An environmentally friendly, long-lasting, antibacterial, and UV-resistant silk floss and its preparation method

Abstract

This invention belongs to the field of textile materials, specifically relating to an environmentally friendly, durable, antibacterial, and UV-resistant silk floss and its preparation method. First, antibacterial and UV-resistant multifunctional microcapsules are prepared using Artemisia argyi essential oil as the core material and sodium alginate oxidized and N-phthalyl chitosan as the wall material. Then, the multifunctional microcapsules are grafted onto silk fibers using a padding-baking technique, thereby developing durable, antibacterial, and UV-resistant silk floss. The durable, antibacterial, and UV-resistant silk floss of this invention exhibits an inhibition rate of 97.3-99.9% against Escherichia coli and Staphylococcus aureus, and the inhibition rate remains above 78% after 30 washes. The UPF of the durable, antibacterial, and UV-resistant silk floss is 55-63, and remains above 40 after 30 washes, indicating that the antibacterial and UV-resistant silk floss possesses excellent antibacterial, UV-resistant, and wash-resistant properties.

Description

Technical Field

[0001] This invention belongs to the field of textile materials, specifically relating to an environmentally friendly, durable, antibacterial, and UV-resistant silk floss and its preparation method. Background Technology

[0002] Silk fiber, known as the "Queen of Fibers," is an important traditional cultural product, widely used in high-end scarves, cheongsams, pajamas, bedding, and other fields. However, silk fiber has poor antibacterial properties, and its protein components provide nutrients for bacterial growth, making it prone to bacterial proliferation. Furthermore, silk fiber has poor UV resistance, causing silk fabrics to yellow easily. Improving the antibacterial and UV resistance properties of silk fiber is of great significance for increasing the added value of silk products.

[0003] Artemisia argyi extract is rich in natural substances such as flavonoids, terpenes, eucalyptols, and tannins, and has excellent antibacterial effects, which has attracted widespread attention in the development of eco-functional textiles. Reference (Xiao Pei, Han Qiandi, Zhao Xin, et al. Extraction of Artemisia argyi pigment and its application in dyeing silk fabrics [J]. Journal of Zhongyuan University of Technology, 2020, 31(2):14-17,28) Metal mordants and Artemisia argyi pigments are used to dye silk fabrics, but metal mordants have significant pollution. Reference (Sun Jingshan, Huo Yuxin, Du Jiachun, et al. Color fixation of Artemisia argyi dyed silk fabrics with dialdehyde chitosan [J]. Dyeing and Finishing Technology, 2022, 44(8):11-15.) In order to overcome the pollution of metal mordants and improve the color fastness of Artemisia argyi dyed silk fabrics, the active group of dialdehyde chitosan is used to achieve cross-linking and color fixation between Artemisia argyi and the fabric, while giving the fabric anti-wrinkle and antibacterial properties and improving wash resistance. However, while the pigments from Artemisia argyi impart functionality to silk fabrics, they also give the silk fabrics a certain color, making subsequent dyeing processes difficult.

[0004] Chinese invention patent CN107419526A discloses a method for producing a natural mosquito-repellent and antibacterial mugwort and silk floss bag for summer cooling. It involves preparing urea-formaldehyde resin mugwort microcapsules using formaldehyde and urea, and then attaching these microcapsules to a silk floss bag using an adhesive. However, the microcapsules prepared by this method have a formaldehyde release problem, which seriously endangers human health. Furthermore, formaldehyde itself is an antibacterial agent, thus the silk floss bag exhibits excellent antibacterial properties. Additionally, the microcapsules rely on the adhesive to form a film and adhere to the silk floss bag, severely impacting its breathability and other properties.

[0005] Artemisia argyi essential oil, with its high concentration of active ingredients and light color, is of great significance for the functional modification of silk floss. However, its volatility and poor stability prevent it from forming a strong bond with silk fibers, resulting in poor durability of the modified silk fibers. Microencapsulation technology, with its good stability and sustained-release properties, can effectively solve this problem. Summary of the Invention

[0006] References (Zhai Yuanyuan, Liu Yanjun, Wang Jin, et al. Preparation and application of antibacterial microcapsules of Artemisia argyi essential oil [J]. Journal of Textile Science and Engineering, 2021, 38(4):50-56) Artemisia argyi essential oil microcapsules were prepared by complex coagulation method using Artemisia argyi essential oil as core material and gelatin and chitosan as wall material. Then, cotton fabrics were finished by applying Artemisia argyi essential oil microcapsules through polyurethane coating. However, this method affects the air permeability of the fabric and cannot be used for the development of functional silk floss products.

[0007] Therefore, using artemisia oil as a core material to prepare environmentally friendly antibacterial and UV-resistant multifunctional microcapsules for the preparation of long-lasting antibacterial and UV-resistant silk floss while maintaining the good hand feel of silk fibers still presents significant challenges.

[0008] To address the aforementioned technical problems, this application provides the following technical solution:

[0009] This invention provides a method for preparing environmentally friendly, long-lasting, antibacterial, and UV-resistant silk floss, comprising the following steps:

[0010] S1: Add mugwort essential oil to an aqueous solution of sodium alginate oxidation, then slowly add an aqueous solution of N-phthalyl chitosan, and adjust the pH to 6-7 to obtain the reaction solution;

[0011] S2: The reaction solution is heated and reacted, then filtered and dried to obtain multifunctional microcapsules;

[0012] S3: Add the multifunctional microcapsules, citric acid, sodium hypophosphite and triethanolamine to water and mix to obtain a mixture;

[0013] S4: The mixture is impregnated and baked onto silk fibers to obtain the environmentally friendly, durable, antibacterial, and UV-resistant silk floss.

[0014] This invention discloses a method for preparing environmentally friendly, long-lasting antibacterial and UV-resistant silk floss. First, antibacterial and UV-resistant multifunctional microcapsules are prepared using Artemisia argyi essential oil as the core material and sodium alginate oxidized and N-phthalyl chitosan as the wall material. Then, the multifunctional microcapsules are grafted onto silk fibers using a padding-baking technique, thereby developing long-lasting antibacterial and UV-resistant silk floss. A schematic diagram of the preparation process of the multifunctional microcapsules is shown below. Figure 3 As shown.

[0015] The N-phthalyl chitosan was prepared according to the reference (Yi Yu, Yang Hao, Ying Guoqing, et al. Synthesis and properties of N-phthalyl chitosan [J]. Chemical Industry and Engineering Progress, 2006, 25(5): 542-545).

[0016] The mugwort essential oil was purchased from Shanghai Xinya New Material Technology Co., Ltd., and the sodium alginate oxide was purchased from Xi'an Qiyue Biotechnology Co., Ltd.

[0017] Preferably, the mass fraction of the solute in the aqueous solution of N-phthalyl chitosan is 0.8-1.3%; and the mass fraction of the solute in the aqueous solution of oxidized sodium alginate is 0.5-2.0%.

[0018] The aqueous solution of N-phthalyl chitosan has a pH of 4-5.

[0019] Preferably, the degree of substitution of the N-phthalyl chitosan is 0.3-0.4.

[0020] Preferably, the mass ratio of N-phthalyl chitosan to sodium alginate is 1-2:1.

[0021] Preferably, the mass ratio of the mugwort essential oil to the reactants is 1:2-3; the reactants are N-phthalyl chitosan and sodium alginate.

[0022] Preferably, the pH is adjusted using sodium hydroxide with a mass fraction of 5-10%.

[0023] Preferably, in step S2, the heating reaction temperature is 60-80℃, and the reaction time is 40-70 min. Under these conditions, the carboxyl group of oxidized sodium alginate and the amino group of N-phthalyl chitosan can form ionic bonds. In addition, the aldehyde group of oxidized sodium alginate can form a Schiff base with the amino group of N-phthalyl chitosan, forming a microcapsule wall material to encapsulate the artemisia essential oil.

[0024] Preferably, in step S2, the drying temperature is 30-50°C.

[0025] Preferably, the diameter of the multifunctional microcapsule is 2.5-5 μm.

[0026] Preferably, the encapsulation rate of Artemisia argyi essential oil in the multifunctional microcapsules is 67-72%.

[0027] Preferably, the concentration of the multifunctional microcapsules in the mixture is 10-15 g / L. Increasing the amount of multifunctional microcapsules increases the antibacterial and UV-resistant properties of the modified silk floss, while excessive amounts are wasteful.

[0028] In the mixture, the concentration of citric acid is 20-30 g / L. The carboxyl groups of citric acid can undergo covalent cross-linking reactions with the hydroxyl and amino groups on the surface of the multifunctional microcapsules and the hydroxyl and amino groups on the silk fibers, thereby grafting the multifunctional microcapsules onto the silk fibers. Citric acid is used as an acid regulator in the preparation process of the multifunctional microcapsules, so the multifunctional microcapsules themselves will contain a certain amount of citric acid. Therefore, the amount of additional citric acid added can be appropriately reduced.

[0029] In the mixture, the concentration of sodium hypophosphite is 15-20 g / L. Sodium hypophosphite can catalyze the esterification and cross-linking reaction between the carboxyl groups of citrate and the active groups of multifunctional microcapsules and silk fibers.

[0030] In the mixture, the concentration of triethanolamine is 20-25 g / L. Triethanolamine acts as a buffer to improve the strength properties of treated silk fibers.

[0031] Preferably, in step S4, the rolling allowance is 90-105%.

[0032] Preferably, in step S4, the baking method includes pre-baking and baking; the pre-baking temperature is 60-80℃, the baking temperature is 140-150℃, and the baking time is 2-3 minutes.

[0033] The present invention also provides an environmentally friendly, durable, antibacterial, and UV-resistant silk floss prepared by the above preparation method.

[0034] The principle of this invention is as follows: the cationic amino groups of N-phthalyl chitosan undergo ionic bonding and Schiff base reaction with the anionic carboxyl and aldehyde groups of sodium alginate, respectively, forming a stable wall material structure, thereby encapsulating Artemisia argyi essential oil and preparing multifunctional microcapsules; the flavonoid and tannic acid components in Artemisia argyi essential oil are rich in hydroxyl groups, which have good compatibility with N-phthalyl chitosan and sodium alginate, and the multifunctional microcapsules have good stability.

[0035] The technical solution of the present invention has the following advantages compared with the prior art:

[0036] The synergistic antibacterial effect is achieved through the interaction of mugwort essential oil, Schiff base structure, and chitosan structure. Therefore, the multifunctional microcapsules exhibit excellent antibacterial properties. Mugwort essential oil, dispersed in microcapsule form on silk fabric, releases and volatilizes in a sustained-release manner, resulting in excellent durability. Furthermore, the flavonoids and tannins in mugwort essential oil possess some UV protection properties, but the effect is limited. The phthalic acid structure in the N-phthalylated chitosan structure has good UV absorption, working synergistically with the flavonoids and tannins to provide UV protection. Therefore, the multifunctional microcapsules possess excellent UV protection properties.

[0037] In the preparation of microcapsules, citric acid is used to provide acidity and improve the solubility of N-phthalyl chitosan. Therefore, the prepared multifunctional microcapsules are embedded with a certain amount of citric acid. When preparing functional silk fibers, a certain amount of citric acid crosslinking agent is added simultaneously. The carboxyl groups of citric acid can undergo covalent crosslinking reactions with the hydroxyl and amino groups of the multifunctional microcapsules and silk fibers. In addition, the surface of the multifunctional microcapsules contains a certain amount of aldehyde groups, which can undergo grafting reactions with the amino and hydroxyl groups of the silk fibers, thereby grafting the multifunctional microcapsules onto the silk fibers and providing lasting functionality. Attached Figure Description

[0038] Figure 1 This is a scanning electron microscope image of the multifunctional microcapsule of the present invention.

[0039] Figure 2 These are test images of the antibacterial properties of the durable antibacterial and UV-resistant silk floss of this invention.

[0040] Figure 3 This is a schematic diagram of the preparation process of multifunctional microcapsules. Detailed Implementation

[0041] The present invention will be further described below with reference to the accompanying drawings and specific embodiments, so that those skilled in the art can better understand and implement the present invention. However, the embodiments described are not intended to limit the present invention.

[0042] Example 1

[0043] A method for preparing environmentally friendly, long-lasting, antibacterial, and UV-resistant silk floss comprises the following steps:

[0044] (1) First, prepare a 1 wt% sodium alginate oxidized solution and a 1 wt% N-phthalyl chitosan solution;

[0045] The N-phthalyl chitosan solution was prepared by adjusting the pH of the solution to 4 with citric acid. Chitosan is easily soluble in acidic solutions. The N-phthalyl chitosan was prepared according to the reference (Yi Yu, Yang Hao, Ying Guoqing, et al. Synthesis and properties of N-phthalyl chitosan [J]. Chemical Industry and Engineering Progress, 2006, 25(5): 542-545).

[0046] The degree of substitution of N-phthalyl chitosan is 0.36; the mass ratio of N-phthalyl chitosan to sodium alginate is 1:1; the mass ratio (core-to-wall ratio) of Artemisia argyi essential oil to N-phthalyl chitosan / sodium alginate is 1:2.

[0047] Artemisia argyi essential oil was added to a sodium alginate oxidase solution, and N-phthalyl chitosan solution was slowly added dropwise. Then, 8 wt% sodium hydroxide solution was added to adjust the pH of the solution to 6. The reaction was carried out at 70℃ for 50 min, filtered, and dried at 40℃ to obtain multifunctional microcapsules. The diameter of the obtained multifunctional microcapsules was 4 μm, and the encapsulation rate of artemisia argyi essential oil was 70%.

[0048] (2) Then, the multifunctional microcapsules, citric acid, sodium hypophosphite and triethanolamine were added to distilled water and dispersed evenly, so that the amount of multifunctional microcapsules was 12 g / L, the amount of citric acid was 25 g / L, the amount of sodium hypophosphite was 17 g / L and the amount of triethanolamine was 23 g / L.

[0049] Multifunctional microcapsules were grafted onto silk fibers using a pad-bake technique with a pad-drying rate of 100%, a pre-drying temperature of 70℃, a baking temperature of 140℃, and a baking time of 2 minutes; thus preparing durable antibacterial and UV-resistant silk floss.

[0050] Example 2

[0051] A method for preparing environmentally friendly, long-lasting, antibacterial, and UV-resistant silk floss comprises the following steps:

[0052] (1) First, prepare a 0.5 wt% sodium alginate oxidized solution and a 0.8 wt% N-phthalyl chitosan solution;

[0053] The N-phthalyl chitosan solution was prepared by adjusting the pH of the solution to 4 with citric acid. Chitosan is easily soluble in acidic solutions. The N-phthalyl chitosan was prepared according to the reference (Yi Yu, Yang Hao, Ying Guoqing, et al. Synthesis and properties of N-phthalyl chitosan [J]. Chemical Industry and Engineering Progress, 2006, 25(5): 542-545).

[0054] The degree of substitution of N-phthalyl chitosan is 0.3; the mass ratio of N-phthalyl chitosan to sodium alginate is 1:1; the mass ratio (core-to-wall ratio) of Artemisia argyi essential oil to N-phthalyl chitosan / sodium alginate is 1:2.

[0055] Artemisia argyi essential oil was added to a sodium alginate oxidase solution, and N-phthalyl chitosan solution was slowly added dropwise. Then, 5 wt% sodium hydroxide solution was added to adjust the pH of the solution to 6. The reaction was carried out at 60℃ for 40 min, filtered, and dried at 30℃ to obtain multifunctional microcapsules. The diameter of the obtained multifunctional microcapsules was 2.5 μm, and the encapsulation rate of Artemisia argyi essential oil was 672%.

[0056] (2) Then, the multifunctional microcapsules, citric acid, sodium hypophosphite and triethanolamine were added to distilled water and dispersed evenly, so that the amount of multifunctional microcapsules was 10 g / L, the amount of citric acid was 20 g / L, the amount of sodium hypophosphite was 15 g / L and the amount of triethanolamine was 20 g / L.

[0057] Multifunctional microcapsules were grafted onto silk fibers using a pad-baking technique with a pad-residue ratio of 90-105%, a pre-drying temperature of 60℃, a baking temperature of 140℃, and a baking time of 2 minutes; thus preparing durable antibacterial and UV-resistant silk floss.

[0058] Example 3

[0059] A method for preparing environmentally friendly, long-lasting, antibacterial, and UV-resistant silk floss comprises the following steps:

[0060] (1) First, prepare a 2.0 wt% sodium alginate oxidized solution and a 1.3 wt% N-phthalyl chitosan solution;

[0061] The N-phthalyl chitosan solution was prepared by adjusting the pH of the solution to 5 with citric acid. Chitosan is easily soluble in acidic solutions. The N-phthalyl chitosan was prepared according to the reference (Yi Yu, Yang Hao, Ying Guoqing, et al. Synthesis and properties of N-phthalyl chitosan [J]. Chemical Industry and Engineering Progress, 2006, 25(5): 542-545).

[0062] The degree of substitution of N-phthalyl chitosan is 0.4; the mass ratio of N-phthalyl chitosan to sodium alginate is 2:1; the mass ratio (core-to-wall ratio) of Artemisia argyi essential oil to N-phthalyl chitosan / sodium alginate is 1:3.

[0063] Artemisia argyi essential oil was added to a sodium alginate oxidase solution, and N-phthalyl chitosan solution was slowly added dropwise. Then, 10 wt% sodium hydroxide solution was added to adjust the pH of the solution to 7. The reaction was carried out at 80℃ for 70 min, filtered, and dried at 50℃ to obtain multifunctional microcapsules. The diameter of the obtained multifunctional microcapsules was 5 μm, and the encapsulation rate of artemisia argyi essential oil was 72%.

[0064] (2) Then, the multifunctional microcapsules, citric acid, sodium hypophosphite and triethanolamine were added to distilled water and dispersed evenly, so that the amount of multifunctional microcapsules was 15 g / L, the amount of citric acid was 30 g / L, the amount of sodium hypophosphite was 20 g / L and the amount of triethanolamine was 25 g / L.

[0065] Multifunctional microcapsules were grafted onto silk fibers using a pad-baking technique with a pad-residue ratio of 105%, a pre-drying temperature of 60–80°C, a baking temperature of 150°C, and a baking time of 3 minutes; thus preparing durable antibacterial and UV-resistant silk floss.

[0066] Effect Evaluation 1

[0067] The antibacterial properties of durable antibacterial and UV-resistant silk floss were tested according to GB / T 20944.3-2008 "Evaluation of antibacterial properties of textiles - Part 3: Shaking method". The results are as follows: Figure 2 As shown.

[0068] The UV protection factor (UPF) of durable antibacterial and UV-resistant silk floss was tested according to GB / T 18830-2009 "Evaluation of UV protection performance of textiles".

[0069] Wash according to AATCC-61-2013 "Color fastness to washing: Acceleration".

[0070] The antibacterial and UV-resistant silk floss of this invention exhibits an inhibition rate of 97.3%–99.9% against Escherichia coli and Staphylococcus aureus, and the inhibition rate remains above 78% even after 30 washes. The UPF of the antibacterial and UV-resistant silk floss is 55–63, and remains above 40 after 30 washes, indicating that the antibacterial and UV-resistant silk floss possesses excellent antibacterial, UV-resistant, and wash-resistant properties.

[0071] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A method for preparing a long-lasting antibacterial and anti-UV cocoon silk fabric, characterized in that, The method comprises the following steps: S1: adding artemisia oil into an aqueous solution of oxidized sodium alginate, slowly dropping an aqueous solution of N-phthaloyl chitosan, adjusting pH to 6-7 to obtain a reaction solution; S2: heating and reacting the reaction solution, filtering and drying to obtain multifunctional microcapsules; S3: mixing the multifunctional microcapsules, citric acid, sodium hypophosphite and triethanolamine in water to obtain a mixed solution; S4: padding and baking the mixed solution on silk fibers to obtain the ring-keeping long-lasting antibacterial and anti-ultraviolet silk velvet; the mass ratio of N-phthaloyl chitosan to oxidized sodium alginate is 1-2:1; the mass ratio of artemisia oil to reactants is 1:2-3; the reactants are N-phthaloyl chitosan and oxidized sodium alginate; in the step S2, the heating and reaction temperature is 60-80℃, and the reaction time is 40-70 min; in the multifunctional microcapsules, the embedding rate of artemisia oil is 70-72%.

2. The production method according to claim 1, wherein The mass fraction of solute in the aqueous solution of N-phthaloyl chitosan is 0.8-1.3%; the mass fraction of solute in the aqueous solution of oxidized sodium alginate is 0.5-2.0%.

3. The production method according to claim 1, wherein The degree of substitution of N-phthaloyl chitosan is 0.3-0.

4.

4. The production method according to claim 1, wherein In the mixed solution, the concentration of multifunctional microcapsules is 10-15 g / L, the concentration of citric acid is 20-30 g / L, the concentration of sodium hypophosphite is 15-20 g / L, and the concentration of triethanolamine is 20-25 g / L.

5. The production method according to claim 1, wherein In the step S4, the baking method comprises pre-baking and baking; the pre-baking temperature is 60-80℃, the baking temperature is 140-150℃, and the baking time is 2-3 min.

6. A ring-keeping long-lasting antibacterial and anti-ultraviolet silk velvet prepared by the preparation method of any one of claims 1-5.

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