposite sides of the graphene layer. Under an applied voltage of 10V, the color of the electro-thermochromic Janus fabric changes from blue to white at a temperature exceeding 45 ℃, as shown in fig. 3. However, the disadvantages are also obvious, and the development of the electrothermal metamorphic fabric has certain limitations in application, large-scale continuous production is difficult, and the conductive material is graphene, so that the cost is high and continuous mass production is difficult to realize.
[1]Devendorf L,Lo J,Howell N,et al.I don't want to wear a screen:probing perceptions of and possibilities for dynamic displays on clothing[C].CHI Conference on Human Factors in Computing Systems,2016:6028-6039.
[2]Pan J,Hao B,Xu P,et al.Highly robust and durable core-sheath nanocomposite yarns for electro-thermochromic performance application[J].Chemical Engineering Journal,2020,384:123376.
[3]Ge F Q,Liang F,Zhang J J,et al.The electrical-triggered high contrast and reversible color-changing Janus fabric based on double side coating[J].ACS Applied Materials&Interfaces,2020,12:21854-21862.
Disclosure of Invention
The invention aims to provide a preparation method of a continuous electrothermal photochromic fiber based on polyester filament, which can realize continuous production of the electrothermal photochromic fiber, and has the advantages of low production cost, controllable fiber diameter and high electrical conductivity of the obtained fiber.
In order to solve the technical problems, the invention provides a preparation method of a continuous electrochromism fiber based on polyester filaments, which comprises the following steps:
s1, winding polyester filament yarns into a ring shape, and removing grease and impurities on the surface;
s2, depositing a metal copper coating on the surface of the polyester filament yarn processed in the step S1 through an electroless deposition process;
s3, annealing the polyester filament yarn with the metal copper coating obtained in the step S2 to obtain a high-conductivity continuous polyester conductive filament yarn;
s4, assembling the polyester conductive filaments obtained in the step S3 on a unreeling shaft, dragging the polyester conductive filaments by using a rolling shaft to enable the polyester conductive filaments to pass through a groove filled with thermochromic ink so as to enable the surfaces of the polyester conductive filaments to be uniformly coated with the thermochromic ink, drying the polyester conductive filaments by using a heating device, and winding the polyester conductive filaments on the rolling shaft to obtain the continuous thermochromic fibers;
in step S3, a composite stabilizer is added to the electroless-deposited copper plating solution, wherein the composite stabilizer is composed of potassium ferrocyanide and 2, 2' -bipyridine; in the copper plating solution, the concentration of potassium ferrocyanide is 5-10mg/L, and the concentration of 2, 2' -bipyridyl is 5-10 mg/L. Preferably, the concentration of potassium ferrocyanide is 10mg/L and the concentration of 2, 2' -bipyridine is 10 mg/L.
In the invention, the added composite stabilizer is a compound which can form a non-catalytic film on the surface of the copper plating layer, on one hand, the non-ionic surfactant is adsorbed on a new core of the copper layer to form an inactive part, thereby inhibiting the development of the copper layer to be nodular and leading metal crystals to be arranged in a certain direction so as to generate a bright and fine copper layer; on the other hand, the stabilizer will react with Cu+Coordinate to form soluble complex to prevent Cu+CuO is generated.
Further, an additive is also added into the copper plating solution, and the additive is polyethylene glycol; in the copper plating solution, the concentration of polyethylene glycol is 0.004-2.000 g/L. The additive is preferably PEG6000, and the concentration of the additive is preferably 1.5 g/L. The polyethylene glycol can better control the oxidation of the nascent copper, so that the copper layer is more smooth and bright; meanwhile, the polyethylene glycol has a wetting function, so that hydrogen can be conveniently separated out, the hydrogen brittleness of the plating layer is reduced, the toughness is increased, and the plating speed is influenced.
Further, a catalyst is added into the copper plating solution, and the catalyst is nickel salt, including but not limited to nickel sulfate and nickel chloride. In the copper plating solution, the concentration of the catalyst is 0.3-0.5g/L, and preferably 0.4 g/L. In the invention, a proper amount of nickel salt is added into the copper plating solution, so that the copper plating process is continuously carried out, and the binding force of a plating layer is increased; on the other hand, the bubbling of the plating layer can be reduced, and the brightness of the copper layer is improved.
Further, in step S1, the polyester filaments are treated with alkali solution to remove grease and impurities on the surfaces of the polyester filaments.
Further, in step S2, the process of electroless deposition includes the following steps:
a. after carrying out plasma treatment on the polyester filament yarn, soaking the polyester filament yarn in a vinyltrimethoxysilane solution to enable silane to react with hydroxyl on the surface of the polyester filament yarn;
b. b, placing the polyester filament yarn obtained in the step a into a methacryloyloxyethyl trimethyl ammonium chloride aqueous solution, and reacting for 10-60min at 80 ℃ by taking potassium persulfate as an initiator to obtain a cationic polymer modified polyester filament yarn;
c. putting the polyester filament yarn obtained in the step b into (NH)4)2PdCl4In aqueous solution, PdCl is separated by ion exchange4 2-Catalytic ions are fixed on the cationic polymer modified polyester filament;
d. and c, at the temperature of 45 ℃, putting the polyester filament yarn obtained in the step c into a copper plating solution for copper deposition, taking out the polyester filament yarn after the reaction is stopped, cleaning and drying the polyester filament yarn to obtain the polyester filament yarn with the metal copper plating layer.
Further, in the step d, the copper plating solution consists of a solution A and a solution B according to the volume ratio of 1:1, wherein the solution A is prepared from sodium hydroxide, copper sulfate pentahydrate and potassium tartrate, and the solution B is a formaldehyde aqueous solution.
Further, in step S3, the annealing process is performed under vacuum, the annealing temperature is 200 ℃, and the annealing time is 20-40min, preferably 30 min.
The invention provides a continuous electrochromism fiber based on polyester filament prepared by the method, and the intelligent discoloring fiber can be used in the fields of intelligent textiles, military camouflage, anti-counterfeiting, micro visualization and the like.
Further, the continuous electrochromic fiber has an average conductivity of 5.9 × 106-6.7×106S/m, preferably 6.5X 106S/m。
Compared with the prior art, the technical scheme of the invention has the following advantages:
1. the invention solves the problem of continuous preparation of the electrothermal discoloring fiber, utilizes the characteristic of softness and smoothness of the polyester filament yarn to wind the polyester filament yarn into a plurality of circles of spiral rings, and can continuously prepare the electrothermal discoloring fiber with the length of several meters by using electroless deposition technology and thermal ink.
2. The invention solves the problem of thicker fiber diameter, the diameter of the polyester filament yarn is thinner (100 mu m), the surface is smooth and uniform, the fibers with better conductivity and thinner diameter can be obtained by adopting the electroless deposition technology, and the problem of larger fiber diameter can be solved by preparing the electrothermal discoloration fiber.
3. The invention solves the problem of overhigh cost, and the electrothermal allochroic fiber prepared by the polyester filament has lower cost.
4. Response time and voltage directly influence the color change performance and the wearability of the fiber, the shorter the response time, the faster the fiber color change, the smaller the voltage, the higher the fiber wearability. The invention solves the problems of response time and response voltage, and the electrothermal color-changing fiber prepared by adopting the polyester filament has shorter response time (0.97s) and smaller required voltage (2.5V).
Drawings
FIGS. 1-3 are electrothermal thermochromic fibers mentioned in the background;
FIG. 4 is a schematic diagram of the principle of producing the polyester conductive fiber according to the present invention;
FIG. 5 is a flow chart of the present invention for making an electrochromic fiber;
FIG. 6 is a schematic view of a polyester filament yarn (a), a polyester conductive fiber (b) prepared according to the present invention, and an electrothermal discoloration fiber (c);
FIG. 7 is a schematic representation of an electrothermal thermochromic fiber prepared in accordance with the present invention before (a) and after (b) energization;
FIG. 8 is a schematic diagram of the circuit and color change under test.
Detailed Description
The present invention is further described below in conjunction with specific examples to enable those skilled in the art to better understand the present invention and to practice it, but the examples are not intended to limit the present invention.
Unless otherwise specified, the reagents according to the examples of the present invention are all commercially available products, and all of them are commercially available.
Example 1
The embodiment provides a preparation method of a continuous electrochromism fiber based on polyester filaments, which comprises the following steps:
1. preparation of terylene conductive filament by electroless deposition method
1) Winding the polyester filament yarn on a reel with the diameter of 5cm for 20min, then taking off the polyester filament yarn from the reel, treating the polyester filament yarn with a standard solution of NaOH for 60min to remove grease and impurities on the surface, wherein the fiber can keep a circular ring shape.
2) Treating the surface of the polyester filament yarn for 5 minutes by using a plasma cleaning machine to improve the hydrophilic property of the polyester filament yarn; and soaking in 2% (v/v) ethanol solution of Vinyltrimethoxysilane (VTMS) for 15min to react silane with the hydroxyl on the fiber surface.
3) The fiber modified by VTMS is put into a 2% (v/v) aqueous solution of methacryloyloxyethyl trimethyl ammonium chloride (METAC) by taking potassium persulfate as an initiator, and reacts for 60min at 80 ℃ in an oil bath kettle.
4) Weighing a certain amount of ammonium tetrachloropalladate ((NH)4)2PdCl4) Dissolving the powder in deionized water to obtain a solution with a concentration of 4 × 10-3Of M (NH)4)2PdCl4An aqueous solution; putting the modified polyester filament yarn in the step (3) into prepared (NH)4)2PdCl4In aqueous solution for 15min, PdCl was added by ion exchange4 2-The catalytic ions are immobilized on the cationic polymer-modified fiber filaments.
5) The copper plating solution consists of 1:1 solution A and solution B, wherein solution A is sodium hydroxide (18.0 g.L)-1) Copper sulfate pentahydrate (19.5 g.L)-1) And potassium tartrate (43.5 g.L)-1) The composition of the solution B is formaldehyde (14.5 mL. L)-1) An aqueous solution. And mixing the solution A and the solution B to prepare a copper plating solution, and then adding a composite stabilizer (potassium ferrocyanide and 2,2 '-bipyridine), an additive (PEG6000) and a catalyst (nickel sulfate heptahydrate) to ensure that the concentration of the potassium ferrocyanide in the copper plating solution is 10mg/L, the concentration of the 2, 2' -bipyridine is 10mg/L, the concentration of the PEG6000 is 1.5g/L and the concentration of the nickel sulfate heptahydrate is 0.4 g/L. And then, at the temperature of 45 ℃ in an oil bath, putting the modified fiber filaments adsorbing the catalytic ions into copper plating solution to deposit copper, taking out the modified fiber filaments after the reaction is stopped, cleaning and drying to obtain the polyester filaments with the metal copper plating layer.
6) And (3) annealing the polyester filament with the metal copper coating for 30min at the vacuum temperature of 200 ℃ to obtain the high-conductivity continuous polyester conductive filament.
2. Continuous preparation of electrothermal allochroic fibre
Assembling the prepared polyester conductive filament yarn on a unreeling shaft, and leading the polyester conductive filament yarn to quickly pass through a groove filled with thermochromic ink at a constant speed by traction of a rolling shaft so as to uniformly coat the surface of the polyester conductive filament yarn with the ink; and drying by a heating device, and winding on a rolling shaft to obtain the continuous electrochromism fiber.
Comparative example 1
The comparative example provides a preparation method of a continuous electrochromism fiber based on polyester filaments, which comprises the following steps:
1. preparation of terylene conductive filament by electroless deposition method
1) Winding the polyester filament yarn on a reel with the diameter of 5cm for 20min, then taking off the polyester filament yarn from the reel, treating the polyester filament yarn with a standard solution of NaOH for 60min to remove grease and impurities on the surface, wherein the fiber can keep a circular ring shape.
2) Treating the surface of the polyester filament yarn for 5 minutes by using a plasma cleaning machine to improve the hydrophilic property of the polyester filament yarn; and soaking in 2% (v/v) ethanol solution of Vinyltrimethoxysilane (VTMS) for 15min to react silane with the hydroxyl on the fiber surface.
3) The fiber modified by VTMS is put into a 2% (v/v) aqueous solution of methacryloyloxyethyl trimethyl ammonium chloride (METAC) by taking potassium persulfate as an initiator, and reacts for 60min at 80 ℃ in an oil bath kettle.
4) Weighing a certain amount of ammonium tetrachloropalladate ((NH)4)2PdCl4) Dissolving the powder in deionized water to obtain a solution with a concentration of 4 × 10-3Of M (NH)4)2PdCl4An aqueous solution; putting the modified polyester filament yarn in the step (3) into prepared (NH)4)2PdCl4In aqueous solution for 15min, PdCl was added by ion exchange4 2-The catalytic ions are immobilized on the cationic polymer-modified fiber filaments.
5) The copper plating solution consists of 1:1 solution A and solution B, wherein solution A is sodium hydroxide (18.0 g.L)-1) Copper sulfate pentahydrate (19.5 g.L)-1) And potassium tartrate (43.5 g.L)-1) The composition of the solution B is formaldehyde (14.5 mL. L)-1) An aqueous solution. And mixing the solution A and the solution B to prepare a copper plating solution, putting the modified fiber filaments adsorbing catalytic ions into the copper plating solution to deposit copper at the temperature of 45 ℃ in an oil bath, taking out after the reaction is stopped, cleaning and drying to obtain the polyester filaments with the metal copper plating layer.
6) And (3) annealing the polyester filament with the metal copper coating for 30min at the vacuum temperature of 200 ℃ to obtain the high-conductivity continuous polyester conductive filament.
2. Continuous preparation of electrothermal allochroic fibre
Assembling the prepared polyester conductive filament yarn on a unreeling shaft, and leading the polyester conductive filament yarn to quickly pass through a groove filled with thermochromic ink at a constant speed by traction of a rolling shaft so as to uniformly coat the surface of the polyester conductive filament yarn with the ink; and drying by a heating device, and winding on a rolling shaft to obtain the continuous electrochromism fiber.
Comparative example 2
The comparative example provides a preparation method of a continuous electrochromism fiber based on polyester filaments, which comprises the following steps:
1. preparation of terylene conductive filament by electroless deposition method
1) Winding the polyester filament yarn on a reel with the diameter of 5cm for 20min, then taking off the polyester filament yarn from the reel, treating the polyester filament yarn with a standard solution of NaOH for 60min to remove grease and impurities on the surface, wherein the fiber can keep a circular ring shape.
2) Treating the surface of the polyester filament yarn for 5 minutes by using a plasma cleaning machine to improve the hydrophilic property of the polyester filament yarn; and soaking in 2% (v/v) ethanol solution of Vinyltrimethoxysilane (VTMS) for 15min to react silane with the hydroxyl on the fiber surface.
3) The fiber modified by VTMS is put into a 2% (v/v) aqueous solution of methacryloyloxyethyl trimethyl ammonium chloride (METAC) by taking potassium persulfate as an initiator, and reacts for 60min at 80 ℃ in an oil bath kettle.
4) Weighing a certain amount of ammonium tetrachloropalladate ((NH)4)2PdCl4) Dissolving the powder in deionized water to obtain a solution with a concentration of 4 × 10-3Of M (NH)4)2PdCl4An aqueous solution; putting the modified polyester filament yarn in the step (3) into prepared (NH)4)2PdCl4In aqueous solution for 15min, PdCl was added by ion exchange4 2-The catalytic ions are immobilized on the cationic polymer-modified fiber filaments.
5) The copper plating solution consists of 1:1 solution A and solution B, wherein solution A is sodium hydroxide (18.0 g.L)-1) Copper sulfate pentahydrate (19.5 g.L)-1) And potassium tartrate (43.5 g.L)-1) The composition of the solution B is formaldehyde (14.5 mL. L)-1) An aqueous solution. And mixing the solution A and the solution B to prepare a copper plating solution, putting the modified fiber filaments adsorbing catalytic ions into the copper plating solution to deposit copper at the temperature of 45 ℃ in an oil bath, taking out after the reaction is stopped, cleaning and drying to obtain the polyester filaments with the metal copper plating layer.
2. Continuous preparation of electrothermal allochroic fibre
Assembling the prepared polyester conductive filament yarn on a unreeling shaft, and leading the polyester conductive filament yarn to quickly pass through a groove filled with thermochromic ink at a constant speed by traction of a rolling shaft so as to uniformly coat the surface of the polyester conductive filament yarn with the ink; and drying by a heating device, and winding on a rolling shaft to obtain the continuous electrochromism fiber.
Performance testing
1. Color changing function verification
Referring to fig. 7 and 8, after the two ends of the electrothermal chromic fibers prepared in example 1 and comparative examples 1 and 2 are electrified, the color of the fibers is changed remarkably, but the color of example 1 is changed more rapidly and the color is more stable, which shows that the fibers prepared by the invention have the electrothermal chromic function.
2. Conductivity test
The resistance values and fiber diameters of the conductive polyester fibers prepared in example 1 and comparative examples 1 and 2 were measured using a four-probe tester, respectively, wherein the length of the fibers was selected to be 5cm, the number of the groups tested was ten, the average value of the conductivity was calculated, and the obtained results are shown in table 1.
TABLE 1 fiber diameter, resistance and conductivity of the polyester conductive fibers of examples and comparative examples
Average resistance (omega/5 cm) | Average diameter (mm) | Average conductivity (S/m) | |
Example 1 | 0.64 | 123.5 | 6.5×106 |
Comparative example 1 | 2.98 | 116 | 1.58*106 |
Comparative example 2 | 5.88 | 117.5 | 7.84*105 |
The results of Table 1 show that the average conductivity of the conductive polyester fiber of comparative example 1 is 1.58X 106S/m, while the average conductivity of the thermochromic fibers of example 1 reached 6.5X 106S/m is increased by 3.5 times compared with comparative example 1. This shows that the invention can add composite stabilizer, additive and catalyst into the copper plating solutionThe conductivity of the polyester conductive fiber is remarkably improved. Comparative example 2 in which the conductive polyester filaments were not annealed, the average conductivity of the obtained conductive fibers was 7.84 × 105Compared with the example 1, the reduction is 8.3 times, which shows that the annealing treatment in a reasonable temperature range can obviously improve the conductivity of the terylene conductive fiber, and the annealing treatment is also related to the growth of copper crystal grains on the surface of the fiber. The improvement of the conductivity of the polyester conductive fiber directly influences the color change stability of the electrothermal color-changing fiber, and the higher the conductivity is, the quicker the color change of the fiber is.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of a continuous electrochromism fiber based on polyester filament is characterized by comprising the following steps:
s1, winding polyester filament yarns into a ring shape, and removing grease and impurities on the surface;
s2, depositing a metal copper coating on the surface of the polyester filament yarn processed in the step S1 through an electroless deposition process;
s3, annealing the polyester filament yarn with the metal copper coating obtained in the step S2 to obtain a polyester conductive filament yarn;
s4, assembling the polyester conductive filaments obtained in the step S3 on a unreeling shaft, dragging the polyester conductive filaments by using a rolling shaft to enable the polyester conductive filaments to pass through a groove filled with thermochromic ink so as to enable the surfaces of the polyester conductive filaments to be uniformly coated with the thermochromic ink, drying the polyester conductive filaments by using a heating device, and winding the polyester conductive filaments on the rolling shaft to obtain the continuous thermochromic fibers;
in step S3, a composite stabilizer is added to the electroless-deposited copper plating solution, wherein the composite stabilizer is composed of potassium ferrocyanide and 2, 2' -bipyridine; in the copper plating solution, the concentration of potassium ferrocyanide is 5-10mg/L, and the concentration of 2, 2' -bipyridyl is 5-10 mg/L.
2. The method for preparing the continuous electrochromism fiber based on the polyester filament yarn as claimed in claim 1, wherein an additive is further added into the copper plating solution, and the additive is polyethylene glycol; in the copper plating solution, the concentration of polyethylene glycol is 0.004-2.000 g/L.
3. The method for preparing the continuous electrochromism fiber based on the polyester filament yarn as claimed in claim 1, wherein a catalyst is further added into the copper plating solution, and the catalyst is nickel salt; in the copper plating solution, the concentration of the catalyst is 0.3-0.5 g/L.
4. The method for preparing continuous electrochromism fibers based on polyester filaments as claimed in claim 3, wherein the nickel salt is nickel sulfate and/or nickel chloride.
5. The method for preparing continuous electrochromism fibers based on polyester filaments as claimed in claim 1, wherein in step S1, the polyester filaments are treated with alkali solution to remove grease and impurities on the surfaces of the polyester filaments.
6. The method for preparing continuous electrochromism fibers based on polyester filaments according to claim 1, wherein in the step S2, the electroless deposition process comprises the following steps:
a. after carrying out plasma treatment on the polyester filament yarn, soaking the polyester filament yarn in a vinyltrimethoxysilane solution to enable silane to react with hydroxyl on the surface of the polyester filament yarn;
b. b, placing the polyester filament yarn obtained in the step a into a methacryloyloxyethyl trimethyl ammonium chloride aqueous solution, and reacting for 10-60min at 80 ℃ by taking potassium persulfate as an initiator to obtain a cationic polymer modified polyester filament yarn;
c. washing the polyester obtained in the step bPutting in (NH)4)2PdCl4In aqueous solution, PdCl is separated by ion exchange4 2-Catalytic ions are fixed on the cationic polymer modified polyester filament;
d. and c, at the temperature of 45 ℃, putting the polyester filament yarn obtained in the step c into a copper plating solution for copper deposition, taking out the polyester filament yarn after the reaction is stopped, cleaning and drying the polyester filament yarn to obtain the polyester filament yarn with the metal copper plating layer.
7. The method as claimed in claim 6, wherein the copper plating solution is composed of a solution A and a solution B at a volume ratio of 1:1, wherein the solution A is prepared from sodium hydroxide, copper sulfate pentahydrate and potassium tartrate, and the solution B is formaldehyde aqueous solution.
8. The method for preparing a continuous electrochromism fiber based on polyester filaments as claimed in claim 1, wherein in step S3, the annealing treatment is performed under vacuum, the annealing temperature is 200 ℃, and the annealing time is 20-40 min.
9. The continuous electrochromism fiber based on polyester filaments prepared by the method according to any one of claims 1 to 8.
10. The continuous electrochrome fiber based on polyester filaments according to claim 9 wherein the average electrical conductivity of the continuous electrochrome fiber is 5.9 x 106-6.7×106S/m。
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