Wool-based antibacterial warm-keeping high-strength flame-retardant yarn and preparation method thereof

Abstract

The invention belongs to the technical field of textiles, and provides a wool-based antibacterial warm-keeping high-strength flame-retardant yarn and a preparation method thereof. The preparation method comprises the following steps: firstly, preparing a bifunctional cross-linking agent containing a phosphorus-nitrogen flame-retardant unit and a terminal alkynyl functional group, and independently preparing a sericin graft modified chitosan derivative as a biological interface lubricant through an enzymatic reaction; the method comprises the following steps: carrying out chemical reduction treatment on wool fibers, and generating an inorganic functional network taking phytic acid metal salt as a main body in situ in the activated fibers; covalently grafting the bifunctional cross-linking agent onto a thiol group of wool keratin by utilizing a photo-initiated thiol-alkyne click chemical reaction to form a three-dimensional organic covalent network penetrating through a fiber matrix; and finally, the surfaces of the fibers are finished by a biological interface lubricant, and the prepared yarn has excellent antibacterial activity, heat retention property, high strength and flame retardance at the same time.

Description

Technical Field

[0001] This invention belongs to the field of textile technology and relates to wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. Background Technology

[0002] The inherent structure and chemical composition of wool fibers result in some inherent performance defects, affecting their application in certain high-performance and functional fields. Firstly, wool fibers have relatively low mechanical properties, especially in wet conditions, where their strength and abrasion resistance are inferior to cotton, linen, and most synthetic fibers. To address this, traditional methods often involve blending wool with high-strength synthetic fibers (such as nylon and polyester), but this sacrifices wool's natural characteristics, biodegradability, and unique feel and comfort to some extent. Secondly, existing wool flame-retardant technologies primarily rely on finishing processes, such as treatment with flame retardants containing halogens, phosphorus, nitrogen, or metal hydroxides. However, halogenated flame retardants release toxic dioxins and corrosive gases during combustion; traditional phosphorus-nitrogen flame retardants are often applied to the fiber surface through single-step padding and baking, resulting in weak bonding with the fiber, poor wash resistance, and easy loss of functionality; while metal hydroxide flame retardants require extremely high dosages to achieve the desired effect, which affects the fabric's hand feel, drape, and wearing comfort.

[0003] Furthermore, wool keratin is rich in nutrients and easily breeds bacteria and microorganisms in hot and humid environments, which can not only produce odors but also pose a threat to human health. Traditional antibacterial finishing methods often use silver ions / nano silver, quaternary ammonium salts, or organic antibacterial agents. These methods also suffer from insufficient functional durability, as antibacterial agents are largely washed away after repeated washing. Summary of the Invention

[0004] To address the shortcomings of existing technologies, the present invention aims to provide a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. This involves chemically activating and in-situ mineralizing wool to construct an inorganic network, followed by using click chemistry to covalently bond a self-made multifunctional crosslinking agent, forming an organic-inorganic interpenetrating network. The resulting yarn possesses excellent high strength, flame retardancy, and antibacterial properties, thus meeting the needs of practical production.

[0005] To achieve this objective, the present invention adopts the following technical solution: In a first aspect, the present invention provides a method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn, the method comprising: S1, L-lysine and ammonium bicarbonate are dispersed in deionized water, and 3-bromopropyne is added to react and give crude N,N-di-di-propylated lysine. Phosphorus oxychloride is dispersed in anhydrous acetonitrile, and an acetonitrile solution of aminoethanol is added to react and give a cyclic phosphoramide flame retardant. Crude N,N-di-di-propylated lysine and the cyclic phosphoramide flame retardant are dispersed in anhydrous dimethylformamide, and N,N'-dicyclohexylcarbodiimide and N-hydroxysuccinimide are added to give a di-propylated phosphoramide crosslinking agent. S2, carboxymethyl chitosan and sericin are dispersed in phosphate buffer to obtain a substrate solution. Glutamine transaminase is added to the substrate solution to react. After the reaction is completed, the mixture is transferred to a dialysis bag for dialysis to obtain a biointerface lubricant. S3, L-cysteine ​​methyl ester hydrochloride is dispersed in deionized water, the pH is adjusted to 8-9, wool is immersed in deionized water to react, and pretreated wool is obtained. The pretreated wool is immersed in phytic acid permeate solution, and immediately after immersion, it is immersed in arginine-zinc chelate mineralization solution to obtain mineralized wool. S4, a diacetylphosphamide crosslinking agent and a photoinitiator are dispersed in a tert-butanol / water mixed solvent. The mineralized wool is immersed in the tert-butanol / water mixed solvent and irradiated with a UV lamp to obtain functionalized wool. A bio-interface lubricant is dispersed in deionized water to obtain a finishing working solution. The functionalized wool is immersed in the finishing working solution to obtain liquid-containing wool and undergoes a two-stage heat treatment. After drawing, roving, and spinning processes, wool-based antibacterial, warm, high-strength, and flame-retardant yarn is obtained.

[0006] Specifically, it includes: A1. Phytic acid is dispersed in deionized water to obtain phytic acid permeate. L-arginine and zinc sulfate heptahydrate are dispersed sequentially in deionized water, and the pH is adjusted to 6.8-7.2 to obtain arginine-zinc chelate mineralization solution. S1, L-lysine and ammonium bicarbonate were dispersed in deionized water, and 3-bromopropyne was added under ice-water bath conditions. The reaction was carried out at room temperature with stirring in the dark to obtain crude N,N-di-di-propyne. Under nitrogen range, phosphorus oxychloride was dispersed in anhydrous acetonitrile, and an acetonitrile solution of aminoethanol was added under ice-water bath conditions. The temperature was adjusted to the first temperature and refluxed to obtain a cyclic phosphoramide flame retardant. Crude N,N-di-di-propyne and the cyclic phosphoramide flame retardant were dispersed in anhydrous dimethylformamide, and N,N'-dicyclohexylcarbodiimide and N-hydroxysuccinimide were added under ice-water bath conditions and mixed evenly. The reaction was carried out with stirring at room temperature. After the reaction was completed, the mixture was filtered, rotary evaporated, and purified to obtain a di-propyne phosphoramide crosslinking agent. S2, carboxymethyl chitosan and sericin are dispersed in phosphate buffer, the temperature is adjusted to the second temperature and stirred in a water bath to obtain a substrate solution, glutamine transaminase is added to the substrate solution and the reaction is continued to be stirred at the second temperature, after the reaction is completed, the temperature is raised to inactivate, the reaction solution is inactivated and cooled and then transferred to a dialysis bag, and the dialysis bag is placed in deionized water for dialysis, and the dialysis reaction solution is freeze-dried to obtain a bio-interface lubricant; S3, L-cysteine ​​methyl ester hydrochloride is dispersed in deionized water and the pH is adjusted to 8-9 using sodium carbonate solution. Wool is then immersed in deionized water and stirred at a third temperature. After the reaction is complete, the wool is washed and spun dry to obtain pretreated wool. The pretreated wool is then immersed in phytic acid permeate solution and subjected to three vacuum-atmospheric pressure cycles. It is then soaked at atmospheric pressure. After soaking, the residual rate is controlled, and the wool is immediately immersed in arginine-zinc chelate mineralization solution at room temperature. After washing and drying, the mineralized wool is obtained. S4. The diacetylphosphamide crosslinking agent and photoinitiator are dispersed in a tert-butanol / water mixed solvent. The mineralized wool is then immersed in the tert-butanol / water mixed solvent and irradiated with a UV lamp. After irradiation, the wool is thoroughly washed and dried to obtain functionalized wool. The bio-interface lubricant is dispersed in deionized water to obtain a finishing working solution. The functionalized wool is then immersed in the finishing working solution to obtain liquid-containing wool and subjected to a two-stage heat treatment. After natural cooling, the wool is processed through drawing, roving, and spinning to obtain wool-based antibacterial, warm, high-strength, and flame-retardant yarn.

[0007] Phytic acid, as a multidentate organophosphate compound, contains multiple phosphate groups in its molecular structure, making it both a phosphorus source for subsequent inorganic phase formation and possessing excellent metal ion chelating ability. The chemical mechanism for preparing the arginine-zinc chelate mineralization solution lies in utilizing the side-chain functional groups of L-arginine (such as guanidinyl and amino groups) as ligands to form stable coordination compounds with divalent zinc ions in zinc sulfate. In step S1, using L-lysine as a raw material, under alkaline conditions, its α- and ε-amino groups act as nucleophiles to undergo a nucleophilic substitution reaction with 3-bromopropyne to generate N,N'-diacetylacetyllysine. This product molecule introduces two terminal alkynyl functional groups. Through the condensation reaction of phosphorus oxychloride and aminoethanol, a cyclic phosphoramide structure containing phosphorus-nitrogen bonds is constructed. This structure is the pre-designed flame-retardant functional unit. Finally, a coupling reaction mediated by N,N'-dicyclohexylcarbodiimide and N-hydroxysuccinimide was used to activate the carboxyl group of N,N'-dipropynyllysine into an NHS active ester. This active ester then reacts with the nucleophilic site on the cyclic phosphoramide flame retardant to form a stable amide bond, covalently linking the flame retardant functional unit to the carboxyl group of the dipropynyllysine backbone, providing a material basis for the subsequent introduction of high strength and high flame retardancy.

[0008] Step S2 prepared a bio-interface lubricant, the chemical mechanism of which is enzyme-catalyzed graft copolymerization. Utilizing the high specificity of glutamine transaminase, it catalyzes the formation of isopeptide bonds between the γ-amide groups of glutamine residues in the sericin molecular chain and the primary amino groups in the carboxymethyl chitosan molecular chain. This enzymatic reaction generates a stable graft copolymer covalently linked by two biopolymers. Step S3 first involves reducing the wool. Under weakly alkaline conditions, L-cysteine ​​methyl ester hydrochloride acts as a reducing agent, converting some of the cross-linking disulfide bonds in wool keratin into highly nucleophilic free thiol groups through a thiol-disulfide bond exchange reaction. This pre-sets numerous covalent anchoring sites for the click chemistry reaction in step S4. Simultaneously, the breaking of disulfide bonds loosens the supramolecular structure of keratin, increasing the porosity within the fiber. Subsequently, in-situ mineralization is performed, using vacuum permeation to efficiently transport and adsorb phytic acid molecules onto the protein network within the fiber. Following this, the fiber is immersed in a zinc ion solution chelated with arginine. Because the fiber interior is enriched with phytate anions, zinc ions slowly dissociating from the chelate preferentially react with phytate inside the fiber to form nano-sized zinc phytate particles. Arginine acts as a reaction rate regulator here, controlling the concentration of free zinc ions through dynamic coordination equilibrium, thereby inhibiting the rapid, random deposition of particles on the fiber surface and achieving a uniform construction of the inorganic functional phase within the fiber.

[0009] Mineralized wool is immersed in a solution containing a diacetylphosphamide crosslinking agent and a photoinitiator. Under ultraviolet radiation, the photoinitiator decomposes to generate active free radicals, which then initiate a thiol-acetylene click chemical reaction. The thiol groups on the wool keratin react with the acetyl groups of the crosslinking agent via free radical addition. Since the crosslinking agent molecule contains two acetyl groups, it can react with different keratin molecular chains, thereby forming a three-dimensional covalent crosslinked network throughout the fiber matrix. This network fixes the phosphorus and nitrogen flame-retardant functional units with covalent bonds, while physically embedding the in-situ generated inorganic phase, forming an organic-inorganic interpenetrating network structure. Finally, the bio-interface lubricant prepared in step S2 is applied to the fiber surface through a pad-bake process. High-temperature conditions promote esterification or amidation reactions between the finishing agent and the functional groups on the fiber surface, forming a durable finishing layer.

[0010] As a preferred embodiment of the present invention, in A1, the mass fraction of the phytic acid permeate is 3-8 wt.%, for example, it can be 3.0 wt.%, 3.5 wt.%, 4.0 wt.%, 4.5 wt.%, 5.0 wt.%, 5.5 wt.%, 6.0 wt.%, 6.5 wt.%, 7.0 wt.%, 7.5 wt.% or 8.0 wt.%, but it is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0011] In some optional embodiments, the mass ratio of L-arginine, zinc sulfate heptahydrate, and deionized water is (28-42):(23-34.5):800, for example, it can be (28, 29.4, 30.8, 32.2, 33.6, 35.0, 36.4, 37.8, 39.2, 40.6, or 42):(23, 24.15, 25.3, 26.45, 27.6, 28.75, 29.9, 31.05, 32.2, 33.35, or 34.5):800, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0012] As a preferred embodiment of the present invention, in S1, the mass-to-volume ratio of L-lysine, ammonium bicarbonate, deionized water, and 3-bromopropyne is (14-15) g : (21-25) g : (450-550) mL : (25-26.8) g, for example, it can be (14.0, 14.1, 14.2, 14.3, 14.4, 14.5, 14.6, 14.7, 14.8, 14.9 or 15.0) g : (21, 21.4, 21.8, 22.2, 22. 6, 23.0, 23.4, 23.8, 24.2, 24.6 or 25) g; (450, 460, 470, 480, 490, 500, 510, 520, 530, 540 or 550) mL; (25, 25.18, 25.36, 25.54, 25.72, 25.9, 26.08, 26.26, 26.44, 26.62 or 26.8) g, but not limited to the listed values, other unlisted values ​​within this range also apply.

[0013] In some optional embodiments, the time for the light-protected stirring reaction is 20-30 hours, for example, 20 hours, 21 hours, 22 hours, 23 hours, 24 hours, 25 hours, 26 hours, 27 hours, 28 hours, 29 hours or 30 hours, but is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0014] In some optional embodiments, the mass-to-volume ratio of the phosphorus oxychloride, anhydrous acetonitrile, and aminoethanol acetonitrile solution is (15-16) g : (180-220) mL : (6-7) g, for example, it can be (15.0, 15.1, 15.2, 15.3, 15.4, 15.5, 15.6, 15.7, 15.8, 15.9, or 16.0) g : (180, 184, 188, 192, 196, 200, 204, 208, 212, 216, or 220) mL : (6.0, 6.1, 6.2, 6.3, 6.4, 6.5, 6.6, 6.7, 6.8, 6.9, or 7.0) g, but is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0015] In some optional embodiments, the concentration of the aminoethanol acetonitrile solution is 2M.

[0016] In some alternative embodiments, the first temperature is 75-85°C, for example, it can be 75°C, 76°C, 77°C, 78°C, 79°C, 80°C, 81°C, 82°C, 83°C, 84°C or 85°C, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0017] In some optional embodiments, the first temperature reflux reaction time is 4-6 hours, for example, 4.0 hours, 4.2 hours, 4.4 hours, 4.6 hours, 4.8 hours, 5.0 hours, 5.2 hours, 5.4 hours, 5.6 hours, 5.8 hours, or 6.0 hours, but is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0018] In some optional embodiments, the mass-to-volume ratio of the crude N,N-dipropyne lysine, cyclic phosphoramide flame retardant, anhydrous dimethylformamide, N,N'-dicyclohexylcarbodiimide, and N-hydroxysuccinimide is (18-20) g : (9.5-10.7) g : (280-320) mL : (18.2-24) g : (9.2-11.3) g, for example, it can be (18.0, 18.2, 18.4, 18.6, 18.8, 19.0, 19.2, 19.4, 19.6, 19.8, or 20.0) g : (9.5, 9.62, 9.74, 9.86, 9.98, 10.1, 10.22, 1 0.34, 10.46, 10.58 or 10.7) g; (280, 284, 288, 292, 296, 300, 304, 308, 312, 316 or 320) mL; (18.2, 18.78, 19.36, 19.94, 20.52, 21.1, 21.68, 22.26, 22.84, 23.42 or 24) g; (9.2, 9.41, 9.62, 9.83, 10.04, 10.25, 10.46, 10.67, 10.88, 11.09 or 11.3) g, but not limited to the listed values, other unlisted values ​​within this range also apply.

[0019] In some optional embodiments, the stirring reaction time at room temperature is 40-50 h, for example, it can be 40 h, 41 h, 42 h, 43 h, 44 h, 45 h, 46 h, 47 h, 48 h, 49 h or 50 h, but is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0020] In a preferred embodiment of the present invention, in step S2, the mass-to-volume ratio of carboxymethyl chitosan, sericin, phosphate buffer, and transglutaminase is (10-12) g : (4-6) g : (800-1000) mL : (0.03-0.075) g, for example, it can be (10.0, 10.2, 10.4, 10.6, 10.8, 11.0, 11.2, 11.4, 11.6, 11.8, or 12.0) g : (4.0, 4.2, 4.4, 4.6, 4.8) g. 5.0, 5.2, 5.4, 5.6, 5.8 or 6.0) g; (800, 820, 840, 860, 880, 900, 920, 940, 960, 980 or 1000) mL; (0.03, 0.0345, 0.039, 0.0435, 0.048, 0.0525, 0.057, 0.0615, 0.066, 0.0705 or 0.075) g, but not limited to the listed values, other unlisted values ​​within this range also apply.

[0021] In some alternative embodiments, the pH of the phosphate buffer solution is 6.8-7.2, for example, pH 6.8, 6.9, 7.0, 7.1 or 7.2, but is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0022] In some alternative embodiments, the second temperature is 45-55°C, for example, it can be 45°C, 46°C, 47°C, 48°C, 49°C, 50°C, 51°C, 52°C, 53°C, 54°C or 55°C, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0023] In some optional embodiments, the stirring time in the second temperature water bath is 0.5-1h, for example, it can be 0.5h, 0.55h, 0.6h, 0.65h, 0.7h, 0.75h, 0.8h, 0.85h, 0.9h, 0.95h or 1.0h, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0024] In some optional embodiments, the activity of the transglutaminase is >100 U / g.

[0025] In some optional embodiments, the stirring reaction time at the second temperature is 5-8 hours, for example, 5.0 hours, 5.3 hours, 5.6 hours, 5.9 hours, 6.2 hours, 6.5 hours, 6.8 hours, 7.1 hours, 7.4 hours, 7.7 hours or 8.0 hours, but is not limited to the listed values. Other unlisted values ​​within this range are also applicable.

[0026] In some optional embodiments, the molecular weight cutoff of the dialysis bag is 3500-5000 Da, for example, it can be 3500 Da, 3650 Da, 3800 Da, 3950 Da, 4100 Da, 4250 Da, 4400 Da, 4550 Da, 4700 Da, 4850 Da or 5000 Da, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0027] In some optional embodiments, the dialysis step involves placing the dialysis bag in deionized water and performing dialysis at 4-10°C for 72 hours, changing the deionized water every 8 hours. For example, it could be: placing the dialysis bag in deionized water and performing dialysis at (4.0, 4.6, 5.2, 5.8, 6.4, 7.0, 7.6, 8.2, 8.8, 9.4, or 10.0)°C for 72 hours, changing the deionized water every 8 hours. However, this is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0028] As a preferred technical solution of the present invention, in S3, the mass ratio of L-cysteine ​​methyl ester hydrochloride, deionized water and wool is (3-8):(2500-3500):100, for example, it can be (3.0, 3.5, 4.0, 4.5, 5.0, 5.5, 6.0, 6.5, 7.0, 7.5 or 8.0):(2500, 2600, 2700, 2800, 2900, 3000, 3100, 3200, 3300, 3400 or 3500):100, but it is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0029] In some optional embodiments, the sodium carbonate solution has a mass fraction of 10 wt.%.

[0030] In some alternative embodiments, the wool is wool that has undergone a scouring and combing process.

[0031] In some alternative embodiments, the third temperature is 25-35°C, for example, it can be 25°C, 26°C, 27°C, 28°C, 29°C, 30°C, 31°C, 32°C, 33°C, 34°C or 35°C, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0032] In some optional embodiments, the stirring reaction time at the third temperature is 1.5-3 hours, for example, 1.5 hours, 1.65 hours, 1.8 hours, 1.95 hours, 2.1 hours, 2.25 hours, 2.4 hours, 2.55 hours, 2.7 hours, 2.85 hours, or 3.0 hours, but is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0033] In some alternative embodiments, the pre-treated wool has a pulverization rate of 80-90%, for example, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, or 90%, but is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0034] In some optional embodiments, the soaking time under normal pressure is 0.8-1.5 h, for example, it can be 0.8 h, 0.87 h, 0.94 h, 1.01 h, 1.08 h, 1.15 h, 1.22 h, 1.29 h, 1.36 h, 1.43 h or 1.5 h, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0035] In some optional embodiments, the controlled residual rate after soaking is 90-110%, for example, it can be 90%, 92%, 94%, 96%, 98%, 100%, 102%, 104%, 106%, 108% or 110%, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0036] In some optional embodiments, the soaking time at room temperature is 3-5 hours, for example, 3.0 hours, 3.2 hours, 3.4 hours, 3.6 hours, 3.8 hours, 4.0 hours, 4.2 hours, 4.4 hours, 4.6 hours, 4.8 hours, or 5.0 hours, but is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0037] As a preferred technical solution of the present invention, in S4, the mass ratio of the diacetylenic phosphoramide crosslinking agent, photoinitiator, tert-butanol / water mixed solvent to the mineralized wool is (10-20):(0.2-1):(2500-3500):100, for example, it can be (10, 11, 12, 13, 14, 15, 16, 17, 18, 19 or 20):(0.2, 0.28, 0.36, 0.44, 0.52, 0.6, 0.68, 0.76, 0.84, 0.92 or 1):(2500, 2600, 2700, 2800, 2900, 3000, 3100, 3200, 3300, 3400 or 3500):100, but it is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0038] In some optional embodiments, the photoinitiator is photoinitiator 2959.

[0039] In some optional embodiments, the volume ratio of tert-butanol to water in the tert-butanol / water mixed solvent is 6:4.

[0040] In some optional embodiments, the power of the ultraviolet lamp is 400-600W, the distance between the ultraviolet lamp and the surface of the tert-butanol / water mixed solvent is 15-25cm, the irradiation time is 15-30min, and the wool is turned over every 5 minutes during the irradiation. For example, the power can be (400, 420, 440, 460, 480, 500, 520, 540, 560, 580 or 600)W, and the ultraviolet lamp and tert-butanol... The distance between the water-mixed solvent surface and the target liquid level is (15, 16, 17, 18, 19, 20, 21, 22, 23, 24 or 25) cm, and the irradiation time is (15, 16.5, 18, 19.5, 21, 22.5, 24, 25.5, 27, 28.5 or 30) min. During the irradiation, the wool should be turned over every 5 minutes, but this is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0041] In some optional embodiments, the concentration of the finishing working solution is 1-3 g / L, for example, it can be 1.0 g / L, 1.2 g / L, 1.4 g / L, 1.6 g / L, 1.8 g / L, 2.0 g / L, 2.2 g / L, 2.4 g / L, 2.6 g / L, 2.8 g / L or 3.0 g / L, but is not limited to the listed values, other unlisted values ​​within this range are also applicable.

[0042] In some alternative embodiments, the residual rate of the liquid-containing wool is 80-90%, for example, it can be 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89% or 90%, but is not limited to the listed values, and other unlisted values ​​within this range are also applicable.

[0043] In some optional embodiments, the two-stage heat treatment is as follows: treatment at 75-85°C for 8-12 minutes, followed by baking at 125-140°C for 2-3 minutes. For example, it could be: treating at (75, 76, 77, 78, 79, 80, 81, 82, 83, 84 or 85) °C for (8.0, 8.4, 8.8, 9.2, 9.6, 10.0, 10.4, 10.8, 11.2, 11.6 or 12.0) min, and then baking at (125, 126.5, 128, 129.5, 131, 132.5, 134, 135.5, 137, 138.5 or 140) °C for (2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9 or 3.0) min, but it is not limited to the listed values; other unlisted values ​​within this range are also applicable.

[0044] In a second aspect, the present invention provides a wool-based antibacterial, warm, high-strength, flame-retardant yarn prepared by the preparation method described in the first aspect.

[0045] Compared with the prior art, the beneficial effects of the present invention are as follows: by chemically activating wool, an inorganic functional network is generated in situ inside the fiber, and then click chemistry is used to covalently bond a self-designed multifunctional crosslinking agent to construct an organic network that interpenetrates with the inorganic network. Through stable covalent bonds, mechanical reinforcement, flame retardancy and antibacterial functions are deeply embedded in the fiber matrix, giving the yarn high strength, high efficiency flame retardancy and broad-spectrum antibacterial properties. Detailed Implementation

[0046] The technical solution of the present invention will be described in detail below with reference to specific embodiments. The embodiments described herein are specific implementations of the present invention and are used to illustrate the concept of the present invention; these descriptions are explanatory and exemplary and should not be construed as limiting the implementation of the present invention or the scope of protection of the present invention. In addition to the embodiments described herein, those skilled in the art can also adopt other obvious technical solutions based on the content disclosed in the claims and the specification of this application. These technical solutions include those that make any obvious substitutions and modifications to the embodiments described herein.

[0047] The chemical reagents used in the embodiments and comparative examples of this invention are all commercially available products and have not undergone any further purification treatment.

[0048] Example 1 This embodiment provides a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. The preparation method specifically includes the following steps: A1. Phytic acid was dispersed in deionized water to obtain a phytic acid permeate with a mass fraction of 4 wt.%. 30 g of L-arginine and 25 g of zinc sulfate heptahydrate were dispersed sequentially in 800 g of deionized water, and the pH was adjusted to 6.9 to obtain an arginine-zinc chelate mineralization solution. S1, 14.2 g of L-lysine and 22 g of ammonium bicarbonate were dispersed in 500 mL of deionized water. 26 g of 3-bromopropyne was added under ice-water bath conditions. The mixture was stirred and reacted at room temperature in the dark for 22 h to obtain crude N,N-dipropyne. Under nitrogen atmosphere, 15.2 g of phosphorus oxychloride was dispersed in 190 mL of anhydrous acetonitrile. 6.2 g of an acetonitrile solution of aminoethanol (concentration 2 M) was added under ice-water bath conditions. The temperature was adjusted... The cyclic phosphoramide flame retardant was obtained by reflux reaction at 78℃ for 5 h. 18.5 g of crude N,N-diacetylacetyl lysine and 9.8 g of cyclic phosphoramide flame retardant were dispersed in 290 mL of anhydrous dimethylformamide. 20 g of N,N'-dicyclohexylcarbodiimide and 9.5 g of N-hydroxysuccinimide were added under ice-water bath conditions and mixed evenly. The mixture was stirred and reacted at room temperature for 42 h. After the reaction was completed, the mixture was filtered, rotary evaporated, and purified to obtain a diacetylacetyl phosphoramide crosslinking agent. S2, 11g of carboxymethyl chitosan and 5g of sericin were dispersed in 900mL of phosphate buffer with a pH of 7.0. The temperature was adjusted to 50℃ and the mixture was stirred in a water bath for 0.8h to obtain a substrate solution. 0.04g of transglutaminase was added to the substrate solution and the reaction was continued at 50℃ for 6h. The activity of the transglutaminase was >100U / g. After the reaction was completed, the reaction solution was heated to inactivate the enzyme. After inactivation and cooling, the reaction solution was transferred to a dialysis bag and the dialysis bag was placed in deionized water for dialysis. The dialysis step involved placing the dialysis bag in deionized water. The molecular weight cutoff of the dialysis bag was 4000Da. Dialysis was performed at 6℃ for 72 hours, with the deionized water replaced every 8 hours. The dialysis solution was then freeze-dried to obtain a bio-interface lubricant. S3, 5g of L-cysteine ​​methyl ester hydrochloride was dispersed in 3000g of deionized water, and the pH was adjusted to 8.5 using sodium carbonate solution with a mass fraction of 10wt.%. 100g of wool was immersed in deionized water. The wool was scouring and combing. The reaction was stirred at 30°C for 2h. After the reaction, the wool was washed and spun dry to obtain pretreated wool. The residual rate of the pretreated wool was 85%. The pretreated wool was immersed in phytic acid permeation solution and subjected to three vacuum-atmospheric pressure cycles. It was then soaked at atmospheric pressure for 1.0h. After soaking, the residual rate was controlled to be 100%. The wool was then immediately immersed in arginine-zinc chelate mineralization solution and soaked at room temperature for 4h. After washing and drying, the mineralized wool was obtained. S4, 15g of diacetylenic phosphoramide crosslinking agent and 0.5g of photoinitiator 2959 are dispersed in 3000g of tert-butanol / water mixed solvent, wherein the volume ratio of tert-butanol to water in the tert-butanol / water mixed solvent is 6:4. Then, 100g of mineralized wool is immersed in the tert-butanol / water mixed solvent and irradiated with a 500W UV lamp. The distance between the UV lamp and the surface of the tert-butanol / water mixed solvent is 20cm, and the irradiation time is 20min. During the irradiation, the wool is turned over every 5 minutes. After the injection, the wool is thoroughly washed and dried to obtain functionalized wool. The bio-interface lubricant is dispersed in deionized water to obtain a finishing working solution with a concentration of 2 g / L. The functionalized wool is immersed in the finishing working solution to obtain liquid-containing wool, which is then subjected to a two-stage heat treatment. The residual rate of the liquid-containing wool is 85%. The two-stage heat treatment is as follows: treatment at 80°C for 10 min, followed by baking at 130°C for 2.5 min. After natural cooling, the wool is processed through drawing, roving, and spinning to obtain wool-based antibacterial, warm, high-strength, and flame-retardant yarn.

[0049] Example 2 This embodiment provides a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. The preparation method specifically includes the following steps: A1. Phytic acid was dispersed in deionized water to obtain a phytic acid permeate with a mass fraction of 7 wt.%. 40 g of L-arginine and 32 g of zinc sulfate heptahydrate were dispersed sequentially in 800 g of deionized water, and the pH was adjusted to 7.1 to obtain an arginine-zinc chelate mineralization solution. S1, 14.8 g of L-lysine and 24 g of ammonium bicarbonate were dispersed in 460 mL of deionized water. 28 g of 3-bromopropyne was added under ice-water bath conditions. The mixture was stirred and reacted at room temperature in the dark for 28 h to obtain crude N,N-dipropyne. Under nitrogen atmosphere, 15.8 g of phosphorus oxychloride was dispersed in 210 mL of anhydrous acetonitrile. 6.8 g of an acetonitrile solution of aminoethanol (concentration 2 M) was added under ice-water bath conditions. The temperature was adjusted to... Cyclic phosphoramide flame retardant was obtained by reflux reaction at 82℃ for 4.5h. 19.5g of crude N,N-dioxypropyl lysine and 10.5g of cyclic phosphoramide flame retardant were dispersed in 310mL of anhydrous dimethylformamide. 22g of N,N'-dicyclohexylcarbodiimide and 10g of N-hydroxysuccinimide were added under ice-water bath conditions and mixed evenly. The mixture was stirred and reacted at room temperature for 48h. After the reaction was completed, the mixture was filtered, rotary evaporated, and purified to obtain dioxypropyl phosphoramide crosslinking agent. S2, 10.5g of carboxymethyl chitosan and 4.5g of sericin were dispersed in 850mL of phosphate buffer with a pH of 6.9. The temperature was adjusted to 48℃ and the mixture was stirred in a water bath for 0.6h to obtain a substrate solution. 0.06g of transglutaminase was added to the substrate solution and the reaction was continued at 48℃ for 7h. The activity of the transglutaminase was >100U / g. After the reaction was completed, the reaction solution was heated to inactivate the enzyme. After inactivation and cooling, the reaction solution was transferred to a dialysis bag and the dialysis bag was placed in deionized water for dialysis. The dialysis step involved placing the dialysis bag in deionized water. The molecular weight cutoff of the dialysis bag was 3800Da. Dialysis was performed at 8℃ for 72 hours, with the deionized water replaced every 8 hours. The dialysis solution was then freeze-dried to obtain a bio-interface lubricant. S3, 7g of L-cysteine ​​methyl ester hydrochloride was dispersed in 2800g of deionized water, and the pH was adjusted to 8.2 using sodium carbonate solution with a mass fraction of 10wt.%. 100g of wool was immersed in deionized water. The wool was scouring and combing. The reaction was stirred at 28°C for 2.5h. After the reaction, the wool was washed and spun dry to obtain pretreated wool with a pickling rate of 82%. The pretreated wool was then immersed in phytic acid permeation solution and subjected to three vacuum-atmospheric pressure cycles. It was then soaked at atmospheric pressure for 1.2h. After soaking, the pickling rate was controlled at 95%. The wool was then immediately immersed in arginine-zinc chelate mineralization solution and soaked at room temperature for 3.5h. After washing and drying, the mineralized wool was obtained. S4, 12g of diacetylenic phosphoramide crosslinking agent and 0.3g of photoinitiator 2959 are dispersed in 2800g of tert-butanol / water mixed solvent, wherein the volume ratio of tert-butanol to water in the tert-butanol / water mixed solvent is 6:4. Then, 100g of mineralized wool is immersed in the tert-butanol / water mixed solvent and irradiated with a 450W UV lamp. The distance between the UV lamp and the surface of the tert-butanol / water mixed solvent is 22cm, and the irradiation time is 25min. During the irradiation, the wool is turned over every 5 minutes. After completion, the wool is thoroughly washed and dried to obtain functionalized wool. The bio-interface lubricant is dispersed in deionized water to obtain a finishing working solution with a concentration of 1.5 g / L. The functionalized wool is immersed in the finishing working solution to obtain liquid-containing wool, which is then subjected to a two-stage heat treatment. The residual rate of the liquid-containing wool is 82%. The two-stage heat treatment is as follows: treatment at 78°C for 11 min, followed by baking at 135°C for 2.2 min. After natural cooling, the wool is processed through drawing, roving, and spinning to obtain wool-based antibacterial, warm, high-strength, and flame-retardant yarn.

[0050] Example 3 This embodiment provides a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. The preparation method specifically includes the following steps: A1. Phytic acid was dispersed in deionized water to obtain a phytic acid permeate with a mass fraction of 5.5 wt.%. 35 g of L-arginine and 28 g of zinc sulfate heptahydrate were dispersed sequentially in 800 g of deionized water, and the pH was adjusted to 7.0 to obtain an arginine-zinc chelate mineralization solution. S1, 15g of L-lysine and 25g of ammonium bicarbonate were dispersed in 540mL of deionized water. 25.5g of 3-bromopropyne was added under ice-water bath conditions. The mixture was stirred and reacted at room temperature in the dark for 25h to obtain crude N,N-dipropyne. Under nitrogen atmosphere, 15.5g of phosphorus oxychloride was dispersed in 200mL of anhydrous acetonitrile. 6.5g of an acetonitrile solution of aminoethanol (concentration 2M) was added under ice-water bath conditions. The temperature was adjusted to... Cyclic phosphoramide flame retardant was obtained by reflux reaction at 80℃ for 5.5h. 19g of crude N,N-dioxypropyl lysine and 10.0g of cyclic phosphoramide flame retardant were dispersed in 300mL of anhydrous dimethylformamide. 21g of N,N'-dicyclohexylcarbodiimide and 10.5g of N-hydroxysuccinimide were added under ice-water bath conditions and mixed evenly. The mixture was stirred and reacted at room temperature for 45h. After the reaction was completed, the mixture was filtered, rotary evaporated, and purified to obtain dioxypropyl phosphoramide crosslinking agent. S2, 12g of carboxymethyl chitosan and 6g of sericin were dispersed in 980mL of phosphate buffer with a pH of 7.2. The temperature was adjusted to 52℃ and the mixture was stirred in a water bath for 0.9h to obtain a substrate solution. 0.05g of transglutaminase was added to the substrate solution and the reaction was continued at 52℃ for 5.5h. The activity of the transglutaminase was >100U / g. After the reaction was completed, the reaction solution was heated to inactivate the enzyme. After inactivation and cooling, the reaction solution was transferred to a dialysis bag and the dialysis bag was placed in deionized water for dialysis. The dialysis step involved placing the dialysis bag in deionized water. The molecular weight cutoff of the dialysis bag was 4500Da. Dialysis was performed at 5℃ for 72 hours, with the deionized water replaced every 8 hours. The dialysis solution was then freeze-dried to obtain a bio-interface lubricant. S3, 6g of L-cysteine ​​methyl ester hydrochloride was dispersed in 3200g of deionized water, and the pH was adjusted to 8.8 using sodium carbonate solution with a mass fraction of 10wt.%. 100g of wool was immersed in deionized water. The wool was scouring and combing. The reaction was stirred at 32°C for 1.8h. After the reaction, the wool was washed and spun dry to obtain pretreated wool with a pickling rate of 88%. The pretreated wool was then immersed in phytic acid permeation solution and subjected to three vacuum-atmospheric pressure cycles. It was then soaked at atmospheric pressure for 1.4h. After soaking, the pickling rate was controlled at 105%. The wool was then immediately immersed in arginine-zinc chelate mineralization solution and soaked at room temperature for 4.5h. After washing and drying, the mineralized wool was obtained. S4, 18g of diacetylenic phosphoramide crosslinking agent and 0.8g of photoinitiator 2959 are dispersed in 3200g of tert-butanol / water mixed solvent, wherein the volume ratio of tert-butanol to water in the tert-butanol / water mixed solvent is 6:4. Then, 100g of mineralized wool is immersed in the tert-butanol / water mixed solvent and irradiated with a 550W UV lamp. The distance between the UV lamp and the surface of the tert-butanol / water mixed solvent is 18cm, and the irradiation time is 28min. During the irradiation, the wool is turned over every 5 minutes. After the injection, the wool is thoroughly washed and dried to obtain functionalized wool. The bio-interface lubricant is dispersed in deionized water to obtain a finishing working solution with a concentration of 2.5 g / L. The functionalized wool is immersed in the finishing working solution to obtain liquid-containing wool, which is then subjected to a two-stage heat treatment. The residual rate of the liquid-containing wool is 88%. The two-stage heat treatment is as follows: treatment at 82°C for 9 min, followed by baking at 138°C for 2.8 min. After natural cooling, the wool is processed through drawing, roving, and spinning to obtain wool-based antibacterial, warm, high-strength, and flame-retardant yarn.

[0051] Example 4 This embodiment provides a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. The preparation method specifically includes the following steps: A1. Phytic acid was dispersed in deionized water to obtain a phytic acid permeate with a mass fraction of 8 wt.%. 42 g of L-arginine and 34.5 g of zinc sulfate heptahydrate were dispersed sequentially in 800 g of deionized water, and the pH was adjusted to 7.2 to obtain an arginine-zinc chelate mineralization solution. S1, 14.5 g of L-lysine and 23 g of ammonium bicarbonate were dispersed in 480 mL of deionized water. 27 g of 3-bromopropyne was added under ice-water bath conditions. The mixture was stirred and reacted at room temperature in the dark for 30 h to obtain crude N,N-dipropyne. Under nitrogen atmosphere, 16 g of phosphorus oxychloride was dispersed in 220 mL of anhydrous acetonitrile. 7 g of an acetonitrile solution of aminoethanol (concentration 2 M) was added under ice-water bath conditions. The temperature was adjusted to 8... Cyclic phosphoramide flame retardant was obtained by reflux reaction at 5℃ for 6 h. 20 g of crude N,N-dioxypropyl lysine and 10.7 g of cyclic phosphoramide flame retardant were dispersed in 320 mL of anhydrous dimethylformamide. 24 g of N,N'-dicyclohexylcarbodiimide and 11.3 g of N-hydroxysuccinimide were added under ice-water bath conditions and mixed evenly. The mixture was stirred and reacted at room temperature for 50 h. After the reaction was completed, the mixture was filtered, rotary evaporated, and purified to obtain dioxypropyl phosphoramide crosslinking agent. S2, 10g of carboxymethyl chitosan and 4g of sericin were dispersed in 800mL of phosphate buffer with a pH of 6.8. The temperature was adjusted to 45℃ and stirred in a water bath for 1h to obtain a substrate solution. 0.075g of transglutaminase was added to the substrate solution and the reaction was continued at 45℃ for 8h. The activity of the transglutaminase was >100U / g. After the reaction was completed, the temperature was raised to inactivate the enzyme. After the reaction solution was inactivated and cooled, it was transferred to a dialysis bag and the dialysis bag was placed in deionized water for dialysis. The dialysis step was performed by placing the dialysis bag in deionized water. The molecular weight cutoff of the dialysis bag was 5000Da. Dialysis was performed at 10℃ for 72 hours, with the deionized water replaced every 8 hours. The dialysis solution was then freeze-dried to obtain a bio-interface lubricant. S3, 8g of L-cysteine ​​methyl ester hydrochloride was dispersed in 3500g of deionized water, and the pH was adjusted to 9 using sodium carbonate solution with a mass fraction of 10wt.%. 100g of wool was immersed in deionized water. The wool was scouring and combing. The reaction was stirred at 35°C for 3h. After the reaction, the wool was washed and spun dry to obtain pretreated wool. The residual rate of the pretreated wool was 90%. The pretreated wool was immersed in phytic acid permeation solution and subjected to three vacuum-atmospheric pressure cycles. It was then soaked at atmospheric pressure for 1.5h. After soaking, the residual rate was controlled at 110%. The wool was then immediately immersed in arginine-zinc chelate mineralization solution and soaked at room temperature for 5h. After washing and drying, the mineralized wool was obtained. S4, 20g of diacetylenic phosphoramide crosslinking agent and 1g of photoinitiator 2959 are dispersed in 3500g of tert-butanol / water mixed solvent, wherein the volume ratio of tert-butanol to water in the tert-butanol / water mixed solvent is 6:4. Then, 100g of mineralized wool is immersed in the tert-butanol / water mixed solvent and irradiated with a 600W UV lamp at a distance of 15cm from the liquid surface for 30 minutes. During irradiation, the wool is turned over every 5 minutes. After irradiation... The wool is thoroughly washed and dried to obtain functionalized wool. A bio-interface lubricant is dispersed in deionized water to obtain a finishing working solution with a concentration of 3 g / L. The functionalized wool is immersed in the finishing working solution to obtain wool with liquid and then subjected to a two-stage heat treatment. The residual rate of the wool with liquid is 90%. The two-stage heat treatment is as follows: treatment at 85°C for 12 min, followed by baking at 140°C for 3 min. After natural cooling, the wool is processed through drawing, roving, and spinning to obtain wool-based antibacterial, warm, high-strength, and flame-retardant yarn.

[0052] Comparative Example 1 This comparative example provides a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. The difference between this example and Example 1 is that the mineralized wool treated in step S3 of Example 1 is not treated in step S4. Instead, the same amount of diacetylphosphamide crosslinking agent and biological interface lubricant as in Example 1 are physically mixed to form a single finishing working solution. The mineralized wool is then finished in one step using a padding-baking process. This process does not involve ultraviolet light irradiation. Other process parameters and operating conditions are exactly the same as in Example 1.

[0053] Comparative Example 2 This comparative example provides a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. The difference between this example and Example 1 is that the wool is not treated in step S3, but directly proceeds to step S4. Other process parameters and operating conditions are exactly the same as in Example 1.

[0054] Comparative Example 3 This comparative example provides a wool-based antibacterial, warm, high-strength, and flame-retardant yarn and its preparation method. The difference between this example and Example 1 is that no diacetylphosphamide crosslinking agent is added in S4, while the other process parameters and operating conditions are exactly the same as in Example 1.

[0055] The wool-based antibacterial, warm, high-strength, and flame-retardant yarns prepared in Examples 1-4 and Comparative Examples 1-3 were tested. The breaking strength was tested according to GB / T 3916-2013; the limiting oxygen index was tested according to GB / T 5454-1997; the antibacterial rate was tested according to GB / T 20944.3-2008; and the warmth retention was tested according to GB / T 11048-2018.

[0056] The test results are shown in Table 1.

[0057] Table 1. Test results of wool-based antibacterial, warm, high-strength, and flame-retardant yarns in Examples 1-4 and Comparative Examples 1-3.

[0058] Table 1 shows that, compared to Example 1, Comparative Example 1 exhibits decreased tensile strength, limiting oxygen index, antibacterial rate, and warmth retention; Comparative Example 2 also shows decreased tensile strength, limiting oxygen index, antibacterial rate, and warmth retention; and Comparative Example 3 shows decreased tensile strength, limiting oxygen index, and warmth retention. In Comparative Example 1, a one-step padding-baking process was used, without UV irradiation. This reduced the chemical cross-linking degree of the diacetylphosphamide cross-linking agent within the fiber, resulting in more physical adsorption. Insufficient cross-linking leads to reduced fiber strength. Furthermore, the flame-retardant functional groups in the diacetylphosphamide cross-linking agent cannot fully form stable chemical bonds with the wool fiber and mineralization layer, thus reducing flame-retardant performance. In Comparative Example 2, no wool treatment was performed, resulting in decreased binding efficiency of the mineralization and cross-linking agents, and reduced mechanical strength. Step S3 helps phytic acid and arginine-zinc chelates to better deposit or complex inside and outside the fiber, improving the stability of the flame-retardant layer. Step S3 also increases the binding sites between wool and zinc ions, thus reducing the antibacterial rate. In Comparative Example 3, no diacetylphosphamide crosslinking agent was used, which prevented the formation of a certain crosslinking network through chemical bonds in the fiber structure. At the same time, the lack of flame-retardant groups resulted in a decrease in breaking strength and flame retardancy.

[0059] The above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn, characterized in that, The preparation method includes: S1, L-lysine and ammonium bicarbonate are dispersed in deionized water, and 3-bromopropyne is added to react and give crude N,N-di-di-propylated lysine. Phosphorus oxychloride is dispersed in anhydrous acetonitrile, and an acetonitrile solution of aminoethanol is added to react and give a cyclic phosphoramide flame retardant. Crude N,N-di-di-propylated lysine and the cyclic phosphoramide flame retardant are dispersed in anhydrous dimethylformamide, and N,N'-dicyclohexylcarbodiimide and N-hydroxysuccinimide are added to give a di-propylated phosphoramide crosslinking agent. S2, carboxymethyl chitosan and sericin are dispersed in phosphate buffer to obtain a substrate solution. Glutamine transaminase is added to the substrate solution to react. After the reaction is completed, the mixture is transferred to a dialysis bag for dialysis to obtain a biointerface lubricant. S3, L-cysteine ​​methyl ester hydrochloride is dispersed in deionized water, the pH is adjusted to 8-9, wool is immersed in deionized water to react, and pretreated wool is obtained. The pretreated wool is immersed in phytic acid permeate solution, and immediately after immersion, it is immersed in arginine-zinc chelate mineralization solution to obtain mineralized wool. S4, a diacetylphosphamide crosslinking agent and a photoinitiator are dispersed in a tert-butanol / water mixed solvent. The mineralized wool is immersed in the tert-butanol / water mixed solvent and irradiated with a UV lamp to obtain functionalized wool. A bio-interface lubricant is dispersed in deionized water to obtain a finishing working solution. The functionalized wool is immersed in the finishing working solution to obtain liquid-containing wool and undergoes a two-stage heat treatment. After drawing, roving, and spinning processes, wool-based antibacterial, warm, high-strength, and flame-retardant yarn is obtained.

2. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 1, characterized in that, The preparation methods for the phytic acid permeate and arginine-zinc chelate mineralization solution include: A1. Phytic acid is dispersed in deionized water to obtain phytic acid permeate. L-arginine and zinc sulfate heptahydrate are dispersed sequentially in deionized water, and the pH is adjusted to 6.8-7.2 to obtain arginine-zinc chelate mineralization solution.

3. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 1, characterized in that, In S1: The mass-to-volume ratio of L-lysine, ammonium bicarbonate, deionized water, and 3-bromopropyne is (14-15) g : (21-25) g : (450-550) mL : (25-26.8) g; The mass-to-volume ratio of the phosphorus oxychloride, anhydrous acetonitrile, and aminoethanol acetonitrile solution is (15-16) g : (180-220) mL : (6-7) g.

4. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 1, characterized in that, In S1: The mass-to-volume ratio of the crude N,N-dipropyne lysine, cyclic phosphoramide flame retardant, anhydrous dimethylformamide, N,N'-dicyclohexylcarbodiimide, and N-hydroxysuccinimide is (18-20) g : (9.5-10.7) g : (280-320) mL : (18.2-24) g : (9.2-11.3) g.

5. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 1, characterized in that, In S2: The mass-to-volume ratio of the carboxymethyl chitosan, sericin, phosphate buffer, and transglutaminase is (10-12) g : (4-6) g : (800-1000) mL : (0.03-0.075) g; The dialysis procedure involves placing the dialysis bag in deionized water and performing dialysis at 4-10°C for 72 hours, during which the deionized water is replaced every 8 hours.

6. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 1, characterized in that, In S3: The mass ratio of L-cysteine ​​methyl ester hydrochloride, deionized water, and wool is (3-8):(2500-3500):

100.

7. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 1, characterized in that, In S4: The mass ratio of the bis(alkynyl)phosphamide crosslinking agent, photoinitiator, tert-butanol / water mixed solvent to the mineralized wool is (10-20):(0.2-1):(2500-3500):

100.

8. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 1, characterized in that, In S4: The power of the ultraviolet lamp is 400-600W, the distance between the ultraviolet lamp and the surface of the tert-butanol / water mixed solvent is 15-25cm, the irradiation time is 15-30min, and the wool is turned over every 5 minutes during the irradiation. The two-stage heat treatment is as follows: treat at 75-85℃ for 8-12 minutes, and then bake at 125-140℃ for 2-3 minutes.

9. The method for preparing wool-based antibacterial, warm, high-strength, and flame-retardant yarn according to claim 2, characterized in that, In A1: The phytic acid permeate has a mass fraction of 3-8 wt.%. The mass ratio of L-arginine, zinc sulfate heptahydrate, and deionized water is (28-42):(23-34.5):

800.

10. A wool-based antibacterial, warm, high-strength, flame-retardant yarn is obtained by the preparation method according to any one of claims 1-9.

Images