Viscose fiber containing hyaluronic acid composite microcapsule and preparation method thereof

Abstract

The invention belongs to the technical field of textile materials, and particularly discloses viscose containing hyaluronic acid composite microcapsules and a preparation method of the viscose. The preparation method of the fiber comprises the following steps: S1, uniformly mixing antibacterial plant essential oil, beta-cyclodextrine and polymethyl methacrylate in a solvent to prepare an oil phase; adding hyaluronic acid powder into water, and uniformly mixing to obtain a water phase; mixing the oil phase with the water phase, adding an emulsifier, and carrying out shear emulsification to obtain an emulsion; and homogenizing the emulsion, and carrying out spray drying to obtain the hyaluronic acid composite microcapsule. S2, adding the hyaluronic acid composite microcapsules in the step S1 into a viscose spinning solution, and uniformly stirring and dispersing to obtain a spinning solution; and S3, carrying out wet spinning on the spinning solution obtained in the step S2 to obtain the viscose fiber containing the hyaluronic acid composite microcapsule. The fiber provided by the invention has lasting moisturizing and antibacterial functions, and is good in washing resistance.

Description

Technical Field

[0001] This application relates to the field of textile materials technology, and in particular to a viscose fiber containing hyaluronic acid composite microcapsules and its preparation method. Background Technology

[0002] Hyaluronic acid, also known as hyaluronan, or HA for short, possesses strong hygroscopic and moisturizing properties. It dissolves slowly and completely in water, forming a viscous, slightly milky white or colorless solution. Developing fabrics with moisturizing and other functional properties based on hyaluronic acid has become one of the innovative research directions in functional home textiles in recent years. However, hyaluronic acid is a water-soluble substance and is easily lost during washing. Microencapsulating hyaluronic acid and then mixing the microcapsules with fiber raw materials, followed by fiber preparation using spinning techniques such as wet spinning and melt spinning, allows the microcapsules to be evenly dispersed inside or outside the fiber. This enables efficient utilization and sustained release of hyaluronic acid within the fiber, thus solving the problem of poor water resistance. However, how to further effectively improve the sustained-release effect of the microcapsules remains a major research focus.

[0003] Viscose fiber is a regenerated cellulose fiber with good breathability and strong moisture absorption. Introducing hyaluronic acid into viscose fiber can allow it to inherit the moisturizing properties of hyaluronic acid, absorbing moisture through hyaluronic acid molecules on the fiber surface, thus improving the fabric's skin-friendliness and comfort. Furthermore, adding other functional components to give viscose fiber even more functional properties, such as antibacterial and flame-retardant properties, aligns with the innovative development direction of viscose fiber and helps to enrich its application scenarios. Summary of the Invention

[0004] In view of the shortcomings of the prior art described above, the purpose of this application is to provide a viscose fiber containing hyaluronic acid composite microcapsules and a method for preparing the same. The hyaluronic acid composite microcapsules contain hyaluronic acid and antibacterial components (such as antibacterial plant essential oils), thereby endowing the viscose fiber with dual functions of moisturizing and skin care and antibacterial properties. At the same time, through the optimized design of the wall material components and the microcapsule preparation process, the functional components in the microcapsules can be released more persistently, further improving the water resistance.

[0005] To achieve the above and other related objectives, this application provides a method for preparing viscose fibers containing hyaluronic acid composite microcapsules, characterized by comprising the following steps: S1. Preparation of hyaluronic acid composite microcapsules: Antibacterial plant essential oil, β-cyclodextrin and polymethyl methacrylate were mixed evenly in a solvent to obtain an oil phase; Hyaluronic acid powder is added to water and mixed evenly to obtain an aqueous phase; After mixing the oil phase and the water phase, an emulsifier is added, and the mixture is sheared and emulsified to obtain an emulsion. After homogenization, the emulsion was spray-dried to obtain hyaluronic acid composite microcapsules; S2. Add the hyaluronic acid composite microcapsules from step S1 to the viscose spinning solution, stir and disperse evenly to obtain the spinning solution. S3. Using the spinning solution from step S2, viscose fibers containing hyaluronic acid composite microcapsules are obtained by wet spinning.

[0006] Furthermore, in step S1, the mass ratio of antibacterial plant essential oil, β-cyclodextrin (β-CD), polymethyl methacrylate (PMMA) and hyaluronic acid is 0.5~2:2~6:10~20:0.5~2.

[0007] Furthermore, in step S1, the concentration of polymethyl methacrylate in the oil phase is 1~3 mg / mL.

[0008] Furthermore, in step S1, the concentration of hyaluronic acid powder in the aqueous phase is 0.5~2 mg / mL.

[0009] Furthermore, in step S1, the oil-to-water ratio is 8~10:1.

[0010] Furthermore, in step S1, the method for preparing the oil phase includes the following steps: adding β-cyclodextrin, polymethyl methacrylate and antibacterial plant essential oil sequentially to an organic solvent, stirring and dispersing evenly to obtain the oil phase.

[0011] Furthermore, in step S1, the antibacterial plant essential oil is selected from at least one of tea tree essential oil, peppermint essential oil, rose essential oil, or lavender essential oil.

[0012] Furthermore, in step S1, the shearing rate is 6000~8000 r / min, and the time is 5~10 min.

[0013] Furthermore, in step S1, the homogenization process includes a primary homogenization process and a secondary homogenization process. The primary homogenization pressure is 15~20 MPa, and the secondary homogenization pressure is 3~5 MPa.

[0014] Furthermore, in step S2, the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:1~15.

[0015] Furthermore, in step S3, the wet spinning process parameters include: a spinneret orifice diameter of 0.05~0.1mm and a spinning speed of 20~80m / min.

[0016] This application also provides a viscose fiber containing hyaluronic acid composite microcapsules prepared according to the method described above.

[0017] As described above, the viscose fiber containing hyaluronic acid composite microcapsules and its preparation method of this application have the following beneficial effects: This application uses hyaluronic acid aqueous solution as the aqueous phase and antibacterial plant essential oil, β-cyclodextrin and polymethyl methacrylate as the oil phase. Hyaluronic acid composite microcapsules are prepared by shear emulsification, homogenization and spray drying. Then, the hyaluronic acid composite microcapsules are added to viscose spinning solution and a new type of viscose fiber with relatively long-lasting moisturizing and antibacterial functions is prepared by wet spinning technology.

[0018] The microcapsules in this application use HA as the core material and PMMA and β-CD as the wall material. The wall material also contains antibacterial plant essential oils. PMMA, as the main component of the wall material, provides a physical barrier to control the release of HA and antibacterial plant essential oils. The addition of β-CD can further improve the sustained-release effect of the two functional components, improve water resistance, and make the fiber have a more lasting moisturizing and antibacterial effect. Detailed Implementation

[0019] The following specific examples illustrate the implementation of this application. Those skilled in the art can easily understand other advantages and effects of this application from the content disclosed in this specification. This application can also be implemented or applied through other different specific embodiments. Various details in this specification can also be modified or changed based on different viewpoints and applications without departing from the spirit of this application. In the absence of conflict, the following embodiments and features in the embodiments can be combined with each other.

[0020] In this application, unless otherwise stated, the term "multiple" means two or more.

[0021] The character " / " indicates that the objects before and after it are in an "or" relationship. For example, A / B means: A or B.

[0022] The term "and / or" describes an association between objects, indicating that three relationships can exist. For example, A and / or B means: A or B, or A and B.

[0023] One embodiment of this application provides a method for preparing viscose fibers containing hyaluronic acid composite microcapsules, characterized by comprising the following steps: S1. Preparation of hyaluronic acid composite microcapsules: Antibacterial plant essential oil, β-CD and PMMA were mixed evenly in a solvent to obtain an oil phase; Hyaluronic acid powder is added to water and mixed evenly to obtain an aqueous phase; After mixing the oil phase and the water phase, an emulsifier is added, and the mixture is sheared and emulsified to obtain an emulsion. After homogenization, the emulsion was spray-dried to obtain hyaluronic acid composite microcapsules; S2. Add the hyaluronic acid composite microcapsules from step S1 to the viscose spinning solution, stir and disperse evenly to obtain the spinning solution. S3. Using the spinning solution from step S2, viscose fibers containing hyaluronic acid composite microcapsules are obtained by wet spinning.

[0024] This application uses hyaluronic acid aqueous solution as the aqueous phase and antibacterial plant essential oil, β-CD and PMMA as the oil phase. Hyaluronic acid composite microcapsules are prepared by shear emulsification, homogenization and spray drying. Then, the hyaluronic acid composite microcapsules are added to viscose spinning solution and a new type of viscose fiber with relatively long-lasting moisturizing and antibacterial functions is prepared by wet spinning technology.

[0025] The microcapsules in this application use HA as the core material, with PMMA and β-CD as the wall material, and also contain antibacterial plant essential oils. PMMA, as the main component of the wall material, provides a physical barrier to control the release of HA and antibacterial plant essential oils. The addition of β-CD further enhances the sustained-release effect of the two functional components, improves washability, and gives the fibers a more lasting moisturizing and antibacterial effect. The reasons for this may be that PMMA has good mechanical strength and film-forming properties, providing good structural support and rupture resistance for the microcapsules. The hydrophilic surface of β-CD forms a more uniform interface with the aqueous phase (HA), thus constructing a denser diffusion barrier inside the microcapsules and slowing down the release rate of HA. The hydrophobic cavities inside β-CD can effectively encapsulate hydrophobic active ingredients such as antibacterial plant essential oils, forming stable inclusion complexes. This inclusion effect further controls the release of antibacterial plant essential oils. Therefore, when β-CD and PMMA are used together as the wall material, they work synergistically to achieve a longer-lasting and more controllable sustained-release effect.

[0026] In some embodiments of this application, in step S1, the mass ratio of antibacterial plant essential oil, β-CD, PMMA, and hyaluronic acid is 0.5~2:2~6:10~20:0.5~2. The concentration of PMMA in the oil phase is, for example, 1~3 mg / mL, and the concentration of hyaluronic acid powder in the aqueous phase is, for example, 0.5~2 mg / mL. The oil-to-water ratio is, for example, 8~10:1. The emulsifier includes, but is not limited to, Span 80, Tween 80, etc., and its amount is, for example, 0.5%~1.0% (this amount is by volume). The antibacterial plant essential oil is selected from at least one of tea tree oil, peppermint oil, rose oil, or lavender oil. In addition to its antibacterial properties, the above-mentioned antibacterial plant essential oil also has an aromatic scent, which can have soothing and sleep-aiding effects.

[0027] In some embodiments of this application, step S1, the method for preparing the oil phase includes the following steps: β-CD, PMMA, and antibacterial plant essential oils are sequentially added to an organic solvent and stirred until evenly dispersed to obtain the oil phase. The organic solvent can be, for example, N,N-dimethylformamide (DMF), but is not limited to this. β-CD has relatively low solubility in organic solvents such as DMF, so it is added first. Heating or other methods can be used to help β-CD dissolve better and faster. Then, PMMA, which is used in the largest quantity, is added and stirred until dissolved and evenly dispersed. Finally, the antibacterial plant essential oil is added and stirred until evenly dispersed to obtain the oil phase.

[0028] In some embodiments of this application, in step S1, the shear rate is 6000~8000 r / min, and the time is 5~10 min. High-speed shear emulsification using a shear emulsifier yields an emulsion forming small droplets.

[0029] In some embodiments of this application, step S1, the homogenization process includes a primary homogenization and a secondary homogenization process. The primary homogenization pressure is 15-20 MPa, and the secondary homogenization pressure is 3-5 MPa. This application preferably employs a two-stage homogenization process: the first stage uses a higher pressure (e.g., 15-20 MPa) for crushing, which can effectively reduce the droplet size to the nanometer scale and improve the encapsulation rate; excessively high pressure may cause mechanical damage to the wall material, while too low pressure will not sufficiently refine the droplets. The second stage uses a lower pressure (e.g., 3-5 MPa) to disperse the crushed small particles and prevent them from re-aggregating. Furthermore, the material is usually preheated to 60-65°C before homogenization to reduce viscosity and improve the homogenization effect.

[0030] In some embodiments of this application, in step S2, the concentration of cellulose in the viscose spinning solution is 3% to 4%, and the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:1 to 15, preferably 100:5 to 15. Increasing the amount of hyaluronic acid composite microcapsules will improve the moisturizing and antibacterial properties of the fiber, but its dosage should not be too high, otherwise it may affect the mechanical properties and other indicators of the fiber.

[0031] In some embodiments of this application, step S3, the wet spinning process includes: conveying the spinning solution to the spinneret, extruding it into the coagulation bath, and stretching it into shape; wherein, the wet spinning process parameters include: the spinneret orifice diameter is 0.05~0.1mm, the spinning speed is 20~80m / min; the coagulation bath is, for example, a mixed aqueous solution composed of 150~160g / L sulfuric acid, 380~400g / L sodium sulfate, and 10~20g / L aluminum sulfate, and the coagulation bath temperature is, for example, 35~45℃.

[0032] Another embodiment of this application provides a viscose fiber containing hyaluronic acid composite microcapsules prepared according to the method described above. The fiber contains microcapsules containing hyaluronic acid and antibacterial plant essential oils, and PMMA and β-CD are used as wall materials. Therefore, it has a relatively long-lasting moisturizing and antibacterial function.

[0033] The following specific examples illustrate the present invention in detail. It should also be understood that the following examples are only for specific illustrative purposes and should not be construed as limiting the scope of protection of the present invention. Any non-essential improvements and adjustments made by those skilled in the art based on the above description of the present invention are within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make appropriate selections within the appropriate range based on the description herein, and are not intended to be limited to the specific values ​​in the examples below.

[0034] Example 1 This embodiment provides a viscose fiber containing hyaluronic acid composite microcapsules, and its preparation method is as follows: S1. Hyaluronic acid composite microcapsules were prepared according to the mass ratio of tea tree oil, β-CD, PMMA, and hyaluronic acid of 1:4:15:1: β-CD was added to DMF and heated and stirred at 50°C to dissolve it. Then PMMA was added and stirred to disperse it evenly. Finally, antibacterial plant essential oil was added and stirred to disperse it evenly to obtain the oil phase. The concentration of PMMA in the oil phase was 1.67 mg / mL. Hyaluronic acid powder is added to water and mixed evenly to obtain an aqueous phase; the concentration of hyaluronic acid powder in the aqueous phase is, for example, 1 mg / mL; The oil and water phases were mixed at a 9:1 oil-to-water ratio, and then Span 80 emulsifier was added. The mixture was sheared and emulsified at 7000 r / min for 8 min to obtain an emulsion. Homogenization was then performed, including a primary homogenization process at 18 MPa and a secondary homogenization process at 4 MPa. Finally, the mixture was spray-dried to obtain hyaluronic acid composite microcapsules.

[0035] S2. Add the hyaluronic acid composite microcapsules from step S1 to the viscose spinning solution with a cellulose concentration of 3%, stir and disperse evenly to obtain the spinning solution; the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:10.

[0036] S3. Using the spinning solution from step S2, viscose fibers containing hyaluronic acid composite microcapsules are obtained by wet spinning. The wet spinning process is as follows: the spinning solution is delivered to a spinneret with an aperture of 0.1 mm, and extruded into a mixed aqueous solution consisting of 150 g / L sulfuric acid, 390 g / L sodium sulfate, and 10 g / L aluminum sulfate at a spinning speed of 60 m / min. The solution is then subjected to a coagulation bath at 40 °C and then stretched into shape.

[0037] Example 2 This embodiment provides a viscose fiber containing hyaluronic acid composite microcapsules, and its preparation method is as follows: S1. Hyaluronic acid composite microcapsules were prepared according to the mass ratio of tea tree oil, β-CD, PMMA, and hyaluronic acid of 0.5:2:10:0.5. β-CD was added to DMF and heated and stirred at 50°C to dissolve it. Then PMMA was added and stirred to disperse it evenly. Finally, antibacterial plant essential oil was added and stirred to disperse it evenly to obtain the oil phase. The concentration of PMMA in the oil phase was 1.11 mg / mL. Hyaluronic acid powder is added to water and mixed evenly to obtain an aqueous phase; the concentration of hyaluronic acid powder in the aqueous phase is, for example, 0.5 mg / mL; The oil and water phases were mixed at a 9:1 oil-to-water ratio, and then Span 80 emulsifier was added. The mixture was sheared and emulsified at 7000 r / min for 8 min to obtain an emulsion. Homogenization was then performed, including a primary homogenization process at 18 MPa and a secondary homogenization process at 4 MPa. Finally, the mixture was spray-dried to obtain hyaluronic acid composite microcapsules.

[0038] S2. Add the hyaluronic acid composite microcapsules from step S1 to the viscose spinning solution with a cellulose concentration of 3%, stir and disperse evenly to obtain the spinning solution; the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:10.

[0039] S3. Using the spinning solution from step S2, viscose fibers containing hyaluronic acid composite microcapsules are obtained by wet spinning. The wet spinning process is as follows: the spinning solution is delivered to a spinneret with an aperture of 0.1 mm, and extruded into a mixed aqueous solution consisting of 150 g / L sulfuric acid, 390 g / L sodium sulfate, and 10 g / L aluminum sulfate at a spinning speed of 60 m / min. The solution is then subjected to a coagulation bath at 40 °C and then stretched into shape.

[0040] Example 3 This embodiment provides a viscose fiber containing hyaluronic acid composite microcapsules, and its preparation method is as follows: S1. Hyaluronic acid composite microcapsules were prepared according to the mass ratio of tea tree oil, β-CD, PMMA, and hyaluronic acid of 2:6:20:2. β-CD was added to DMF and heated and stirred at 50°C to dissolve it. Then PMMA was added and stirred to disperse it evenly. Finally, antibacterial plant essential oil was added and stirred to disperse it evenly to obtain the oil phase. The concentration of PMMA in the oil phase was 2.22 mg / mL. Hyaluronic acid powder is added to water and mixed evenly to obtain an aqueous phase; the concentration of hyaluronic acid powder in the aqueous phase is, for example, 2 mg / mL; The oil and water phases were mixed at a 9:1 oil-to-water ratio, and then Span 80 emulsifier was added. The mixture was sheared and emulsified at 7000 r / min for 8 min to obtain an emulsion. Homogenization was then performed, including a primary homogenization process at 18 MPa and a secondary homogenization process at 4 MPa. Finally, the mixture was spray-dried to obtain hyaluronic acid composite microcapsules.

[0041] S2. Add the hyaluronic acid composite microcapsules from step S1 to the viscose spinning solution with a cellulose concentration of 3%, stir and disperse evenly to obtain the spinning solution; the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:10.

[0042] S3. Using the spinning solution from step S2, viscose fibers containing hyaluronic acid composite microcapsules are obtained by wet spinning. The wet spinning process is as follows: the spinning solution is delivered to a spinneret with an aperture of 0.1 mm, and extruded into a mixed aqueous solution consisting of 150 g / L sulfuric acid, 390 g / L sodium sulfate, and 10 g / L aluminum sulfate at a spinning speed of 60 m / min. The solution is then subjected to a coagulation bath at 40 °C and then stretched into shape.

[0043] Example 4 This embodiment provides a viscose fiber containing hyaluronic acid composite microcapsules. The only difference between its preparation method and that of Example 1 is that in step S1, the oil-water ratio is 8:1.

[0044] Example 5 This embodiment provides a viscose fiber containing hyaluronic acid composite microcapsules. The only difference between its preparation method and that of Example 1 is that in step S1, the oil-to-water ratio is 10:1.

[0045] Example 6 This embodiment provides a viscose fiber containing hyaluronic acid composite microcapsules. The only difference between the preparation method and that of Embodiment 1 is that in step S2, the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:5.

[0046] Example 7 This embodiment provides a viscose fiber containing hyaluronic acid composite microcapsules. The only difference between this preparation method and that of Embodiment 1 is that in step S2, the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:15.

[0047] Comparative Example 1 This comparative example provides a viscose fiber containing hyaluronic acid composite microcapsules, and its preparation method is as follows: S1. Hyaluronic acid composite microcapsules were prepared according to the mass ratio of tea tree oil, PMMA, and hyaluronic acid of 1:15:1: PMMA was added to DMF and stirred until dissolved. Then, antibacterial plant essential oil was added and stirred until evenly dispersed to obtain the oil phase. The concentration of PMMA in the oil phase was 1.67 mg / mL. Hyaluronic acid powder is added to water and mixed evenly to obtain an aqueous phase; the concentration of hyaluronic acid powder in the aqueous phase is, for example, 1 mg / mL; The oil and water phases were mixed at a 9:1 oil-to-water ratio, and then Span 80 emulsifier was added. The mixture was sheared and emulsified at 7000 r / min for 8 min to obtain an emulsion. Homogenization was then performed, including a primary homogenization process at 18 MPa and a secondary homogenization process at 4 MPa. Finally, the mixture was spray-dried to obtain hyaluronic acid composite microcapsules.

[0048] S2. Add the hyaluronic acid composite microcapsules from step S1 to the viscose spinning solution with a cellulose concentration of 3%, stir and disperse evenly to obtain the spinning solution; the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:10.

[0049] S3. Using the spinning solution from step S2, viscose fibers containing hyaluronic acid composite microcapsules are obtained by wet spinning. The wet spinning process is as follows: the spinning solution is delivered to a spinneret with an aperture of 0.1 mm, and extruded into a mixed aqueous solution consisting of 150 g / L sulfuric acid, 390 g / L sodium sulfate, and 10 g / L aluminum sulfate at a spinning speed of 60 m / min. The solution is then subjected to a coagulation bath at 40 °C and then stretched into shape.

[0050] Performance testing The fibers from Examples 1-3 and Comparative Example 1 were respectively prepared into fabrics as samples, and the hyaluronic acid content and antibacterial properties of the fabrics before and after washing were tested according to the following method. The test results are shown in Tables 1 and 2.

[0051] 1. Hyaluronic acid content test: The hyaluronic acid content in the sample was determined according to Q / 320691KDA67-2019 "Determination of Hyaluronic Acid Content in Textiles".

[0052] 2. Antibacterial test: Cut the fabric into 5mm*5mm pieces, weigh 0.75±0.05g as a sample, wrap it in paper, and put the small paper package containing the sample into an autoclave. Sterilize at 121℃ and 103kPa for 15min. Test the antibacterial properties of the sample according to GB / T20994.3-2008 Evaluation of antibacterial properties of textiles - Part 3: Vibration method. The result is recorded as the antibacterial rate.

[0053] 3. Water wash resistance test: According to GB / T 8629-2017 "Home Washing and Drying Procedures for Textile Testing", each sample was washed, and the hyaluronic acid content and antibacterial properties of each sample were determined after 5, 15, and 30 washes.

[0054] The washing steps for each sample are as follows: Cut each sample into three 20*20cm fabric pieces, pour detergent into water, and prepare a washing solution at a concentration of 5ml / L. Soak the fabric sample in the washing solution and stir and rinse for 5 minutes; remove the fabric sample and rinse with clean water, stirring for 5 minutes each time, changing the water after each rinse, for a total of three rinses; remove the fabric sample, place it in a drying basket, and lay it flat to dry at room temperature, away from light. The washing process was repeated, and fabric samples were finally obtained after 5, 15, and 30 rinsings, respectively.

[0055] Table 1. Hyaluronic acid content (unit: mg / kg) before and after water washing

[0056] Table 2. Antibacterial rate (unit: %) before and after washing

[0057] Note: Strain 1 is Staphylococcus aureus (ATCC6538), and strain 2 is Escherichia coli (ATCC25922).

[0058] As shown in Table 1, after 30 washes, the hyaluronic acid loss rates of fabrics made from the fibers of Examples 1-3 were 30.1%, 29.7%, and 30.7%, respectively, while the hyaluronic acid loss rate of fabric made from the fibers of Comparative Example 1 was 50.4%. The comparison between Example 1 and Comparative Example 1 shows that the addition of cyclodextrin can reduce the hyaluronic acid loss rate. This indicates that the addition of cyclodextrin improves the sustained-release effect of hyaluronic acid in the microcapsules, improves wash resistance, and enables the fibers and fabrics made from them to have a more lasting moisturizing effect.

[0059] As shown in Table 2, after 30 washes, the antibacterial rate of the fabric made from the fiber of Example 1 decreased less than that of Comparative Example 1. This indicates that the addition of cyclodextrin improved the sustained-release effect of tea tree oil in the microcapsules, improved the washability, and enabled the fiber and the fabric made from it to have a more lasting antibacterial effect.

[0060] The above embodiments are merely illustrative of the principles and effects of this application and are not intended to limit this application. Any person skilled in the art can modify or alter the above embodiments without departing from the spirit and scope of this application. Therefore, all equivalent modifications or alterations made by those skilled in the art without departing from the spirit and technical concept disclosed in this application should still be covered by the claims of this application.

Claims

1. A method for preparing viscose fiber containing hyaluronic acid composite microcapsules, characterized in that, Includes the following steps: S1. Preparation of hyaluronic acid composite microcapsules: Antibacterial plant essential oil, β-cyclodextrin and polymethyl methacrylate were mixed evenly in a solvent to obtain an oil phase; Hyaluronic acid powder is added to water and mixed evenly to obtain an aqueous phase; After mixing the oil phase and the water phase, an emulsifier is added, and the mixture is sheared and emulsified to obtain an emulsion. After homogenization, the emulsion was spray-dried to obtain hyaluronic acid composite microcapsules; S2. Add the hyaluronic acid composite microcapsules from step S1 to the viscose spinning solution, stir and disperse evenly to obtain the spinning solution. S3. Using the spinning solution from step S2, viscose fibers containing hyaluronic acid composite microcapsules are obtained by wet spinning.

2. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to claim 1, characterized in that: In step S1, the mass ratio of antibacterial plant essential oil, β-cyclodextrin, polymethyl methacrylate and hyaluronic acid is 0.5~2:2~6:10~20:0.5~2.

3. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to claim 2, characterized in that: In step S1, the concentration of polymethyl methacrylate in the oil phase is 1~3 mg / mL; And / or, the concentration of hyaluronic acid powder in the aqueous phase is 0.5~2 mg / mL; And / or, the oil-to-water ratio is 8~10:

1.

4. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to claim 1, characterized in that: In step S1, the method for preparing the oil phase includes the following steps: β-cyclodextrin, polymethyl methacrylate, and antibacterial plant essential oil were added sequentially to an organic solvent and stirred until evenly dispersed to obtain the oil phase.

5. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to any one of claims 1 to 4, characterized in that: In step S1, the antibacterial plant essential oil is selected from at least one of tea tree essential oil, peppermint essential oil, rose essential oil, or lavender essential oil.

6. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to claim 1, characterized in that: In step S1, the shearing rate is 6000~8000 r / min and the time is 5~10 min.

7. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to claim 1 or 6, characterized in that: In step S1, the homogenization process includes a primary homogenization process and a secondary homogenization process. The primary homogenization pressure is 15~20 MPa, and the secondary homogenization pressure is 3~5 MPa.

8. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to claim 1, characterized in that: In step S2, the mass ratio of the viscose spinning solution to the hyaluronic acid composite microcapsules is 100:1~15.

9. The method for preparing viscose fiber containing hyaluronic acid composite microcapsules according to claim 1, characterized in that: In step S3, the wet spinning process parameters include: spinneret orifice diameter of 0.05~0.1mm and spinning speed of 20~80m / min.

10. Viscose fiber containing hyaluronic acid composite microcapsules prepared by the method according to any one of claims 1 to 9.

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