Plant source composite ultra-short fiber containing xylitol and preparation method of plant source composite ultra-short fiber

Abstract

The invention relates to the technical field of textile, in particular to a xylitol-containing plant-source composite ultra-short fiber and a preparation method thereof.The xylitol-containing plant-source composite ultra-short fiber comprises an ultra-short fiber base material and plant-source functional particles, the plant-source functional particles are obtained by conducting chemical modification, microencapsulation and nanocrystallization treatment on citramalic acid, xylitol and plant-source extracts, and the plant-source functional particles are prepared from the ultra-short fiber base material and the plant-source extracts. According to the present invention, the heat absorption characteristic of xylitol is utilized to achieve the contact cool feeling effect, the antibacterial components of the plant source extract are adopted to form the antibacterial barrier so as to prevent the growth and the reproduction of bacteria and achieve the antibacterial effect, and the stability of the functional components is significantly enhanced through the chemical modification of citramalic acid; microencapsulation and nanocrystallization treatment improve the dispersibility and compatibility of the plant-derived functional particles in fibers and ensure more lasting and effective functional performance, and meanwhile, the components of the plant-derived functional particles are all derived from the nature and have the characteristics of reproducibility and degradability, so that the plant-derived functional particles can effectively replace traditional organic synthesis functional modification aids.

Description

Technical Field

[0001] The invention relates to the technical field of textiles, in particular to a plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof. Background Art

[0002] Ultra-short fibers refer to any short fibers with a cut length of less than 20 mm. They have high breaking strength, low breaking elongation, low shrinkage in boiling water and hot air, a cut length shorter than that of conventional short fibers, high dispersibility in the medium, antistatic properties, etc. During the textile processing, on the one hand, they are easier to mix evenly with other fibers to form a more stable and uniform yarn structure, thereby improving the quality and production efficiency of textiles; on the other hand, their relatively short length also facilitates special processing techniques such as non-woven fabrics, and can be directly made into products of various shapes and uses through processes such as combing, laying nets, and reinforcement.

[0003] As people pay more and more attention to health, in order to meet consumers' increasingly diversified demands for textiles, ultra-short fibers can be developed in a multifunctional direction by blending with other fibers or self-modification, and develop products with basic properties such as moisture absorption, breathability, softness and comfort. However, most of the existing functional modification additives are chemical reagents, and there are few related studies on the use of plant-based functional modification additives. In view of this, we propose a plant-based composite ultra-short fiber containing xylitol and a preparation method thereof. Summary of the invention

[0004] The object of the present invention is to provide a plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, so as to solve the problems raised in the above-mentioned background technology.

[0005] To achieve the above-mentioned purpose, the present invention provides a plant-based composite ultra-short fiber containing xylitol, comprising an ultra-short fiber substrate and plant-based functional particles, wherein the plant-based functional particles are obtained by chemically modifying, microencapsulating and nano-processing citramalic acid, xylitol and a plant-based extract.

[0006] Preferably, the preparation method of the plant-derived functional particles is as follows: S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 80-100°C, continue stirring, turn on the vacuum pump, turn it off after 10-15 minutes, keep it on for 20-30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 2-4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature to 80-100°C, exhaust temperature to 60-80°C, pump speed to 5-15mL / min, nozzle pressure to 0.2-0.4MPa, air flow rate to 300-600m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3. Use zirconium oxide with a diameter of 0.1-1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium at a ratio of 10 to 15:1, use a ball mill, set the speed to 300-600 rpm, and the ball milling time to 3-5 hours. Separate the larger particles through a sieve to obtain plant-derived functional particles.

[0007] Preferably, in S1.1, the plant-derived extract is selected from one or more combinations of Japanese cypress extract, sunflower extract, jasmine extract, white magnolia extract, and camellia extract; the mass ratio of citramalic acid, xylitol and plant-derived extract is 14:5-7:4-8; and the amount of p-toluenesulfonic acid added is 1-3% of the total mass of citramalic acid, xylitol and plant-derived extract.

[0008] Preferably, in S1.2, the wall material is selected from any one of gelatin, gum arabic, chitosan, polylactic acid, and polyurethane; the mass ratio of the chemically modified plant source to the wall material is 1:4-8; and the amount of Tween 80 added is 0.5-2% of the total mass of the chemically modified plant source and the wall material.

[0009] Preferably, in S1.3, the particle size of the plant-derived functional particles is 100-500 nm.

[0010] Preferably, the substrate of the ultrashort fibers includes a regenerated cellulose fiber substrate or a synthetic fiber substrate, the regenerated cellulose fiber substrate is any one of viscose fiber, modal fiber, and lyocell fiber pulp, and the synthetic fiber substrate includes any one of polyester chips and polyamide chips.

[0011] Due to their extremely short length, ultra-short fibers have a larger surface area per unit mass, which enables them to be better dispersed in composites and increases the contact area with other components. When used as the reinforcing phase of a composite material, ultra-short fibers can provide additional strength and modulus without significantly increasing the weight.

[0012] Xylitol is a five-carbon sugar alcohol. Since xylitol absorbs heat when dissolved on the skin surface, it can provide a cool feeling to the fiber. Japanese cypress extract, sunflower extract, jasmine extract, magnolia extract and camellia plant extract all have antibacterial properties. For example, Japanese cypress extract contains hinokitiol, which has antioxidant and anti-infection effects, and can therefore provide an antibacterial effect to the fiber.

[0013] However, since xylitol, Japanese cypress extract, sunflower extract, jasmine extract, white magnolia extract and camellia plant extract contain active hydroxyl and amino functional groups and are sensitive to water, heat and light, they are chemically modified with citramalic acid to undergo esterification and amidation with the active hydroxyl and amino functional groups, thereby reducing the degree of exposure of the active functional groups during the spinning process, thereby reducing their sensitivity to water, heat and light factors and improving the stability of the plant source. Microencapsulation can further protect the active components of the plant source and provide a gradual release of the active ingredients, thereby improving the stability and durability of the plant source. On the other hand, the microencapsulated particles have good fluidity and dispersibility, which helps to be more evenly distributed in the spinning solution or melt. Finally, nano-processing is performed. First, nano-scale particles are more easily dispersed evenly in the matrix, reducing the possibility of agglomeration and improving the fiber material. Consistency and uniformity. Secondly, nano-sized particles have a larger specific surface area, which means that more xylitol and plant extracts can come into contact with the skin, thereby enhancing the cooling effect and antibacterial functional performance. Finally, due to the small size of nanoparticles, they can penetrate deeper into the fiber or come into closer contact with the skin surface, providing a more delicate and soft feel. At the same time, they can also better fit the human body curve and improve wearing comfort. Therefore, a plant-derived composite material with good dispersion, stability and compatibility is obtained through chemical modification, microencapsulation and nano-treatment. It is suitable for the ultra-short fiber preparation process of regenerated cellulose fiber substrates and synthetic fiber substrates, has good market application value, and can meet the special functional requirements of textiles in different fields, such as traditional underwear, sportswear, outdoor clothing, fashionable women's wear, bedding, curtains, sofa fabrics, carpets and disposable medical supplies.

[0014] On the other hand, the present invention provides a method for preparing plant-based composite ultra-short fibers containing xylitol, which is used for any of the plant-based composite ultra-short fibers containing xylitol described above, including the preparation, spinning, drying and mechanical cutting of plant-based functional particle spinning solution or plant-based functional particle melt solution.

[0015] Preferably, the specific preparation steps of preparing the plant-derived composite ultra-short fibers containing xylitol by using the plant-derived functional particle spinning solution are as follows: The treated regenerated cellulose fiber substrate is dissolved and mixed, and plant-derived functional particles are added. A high-shear mixer is used to fully stir and disperse the particles. The mixed solution is filtered to obtain a plant-derived functional particle spinning solution. The plant-derived functional particle spinning solution is extruded from a nozzle in a spinning machine to form continuous fibers. After the fibers are solidified, they are cleaned to remove residual chemicals, dried, and mechanical cutting devices are used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0016] Preferably, the specific preparation steps of preparing the plant-based composite ultra-short fibers containing xylitol by using the plant-based functional particle melt are as follows: The synthetic fiber substrate is heated and melted, and mixed with plant-derived functional particles to obtain a molten liquid of plant-derived functional particles, which is then extruded through a melt spinning machine to obtain continuous fibers. After the fibers are solidified, they are dried and a mechanical cutting device is used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0017] Preferably, the added amount of the plant-source functional particles is 26-35% of the mass of the plant-source functional particle spinning solution, and the added amount of the plant-source functional particles is 26-35% of the mass of the plant-source functional particle melt. The diameter of the plant-source composite ultra-short fibers containing xylitol is 0.1-1mm and the length is 1-5mm.

[0018] Compared with the prior art, the present invention has the following beneficial effects: In the plant-based composite ultra-short fiber containing xylitol and the preparation method thereof, citramalic acid, xylitol and plant-based extracts are chemically modified, microencapsulated and nano-processed to obtain plant-based functional particles, which are then composited with a fiber substrate to obtain plant-based composite ultra-short fibers with more stable and uniform performance, providing basic materials for the development of high-end, high-performance textiles. In addition, by introducing natural plant-based functional additives such as xylitol and plant-based extracts, the fibers are modified to give the fibers excellent antibacterial, cooling and other functions, thereby meeting the special functional requirements of textiles in different fields and having broad application prospects.

[0019] After testing, the xylitol plant-derived composite ultra-short fibers prepared by the present invention have good functional durability. After being washed 100 times, the loss rate of the antibacterial rate against common bacteria (Staphylococcus aureus, Escherichia coli, Candida albicans) was less than 3%. According to the microspectral LC-MSMS test results, the maximum xylitol content was 9314.13 mg / kg after baking at 80°C for 1 hour. DETAILED DESCRIPTION

[0020] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of 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.

[0021] The plant-derived composite ultra-short fiber containing xylitol of the present invention comprises an ultra-short fiber substrate and plant-derived functional particles, wherein the plant-derived functional particles are obtained by chemically modifying, microencapsulating and nano-processing citramalic acid, xylitol and a plant-derived extract; Among them, the plant-derived extract is preferably Japanese cypress extract; the wall material is preferably gum arabic; the substrate of the ultra-short fiber includes a regenerated cellulose fiber substrate and a synthetic fiber substrate, the regenerated cellulose fiber substrate is preferably viscose fiber pulp, and the synthetic fiber substrate is preferably polyester chips; The specific preparation steps of the regenerated cellulose fiber substrate are: The viscose fiber pulp is immersed in a sodium hydroxide solution with a mass fraction of 18-20%, and the alkalization temperature is 20-25°C to form alkali cellulose, and the alkali cellulose is squeezed to remove excess alkali solution and crushed, and the crushed alkali cellulose is mixed with carbon disulfide for yellowing, and the mass ratio of carbon disulfide to alkali cellulose is 1:2-3, and the temperature is maintained at 20-30°C. The yellowing time is 50-60min to form cellulose xanthate, and the generated cellulose xanthate is dissolved in a sodium hydroxide solution with a mass fraction of 3-5%, to obtain a regenerated cellulose fiber substrate; Embodiment 1: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:5:4; the amount of p-toluenesulfonic acid added is 1% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:5; the amount of Tween 80 added is 1% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 300nm; the amount of plant-derived functional particles added is 26% of the mass of the plant-derived functional particle spinning solution, and the diameter of the plant-derived composite ultra-short fiber containing xylitol is 1mm and the length is 5mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The treated regenerated cellulose fiber substrate is dissolved and mixed, and plant-derived functional particles are added. A high-shear mixer is used to fully stir and disperse the particles. The mixed solution is filtered to obtain a plant-derived functional particle spinning solution. The plant-derived functional particle spinning solution is extruded from a nozzle in a spinning machine to form continuous fibers. After the fibers are solidified, they are cleaned to remove residual chemicals, dried, and mechanical cutting devices are used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0022] Embodiment 2: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:6:6; the amount of p-toluenesulfonic acid added is 1% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:5; the amount of Tween 80 added is 1% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 300nm; the amount of plant-derived functional particles added is 30% of the mass of the plant-derived functional particle spinning solution, and the diameter of the plant-derived composite ultra-short fiber containing xylitol is 1mm and the length is 5mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The treated regenerated cellulose fiber substrate is dissolved and mixed, and plant-derived functional particles are added. A high-shear mixer is used to fully stir and disperse the particles. The mixed solution is filtered to obtain a plant-derived functional particle spinning solution. The plant-derived functional particle spinning solution is extruded from a nozzle in a spinning machine to form continuous fibers. After the fibers are solidified, they are cleaned to remove residual chemicals, dried, and mechanical cutting devices are used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0023] Example 3: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:7:8; the amount of p-toluenesulfonic acid added is 1% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:5; the amount of Tween 80 added is 1% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 300nm; the amount of plant-derived functional particles added is 35% of the mass of the plant-derived functional particle spinning solution, and the diameter of the plant-derived composite ultra-short fiber containing xylitol is 1mm and the length is 5mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The treated regenerated cellulose fiber substrate is dissolved and mixed, and plant-derived functional particles are added. A high-shear mixer is used to fully stir and disperse the particles. The mixed solution is filtered to obtain a plant-derived functional particle spinning solution. The plant-derived functional particle spinning solution is extruded from a nozzle in a spinning machine to form continuous fibers. After the fibers are solidified, they are cleaned to remove residual chemicals, dried, and mechanical cutting devices are used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0024] Example 4: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:7:8; the amount of p-toluenesulfonic acid added is 3% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:8; the amount of Tween 80 added is 2% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 100nm; the amount of plant-derived functional particles added is 35% of the plant-derived functional particle spinning solution, and the diameter of the plant-derived composite ultra-short fiber containing xylitol is 0.5mm and the length is 3mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The treated regenerated cellulose fiber substrate is dissolved and mixed, and plant-derived functional particles are added. A high-shear mixer is used to fully stir and disperse the particles. The mixed solution is filtered to obtain a plant-derived functional particle spinning solution. The plant-derived functional particle spinning solution is extruded from a nozzle in a spinning machine to form continuous fibers. After the fibers are solidified, they are cleaned to remove residual chemicals, dried, and mechanical cutting devices are used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0025] Example 5: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:5:4; the amount of p-toluenesulfonic acid added is 1% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:5; the amount of Tween 80 added is 1% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 300nm; the amount of plant-derived functional particles added is 26% of the mass of the plant-derived functional particle melt, and the diameter of the plant-derived composite ultra-short fiber containing xylitol is 1mm and the length is 5mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The synthetic fiber substrate is heated and melted, and mixed with plant-derived functional particles to obtain a molten liquid of plant-derived functional particles, which is then extruded through a melt spinning machine to obtain continuous fibers. After the fibers are solidified, they are dried and a mechanical cutting device is used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0026] Example 6: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:6:6; the amount of p-toluenesulfonic acid added is 1% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:5; the amount of Tween 80 added is 1% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 300nm; the amount of plant-derived functional particles added is 30% of the mass of the plant-derived functional particle melt, and the diameter of the plant-derived composite ultrashort fiber containing xylitol is 1mm and the length is 5mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The synthetic fiber substrate is heated and melted, and mixed with plant-derived functional particles to obtain a molten liquid of plant-derived functional particles, which is then extruded through a melt spinning machine to obtain continuous fibers. After the fibers are solidified, they are dried and a mechanical cutting device is used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0027] Example 7: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:7:8; the amount of p-toluenesulfonic acid added is 1% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:5; the amount of Tween 80 added is 1% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 300nm; the amount of plant-derived functional particles added is 35% of the mass of the plant-derived functional particle melt, and the diameter of the plant-derived composite ultra-short fiber containing xylitol is 1mm and the length is 5mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The synthetic fiber substrate is heated and melted, and mixed with plant-derived functional particles to obtain a molten liquid of plant-derived functional particles, which is then extruded through a melt spinning machine to obtain continuous fibers. After the fibers are solidified, they are dried and a mechanical cutting device is used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0028] Example 8: A plant-derived composite ultra-short fiber containing xylitol and a preparation method thereof, comprising the following steps: The mass ratio of citramalic acid, xylitol and plant-derived extract is 14:7:8; the amount of p-toluenesulfonic acid added is 3% of the total mass of citramalic acid, xylitol and plant-derived extract; the mass ratio of chemically modified plant source to wall material is 1:8; the amount of Tween 80 added is 2% of the total mass of chemically modified plant source and wall material; the particle size of plant-derived functional particles is 100nm; the amount of plant-derived functional particles added is 35% of the mass of the plant-derived functional particle melt, and the diameter of the plant-derived composite ultra-short fiber containing xylitol is 0.5mm and the length is 3mm; S1.1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 90°C, continue stirring, turn on the vacuum pump, turn it off after 10 minutes, keep it on for 30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature at 80°C, exhaust temperature at 60°C, pump speed at 10mL / min, nozzle pressure at 0.3MPa, air flow rate at 500m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.3, using zirconium oxide with a diameter of 1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium in a ratio of 10:1, use a ball mill, set the speed to 400 rpm, the ball milling time to 5 h, separate the larger particles through a sieve, and obtain the plant-derived functional particles; The synthetic fiber substrate is heated and melted, and mixed with plant-derived functional particles to obtain a molten liquid of plant-derived functional particles, which is then extruded through a melt spinning machine to obtain continuous fibers. After the fibers are solidified, they are dried and a mechanical cutting device is used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

[0029] Comparative Example 1: The method of Example 3 was adopted without adding plant-derived functional particles.

[0030] Comparative Example 2: The method of Example 7 was adopted without adding plant-derived functional particles.

[0031] Comparative Example 3: The method of Example 3 was adopted, and xylitol and the plant-derived extract were directly used without modifying the xylitol and the plant-derived extract by citramalic acid.

[0032] Comparative Example 4: The method of Example 7 was adopted, and xylitol and the plant-derived extract were directly used without modifying the xylitol and the plant-derived extract by citramalic acid.

[0033] The present invention uses plant-derived functional particles to prepare plant-derived composite ultra-short fibers containing xylitol, wherein the performance index inspection items and inspection standards of the plant-derived composite ultra-short fibers containing xylitol are as follows: According to GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method", the antibacterial rate was tested. The samples were washed 100 times by a household double-tub washing machine, sterilized by high-pressure steam, and then incubated with the bacterial solution for 18 hours. Among them, Klebsiella pneumoniae ATCC 4352: 3.3×10 5 CFU / mL, Staphylococcus aureus ATCC 6538: 3.2×10 5 CFU / mL, E. coli 8099: 3.2×10 5 CFU / mL, Candida albicans ATCC 10231: 3.1×10 5 CFU / mL.

[0034] According to GB / T 35263.2017 "Testing and Evaluation of the Instantaneous Cooling Performance of Textiles upon Contact", testing the cooling coefficient is an important parameter to measure the instantaneous cooling performance of textiles upon contact. It mainly relies on the principle of heat conduction to evaluate the instantaneous cooling effect produced when the fiber or fabric surface comes into contact with the skin. It reflects the speed at which heat is transferred from the skin to the fabric when the skin (or a thermal probe simulating the skin) comes into contact with the fabric surface.

[0035] According to the above standards, the plant-derived composite ultra-short fibers containing xylitol prepared in the above Examples 1-8 and Comparative Examples 1-4 were tested, and the obtained data are shown in Table 1: Table 1 Performance data of Examples 1-8 and Comparative Examples 1-4 The above data fully demonstrate that compared with Comparative Examples 1-4, Examples 1-8 can fully show the effect of plant-derived functional particles on the antibacterial and contact cool properties of plant-derived composite ultrashort fibers containing xylitol.

[0036] In addition, it has been found through testing that the xylitol plant-based composite ultra-short fibers prepared by the present invention have good functional durability. After being washed 100 times, the loss rate of the antibacterial rate against common bacteria (Staphylococcus aureus, Escherichia coli, Candida albicans) was less than 3%.

[0037] According to the microspectral LC-MSMS test results, the maximum xylitol content detected was 9314.13 mg / kg after baking at 80°C for 1 hour.

[0038] Since the present invention uses plant-derived functional particles to prepare plant-derived composite ultra-short fibers containing xylitol, the plant-derived functional particles effectively improve the performance of the plant-derived composite ultra-short fibers containing xylitol, as follows: It can be seen from Examples 1-3 that in the preparation of plant-derived composite ultra-short fibers containing xylitol from the spinning solution of plant-derived functional particles, as the proportion and content of the plant-derived functional particles continue to increase, the antibacterial and contact cool effects of the ultra-short fibers are significantly improved. As the content of the plant-derived functional particles increases, the number of antibacterial components and cool components per unit volume also increases. Hinokitiol can achieve antibacterial effects by destroying bacterial cell membranes or interfering with their metabolic processes. When the concentration of these components in the fiber increases, they can more effectively cover the fiber surface to form a denser antibacterial barrier to prevent bacterial growth and reproduction. Xylitol has an endothermic solubility characteristic, that is, when it comes into contact with the skin, it absorbs heat and dissolves in sweat, giving people a cool feeling. As the content of xylitol increases, the number of xylitol molecules that can participate in this process per unit area increases, resulting in a stronger cool experience. After chemical modification, microencapsulation and nano-treatment of the plant-derived functional particles, their stability is effectively guaranteed, and their dispersibility in the spinning solution and compatibility with the substrate are significantly improved.

[0039] It can be seen from Examples 3 and 4 that with the continuous changes in the content of other components, the antibacterial and cool contact effects of the ultrashort fibers do not change significantly, indicating that small changes in other components within a certain range are not sufficient to significantly affect the antibacterial and cool contact effects of the ultrashort fibers.

[0040] It can be seen from Examples 5-7 that in the preparation of xylitol-containing plant-derived composite ultra-short fibers from the melt of plant-derived functional particles, with the continuous increase in the proportion and content of the plant-derived functional particles, the antibacterial and contact cooling effects of the ultra-short fibers are significantly improved. The increase in the content of plant-derived functional particles directly leads to an increase in the concentration of effective ingredients in the ultra-short fibers, while chemical modification, microencapsulation and nano-treatment ensure that these ingredients can be well distributed and utilized efficiently in the fibers. Therefore, the antibacterial and contact cooling effects of the fibers are significantly improved with the increase in the content of plant-derived functional particles.

[0041] It can be seen from Examples 7 and 8 that with the continuous changes in the content of other components, the antibacterial and cool contact effects of the ultrashort fibers do not change significantly, which further demonstrates that the other components have little effect on the antibacterial and cool contact effects of the ultrashort fibers, and that the determining factor of the antibacterial and cool contact effects of the ultrashort fibers is the plant-derived functional particles.

[0042] According to the above test experiments, the plant-based composite ultra-short fibers containing xylitol prepared according to Example 3 and Example 7 have the best performance, so Example 3 and Example 7 are taken as the best examples; It can be seen from Example 3 and Comparative Example 1, as well as Example 7 and Comparative Example 3, that without adding plant-derived functional particles, the antibacterial and contact cooling effects of the ultra-short fibers are poorer. Without adding plant-derived functional particles, the fibers lack effective ingredients that can inhibit bacterial growth, and the heat absorption properties provided by xylitol also fail to provide a significant contact cooling experience.

[0043] It can be seen from Example 3 and Comparative Example 2, as well as Example 7 and Comparative Example 4, that when xylitol and plant-derived extracts are used directly without being modified by citramalic acid, the antibacterial and contact cool effects of the ultrashort fibers are poor. Although xylitol and plant-derived extracts are directly added, since they are not modified by citramalic acid, xylitol and plant-derived extracts contain more active hydroxyl and amino functional groups, which are easily affected by water, light and heat, resulting in loss of activity. The citramalic acid modification reduces the activity of these functional groups through esterification and amidation reactions, thereby improving the stability of the material and prolonging the functional effect.

[0044] In summary, by utilizing the heat absorption characteristics of xylitol itself, it can quickly trigger a water absorption and heat absorption reaction, and then absorb the surrounding heat to achieve a cool touch effect. The antibacterial components of plant-derived extracts can effectively cover the fiber surface to form a dense antibacterial barrier, thereby preventing the growth and reproduction of bacteria and achieving an antibacterial effect. The chemical modification of citramalic acid significantly enhances the stability of the functional ingredients. Microencapsulation and nano-treatment improve their dispersibility and compatibility in the fiber, ensuring a more lasting and effective functional performance. At the same time, because the components of the plant-derived functional particles are all derived from nature, they are renewable and degradable, and therefore can effectively replace traditional organic synthesis functional modification additives, and have broad application prospects.

[0045] The above shows and describes the basic principles, main features and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited by the above embodiments, and the above embodiments and descriptions are only preferred examples of the present invention, and are not intended to limit the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the present invention to be protected.

Claims

1. A plant-derived composite ultra-short fiber containing xylitol, characterized in that: The invention comprises an ultra-short fiber substrate and plant-derived functional particles, wherein the plant-derived functional particles are obtained by chemically modifying, microencapsulating and nano-processing citramalic acid, xylitol and plant-derived extracts.

2. The plant-derived composite ultra-short fiber containing xylitol according to claim 1, characterized in that: The preparation method of the plant-derived functional particles is as follows: S1.

1. Add citramalic acid, xylitol and plant extract to a round-bottom flask, then add p-toluenesulfonic acid, stir well, place the round-bottom flask with the reactants in an oil bath, install a reflux condenser, introduce nitrogen to exclude air, heat to 80-100°C, continue stirring, turn on the vacuum pump, turn it off after 10-15 minutes, keep it on for 20-30 minutes, continue to turn on the vacuum pump, repeat the intermittent operation of turning on the vacuum pump, stop heating after the reaction time is 2-4 hours, cool naturally to room temperature, filter and dry to obtain the chemically modified plant source; S1.2, disperse the chemically modified plant source and Tween 80 in water, then add the wall material and stir thoroughly until uniformly dispersed to obtain a mixed solution, add the mixed solution into a spray dryer, set the parameters of inlet temperature to 80-100°C, exhaust temperature to 60-80°C, pump speed to 5-15mL / min, nozzle pressure to 0.2-0.4MPa, air flow rate to 300-600m³ / h, start the spray dryer, and collect the microencapsulated plant source; S1.

3. Use zirconium oxide with a diameter of 0.1-1 mm as the grinding medium, mix the microencapsulated plant source and the grinding medium at a ratio of 10 to 15:1, use a ball mill, set the speed to 300-600 rpm, and the ball milling time to 3-5 hours. Separate the larger particles through a sieve to obtain plant-derived functional particles.

3. The plant-derived composite ultra-short fiber containing xylitol according to claim 2, characterized in that: In S1.1, the plant-derived extract is selected from one or more combinations of Japanese cypress extract, sunflower extract, jasmine extract, white magnolia extract, and camellia extract; the mass ratio of citramalic acid, xylitol, and plant-derived extract is 14:5 to 7:4 to 8; and the amount of p-toluenesulfonic acid added is 1-3% of the total mass of citramalic acid, xylitol, and plant-derived extract.

4. The plant-derived composite ultra-short fiber containing xylitol according to claim 2, characterized in that: In S1.2, the wall material is selected from any one of gelatin, gum arabic, chitosan, polylactic acid, and polyurethane; the mass ratio of the chemically modified plant source to the wall material is 1:4-8; and the amount of Tween 80 added is 0.5-2% of the total mass of the chemically modified plant source and the wall material.

5. The plant-derived composite ultra-short fiber containing xylitol according to claim 2, characterized in that: In S1.3, the particle size of the plant-derived functional particles is 100-500nm.

6. The plant-derived composite ultra-short fiber containing xylitol according to claim 1, characterized in that: The substrate of the ultra-short fibers includes a regenerated cellulose fiber substrate or a synthetic fiber substrate. The regenerated cellulose fiber substrate is any one of viscose fiber, modal fiber, and lyocell fiber pulp. The synthetic fiber substrate includes any one of polyester chips and polyamide chips.

7. A method for preparing a plant-derived composite ultra-short fiber containing xylitol, for preparing a plant-derived composite ultra-short fiber containing xylitol according to any one of claims 1 to 6, characterized in that: The invention comprises the preparation, spinning, drying and mechanical cutting of a plant-derived functional particle spinning solution or a plant-derived functional particle molten solution.

8. The method for preparing the plant-derived composite ultra-short fibers containing xylitol according to claim 7, characterized in that: The specific preparation steps of preparing the plant-based composite ultra-short fibers containing xylitol using the plant-based functional particle spinning solution are as follows: The treated regenerated cellulose fiber substrate is dissolved and mixed, and plant-derived functional particles are added. A high-shear mixer is used to fully stir and disperse the particles. The mixed solution is filtered to obtain a plant-derived functional particle spinning solution. The plant-derived functional particle spinning solution is extruded from a nozzle in a spinning machine to form continuous fibers. After the fibers are solidified, they are cleaned to remove residual chemicals, dried, and mechanical cutting devices are used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

9. The method for preparing the plant-derived composite ultra-short fibers containing xylitol according to claim 7, characterized in that: The specific preparation steps of preparing the plant-based composite ultra-short fibers containing xylitol by using the plant-based functional particle melt are as follows: The synthetic fiber substrate is heated and melted, and mixed with plant-derived functional particles to obtain a molten liquid of plant-derived functional particles, which is then extruded through a melt spinning machine to obtain continuous fibers. After the fibers are solidified, they are dried and a mechanical cutting device is used to accurately control the cutting length to obtain plant-derived composite ultra-short fibers containing xylitol.

10. The method for preparing the plant-derived composite ultra-short fibers containing xylitol according to claim 7, characterized in that: The added amount of the plant-based functional particles is 26-35% of the mass of the plant-based functional particle spinning solution, and the added amount of the plant-based functional particles is 26-35% of the mass of the plant-based functional particle melt. The diameter of the plant-based composite ultra-short fibers containing xylitol is 0.1-1mm and the length is 1-5mm.

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