Preparation method of viscose fiber modified by active ingredient composition of angelica sinensis or astragalus membranaceus

Abstract

The invention discloses a preparation method of viscose fibers modified by an active ingredient composition of angelica sinensis or astragalus membranaceus. The modified beta-cyclodextrin is adopted to load active ingredients of angelica sinensis or astragalus membranaceus, so that the retention rate of the active ingredients is high, the function is washable, the durability is high, and various requirements of daily use can be met. The process disclosed by the invention has good universality and is not limited to a certain specific active component, the angelica sinensis or the astragalus membranaceus can be selected according to actual requirements, and a feasible technical path is provided for industrial application of the functional viscose fiber.

Description

Technical Field

[0001] This invention relates to the field of functional textile materials technology, and in particular to a method for preparing viscose fibers modified with a composition of active ingredients from Angelica sinensis or Astragalus membranaceus. Background Technology

[0002] Angelica sinensis and Astragalus membranaceus, as traditional Chinese medicinal herbs, have a long history of application in the field of traditional Chinese medicine, and their medicinal value has been widely confirmed by modern scientific research. Angelica sinensis is rich in ferulic acid, artemisinin, and other bioactive components, and has significant effects such as promoting blood circulation, nourishing blood, antibacterial and anti-inflammatory properties. Astragalus membranaceus contains astragaloside A, flavonoids, and other effective components, which can enhance the body's immunity and exert antibacterial effects. With the increasing health awareness of people and the rapid development of the functional textile market, introducing the active ingredients of Angelica sinensis and Astragalus membranaceus into the textile field and developing textile products with health-preserving functions has become a hot research direction in the industry. Such products can not only meet consumers' demand for healthy functional textiles, but also expand the application fields of traditional Chinese medicinal herbs, and have important economic and social significance.

[0003] However, in practical applications, especially in the use of intimate textiles such as socks, traditional textiles loaded with active ingredients from traditional Chinese medicine face the serious challenge of insufficient functional durability. Socks are in close contact with the feet for extended periods during daily wear. Due to the high volume of sweat and frequent friction between the feet and shoes, the active ingredients are easily lost. On the one hand, soaking in sweat and frequent washing cause rapid dissolution and loss of active ingredients; on the other hand, continuous friction between the feet and socks / shoes accelerates the shedding of active ingredients from the fiber surface. This results in a significant reduction or even complete loss of the health benefits of angelica and astragalus after a short period of use, severely impacting the product's practical value and consumer experience.

[0004] Currently, existing technologies for incorporating the active ingredients of Angelica sinensis or Astragalus membranaceus into viscose fibers for functional socks primarily employ traditional surface treatment processes such as padding and coating. While these methods can impart antibacterial and health-promoting functions to the socks to some extent, the active ingredients adhere to the fiber surface only through physical adsorption or simple coating, failing to form a strong bond with the fiber matrix. During daily wear and repeated washing, the active ingredients are easily shed and lost, making it difficult to ensure the long-term maintenance of the health benefits of Angelica sinensis and Astragalus membranaceus. Therefore, there is an urgent need to develop a new technological solution that can stably and persistently bind the active ingredients of traditional Chinese medicine into viscose fibers, achieving long-lasting functionality and broadening its application scope in the textile industry. Summary of the Invention

[0005] The purpose of this invention is to solve the technical problems of weak binding force, easy loss and poor functional durability of the active ingredients of Angelica sinensis or Astragalus membranaceus in viscose fibers in the prior art, and to provide a method for preparing viscose fibers modified with a composition of active ingredients of Angelica sinensis or Astragalus membranaceus.

[0006] To achieve the above objectives, the present invention adopts the following technical solution: This invention provides a method for preparing viscose fiber modified with a composition of active ingredients from Angelica sinensis or Astragalus membranaceus, comprising the following steps: S1: Preparation of composite microspheres containing active ingredients of Angelica sinensis or Astragalus membranaceus Add an ethanol solution of Angelica sinensis or Astragalus membranaceus active ingredients dropwise to a 5%-20% modified β-cyclodextrin aqueous solution while stirring. After thorough stirring, equilibrate at 5°C for 15 hours and then dry at 50°C to obtain composite microspheres of Angelica sinensis or Astragalus membranaceus active ingredients.

[0007] The modified β-cyclodextrin described in S1 is hydroxypropyl-β-cyclodextrin.

[0008] The mass ratio of the active ingredient of Angelica sinensis or Astragalus membranaceus in S1 to the modified β-cyclodextrin is 1:5-14.

[0009] Preferably, the mass ratio of the active ingredient of Angelica sinensis or Astragalus membranaceus to the modified β-cyclodextrin is 1:11.

[0010] The homogenization rate of the stirring described in S1 is 8000-12000 RPM, and the stirring speed is 1000-1300 RPM. Under these conditions, the average particle size distribution of the angelica or astragalus active ingredient composite microparticles is more concentrated. If the stirring speed is too high, it will cause the hydrophobic bonds in β-cyclodextrin to bind, which is not conducive to the formation of microspheres.

[0011] This invention addresses the core technical challenge of maintaining the functional durability of textiles. To fully leverage the functional value of natural medicinal ingredients, it selects the active components of Angelica sinensis or Astragalus membranaceus, extracted with 70% ethanol, as the core functional source. Angelica sinensis ethanol extract is rich in artemisinin and coumarins, which are fat-soluble active substances, while Astragalus membranaceus ethanol extract is mainly composed of fat-soluble and moderately polar flavonoids and saponins. Both types of components possess excellent potential functional activities. This technical solution utilizes modified β-cyclodextrin to load the active components, precisely controlling the intermolecular interactions between the hydrophobic cavities of the modified β-cyclodextrin and the active components. The active components of Angelica sinensis or Astragalus membranaceus are efficiently encapsulated within the cavities, forming a stable composite structure, thus improving their acid and alkali resistance in viscose wet spinning processes. Meanwhile, modified β-cyclodextrin can achieve stable dispersion and no agglomeration of composite microspheres even when the addition amount (10-20%) is high during the preparation of viscose fiber. This avoids the precipitation phenomenon when the addition amount is greater than 10% in the existing technology, and significantly improves the solubility and dispersion uniformity of composite microspheres in viscose spinning solution.

[0012] S2: Preparation of composite viscose spinning solution Add the composite microspheres containing active ingredients of Angelica sinensis or Astragalus membranaceus to the viscose spinning solution and dissolve them completely at 25°C to obtain the composite viscose spinning solution.

[0013] The viscose spinning solution described in S2 contains 8-10% methyl cellulose and 5-8% sodium hydroxide.

[0014] The amount of the Angelica sinensis or Astragalus membranaceus active ingredient composite microspheres added in S2 is 1-20% of the methyl cellulose content in the viscose spinning dope.

[0015] S3: Spinning and forming The composite viscose spinning solution is extruded through a spinneret, coagulated in a coagulation bath, stretched, desulfurized, washed, oiled, and dried to obtain the fiber.

[0016] The coagulation bath consists of 100-120 g / L sulfuric acid, 200-250 g / L sodium sulfate, and 10-20 g / L zinc sulfate. The reaction temperature is 45℃, and the spinning speed is 35 m / min.

[0017] S4: Post-processing modification S41: Immerse the fiber in γ-glycidyl oxypropyltrimethoxysilane ethanol solution, dry at 80℃ after 1-3 hours, adjust the pH to 4.5 with 0.5% acetic acid aqueous solution, react at 45℃ for 50 minutes to obtain the initial fiber; S42: Immerse the raw fiber in a 0.2% sodium bicarbonate aqueous solution at room temperature for 20 minutes until the solution pH stabilizes at 6.5-7.4. Then wash with water and dry at 65°C for 40 minutes until the moisture content is <8%, thus obtaining the viscose fiber modified by the Angelica or Astragalus active ingredient composition.

[0018] The concentration of the γ-glycidyl etheroxypropyltrimethoxysilane ethanol solution described in S41 is 1-3%.

[0019] The bath ratio of the viscose fiber to the γ-glycidoxypropyltrimethoxysilane ethanol solution in S41 is 1:20.

[0020] The epoxy groups in γ-glycidoxypropyltrimethoxysilane can react with the active groups in the modified β-cyclodextrin on the surface of viscose fibers. At the same time, the siloxane chain forms hydrogen bonds or covalent bonds with the cellulose hydroxyl groups in the viscose fiber molecular chain, constructing a three-dimensional network structure of fiber-silane-active ingredient. This allows the post-treated modified viscose fiber to have better functional durability when made into fabrics, especially when made into socks, where it can still maintain excellent multi-functionality in daily washing and constant friction.

[0021] The beneficial effects of this invention are: 1. A good balance between the mechanical properties and functionality of viscose fibers is achieved. The addition of traditional functional powders often leads to a significant decrease in the breaking strength and elongation of viscose fibers due to the foreign body effect. However, this invention, through microencapsulation and surface modification technology, can introduce natural functional components while still ensuring that the mechanical properties of viscose fibers meet the first-class technical requirements of the national standard GB / T14463-2022 for viscose staple fibers, and under optimal conditions, can reach the superior grade standard.

[0022] 2. This invention achieves long-lasting functionality of active ingredients in fabrics. Viscose fibers containing Angelica sinensis active ingredients not only possess excellent antibacterial properties but also exhibit far-infrared emission capabilities, promoting blood circulation; viscose fibers containing Astragalus membranaceus active ingredients demonstrate significant antibacterial effects. More importantly, the technical solution of this invention achieves high retention rates of active ingredients, resulting in wash-resistant and durable functionality that meets various daily usage needs. Correspondingly, the antibacterial performance maintains an inhibition rate of over 90% against three types of bacteria even after 50 washes, while the far-infrared emission performance also meets national standards.

[0023] 3. This invention employs a pre-spinning addition process combined with post-treatment modification. On the one hand, the active ingredients of Angelica sinensis or Astragalus membranaceus exhibit good dispersion stability during pre-spinning addition, laying the foundation for the uniformity of fabric function. On the other hand, they possess good acid and alkali resistance stability during wet spinning. Combined with post-treatment modification, a three-dimensional network structure of fiber-silane-active ingredient is constructed, enabling the fabric to meet national standard requirements even after multiple washes, thus broadening the application range of the fiber to a certain extent.

[0024] 4. The process of this invention has good versatility and is not limited to a specific active ingredient. Angelica sinensis or Astragalus membranaceus can be selected according to actual needs, providing a feasible technical path for the industrial application of functional viscose fibers. Detailed Implementation

[0025] Example 1: Viscose fiber rich in Angelica sinensis active ingredients A method for preparing viscose fiber modified with an Angelica sinensis active ingredient composition includes the following steps: S1: Preparation of Angelica sinensis active ingredient composite microspheres An ethanol solution of Angelica sinensis active ingredients was added dropwise to a 15% modified β-cyclodextrin aqueous solution while stirring. After thorough stirring, the mixture was equilibrated at 5°C for 15 hours and then dried at 50°C to obtain Angelica sinensis active composite microspheres.

[0026] The modified β-cyclodextrin described in S1 is hydroxypropyl-β-cyclodextrin.

[0027] The mass ratio of the active ingredient of Angelica sinensis to the modified β-cyclodextrin in S1 is 1:11.

[0028] The homogenization speed of the stirring in S1 is 10000 RPM, and the stirring speed is 1200 RPM.

[0029] S2: Preparation of composite viscose spinning solution Add the angelica active ingredient composite microspheres to the viscose spinning solution and dissolve them completely at 25°C to obtain the composite viscose spinning solution.

[0030] The viscose spinning solution described in S2 contains 8-10% methyl cellulose and 5-8% sodium hydroxide.

[0031] The amount of Angelica sinensis active ingredient composite microspheres added in S2 is 15% of the methyl cellulose content in the viscose spinning dope.

[0032] S3: Spinning and forming The composite viscose spinning solution is extruded through a spinneret, coagulated in a coagulation bath, stretched, desulfurized, washed, oiled, and dried to obtain the fiber.

[0033] The coagulation bath consisted of 110 g / L sulfuric acid, 200 g / L sodium sulfate, and 15 g / L zinc sulfate. The reaction temperature was 45 °C, and the spinning speed was 35 m / min.

[0034] S4: Post-processing modification S41: The composite viscose spinning solution is spun using a wet spinning process. The spun viscose fibers are immersed in a 2% γ-glycidyl etheroxypropyltrimethoxysilane ethanol solution, dried at 80°C after 2.5 hours, and the pH is adjusted to 4.5 with a 0.5% acetic acid aqueous solution. After reacting at 45°C for 50 minutes, the initial fibers are obtained. S42: Immerse the raw fibers in a 0.2% sodium bicarbonate aqueous solution at room temperature for 20 minutes until the solution pH stabilizes at 6.5. Then wash with water and dry at 65°C for 40 minutes until the moisture content is <8%, thus obtaining the viscose fiber modified by the Angelica sinensis active ingredient composition.

[0035] The bath ratio of the viscose fiber to the γ-glycidoxypropyltrimethoxysilane ethanol solution in S41 is 1:20.

[0036] Example 2: Viscose fiber rich in Astragalus membranaceus active ingredients A method for preparing viscose fiber modified with an Astragalus membranaceus active ingredient composition includes the following steps: S1: Preparation of Astragalus active ingredient composite microspheres An ethanol solution of Astragalus membranaceus active ingredients was added dropwise to a 15% modified β-cyclodextrin aqueous solution while stirring. After thorough stirring, the mixture was equilibrated at 5°C for 15 hours and then dried at 50°C to obtain Astragalus membranaceus active composite microspheres.

[0037] The modified β-cyclodextrin described in S1 is hydroxypropyl-β-cyclodextrin.

[0038] The solvent for the modified β-cyclodextrin solution in S1 is an ethanol:water composite solvent with a volume ratio of 2:1.

[0039] The mass ratio of Astragalus active ingredient to modified β-cyclodextrin in S1 is 1:11.

[0040] The homogenization speed of the stirring in S1 is 10000 RPM, and the stirring speed is 1200 RPM.

[0041] S2: Preparation of composite viscose spinning solution The composite microspheres containing Astragalus membranaceus active ingredients were added to the viscose spinning solution and dissolved completely at 25°C to obtain the composite viscose spinning solution.

[0042] The viscose spinning solution described in S2 contains 8-10% methyl cellulose and 5-8% sodium hydroxide.

[0043] The amount of Astragalus active ingredient composite microspheres added in S2 is 15% of the methyl cellulose content in the viscose spinning dope.

[0044] S3: Spinning and forming The composite viscose spinning solution is extruded through a spinneret, coagulated in a coagulation bath, stretched, desulfurized, washed, oiled, and dried to obtain the fiber.

[0045] The coagulation bath consisted of 110 g / L sulfuric acid, 200 g / L sodium sulfate, and 15 g / L zinc sulfate. The reaction temperature was 45 °C, and the spinning speed was 35 m / min.

[0046] S4: Post-processing modification S41: The composite viscose spinning solution is spun using a wet spinning process. The spun viscose fibers are immersed in a 2% γ-glycidyl etheroxypropyltrimethoxysilane ethanol solution, dried at 80°C after 2.5 hours, and the pH is adjusted to 4.5 with a 0.5% acetic acid aqueous solution. After reacting at 45°C for 50 minutes, the initial fibers are obtained. S42: Immerse the raw fiber in a 0.2% sodium bicarbonate aqueous solution at room temperature for 20 minutes until the solution pH stabilizes at 6.5. Then wash with water and dry at 65°C for 40 minutes until the water content is <8%, thus obtaining the viscose fiber modified by the Astragalus active ingredient composition.

[0047] The bath ratio of the viscose fiber to the γ-glycidoxypropyltrimethoxysilane ethanol solution in S41 is 1:20.

[0048] Comparative Example 1: Similar to Example 1, except that in step S1, β-cyclodextrin is used to load the active ingredient of Angelica sinensis.

[0049] Comparative Example 2: Similar to Example 1, except that step S1 is omitted, and in step S2, the active ingredient of Angelica sinensis is directly added to the viscose spinning solution for spinning.

[0050] Comparative Example 3: Same as Example 1, except that there is no S4 post-processing modification step.

[0051] The viscose fibers prepared in Examples 1-2 and Comparative Examples 1-3 were tested for dry breaking strength (GB / T 14463-2022), wet breaking strength (GB / T 14463-2022), and antibacterial rate (GB / T 20944.3-2008). The viscose fibers prepared in Examples 1-2 and Comparative Examples 1-3 were used to make fabrics (fabric specifications: 237g / m²). 2 (36% Angelica or Astragalus viscose fiber, 64% cotton) The far-infrared emissivity test (GB / T 30127-2013) is detailed in Table 1.

[0052] Table 1 This invention encompasses any substitutions, modifications, equivalent methods, and solutions made within the spirit and scope of this invention. To provide the public with a thorough understanding of this invention, specific details are described in detail in the following preferred embodiments; however, those skilled in the art will fully understand the invention even without these details. Furthermore, to avoid unnecessary misunderstanding of the essence of this invention, well-known methods, processes, procedures, components, and circuits are not described in detail.

[0053] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing viscose fiber modified with a composition of active ingredients from Angelica sinensis or Astragalus membranaceus, characterized in that, Includes the following steps: S1: Preparation of composite microspheres containing active ingredients of Angelica sinensis or Astragalus membranaceus; S2: Preparation of composite viscose spinning solution; S3: Spinning and forming; S4: Post-processing modification.

2. The preparation method according to claim 1, characterized in that, The method for preparing the Angelica sinensis or Astragalus membranaceus active ingredient composite microspheres described in S1 is as follows: add an ethanol solution of Angelica sinensis or Astragalus membranaceus active ingredients dropwise to a 5%-20% modified β-cyclodextrin aqueous solution while stirring. After thorough stirring, equilibrate at 5°C for 15 hours, and then dry at 50°C to obtain the Angelica sinensis or Astragalus membranaceus active ingredient composite microspheres.

3. The preparation method according to claim 2, characterized in that, The modified β-cyclodextrin is hydroxypropyl-β-cyclodextrin.

4. The preparation method according to claim 2, characterized in that, The mass ratio of the active ingredient of Angelica sinensis or Astragalus membranaceus to the modified β-cyclodextrin is 1:5-14.

5. The preparation method according to claim 2, characterized in that, The homogenization rate of the stirring is 8000-12000 RPM, and the stirring speed is 1000-1300 RPM.

6. The preparation method according to claim 1, characterized in that, The method for preparing the modified composite viscose spinning solution described in S2 is as follows: add the composite microspheres of active ingredients of Angelica sinensis or Astragalus membranaceus to the viscose spinning solution and dissolve them completely at 25°C to obtain the composite viscose spinning solution.

7. The preparation method according to claim 6, characterized in that, The amount of the composite microspheres containing the active ingredients of Angelica sinensis or Astragalus membranaceus added is 1-20% of the methyl cellulose content in the viscose spinning dope.

8. The preparation method according to claim 1, characterized in that, The spinning method described in S3 is as follows: the composite viscose spinning solution is extruded through a spinneret, subjected to a coagulation bath, drawn, desulfurized, washed, oiled, and dried to obtain fiber filaments.

9. The preparation method according to claim 8, characterized in that, The coagulation bath is 100-120 °C. The reaction mixture consists of 200-250 g / L sulfuric acid, 10-20 g / L sodium sulfate, and 10-20 g / L zinc sulfate. The reaction temperature is 45℃, and the spinning speed is 35 m / min.

10. The preparation method according to claim 1, characterized in that, The spinning modification method described in S4 includes the following steps: S41: The composite viscose spinning solution is spun using a wet spinning process. The spun viscose fibers are immersed in a γ-glycidyl etheroxypropyltrimethoxysilane ethanol solution and dried at 80°C after 1-3 hours. The pH is adjusted to 4.5 with a 0.5% acetic acid aqueous solution and reacted at 45°C for 50 minutes to obtain the initial fibers. S42: Immerse the raw fiber in a 0.2% sodium bicarbonate aqueous solution at room temperature for 20 minutes until the solution pH stabilizes at 6.5-7.

4. Then wash with water and dry at 65°C for 40 minutes until the water content is <8%, thus obtaining the viscose fiber modified by the Angelica or Astragalus active ingredient composition. The concentration of the γ-glycidyl etheroxypropyltrimethoxysilane ethanol solution described in S41 is 1-3%; The bath ratio of the spun viscose fiber to the γ-glycidyl etheroxypropyltrimethoxysilane ethanol solution, as described in S41, is 1:20.

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