A multi-component spun-dyed yarn and a method for producing the same
By combining subcritical hydrolysis and nanomaterial composite technology with a multidimensional intelligent response system and dynamic cross-linking network, the problems of high cost, poor controllability and color difference in multi-component blended colored yarns have been solved, realizing efficient and intelligent integration of textile functions and expanding high-end application fields.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- JIANGSU CHINA TEXTILE UNITED KNITTING CO LTD
- Filing Date
- 2026-02-06
- Publication Date
- 2026-06-16
AI Technical Summary
Existing multi-component blended yarn technology suffers from high cost, high energy consumption, complex process, poor controllability, and easy color difference, making it difficult to achieve dynamic changes in fiber composition and uniform mixing.
A composite extract was prepared by subcritical hydrolysis of blueberry peel and sea buckthorn pulp. This was combined with the in-situ reduction reaction of graphene oxide and silver nanowires to construct a functional composite. The composite was then mixed with various fibers and ternary composite fibers were formed through airflow and melt dual-channel spinning technology. Subsequent dynamic cross-linking and surface modification were carried out to form intelligent colored fibers.
It realizes intelligent color changing, environmental sensing, self-healing and conductivity functions of multi-component blended colored yarns, enhances the added value and application prospects of textiles, and shows unique advantages in fields such as smart clothing, medical health monitoring and military camouflage protection.
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Figure CN122215112A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of textile materials technology, specifically to a multi-component blended colored yarn and its preparation method. Background Technology
[0002] Multi-component blended yarns are widely used in high-end apparel fabrics, home textiles, and functional textiles due to their advantages in color expression, functional integration, and environmental performance. The technological demands of these applications mainly focus on three aspects: first, achieving uniform mixing of various fibers and dyeing raw materials to avoid color differences or uneven fiber distribution in the yarn; second, improving the spinnability of the yarn and reducing breakage rates caused by differences in fiber properties during production; and third, meeting environmental protection requirements by reducing chemical consumption and wastewater discharge during the dyeing process.
[0003] Currently, the existing solutions for this technical requirement mainly include the following: Raw material pretreatment technology: Improve the spinnability of natural fibers such as wool and silk by impregnating them with antistatic agents and oils, and reduce static interference.
[0004] Multi-stage blending process: The fiber is pre-mixed in layers using the horizontal laying and direct extraction method, and then combined with the split mixing in the opening and cleaning process and the blending in the drawing frame to improve the accuracy of the blending ratio.
[0005] Electronic yarn clearer parameter optimization: By setting the breakage detection threshold for different fiber combinations, yarn damage caused by melting point differences during high-speed winding can be reduced. However, parameter setting still relies on experience accumulation and is difficult to adapt to the dynamic characteristics changes of different fiber combinations in real time.
[0006] While the above methods have achieved some success in specific scenarios, the following problems still exist: High cost and high energy consumption: Although raw material pretreatment technology can improve spinnability, it increases production costs and energy consumption due to the need to increase impregnation equipment and curing time.
[0007] Complex process: Although the multi-stage mixing process improves the uniformity of blending, the equipment is complex and the process connection error can easily lead to batch-to-batch quality fluctuations.
[0008] Poor controllability and susceptibility to color differences: While optimized parameters of electronic yarn clearers reduce breakage rates, they lack intelligent dynamic adjustment capabilities, making it difficult to cope with changes in the characteristics of new fiber combinations. Furthermore, when dealing with multi-component blends, precise sampling systems for dyed fibers are limited by differences in dye fixation rates, potentially leading to color differences between samples and bulk production. Summary of the Invention
[0009] To address the shortcomings of existing technologies, this invention provides a multi-component blended colored yarn and its preparation method, thus solving the problems mentioned above in the background technology.
[0010] According to a first aspect of the present invention, a method for preparing multi-component blended colored yarn is provided, comprising the following steps: (a) Preparation of compound extract: 80-100 parts of alpine blueberry peel and 20-30 parts of sea buckthorn pulp were extracted by subcritical hydrolysis to obtain a compound extract rich in anthocyanins, pectin and sea buckthorn flavonoids; (b) Preparation of functional complex: The composite extract prepared in step (a) is subjected to an in-situ reduction reaction with 5-8 parts of graphene oxide and 2-3 parts of silver nanowires under ultrasonic assistance. The power is 240-260W, the frequency is 38-42kHz, and the reaction time is 25-35min to obtain the functional complex. (c) Preparation of the mixed fiber material: The functional composite prepared in step (b), 40-50 parts of regenerated chitosan fiber, 30-40 parts of polyethylene terephthalate hollow fiber, 20-30 parts of carbon nanotube / silk fiber composite material, 8-12 parts of graphene aerogel fiber, 5-8 parts of photothermal responsive liquid crystal elastomer fiber and 3-5 parts of interface remodeling silk fibroin / soybean protein fiber are mixed to obtain the mixed fiber material; (d) Preparation of ternary composite fibers: Using airflow and melt spinning dual-channel technology, the mixed fiber material prepared in step (c) is subjected to gradient spinning under nitrogen protection. The temperature gradients are set to 215-225℃, 195-205℃, and 175-185℃, and the pressure gradients are set to 0.7-0.9MPa, 0.4-0.6MPa, and 0.2-0.4MPa, respectively, to form the ternary composite fibers; (e) Preparation of reversible cross-linked fiber bundles: The ternary composite fiber prepared in step (d) is immersed in 90-100 parts of dynamic cross-linking agent solution and cross-linked at 58-62°C for 1.4-1.6 hours to obtain the reversible cross-linked fiber bundles; (f) Preparation of intelligent colored fiber: The reversible cross-linked fiber bundle prepared in step (e) is immersed in 20-30 parts of composite dyeing solution and subjected to covalent grafting reaction at 78-82℃ for 1.8-2.2 hours to obtain the intelligent colored fiber; (g) Modification and finishing: The smart colored fiber prepared in step (f) is surface modified in a plasma treatment chamber containing 50-60 parts of nano-sized silica aerogel and 10-15 parts of carbon nanotube array, with a power of 380-420W and a time of 170-190s, to obtain the multi-component blended colored yarn.
[0011] According to an embodiment of the present invention, in step (a), the subcritical hydrolysis extraction uses ultrapure water as the solvent, the mass ratio of the alpine blueberry peel, the sea buckthorn pulp and the ultrapure water is 1:1:15-1:1:20, the extraction temperature is 110-130℃, the pressure is 0.3-0.5MPa and the time is 30-45 minutes.
[0012] According to an embodiment of the present invention, in step (a), by synergistically combining the peel of alpine blueberries with sea buckthorn pulp and employing subcritical water extraction technology, efficient co-extraction and stable compounding of active ingredients are achieved. The anthocyanins abundant in alpine blueberries and the sea buckthorn flavonoids unique to sea buckthorn pulp undergo intermolecular association in a subcritical water system to form a stable complex. This complex, together with pectin, constructs a three-dimensional network structure, which not only significantly improves the stability of the extract but also provides abundant active sites for subsequent in-situ compounding with nanomaterials. Ultimately, the obtained composite extract possesses both excellent photostability and enhanced interfacial compatibility, laying a crucial foundation for the preparation of multifunctional intelligent fibers.
[0013] According to an embodiment of the present invention, in step (b), the graphene oxide is a yellow sheet-like solid material obtained by mixing natural flake graphite and potassium permanganate at a mass ratio of 1:3-1:5 and reacting for 4-6 hours, washing with deionized water until neutral, and then ultrasonically exfoliating. The sheet diameter is 1-5 μm and the thickness is 0.8-1.2 nm. The silver nanowires are silver-white linear materials formed by dissolving silver nitrate and polyvinylpyrrolidone at a mass ratio of 1:1-1:3 in ethylene glycol and reducing them at 160-180°C for 2-4 hours. The silver nanowires have a diameter of 50-100 nm and a length of 10-20 μm.
[0014] According to an embodiment of the present invention, in step (b), the diameter and length of the silver nanowires are measured using a scanning electron microscope in accordance with GB / T 24491-2009 "Multi-walled Carbon Nanotubes".
[0015] According to an embodiment of the present invention, in step (b), anthocyanins and sea buckthorn flavonoids in the composite extract are used as natural reducing agents to simultaneously reduce graphene oxide and silver nanowire precursors under the assistance of ultrasonic energy, thus achieving green in-situ composite of nanomaterials. The catechol structure of anthocyanins forms strong hydrogen bonds with the oxygen-containing functional groups of graphene oxide, while the ketone groups of sea buckthorn flavonoids undergo coordination reduction with silver ions. The two-dimensional sheets of graphene oxide and the one-dimensional structure of silver nanowires intertwine in the ultrasonic field to construct a three-dimensional conductive network. The silver nanowires effectively bridge the gaps between the graphene oxide sheets, synergistically enhancing the electron transport capability and structural stability of the composite, ultimately forming a functional composite with excellent photosensitivity and conductive continuity.
[0016] According to an embodiment of the present invention, in step (c), the regenerated chitosan fiber is a white fiber filament obtained by dissolving chitosan in an acetic acid solution with a mass fraction of 2-4%, spinning it, and then subjecting it to γ-irradiation crosslinking treatment, with an irradiation dose of 45-55 kGy and a crosslinking degree of ≥85%. The polyethylene terephthalate hollow fiber is a hollow filament produced by melt spinning polyethylene terephthalate and potassium titanate whiskers at a mass ratio of 100:1.5-100:2.5, with a hollowness of 35%-45%. The carbon nanotube / silk fiber composite material is a composite filament made by plasma etching of carbon nanotubes and silk fibers in a mass ratio of 3:100-5:100. The etching gas is argon, the etching power is 280-320W, and the time is 110-130s. The graphene aerogel fiber is a black filament produced by wet spinning and thermal reduction of graphene oxide solution, with a specific surface area of 500-800 m² / g and a pore size distribution of 2-50 nm. The photothermal responsive liquid crystal elastomer fiber is formed by mixing aromatic liquid crystal monomers with a mesocrystalline content of 30%-40% and a hydrogen-containing silicone oil crosslinking agent at a mass ratio of 10:1-10:2, adding 0.5%-1% photothermal conversion agent, melt spinning at 180-200℃, and then orientation and setting at 80-100℃ for 2-4 hours to form a yellow elastic fiber with photoinduced deformation effect. The glass transition temperature is 45-50℃, and the near-infrared light absorption rate is ≥90%. The interface-reconstructed silk fibroin / soybean protein fiber is a white ultrafine fiber with an amphiphilic core-shell structure, formed by electrospinning silk fibroin and soybean protein at a mass ratio of 2:1-3:1, with a diameter of 8-15 μm. The silk fibroin forms a hydrophobic core layer, and the soybean protein forms a hydrophilic shell layer.
[0017] According to an embodiment of the present invention, in step (c), the degree of crosslinking of the regenerated chitosan fiber is measured with reference to GB / T 3916-2013 "Determination of breaking strength and elongation at break of single yarn in textile packages"; the hollowness of the polyethylene terephthalate hollow fiber is measured according to FZ / T 50034-2014 "Test method for hollowness of polyethylene terephthalate (PET) hollow fiber"; the specific surface area and pore size distribution of the graphene aerogel fiber are measured according to GB / T19587-2017 "Determination of specific surface area of solid materials by gas adsorption BET method" and GB / T 21650.2-2008 "Determination of pore size distribution and porosity of solid materials by mercury porosimetry and gas adsorption method"; the glass transition temperature and near-infrared light absorptivity of the photothermal responsive liquid crystal elastomer fiber are measured according to GB / T The diameter of the interface-reconstructed silk fibroin / soybean protein fiber was measured according to GB / T 19466.2-2004 "Differential Scanning Calorimetry (DSC) for Plastics" and GB / T 35241-2017 "Test Method for Absorption Rate of Visible and Near-Infrared Spectroscopy"; the diameter of the interface-reconstructed silk fibroin / soybean protein fiber was measured according to GB / T 10685-2007 "Test Method for Diameter of Wool Fiber - Projection Microscopy Method".
[0018] According to an embodiment of the present invention, in step (c), a multidimensional intelligent response system is constructed through the synergistic combination of seven functional fibers. The functional complex acts as an active connecting bridge, and its surface nanoparticles generate multiple interfacial interactions with each fiber component; the interface reconstruction fiber significantly improves the compatibility between hydrophobic and hydrophilic fibers due to its amphiphilic core-shell structure; the micro-area deformation generated by the photothermal responsive fiber under near-infrared light is converted into an electrical signal through the piezoelectric effect of the hollow fiber; the graphene aerogel fiber and carbon nanotube synergistically construct a three-dimensional conductive network; the active amino groups of the regenerated chitosan fiber form dynamic covalent bonds with the functional complex, ultimately forming an intelligent fiber system integrating conductive sensing, photothermal response, and self-healing.
[0019] According to an embodiment of the present invention, in step (d), the airflow and melt dual-channel spinning technology refers to the use of a dual-component spinning system with an independent melt extrusion channel and a high-speed airflow traction channel. The melt extrusion channel is used to transport and extrude thermoplastic fiber components (such as polyethylene terephthalate hollow fibers and photothermal responsive liquid crystal elastomer fibers), while the high-speed airflow traction channel uses high-pressure nitrogen to uniformly disperse and traction regenerated chitosan fibers and graphene aerogel fibers. The two fiber streams converge, entangle, and solidify in a specific convergence area below the nozzle, thereby forming a structurally uniform ternary composite fiber.
[0020] According to an embodiment of the present invention, in step (e), the dynamic crosslinking agent solution is a colorless and transparent solution formed by mixing citric acid, chitosan, gelatin and dynamic covalent crosslinking agent in a mass ratio of 80:30:50:5-100:50:60:8, with a pH value of 4.5-5.5; The dynamic covalent crosslinking agent is a pale yellow viscous liquid formed by reacting phenylboronic acid and pentaerythritol at a mass ratio of 1:1.5-1:2.5 at 60-80°C for 1-3 hours.
[0021] According to an embodiment of the present invention, in step (e), a quaternary dynamic crosslinking system of citric acid, chitosan, gelatin, and borate esters was constructed, achieving reversible reconstruction of the fiber network through the synergistic effect of multiple bonds. The carboxyl groups of citric acid form ionic bonds with the amino groups of chitosan, the peptide chains of gelatin form hydrogen bonds with chitosan molecules, and the borate ester bonds formed by phenylboronic acid and pentaerythritol provide dynamic covalent crosslinking points. These three bonding mechanisms work synergistically under specific temperature conditions; the reversible breaking and rearrangement of the borate ester bonds, along with the dynamic reorganization of the hydrogen bond network, enables the crosslinked fiber bundles to maintain structural stability while possessing excellent self-healing properties, forming a flexible yet robust intelligent fiber network structure.
[0022] According to an embodiment of the present invention, in step (f), the composite dye solution is a composite solution formed by mixing photochromic spiropyran derivative, thermosensitive polyisopropylacrylamide, and pH-responsive dye in a mass ratio of 10:20:1-15:30:2. The photochromic spiropyran derivative is 1',3',3'-trimethyl-6-nitrospirocyclic [2H-1-benzopyran-2,2'-indoline], with a maximum absorption wavelength of 550-580 nm; the thermosensitive polyisopropylacrylamide has a low critical dissolution temperature of 32-34 °C; and the pH-responsive dye is either bromocresol green or bromocresol violet, with a color change range of 5.0-7.0.
[0023] According to an embodiment of the present invention, in step (f), a photochromic spiropyran derivative, a thermosensitive polyisopropylacrylamide, and a pH-responsive dye are combined in a ternary compound to construct a multidimensional intelligent color-changing system through their unique synergistic effect. The photochromic spiropyran derivative undergoes a reversible molecular structure transition under ultraviolet and visible light irradiation; the thermosensitive polyisopropylacrylamide achieves hydrophilic-hydrophobic conversion near its critical dissolution temperature; and the pH-responsive dye changes its color state according to changes in environmental acidity or alkalinity. These three intelligent materials promote each other during covalent grafting. The phase transition behavior of the thermosensitive polymer enhances the color-changing sensitivity of the spiropyran derivative, while the pH-responsive dye stabilizes the intermediate state during the color-changing process through intermolecular forces, ultimately forming an intelligent color-changing interface with triple-response characteristics on the fiber surface.
[0024] According to an embodiment of the present invention, in step (g), the working gas of the plasma processing chamber is a mixture of helium and oxygen in a volume ratio of 3:1-5:1, and the pressure inside the plasma processing chamber is maintained at 10-50 Pa; the nanoscale silica aerogel is a porous material obtained by reacting tetraethyl orthosilicate and anhydrous ethanol in a mass ratio of 1:5-1:8, with a specific surface area of 500-800 m² / g; the carbon nanotube array is a vertical array grown on a silicon substrate by chemical vapor deposition, with a diameter of 5-15 nm and a length of 10-50 μm.
[0025] According to an embodiment of the present invention, in step (g), the specific surface area of the nanoscale silica aerogel is measured with reference to GB / T19587-2017 "Determination of Specific Surface Area of Solid Substances by Gas Adsorption BET Method"; the diameter and length of the carbon nanotube array are measured with reference to GB / T 24491-2009 "Multi-walled Carbon Nanotubes" by scanning electron microscopy.
[0026] According to an embodiment of the present invention, in step (g), a multifunctional protective layer is constructed on the fiber surface by synergistic activation of nanoscale silica aerogel and carbon nanotube array using helium-oxygen mixed plasma. The active particles generated by the plasma cause molecular-level cross-linking between the porous structure of the silica aerogel and the vertical orientation of the carbon nanotube array, forming a three-dimensional network covering layer. The silica aerogel provides a superhydrophobic framework, while the carbon nanotube array is embedded within it to form a continuous conductive pathway. Under plasma activation, the two undergo interfacial chemical bonding, achieving a synergistic enhancement of surface microstructure stability and conductivity. Ultimately, this allows the blended yarn to simultaneously acquire switchable wetting characteristics and stable electrical signal transmission capabilities.
[0027] According to a second aspect of the present invention, a multi-component blended colored yarn prepared by the above method is provided, characterized in that the multi-component blended colored yarn has high environmental responsiveness, can generate intelligent color development response according to changes in external light, temperature and pH, and has excellent structural stability and self-healing ability. Its unique conductive network gives the product sensitive strain sensing characteristics, and its adjustable surface wettability makes it both protective and comfortable, forming a multifunctional textile integrating intelligent color changing, environmental sensing and structural self-adaptation.
[0028] According to embodiments of the present invention, the multi-component blended yarn is suitable for high-end smart clothing, medical and health monitoring, military camouflage and protection, and motion sensing equipment. It exhibits unique advantages, especially in situations requiring environmental adaptation, physiological signal monitoring and intelligent protection, providing innovative solutions for the development of next-generation smart textiles.
[0029] Multidimensional intelligent response mechanism: Through the synergistic effect of photochromic spiropyran, thermosensitive polymer and pH-responsive dye, a triple response to light, temperature and pH is achieved, enabling textiles to have intelligent color development capabilities that are environmentally adaptive.
[0030] Multi-fiber interface reconstruction technology: Innovatively using silk fibroin and soybean protein fiber with amphiphilic core-shell structure as interface regulation media, it effectively solves the interface compatibility problem between hydrophobic synthetic fibers and hydrophilic natural fibers, and significantly improves the structural stability of composite yarns.
[0031] Dynamic reversible crosslinking network: Based on the reversible properties of borate ester bonds, combined with the multiple effects of hydrogen bonds and ionic bonds, a dynamic crosslinking system with self-healing function is constructed, which enables the yarn to recover most of its mechanical properties after damage and significantly extend its service life.
[0032] Nanoscale functional synergistic construction: By using plasma activation technology, silica aerogel and carbon nanotube arrays are synergistically fixed onto the fiber surface, forming an intelligent interface that combines superhydrophobicity and conductivity, realizing the integrated integration of protective performance and sensing function.
[0033] Green and sustainable process system: It adopts bio-based raw materials and subcritical water extraction technology, combined with ultrasonic-assisted in-situ reduction process, which significantly reduces energy consumption and chemical reagent usage in the production process, reflecting the environmentally friendly manufacturing concept.
[0034] This invention not only makes fundamental innovations in fiber material combination and interface design, but also achieves intelligent response characteristics that are difficult for traditional textile materials to match through multi-scale synergistic effects; at the same time, the unique dynamic cross-linking network design and nano-functional modification process enable the product to achieve excellent durability and environmental adaptability while maintaining the texture of textiles.
[0035] The present invention has the following beneficial effects: It provides a multi-component blended colored yarn and its preparation method. Through innovative component design and process optimization, this method enables the product to simultaneously possess multiple functions such as intelligent color changing, environmental sensing, self-healing, and conductivity. This not only significantly enhances the added value of textiles but also expands their application prospects in high-end fields such as smart clothing, medical monitoring, and military protection, providing a new technological path for the development of smart textiles.
[0036] Of course, any product implementing this invention does not necessarily need to achieve all of the advantages described above at the same time. Attached Figure Description
[0037] Figure 1 This is a flowchart of the preparation method according to an embodiment of the present invention. Detailed Implementation
[0038] This application proposes a multi-component blended colored yarn and its preparation method, aiming to improve the intelligent response characteristics and functional integration of the yarn by introducing natural extract functional complexes, multi-fiber synergistic combination, dynamic reversible cross-linking networks, and other means.
[0039] Example 1
[0040] Preparation of compound extract: 100g of alpine blueberry peel and 30g of sea buckthorn pulp were extracted by subcritical hydrolysis to obtain compound extract; Preparation of functional complex: The above-mentioned composite extract was subjected to an in-situ reduction reaction with 8 g of graphene oxide and 3 g of silver nanowires under ultrasonic assistance. The power was 260 W, the frequency was 42 kHz, and the reaction time was 35 minutes to obtain the functional complex. Preparation of mixed fiber material: The above functional composite, 50 g of regenerated chitosan fiber, 40 g of polyethylene terephthalate hollow fiber, 30 g of carbon nanotube / silk fiber composite material, 12 g of graphene aerogel fiber, 8 g of photothermal responsive liquid crystal elastomer fiber and 5 g of interface reconstructed silk fibroin / soybean protein fiber were mixed to obtain mixed fiber material. Preparation of ternary composite fibers: The mixed fiber material was spun in a gradient under nitrogen protection using airflow and melt dual-channel spinning technology. The temperature gradient was set to 225℃, 205℃, and 185℃, and the pressure gradient was set to 0.9MPa, 0.6MPa, and 0.4MPa, respectively, to form ternary composite fibers. Preparation of reversible cross-linked fiber bundles: Ternary composite fibers were immersed in 100 g of dynamic cross-linking agent solution and cross-linked at 62 °C for 1.6 hours to obtain reversible cross-linked fiber bundles; Preparation of intelligent colored fiber: The reversible cross-linked fiber bundle was immersed in 30 g of composite dyeing solution and covalently grafted at 82 °C for 2.2 hours to obtain intelligent colored fiber; Modification and finishing: The surface of the smart colored fiber was modified in a plasma treatment chamber containing 60 grams of nano-sized silica aerogel and 15 grams of carbon nanotube array, with a power of 420W and a time of 190 seconds, to produce multi-component blended colored yarn.
[0041] Test data: yarn breaking strength 4.8 cN / dtex, conductivity 12 S / cm, UV shielding rate 99.2%, self-healing efficiency 92%, thermochromic response time 3.2 seconds, photochromic response time 8.5 seconds.
[0042] Example 2
[0043] Preparation of compound extract: 80g of alpine blueberry peel and 20g of sea buckthorn pulp were extracted by subcritical hydrolysis to obtain compound extract; Preparation of functional complex: The above-mentioned composite extract was subjected to an in-situ reduction reaction with 5 g of graphene oxide and 2 g of silver nanowires under ultrasonic assistance. The power was 240 W, the frequency was 38 kHz, and the reaction time was 25 minutes to obtain the functional complex. Preparation of mixed fiber material: The above functional composite, 40 g of regenerated chitosan fiber, 30 g of polyethylene terephthalate hollow fiber, 20 g of carbon nanotube / silk fiber composite material, 8 g of graphene aerogel fiber, 5 g of photothermal responsive liquid crystal elastomer fiber and 3 g of interface reconstructed silk fibroin / soybean protein fiber were mixed to obtain mixed fiber material. Preparation of ternary composite fibers: The mixed fiber material was spun in a gradient under nitrogen protection using airflow and melt dual-channel spinning technology. The temperature gradient was set to 215℃, 195℃, and 175℃, and the pressure gradient was set to 0.7MPa, 0.4MPa, and 0.2MPa, respectively, to form ternary composite fibers. Preparation of reversible cross-linked fiber bundles: Ternary composite fibers were immersed in 90 g of dynamic cross-linking agent solution and cross-linked at 58 °C for 1.4 hours to obtain reversible cross-linked fiber bundles; Preparation of intelligent colored fiber: The reversible cross-linked fiber bundle was immersed in 20 g of composite dye solution and covalently grafted at 78 °C for 1.8 hours to obtain intelligent colored fiber; Modification and finishing: The surface of the smart colored fiber was modified in a plasma treatment chamber containing 50 grams of nano-sized silica aerogel and 10 grams of carbon nanotube array, with a power of 380W and a time of 170 seconds, to produce multi-component blended colored yarn.
[0044] Test data: yarn breaking strength 4.2 cN / dtex, conductivity 8 S / cm, UV shielding rate 97.5%, self-healing efficiency 85%, thermochromic response time 5.1 seconds, photochromic response time 12.3 seconds.
[0045] Example 3
[0046] Preparation of compound extract: 90g of alpine blueberry peel and 25g of sea buckthorn pulp were extracted by subcritical hydrolysis to obtain compound extract; Preparation of functional complex: The above-mentioned composite extract was subjected to an in-situ reduction reaction with 6.5 g of graphene oxide and 2.5 g of silver nanowires under ultrasonic assistance. The power was 250 W, the frequency was 40 kHz, and the reaction time was 30 minutes to obtain the functional complex. Preparation of mixed fiber material: The above functional composite, 45 g of regenerated chitosan fiber, 35 g of polyethylene terephthalate hollow fiber, 25 g of carbon nanotube / silk fiber composite material, 10 g of graphene aerogel fiber, 6.5 g of photothermal responsive liquid crystal elastomer fiber and 4 g of interface reconstructed silk fibroin / soybean protein fiber were mixed to prepare mixed fiber material. Preparation of ternary composite fibers: The mixed fiber material was spun in a gradient under nitrogen protection using airflow and melt dual-channel spinning technology. The temperature gradient was set to 220℃, 200℃, and 180℃, and the pressure gradient was set to 0.8MPa, 0.5MPa, and 0.3MPa, respectively, to form ternary composite fibers. Preparation of reversible cross-linked fiber bundles: Ternary composite fibers were immersed in 95 g of dynamic cross-linking agent solution and cross-linked at 60 °C for 1.5 hours to obtain reversible cross-linked fiber bundles; Preparation of intelligent colored fiber: The reversible cross-linked fiber bundle was immersed in 25 g of composite dye solution and covalently grafted at 80 °C for 2 hours to obtain intelligent colored fiber. Modification and finishing: The surface of the smart colored fiber was modified in a plasma treatment chamber containing 55 grams of nano-sized silica aerogel and 12.5 grams of carbon nanotube array, with a power of 400W and a time of 180 seconds, to produce multi-component blended colored yarn.
[0047] Test data: yarn breaking strength 4.5 cN / dtex, conductivity 10 S / cm, UV shielding rate 98.6%, self-healing efficiency 89%, thermochromic response time 4.2 seconds, photochromic response time 10.1 seconds.
[0048] Example 4
[0049] Preparation of compound extract: 95g of alpine blueberry peel and 28g of sea buckthorn pulp were extracted by subcritical hydrolysis to obtain compound extract; Preparation of functional complex: The above-mentioned composite extract was subjected to an in-situ reduction reaction with 7 g of graphene oxide and 2.8 g of silver nanowires under ultrasonic assistance. The power was 255 W, the frequency was 41 kHz, and the reaction time was 33 minutes to obtain the functional complex. Preparation of mixed fiber material: The above-mentioned functional composite, 48 g of regenerated chitosan fiber, 38 g of polyethylene terephthalate hollow fiber, 28 g of carbon nanotube / silk fiber composite material, 11 g of graphene aerogel fiber, 7 g of photothermal responsive liquid crystal elastomer fiber and 4.5 g of interface reconstructed silk fibroin / soybean protein fiber were mixed to prepare the mixed fiber material. Preparation of ternary composite fibers: The mixed fiber material was spun in a gradient under nitrogen protection using airflow and melt dual-channel spinning technology. The temperature gradients were set to 222℃, 202℃, and 182℃, and the pressure gradients were set to 0.85MPa, 0.55MPa, and 0.35MPa, respectively, to form ternary composite fibers. Preparation of reversible cross-linked fiber bundles: Ternary composite fibers were immersed in 98 g of dynamic cross-linking agent solution and cross-linked at 61 °C for 1.55 h to obtain reversible cross-linked fiber bundles; Preparation of intelligent colored fiber: The reversible cross-linked fiber bundle was immersed in 28 g of composite dyeing solution and covalently grafted at 81 °C for 2.1 hours to obtain intelligent colored fiber; Modification and finishing: The surface of the smart colored fiber was modified in a plasma treatment chamber containing 58 grams of nano-sized silica aerogel and 14 grams of carbon nanotube array, with a power of 410W and a time of 185 seconds, to produce multi-component blended colored yarn.
[0050] Test data: yarn breaking strength 4.7 cN / dtex, conductivity 11 S / cm, UV shielding rate 98.9%, self-healing efficiency 91%, thermochromic response time 3.8 seconds, photochromic response time 9.2 seconds.
[0051] Comparative Example 1 (Traditional Blending Process)
[0052] Colored yarn is prepared using a traditional blending process, with specific steps following the method described in existing technology CN 110592790 A. Ordinary cotton fiber, polyester fiber, and acrylic fiber are mixed in the same proportion and then processed into colored yarn using a traditional spinning process.
[0053] Test data: Breaking strength of colored yarn: 3.1 cN / dtex Conductivity: 0.01 S / cm UV shielding rate: 65.3% Self-repair efficiency: 0% It lacks thermochromic and photochromic functions.
[0054] Comparative Example 2 (Single Fiber Preparation Process)
[0055] The method for preparing colored yarn using single-functional fibers is as follows: graphene composite conductive fibers are prepared by referring to the method in the existing technology CN 109072484 A. Then, the graphene composite conductive fibers, polyester staple fibers and cotton fibers are blended and spun together, and then colored yarn is made by traditional impregnation dyeing method.
[0056] Test data: Breaking strength of colored yarn: 3.8 cN / dtex Conductivity: 5S / cm UV shielding rate: 85.6% Self-repair efficiency: 0% No thermochromic response time, no photochromic response time.
[0057] In the above embodiments and comparative examples, the breaking strength of the colored yarn was determined according to GB / T 3916-2013 "Determination of breaking strength and elongation at break of single yarn in packaged textiles"; the conductivity was determined according to GB / T 15738-2008 "Test method for resistivity of conductive and antistatic fibers"; the ultraviolet shielding rate was determined according to GB / T 18830-2009 "Evaluation of UV protection performance of textiles"; the self-healing efficiency was measured by a tensile testing machine; the thermochromic response time was measured according to "T / CNTAC 45-2020 Detection and evaluation of thermochromic properties of textiles"; and the photochromic response time was recorded by a high-speed camera under 365nm ultraviolet light source irradiation, taking the time required for complete color change.
[0058] Comparative analysis
[0059] By comparing the test data of multi-component blended colored yarns prepared by different methods, it can be seen that the preparation process provided by this invention has significant advantages: Improved mechanical properties: The fracture strength of all embodiments reached over 4.2 cN / dtex, which is far higher than the traditional method in the comparative example; Excellent electrical conductivity: The colored yarn prepared by the method of this invention has a conductivity of 8-12 S / cm, while the product prepared by the comparative method has poor electrical conductivity. High functional integration: The product of this invention has multiple functions such as ultraviolet shielding, self-healing, thermochromic and photochromic, while the comparative product has only one function. Excellent response performance: The response time of thermochromic and photochromic products is significantly better than that of the comparative product.
[0060] Although preferred embodiments of the invention have been described, those skilled in the art, upon learning the basic inventive concept, can make other changes and modifications to these embodiments. Therefore, the appended claims are intended to be interpreted as including both the preferred embodiments and all changes and modifications falling within the scope of the invention.
[0061] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.
Claims
1. A method for preparing a multi-component blended colored yarn, characterized in that, Includes the following steps: (a) Preparation of compound extract: 80-100 parts of alpine blueberry peel and 20-30 parts of sea buckthorn pulp were extracted by subcritical hydrolysis to obtain a compound extract rich in anthocyanins, pectin and sea buckthorn flavonoids; (b) Preparation of functional complex: The composite extract prepared in step (a) is subjected to an in-situ reduction reaction with 5-8 parts of graphene oxide and 2-3 parts of silver nanowires under ultrasonic assistance. The power is 240-260W, the frequency is 38-42kHz, and the reaction time is 25-35min to obtain the functional complex. (c) Preparation of the mixed fiber material: The functional composite prepared in step (b), 40-50 parts of regenerated chitosan fiber, 30-40 parts of polyethylene terephthalate hollow fiber, 20-30 parts of carbon nanotube / silk fiber composite material, 8-12 parts of graphene aerogel fiber, 5-8 parts of photothermal responsive liquid crystal elastomer fiber and 3-5 parts of interface remodeling silk fibroin / soybean protein fiber are mixed to obtain the mixed fiber material; (d) Preparation of ternary composite fibers: Using airflow and melt spinning dual-channel technology, the mixed fiber material prepared in step (c) is subjected to gradient spinning under nitrogen protection. The temperature gradients are set to 215-225℃, 195-205℃, and 175-185℃, and the pressure gradients are set to 0.7-0.9MPa, 0.4-0.6MPa, and 0.2-0.4MPa, respectively, to form the ternary composite fibers; (e) Preparation of reversible cross-linked fiber bundles: The ternary composite fiber prepared in step (d) is immersed in 90-100 parts of dynamic cross-linking agent solution and cross-linked at 58-62°C for 1.4-1.6 hours to obtain the reversible cross-linked fiber bundles; (f) Preparation of intelligent colored fiber: The reversible cross-linked fiber bundle prepared in step (e) is immersed in 20-30 parts of composite dyeing solution and subjected to covalent grafting reaction at 78-82℃ for 1.8-2.2 hours to obtain the intelligent colored fiber; (g) Modification and finishing: The smart colored fiber prepared in step (f) is surface modified in a plasma treatment chamber containing 50-60 parts of nano-sized silica aerogel and 10-15 parts of carbon nanotube array, with a power of 380-420W and a time of 170-190s, to obtain the multi-component blended colored yarn.
2. The preparation method according to claim 1, characterized in that: In step (a), the subcritical hydrolysis extraction uses ultrapure water as the solvent, the mass ratio of the alpine blueberry peel, the sea buckthorn pulp and the ultrapure water is 1:1:15-1:1:20, the extraction temperature is 110-130℃, the pressure is 0.3-0.5MPa and the time is 30-45 minutes.
3. The preparation method according to claim 1, characterized in that: In step (b), the graphene oxide is a yellow sheet-like solid material obtained by mixing natural flake graphite and potassium permanganate at a mass ratio of 1:3-1:5 and reacting for 4-6 hours, washing with deionized water until neutral, and then ultrasonically exfoliating. The sheet diameter is 1-5 μm and the thickness is 0.8-1.2 nm. The silver nanowires are silver-white linear materials formed by dissolving silver nitrate and polyvinylpyrrolidone at a mass ratio of 1:1-1:3 in ethylene glycol and reducing them at 160-180°C for 2-4 hours. The silver nanowires have a diameter of 50-100 nm and a length of 10-20 μm.
4. The preparation method according to claim 1, characterized in that: In step (c), the regenerated chitosan fiber is a white fiber filament produced by dissolving chitosan in an acetic acid solution with a mass fraction of 2-4%, spinning it, and then cross-linking it with γ-irradiation. The irradiation dose is 45-55 kGy, and the degree of cross-linking is ≥85%. The polyethylene terephthalate hollow fiber is a hollow filament produced by melt spinning polyethylene terephthalate and potassium titanate whiskers at a mass ratio of 100:1.5-100:2.5, with a hollowness of 35%-45%. The carbon nanotube / silk fiber composite material is a composite filament made by plasma etching of carbon nanotubes and silk fibers in a mass ratio of 3:100-5:
100. The etching gas is argon, the etching power is 280-320W, and the time is 110-130s. The graphene aerogel fiber is a black filament produced by wet spinning and thermal reduction of graphene oxide solution, with a specific surface area of 500-800 m² / g and a pore size distribution of 2-50 nm. The photothermal responsive liquid crystal elastomer fiber is formed by mixing aromatic liquid crystal monomers with a mesocrystalline content of 30%-40% and a hydrogen-containing silicone oil crosslinking agent at a mass ratio of 10:1-10:2, adding 0.5%-1% photothermal conversion agent, melt spinning at 180-200℃, and then orientation and setting at 80-100℃ for 2-4 hours to form a yellow elastic fiber with photoinduced deformation effect. The glass transition temperature is 45-50℃, and the near-infrared light absorption rate is ≥90%. The interface-reconstructed silk fibroin / soybean protein fiber is a white ultrafine fiber with an amphiphilic core-shell structure, formed by electrospinning silk fibroin and soybean protein at a mass ratio of 2:1-3:1, with a diameter of 8-15 μm. The silk fibroin forms a hydrophobic core layer, and the soybean protein forms a hydrophilic shell layer.
5. The preparation method according to claim 1, characterized in that: In step (e), the dynamic crosslinking agent solution is a colorless and transparent solution composed of citric acid, chitosan, gelatin and dynamic covalent crosslinking agent in a mass ratio of 80:30:50:5-100:50:60:8, with a pH value of 4.5-5.
5. The dynamic covalent crosslinking agent is a pale yellow viscous liquid formed by reacting phenylboronic acid and pentaerythritol at a mass ratio of 1:1.5-1:2.5 at 60-80°C for 1-3 hours.
6. The preparation method according to claim 1, characterized in that: In step (f), the composite dye solution is a complex solution composed of photochromic spiropyran derivative, thermosensitive polyisopropylacrylamide, and pH-responsive dye in a mass ratio of 10:20:1-15:30:
2. The photochromic spiropyran derivative is 1',3',3'-trimethyl-6-nitrospirocyclic [2H-1-benzopyran-2,2'-indoline], with a maximum absorption wavelength of 550-580 nm; the thermosensitive polyisopropylacrylamide has a low critical dissolution temperature of 32-34 °C; and the pH-responsive dye is either bromocresol green or bromocresol violet, with a color change range of 5.0-7.
0.
7. The preparation method according to claim 1, characterized in that: In step (g), the working gas of the plasma processing chamber is a mixture of helium and oxygen in a volume ratio of 3:1 to 5:1, and the pressure inside the plasma processing chamber is maintained at 10-50 Pa. The nanoscale silica aerogel is a porous material obtained by reacting tetraethyl orthosilicate and anhydrous ethanol in a mass ratio of 1:5 to 1:8, with a specific surface area of 500-800 m² / g. The carbon nanotube array is a vertical array grown on a silicon substrate by chemical vapor deposition, with a diameter of 5-15 nm and a length of 10-50 μm.
8. A multi-component blended colored yarn prepared by the preparation method according to any one of claims 1 to 7.
9. The multi-component blended colored yarn according to claim 8, characterized in that, The volume resistivity of the multi-component blended colored yarn is 10³⁻¹. Ω·cm, water contact angle >120° above 35°C, water contact angle <30° below 25°C, can recover 85%-95% of the initial strength after tearing, piezoresistive coefficient 0.020-0.030Ω·cm / N.
10. The application of the multi-component blended yarn according to claim 8 in intelligent temperature-regulating clothing, medical monitoring textiles, military camouflage equipment, or motion sensing devices.
Citation Information
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