Functional viscose fiber containing traditional Chinese medicine ingredients and preparation method thereof

By grafting baicalein and guanylic acid end-capping agents with γ-cyclodextrin, the problem of functional substance loss in functional viscose fibers during washing was solved, thereby improving antibacterial and flame-retardant properties and enhancing the fiber's washability and service life.

CN117552239BActive Publication Date: 2026-04-14BEIJING CHUNFENG PHARMACEUTICAL CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
BEIJING CHUNFENG PHARMACEUTICAL CO LTD
Filing Date
2023-11-13
Publication Date
2026-04-14

AI Technical Summary

Technical Problem

In existing technologies, functional viscose fibers are prone to loss of functional substances during the washing process, resulting in a decrease in fiber functionality, and there is little to no discussion of flame retardancy.

Method used

Cyclodextrin microcapsules were prepared by encapsulating baicalin with γ-cyclodextrin, and then grafted onto the polyethylene glycol backbone using guanylic acid end-capping agent. This compound reacted with diphenyl chlorophosphate to form an antibacterial and flame-retardant composite modifier, which was then bonded to carboxylated viscose fibers to form amide bonds, giving the fibers excellent antibacterial and flame-retardant properties.

Benefits of technology

It improves the washability and flame retardancy of functional viscose fibers, extends their service life, reduces production costs, and improves the dispersibility of functional substances on the fibers.

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Abstract

The present application relates to viscose fiber technical field, disclose the functional viscose fiber containing traditional Chinese medicine component and its preparation method;The present application is prepared by wrapping baicalin in the inside of gamma-cyclodextrin to obtain cyclodextrin microcapsule containing traditional Chinese medicine component;Through the oxidation of guanosine under the action of 2-iodine acyl benzoic acid to prepare guanosine end-capping agent. With polyethylene glycol as modifier main chain, guanosine end-capping agent successfully grafted guanosine on both ends of polyethylene glycol, then cyclodextrin microcapsule and guanosine end-capping polyethylene glycol are grafted on the polyethylene glycol main chain, and then reacted with diphenyl chlorophosphate to graft on the surface of cyclodextrin microcapsule to prepare a polyethylene glycol modifier containing traditional Chinese medicine component with antibacterial and flame retardant properties;Finally, the amino group in the guanosine molecule at both ends of the polyethylene glycol modifier is reacted with the carboxyl group in the carboxylated viscose fiber to form an amide bond to prepare a functional viscose fiber containing traditional Chinese medicine component.
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Description

Technical Field

[0001] This invention relates to the field of viscose fiber technology, specifically to functional viscose fibers containing traditional Chinese medicine ingredients and their preparation methods. Background Technology

[0002] Viscose fiber, as a widely used textile material, is extensively applied in various fields such as clothing, bedding, medical and health products. Currently, in the preparation of viscose fiber, various functional Chinese herbal medicine ingredients are added to the viscose fiber solution for blending and spinning to obtain functional viscose fiber, avoiding the side effects and radiation pollution caused by traditional chemical reagents and mineral methods. However, there are few reports on the wash resistance of functional viscose fiber. Using physical blending spinning methods to prepare fibers, functional substances are easily lost during washing, resulting in a decrease in fiber functionality and a reduced lifespan. Furthermore, there is little research on the flame retardancy of functional viscose fiber.

[0003] Therefore, the invention of water-resistant and flame-retardant viscose fibers containing traditional Chinese medicine ingredients and their preparation methods are of great significance. Summary of the Invention

[0004] The purpose of this invention is to provide functional viscose fibers containing traditional Chinese medicine ingredients and their preparation method, so as to solve the problems mentioned in the background art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0006] A method for preparing functional viscose fibers containing traditional Chinese medicine ingredients includes the following steps:

[0007] S1: Polyethylene glycol and carbonyl diimidazole are added to tetrahydrofuran, heated to 50-55℃ and allowed to stand for 18-20 hours. Ethylenediamine is added, and the reaction is maintained at this temperature for 2-2.5 hours. The product is added to ethanol, filtered, and washed to obtain amine-terminated polyethylene glycol. The amine-terminated polyethylene glycol and cyclodextrin microcapsules containing traditional Chinese medicine ingredients are added to deionized water, heated to 25-30℃, sonicated for 2-3 hours, cooled, and allowed to stand to obtain traditional Chinese medicine-modified polyethylene glycol. The traditional Chinese medicine-modified polyethylene glycol and guanylic acid end-capping agent are added to N,N-dimethylformamide, heated to 60-65℃, and reacted for 7-8 hours. The product is added to acetone, filtered, and obtained guanylic acid-terminated polyethylene glycol.

[0008] S2: Guanylic acid-terminated polyethylene glycol is added to dimethyl sulfoxide, followed by triethylamine and diphenyl chlorophosphate. The mixture is heated to 30-35°C and reacted for 4-5 hours. The product is then added to acetone, filtered, and washed to obtain flame-retardant polyethylene glycol containing traditional Chinese medicine components. Flame-retardant polyethylene glycol containing traditional Chinese medicine components and carboxylated viscose fiber are added to a 50% ethanol solution and stirred until homogeneous. The mixture is heated to 50-75°C, and N,N'-dicyclohexylcarbodiimide ethanol solution is added. The mixture is shaken and reacted for 2-5 hours. After washing and drying, functional viscose fiber containing traditional Chinese medicine components is obtained.

[0009] Furthermore, the preparation method of the cyclodextrin microcapsules containing traditional Chinese medicine ingredients includes the following steps:

[0010] γ-Cyclodextrin was added to deionized water and stirred until homogeneous to obtain a cyclodextrin solution. Baicalein was added to deionized water and stirred until homogeneous. The cyclodextrin solution was then added, and the mixture was heated to reflux for 6-8 hours. After cooling, the mixture was filtered, washed, and dried at 60-65℃ to obtain cyclodextrin microcapsules containing traditional Chinese medicine ingredients.

[0011] Furthermore, the mass ratio of γ-cyclodextrin to baicalein is 1:(0.1-0.15).

[0012] Furthermore, the preparation method of the guanylic acid capping agent includes the following steps:

[0013] Guanylic acid and 2-iodobenzoic acid were added to dimethyl sulfoxide and stirred until homogeneous to obtain guanylic acid solution and 2-iodobenzoic acid solution, respectively. The 2-iodobenzoic acid solution was added to the guanylic acid solution and heated to 25-30℃ for 6-8 hours. The product was added to acetone, filtered, washed, and dried under vacuum at 80-85℃ to obtain the guanylic acid end-capping agent.

[0014] Furthermore, the mass ratio of guanylic acid to 2-iodobenzoic acid is 1:(0.5-1).

[0015] Furthermore, the method for preparing the carboxylated viscose fiber includes the following steps:

[0016] Viscose fibers were added to a 0.5 wt% sodium hydroxide solution and boiled for 30-45 minutes. After washing, neutral cellulase was added and the mixture was heated to 30-35℃ for 4-4.5 hours. After filtration and washing, glucose oxidase was added and the mixture was heated to 55-60℃ for 4-4.5 hours. After filtration, washing, and drying, carboxylated viscose fibers were obtained.

[0017] Furthermore, the neutral cellulase has a pH of 7-7.5; the glucose oxidase has a pH of 5-5.5.

[0018] Furthermore, the mass ratio of polyethylene glycol: carbonyl diimidazole: ethylenediamine is 50:1:(100-120); the mass ratio of terminal amine polyethylene glycol: cyclodextrin microcapsules containing traditional Chinese medicine ingredients is 1:(4-5); and the mass ratio of traditional Chinese medicine modified polyethylene glycol: guanylic acid end-capsulating agent is 5:(1-1.5).

[0019] Furthermore, the mass ratio of guanylic acid-terminated polyethylene glycol to diphenyl chlorophosphate is (3-4):1; the mass ratio of flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients to carboxylated adhesive is 1:(1-2); the pH of the 50% ethanol solution is 3-6; and the concentration of the N,N'-dicyclohexylcarbodiimide ethanol solution is 0.5-0.6 mg / L.

[0020] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0021] This invention utilizes the inclusion effect of γ-cyclodextrin to encapsulate baicalein within γ-cyclodextrin to prepare cyclodextrin microcapsules containing traditional Chinese medicine components; and prepares guanylic acid end-capping agents by oxidizing guanylic acid to aldehyde groups under the action of 2-iodobenzoic acid. Using polyethylene glycol (PEG) as the main chain of the modifier, guanylic acid end-capping agent was successfully grafted onto both ends of PEG. Then, cyclodextrin microcapsules containing traditional Chinese medicine components were used as antibacterial functional substances and reacted with the guanylic acid-capped PEG to graft onto the PEG main chain. Next, it was reacted with the flame-retardant functional substance diphenyl chlorophosphate and grafted onto the surface of the cyclodextrin microcapsules containing traditional Chinese medicine components to prepare a PEG modifier with antibacterial and flame-retardant properties containing traditional Chinese medicine components. Finally, the amino groups in the guanylic acid molecules at both ends of the PEG modifier react with the carboxyl groups in the carboxylated viscose fibers to form amide bonds, successfully grafting the modifier into the viscose fibers and endowing them with excellent antibacterial, flame-retardant, and wash-resistant properties. Compared with traditional physical blending and spinning of flame retardants and antibacterial agents, this application utilizes guanylic acid as a "bridge" connecting modified polyethylene glycol and viscose fiber. On the one hand, it avoids the problems of uneven dispersion and easy agglomeration of traditional flame retardants and antibacterial agents in the system, reduces the use of dispersants in the system, greatly reduces production costs and preparation processes, and greatly improves production efficiency. On the other hand, grafting flame retardant and antibacterial composite modifiers onto viscose fiber greatly improves the wash resistance of functional substances on viscose fiber and greatly extends the service life of functional viscose fiber. At the same time, guanylic acid, as a substance containing nitrogen and phosphorus, not only provides a "bridge" connection but also synergistically enhances the flame retardant properties of viscose fiber with the diphenyl chlorophosphate flame retardant on the surface of microcapsules. Detailed Implementation

[0022] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0023] In the following examples, the baicalein specification is: concentration 1.0 × 10⁻⁶. -4 mol / L, purchased from Shanxi University of Traditional Chinese Medicine; viscose fiber, purchased from Sichuan Yibin Huimei Thread Industry Co., Ltd.; guanylic acid, purchased from Hebei Baiwei Biotechnology Co., Ltd.; glucose oxidase, specification: 100u / mg, purchased from Shanghai Chiwei Industrial Co., Ltd.; cellulase, specification: 10000u / g, purchased from Dongheng Huadao Biotechnology Co., Ltd.; polyethylene glycol, specification: molecular weight 1000, purchased from Sigma Reagent Co., Ltd.; the remaining raw materials were commercially available.

[0024] The preparation method of the cyclodextrin microcapsules containing traditional Chinese medicine ingredients includes the following steps:

[0025] 10g of γ-cyclodextrin was added to deionized water and stirred until homogeneous to obtain a cyclodextrin solution. 1g of baicalein was added to deionized water and stirred until homogeneous. The cyclodextrin solution was then added, and the mixture was heated to reflux for 6 hours. After cooling, the mixture was filtered, washed, and dried at 60℃ to obtain cyclodextrin microcapsules containing traditional Chinese medicine ingredients.

[0026] The method for preparing the carboxylated viscose fiber includes the following steps:

[0027] Add 5g of viscose fiber to 100mL of 0.5wt% sodium hydroxide solution, boil for 30min, wash, add 10g of neutral cellulase and 90mL of deionized water, heat to 30℃ and react for 4h, filter, wash, add 7.5g of glucose oxidase and 92.5g of deionized water, heat to 55℃ and react for 4h, filter, wash, and dry at 40℃ to obtain carboxylated viscose fiber.

[0028] Example 1: Preparation method of functional viscose fiber containing traditional Chinese medicine ingredients: S1: 10g of guanylic acid and 5g of 2-iodobenzoic acid were added to dimethyl sulfoxide and stirred evenly to obtain guanylic acid solution and 2-iodobenzoic acid solution respectively; the 2-iodobenzoic acid solution was added to the guanylic acid solution, heated to 25°C and reacted for 6h; the product was added to acetone, filtered, washed, and vacuum dried at 80°C to obtain guanylic acid end-capping agent;

[0029] S2: Add 50g polyethylene glycol and 1g carbonyl diimidazole to tetrahydrofuran, heat to 50℃ and let stand for 18h, add 100g ethylenediamine, keep warm and react for 2h, add the product to ethanol, filter, wash, and obtain amine-terminated polyethylene glycol; add 10g amine-terminated polyethylene glycol and 40g cyclodextrin microcapsules containing traditional Chinese medicine ingredients to deionized water, heat to 25℃ and sonicate for 2h, cool and let stand, and obtain traditional Chinese medicine modified polyethylene glycol; add 50g traditional Chinese medicine modified polyethylene glycol and 10g guanylic acid end-capping agent to N,N-dimethylformamide, heat to 60℃ and react for 7h, add the product to acetone, filter, and obtain guanylic acid-terminated polyethylene glycol;

[0030] S3: Add 40g of guanylic acid-terminated polyethylene glycol to dimethyl sulfoxide, add 5g of triethylamine and 10g of diphenyl chlorophosphate, heat to 30℃ and react for 4h, add the product to acetone, filter, wash, and obtain flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients; add 10g of flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients and 20g of carboxylated viscose fiber to 50% ethanol solution and stir evenly, heat to 60℃, add N,N'-dicyclohexylcarbodiimide ethanol solution, shake and react for 3h, wash, dry, and obtain functional viscose fiber containing traditional Chinese medicine ingredients.

[0031] Example 2: Preparation method of functional viscose fiber containing traditional Chinese medicine ingredients: S1: 10g of guanylic acid and 5g of 2-iodobenzoic acid were added to dimethyl sulfoxide and stirred evenly to obtain guanylic acid solution and 2-iodobenzoic acid solution respectively; the 2-iodobenzoic acid solution was added to the guanylic acid solution, heated to 25°C and reacted for 6h; the product was added to acetone, filtered, washed, and vacuum dried at 80°C to obtain guanylic acid end-capping agent;

[0032] S2: Add 50g polyethylene glycol and 1g carbonyl diimidazole to tetrahydrofuran, heat to 50℃ and let stand for 18h, add 100g ethylenediamine, keep warm and react for 2h, add the product to ethanol, filter, wash, and obtain amine-terminated polyethylene glycol; add 10g amine-terminated polyethylene glycol and 45g cyclodextrin microcapsules containing traditional Chinese medicine ingredients to deionized water, heat to 25℃ and sonicate for 2h, cool and let stand, and obtain traditional Chinese medicine modified polyethylene glycol; add 50g traditional Chinese medicine modified polyethylene glycol and 10g guanylic acid end-capping agent to N,N-dimethylformamide, heat to 60℃ and react for 7h, add the product to acetone, filter, and obtain guanylic acid-terminated polyethylene glycol;

[0033] S3: Add 38.9g of guanylic acid-terminated polyethylene glycol to dimethyl sulfoxide, add 5g of triethylamine and 11.1g of diphenyl chlorophosphate, heat to 30℃ and react for 4h, add the product to acetone, filter, wash and obtain flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients; add 12g of flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients and 18g of carboxylated viscose fiber to 50% ethanol solution and stir evenly, heat to 60℃, add N,N'-dicyclohexylcarbodiimide ethanol solution, shake and react for 3h, wash and dry to obtain functional viscose fiber containing traditional Chinese medicine ingredients.

[0034] Example 3: Preparation method of functional viscose fiber containing traditional Chinese medicine ingredients: S1: 10g of guanylic acid and 5g of 2-iodobenzoic acid were added to dimethyl sulfoxide and stirred evenly to obtain guanylic acid solution and 2-iodobenzoic acid solution respectively; the 2-iodobenzoic acid solution was added to the guanylic acid solution, heated to 25°C and reacted for 6h; the product was added to acetone, filtered, washed, and vacuum dried at 80°C to obtain guanylic acid end-capping agent;

[0035] S2: Add 50g polyethylene glycol and 1g carbonyl diimidazole to tetrahydrofuran, heat to 50℃ and let stand for 18h, add 100g ethylenediamine, keep warm and react for 2h, add the product to ethanol, filter, wash, and obtain amine-terminated polyethylene glycol; add 10g amine-terminated polyethylene glycol and 50g cyclodextrin microcapsules containing traditional Chinese medicine ingredients to deionized water, heat to 25℃ and sonicate for 2h, cool and let stand, and obtain traditional Chinese medicine modified polyethylene glycol; add 50g traditional Chinese medicine modified polyethylene glycol and 10g guanylic acid end-capping agent to N,N-dimethylformamide, heat to 60℃ and react for 7h, add the product to acetone, filter, and obtain guanylic acid-terminated polyethylene glycol;

[0036] S3: Add 37.5g of guanylic acid-terminated polyethylene glycol to dimethyl sulfoxide, add 5g of triethylamine and 12.5g of diphenyl chlorophosphate, heat to 30℃ and react for 4h. Add the product to acetone, filter, and wash to obtain flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients. Add 15g of flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients and 15g of carboxylated viscose fiber to 50% ethanol solution and stir evenly. Heat to 60℃, add N,N'-dicyclohexylcarbodiimide ethanol solution, shake and react for 3h, wash, and dry to obtain functional viscose fiber containing traditional Chinese medicine ingredients.

[0037] Comparative Example 1: Preparation method of functional viscose fiber containing traditional Chinese medicine ingredients: S1: 10g of guanylic acid and 5g of 2-iodobenzoic acid were added to dimethyl sulfoxide and stirred evenly to obtain guanylic acid solution and 2-iodobenzoic acid solution respectively; the 2-iodobenzoic acid solution was added to the guanylic acid solution, heated to 25℃ and reacted for 6h, the product was added to acetone, filtered, washed, and vacuum dried at 80℃ to obtain guanylic acid end-capping agent;

[0038] S2: Add 50g polyethylene glycol and 1g carbonyl diimidazole to tetrahydrofuran, heat to 50℃ and let stand for 18h, add 100g ethylenediamine, keep warm and react for 2h, add the product to ethanol, filter, wash, and obtain amine-terminated polyethylene glycol; add 10g amine-terminated polyethylene glycol and 40g cyclodextrin microcapsules containing traditional Chinese medicine ingredients to deionized water, heat to 25℃ and sonicate for 2h, cool and let stand, and obtain traditional Chinese medicine modified polyethylene glycol; add 50g traditional Chinese medicine modified polyethylene glycol and 10g guanylic acid end-capping agent to N,N-dimethylformamide, heat to 60℃ and react for 7h, add the product to acetone, filter, and obtain guanylic acid-terminated polyethylene glycol;

[0039] S3: Add 10g of guanylic acid-terminated polyethylene glycol, 10g of diphenyl chlorophosphate, and 20g of carboxylated viscose fiber to a 50% ethanol solution and stir until homogeneous. Heat to 60℃, add N,N'-dicyclohexylcarbodiimide ethanol solution, shake and react for 3 hours, wash, and dry to obtain functional viscose fiber containing traditional Chinese medicine ingredients.

[0040] Comparative Example 2: Preparation method of functional viscose fiber containing traditional Chinese medicine ingredients: S1: 10g of guanylic acid and 5g of 2-iodobenzoic acid were added to dimethyl sulfoxide and stirred evenly to obtain guanylic acid solution and 2-iodobenzoic acid solution respectively; the 2-iodobenzoic acid solution was added to the guanylic acid solution, heated to 25℃ and reacted for 6h, the product was added to acetone, filtered, washed, and vacuum dried at 80℃ to obtain guanylic acid end-capping agent;

[0041] S2: Add 50g polyethylene glycol and 1g carbonyl diimidazole to tetrahydrofuran, heat to 50℃ and let stand for 18h, add 100g ethylenediamine, keep warm and react for 2h, add the product to ethanol, filter, wash to obtain amine-terminated polyethylene glycol; add 10g amine-terminated polyethylene glycol and 40g α-cyclodextrin to deionized water, heat to 25℃ and sonicate for 2h, cool and let stand to obtain α-cyclodextrin-modified polyethylene glycol; add 50g α-cyclodextrin-modified polyethylene glycol and 10g guanylic acid end-capping agent to N,N-dimethylformamide, heat to 60℃ and react for 7h, add the product to acetone and filter to obtain guanylic acid-terminated polyethylene glycol;

[0042] S3: Add 40g of guanylic acid-terminated polyethylene glycol to dimethyl sulfoxide, add 5g of triethylamine and 10g of diphenyl chlorophosphate, heat to 30℃ and react for 4h, add the product to acetone, filter, wash and obtain flame-retardant polyethylene glycol; add 10g of flame-retardant polyethylene glycol, 10g of baicalin and 20g of carboxylated viscose fiber to 50% ethanol solution and stir evenly, heat to 60℃, add N,N'-dicyclohexylcarbodiimide ethanol solution, shake and react for 3h, wash and dry to obtain functional viscose fiber containing traditional Chinese medicine ingredients.

[0043] Comparative Example 3: Preparation method of functional viscose fiber containing traditional Chinese medicine ingredients: S1: Add 50g polyethylene glycol and 1g carbonyl diimidazole to tetrahydrofuran, heat to 50℃ and let stand for 18h, add 100g ethylenediamine, keep warm and react for 2h, add the product to ethanol, filter, wash, and obtain terminal amine polyethylene glycol; add 10g terminal amine polyethylene glycol and 40g cyclodextrin microcapsules containing traditional Chinese medicine ingredients to deionized water, heat to 25℃ and sonicate for 2h, cool and let stand, and obtain traditional Chinese medicine modified polyethylene glycol;

[0044] S3: Add 40g of herbal-modified polyethylene glycol to dimethyl sulfoxide, add 5g of triethylamine and 10g of diphenyl chlorophosphate, heat to 30℃ and react for 4h, add the product to acetone, filter, wash, and obtain flame-retardant polyethylene glycol containing herbal ingredients; add 10g of flame-retardant polyethylene glycol containing herbal ingredients and 20g of carboxylated viscose fiber to 50% ethanol solution and stir evenly, heat to 60℃, add N,N'-dicyclohexylcarbodiimide ethanol solution, shake and react for 3h, wash, dry, and obtain functional viscose fiber containing herbal ingredients.

[0045] Experiment: Limiting Oxygen Index Test: Functional viscose fibers containing traditional Chinese medicine ingredients were woven into 150g / m² sheets. 2 The fiber was tested using a limiting oxygen index meter according to GB 5454-85, with a 5mm × 15mm sample ignited in a methane flame.

[0046] Antibacterial performance test: According to GB / T 209441-2007, two strains of Gram-positive Staphylococcus aureus were cultured in nutrient broth at 37℃ with shaking speed of 130 r / min for 18 h. After dilution with PBS buffer, 0.1 mL of 3×10⁻⁶ saturated broth was taken. 8 Inject the CFU / mL inoculation suspension into a sterile nutrient agar plate and spread it evenly until it solidifies. Spread the adhesive fibers into a 25mm circle, press it gently onto the agar plate, and add PBS buffer to moisten the fibers. Place the entire agar plate in a 37℃ incubator for 24 hours and observe the formation of an antibacterial band on the fibers.

[0047] Washing durability test: According to GB / T 17595-1998, a horizontal rotary drum machine is used for washing. After washing, the limiting oxygen index test and antibacterial performance test are carried out. The washing time is 12 minutes and the temperature is 30℃. The test is conducted after washing and drying.

[0048] Table 1. Viscose Fiber Performance Test Data

[0049]

[0050] Conclusion: The functional viscose fibers prepared in Examples 1-3 have excellent water resistance, flame retardancy, and antibacterial properties.

[0051] In Comparative Example 1, the flame retardant diphenyl chlorophosphate was directly added to carboxylated viscose fibers for physical blending to prepare functional viscose fibers; the flame retardant dispersion and water washability were reduced, resulting in a decrease in flame retardant performance.

[0052] In Comparative Example 2, baicalin was directly added to carboxylated viscose fibers for physical blending to prepare functional viscose fibers. The lack of cyclodextrin inclusion grafting on the viscose fibers in the physical blending of baicalin resulted in a reduction in the amount of functional substances carried on the viscose fibers, a decrease in water washability, and a reduction in antibacterial properties.

[0053] In Comparative Example 3, diphenyl chlorophosphate was used to end-cap polyethylene glycol with amine groups. The resulting functional polyethylene glycol was then directly added to carboxylated viscose fibers for physical blending to prepare functional viscose fibers. This resulted in a decrease in water washability and a reduction in antibacterial and flame retardant properties after washing.

[0054] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing functional viscose fibers containing traditional Chinese medicine ingredients, characterized in that: Includes the following steps: S1: Polyethylene glycol and carbonyl diimidazole are added to tetrahydrofuran, heated to 50-55℃ and allowed to stand for 18-20 hours. Ethylenediamine is added and the reaction is maintained at this temperature for 2-2.5 hours. The product is added to ethanol, filtered, and washed to obtain amine-terminated polyethylene glycol. The amine-terminated polyethylene glycol and cyclodextrin microcapsules containing traditional Chinese medicine ingredients are added to deionized water, heated to 25-30℃ and sonicated for 2-3 hours. After cooling and standing, traditional Chinese medicine modified polyethylene glycol is obtained. Traditional Chinese medicine-modified polyethylene glycol and guanylic acid end-capping agent were added to N,N-dimethylformamide, heated to 60-65℃ and reacted for 7-8 hours. The product was then added to acetone and filtered to obtain guanylic acid-end-capped polyethylene glycol. S2: Guanylic acid-terminated polyethylene glycol is added to dimethyl sulfoxide, followed by triethylamine and diphenyl chlorophosphate. The mixture is heated to 30-35°C and reacted for 4-5 hours. The product is then added to acetone, filtered, and washed to obtain flame-retardant polyethylene glycol containing traditional Chinese medicine components. Flame-retardant polyethylene glycol containing traditional Chinese medicine components and carboxylated viscose fiber are added to a 50% ethanol solution and stirred until homogeneous. The mixture is heated to 50-75°C, and N,N'-dicyclohexylcarbodiimide ethanol solution is added. The mixture is shaken and reacted for 2-5 hours. After washing and drying, functional viscose fiber containing traditional Chinese medicine components is obtained. The preparation method of the guanylic acid capping agent includes the following steps: Guanylic acid and 2-iodobenzoic acid were added to dimethyl sulfoxide and stirred until homogeneous to obtain guanylic acid solution and 2-iodobenzoic acid solution, respectively. The 2-iodobenzoic acid solution was added to the guanylic acid solution and heated to 25-30℃ for 6-8 hours. The product was added to acetone, filtered, washed, and dried under vacuum at 80-85℃ to obtain the guanylic acid end-capping agent. The method for preparing the carboxylated viscose fiber includes the following steps: Viscose fibers were added to a 0.5 wt% sodium hydroxide solution and boiled for 30-45 minutes. After washing, neutral cellulase was added and the mixture was heated to 30-35℃ for 4-4.5 hours. After filtration and washing, glucose oxidase was added and the mixture was heated to 55-60℃ for 4-4.5 hours. After filtration, washing, and drying, carboxylated viscose fibers were obtained.

2. The method for preparing functional viscose fiber containing traditional Chinese medicine ingredients according to claim 1, characterized in that: The method for preparing the cyclodextrin microcapsules containing traditional Chinese medicine ingredients includes the following steps: adding γ-cyclodextrin to deionized water and stirring until homogeneous to obtain a cyclodextrin solution; adding baicalein to deionized water and stirring until homogeneous; adding the cyclodextrin solution; heating to reflux for 6-8 hours; cooling; filtering; washing; and drying at 60-65℃ to obtain cyclodextrin microcapsules containing traditional Chinese medicine ingredients.

3. The method for preparing functional viscose fiber containing traditional Chinese medicine ingredients according to claim 2, characterized in that: The mass ratio of γ-cyclodextrin to baicalein is 1:(0.1-0.15).

4. The method for preparing functional viscose fiber containing traditional Chinese medicine ingredients according to claim 1, characterized in that: The mass ratio of guanylic acid to 2-iodobenzoic acid is 1:(0.5-1).

5. The method for preparing functional viscose fiber containing traditional Chinese medicine ingredients according to claim 1, characterized in that: The neutral cellulase has a pH of 7-7.5; the glucose oxidase has a pH of 5-5.

5.

6. The method for preparing functional viscose fiber containing traditional Chinese medicine ingredients according to claim 1, characterized in that: The mass ratio of polyethylene glycol: carbonyl diimidazole: ethylenediamine is 50:1:(100-120); the mass ratio of terminal amine polyethylene glycol: cyclodextrin microcapsules containing traditional Chinese medicine ingredients is 1:(4-5). The mass ratio of the modified polyethylene glycol to the guanylic acid capping agent is 5:(1-1.5).

7. The method for preparing functional viscose fiber containing traditional Chinese medicine ingredients according to claim 1, characterized in that: The mass ratio of guanylic acid-terminated polyethylene glycol to diphenyl chlorophosphate is (3-4):1; the mass ratio of flame-retardant polyethylene glycol containing traditional Chinese medicine ingredients to carboxylated adhesive is 1:(1-2); the pH of the 50% ethanol solution is 3-6; and the concentration of the N,N'-dicyclohexylcarbodiimide ethanol solution is 0.5-0.6 mg / L.

8. The viscose fiber prepared by the method for preparing functional viscose fiber containing traditional Chinese medicine ingredients according to any one of claims 1-7.

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