Plant antibacterial and antiallergic viscose fiber and its preparation method

Abstract

The present application belongs to the field of textile fiber processing technology, and discloses a plant antibacterial and antiallergic viscose fiber and a preparation method thereof. The viscose fiber comprises a viscose fiber substrate, silk fibroin and a supercritical carbon dioxide extract derived from a plant traditional Chinese medicine composition. The plant traditional Chinese medicine composition is composed of clove, mint, wormwood, rosemary and licorice. The preparation method comprises the following steps: drying and crushing the plant traditional Chinese medicine composition to obtain plant traditional Chinese medicine particles; extracting the plant traditional Chinese medicine particles by using a supercritical carbon dioxide extraction technology, and then performing filtration, low-temperature concentration and decolorization treatment to obtain refined antibacterial and antiallergic extract. The present application uses natural plant traditional Chinese medicine active ingredients, combines silk fibroin to enhance fixation, and endows the viscose fiber with natural and durable antibacterial and antiallergic properties. The bacteriostatic rate and the antiallergic rate are both above 95%, and the problem of biological toxicity and white pollution of chemical reagents is avoided, so that the present application has good environmental protection and comfort.

Description

Technical Field

[0001] This invention relates to the field of textile fiber processing technology, and more specifically, to a plant-based antibacterial and anti-allergic viscose fiber and its preparation method. Background Technology

[0002] Viscose fiber is a type of regenerated cellulose fiber, and the fiber itself is biodegradable. Its surface is smooth and lacks a noticeable roughness, resulting in fabrics that are soft, delicate, and comfortable to wear. However, it has poor abrasion resistance. Due to its low tensile strength and poor elastic recovery, viscose fiber is prone to brittleness and deformation. Currently, chemical antibacterial agents are mostly used to prepare viscose fibers with antibacterial, bacteriostatic, and anti-allergic properties. Common chemical reagents, such as silver-based antibacterial agents and quaternary ammonium salts, are introduced into the fiber through blending or finishing processes. However, these chemical reagents have drawbacks; they may have biotoxicity or environmental residue issues, easily causing "white pollution."

[0003] The main problems with existing technologies include: defects in chemical reagents, which may have biotoxicity or environmental residues, affecting not only the physical properties of viscose fibers themselves, but also causing "white pollution"; and the current natural antibacterial and anti-allergic solvents have a narrow antibacterial spectrum and insufficient anti-allergenic properties, with poor biocompatibility and stability, and the antibacterial and anti-allergic effects are not long-lasting.

[0004] Therefore, how to provide a viscose fiber that has both high efficiency and long-lasting antibacterial and anti-allergic properties, is environmentally friendly, and does not affect the physical properties of the fiber, and its preparation method, is a technical problem that urgently needs to be solved in this field. Summary of the Invention

[0005] The purpose of this invention is to address the shortcomings of existing technologies by proposing a plant-based antibacterial and anti-allergic viscose fiber and its preparation method. This invention solves the technical problems of existing antibacterial and anti-allergic treatments of viscose fibers, such as the biotoxicity of chemical reagents, the tendency to cause white pollution, and the narrow antibacterial spectrum and insufficient anti-allergenic properties of natural antibacterial and anti-allergic solvents.

[0006] To solve the above problems, the present invention adopts the following technical solution:

[0007] A plant-based antibacterial and anti-allergic viscose fiber, the viscose fiber comprising a viscose fiber matrix, fibroin, and a supercritical carbon dioxide extract derived from a plant-based herbal composition;

[0008] The herbal composition consists of cloves, peppermint, mugwort, rosemary, and licorice.

[0009] The mass ratio of the silk fibroin to the viscose in the viscose fiber matrix is ​​(5-15):(85-95).

[0010] This invention also provides a method for preparing the aforementioned plant-based antibacterial and anti-allergic viscose fiber, comprising the following steps:

[0011] I. Raw material pretreatment: The herbal composition is dried and pulverized to obtain herbal granules; the herbal composition consists of clove, peppermint, mugwort, rosemary and licorice.

[0012] II. Supercritical CO2 extraction: The herbal granules obtained in step one are extracted using supercritical carbon dioxide extraction technology to obtain the extract, which is then filtered, concentrated at low temperature and decolorized to obtain a refined antibacterial and anti-allergic extract.

[0013] 3. Preparation of viscose spinning solution: Blend silk fibroin with viscose spinning solution to obtain mixed spinning solution;

[0014] IV. Wet spinning: The refined antibacterial and anti-allergic extract obtained in step 2 is blended with the mixed spinning solution obtained in step 3, and then plant-based antibacterial and anti-allergic viscose fiber is prepared by wet spinning process.

[0015] As a preferred technical solution: in step one, the drying temperature is 40~50℃; the particle size of the pulverized material is 3mm.

[0016] As a preferred technical solution: In step two, the supercritical carbon dioxide extraction includes static extraction and dynamic cyclic extraction;

[0017] The static extraction conditions are: extraction pressure 35~45MPa, extraction temperature 35~55℃, and standing soaking time 30~60min.

[0018] The conditions for dynamic cyclic extraction are: maintain constant temperature and pressure, and cyclic extraction for 2-4 hours.

[0019] As a preferred technical solution:

[0020] In step two, after supercritical carbon dioxide extraction, there is also a desorption and separation step: supercritical carbon dioxide carrying the active ingredients is introduced into the separation vessel, the pressure is reduced to 5~10MPa, and the temperature is controlled at 45~60℃, so that the active ingredients are desorbed and aggregated.

[0021] As a preferred technical solution: In step two, the filtration is carried out by using 2 to 4 layers of filter paper and combining the filtrates 3 to 5 times;

[0022] The conditions for the low-temperature concentration are: vacuum pressure -0.07 to -0.09 MPa, and temperature 40 to 55°C.

[0023] The decolorization process is as follows: 2% to 6% ethanol by weight of viscose spinning solution is added to the concentrated extract, and the mixture is stirred at room temperature for 45 to 80 minutes, and then filtered through a microporous membrane.

[0024] As a preferred technical solution: In step three, the mass ratio of the fibroin to the viscose in the viscose spinning solution is (5-15):(85-95).

[0025] As a preferred technical solution: In step 4), the wet spinning process includes filtration, defoaming, spinning, coagulation, stretching, alkali washing, drying and heat setting processes.

[0026] Compared with the prior art, the advantages of this invention are:

[0027] I. The five herbal ingredients in this formula—clove, peppermint, mugwort, rosemary, and licorice—are common antibacterial and anti-allergic herbal medicines. They all contain active antibacterial and anti-allergic components such as volatile oils, flavonoids, and polyphenols. These five herbal medicines achieve their antibacterial effect by disrupting cell membranes and inhibiting nucleic acid protein metabolism, thereby blocking bacterial proliferation and biofilm formation. They also achieve their anti-allergic effect by stabilizing mast cells, inhibiting the release of allergy mediators, regulating immune balance, providing antioxidant and anti-inflammatory effects, and repairing the skin barrier.

[0028] II. In this solution, the viscose and fibroin blended spinning solution physically encapsulates the antibacterial and anti-allergic components of the herbal medicines within the fiber during the wet spinning process. Simultaneously, the fibroin molecules exhibit good compatibility with viscose cellulose, and their abundant amino and carboxyl groups further enhance the interaction with the antibacterial and anti-allergic components of the herbal medicines, strengthening their adhesion to the fiber. The antibacterial and anti-allergic components in the herbal medicines are all natural macromolecules, green and pollution-free.

[0029] Third, the fibroin in this formulation possesses excellent moisture absorption, breathability, softness, and comfort. Its protein structure endows fibroin with high tensile strength and elastic recovery rate. Adding different proportions of fibroin to viscose spinning solutions can adjust the viscosity and flowability of the solution, improve the stability of wet spinning, and simultaneously enhance the moisture absorption, breathability, softness, comfort, tensile strength, and elastic recovery of viscose fibers, making the spun fabric more abrasion-resistant. Furthermore, fibroin contains amino acids such as serine, tyrosine, and lysine, as well as polar groups such as peptide bonds, hydroxyl (-OH), and amino (-NH2). The amino acids in fibroin can interact with the surface of bacterial and microbial cell membranes, leading to bacterial and microbial death. The fibroin peptides in fibroin protein can further enhance antibacterial and anti-allergic effects.

[0030] IV. The plant-based antibacterial and anti-allergic viscose fiber prepared by this invention, as tested according to GB / T31713-2015 standard, has an antibacterial and anti-allergic rate of over 95%, achieving natural, long-lasting, and highly efficient antibacterial and anti-allergic properties. At the same time, it avoids the biological toxicity and white pollution problems caused by chemical reagents, and has good environmental protection and comfort. It can be widely used in the field of functional textile materials. Attached Figure Description

[0031] Figure 1 This is a process flow diagram of the present invention. Detailed Implementation

[0032] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0033] Example 1

[0034] like Figure 1 As shown, a plant-based antibacterial and anti-allergic viscose fiber and its preparation method are disclosed. The specific process is as follows:

[0035] I. Raw material pretreatment: Select 200g of five Chinese herbal medicines: clove, peppermint, mugwort, rosemary, and licorice. Control the drying temperature to 40℃ and pulverize to a particle size of about 3mm to ensure uniform particle size and prevent uneven extraction.

[0036] II. Supercritical CO2 Extraction:

[0037] ① Preparation for supercritical CO2 extraction: Evenly fill the extraction vessel with the pulverized herbal medicine particles, press them appropriately and ensure that the flow channel is unobstructed, close the vessel door and seal it for inspection, check the pipeline, pressure regulating valve, separation vessel and cooling system, and purge the air in the equipment to avoid oxidation affecting the active ingredients;

[0038] ② CO2 refrigeration and liquefaction: The refrigeration unit cools down to the critical temperature of 31.1℃ and the critical pressure of 7.38MPa, condensing gaseous CO2 into liquid CO2 and maintaining low temperature and stable pressure;

[0039] ③ Supercritical CO2 static extraction: Set the extraction pressure to 35 MPa and the extraction temperature to 35 °C, and maintain the set pressure and temperature for static soaking for 30 min;

[0040] ④ Supercritical CO2 dynamic circulation extraction: Start the circulation, supercritical CO2 promotes the continuous dissolution of active ingredients, maintain constant temperature and pressure, and circulate for 2 hours;

[0041] ⑤ Separation: Supercritical CO2 carries the active ingredients into the separation vessel, the pressure is reduced to 5MPa, and the temperature is controlled at 45℃, so that the fat-soluble antibacterial and anti-allergic herbal ingredients are desorbed and accumulate at the bottom of the separation vessel;

[0042] ⑥ Filtration: The crude extract collected from the outlet of the separation vessel is filtered through 4 layers of filter paper, and the filtrates from the three filtrations are combined to obtain a crude extract containing antibacterial and anti-allergic components.

[0043] ⑦ Low-temperature concentration: Place the filtered crude extract in a vacuum low-temperature concentration container, control the vacuum pressure to -0.07MPa and the temperature to 40℃, and concentrate under reduced pressure to obtain concentrated crude extract;

[0044] ⑧ Decolorization treatment: Add 2% ethanol (by weight of viscose spinning solution) to the concentrated crude extract, stir at room temperature for 45 minutes, and then filter through a microporous membrane to obtain a refined antibacterial and anti-allergic extract.

[0045] III. Preparation of viscose spinning solution:

[0046] Add silk fibroin to the viscose spinning solution and control the mass ratio of silk fibroin to viscose to be 15:85 to obtain a mixed spinning solution.

[0047] IV. Wet spinning:

[0048] The refined antibacterial and anti-allergic extract obtained in step two is blended with the mixed spinning solution obtained in step three, and wet spinning is used. The antibacterial and anti-allergic viscose fiber is prepared through processes such as filtration, degassing, spinning, coagulation, stretching, alkali washing, drying, and heat setting.

[0049] Example 2

[0050] This embodiment is basically the same as Embodiment 1, except that the process parameters are adjusted as follows:

[0051] I. Raw material pretreatment: Select 250g of five Chinese herbal medicines: clove, mint, mugwort, rosemary, and licorice. Control the drying temperature at 45℃ and pulverize them to a particle size of about 3mm.

[0052] II. Supercritical CO2 Extraction:

[0053] ① Preparation for supercritical CO2 extraction: Evenly fill the extraction vessel with the pulverized herbal medicine particles, press them appropriately and ensure that the flow channel is unobstructed, close the vessel door and seal it for inspection, check the pipeline, pressure regulating valve, separation vessel and cooling system, and purge the air in the equipment to avoid oxidation affecting the active ingredients;

[0054] ② CO2 refrigeration and liquefaction: The refrigeration unit cools down to the critical temperature of 31.1℃ and the critical pressure of 7.38MPa, condensing gaseous CO2 into liquid CO2 and maintaining low temperature and stable pressure;

[0055] ③ Static extraction: Extraction pressure is 40 MPa, extraction temperature is 45℃, and the mixture is allowed to stand for 45 minutes.

[0056] ④ Dynamic Circulation Extraction: Circulation extraction for 3 hours;

[0057] ⑤ Separation: Reduce the pressure to 7MPa and control the temperature at 55℃;

[0058] ⑥ Filtration: Use 3 layers of filter paper for filtration, and combine the filtrates from 4 filtrations;

[0059] ⑦ Low-temperature concentration: vacuum pressure is -0.08MPa, temperature is 50℃;

[0060] ⑧ Decolorization treatment: Add 4% ethanol by weight of viscose spinning solution and stir at room temperature for 60 minutes.

[0061] III. Preparation of viscose spinning solution: Control the mass ratio of silk fibroin to viscose to be 10:90;

[0062] The remaining operations (including extraction preparation, CO2 refrigeration liquefaction, wet spinning, etc.) are the same as in Example 1.

[0063] Example 3

[0064] This embodiment is basically the same as Embodiment 1, except that the process parameters are adjusted as follows:

[0065] I. Raw material pretreatment: Select 300g of five Chinese herbal medicines: clove, mint, mugwort, rosemary, and licorice. Control the drying temperature at 50℃ and pulverize them to a particle size of about 3mm.

[0066] II. Supercritical CO2 Extraction:

[0067] ① Preparation for supercritical CO2 extraction: Evenly fill the extraction vessel with the pulverized herbal medicine particles, press them appropriately and ensure that the flow channel is unobstructed, close the vessel door and seal it for inspection, check the pipeline, pressure regulating valve, separation vessel and cooling system, and purge the air in the equipment to avoid oxidation affecting the active ingredients;

[0068] ② CO2 refrigeration and liquefaction: The refrigeration unit cools down to the critical temperature of 31.1℃ and the critical pressure of 7.38MPa, condensing gaseous CO2 into liquid CO2 and maintaining low temperature and stable pressure;

[0069] ③ Static extraction: Extraction pressure is 45 MPa, extraction temperature is 55℃, and the mixture is allowed to stand for 60 minutes.

[0070] ④ Dynamic Circulation Extraction: Circulation extraction for 4 hours;

[0071] ⑤ Separation: Reduce the pressure to 10 MPa and control the temperature at 60℃;

[0072] ⑥ Filtration: Use 4 layers of filter paper for filtration, and combine the filtrates from 5 filtrations;

[0073] ⑦ Low-temperature concentration: vacuum pressure is -0.09MPa, temperature is 55℃;

[0074] ⑧ Decolorization treatment: Add 6% ethanol by weight of viscose spinning solution and stir at room temperature for 80 minutes.

[0075] III. Preparation of viscose spinning solution: Control the mass ratio of silk fibroin to viscose to be 5:95;

[0076] The remaining operations (including extraction preparation, CO2 refrigeration liquefaction, wet spinning, etc.) are the same as in Example 1.

[0077] Performance test results

[0078] The plant-based antibacterial and anti-allergic viscose fibers prepared in Examples 1-3 were tested for antibacterial (Staphylococcus aureus) and anti-allergic properties according to GB / T31713-2015 and 20251598-T-608 standards. The results are shown in the table below:

[0079] Example Silk fibroin: viscose mass ratio Antibacterial rate (%) Anti-allergy rate (%) 1 15:85 96.2 95.8 2 10:90 97.1 96.5 3 5:95 95.9 95.3

[0080] As shown in the table above, the plant-based antibacterial and anti-allergic viscose fiber prepared by this invention has an antibacterial rate and an anti-allergy rate of over 95%, exhibiting excellent and long-lasting antibacterial and anti-allergic properties.

[0081] The above description is merely a preferred embodiment of the present invention; however, the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and its improved concepts, should be covered within the scope of protection of the present invention.

Claims

1. A plant-based antibacterial and hypoallergenic viscose fiber, characterized in that, The viscose fiber comprises a viscose fiber matrix, fibroin, and a supercritical carbon dioxide extract derived from a herbal composition. The herbal composition consists of cloves, peppermint, mugwort, rosemary, and licorice.

2. The plant-based antibacterial and anti-allergic viscose fiber according to claim 1, characterized in that, The mass ratio of the silk fibroin to the viscose in the viscose fiber matrix is ​​(5-15):(85-95).

3. A method for producing plant-based antibacterial and anti-allergic viscose fiber as described in claim 1 or 2, characterized in that, Includes the following steps: I. Raw material pretreatment: The herbal composition is dried and pulverized to obtain herbal granules; the herbal composition consists of clove, peppermint, mugwort, rosemary and licorice. II. Supercritical CO2 extraction: The herbal granules obtained in step one are extracted using supercritical carbon dioxide extraction technology to obtain the extract, which is then filtered, concentrated at low temperature and decolorized to obtain a refined antibacterial and anti-allergic extract.

3. Preparation of viscose spinning solution: Blend silk fibroin with viscose spinning solution to obtain mixed spinning solution; IV. Wet spinning: The refined antibacterial and anti-allergic extract obtained in step 2 is blended with the mixed spinning solution obtained in step 3, and then plant-based antibacterial and anti-allergic viscose fiber is prepared by wet spinning process.

4. The method for preparing plant-based antibacterial and anti-allergic viscose fiber according to claim 3, characterized in that, In step one, the drying temperature is 40~50℃; the particle size of the pulverized material is 3mm.

5. The method for preparing plant-based antibacterial and anti-allergic viscose fiber according to claim 3, characterized in that, In step two, the supercritical carbon dioxide extraction includes static extraction and dynamic cyclic extraction; The static extraction conditions are: extraction pressure 35~45MPa, extraction temperature 35~55℃, and standing soaking time 30~60min. The conditions for dynamic cyclic extraction are: maintain constant temperature and pressure, and cyclic extraction for 2-4 hours.

6. A method for preparing plant-based antibacterial and anti-allergic viscose fiber according to claim 3 or 5, characterized in that, In step two, after supercritical carbon dioxide extraction, there is also a desorption and separation step: supercritical carbon dioxide carrying the active ingredients is introduced into the separation vessel, the pressure is reduced to 5~10MPa, and the temperature is controlled at 45~60℃, so that the active ingredients are desorbed and aggregated.

7. The method for preparing plant-based antibacterial and anti-allergic viscose fiber according to claim 3, characterized in that, In step two, the filtration is carried out using 2 to 4 layers of filter paper, and the filtrates are combined 3 to 5 times; The conditions for the low-temperature concentration are: vacuum pressure -0.07 to -0.09 MPa, and temperature 40 to 55°C. The decolorization process is as follows: 2% to 6% ethanol by weight of viscose spinning solution is added to the concentrated extract, and the mixture is stirred at room temperature for 45 to 80 minutes, and then filtered through a microporous membrane.

8. The method for preparing plant-based antibacterial and anti-allergic viscose fiber according to claim 3, characterized in that, In step three, the mass ratio of the fibroin to the viscose in the viscose spinning solution is (5-15):(85-95).

9. The method for preparing plant-based antibacterial and anti-allergic viscose fiber according to claim 3, characterized in that, In step 4), the wet spinning process includes filtration, defoaming, spinning, coagulation, stretching, alkali washing, drying and heat setting.

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