阅读说明：本技术 一种抗菌纤维和抗菌羊绒纱线以及其制备方法 (Antibacterial fiber, antibacterial cashmere yarn and preparation method thereof ) 是由 金光 王进美 邱定坤 吴倩 薛惊理 郭嫣 侯会 于 2020-07-21 设计创作，主要内容包括：本发明公开了一种抗菌纤维和抗菌羊绒纱线以及其制备方法,涉及纺织技术领域,一种抗菌纤维,将羊绒、羊毛、涤纶、粘胶或棉的一种或多种采用具有壳聚糖/TiO<Sub>2</Sub>溶胶-壳聚糖/ZnO溶胶的抗菌整理剂或具有壳聚糖/TiO<Sub>2</Sub>溶胶-壳聚糖/ZnO溶胶-纳米银的抗菌整理剂利用散染设备通过浸渍吸尽法进行抗菌整理获得具有核壳结构的抗菌纤维。通过本发明抗菌纱线以及抗菌纤维制备的针织织物经50次洗涤之后,针织织物对金黄葡萄球菌、大肠杆菌、白色念珠菌的抑菌率均大于90%,并且其他基本物理机械性能均达到国家标准一等品要求。(The invention disclosesAn antibacterial fibre is prepared from one or more of cashmere, wool, terylene, viscose and cotton through preparing chitosan/TiO, and preparing the antibacterial cashmere yarn 2 Antibacterial finishing agent of sol-chitosan/ZnO sol or chitosan/TiO sol 2 The sol-chitosan/ZnO sol-nano silver antibacterial finishing agent is subjected to antibacterial finishing by a dip-exhaust method by using a disperse dyeing device to obtain the antibacterial fiber with the core-shell structure. After the knitted fabric prepared from the antibacterial yarn and the antibacterial fiber is washed for 50 times, the inhibition rates of the knitted fabric on staphylococcus aureus, escherichia coli and candida albicans are all greater than 90%, and other basic physical and mechanical properties all meet the requirements of first-class products of national standards.)

1. An antibacterial fibre is prepared from one or more of cashmere, wool, terylene, viscose and cotton through mixing with chitosan/TiO₂Antibacterial finishing agent of sol-chitosan/ZnO sol or chitosan/TiO sol₂The sol-chitosan/ZnO sol-nano silver antibacterial finishing agent is subjected to antibacterial finishing by a dip-exhaust method by using a disperse dyeing device to obtain the antibacterial fiber with the core-shell structure.

2. An antimicrobial finish for antimicrobial fibres as claimed in claim 1, characterised in that the antimicrobial finish is made of chitosan/TiO₂The sol, the chitosan/ZnO sol, the nano silver solution, the waterborne polyurethane and the emulsifying dispersant are prepared or are prepared by chitosan/TiO₂Sol, chitosan/ZnO sol, waterborne polyurethane and emulsifying dispersant.

3. A process for the preparation of an antimicrobial finish according to claim 2, comprising the steps of:

step A: preparation of Chitosan/TiO₂The sol is prepared by taking 1 part by mass of butyl titanate, 0.6-0.8 part by mass of chitosan, 20-part by mass of absolute ethyl alcohol, 8-10 parts by mass of water and 0.8-1.2 parts by mass of ammonia water, firstly mixing 2/3 volumes of absolute ethyl alcohol, ammonia water and butyl titanate, putting the mixture on a magnetic stirrer to be uniformly stirred to form solution A, then carrying out water bath on the solution A at the pH value of 7-8 and the temperature of 30-40 ℃, then mixing 1/3 volumes of absolute ethyl alcohol, chitosan and water to prepare solution B, then gradually dripping the solution B into the solution A in the water bath, carrying out ultrasonic dispersion on the solution A in the dripping process, and continuously stirring the solution A and the solution B after mixing until creamy yellow chitosan/TiO is obtained₂Sol;

and B: preparing chitosan/ZnO sol, dissolving 5-6% of chitosan in 94-95% of ethanol by mass percent to form a chitosan ethanol solution, dissolving 5-7 parts by mass of zinc acetate Zn (Ac) 2.2H 2O in 50-70 parts by mass of boiling chitosan ethanol solution, cooling to 0 ℃ and supplementing volatilized ethanol to obtain solution C, dissolving 5-7 parts of lithium hydroxide powder in 50-60 parts of ethanol by ultrasonic wave at room temperature, cooling to 0 ℃ to obtain solution D, slowly adding the solution D into the solution C under the action of ultrasonic waves at 0 ℃, then continuously adding 100-200 parts of n-hexane, generating white precipitate under the action of continuous ultrasonic waves, filtering after the precipitate is completely precipitated, and filtering for several times to obtain non-precipitate milky chitosan/ZnO sol;

and C: mixing chitosan/TiO 2 sol, chitosan/ZnO sol and deionized water to form a chitosan cation solution under the conditions of vacuum degree of-0.1 to-0.2 mpa and 16000-;

step D: mixing 25-50 parts by mass of chitosan cation liquid-phase monodisperse composite nano solution, 8-10 parts by mass of aqueous polyurethane solution and 40-67 parts by mass of deionized water to obtain chitosan cation finishing agent solution.

4. A process for the preparation of an antimicrobial finish according to claim 2, comprising the steps of:

step A: preparation of Chitosan/TiO₂The sol is prepared by taking 1 part by mass of butyl titanate, 0.6-0.8 part by mass of chitosan, 20-part by mass of absolute ethyl alcohol, 8-10 parts by mass of water and 0.8-1.2 parts by mass of ammonia water, firstly mixing 2/3 volumes of absolute ethyl alcohol, ammonia water and butyl titanate, putting the mixture on a magnetic stirrer to be uniformly stirred to form solution A, then carrying out water bath on the solution A at the pH value of 7-8 and the temperature of 30-40 ℃, then mixing 1/3 volumes of absolute ethyl alcohol, chitosan and water to prepare solution B, then gradually dripping the solution B into the solution A in the water bath, carrying out ultrasonic dispersion on the solution A in the dripping process, and continuing stirring the solution A and the solution B after mixing until the solution A and the solution B are stirred until the solution A and the solution B are uniformly stirredObtaining creamy yellow chitosan/TiO₂Sol;

and B: preparing chitosan/ZnO sol, dissolving 5-6% of chitosan in 94-95% of ethanol by mass percent to form a chitosan ethanol solution, dissolving 5-7 parts by mass of zinc acetate Zn (Ac) 2.2H 2O in 50-70 parts by mass of boiling chitosan ethanol solution, cooling to 0 ℃ and supplementing volatilized ethanol to obtain solution C, dissolving 5-7 parts of lithium hydroxide powder in 50-60 parts of ethanol by ultrasonic wave at room temperature, cooling to 0 ℃ to obtain solution D, slowly adding the solution D into the solution C under the action of ultrasonic waves at 0 ℃, then continuously adding 100-200 parts of n-hexane, generating white precipitate under the action of continuous ultrasonic waves, filtering after the precipitate is completely precipitated, and filtering for several times to obtain non-precipitate milky chitosan/ZnO sol;

and C: mixing chitosan/TiO 2 sol, chitosan/ZnO sol and deionized water to form a chitosan cation solution under the conditions of vacuum degree of-0.1 to-0.2 mpa and 16000-;

step D: mixing 25-50 parts by mass of chitosan cation liquid-phase monodisperse composite nano solution, 8-10 parts by mass of aqueous polyurethane solution and 40-67 parts by mass of deionized water to obtain chitosan cation finishing agent solution;

step E: adding 100 parts by mass of the chitosan cation finishing agent solution into 20-40 parts by mass of liquid-phase monodisperse nano silver ion sol, wherein the content of nano silver is not less than 50 ppm, and then stirring for 1-3 hours to form the nano silver chitosan cation composite finishing agent solution.

5. A method for preparing antibacterial fiber according to claim 1, characterized in that, firstly, one or more of cashmere, wool, terylene, viscose or cotton is soaped to remove residual oil agent and wax on the fiber;

weighing 2-4% of an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol or an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol-nano silver according to the weight of the fiber;

then weighing 70-100% of deionized water and an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol or an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol-nano silver according to the weight of the fiber to prepare an antibacterial finishing liquid;

and then spraying the antibacterial finishing liquid on the fibers in a drum dryer by using a spraying device, impregnating after the spraying is finished, wherein the impregnating time is 1-1.5 hours, drying after the impregnating is finished, and gradually raising the temperature to 110-120 ℃ for baking for 5-10 minutes.

6. The method of claim 5, wherein the fibers are dyed before the antimicrobial finish is applied to the fibers.

7. An antibacterial cashmere yarn, which is characterized in that the antibacterial cashmere yarn is formed by blending cashmere fibers and one or more antibacterial fibers in claim 1 through the steps of wool blending, carding, spun yarn spinning, spooling, doubling and double twisting;

or the cashmere antibacterial fiber in claim 1 and one or more antibacterial fibers in claim 1 are blended through the steps of wool blending, carding, spinning, winding, doubling and two-for-one twisting.

8. A process for the preparation of an antibacterial cashmere yarn according to claim 7, characterized in that it comprises the following steps,

step A: mixing the mixed fibers, opening the mixed fibers by an opener during mixing, then adding the crude oil, sealing down for at least 10 hours, and controlling the on-machine moisture regain within 15 +/-10% during mixing;

and B: carding the mixed fibers, wherein the distance of a carding area is 7-10 threads during carding;

and C: carrying out spinning treatment on the mixed fiber, wherein the back zone draft multiple is as follows: 1.15-1.35, spinning frame rotating speed: 6000 rpm-8500 rpm, rear zone spacing: 60 mm-75 mm;

step D: performing spooling treatment on the mixed fiber, wherein the spinning speed is 250-650 m/min, and the fixed length is set to 28600 m;

step E: performing doubling treatment on the mixed fibers, wherein the speed is 250-650 m/min, and the fixed length is 14300 m;

step F: and (3) carrying out double-twisting treatment on the mixed fibers, wherein the speed is 5000-7000 rpm, and the twisting direction is Z.

9. The method of claim 8, wherein in step a, the wool agent comprises FX-906 and wool oil 3% and FX-AS301 antistatic agent 1.5% by weight.

Technical Field

The invention relates to the technical field of spinning, in particular to an antibacterial fiber, a fiber antibacterial agent and an antibacterial yarn.

Background

Antibacterial textiles have a long history, and ancient Egypt people used certain medicinal plants for antibacterial purposes in a protective wrap around mummy buried in a pyramid four thousand years ago. In recent years, as the requirement for human health and comfort wearing is increasing, antibacterial textiles as health functional fabrics and health functional fabrics are rapidly developed to meet the social demands, and the research of antibacterial textiles is active in various countries. However, the series of products at home and abroad have certain defects in the aspects of variety and quality, the antibacterial effect and the washing-resistant effect of the antibacterial products are not ideal enough, and particularly, some antibacterial finishing agents have certain physiological toxicity to human bodies, and the research and development of reinforcing antibacterial and antimicrobial textiles have important research significance for guaranteeing the health of people, improving the grade of the textiles and increasing the added value of the textiles.

Disclosure of Invention

The invention provides an antibacterial fiber, an antibacterial finishing agent, a preparation method of the antibacterial fiber, an antibacterial cashmere yarn and a preparation method of the antibacterial cashmere yarn aiming at the defects in the prior art. The antibacterial fiber in the application is simple to manufacture, good in physical performance, and suitable for different weaving methods, has a good antibacterial effect under the condition that the original fiber performance is not changed, and is wide in application range. The antibacterial cashmere yarn has the comfort characteristic of cashmere and has a good antibacterial effect.

After the knitted fabric prepared from the antibacterial yarn and the antibacterial fiber is washed for 50 times, the bacteriostatic rates of the knitted fabric on staphylococcus aureus, escherichia coli and candida albicans are all greater than 90%, and other basic physical and mechanical properties all meet the requirements of first-class products of national standards.

In order to solve the technical problem, the invention is solved by the following technical scheme: an antibacterial fiber is prepared from one or more of cashmere, wool, dacron, viscose and cotton by adding chitosan/TiO₂Antibacterial finishing agent of sol-chitosan/ZnO sol or chitosan/TiO sol₂The sol-chitosan/ZnO sol-nano silver antibacterial finishing agent is subjected to antibacterial finishing by a dip-exhaust method by using a disperse dyeing device to obtain the antibacterial fiber with the core-shell structure.

An antibacterial finishing agent is prepared from chitosan/TiO₂The sol, the chitosan/ZnO sol, the nano silver solution, the waterborne polyurethane and the emulsifying dispersant are prepared or are prepared by chitosan/TiO₂Sol, chitosan/ZnO sol, waterborne polyurethane and emulsifying dispersant.

A preparation method of the antibacterial finishing agent comprises the following steps: step A: preparation of Chitosan/TiO₂The sol is prepared from (by mass) butyl titanate 1 part, chitosan 0.6-0.8 part, and chitosan 20-partsFirstly, 2/3 volumes of absolute ethyl alcohol, ammonia water and butyl titanate are mixed, the mixture is put on a magnetic stirrer to be uniformly stirred into solution A, then the solution A is subjected to water bath at the pH value of 7-8 and the temperature of 30-40 ℃, 1/3 volumes of absolute ethyl alcohol, chitosan and water are mixed to prepare solution B, the solution B is gradually dripped into the solution A in the water bath, the solution A is subjected to ultrasonic dispersion in the dripping process, the solution A and the solution B are mixed and then continuously stirred until creamy yellow chitosan/TiO is obtained₂Sol; and B: preparing chitosan/ZnO sol, dissolving 5-6% of chitosan in 94-95% of ethanol by mass percent to form a chitosan ethanol solution, dissolving 5-7 parts by mass of zinc acetate Zn (Ac) 2.2H 2O in 50-70 parts by mass of boiling chitosan ethanol solution, cooling to 0 ℃ and supplementing volatilized ethanol to obtain solution C, dissolving 5-7 parts of lithium hydroxide powder in 50-60 parts of ethanol by ultrasonic wave at room temperature, cooling to 0 ℃ to obtain solution D, slowly adding the solution D into the solution C under the action of ultrasonic waves at 0 ℃, then continuously adding 100-200 parts of n-hexane, generating white precipitate under the action of continuous ultrasonic waves, filtering after the precipitate is completely precipitated, and filtering for several times to obtain non-precipitate milky chitosan/ZnO sol; and C: mixing chitosan/TiO 2 sol, chitosan/ZnO sol and deionized water to form a chitosan cation solution under the conditions of vacuum degree of-0.1 to-0.2 mpa and 16000-; step D: mixing 25-50 parts by mass of chitosan cation liquid-phase monodisperse composite nano solution, 8-10 parts by mass of aqueous polyurethane solution and 40-67 parts by mass of deionized water to obtain chitosan cation finishing agent solution.

The preparation method of the other antibacterial finishing agent comprises the following stepsThe method comprises the following steps: step A: preparation of Chitosan/TiO₂The sol is prepared by taking 1 part by mass of butyl titanate, 0.6-0.8 part by mass of chitosan, 20-part by mass of absolute ethyl alcohol, 8-10 parts by mass of water and 0.8-1.2 parts by mass of ammonia water, firstly mixing 2/3 volumes of absolute ethyl alcohol, ammonia water and butyl titanate, putting the mixture on a magnetic stirrer to be uniformly stirred to form solution A, then carrying out water bath on the solution A at the pH value of 7-8 and the temperature of 30-40 ℃, then mixing 1/3 volumes of absolute ethyl alcohol, chitosan and water to prepare solution B, then gradually dripping the solution B into the solution A in the water bath, carrying out ultrasonic dispersion on the solution A in the dripping process, and continuously stirring the solution A and the solution B after mixing until creamy yellow chitosan/TiO is obtained₂Sol; and B: preparing chitosan/ZnO sol, dissolving 5-6% of chitosan in 94-95% of ethanol by mass percent to form a chitosan ethanol solution, dissolving 5-7 parts by mass of zinc acetate Zn (Ac) 2.2H 2O in 50-70 parts by mass of boiling chitosan ethanol solution, cooling to 0 ℃ and supplementing volatilized ethanol to obtain solution C, dissolving 5-7 parts of lithium hydroxide powder in 50-60 parts of ethanol by ultrasonic wave at room temperature, cooling to 0 ℃ to obtain solution D, slowly adding the solution D into the solution C under the action of ultrasonic waves at 0 ℃, then continuously adding 100-200 parts of n-hexane, generating white precipitate under the action of continuous ultrasonic waves, filtering after the precipitate is completely precipitated, and filtering for several times to obtain non-precipitate milky chitosan/ZnO sol; and C: mixing chitosan/TiO 2 sol, chitosan/ZnO sol and deionized water to form a chitosan cation solution under the conditions of vacuum degree of-0.1 to-0.2 mpa and 16000-; step D: mixing 25-50 parts by mass of chitosan cation liquid phase monodisperse composite nano solution, 8-10 parts by mass of aqueous polyurethane solution and 40-67 parts by mass of deionized water to obtainTo a chitosan cationic finishing agent solution; step E: adding 100 parts by mass of the chitosan cation finishing agent solution into 20-40 parts by mass of liquid-phase monodisperse nano silver ion sol, wherein the content of nano silver is not less than 50 ppm, and then stirring for 1-3 hours to form the nano silver chitosan cation composite finishing agent solution.

A preparation method of antibacterial fiber comprises soaping one or more of cashmere, wool, terylene, viscose or cotton to remove residual oil and wax; weighing 2-4% of an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol or an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol-nano silver according to the weight of the fiber; then weighing 70-100% of deionized water and an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol or an antibacterial finishing agent with chitosan/TiO 2 sol-chitosan/ZnO sol-nano silver according to the weight of the fiber to prepare an antibacterial finishing liquid; and then spraying the antibacterial finishing liquid on the fibers in a drum dryer by using a spraying device, impregnating after the spraying is finished, wherein the impregnating time is 1-1.5 hours, drying after the impregnating is finished, and gradually raising the temperature to 110-120 ℃ for baking for 5-10 minutes.

Preferably, in the above technical solution, before the antibacterial finishing liquid is sprayed to the fibers, the fibers may be dyed first.

An antibacterial cashmere yarn is formed by blending cashmere fibers and one or more antibacterial fibers in claim 1 through the steps of wool blending, carding, spun yarn spinning, spooling, doubling and double twisting; or the cashmere antibacterial fiber in claim 1 and one or more antibacterial fibers in claim 1 are blended through the steps of wool blending, carding, spinning, winding, doubling and two-for-one twisting.

A preparation method of antibacterial cashmere yarns comprises the following steps: mixing the mixed fibers, opening the mixed fibers by an opener during mixing, then adding the crude oil, sealing down for at least 10 hours, and controlling the on-machine moisture regain within 22 +/-2% during mixing; and B: carding the mixed fibers, wherein the distance between carding areas is 7-10 filaments during carding; and C: carrying out spinning treatment on the mixed fiber, wherein the back zone draft multiple is as follows: 1.15-1.35, spinning frame rotating speed: 6000-8500 r/min, rear zone spacing: 60-75 mm; step D: performing spooling treatment on the mixed fiber, wherein the spinning speed is 250-650 m/min, and the fixed length is set to 28600 m; step E: performing doubling treatment on the mixed fibers, wherein the speed is 250-650 m/min, and the fixed length is 14300 m; step F: and (3) carrying out double-twisting treatment on the mixed fibers, wherein the speed is 5000-7000 rpm, and the twisting direction is Z.

Preferably, in the technical scheme, in the step A, the wool agent comprises 3% of FX-906 and wool oil and 1.5% of FX-AS301 antistatic agent in percentage by mass.

The application provides an antibacterial fiber, an antibacterial finishing agent and an antibacterial cashmere yarn. Wherein the antibacterial finishing agent is prepared by using an ultrasonic monodisperse technology under the protection of Chitosan (CS) cationic protein₂ZnO nano micelle structure antibacterial material made of chitosan TiO₂And ZnO composite nano sol is taken as a base and is compounded with advanced high molecular adhesive to further prepare nano silver composite nano antibacterial material to form the nano antibacterial finishing agent. The principle is that chitosan and TiO are respectively sheared by a vacuum high-speed shearing method₂The ZnO composite nano sol, the nano silver composite material, the high molecular adhesive and the emulsifying dispersant are compounded to form the excellent broad-spectrum nano silver antibacterial finishing agent. The antibacterial fiber is prepared by adopting a dipping exhaustion method for dyed fibers and utilizing spray dipping to finish the fibers in a drum dryer to form antibacterial cashmere, wool, terylene, viscose and cotton fibers with a core-shell structure. The antibacterial cashmere yarn is developed by adopting a carded wool spinning yarn blended by different fibers, and comprises novel wool and finish oil agent selection, a special carded wool carding process and a spun yarn process.

After the knitted fabric prepared from the antibacterial yarn and the antibacterial fiber is washed for 50 times, the inhibition rates of the knitted fabric on staphylococcus aureus, escherichia coli and candida albicans are all greater than 90%, and other basic physical and mechanical properties all meet the requirements of first-class products of national standards. The antibacterial fiber and the antibacterial yarn can be widely applied to processing various health functional textiles so as to meet the requirements of daily clothes, medical protection, household, outdoor, occupational and other textile products, and have important social and economic significance.

Detailed Description