Antibacterial regenerated wool blended yarn and production process thereof

Through gradient structure design and the construction of a multi-level antibacterial network, the problems of length loss and short antibacterial time of regenerated wool fibers are solved, efficient resource recycling and antibacterial durability of yarns are achieved, and the environmental protection and performance of the textile industry are improved.

CN120759022AActive Publication Date: 2025-10-10JINTA CASHMERE TEXTILE (JIANGSU) CO LTD +1

Patent Information

Application Number
CN202511296211.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-11
Publication Date
2025-10-10
Estimated Expiration
2045-09-11

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Abstract

The invention belongs to the technical field of textile materials, and particularly relates to an antibacterial regenerated wool blended yarn and a production process thereof.The antibacterial regenerated wool blended yarn is prepared from, by weight, 35 parts of regenerated wool fibers, 25-33 parts of LF tencel, 15-27 parts of cellulosic fibers, 8-12 parts of antibacterial chinlon 6 and 5 parts of an antibacterial complexing agent; according to the regenerated wool fiber prepared from the waste wool product through a synergistic improvement process of biological enzyme targeted cleaning and plasma etching, the natural properties of the wool fiber are reserved, and meanwhile, a surface pore structure capable of being combined with an antibacterial complexing agent is also formed; through a Z / S double-twist asynchronous spinning process, dynamic balance of a multilayer structure and hygroscopicity and strength of the blended yarn is achieved, and environment friendliness and commercial feasibility are both achieved.
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Description

Technical Field

[0001] The invention belongs to the technical field of textile materials, and particularly relates to an antibacterial regenerated wool blended yarn and a production process thereof. Background Art

[0002] In traditional textile manufacturing, the recycling of knitted fabric waste has long faced technical bottlenecks. Existing regenerated wool fiber production often relies on a crude processing method involving mechanical crushing and combing, resulting in significant fiber length loss and surface structural damage. This makes it difficult to meet the spinning requirements of high-count yarns, and recycling value can usually only be achieved through low-ratio blending or downgrading. Furthermore, the development of antimicrobial textiles in the market generally relies on finishing processes using a single chemical auxiliaries, which presents issues such as short antimicrobial efficacy, poor washability, and ecotoxicity risks, making it difficult to balance environmental standards with the need for long-term antibacterial effects. In terms of constructing blended systems, conventional processes often simply superimpose the physical blending of different fibers, lacking in-depth design of fiber functional complementarity and structural synergy. In particular, the interfacial bonding strength between regenerated fibers and functionalized synthetic fibers is insufficient, making it difficult to balance the mechanical properties of the yarn with its durability. Furthermore, with increasingly stringent requirements for sustainable production in the textile industry, existing technologies still lack systematic solutions for key aspects such as energy consumption control during waste treatment and the environmental compatibility of fiber modifiers, hindering the development of recycled textiles towards high-end and functionalized textiles. In this context, the development of composite spinning technology that combines efficient resource recycling, multiple antibacterial synergy and structural performance optimization has become an important breakthrough in promoting the green transformation of the textile industry. Summary of the Invention

[0003] In response to the above situation, the present invention provides an antibacterial regenerated wool blended yarn and its production process, which focuses on the high-value recycling of knitting waste. On the basis of retaining the original properties of regenerated wool fibers, the precise control of the fiber surface structure is achieved through the synergistic effect of physical etching and chemical modification. The fiber pores and charge characteristics are used to establish a multi-level antibacterial network. Through the gradient structure design of core layer moisture absorption, middle layer softening, and outer layer protection, the interface enhancement and performance complementarity of regenerated fibers and functional fibers are achieved, providing the textile industry with a sustainable solution that has both ecological value and commercial feasibility.

[0004] To achieve the above object, the technical solution adopted by the present invention is as follows: The invention provides an antibacterial regenerated wool blended yarn. The blended yarn comprises the following raw materials in parts by weight: 35 parts of regenerated wool fiber, 25-33 parts of LF Tencel, 15-27 parts of cellulose fiber, 8-12 parts of antibacterial nylon 6 and 5 parts of an antibacterial composite agent.

[0005] Furthermore, the cellulose fiber is selected from any one of Modal fiber, Lyocell fiber, bamboo pulp fiber and cuprammonium fiber.

[0006] Furthermore, the antibacterial composite is prepared from the following raw materials in parts by weight: 4-5 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 1-2 parts of xanthan gum, 20-25 parts of deionized water and 20-25 parts of pH 5.0 acetate buffer.

[0007] The preparation method of the antibacterial composite comprises the following steps: S1: Weigh 4-5 parts of silver-loaded zeolite and 20-25 parts of deionized water, mix them, pre-disperse them in a high-speed disperser, and sonicate them in an ultrasonic reactor to obtain a dispersion. Weigh 2 parts of chitosan quaternary ammonium salt and dissolve them in 20-25 parts of pH 5.0 acetate buffer to obtain a chitosan quaternary ammonium salt solution. S2: Weigh 1.5 parts of tea polyphenols and 0.5 parts of zinc sulfate and add them to the dispersion. Stir in a water bath at 60°C for 40 min to obtain a primary mixed solution. Slowly add the primary mixed solution to the chitosan quaternary ammonium salt solution, homogenize in a high-speed shear emulsifier at 12,000 rpm for 15 min, and then stir magnetically at 500 rpm for 30 min to obtain a composite solution. S3: Weigh 1-2 portions of xanthan gum and add them to the composite liquid in portions. Stir slowly after each addition until it is completely dissolved. Transfer the mixture to a vacuum degassing tank and degas for 20 minutes to obtain an antibacterial composite.

[0008] Furthermore, the regenerated wool fiber is prepared by treating waste wool products with a bio-enzyme cleaning agent, a fiber repair agent, and a softening auxiliary agent, specifically comprising the following steps: X1: After removing chemical fiber blends from waste wool products through a photoelectric sorting system, the waste wool products were placed in a loose untwisting machine and soaked in 40°C purified water for 30 minutes to obtain single fibers. The single fibers were then placed in a pH 9.5 carbonate buffer solution at a mass ratio of 1:20, and a bio-enzyme cleaning agent was weighed and added to the buffer. After 1 hour, the treated single fibers were ultrasonically cleaned and air-dried to obtain clean fibers. X2: The clean fiber was immersed in a fiber repair agent and treated at 45°C under vacuum for 2 h. It was then irradiated with microwaves at 3000 MHz and a power density of 10 W / g for 8 min to obtain the repaired fiber. The repaired fiber was then treated with an atmospheric pressure low-temperature plasma system at a discharge power of 300 W for 6 min to obtain the activated fiber. X3: The activated fiber is immersed in a softening agent for 30 minutes and then taken out. The softening agent is then sprayed onto the activated fiber using a spray gun, and then dried and shaped at 85°C under far-infrared radiation for 20 minutes to obtain regenerated wool fiber.

[0009] Furthermore, the dosage of the bio-enzyme cleaning agent, fiber repair agent and softening auxiliary agent is 2.5%, 15% and 1.2% of the mass of the waste wool products, respectively.

[0010] Furthermore, the bio-enzyme cleaning agent consists of alkaline protease (2000 U / g) and lipase (1500 U / g) in a mass ratio of 3:1.

[0011] Furthermore, the fiber repair agent is a composite solution composed of hydroxypropyl chitosan, polyethylene glycol 4000 and trisodium citrate in a mass ratio of 5:3:2, and the total mass concentration of the composite solution is 8%.

[0012] Furthermore, the softening auxiliary agent is composed of a combination of an organosilicon microemulsion (particle size ≤ 50 nm) and octadecyltrimethylammonium chloride in a mass ratio of 4:1.

[0013] The present invention also provides a production process for antibacterial regenerated wool blended yarn, which specifically comprises the following steps: Step 1: Weigh 35 parts of regenerated wool fiber and 25-33 parts of LF Tencel, and blend them using a rotor spinning machine at a rotor speed of 50,000-75,000 rpm and a Z twist coefficient of 380 T / m to obtain a core yarn; Step 2: Weigh 15-27 parts of cellulose fiber, use a ring spinning system to reversely wrap the cellulose fiber with an S twist of 700 T / m around the core yarn, with a spindle speed of 9000-12000 rpm and a wrapping angle of 55° to obtain a middle-layer spinning yarn, weigh 8-12 parts of antibacterial nylon 6 and use a false twister to spirally wrap the antibacterial nylon 6 with the middle-layer spinning yarn with an overfeed rate of 6-10% to obtain a pre-blended yarn; Step 3: Weigh 5 parts of the antibacterial compound and atomize it with a 50 kV high-voltage electrostatic generator, then spray it on the surface of the primary blended yarn. After spraying, shape it under a hot roller at 180°C to obtain the antibacterial regenerated wool blended yarn.

[0014] The beneficial effects achieved by the present invention are as follows: The antibacterial regenerated wool blended yarn provided by the present invention realizes the efficient regeneration and functional upgrading of waste wool resources. Through the synergistic effect of bio-enzyme targeted cleaning and plasma etching, while completely retaining the natural structure of wool fibers, nano-scale surface pores and active structures are precisely constructed, providing physical anchoring points and chemical binding interfaces for the multi-level loading of antibacterial components. The innovatively developed multi-component antibacterial composite system utilizes the sustained-release antibacterial effect of silver-loaded zeolite, the charge adsorption destruction of chitosan quaternary ammonium salt, and the antioxidant blocking effect of tea polyphenols to form a three-dimensional protective network, breaking through the technical bottleneck of the easy failure of a single antibacterial mechanism. In the spinning process, the core layer of the composite of regenerated wool and Tencel achieves a dynamic balance between hygroscopicity and strength through Z / S double-twist asynchronous twisting, while the outer spiral winding of the antibacterial nylon forms a micro-nano topological structure similar to the lotus leaf surface under the action of thermal deformation, so that the antibacterial function and physical protection produce a spatial coupling effect. This scheme organically integrates the recycling of waste textiles, the molecular design of functional materials and the bionic construction of yarn structure. It not only retains the ecological properties of natural fibers, but also gives them long-lasting antibacterial properties that surpass conventional synthetic fibers, providing an innovative direction with both scientific value and practical prospects for the green transformation of the textile industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 The results of the antibacterial performance test of the antibacterial regenerated wool blended yarn prepared in Examples 2, 4, 6 and Comparative Examples 1-2 are shown; Figure 2 The results of durability test on the antibacterial regenerated wool blended yarns prepared in Examples 1-6 and Comparative Examples 1-2 are as follows; Figure 3 The electron microscopy morphology characterization results of the regenerated wool fiber prepared in the example before and after rubbing and washing; Figure 4 These are the test results of the pore density and antibacterial composite coverage of the antibacterial regenerated wool blended yarns prepared in Examples 1-6 and Comparative Examples 1-2. DETAILED DESCRIPTION

[0016] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0017] Unless otherwise defined, all technical and scientific terms used herein have the same meanings as those familiar to those skilled in the art. Furthermore, any methods and materials similar or equivalent to those described herein can be applied to the present invention. The preferred embodiments and materials described herein are for illustrative purposes only and are not intended to limit the scope of this application.

[0018] In the following examples, unless otherwise specified, conventional methods are used; the materials used in the following examples and comparative examples, unless otherwise specified, are all new materials purchased from the market.

[0019] In the following examples and comparative examples, the regenerated wool fibers were prepared by treating 200 parts by weight of waste wool products with 5 parts by weight of a bio-enzyme cleaning agent, 30 parts by weight of a fiber repair agent, and 2.4 parts by weight of a softening auxiliary agent; The waste wool products include 120 parts by weight of wool knitting scraps, 50 parts by weight of worsted wool waste yarn and 30 parts by weight of blended wool waste clothing. The materials are all pre-cleaned and free of foreign matter. The color fastness test is ≥ level 4 and the wool content is ≥ 95%. The mass ratio of alkaline protease to lipase in the bio-enzyme cleaning agent is 3:1. Before use, alkaline protease is activated at 60°C for 40 minutes, and lipase is activated at 50°C for 30 minutes. The fiber repair agent contains hydroxypropyl chitosan, polyethylene glycol 4000 and trisodium citrate, and the deacetylation degree of the hydroxypropyl chitosan used is 92%; The average particle size of the silicone microemulsion in the softening auxiliary agent was 37.4 nm and the PDI was 0.163; The specific preparation method of the regenerated wool fiber is as follows: X1: Weigh 200 parts of waste wool products and remove chemical fiber blends through infrared spectroscopy identification by a photoelectric sorting system. Then put them into a loose untwisting machine and soak them in purified water at 40°C for 30 minutes to obtain single fibers. The single fibers are placed in a pH 9.5 carbonate buffer solution at a mass ratio of 1:20, and 5 parts of a bio-enzyme detergent are weighed and added thereto to remove the wool scale layer lipids in the single fibers. The removal rate is 97%. After 1 hour, the treated single fibers are subjected to an oscillating test at 28 kHz and 0.5 W / cm 3 Ultrasonic cleaning under high power density and drying were performed to obtain clean fibers, and the whiteness CIE value of the clean fibers was measured to be 78; X2: The clean fiber was immersed in 30 parts of fiber repair agent, treated at 45°C under vacuum for 2 hours, and then irradiated with 3000 MHz microwaves at a power density of 10 W / g for 8 minutes to obtain repaired fiber. The repaired fiber was treated with an atmospheric pressure low-temperature plasma system for 6 minutes using a helium / oxygen mixture with a volume ratio of 9:1 and a discharge power of 300 W to obtain activated fiber. The wetting contact angle of the activated fiber was 33°. X3: The activated fiber is first immersed in a softening agent for 30 minutes and then taken out. The softening agent is then sprayed onto the activated fiber through a spray gun, and then dried and shaped at 85°C under far-infrared radiation for 20 minutes to obtain regenerated wool fiber. The dynamic friction coefficient of the regenerated wool fiber is 0.15, the fiber regain is stable at 14-16%, the short fiber rate is 6.7%, and the defect content is ≤10 / g.

[0020] Example 1: This example provides an antibacterial regenerated wool blended yarn, which comprises the following raw materials in parts by weight: 35 parts of regenerated wool fiber, 25 parts of LF Tencel, 27 parts of Modal fiber, 8 parts of antibacterial nylon 6, and 5 parts of an antibacterial compound; The antibacterial composite is prepared from the following raw materials in parts by weight: 4 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 2 parts of xanthan gum, 20 parts of deionized water and 20 parts of pH 5.0 acetate buffer.

[0021] The preparation method of the antibacterial composite comprises the following steps: S1: Weigh 4 parts of silver-loaded zeolite and 20 parts of deionized water, mix them, and then pre-disperse them in a high-speed disperser at 5000 rpm for 5 minutes and in an ultrasonic reactor at 40 kHz and 1.2 W / cm 3 , ultrasonically treated at 50°C for 20 min to obtain a dispersion, and the particle size of the silver-loaded zeolite in the dispersion was detected to be 675.2 nm. 2 parts of chitosan quaternary ammonium salt were weighed and dissolved in 20 parts of pH 5.0 acetate buffer to obtain a chitosan quaternary ammonium salt solution; S2: 1.5 parts of tea polyphenols and 0.5 parts of zinc sulfate were weighed and added to the dispersion. The mixture was stirred at 800 rpm in a 60°C water bath for 40 min. The viscosity of the solution was measured by a rotational viscometer and was 206.5 mPa·s to obtain a preliminary mixed solution. The preliminary mixed solution was slowly added to the chitosan quaternary ammonium salt solution. The mixture was homogenized in a high-speed shear emulsifier at 12,000 rpm for 15 min, and then magnetically stirred at 500 rpm for 30 min to obtain a composite solution. S3: Weigh 2 parts of xanthan gum and add it to the composite liquid in three times. Stir slowly after each addition until it is completely dissolved. Transfer it to a vacuum degassing tank and degas for 20 minutes. The viscosity is measured to be 224.1 mPa·s. After filtering through a 0.45 μm filter membrane, the antibacterial composite agent is obtained.

[0022] This embodiment also provides a production process for antibacterial regenerated wool blended yarn, which specifically includes the following steps: Step 1: 35 parts of regenerated wool fiber and 25 parts of LF Tencel were weighed and mixed using a rotor spinning machine at a rotor speed of 50,000 rpm and a Z twist coefficient of 380 T / m to obtain a core yarn; Step 2: Weigh 27 parts of Modal fiber and use a ring spinning system to reversely wrap the Modal fiber around the core yarn with an S twist of 700 T / m, a spindle speed of 9000 rpm, and a wrapping angle of 55° to obtain a middle-layer spinning yarn. Weigh 8 parts of antibacterial nylon 6 and use a false twister to spirally wrap the antibacterial nylon 6 with the middle-layer spinning yarn with an overfeed rate of 8% to obtain a pre-blended yarn. Step 3: Weigh 5 parts of the antibacterial compound and atomize it with a 50 kV high-voltage electrostatic generator, then spray it on the surface of the primary blended yarn. After spraying, shape it under a hot roller at 180°C to obtain the antibacterial regenerated wool blended yarn.

[0023] Example 2: This example provides an antibacterial regenerated wool blended yarn, which comprises the following raw materials in parts by weight: 35 parts of regenerated wool fiber, 30 parts of LF Tencel, 20 parts of Modal fiber, 10 parts of antibacterial nylon 6, and 5 parts of an antibacterial compound; The antibacterial composite is prepared from the following raw materials in parts by weight: 5 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 1 part of xanthan gum, 25 parts of deionized water and 25 parts of pH 5.0 acetate buffer.

[0024] The preparation method of the antibacterial composite comprises the following steps: S1: Weigh 5 parts of silver-loaded zeolite and 25 parts of deionized water, mix them, and then pre-disperse them in a high-speed disperser at 5000 rpm for 5 minutes and in an ultrasonic reactor at 40 kHz and 1.2 W / cm 3 , ultrasonically treated at 50°C for 20 min to obtain a dispersion, and the particle size of the silver-loaded zeolite in the dispersion was detected to be 658.3 nm. 2 parts of chitosan quaternary ammonium salt were weighed and dissolved in 25 parts of pH 5.0 acetate buffer to obtain a chitosan quaternary ammonium salt solution; S2: 1.5 parts of tea polyphenols and 0.5 parts of zinc sulfate were weighed and added to the dispersion. The mixture was stirred at 800 rpm in a 60°C water bath for 40 min. The viscosity of the solution was measured by a rotational viscometer and was 204.7 mPa·s to obtain a preliminary mixed solution. The preliminary mixed solution was slowly added to the chitosan quaternary ammonium salt solution. The mixture was homogenized in a high-speed shear emulsifier at 12,000 rpm for 15 min, and then magnetically stirred at 500 rpm for 30 min to obtain a composite solution. S3: Weigh 1 part of xanthan gum and add it to the composite liquid in two portions. Stir slowly after each addition until it is completely dissolved. Transfer the mixture to a vacuum degassing tank and degas for 20 minutes. The viscosity is measured to be 213.5 mPa·s. Filter through a 0.45 μm filter membrane to obtain the antibacterial composite.

[0025] This embodiment also provides a production process for antibacterial regenerated wool blended yarn, which specifically includes the following steps: Step 1: 35 parts of regenerated wool fiber and 30 parts of LF Tencel were weighed and mixed using a rotor spinning machine at a rotor speed of 50,000 rpm and a Z twist coefficient of 380 T / m to obtain a core yarn; Step 2: Weigh 20 parts of Modal fiber and use a ring spinning system to reversely wrap the Modal fiber around the core yarn with an S twist of 700 T / m, a spindle speed of 9000 rpm, and a wrapping angle of 55° to obtain a middle-layer spinning yarn. Weigh 10 parts of antibacterial nylon 6 and use a false twister to spirally wrap the antibacterial nylon 6 with the middle-layer spinning yarn with an overfeed rate of 12% to obtain a pre-blended yarn. Step 3: Weigh 5 parts of the antibacterial compound and atomize it with a 50 kV high-voltage electrostatic generator, then spray it on the surface of the primary blended yarn. After spraying, shape it under a hot roller at 180°C to obtain the antibacterial regenerated wool blended yarn.

[0026] Example 3: This example provides an antibacterial regenerated wool blended yarn, which comprises the following raw materials in parts by weight: 35 parts of regenerated wool fiber, 30 parts of LF Tencel, 20 parts of Lyocell fiber, 10 parts of antibacterial nylon 6, and 5 parts of an antibacterial compound; The antibacterial composite is prepared from the following raw materials in parts by weight: 4 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 2 parts of xanthan gum, 20 parts of deionized water and 20 parts of pH 5.0 acetate buffer.

[0027] The preparation method of the antibacterial composite comprises the following steps: S1: Weigh 4 parts of silver-loaded zeolite and 20 parts of deionized water, mix them, and then pre-disperse them in a high-speed disperser at 5000 rpm for 5 minutes and in an ultrasonic reactor at 40 kHz and 1.2 W / cm 3 , ultrasonically treated at 50°C for 20 min to obtain a dispersion, and the particle size of the silver-loaded zeolite in the dispersion was detected to be 688.6 nm. 2 parts of chitosan quaternary ammonium salt were weighed and dissolved in 20 parts of pH 5.0 acetate buffer to obtain a chitosan quaternary ammonium salt solution; S2: 1.5 parts of tea polyphenols and 0.5 parts of zinc sulfate were weighed and added to the dispersion. The mixture was stirred at 800 rpm in a 60°C water bath for 40 min. The viscosity of the solution was measured by a rotational viscometer and was 209.3 mPa·s to obtain a preliminary mixed solution. The preliminary mixed solution was slowly added to the chitosan quaternary ammonium salt solution. The mixture was homogenized in a high-speed shear emulsifier at 12,000 rpm for 15 min, and then magnetically stirred at 500 rpm for 30 min to obtain a composite solution. S3: Weigh 2 parts of xanthan gum and add it to the composite liquid in three times. Stir slowly after each addition until it is completely dissolved. Transfer the mixture to a vacuum degassing tank and degas for 20 minutes. The viscosity is measured to be 219.4 mPa·s. Filter through a 0.45 μm filter membrane to obtain the antibacterial composite.

[0028] This embodiment also provides a production process for antibacterial regenerated wool blended yarn, which specifically includes the following steps: Step 1: 35 parts of regenerated wool fiber and 30 parts of LF Tencel were weighed and mixed using a rotor spinning machine at a rotor speed of 60,000 rpm and a Z twist coefficient of 380 T / m to obtain a core yarn; Step 2: Weigh 20 parts of Lyocell fiber and use a ring spinning system to reversely wrap the Lyocell fiber with an S twist of 700 T / m around the core yarn at a spindle speed of 10,000 rpm and a wrapping angle of 55° to obtain a middle-layer spinning yarn. Weigh 10 parts of antibacterial nylon 6 and use a false twister to spirally wrap the antibacterial nylon 6 with the middle-layer spinning yarn at an overfeed rate of 8% to obtain a pre-blended yarn. Step 3: Weigh 5 parts of the antibacterial compound and atomize it with a 50 kV high-voltage electrostatic generator, then spray it on the surface of the primary blended yarn. After spraying, shape it under a hot roller at 180°C to obtain the antibacterial regenerated wool blended yarn.

[0029] Example 4: This example provides an antibacterial regenerated wool blended yarn, which comprises the following raw materials in parts by weight: 35 parts of regenerated wool fiber, 33 parts of LF Tencel, 15 parts of Lyocell fiber, 12 parts of antibacterial nylon 6, and 5 parts of an antibacterial compound; The antibacterial composite is prepared from the following raw materials in parts by weight: 5 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 1 part of xanthan gum, 25 parts of deionized water and 25 parts of pH 5.0 acetate buffer.

[0030] The preparation method of the antibacterial composite comprises the following steps: S1: Weigh 5 parts of silver-loaded zeolite and 25 parts of deionized water, mix them, and then pre-disperse them in a high-speed disperser at 5000 rpm for 5 minutes and in an ultrasonic reactor at 40 kHz and 1.2 W / cm 3 , ultrasonically treated at 50°C for 20 min to obtain a dispersion, and the particle size of the silver-loaded zeolite in the dispersion was detected to be 661.3 nm. 2 parts of chitosan quaternary ammonium salt were weighed and dissolved in 25 parts of pH 5.0 acetate buffer to obtain a chitosan quaternary ammonium salt solution; S2: 1.5 parts of tea polyphenols and 0.5 parts of zinc sulfate were weighed and added to the dispersion. The mixture was stirred at 800 rpm in a 60°C water bath for 40 min. The viscosity of the solution was measured by a rotational viscometer and was 214.7 mPa·s to obtain a preliminary mixed solution. The preliminary mixed solution was slowly added to the chitosan quaternary ammonium salt solution. The mixture was homogenized in a high-speed shear emulsifier at 12,000 rpm for 15 min, and then magnetically stirred at 500 rpm for 30 min to obtain a composite solution. S3: Weigh 1 part of xanthan gum and add it to the composite liquid in two portions. Stir slowly after each addition until it is completely dissolved. Transfer the mixture to a vacuum degassing tank and degas for 20 minutes. The viscosity is measured to be 207.9 mPa·s. Filter through a 0.45 μm filter membrane to obtain the antibacterial composite.

[0031] This embodiment also provides a production process for antibacterial regenerated wool blended yarn, which specifically includes the following steps: Step 1: 35 parts of regenerated wool fiber and 33 parts of LF Tencel were weighed and mixed using a rotor spinning machine at a rotor speed of 75,000 rpm and a Z twist coefficient of 380 T / m to obtain a core yarn; Step 2: Weigh 15 parts of Lyocell fiber and use a ring spinning system to reversely wrap the Lyocell fiber around the core yarn with an S twist of 700 T / m, a spindle speed of 12000 rpm, and a wrapping angle of 55° to obtain a middle-layer spinning yarn. Weigh 12 parts of antibacterial nylon 6 and use a false twister to spirally wrap the antibacterial nylon 6 with the middle-layer spinning yarn with an overfeed rate of 10% to obtain a pre-blended yarn. Step 3: Weigh 5 parts of the antibacterial compound and atomize it with a 50 kV high-voltage electrostatic generator, then spray it on the surface of the primary blended yarn. After spraying, shape it under a hot roller at 180°C to obtain the antibacterial regenerated wool blended yarn.

[0032] Example 5: This example provides an antibacterial regenerated wool blended yarn, which comprises the following raw materials in parts by weight: 35 parts of regenerated wool fiber, 33 parts of LF Tencel, 15 parts of bamboo pulp fiber, 12 parts of antibacterial nylon 6, and 5 parts of an antibacterial compound; The antibacterial composite is prepared from the following raw materials in parts by weight: 5 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 1 part of xanthan gum, 25 parts of deionized water and 25 parts of pH 5.0 acetate buffer.

[0033] The preparation method of the antibacterial composite comprises the following steps: S1: Weigh 5 parts of silver-loaded zeolite and 25 parts of deionized water, mix them, and then pre-disperse them in a high-speed disperser at 5000 rpm for 5 minutes and in an ultrasonic reactor at 40 kHz and 1.2 W / cm 3 , ultrasonically treated at 50°C for 20 min to obtain a dispersion, and the particle size of the silver-loaded zeolite in the dispersion was detected to be 664.8 nm. 2 parts of chitosan quaternary ammonium salt were weighed and dissolved in 25 parts of pH 5.0 acetate buffer to obtain a chitosan quaternary ammonium salt solution; S2: take tea polyphenols 1.5 parts and zinc sulfate 0.5 parts and add them to the dispersion liquid, stir at 60°C water bath 800 rpm for 40 min, and detect the solution viscosity with a rotary viscometer to be 215.2 mPa·s, to obtain a primary mixed liquid, slowly add the primary mixed liquid to the chitosan quaternary ammonium salt solution, homogenize in a high-speed shearing emulsifier at 12000 rpm for 15 min, and then stir at 500 rpm for 30 min to obtain a composite liquid; S3: take xanthan gum 1 part and add it to the composite liquid in two portions, slowly stir after each addition until completely dissolved, transfer to a vacuum degassing tank and degas for 20 min, measure the viscosity to be 211.4 mPa·s, and filter through a 0.45 μm filter membrane to obtain an antibacterial composite agent.

[0034] The embodiment also provides a production process of the antibacterial regenerated wool blended yarn, which specifically comprises the following steps: Step 1: take 35 parts of regenerated wool fibers and 30 parts of LF tencel, mix the fibers by using a rotor spinning machine, the rotor speed is 75000 rpm, and the Z twist factor is 380 T / m, to obtain a core yarn; Step 2: take 20 parts of bamboo pulp fibers, wrap the core yarn with the bamboo pulp fibers in a S twist reverse direction with a twist factor of 700 T / m by using a ring spinning system, the spindle speed is 12000 rpm, and the wrapping angle is 55°, to obtain a middle layer yarn, take 10 parts of the antibacterial nylon 6, and spiral wrap the antibacterial nylon 6 and the middle layer yarn by using a false twister, the overfeed rate is 10%, to obtain a primary blended yarn; Step 3: take 5 parts of the antibacterial composite agent, atomize the antibacterial composite agent by using a 50 kV high-voltage static generator, spray the antibacterial composite agent on the surface of the primary blended yarn, and then set the yarn under a hot roller at 180°C, to obtain an antibacterial regenerated wool blended yarn.

[0035] Embodiment 6: The embodiment provides an antibacterial regenerated wool blended yarn, which comprises the following raw materials in parts by weight: 35 parts of regenerated wool fibers, 33 parts of LF tencel, 15 parts of cuprammonium fiber, 12 parts of antibacterial nylon 6, and 5 parts of an antibacterial composite agent. The antibacterial composite agent is prepared from the following raw materials in parts by weight: 5 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 1 part of xanthan gum, 25 parts of deionized water, and 25 parts of pH 5.0 acetic acid buffer.

[0036] The preparation method of the antibacterial composite agent comprises the following steps: S1: mix 5 parts of silver-loaded zeolite and 25 parts of deionized water, and then pre-disperse the mixture by using a high-speed dispersion machine at 5000 rpm for 5 min and ultrasonic wave in an ultrasonic wave reactor at 40 kHz and 1.2 W / cm 3, 50℃ ultrasonic for 20 min to obtain a dispersion liquid, and the particle size of the silver-loaded zeolite in the dispersion liquid was 673.5 nm; 2 parts of chitosan quaternary ammonium salt were weighed and dissolved in 25 parts of pH 5.0 acetic acid buffer to obtain a chitosan quaternary ammonium salt solution; S2: 1.5 parts of tea polyphenol and 0.5 parts of zinc sulfate were weighed and added into the dispersion liquid, and the solution was stirred at 60℃ for 40 min at 800 rpm; the viscosity of the solution was 212.0 mPa·s detected by a rotational viscometer, to obtain a preliminary mixed solution; the preliminary mixed solution was slowly added into the chitosan quaternary ammonium salt solution, and then homogenized in a high-speed shearing emulsifier at 12000 rpm for 15 min, and then stirred at 500 rpm for 30 min to obtain a composite liquid; S3: 1 part of xanthan gum was added into the composite liquid in two portions, and each portion was slowly stirred until completely dissolved; the solution was transferred into a vacuum degassing tank and degassed for 20 min; the viscosity was 208.7 mPa·s, and the antibacterial composite agent was obtained after filtration through a 0.45 μm filter membrane.

[0037] The embodiment also provides a production process of the antibacterial regenerated wool blended yarn, and specifically includes the following steps: Step 1: 35 parts of regenerated wool fibers and 30 parts of LF tencel were weighed and mixed by using a rotor spinning machine, the rotor speed was 75000 rpm, and the Z twist factor was 380 T / m to obtain a core yarn; Step 2: 20 parts of cuprammonium fiber were weighed and wrapped around the core yarn in a reverse S twist direction at a twist factor of 700 T / m by using a ring spinning system, the spindle speed was 12000 rpm, and the wrapping angle was 55° to obtain a middle layer yarn; 10 parts of antibacterial nylon 6 was weighed and spirally wound with the middle layer yarn by using a false twister, and the overfeed rate was 10% to obtain a preliminary blended yarn; Step 3: 5 parts of the antibacterial composite agent was atomized by a 50 kV high-voltage static generator and sprayed on the surface of the preliminary blended yarn; after the spraying was completed, the yarn was set on a hot roller at 180℃ to obtain the antibacterial regenerated wool blended yarn.

[0038] The difference between the comparative example 1 and the embodiment 2 lies in that the same weight of newly made wool fibers is used to replace the regenerated wool fibers for preparation, and the remaining parts are the same as those of the embodiment 2.

[0039] The difference between the comparative example 2 and the embodiment 4 lies in that the same weight of purified water is used to replace the antibacterial composite agent for preparation, and the remaining parts are the same as those of the embodiment 4.

[0040] Mechanical property investigation Blended yarn performance testing was conducted according to ISO 2062 and ASTM D2256. Blended yarn samples prepared in Examples 1-6 and Comparative Examples 1-2 were equilibrated in a standard temperature and humidity environment for 24 hours and then tested using a constant-rate elongation tester (CRE) with a clamping distance of 500 mm and a tensile speed of 500 mm / min. Each sample was tested 30 times, and the average value was calculated. The breaking strength was calculated by the ratio of the maximum breaking force to the yarn linear density, and the elongation at break was calculated by dividing the elongation at break by the initial length. The hairiness index was tested using a photoelectric hairiness meter, with a hairiness length of 3 mm or more as the statistical standard. The yarn passed through the detection area at a speed of 50 m / min, and the cumulative hairiness count within a length of 10 m was detected. The yarn evenness was measured using an Uster evenness meter. The yarn passed through a capacitive sensor at a speed of 400 m / min, and the coefficient of variation (CV%) of mass within a length of 100 m was recorded. During the test, the yarn tension was kept constant (0.5 cN / tex) and external vibration interference was eliminated. The test results are shown in Table 1.

[0041] Antibacterial performance test The antibacterial properties were quantitatively evaluated according to the AATCC 100 standard. The blended yarn samples prepared in Examples 2, 4, 6 and Comparative Examples 1-2 were cut into circular specimens with a diameter of 4.8 ± 0.1 cm, sterilized by ultraviolet light for 30 min, and then immersed in a solution containing 1 × 10 3 The inoculated samples were placed in a bacterial suspension of Escherichia coli (ATCC 25922) or Staphylococcus aureus (ATCC 6538) at a concentration of 100 CFU / mL, ensuring that the fiber was completely infiltrated by the bacterial solution. The inoculated samples were placed in a sterile sealed bag and incubated at 37°C for 24 h. After removal, 100 mL of neutralizing solution (physiological saline containing 0.5% Tween 80) was added and vortexed for 2 min to elute the residual bacteria. 1 mL of the eluate was diluted serially and spread on a nutrient agar plate. After incubation at 37°C for 48 h, the colony forming units (CFU) were counted. The inhibition rate was calculated as (CFU of the blank control group - CFU of the sample group) / CFU of the blank control group × 100%. The washing durability test was carried out in accordance with GB / T 3921-2008 standard. A solution containing 0.5% standard detergent (40°C) was used. The washing cycle was repeated 50 times with a bath ratio of 1:50 and oscillation for 30 min. The inhibition rate was tested. The results are shown in the table. Figure 1 .

[0042] Durability testing The silver ion retention rate test was completed by inductively coupled plasma optical emission spectroscopy (ICP-OES). The blended yarn samples prepared in Examples 1-6 and Comparative Examples 1-2 were washed 50 times and then subjected to microwave digestion (nitric acid-hydrofluoric acid system). The volume was fixed to 50 mL and then the silver content was determined by ICP-OES. The retention rate was calculated by comparing the content with that of the unwashed sample. The breaking strength retention rate test was carried out under the same physical and mechanical property test conditions to compare the changes in breaking strength before and after washing. In order to eliminate test errors, each group of samples was tested in parallel 5 times. The water temperature (40±2°C) and mechanical action intensity (oscillation frequency 120rpm) were strictly controlled during the washing process to ensure the consistency of the experimental conditions. The results are shown in FIG. Figure 2 .

[0043] Fiber surface morphology characterization The microstructure of regenerated wool fibers was observed using field emission scanning electron microscopy (FE-SEM). The prepared regenerated wool fiber samples and the regenerated wool fiber samples after rubbing and washing for 10 times were fixed on conductive glue, and then a 5 nm thick gold film was sputtered by an ion sputtering instrument to enhance the conductivity. The samples were then observed under the conditions of accelerating voltage of 5 kV and working distance of 8 mm. The electron microscopy results of the regenerated wool fibers before and after rubbing and washing are shown in Figure 3. Figure 3 ; The blended yarn samples prepared in Examples 1-6 and Comparative Examples 1-2 were taken separately and treated in the same manner. The surface pore distribution and the adhesion state of the antimicrobial agent were analyzed. The pore density was statistically analyzed at 10 different fields of view (magnification 5000×). The number of pores per unit area was calculated using ImageJ image processing software. The antimicrobial agent coverage was calculated by energy spectrum analysis (EDS) combined with surface scanning mode to calculate the proportion of the silver element distribution area to the total surface area. The pore density and antimicrobial compound coverage results are shown in FIG. Figure 4 .

[0044] Environmental protection index testing Water consumption was measured according to GB / T 7119, accumulating fresh water consumption per ton of blended yarn (including processes such as washing, rinsing, and finishing). Wastewater COD was determined using the potassium dichromate method. Mixed wastewater samples discharged during production were digested and then measured for absorbance at 620 nm. COD concentrations were calculated against a standard curve. Raw material costs, including direct material expenses such as waste wool procurement, enzyme preparations, antimicrobial compounds, and functional fibers, were calculated and totaled per production batch and converted to a cost per ton of finished product. During the test, representative wastewater sampling was ensured (instantaneous samples were collected every 30 minutes and combined into a 24-minute composite sample), and indirect costs such as equipment depreciation and energy consumption were excluded. The results are shown in Table 2.

[0045] Table 1 Mechanical properties of blended yarn

[0046] The results in Table 1 show that Example 4 benefits from the dense core structure formed by high-speed spinning and the high modulus characteristics of Lyocell fiber, while the breaking strength of Comparative Example 2 decreases to 17.3 cN / tex and the hairiness index increases to 6.8 yarns / m due to the increase in the friction coefficient between fibers, verifying the protective effect of the antibacterial coating on the structural integrity of the yarn.

[0047] Figure 1 The antibacterial performance test shows that the blended yarn prepared in Example 4 has an antibacterial rate of 99.9%, and Example 6 (copper ammonium fiber + silver-loaded zeolite, antibacterial rate 99.7%) achieves a high antibacterial effect by virtue of the antibacterial property of the fiber itself and the synergistic effect of the composite agent. The high loading amount of silver-loaded zeolite (5%) and the ion release mechanism of the copper ammonium fiber form a dual bactericidal path; while Comparative Example 2 only relies on physical barrier and the antibacterial effect of the fiber itself, and the antibacterial rate is less than 75%, highlighting the necessity of surface etching and the addition of antibacterial composite agents in the regeneration process.

[0048] Figure 2 The durability test results show that the silver ion retention rate of Example 4 after 50 washes is 93.5%, which is attributed to the physical locking of the silver-loaded zeolite by the dense pore structure of the Lyocell fiber and the chemical bonding of the chitosan quaternary ammonium salt; in contrast, Example 5 (bamboo pulp fiber) has a smooth fiber surface, resulting in weak binding force of the antibacterial compound, and the silver ion retention rate is only 82.9%. The breaking strength retention rate (86.4%) is also the lowest, confirming the important influence of fiber type on functional durability.

[0049] Figure 3 The results show that the structure of regenerated wool fibers changes significantly before and after rubbing and washing, with high mechanical strength, stable properties and structure, and not easy to break.

[0050] Figure 4 The results show that the pore density and antibacterial compound coverage of the blended yarn prepared in Comparative Example 1 using new wool fiber instead of regenerated wool fiber are lower than those of the blended yarn prepared in Example 2; the pore density of the blended yarns prepared in Example 2 and Example 4 are similar, and the antibacterial compound coverage is higher than 85%, among which the pore density and antibacterial compound coverage of the blended yarn prepared in Example 4 are 16.5 / μm respectively. 2 and 92.7%, which performed better, indicating the key role of the regeneration process in surface activation.

[0051] Table 2 Environmental protection index detection

[0052] The results in Table 2 show that the process water consumption and wastewater COD value of the blended yarn prepared by the new wool fiber in Comparative Example 1 are 32.7 tons / ton of product and 145 mg / L, respectively, which are significantly higher than the process indicators of the blended yarn prepared by the regenerated wool fiber in Example 2 and Example 4, indicating a breakthrough in resource efficiency and clean production in the process of this scheme.

[0053] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.

[0054] The above description of the present invention and its embodiments is non-limiting. The drawings show only one embodiment of the present invention, and actual applications are not limited thereto. In short, if a person skilled in the art is inspired by the above and, without departing from the purpose of the present invention, devises methods and embodiments similar to the technical solution without inventiveness, they shall fall within the scope of protection of the present invention.

Claims

1. An antibacterial regenerated wool blended yarn, characterized in that: The blended yarn comprises the following raw materials in parts by weight: 35 parts of regenerated wool fiber, 25-33 parts of LF Tencel, 15-27 parts of cellulose fiber, 8-12 parts of antibacterial nylon 6 and 5 parts of antibacterial compound; The regenerated wool fiber is prepared by treating waste wool products with a biological enzyme cleaning agent, a fiber repair agent, and a softening auxiliary agent, and specifically comprises the following steps: X1: Untwist the waste wool products and treat them with a bio-enzyme cleaning agent to obtain clean fibers; X2: Immerse the clean fiber in a fiber repair agent and irradiate it with microwaves to obtain activated fiber; X3: Spray the softening agent onto the activated fiber, dry and shape it to obtain regenerated wool fiber; The antibacterial composite is prepared from the following raw materials in parts by weight: 4-5 parts of silver-loaded zeolite, 2 parts of chitosan quaternary ammonium salt, 1.5 parts of tea polyphenols, 0.5 parts of zinc sulfate, 1-2 parts of xanthan gum, 20-25 parts of deionized water, and 20-25 parts of pH 5.0 acetate buffer. The preparation method of the antibacterial composite comprises the following steps: S1: mixing and pre-dispersing silver-loaded zeolite and deionized water to obtain a dispersion, dissolving chitosan quaternary ammonium salt in pH 5.0 acetate buffer to obtain a chitosan quaternary ammonium salt solution; S2: Weighing tea polyphenols and zinc sulfate, adding them to the dispersion to perform initial mixing, and then adding chitosan quaternary ammonium salt solution to the dispersion to perform homogenization to obtain a composite solution; S3: Add xanthan gum to the composite liquid to dissolve and degas to obtain an antibacterial composite.

2. The antibacterial regenerated wool blended yarn according to claim 1, characterized in that: The cellulose fiber is selected from any one of Modal fiber, Lyocell fiber, bamboo pulp fiber and cuprammonium fiber.

3. The antibacterial regenerated wool blended yarn according to claim 1, characterized in that: The dosage of the bio-enzyme cleaning agent, fiber repair agent and softening auxiliary agent is 2.5%, 15% and 1.2% of the mass of the waste wool products respectively; The bio-enzyme cleaning agent is composed of alkaline protease and lipase in a mass ratio of 3:1; The fiber repair agent is a composite solution composed of hydroxypropyl chitosan, polyethylene glycol 4000 and trisodium citrate in a mass ratio of 5:3:2; The softening auxiliary agent consists of an organic silicon microemulsion and octadecyltrimethylammonium chloride in a mass ratio of 4:

1.

4. A production process for an antibacterial regenerated wool blended yarn according to any one of claims 1 to 3, characterized in that: The specific steps include: Step 1: Weigh regenerated wool fiber and LF Tencel and blend them to obtain core yarn; Step 2: After wrapping the core yarn with cellulose fiber, it is then intertwined with antibacterial nylon 6 to obtain the primary blended yarn; Step 3: Weigh the antibacterial compound, atomize it, and then spray it on the surface of the primary blended yarn, and shape it to obtain the antibacterial regenerated wool blended yarn.

5. The production process of an antibacterial regenerated wool blended yarn according to claim 4, characterized in that: In step 1, the yarn mixing process adopts a Z-twist process, and in step 2, the cellulose fiber wrapping core yarn process adopts an S-twist process.

Citation Information

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