A viscose large biological fiber containing active ingredients of valeriana and a preparation method thereof

Abstract

The application provides viscose large biological fibers containing active ingredients of radix valerianae and a preparation method thereof, and belongs to the field of viscose fibers; the preparation method comprises the steps of pretreatment of radix valerianae extract, dissolution, preparation of modified pyrophyllite, loading, preparation of blended spinning liquid and spinning; in the dissolution, the pretreated radix valerianae extract is mixed with deionized water, then coconut oil acid, glucose and pentaerythritol are added, uniform stirring is carried out, and then precooling treatment is carried out, the precooling temperature is 0.6-1.2 DEG C, the precooling time is 23-30 min, after the precooling is completed, freezing treatment is carried out, the freezing temperature is -14 to -10 DEG C, the freezing time is 16-25 min, after the freezing treatment is completed, the solution containing radix valerianae extract is naturally restored to room temperature. The fiber prepared by the application has high and long-lasting antibacterial performance, low dimensional deformation rate, excellent and stable strength performance, and high strength performance retention rate after ultraviolet irradiation.

Description

Technical Field

[0001] This invention belongs to the field of viscose fiber technology, specifically relating to a viscose macro-biofiber containing active ingredients of *Hydrangea macrophylla* and its preparation method. Background Technology

[0002] Viscose fiber, also known as viscose cellulose, is made from natural fibers. It is produced by alkalizing, aging, and sulfonating natural fibers to form soluble cellulose xanthate, which is then dissolved in a dilute alkali solution to form viscose. Viscose fiber is then produced by wet spinning. Its moisture absorption meets the physiological needs of human skin, and it has the advantages of being smooth and cool, breathable, antistatic, UV-resistant, and having good color fastness. It is widely used in various fields such as underwear, textiles, and clothing.

[0003] Viscose bio-fibers refer to viscose polymers incorporating certain biofunctional materials to impart one or more properties to the fibers.

[0004] Valerian, also known as sleep herb, is a traditional Chinese medicine. It is mainly used to treat restlessness, weak stomach, back pain, irregular menstruation, and injuries from falls and blows. It also has the effects of lowering blood pressure, relieving insomnia and anxiety, and has excellent antibacterial properties.

[0005] Adding the active ingredient of Hydrangea scabra during the preparation of viscose fiber can improve the antibacterial properties of the fiber. However, the applicant found in the research process that the direct addition method is easy to lose during the subsequent spinning and post-processing, resulting in poor antibacterial properties, short-lasting effect, and failure to meet the requirements for use. Furthermore, the viscose bio-fibers produced by existing technologies have unstable strength properties, and after being exposed to ultraviolet light, their strength properties are significantly reduced, severely shortening their service life. Summary of the Invention

[0006] To address the technical problems existing in the prior art, this invention provides a viscose macro-biofiber containing active ingredients of *Hydrangea macrophylla* and its preparation method, while simultaneously solving the following technical problems: 1. Excellent antibacterial properties and long-lasting effect; 2. It has excellent and stable strength performance, and maintains high strength performance even after being exposed to ultraviolet light.

[0007] To address the aforementioned technical problems, the present invention adopts the following technical solution: 1. Pretreatment of Hypnos nux-vomica extract The extract of *Hydrangea macrophylla* was immersed twice in a pretreatment solution. The temperature of the first immersion was controlled at 14-18℃ and the immersion time was 27-33 min. After the first immersion, a second immersion was performed, with the temperature controlled at 35-40℃ and the immersion time being 23-29 min. During both immersions, ultraviolet-ultrasound treatment was performed. The center wavelength of the ultraviolet lamp was 207-233 nm and the power of the ultraviolet lamp was 263-285 W. The ultrasonic power was 314-337 W. After immersion, the extract was dried to obtain the pretreated extract of *Hydrangea macrophylla*. The extract of *Hydrangea macrophylla* has a particle size of 80-120 nm. The mass ratio of the *Hydrangea macrophylla* extract to the pretreatment solution is 1:2.8-3.5; The pretreatment solution is composed of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid, and the mass ratio of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid is 2.3-2.7:2.0-2.2:1.4-1.8:1.7-2.1:1.0-1.4.

[0008] 2. Dissolve The pretreated Sophora flavescens extract was mixed with deionized water, and then coconut oil, glucose and pentaerythritol were added. After stirring evenly, the mixture was pre-cooled at a temperature of 0.6-1.2℃ for 23-30 minutes. After pre-cooling, the mixture was frozen at a temperature of -14 to -10℃ for 16-25 minutes. After freezing, the mixture was allowed to return to room temperature naturally to obtain a solution containing Sophora flavescens extract. The mass ratio of the pretreated *Symplocos edulis* extract, deionized water, coconut oil acid, glucose, and pentaerythritol is 9-11:88-114:1.4-1.8:0.8-1.3:2.0-2.5.

[0009] 3. Preparation of modified pyrophyllite (1) Sealing treatment Pyrophyllite was washed in potassium permanganate solution for 2.2-2.5 hours. After washing, it was placed in a sealed container and evacuated to a vacuum of 0.06-0.09 MPa. Nitrogen gas was then introduced until the pressure reached 5.0-5.3 MPa. The temperature was raised to 125-128℃ and maintained at that temperature and pressure for 37-45 minutes. After the temperature and pressure were maintained, the pressure was reduced to 3.3-3.9 MPa and the temperature was raised to 137-150℃ and maintained at that temperature and pressure for 30-35 minutes. After the temperature and pressure were maintained, the pressure was immediately released and the temperature was lowered to room temperature to obtain the sealed pyrophyllite. The pyrophyllite has a particle size of 120-160 mesh, a SiO2 mass content of 72-74%, and an Al2O3 mass content of 18-20%. The potassium permanganate solution has a mass concentration of 38-42%. The mass ratio of pyrophyllite to potassium permanganate solution is 1:3.5-4.0; (2) Modification The sealed pyrophyllite was mixed with deionized water, and then carboxymethyl cellulose, palmitic acid, sodium stearate and fatty alcohol polyoxyethylene ether were added. The stirring time was controlled at 25-31 min and the stirring speed was 205-223 rpm. After stirring, the pyrophyllite was dried to obtain the modified pyrophyllite. The mass ratio of the sealed pyrophyllite, deionized water, carboxymethyl cellulose, palmitic acid, sodium stearate, and fatty alcohol polyoxyethylene ether is 25-30:100-120:2.6-3.0:1.6-2.2:3.3-3.8:1.8-2.2.

[0010] 4. Load The modified pyrophyllite was mixed with a solution containing Sophora flavescens extract, and then sodium citrate, sodium dodecylbenzenesulfonate, betaine and adjuvants were added. The mixture was stirred for 37-44 minutes at a stirring speed of 253-267 rpm until it was homogeneous, and then the functional liquid containing Sophora flavescens extract was obtained. The mass ratio of the modified pyrophyllite, the solution containing the extract of *Hydrangea macrophylla*, sodium citrate, sodium dodecylbenzenesulfonate, betaine, and adjuvants is 9-11:99-130:1.6-2.0:2.6-3.1:1.3-1.5:1.0-1.4. The preparation method of the additive is as follows: xanthan gum, gum arabic and gelatin are mixed, then carbon black is added, and ball milling is performed. The ball milling time is controlled at 20-27 min and the ball milling speed is 300-308 rpm. After ball milling, dimethyl silicone oil is added, mixed evenly, and heat-treated at 62-66℃ for 15-20 min. After heat treatment, the mixture is cooled to room temperature to obtain the additive. The mass ratio of xanthan gum, gum arabic, gelatin, carbon black and dimethyl silicone oil is 3.0-3.4:2.6-2.8:4.4-4.8:4.8-5.2:1.7-1.9.

[0011] 5. Preparation of blend spinning solution A blended spinning solution was prepared by mixing a functional liquid containing sleep grass extract with a spinning solution, followed by filtration, degassing, and aging. The mass ratio of the functional dispersion to the spinning solution is 16-18:100; The spinning solution has a cellulose content of 8.6-8.8% and a viscosity of 43-45s.

[0012] 6. Spinning The blended spinning solution is sprayed into a coagulation bath for spinning treatment. After the spinning is solidified, it is washed with water, oiled, and dried to obtain viscose macro-fiber containing the active ingredient of Sophora flavescens.

[0013] The coagulation bath contains the following components: sulfuric acid 96-98 g / L, sodium sulfate 195-197 g / L, and zinc sulfate 21-23 g / L.

[0014] Compared with the prior art, the present invention achieves the following beneficial effects: 1. This invention employs a specific method to pretreat the extract of *Hydrangea macrophylla* and a specific method to dissolve it, thereby improving its dispersion and stability. It also employs specific modified pyrophyllite and auxiliaries for loading, resulting in good immobilization effect. This improves the antibacterial durability while ensuring strength performance. The resulting fiber has a uniform and stable internal structure, low dimensional deformation rate, and maintains high strength performance even after ultraviolet irradiation. 2. The viscose bio-fiber containing the active ingredient of *Hedyotis diffusa* obtained by this invention has an antibacterial rate of 95.3-96.4% against *Escherichia coli*, an antibacterial rate of 93.0-95.8% against *Candida albicans*, and an antibacterial rate of 92.1-95.0% against *Staphylococcus aureus*. The viscose macrofiber containing the active ingredient of *Hedyotis diffusa* obtained by this invention has excellent strength properties, with a dry breaking strength of 4.3-4.9 cN / dtex, a wet breaking strength of 2.8-3.1 cN / dtex, and an elongation at break of 27.6-30.4%. The viscose bio-fiber containing the active ingredient of *Hedyotis diffusa* obtained by this invention has a low dimensional deformation rate. After standing at 72°C for 7 days, the dimensional deformation rate is 1.1-1.6%, and after 50 standard washes, the dimensional deformation rate is 0.5-0.7%. 3. The viscose bio-fiber containing active ingredients of *Hydrangea macrophylla* obtained by this invention has long-lasting antibacterial properties, and can be stored at 600W / m². 2 After 15 days of irradiation under ultraviolet light, the inhibition rate against Escherichia coli was 87.5-89.7%, against Candida albicans was 86.1-87.6%, and against Staphylococcus aureus was 85.5-86.8%. 4. The viscose macrofiber containing the active ingredient of *Hydrangea macrophylla* obtained by this invention has stable strength properties, and can withstand 600 W / m². 2 After 15 days of irradiation under ultraviolet light, the dry fracture strength was 4.0-4.8 cN / dtex, the wet fracture strength was 2.5-2.9 cN / dtex, and the elongation at break was 26.1-29.5%. Detailed Implementation

[0015] To provide a clearer understanding of the technical features, objectives, and effects of the present invention, specific embodiments of the present invention are now described.

[0016] Example 1 1. Pretreatment of Hypnos nux-vomica extract The extract of *Hypophthalmia ulmoides* was immersed twice in a pretreatment solution. The first immersion temperature was controlled at 16℃ and the immersion time was 30 min. After the first immersion, a second immersion was performed, with the temperature controlled at 37℃ and the immersion time being 26 min. During both immersions, ultraviolet-ultrasound treatment was performed. The center wavelength of the ultraviolet lamp was 220 nm, the power of the ultraviolet lamp was 274 W, and the ultrasonic power was 325 W. After immersion, the extract was dried to obtain the pretreated extract of *Hypophthalmia ulmoides*. The extract of the sleepwort has a particle size of 100 nm. The mass ratio of the *Hydrangea macrophylla* extract to the pretreatment solution was 1:3.2; The pretreatment solution is composed of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid, and the mass ratio of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid is 2.5:2.1:1.6:1.9:1.2.

[0017] 2. Dissolve The pretreated Sophora flavescens extract was mixed with deionized water, and then coconut oil, glucose and pentaerythritol were added. After stirring evenly, the mixture was pre-cooled at 0.8℃ for 27 minutes. After pre-cooling, the mixture was frozen at -12℃ for 20 minutes. After freezing, the mixture was allowed to return to room temperature naturally to obtain a solution containing Sophora flavescens extract. The mass ratio of the pretreated *Symplocos edulis* extract, deionized water, coconut oil acid, glucose, and pentaerythritol was 10:100:1.6:1.0:2.3.

[0018] 3. Preparation of modified pyrophyllite (1) Sealing treatment Pyrophyllite was washed in potassium permanganate solution for 2.4 h. After washing, it was placed in a sealed container and evacuated to a vacuum of 0.07 MPa. Nitrogen gas was then introduced until the pressure reached 5.2 MPa. The temperature was raised to 126 °C and maintained at that temperature and pressure for 40 min. After the temperature and pressure maintenance, the pressure was reduced to 3.7 MPa and the temperature was raised to 143 °C and maintained at that temperature and pressure for 32 min. After the temperature and pressure maintenance, the pressure was immediately released and the temperature was lowered to room temperature to obtain the sealed pyrophyllite. The pyrophyllite has a particle size of 140 mesh, a SiO2 mass content of 73%, and an Al2O3 mass content of 19%. The potassium permanganate solution has a mass concentration of 40%. The mass ratio of pyrophyllite to potassium permanganate solution is 1:3.7; (2) Modification The sealed pyrophyllite was mixed with deionized water, and then carboxymethyl cellulose, palmitic acid, sodium stearate and fatty alcohol polyoxyethylene ether were added. The stirring time was controlled at 27 min and the stirring speed was 214 rpm. After stirring, the pyrophyllite was dried to obtain the modified pyrophyllite. The mass ratio of the sealed pyrophyllite, deionized water, carboxymethyl cellulose, palmitic acid, sodium stearate, and fatty alcohol polyoxyethylene ether is 27:106:2.8:1.9:3.6:2.0.

[0019] 4. Load The modified pyrrolizite was mixed with a solution containing Sophora flavescens extract, and then sodium citrate, sodium dodecylbenzenesulfonate, betaine and adjuvants were added. The mixture was stirred for 40 minutes at a stirring speed of 260 rpm until it was homogeneous, and then the functional liquid containing Sophora flavescens extract was obtained. The mass ratio of the modified pyrophyllite, the solution containing the extract of *Hydrangea macrophylla*, sodium citrate, sodium dodecylbenzenesulfonate, betaine, and adjuvants is 10:120:1.8:2.9:1.4:1.2. The preparation method of the additive is as follows: xanthan gum, gum arabic and gelatin are mixed, then carbon black is added, and ball milling is performed. The ball milling time is controlled at 24 min and the ball milling speed is 304 rpm. After ball milling, dimethyl silicone oil is added, mixed evenly, and heat-treated at 64°C for 17 min. After heat treatment, the mixture is lowered to room temperature to obtain the additive. The mass ratio of xanthan gum, gum arabic, gelatin, carbon black and dimethyl silicone oil is 3.2:2.7:4.6:5.0:1.8.

[0020] 5. Preparation of blend spinning solution A blended spinning solution was prepared by mixing a functional liquid containing sleep grass extract with a spinning solution, followed by filtration, degassing, and aging. The mass ratio of the functional dispersion to the spinning solution is 17:100; The spinning solution has a carbonyl content of 8.7% and a viscosity of 44s.

[0021] 6. Spinning The blended spinning solution is sprayed into a coagulation bath for spinning treatment. After the spinning is solidified, it is washed with water, oiled, and dried to obtain viscose macro-fiber containing the active ingredient of Sophora flavescens.

[0022] The coagulation bath contains the following components: sulfuric acid 97 g / L, sodium sulfate 196 g / L, and zinc sulfate 22 g / L.

[0023] Example 2 1. Pretreatment of Hypnos nux-vomica extract The extract of *Hydrangea macrophylla* was immersed twice in a pretreatment solution. The first immersion temperature was controlled at 14℃ and the immersion time was 27 min. After the first immersion, a second immersion was performed, with the temperature controlled at 35℃ and the immersion time being 29 min. During both immersions, ultraviolet-ultrasound treatment was performed. The center wavelength of the ultraviolet lamp was 207 nm, the power of the ultraviolet lamp was 285 W, and the ultrasonic power was 314 W. After immersion, the extract was dried to obtain the pretreated extract of *Hydrangea macrophylla*. The extract of the sleepwort has a particle size of 80 nm. The mass ratio of the *Hydrangea macrophylla* extract to the pretreatment solution was 1:2.8; The pretreatment solution is composed of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid, and the mass ratio of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid is 2.3:2.0:1.4:1.7:1.0.

[0024] 2. Dissolve The pretreated Sophora flavescens extract was mixed with deionized water, and then coconut oil, glucose and pentaerythritol were added. After stirring evenly, the mixture was pre-cooled at 0.6℃ for 23 minutes. After pre-cooling, the mixture was frozen at -14℃ for 16 minutes. After freezing, the mixture was allowed to return to room temperature naturally to obtain a solution containing Sophora flavescens extract. The pretreated *Symplocos edulis* extract, deionized water, coconut oil acid, glucose, and pentaerythritol were in a mass ratio of 9:88:1.4:0.8:2.0.

[0025] 3. Preparation of modified pyrophyllite (1) Sealing treatment Pyrophyllite was washed in potassium permanganate solution for 2.2 h. After washing, it was placed in a sealed container and evacuated to a vacuum of 0.06 MPa. Nitrogen gas was then introduced until the pressure reached 5.0 MPa. The temperature was raised to 128 °C and maintained at that temperature and pressure for 37 min. After the temperature and pressure maintenance, the pressure was reduced to 3.9 MPa and the temperature was raised to 150 °C and maintained at that temperature and pressure for 30 min. After the temperature and pressure maintenance, the pressure was immediately released and the temperature was lowered to room temperature to obtain the sealed pyrophyllite. The pyrophyllite has a particle size of 120 mesh, a SiO2 mass content of 72%, and an Al2O3 mass content of 18%. The potassium permanganate solution has a mass concentration of 38%. The mass ratio of pyrophyllite to potassium permanganate solution is 1:3.5; (2) Modification The sealed pyrophyllite was mixed with deionized water, and then carboxymethyl cellulose, palmitic acid, sodium stearate and fatty alcohol polyoxyethylene ether were added. The stirring time was controlled at 25 min and the stirring speed was 205 rpm. After stirring, the pyrophyllite was dried to obtain the modified pyrophyllite. The mass ratio of the sealed pyrophyllite, deionized water, carboxymethyl cellulose, palmitic acid, sodium stearate, and fatty alcohol polyoxyethylene ether is 25:100:2.6:1.6:3.3:1.8.

[0026] 4. Load The modified pyrophyllite was mixed with a solution containing Sophora flavescens extract, and then sodium citrate, sodium dodecylbenzenesulfonate, betaine and adjuvants were added. The mixture was stirred for 37 minutes at a stirring speed of 253 rpm until it was homogeneous, and then the functional liquid containing Sophora flavescens extract was obtained. The mass ratio of the modified pyrophyllite, the solution containing the extract of *Hydrangea macrophylla*, sodium citrate, sodium dodecylbenzenesulfonate, betaine, and adjuvants is 9:99:1.6:2.6:1.3:1.0. The preparation method of the additive is as follows: xanthan gum, gum arabic and gelatin are mixed, then carbon black is added, and ball milling is performed. The ball milling time is controlled at 20 min and the ball milling speed is 300 rpm. After ball milling, dimethyl silicone oil is added, mixed evenly, and heat-treated at 62°C for 20 min. After heat treatment, the mixture is lowered to room temperature to obtain the additive. The mass ratio of xanthan gum, gum arabic, gelatin, carbon black and dimethyl silicone oil is 3.0:2.6:4.4:4.8:1.7.

[0027] 5. Preparation of blend spinning solution A blended spinning solution was prepared by mixing a functional liquid containing sleep grass extract with a spinning solution, followed by filtration, degassing, and aging. The mass ratio of the functional dispersion to the spinning solution is 16:100; The spinning solution has a carbonyl content of 8.6% and a viscosity of 43s.

[0028] 6. Spinning The blended spinning solution is sprayed into a coagulation bath for spinning treatment. After the spinning is solidified, it is washed with water, oiled, and dried to obtain viscose macro-fiber containing the active ingredient of Sophora flavescens.

[0029] The coagulation bath contains the following components: sulfuric acid 96 g / L, sodium sulfate 195 g / L, and zinc sulfate 21 g / L.

[0030] Example 3 1. Pretreatment of Hypnos nux-vomica extract The extract of *Hypophthalmia ulmoides* was immersed twice in a pretreatment solution. The first immersion temperature was controlled at 18℃ and the immersion time was 33 min. After the first immersion, a second immersion was performed, with the temperature controlled at 40℃ and the immersion time being 23 min. During both immersions, ultraviolet-ultrasound treatment was performed. The center wavelength of the ultraviolet lamp was 233 nm, the power of the ultraviolet lamp was 263 W, and the ultrasonic power was 337 W. After immersion, the extract was dried to obtain the pretreated extract of *Hypophthalmia ulmoides*. The extract of the sleepwort has a particle size of 120 nm. The mass ratio of the *Hydrangea macrophylla* extract to the pretreatment solution is 1:3.5; The pretreatment solution is composed of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid, and the mass ratio of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid is 2.7:2.2:1.8:2.1:1.4.

[0031] 2. Dissolve The pretreated Sophora flavescens extract was mixed with deionized water, and then coconut oil, glucose and pentaerythritol were added. After stirring evenly, the mixture was pre-cooled at 1.2℃ for 30 minutes. After pre-cooling, the mixture was frozen at -10℃ for 25 minutes. After freezing, the mixture was allowed to return to room temperature naturally to obtain a solution containing Sophora flavescens extract. The mass ratio of the pretreated *Symplocos edulis* extract, deionized water, coconut oil acid, glucose, and pentaerythritol was 11:114:1.8:1.3:2.5.

[0032] 3. Preparation of modified pyrophyllite (1) Sealing treatment Pyrophyllite was washed in potassium permanganate solution for 2.5 hours. After washing, it was placed in a sealed container and evacuated to a vacuum of 0.09 MPa. Nitrogen gas was then introduced until the pressure reached 5.3 MPa. The temperature was raised to 125°C and maintained at that temperature and pressure for 45 minutes. After the temperature and pressure maintenance, the pressure was reduced to 3.3 MPa and the temperature was raised to 137°C and maintained at that temperature and pressure for 35 minutes. After the temperature and pressure maintenance, the pressure was immediately released and the temperature was lowered to room temperature to obtain the sealed pyrophyllite. The pyrophyllite has a particle size of 160 mesh, a SiO2 mass content of 74%, and an Al2O3 mass content of 20%. The potassium permanganate solution has a mass concentration of 42%. The mass ratio of pyrophyllite to potassium permanganate solution is 1:4.0; (2) Modification The sealed pyrophyllite was mixed with deionized water, and then carboxymethyl cellulose, palmitic acid, sodium stearate and fatty alcohol polyoxyethylene ether were added. The stirring time was controlled at 31 min and the stirring speed was 223 rpm. After stirring, the pyrophyllite was dried to obtain the modified pyrophyllite. The mass ratio of the sealed pyrophyllite, deionized water, carboxymethyl cellulose, palmitic acid, sodium stearate, and fatty alcohol polyoxyethylene ether is 30:120:3.0:2.2:3.8:2.2.

[0033] 4. Load The modified pyrophyllite was mixed with a solution containing Sophora flavescens extract, and then sodium citrate, sodium dodecylbenzenesulfonate, betaine and adjuvants were added. The mixture was stirred for 44 minutes at a stirring speed of 267 rpm until it was homogeneous, and then the functional liquid containing Sophora flavescens extract was obtained. The mass ratio of the modified pyrophyllite, the solution containing the extract of *Hydrocotyle sibthorpioides*, sodium citrate, sodium dodecylbenzenesulfonate, betaine, and adjuvants is 11:130:2.0:3.1:1.5:1.4. The preparation method of the additive is as follows: xanthan gum, gum arabic and gelatin are mixed, then carbon black is added, and ball milling is performed. The ball milling time is controlled at 27 min and the ball milling speed is 308 rpm. After ball milling, dimethyl silicone oil is added, mixed evenly, and heat-treated at 66°C for 15 min. After heat treatment, the mixture is lowered to room temperature to obtain the additive. The mass ratio of xanthan gum, gum arabic, gelatin, carbon black and dimethyl silicone oil is 3.4:2.8:4.8:5.2:1.9.

[0034] 5. Preparation of blend spinning solution A blended spinning solution was prepared by mixing a functional liquid containing sleep grass extract with a spinning solution, followed by filtration, degassing, and aging. The mass ratio of the functional dispersion to the spinning solution is 18:100; The spinning solution has a carbonyl content of 8.8% and a viscosity of 45s.

[0035] 6. Spinning The blended spinning solution is sprayed into a coagulation bath for spinning treatment. After the spinning is solidified, it is washed with water, oiled, and dried to obtain viscose macro-fiber containing the active ingredient of Sophora flavescens.

[0036] The coagulation bath contains the following components: sulfuric acid 98 g / L, sodium sulfate 17 g / L, and zinc sulfate 23 g / L.

[0037] Comparative Example 1 Based on Example 1, the change is that the dissolution step is to directly mix the untreated Sophora flavescens extract with deionized water to obtain a solution containing Sophora flavescens extract; all other operations are the same. The extract of *Hydrangea macrophylla* has a particle size of 100 nm, and the mass ratio of the pretreated extract of *Hydrangea macrophylla* to deionized water is 10:100.

[0038] Comparative Example 2 Based on Example 1, the change is that the loading step is to mix the solution containing the extract of *Hydrangea macrophylla* with untreated pyrophyllite and stir evenly to obtain a functional liquid containing the extract of *Hydrangea macrophylla*. All other operations are the same. The pyrophyllite has a particle size of 140 mesh, a SiO2 mass content of 73%, and an Al2O3 mass content of 19%; the mass ratio of the pyrophyllite to the solution containing the extract of *Hydrocotyle sepium* is 10:120.

[0039] Performance testing (1) Basic performance

[0040] (2) Placed at 600W / m 2 After 15 days of irradiation under ultraviolet light

[0041] Unless otherwise stated, all percentages used in this invention are mass percentages.

[0042] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is 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 viscose macrocellulose containing active ingredients of *Hydrangea macrophylla*, characterized in that, The preparation method includes the following steps: pretreatment of Sophora flavescens extract, dissolution, preparation of modified pyrophyllite, loading, preparation of blend spinning solution, and spinning. The pretreatment of the *Hypophthalmia ulmoides* extract involves immersing the extract in a pretreatment solution twice. The first immersion temperature is controlled at 14-18℃, and the immersion time is 27-33 min. After the first immersion, a second immersion is performed, with the temperature controlled at 35-40℃ and the immersion time being 23-29 min. Both immersions are simultaneously subjected to UV-ultrasound treatment. The center wavelength of the UV lamp is 207-233 nm, the UV lamp power is 263-285 W, and the ultrasonic power is 314-337 W. After immersion, the extract is dried to obtain the pretreated *Hypophthalmia ulmoides* extract. The pretreatment solution is composed of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid; the dissolution is carried out by mixing the pretreated sleep grass extract with deionized water, then adding coconut oil acid, glucose and pentaerythritol, stirring evenly and then pre-cooling at a temperature of 0.6-1.2℃ for 23-30 min. After pre-cooling, freezing is carried out at a temperature of -14 to -10℃ for 16-25 min. After freezing, the solution is allowed to return to room temperature naturally to obtain a solution containing sleep grass extract. The preparation of modified pyrophyllite includes a sealing treatment and a modification step; The sealing treatment involves washing pyrophyllite in a potassium permanganate solution for 2.2-2.5 hours, then placing it in a sealed container. The container is then evacuated to a vacuum level of 0.06-0.09 MPa, and nitrogen gas is introduced until the pressure reaches 5.0-5.3 MPa. The temperature is then increased to 125-128°C and maintained at that temperature and pressure for 37-45 minutes. After the temperature and pressure maintenance, the pressure is reduced to 3.3-3.9 MPa, and the temperature is further increased to 137-150°C and maintained at that temperature and pressure for 30-35 minutes. After the temperature and pressure maintenance, the pressure is immediately released and the temperature is lowered to room temperature to obtain the sealed pyrophyllite. The modification involves mixing sealed pyrophyllite with deionized water, then adding carboxymethyl cellulose, palmitic acid, sodium stearate and fatty alcohol polyoxyethylene ether, controlling the stirring time to be 25-31 min and the stirring speed to be 205-223 rpm, and drying after stirring to obtain modified pyrophyllite. The loading process involves mixing modified pyrrolizite with a solution containing *Hymenochaene salsa* extract, then adding sodium citrate, sodium dodecylbenzenesulfonate, betaine, and auxiliaries, stirring for 37-44 minutes at a stirring speed of 253-267 rpm, and finally stirring until homogeneous to obtain a functional liquid containing *Hymenochaene salsa* extract.

2. The method for preparing viscose macrocellulose containing the active ingredient of *Hydrangea macrophylla* according to claim 1, characterized in that, In the pretreatment step of the sleep herb extract, the sleep herb extract has a particle size of 80-120 nm. The mass ratio of the *Hydrangea macrophylla* extract to the pretreatment solution is 1:2.8-3.5; In the pretreatment solution, the mass ratio of gelatin, xylitol, ethylene glycol, glycerin and hyaluronic acid is 2.3-2.7:2.0-2.2:1.4-1.8:1.7-2.1:1.0-1.

4.

3. The method for preparing viscose macrocellulose containing the active ingredient of *Hydrangea macrophylla* according to claim 1, characterized in that, In the dissolution step, the mass ratio of the pretreated *Sedum morganianum* extract, deionized water, coconut oil acid, glucose, and pentaerythritol is 9-11:88-114:1.4-1.8:0.8-1.3:2.0-2.

5.

4. The method for preparing viscose macrocellulose containing the active ingredient of *Hydrangea macrophylla* according to claim 1, characterized in that, In the sealing process, the pyrophyllite has a particle size of 120-160 mesh, a SiO2 mass content of 72-74%, and an Al2O3 mass content of 18-20%. The potassium permanganate solution has a mass concentration of 38-42%. The mass ratio of pyrophyllite to potassium permanganate solution is 1:3.5-4.

0.

5. The method for preparing viscose macrocellulose containing the active ingredient of *Hydrangea macrophylla* according to claim 1, characterized in that, In the modification step, the mass ratio of the sealed pyrophyllite, deionized water, carboxymethyl cellulose, palmitic acid, sodium stearate, and fatty alcohol polyoxyethylene ether is 25-30:100-120:2.6-3.0:1.6-2.2:3.3-3.8:1.8-2.2; In the loading step, the mass ratio of the modified pyrophyllite, the solution containing the extract of *Hydrocotyle sibthorpioides*, sodium citrate, sodium dodecylbenzenesulfonate, betaine, and the adjuvant is 9-11:99-130:1.6-2.0:2.6-3.1:1.3-1.5:1.0-1.

4. The preparation method of the additive is as follows: xanthan gum, gum arabic and gelatin are mixed, then carbon black is added, and ball milling is performed. The ball milling time is controlled at 20-27 min and the ball milling speed is 300-308 rpm. After ball milling, dimethyl silicone oil is added, mixed evenly, and heat-treated at 62-66℃ for 15-20 min. After heat treatment, the mixture is cooled to room temperature to obtain the additive. The mass ratio of xanthan gum, gum arabic, gelatin, carbon black, and dimethyl silicone oil is 3.0-3.4:2.6-2.8:4.4-4.8:4.8-5.2:1.7-1.

9. The preparation of the blended spinning solution involves mixing a functional liquid containing the extract of *Symplocos edulis* with a spinning solution, followed by filtration, degassing, and aging to obtain the blended spinning solution. The mass ratio of the functional liquid containing the sleep grass extract to the spinning solution is 16-18:100; The spinning solution has a cellulose content of 8.6-8.8% and a viscosity of 43-45s.

6. The method for preparing viscose macrocellulose containing the active ingredient of *Hydrangea macrophylla* according to claim 1, characterized in that, The spinning process involves spraying the blended spinning solution into a coagulation bath for spinning treatment. After the spinning is solidified, the fibers are washed with water, oiled, and dried to obtain viscose macro-fibers containing active ingredients of *Sedum aizoon*. The coagulation bath contains the following components: sulfuric acid 96-98 g / L, sodium sulfate 195-197 g / L, and zinc sulfate 21-23 g / L.

7. Viscose biofiber containing the active ingredient of *Hydrangea macrophylla* prepared by the preparation method according to any one of claims 1-6.

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