Flavonoid functional textile fiber and preparation method thereof

Abstract

The invention relates to the technical field of textile fibers, in particular to a flavonoid functional textile fiber and a preparation method thereof. The motherwort microcapsule is prepared by using a motherwort solution, and motherwort is rich in flavone components and can play a good antibacterial effect. Licoflavone and cacumen biotae flavone are also added, and glycyrrhizic acid and liquiritigenin in liquorice also have an excellent bacteriostatic effect; meanwhile, the activity of tyrosinase can be inhibited, the effect of an endothelin antagonist can be played, and oxygen free radical scavenging capacity and antioxidant capacity are achieved. The wormwood fiber and the ES fiber are used for preparing the textile fiber, flavonoid compounds in the wormwood fiber have good anti-oxidation and antibacterial performance, and the performance of the textile fiber can be enhanced by adding the flavonoid compounds into the textile fiber. Finally, the mixed fibers are added into flavone steeping liquor for steeping treatment, dodecafluoroheptyl methacrylate is added into the flavone steeping liquor, the hydrophobicity of the textile fibers is further enhanced, and therefore the antibacterial performance of the fibers is enhanced.

Description

Technical Field

[0001] The invention relates to the technical field of textile fibers, in particular to a flavonoid functional textile fiber and a preparation method thereof. Background Art

[0002] Flavonoids are a class of natural products containing an aromatic structure and a hydroxyl group on two aromatic rings. They have a wide range of biological activities, including antibacterial, anti-inflammatory, antioxidant, and tyrosinase inhibition. Flavonoids such as flavones, isoflavones, and flavonols interact with the lipid bilayer of bacterial cell walls or cell membranes, thereby causing cell death or inhibiting their growth, showing significant antibacterial activity; flavonoids can also inhibit tyrosinase activity, and have oxygen free radical scavenging and antioxidant abilities.

[0003] In the development of antibacterial function of textiles, the introduction of flavonoids into fiber materials can effectively improve the antibacterial properties of textiles, extend the service life, and reduce the odor problem caused by bacterial growth. Therefore, flavonoid textile fibers have broad application prospects in the fields of medical treatment, sportswear, household goods, etc. However, it is difficult to ensure the uniform distribution of flavonoids by directly adding them to the fibers, resulting in poor functional effects of textile fibers.

[0004] In order to solve the above problems and improve the antibacterial effect of textile fibers, the present invention provides a flavonoid textile fiber with antibacterial, antioxidant and tyrosinase activity inhibition properties and a preparation method thereof. Summary of the invention

[0005] The object of the present invention is to provide a flavonoid textile fiber and a preparation method thereof, so as to solve the problems raised in the above background technology.

[0006] In order to solve the above technical problems, the present invention provides the following technical solutions: A method for preparing flavonoid textile fibers comprises the following steps: Step 1: adding the wormwood fiber to the motherwort microcapsule impregnation solution and immersing it for 3-5 hours to obtain the treated wormwood fiber; Step 2: Take the processed mugwort fiber and ES fiber, open, comb, and spunlace to obtain mixed fiber; Step 3: Take liquorice flavonoids, Platycladus orientalis leaf flavonoids, dodecafluoroheptyl methacrylate, 2,2-dimethoxy-2-phenylacetophenone, and N,N-dimethylformamide solution, stir evenly, and obtain a flavonoid impregnation solution; Step 4: Add the mixed fiber into the flavonoid impregnation solution and immerse for 3-5 hours to obtain flavonoid functional textile fiber.

[0007] More optimally, the method for preparing the motherwort microcapsule impregnation solution is: take motherwort microcapsules, fatty alcohol polyoxyethylene ether, citric acid, and deionized water, stir them evenly, and obtain the motherwort microcapsule impregnation solution.

[0008] Preferably, the preparation method of the motherwort microcapsules comprises the following steps: S1: Take motherwort and deionized water, stir evenly, heat to 100°C, react for 3-4h, filter, and obtain motherwort solution; S2: Take a surfactant, sorbitan monooleate, and paraffin, stir evenly, add sodium alginate, motherwort solution, and sodium hydroxide solution, stir until there is no precipitation, and obtain a mixed solution; S3: Take thiolated chitosan and acetic acid solution, stir evenly, add the mixed solution dropwise, adjust the pH value to 5, stir for 15-30 minutes, adjust the pH value to 9.5, add genipin aqueous solution, stir for 3-4 hours, filter, wash and dry to obtain motherwort microcapsules.

[0009] More optimally, the preparation method of the thiolated chitosan is: take genipin solution and chitosan gel, stir for 30-40 minutes, let stand for 44-48 hours, wash, and obtain cross-linked chitosan; take L-cysteine ​​solution and cross-linked chitosan, stir evenly, oscillate for 24-26 hours, wash with deionized water, and dry to obtain thiolated chitosan.

[0010] More optimally, the preparation method of the chitosan gel is: take acetic acid, add chitosan, stir evenly to obtain a chitosan solution; then spray the chitosan solution into a sodium hydroxide solution, stir for 1-2 hours, let stand for 12-14 hours, filter, wash, and obtain the chitosan gel.

[0011] More optimally, the preparation method of the glycyrrhizin flavonoids is: take licorice, crush it, and sieve it to obtain licorice powder; take licorice powder and ethanol solution, ultrasonically disperse them for 1-2 hours under the conditions of ultrasonic frequency 45-50kHz, power 100W, and temperature 60-65°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain glycyrrhizin flavonoids.

[0012] More optimally, the preparation method of the Platycladus orientalis leaf flavonoids is: take Platycladus orientalis leaves, crush them, and sieve them to obtain Platycladus orientalis leaf powder; take Platycladus orientalis leaf powder and ethanol solution, ultrasonically disperse them for 1-2 hours under the conditions of ultrasonic frequency of 45-50kHz, power of 100W, and temperature of 60-65°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain Platycladus orientalis leaf flavonoids.

[0013] Compared with the prior art, the beneficial effects achieved by the present invention are: (1) The present invention uses motherwort solution to prepare a motherwort microcapsule. Motherwort is rich in flavonoids and has a good antibacterial effect. The present invention also adds licorice flavonoids and arborvitae leaf flavonoids. Glycyrrhizic acid and glycyrrhizin in licorice also have excellent antibacterial effects.

[0014] (2) The present invention uses motherwort solution to prepare a motherwort microcapsule. Motherwort is rich in flavonoid components. The present invention also adds licorice flavonoids and arborvitae leaf flavonoids. Plant flavonoids are a class of small molecule natural whitening ingredients with certain biological activity. They can inhibit the activity of tyrosinase, play the role of endothelin antagonists, and have oxygen free radical scavenging ability and antioxidant ability.

[0015] The present invention uses wormwood fiber and ES fiber to prepare textile fiber. The flavonoids in the wormwood fiber have good anti-oxidation, anti-bacterial and tyrosinase activity inhibition properties. Adding the flavonoids to the textile fiber can enhance the anti-bacterial, anti-oxidation and tyrosinase activity inhibition properties of the textile fiber. The present invention grafts the sulfhydryl group in L-cysteine ​​onto cross-linked chitosan, and uses thiolated chitosan to prepare a motherwort microcapsule containing a motherwort solution. The motherwort microcapsule impregnation solution is used to impregnate the wormwood fiber, and a sulfhydryl group is grafted onto the wormwood fiber.

[0016] Finally, the mixed fibers were added to the flavonoid impregnation solution for impregnation treatment, to which dodecafluoroheptyl methacrylate was added. At this time, the thiol groups grafted on the mugwort fibers could participate in the thiol-olefin click reaction, and dodecafluoroheptyl methacrylate was grafted on the surface of the textile fibers, further enhancing the hydrophobicity of the textile fibers, thereby enhancing the antibacterial, antioxidant, and tyrosinase activity inhibition properties of the fibers. DETAILED DESCRIPTION

[0017] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0018] There is no particular restriction on the manufacturers of the raw materials involved in the present invention, and illustratively include: mugwort fiber: 38 mm in length, 1.6 dtex in linear density, which can be purchased from Tangshan Sanyou Group Chemical Fiber Co., Ltd.; ES fiber: 38 mm in length, 2.2 dtex in linear density, which can be purchased from Beijing Jinglan Nonwoven Fabric Co., Ltd.; Motherwort: can be purchased from Shangyuantang Pharmacy; Licorice: can be purchased from Shangyuantang Pharmacy; Platycladus orientalis leaves: can be purchased from Shangyuantang Pharmacy.

[0019] Embodiment 1: A method for preparing flavonoid functional textile fibers, comprising the following steps: Step 1: Preparation of thiolated chitosan: S1: Take 100 mL of 5% acetic acid, add 3 g of chitosan, stir evenly to obtain a chitosan solution; then spray the chitosan solution into a 0.5 mol / L sodium hydroxide solution, stir for 1.5 h, let stand for 13 h, filter and wash to obtain a chitosan gel; S2: Take 6 mL of 3% genipin solution and 3 g of chitosan gel, stir for 35 min, let stand for 46 h, and wash with deionized water at 50 °C to obtain cross-linked chitosan; S3: Take 6 mL of 1.8% L-cysteine ​​solution and 3 g of cross-linked chitosan, stir evenly, shake for 25 h, wash with deionized water, and dry to obtain thiolated chitosan; Step 2: Preparation of Motherwort Solution: Take 20g of motherwort and 500mL of deionized water, stir evenly, heat to 100℃, react for 3.5h, filter, and obtain motherwort solution; Step 3: Preparation of motherwort microcapsules: Take 3g of surfactant sorbitan monooleate and 80mL of paraffin, stir evenly, add 4g of sodium alginate and 5g of motherwort solution, add 1mol / L sodium hydroxide solution, adjust the pH value to 11, stir until there is no precipitation, and obtain a mixed solution; Take 3g of thiolated chitosan and 25mL of acetic acid solution, stir evenly, add the mixed solution dropwise, adjust the pH value to 5, stir for 20min at a speed of 800r / min, adjust the pH value to 9.5, add 10mL of 10% genipin aqueous solution, stir for 3.5h at a speed of 500r / min, filter, wash and dry to obtain motherwort microcapsules; Step 4: Preparation of treated wormwood fiber: Take 5g of motherwort microcapsules, 3g of fatty alcohol polyoxyethylene ether, 2g of citric acid, and 500mL of deionized water, stir evenly to obtain a motherwort microcapsule impregnation solution; add 20g of wormwood fiber to 500mL of motherwort microcapsule impregnation solution and immerse for 4h to obtain treated wormwood fiber; Step 5: Preparation of Licorice Flavonoids and Platycladus orientalis Leaf Flavonoids: Take licorice, crush it, and pass it through a 60-mesh sieve to obtain licorice powder; take 2g of licorice powder and 100mL of 60% ethanol solution, ultrasonically disperse it for 1.5h under the conditions of ultrasonic frequency of 48kHz, power of 100W, and temperature of 62℃, centrifuge it, rotary evaporate the supernatant, and freeze-dry it to obtain glycyrrhizin; Take Platycladus orientalis leaves, crush them, and pass them through a 60-mesh sieve to obtain Platycladus orientalis leaf powder; take 2 g of Platycladus orientalis leaf powder and 100 mL of 60% ethanol solution, ultrasonically disperse them for 1.5 h at an ultrasonic frequency of 48 kHz, a power of 100 W, and a temperature of 63°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain Platycladus orientalis leaf flavonoids; Step 6: Preparation of flavonoid functional textile fibers: 20% of the processed wormwood fiber and 80% of the ES fiber are taken, opened, combed and hydroentangled to obtain a mixed fiber; Take 2g of licorice flavonoids, 2g of Platycladus orientalis leaf flavonoids, 7mL of dodecafluoroheptyl methacrylate, 0.05g of 2,2-dimethoxy-2-phenylacetophenone, and 200mL of N,N-dimethylformamide solution, stir evenly to obtain a flavonoid impregnation solution; 20 g of the mixed fiber was added into 500 mL of flavonoid impregnation solution and immersed for 4 h to obtain flavonoid functional textile fiber.

[0020] Embodiment 2: A method for preparing flavonoid functional textile fibers, comprising the following steps: Step 1: Preparation of thiolated chitosan: S1: Take 100 mL of 5% acetic acid, add 3 g of chitosan, stir evenly to obtain a chitosan solution; then spray the chitosan solution into a 0.5 mol / L sodium hydroxide solution, stir for 1 h, let stand for 12 h, filter and wash to obtain a chitosan gel; S2: Take 6 mL of 3% genipin solution and 3 g of chitosan gel, stir for 30 min, let stand for 44 h, and wash with deionized water at 50 °C to obtain cross-linked chitosan; S3: Take 6 mL of 1.8% L-cysteine ​​solution and 3 g of cross-linked chitosan, stir evenly, shake for 24 h, wash with deionized water, and dry to obtain thiolated chitosan; Step 2: Preparation of Motherwort Solution: Take 20g of motherwort and 500mL of deionized water, stir evenly, heat to 100℃, react for 3h, filter, and obtain motherwort solution; Step 3: Preparation of motherwort microcapsules: Take 3g of surfactant sorbitan monooleate and 80mL of paraffin, stir evenly, add 4g of sodium alginate and 5g of motherwort solution, add 1mol / L sodium hydroxide solution, adjust the pH value to 11, stir until there is no precipitation, and obtain a mixed solution; Take 3g of thiolated chitosan and 25mL of acetic acid solution, stir evenly, add the mixed solution dropwise, adjust the pH value to 5, stir for 15min at a speed of 800r / min, adjust the pH value to 9.5, add 10mL of 10% genipin aqueous solution, stir for 3h at a speed of 500r / min, filter, wash and dry to obtain motherwort microcapsules; Step 4: Preparation of treated wormwood fiber: Take 5g of motherwort microcapsules, 3g of fatty alcohol polyoxyethylene ether, 2g of citric acid, and 500mL of deionized water, stir evenly to obtain a motherwort microcapsule impregnation solution; add 20g of wormwood fiber to 500mL of motherwort microcapsule impregnation solution and immerse for 3h to obtain treated wormwood fiber; Step 5: Preparation of Licorice Flavonoids and Platycladus orientalis Leaf Flavonoids: Take licorice, crush it, and pass it through a 60-mesh sieve to obtain licorice powder; take 2g of licorice powder and 100mL of 60% ethanol solution, ultrasonically disperse it for 1h under the conditions of ultrasonic frequency of 45kHz, power of 100W, and temperature of 60℃, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain glycyrrhizin; Take Platycladus orientalis leaves, crush them, and pass them through a 60-mesh sieve to obtain Platycladus orientalis leaf powder; take 2 g of Platycladus orientalis leaf powder and 100 mL of 60% ethanol solution, ultrasonically disperse them for 1 h under the conditions of ultrasonic frequency of 45 kHz, power of 100 W, and temperature of 60°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain Platycladus orientalis leaf flavonoids; Step 6: Preparation of flavonoid functional textile fibers: 20% of the processed wormwood fiber and 80% of the ES fiber are taken, opened, combed and hydroentangled to obtain a mixed fiber; Take 2g of licorice flavonoids, 2g of Platycladus orientalis leaf flavonoids, 7mL of dodecafluoroheptyl methacrylate, 0.05g of 2,2-dimethoxy-2-phenylacetophenone, and 200mL of N,N-dimethylformamide solution, stir evenly to obtain a flavonoid impregnation solution; 20 g of the mixed fiber was added into 500 mL of flavonoid impregnation solution and immersed for 3 h to obtain flavonoid functional textile fiber.

[0021] Embodiment 3: A method for preparing flavonoid functional textile fibers, comprising the following steps: Step 1: Preparation of thiolated chitosan: S1: Take 100 mL of 5% acetic acid, add 3 g of chitosan, stir evenly to obtain a chitosan solution; then spray the chitosan solution into a 0.5 mol / L sodium hydroxide solution, stir for 2 h, let stand for 14 h, filter and wash to obtain a chitosan gel; S2: Take 6 mL of 3% genipin solution and 3 g of chitosan gel, stir for 40 min, let stand for 48 h, and wash with deionized water at 50 °C to obtain cross-linked chitosan; S3: Take 6 mL of 1.8% L-cysteine ​​solution and 3 g of cross-linked chitosan, stir evenly, shake for 26 h, wash with deionized water, and dry to obtain thiolated chitosan; Step 2: Preparation of Motherwort Solution: Take 20g of motherwort and 500mL of deionized water, stir evenly, heat to 100℃, react for 4h, filter, and obtain motherwort solution; Step 3: Preparation of motherwort microcapsules: Take 3g of surfactant sorbitan monooleate and 80mL of paraffin, stir evenly, add 4g of sodium alginate and 5g of motherwort solution, add 1mol / L sodium hydroxide solution, adjust the pH value to 11, stir until there is no precipitation, and obtain a mixed solution; Take 3g of thiolated chitosan and 25mL of acetic acid solution, stir evenly, add the mixed solution dropwise, adjust the pH value to 5, stir for 30min at a speed of 800r / min, adjust the pH value to 9.5, add 10mL of 10% genipin aqueous solution, stir for 4h at a speed of 500r / min, filter, wash and dry to obtain motherwort microcapsules; Step 4: Preparation of treated wormwood fiber: Take 5g of motherwort microcapsules, 3g of fatty alcohol polyoxyethylene ether, 2g of citric acid, and 500mL of deionized water, stir evenly to obtain a motherwort microcapsule impregnation solution; add 20g of wormwood fiber to 500mL of motherwort microcapsule impregnation solution and immerse for 5h to obtain treated wormwood fiber; Step 5: Preparation of Licorice Flavonoids and Platycladus orientalis Leaf Flavonoids: Take licorice, crush it, and pass it through a 60-mesh sieve to obtain licorice powder; take 2g of licorice powder and 100mL of 60% ethanol solution, ultrasonically disperse it for 2h under the conditions of ultrasonic frequency of 50kHz, power of 100W, and temperature of 65℃, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain glycyrrhizin; Take Platycladus orientalis leaves, crush them, and pass them through a 60-mesh sieve to obtain Platycladus orientalis leaf powder; take 2 g of Platycladus orientalis leaf powder and 100 mL of 60% ethanol solution, ultrasonically disperse them for 2 h under the conditions of ultrasonic frequency of 50 kHz, power of 100 W, and temperature of 65°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain Platycladus orientalis leaf flavonoids; Step 6: Preparation of flavonoid functional textile fibers: 20% of the processed wormwood fiber and 80% of the ES fiber are taken, opened, combed and hydroentangled to obtain a mixed fiber; Take 2g of licorice flavonoids, 2g of Platycladus orientalis leaf flavonoids, 7mL of dodecafluoroheptyl methacrylate, 0.05g of 2,2-dimethoxy-2-phenylacetophenone, and 200mL of N,N-dimethylformamide solution, stir evenly to obtain a flavonoid impregnation solution; 20 g of the mixed fiber was added into 500 mL of flavonoid impregnation solution and immersed for 5 h to obtain flavonoid functional textile fiber.

[0022] Comparative Example 1: No motherwort microcapsules were added, and the rest was the same as Example 1: Step 1: Preparation of thiolated chitosan: S1: Take 100 mL of 5% acetic acid, add 3 g of chitosan, stir evenly to obtain a chitosan solution; then spray the chitosan solution into a 0.5 mol / L sodium hydroxide solution, stir for 1.5 h, let stand for 13 h, filter and wash to obtain a chitosan gel; S2: Take 6 mL of 3% genipin solution and 3 g of chitosan gel, stir for 35 min, let stand for 46 h, and wash with deionized water at 50 °C to obtain cross-linked chitosan; S3: Take 6 mL of 1.8% L-cysteine ​​solution and 3 g of cross-linked chitosan, stir evenly, shake for 25 h, wash with deionized water, and dry to obtain thiolated chitosan; Step 3: Preparation of Licorice Flavonoids and Platycladus orientalis Leaf Flavonoids: Take licorice, crush it, and pass it through a 60-mesh sieve to obtain licorice powder; take 2g of licorice powder and 100mL of 60% ethanol solution, ultrasonically disperse it for 1.5h under the conditions of ultrasonic frequency of 48kHz, power of 100W, and temperature of 62℃, centrifuge it, rotary evaporate the supernatant, and freeze-dry it to obtain glycyrrhizin; Take Platycladus orientalis leaves, crush them, and pass them through a 60-mesh sieve to obtain Platycladus orientalis leaf powder; take 2 g of Platycladus orientalis leaf powder and 100 mL of 60% ethanol solution, ultrasonically disperse them for 1.5 h at an ultrasonic frequency of 48 kHz, a power of 100 W, and a temperature of 63°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain Platycladus orientalis leaf flavonoids; Step 5: Preparation of flavonoid functional textile fibers: Take 20% of mugwort fiber and 80% of ES fiber, open, card and hydroentangle to obtain mixed fiber; Take 2g of licorice flavonoids, 2g of Platycladus orientalis leaf flavonoids, 7mL of dodecafluoroheptyl methacrylate, 0.05g of 2,2-dimethoxy-2-phenylacetophenone, and 200mL of N,N-dimethylformamide solution, stir evenly to obtain a flavonoid impregnation solution; 20 g of the mixed fiber was added into 500 mL of flavonoid impregnation solution and immersed for 4 h to obtain flavonoid functional textile fiber.

[0023] Comparative Example 2: Chitosan was not thiol-modified, and the rest was the same as Example 1: Step 1: Preparation of Motherwort Solution: Take 20g of motherwort and 500mL of deionized water, stir evenly, heat to 100℃, react for 3.5h, filter, and obtain motherwort solution; Step 2: Preparation of motherwort microcapsules: Take 3g of surfactant sorbitan monooleate and 80mL of paraffin, stir evenly, add 4g of sodium alginate and 5g of motherwort solution, add 1mol / L sodium hydroxide solution, adjust the pH value to 11, stir until there is no precipitation, and obtain a mixed solution; Take 3g chitosan and 25mL acetic acid solution, stir evenly, add the mixed solution dropwise, adjust the pH value to 5, stir for 20min at a speed of 800r / min, adjust the pH value to 9.5, add 10mL of 10% genipin aqueous solution, stir for 3.5h at a speed of 500r / min, filter, wash and dry to obtain motherwort microcapsules; Step 3: Preparation of treated wormwood fiber: Take 5g of motherwort microcapsules, 3g of fatty alcohol polyoxyethylene ether, 2g of citric acid, and 500mL of deionized water, stir evenly to obtain a motherwort microcapsule impregnation solution; add 20g of wormwood fiber to 500mL of motherwort microcapsule impregnation solution and immerse for 4h to obtain treated wormwood fiber; Step 4: Preparation of Licorice Flavonoids and Platycladus orientalis Leaf Flavonoids: Take licorice, crush it, and pass it through a 60-mesh sieve to obtain licorice powder; take 2g of licorice powder and 100mL of 60% ethanol solution, ultrasonically disperse it for 1.5h under the conditions of ultrasonic frequency of 48kHz, power of 100W, and temperature of 62℃, centrifuge it, rotary evaporate the supernatant, and freeze-dry it to obtain glycyrrhizin; Take Platycladus orientalis leaves, crush them, and pass them through a 60-mesh sieve to obtain Platycladus orientalis leaf powder; take 2 g of Platycladus orientalis leaf powder and 100 mL of 60% ethanol solution, ultrasonically disperse them for 1.5 h at an ultrasonic frequency of 48 kHz, a power of 100 W, and a temperature of 63°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain Platycladus orientalis leaf flavonoids; Step 5: Preparation of flavonoid functional textile fibers: 20% of the processed wormwood fiber and 80% of the ES fiber are taken, opened, combed and hydroentangled to obtain a mixed fiber; Take 2g of licorice flavonoids, 2g of Platycladus orientalis leaf flavonoids, 7mL of dodecafluoroheptyl methacrylate, 0.05g of 2,2-dimethoxy-2-phenylacetophenone, and 200mL of N,N-dimethylformamide solution, stir evenly to obtain a flavonoid impregnation solution; 20 g of the mixed fiber was added into 500 mL of flavonoid impregnation solution and immersed for 4 h to obtain flavonoid functional textile fiber.

[0024] Comparative Example 3: No dodecafluoroheptyl methacrylate was added, and the rest was the same as Example 1: Step 1: Preparation of thiolated chitosan: S1: Take 100 mL of 5% acetic acid, add 3 g of chitosan, stir evenly to obtain a chitosan solution; then spray the chitosan solution into a 0.5 mol / L sodium hydroxide solution, stir for 1.5 h, let stand for 13 h, filter and wash to obtain a chitosan gel; S2: Take 6 mL of 3% genipin solution and 3 g of chitosan gel, stir for 35 min, let stand for 46 h, and wash with deionized water at 50 °C to obtain cross-linked chitosan; S3: Take 6 mL of 1.8% L-cysteine ​​solution and 3 g of cross-linked chitosan, stir evenly, shake for 25 h, wash with deionized water, and dry to obtain thiolated chitosan; Step 2: Preparation of Motherwort Solution: Take 20g of motherwort and 500mL of deionized water, stir evenly, heat to 100℃, react for 3.5h, filter, and obtain motherwort solution; Step 3: Preparation of motherwort microcapsules: Take 3g of surfactant sorbitan monooleate and 80mL of paraffin, stir evenly, add 4g of sodium alginate and 5g of motherwort solution, add 1mol / L sodium hydroxide solution, adjust the pH value to 11, stir until there is no precipitation, and obtain a mixed solution; Take 3g of thiolated chitosan and 25mL of acetic acid solution, stir evenly, add the mixed solution dropwise, adjust the pH value to 5, stir for 20min at a speed of 800r / min, adjust the pH value to 9.5, add 10mL of 10% genipin aqueous solution, stir for 3.5h at a speed of 500r / min, filter, wash and dry to obtain motherwort microcapsules; Step 4: Preparation of treated wormwood fiber: Take 5g of motherwort microcapsules, 3g of fatty alcohol polyoxyethylene ether, 2g of citric acid, and 500mL of deionized water, stir evenly to obtain a motherwort microcapsule impregnation solution; add 20g of wormwood fiber to 500mL of motherwort microcapsule impregnation solution and immerse for 4h to obtain treated wormwood fiber; Step 5: Preparation of Licorice Flavonoids and Platycladus orientalis Leaf Flavonoids: Take licorice, crush it, and pass it through a 60-mesh sieve to obtain licorice powder; take 2g of licorice powder and 100mL of 60% ethanol solution, ultrasonically disperse it for 1.5h under the conditions of ultrasonic frequency of 48kHz, power of 100W, and temperature of 62℃, centrifuge it, rotary evaporate the supernatant, and freeze-dry it to obtain glycyrrhizin; Take Platycladus orientalis leaves, crush them, and pass them through a 60-mesh sieve to obtain Platycladus orientalis leaf powder; take 2 g of Platycladus orientalis leaf powder and 100 mL of 60% ethanol solution, ultrasonically disperse them for 1.5 h at an ultrasonic frequency of 48 kHz, a power of 100 W, and a temperature of 63°C, centrifuge, rotary evaporate the supernatant, and freeze-dry to obtain Platycladus orientalis leaf flavonoids; Step 6: Preparation of flavonoid functional textile fibers: 20% of the processed wormwood fiber and 80% of the ES fiber are taken, opened, combed and hydroentangled to obtain a mixed fiber; Take 2g of licorice flavonoids, 2g of Platycladus orientalis leaf flavonoids, and 200mL of N,N-dimethylformamide solution, stir evenly to obtain a flavonoid impregnation solution; 20 g of the mixed fiber was added into 500 mL of flavonoid impregnation solution and immersed for 4 h to obtain flavonoid functional textile fiber.

[0025] experiment: The flavonoid functional textile fibers prepared in Examples 1-3 and Comparative Examples 1-3 were used for performance testing. The flavonoid functional textile fibers were cut into 5 cm × 10 cm × 0.2 cm specimens, and then subjected to a tensile performance test. The upper and lower clamping distance was 10 cm, and the transverse breaking strength was tested. The flavonoid functional textile fibers were cut into 2 cm × 2 cm × 0.2 cm specimens, sterilized, and then an Escherichia coli bacterial suspension was added. The samples were cultured at 37 ° C for 24 h, and the antibacterial rate was tested. The data obtained are shown in the following table:

[0026] Conclusion: Comparative Example 1 does not add motherwort microcapsules, and the antibacterial effect is poor. Comparative Example 2 does not perform thiolation modification on chitosan, and the adhesion of dodecafluoroheptyl methacrylate on the surface of textile fibers is weakened, and the antibacterial property becomes poor. Comparative Example 3 does not add dodecafluoroheptyl methacrylate, and the hydrophobicity of textile fibers deteriorates and the antibacterial property is weakened. Examples 1-3 of the present invention use motherwort solution to prepare a motherwort microcapsule. Motherwort is rich in flavonoid components and can have a good antibacterial effect. The thiol group in L-cysteine ​​is grafted onto cross-linked chitosan, and a motherwort microcapsule containing motherwort solution is prepared using thiolated chitosan. The wormwood fiber is impregnated with motherwort microcapsule impregnation solution, and thiol groups are grafted onto the wormwood fiber. The mixed fibers are added to the flavonoid impregnation solution for impregnation treatment, to which dodecafluoroheptyl methacrylate is added. At this time, the thiol groups grafted on the wormwood fibers can participate in the thiol-olefin click reaction, and dodecafluoroheptyl methacrylate is grafted on the surface of the textile fibers, further enhancing the hydrophobicity of the textile fibers, thereby enhancing the antibacterial properties of the fibers.

[0027] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing flavonoid functional textile fibers, characterized in that: The following steps are involved: Step 1: adding the wormwood fiber to the motherwort microcapsule impregnation solution and immersing it for 3-5 hours to obtain the treated wormwood fiber; Step 2: Take the processed mugwort fiber and ES fiber, open, comb, and spunlace to obtain mixed fiber; Step 3: Take liquorice flavonoids, Platycladus orientalis leaf flavonoids, dodecafluoroheptyl methacrylate, 2,2-dimethoxy-2-phenylacetophenone, and N,N-dimethylformamide solution, stir evenly, and obtain a flavonoid impregnation solution; Step 4: Add the mixed fiber into the flavonoid impregnation solution and immerse for 3-5 hours to obtain flavonoid functional textile fiber.

2. The method for preparing a flavonoid functional textile fiber according to claim 1, characterized in that: The preparation method of the motherwort microcapsule impregnation liquid is as follows: taking motherwort microcapsules, fatty alcohol polyoxyethylene ether, citric acid and deionized water, stirring them evenly, and obtaining the motherwort microcapsule impregnation liquid.

3. The method for preparing a flavonoid functional textile fiber according to claim 2, characterized in that: The preparation method of the motherwort microcapsule is as follows: The following steps are involved: S1: Take motherwort and deionized water, stir evenly, heat to 100°C, react for 3-4h, filter, and obtain motherwort solution; S2: Take a surfactant, sorbitan monooleate, and paraffin, stir evenly, add sodium alginate, motherwort solution, and sodium hydroxide solution, stir until there is no precipitation, and obtain a mixed solution; S3: Take thiolated chitosan and acetic acid solution, stir evenly, add the mixed solution dropwise, adjust the pH value to 5, stir for 15-30 minutes, adjust the pH value to 9.5, add genipin aqueous solution, stir for 3-4 hours, filter, wash and dry to obtain motherwort microcapsules.

4. The method for preparing a flavonoid functional textile fiber according to claim 3, characterized in that: The preparation method of the thiolated chitosan comprises: taking a genipin solution and a chitosan gel, stirring for 30-40 minutes, standing for 44-48 hours, washing, and obtaining cross-linked chitosan; taking an L-cysteine ​​solution and a cross-linked chitosan, stirring evenly, shaking for 24-26 hours, washing with deionized water, and drying, and obtaining the thiolated chitosan.

5. The method for preparing a flavonoid functional textile fiber according to claim 4, characterized in that: The preparation method of the chitosan gel is as follows: taking acetic acid, adding chitosan, stirring evenly to obtain a chitosan solution; then spraying the chitosan solution into a sodium hydroxide solution, stirring for 1-2 hours, standing for 12-14 hours, filtering, washing, and obtaining the chitosan gel.

6. The method for preparing a flavonoid functional textile fiber according to claim 1, characterized in that: The preparation method of the glycyrrhizin flavonoids comprises the following steps: taking licorice, crushing it, and sieving it to obtain licorice powder; taking the licorice powder and ethanol solution, ultrasonically dispersing them for 1-2 hours under the conditions of ultrasonic frequency of 45-50kHz, power of 100W, and temperature of 60-65°C, centrifuging them, rotary evaporating the supernatant, and freeze-drying them to obtain glycyrrhizin flavonoids.

7. The method for preparing a flavonoid functional textile fiber according to claim 1, characterized in that: The preparation method of the Platycladus orientalis leaf flavonoids comprises: taking Platycladus orientalis leaves, crushing and sieving to obtain Platycladus orientalis leaf powder; taking Platycladus orientalis leaf powder and ethanol solution, ultrasonically dispersing them for 1-2 hours under the conditions of ultrasonic frequency of 45-50kHz, power of 100W and temperature of 60-65°C, centrifuging, rotary evaporating the supernatant, and freeze-drying to obtain Platycladus orientalis leaf flavonoids.

8. The flavonoid functional textile fiber prepared according to the method for preparing the flavonoid functional textile fiber according to any one of claims 1 to 7.

Images