Preparation method of viscose fiber containing active components of tree peony
By using plasma treatment and β-cyclodextrin inclusion combined with montmorillonite/modified diatomaceous earth composite carrier, the stability and uniformity of peony active ingredients in viscose fiber were solved, achieving long-lasting antioxidant, antibacterial and soothing effects of functional fiber, while avoiding environmental hazards.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- YIXIANG PERSONAL HOME CARE HEALTH RESEARCH (HENAN) CO LTD
- Filing Date
- 2026-03-31
- Publication Date
- 2026-06-02
AI Technical Summary
In existing viscose fibers, the active ingredients of peony have poor stability and are easily affected by acid and alkali environments, temperature changes and mechanical shearing. They have low binding strength, poor functional durability and poor dispersion uniformity. In addition, some modification processes pose environmental risks.
Peony flower powder was activated by plasma treatment, and peony microcapsules were formed by inclusion with β-cyclodextrin. The composite carrier was prepared by ultrasonic dispersion and spray drying to achieve stable loading of peony microcapsules. A blended spinning solution was prepared by two-stage gradient dispersion and spinning process, and finally spinning and post-treatment were carried out.
It improves the stability and uniformity of peony active ingredients, ensures stability and functional durability during the spinning process, achieves long-lasting effects of anti-oxidation, antibacterial and soothing, and avoids the environmental hazards of chemical reagents.
Smart Images
Figure CN122128818A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical fiber processing technology, and specifically to a method for preparing viscose fiber containing peony active ingredients. Background Technology
[0002] Viscose fiber, as an important category of regenerated cellulose fiber, is widely used in clothing, home textiles, and medical and health fields due to its excellent moisture absorption, breathability, softness, and biocompatibility. With increasing consumer health awareness, viscose fiber that combines functionality and safety has become a hot topic in the industry. Among them, viscose fiber modified with natural plant active ingredients has attracted much attention due to its advantages such as no chemical irritation and gentle properties.
[0003] However, existing plant-based active ingredient modified viscose fibers still face several technical bottlenecks: First, the active ingredients have poor stability. Peony active ingredients are easily affected by acid and alkali environments, temperature changes, and mechanical shearing during spinning, leading to degradation or deactivation and insufficient fiber functionality. Second, the binding strength is low. Traditional physical mixing or simple impregnation methods cause the active ingredients to adhere only to the fiber surface or shallow layer, making them easily lost during washing and use, resulting in poor functional durability. Third, the dispersion uniformity is poor. Peony active ingredients tend to agglomerate in viscose spinning solutions, leading to uneven fiber performance and potentially affecting fiber mechanical properties. Fourth, some modification processes use chemical grafting agents or heavy metal antibacterial agents, posing environmental hazards and skin irritation risks, which are inconsistent with the trend of green and healthy development.
[0004] Among the existing related patent technologies, patent publication number CN113463384A discloses a method for preparing peony flower fiber, which uses a spraying method to load peony flower extract onto the surface of cationic viscose fiber. The advantages are that the preparation does not involve strong acids or alkalis, high temperatures, or degradation of active ingredients. Spraying after opening improves the uniformity of extract adhesion. The continuous chain network process can be mass-produced and reduces the fiber defect rate. However, the extract is only physically adsorbed onto the fiber surface, which is easy to lose and has poor functional durability. At the same time, the process is only suitable for cationic viscose fiber and has poor adaptability to conventional viscose fiber, limiting its application scenarios. Invention patent CN114808174B discloses a viscose fiber containing orange and tea active ingredients and its preparation method. It achieves synergistic loading of orange and tea active ingredients by using plasma pretreatment of raw materials, supercritical CO2 modified carrier, and β-cyclodextrin coating, which improves the stability of components and the mechanical properties of fibers. It also optimizes component dispersibility and reduces fiber defects by premixing current treatment and adding reinforcing agents. However, this technology requires high pressure and precise temperature control for carrier pretreatment, has high equipment costs, a complicated preparation process, and strict requirements for proportioning, making mass production difficult.
[0005] Therefore, developing a simple, widely adaptable method for preparing functional viscose fibers that can achieve stable loading and long-lasting effects of peony active ingredients, and applying it to products such as dry wipes, disposable underwear, diapers, and diaper pads, has significant practical application value and market prospects. Summary of the Invention
[0006] The purpose of this invention is to provide a method for preparing viscose fiber containing peony active ingredients, so as to solve the problems mentioned in the background art.
[0007] To achieve the above objectives, the present invention provides the following technical solution: A method for preparing viscose fiber containing peony active ingredients includes the following steps: S100. Add the concentrated active peony extract dropwise to the β-cyclodextrin solution for inclusion. After inclusion, filter and wash the precipitate, and then freeze-dry to obtain peony microcapsule powder. S200. Montmorillonite and modified diatomaceous earth are mixed at a mass ratio of 2:1 to 3:1 to obtain a composite mixture. Deionized water is added at a solid-liquid ratio of 1:15 g / mL. The mixture is ultrasonically dispersed for 1 to 1.5 h at a power of 300 to 400 W and a frequency of 20 kHz. Then, 5 to 8% (by mass) of polyethylene glycol 6000 is added to the composite mixture and stirred until homogeneous. The mixture is then spray-dried at an inlet air temperature of 160 to 180 °C, an outlet air temperature of 80 to 90 °C, and a feed rate of 5 to 8 mL / min to obtain a composite carrier with a particle size of 0.5 to 3 μm. The carrier is then sealed and stored in a desiccator. S300: Mix the viscose solution, peony microcapsule powder and composite carrier, disperse in a two-stage gradient, filter, degas and mature to obtain a blended spinning solution. S400. The blended spinning solution is extruded into the coagulation bath through a spinneret for spinning. The nascent filament is drawn, plasticized and shaped and then cut to obtain short fibers. The short fibers are then treated in sequence by a desulfurization bath, water washing and oil bath, and then dried to constant weight to obtain viscose fibers containing peony active ingredients. The preparation methods for modified diatomaceous earth include: S210. The diatomaceous earth is crushed, sieved, calcined, and cooled to room temperature in sequence. It is then soaked in hydrochloric acid solution and washed with deionized water until neutral. S220. After washing, the diatomaceous earth is dried, mixed with a silane coupling agent, ultrasonically dispersed, and then dried to obtain modified diatomaceous earth.
[0008] Preferably, in step S100, the preparation of the peony active concentrate includes: S110. Rinse fresh peony petals with deionized water, dry them at 60~70℃, pulverize them and pass them through a 100~200 mesh sieve to obtain peony flower powder; treat the peony flower powder with plasma, using nitrogen as the working gas, controlling the power at 300~400 W for 15~20 min, to activate the active sites on the surface of the peony flower powder, and obtain pretreated peony flower powder. S120. Add the pretreated peony flower powder to a 50-60% ethanol solution at a solid-liquid ratio of 1:20~1:30 g / mL. Extract the solution by ultrasonication at 50-55℃, 400-500 W, and 20-25 kHz for 2-3 h. Collect the filtrate by filtration through a 300-mesh filter. At the same time, extract the residue a second time under the same conditions. Combine the two filtrates and distill them under reduced pressure to 1 / 5 of the original volume to obtain the concentrated peony active liquid.
[0009] Preferably, in step S100, the inclusion is as follows: Add β-cyclodextrin to deionized water and stir to dissolve at 60-70℃ to prepare a β-cyclodextrin aqueous solution with a mass concentration of 5-8%. Add peony active concentrated solution dropwise to the β-cyclodextrin aqueous solution at a rate of 1-2 mL / min, keep the temperature at 60-70℃ and stir for 1.5-2 h, then cool to room temperature and refrigerate at 2-4℃ for 4-6 h. The mass ratio of β-cyclodextrin to peony active concentrate is 3:1 to 5:1.
[0010] Preferably, in step S100, after the inclusion is completed and filtered, the precipitate is washed 2-3 times with anhydrous ethanol, and then the precipitate is freeze-dried under vacuum at -20 to -15°C and 300 to 350 Pa for 24 to 30 hours to obtain peony microcapsule powder.
[0011] Preferably, the preparation of modified diatomaceous earth specifically includes: The diatomaceous earth was crushed and passed through a 200-mesh sieve, calcined at 500-550℃ for 2-3 hours, cooled to room temperature, and then soaked in 10-15% hydrochloric acid solution at a solid-liquid ratio of 1:10g / mL for 4-6 hours. Wash the solution by centrifugation with deionized water at 3000-4000 rpm for 5-10 min until the pH of the washing solution is 6.5-7.0. After drying, mix with 3-5% silane coupling agent at a solid-liquid ratio of 1:8 g / mL. Disperse the mixture by ultrasonication at 300-400 W power and 20 kHz frequency for 30-40 min. Dry at 80-85℃ to obtain the final product.
[0012] The preferred silane coupling agent is KH-570.
[0013] Preferably, in step S300, the viscose stock solution is prepared using a conventional viscose preparation process, with the cellulose content controlled at 9.0~9.5% and the total alkali content at 2.8~6.0%, and after filtration, it is placed at a constant temperature of 25~30℃ for 12~16 h.
[0014] Preferably, in step S300, the ratio of viscose stock solution: peony microcapsule powder: composite carrier by mass is 100:(1~3):(0.5~1.5).
[0015] Preferably, in step S300, the two-stage gradient dispersion is as follows: initial dispersion at 20~60℃, stirring at 100~150 rpm for 10 min, followed by stirring at 300~400 rpm for 30~40 min.
[0016] Preferably, in step S300, after degassing at a vacuum of -0.08 to -0.09 MPa and maturing at 20 to 38°C for 0.5 to 30 hours, a blended spinning solution is obtained.
[0017] Preferably, in step S400, the coagulation bath includes 95~130 g / L sulfuric acid, 280~360 g / L sodium sulfate, and 8.5~18.5 g / L zinc sulfate. The spinning temperature is controlled at 20~45℃, the spinning speed at 10~85 m / min, the immersion length at 0.5~1.0 m, and the nascent filament bundle is drawn at 0.35~2.0 times.
[0018] Preferably, in step S400, the short fibers are sequentially subjected to a desulfurization bath of 3~10 g / L sulfide, water washing, and oil bath treatment of 8~15 g / L, and then dried at 100~105℃ to constant weight.
[0019] Preferably, in step S110, the peony petals are crushed and passed through a 100-120 mesh sieve; in step S120, after ultrasonic extraction, they are filtered through a 300 mesh sieve; in step S300, after two-stage dispersion, they are filtered through a 5-15 μm metal filter.
[0020] The beneficial effects of the above-described technical solution of the present invention are as follows: (1) This invention uses plasma treatment. High-energy plasma particles bombard the powder surface, which can not only construct a rough porous structure through micro-nano-level physical etching and greatly increase the specific surface area of the powder, but also break the covalent bonds of the surface matrix molecules and generate hydrophilic active functional groups such as hydroxyl and carboxyl groups in situ. Combined with the nitrogen inert atmosphere to isolate oxygen, it can effectively avoid the oxidation and degradation of active sites of powder and active ingredients of peony, accurately activate surface active sites, and greatly improve the dissolution efficiency and extraction yield of active ingredients in subsequent extraction processes.
[0021] (2) This invention utilizes the unique hollow cylindrical structure of β-cyclodextrin, which is "hydrophilic on the outside and hydrophobic on the inside". Based on the principle of "like dissolves like", hydrophobic / weakly hydrophilic active ingredients such as peony flavonoids, phenolic acids, and paeonol are encapsulated in its hydrophobic cavity to form stable peony microcapsules. This constructs a core-shell protective structure, which completely isolates external adverse factors such as acid and alkali environment, temperature fluctuations, and mechanical shearing during the spinning process, prevents the degradation and inactivation of active ingredients, and achieves efficient retention of active substances.
[0022] (3) This invention utilizes the layered porous structure of the montmorillonite / modified diatomite composite carrier to provide sufficient adsorption sites, and with the chemical bridging effect of the silane coupling agent, achieves a strong chemical bond and uniform physical loading between the peony microcapsules and the composite carrier. Relying on the structural complementarity of the two carriers and the dispersing synergistic effect of polyethylene glycol, it ensures that the composite carrier loaded with microcapsules is uniformly dispersed in the viscose spinning solution, completely inhibits agglomeration and clumping, and ensures the stability of the spinning process.
[0023] (4) After the fiber prepared by this invention is put into use, the microcapsule controlled release system drives the slow and sustained release of peony active ingredients. Flavonoids and phenolic acid components can remove free radicals to exert antioxidant effects and destroy bacterial cell membranes to achieve antibacterial effects. Paeonol can inhibit the release of inflammatory mediators and soothe skin sensitivity and discomfort. The synergistic effect of multiple active ingredients can achieve long-lasting and gentle effects of antioxidant, antibacterial and soothing effects, which is the key manifestation of the core function value of this functional viscose fiber. Attached Figure Description
[0024] Figure 1 This is a schematic flowchart of the viscose fiber preparation method of the present invention; Figure 2 This is a schematic diagram of the viscose fiber containing peony microcapsules of the present invention; Figure 3 This is a schematic diagram of the wet spinning process of the present invention. Detailed Implementation
[0025] The following embodiments are provided to better understand the present invention and are not limited to the preferred embodiments described. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention.
[0026] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products. Example 1
[0027] A method for preparing viscose fiber containing peony active ingredients, such as... Figure 1 The flowchart shows the following steps: Step 1: Extraction and Modification of Active Ingredients from Peony (1) Raw material pretreatment: Select fresh peony petals, rinse them with deionized water, dry them in a vacuum drying oven at 65℃ to constant weight, grind them through a 120-mesh sieve to obtain peony flower powder; place the powder in a plasma treatment instrument, use nitrogen as the working gas, control the treatment power at 400 W and the time at 15 min, and activate the active sites on the powder surface.
[0028] (2) Extraction: The pretreated peony flower powder was added to a 50% ethanol solution at a solid-liquid ratio of 1:30 g / mL. The mixture was ultrasonically extracted for 3 h at 55℃, ultrasonic power of 400 W and frequency of 25 kHz. The filtrate was collected by filtering through a 300-mesh filter cloth. The residue was extracted twice under the same conditions. The two filtrates were combined and concentrated by vacuum distillation to 1 / 5 of the original volume to obtain peony active concentrate.
[0029] (3) Microcapsule preparation: β-cyclodextrin was added to deionized water and heated to 65°C with stirring to dissolve, preparing a 7% β-cyclodextrin solution. The concentrate was added dropwise to the β-cyclodextrin solution at a rate of 1 mL / min according to a β-cyclodextrin to peony active concentrate mass ratio of 4:1. The solution was stirred at 65°C for 1.5 h, cooled to room temperature, and then refrigerated at 4°C for 6 h. After filtration, the precipitate was washed three times with anhydrous ethanol. The precipitate was then freeze-dried under vacuum at -20°C and 300 Pa for 26 h to obtain peony microcapsule powder (structure as shown in the figure). Figure 2 (as described).
[0030] Step 2: Preparation of the composite carrier (1) Preparation of modified diatomaceous earth: The diatomaceous earth was crushed and passed through a 200-mesh sieve, placed in a calcining furnace at 550℃ for 2 h, cooled to room temperature, and then soaked in 15% hydrochloric acid solution at a solid-liquid ratio of 1:10 g / mL for 4 h. It was then washed with deionized water at a speed of 3000 rpm until the pH of the washing solution was 6.5~7.0. After drying, it was mixed with 5% silane coupling agent KH-570 solution at a solid-liquid ratio of 1:8 g / mL, ultrasonically dispersed for 30 min at a power of 400 W and a frequency of 20 kHz, and dried in an oven at 80℃ to obtain modified diatomaceous earth.
[0031] (2) Preparation of composite carrier: Montmorillonite and modified diatomite were mixed at a mass ratio of 2.5:1 to obtain a composite mixture. The mixture was added to deionized water at a solid-liquid ratio of 1:15 g / mL and ultrasonically dispersed for 1 h at a power of 400 W and a frequency of 20 kHz. Then, polyethylene glycol 6000, accounting for 7% of the mass of the composite mixture, was added and stirred evenly. Spray drying was carried out at an inlet air temperature of 180℃, an outlet air temperature of 90℃, and a feed rate of 6 mL / min to obtain a composite carrier with a particle size of 0.5~3 μm. The carrier was then sealed and stored in a desiccator.
[0032] Step 3: Preparation of Blend Spinning Solution (1) Pretreatment of viscose stock solution: Viscose stock solution was prepared by conventional viscose preparation process, with the cellulose content controlled at 9.0% and the total alkali content at 4%. After filtration, it was placed in a constant temperature environment of 25~30℃ for 12~16 h to mature.
[0033] (2) Blending: 2% of the viscose stock solution was added to peony microcapsule powder and 1% to composite carrier. The mixture was initially dispersed at 130 rpm for 10 min under 40℃ conditions, and then stirred at 300 rpm for 35 min. The mixture was filtered through a 10 μm metal filter and degassed under a vacuum of -0.08 MPa. After maturing at 30℃ for 20 h, the blended spinning solution was obtained.
[0034] Step 4: Spinning and Post-processing (1) Spinning: such as Figure 3 As shown, the blended spinning solution was extruded into a coagulation bath through a spinneret. The coagulation bath consisted of 110 g / L sulfuric acid, 320 g / L sodium sulfate, and 13 g / L zinc sulfate. The spinning temperature was controlled at 30℃, the spinning speed at 45 m / min, and the immersion length at 1 m. The nascent filament bundle was cut after being stretched once and plasticized to obtain short fibers.
[0035] (2) Post-treatment: The short fibers were successively subjected to a desulfurization bath with 6 g / L sulfide, water washing, and oil bath treatment with an oil concentration of 12 g / L. Then, they were dried in an oven at 100℃ to constant weight, and finally viscose fiber containing peony active ingredients was obtained. Figure 2 ). Example 2
[0036] A method for preparing viscose fiber containing peony active ingredients includes the following steps: Step 1: Extraction and Modification of Active Ingredients from Peony (1) Raw material pretreatment: Select fresh peony petals, rinse them with deionized water, dry them in a vacuum drying oven at 65℃ to constant weight, grind them through a 120-mesh sieve to obtain peony flower powder; place the powder in a plasma treatment instrument, use nitrogen as the working gas, control the treatment power at 400 W and the time at 15 min, and activate the active sites on the powder surface.
[0037] (2) Extraction: The pretreated peony flower powder was added to a 60% ethanol solution at a solid-liquid ratio of 1:20 g / mL. The mixture was ultrasonically extracted for 2 h at 55℃, ultrasonic power of 500 W and frequency of 25 kHz. The filtrate was collected by filtering through a 300-mesh filter cloth. The residue was extracted twice under the same conditions. The two filtrates were combined and concentrated by vacuum distillation to 1 / 5 of the original volume to obtain peony active concentrate.
[0038] (3) Microcapsule preparation: β-cyclodextrin was added to deionized water, heated to 70°C and stirred to dissolve, and a 5% β-cyclodextrin solution was prepared. The concentrate was added dropwise to the β-cyclodextrin solution at a rate of 1 mL / min according to the mass ratio of β-cyclodextrin to peony active concentrate of 3:1. The solution was stirred at 70°C for 1.5 h, cooled to room temperature, and then refrigerated at 4°C for 6 h. After filtration, the precipitate was washed three times with anhydrous ethanol. The precipitate was then freeze-dried under vacuum at -20°C and 300 Pa for 26 h to obtain peony microcapsule powder.
[0039] Step 2: Preparation of the composite carrier (1) Preparation of modified diatomaceous earth: The diatomaceous earth was crushed and passed through a 200-mesh sieve, placed in a calcining furnace at 500℃ for 3 h, cooled to room temperature, and then soaked in 10% hydrochloric acid solution at a solid-liquid ratio of 1:10 g / mL for 6 h. It was then washed with deionized water at a speed of 4000 rpm until the pH of the washing solution was 6.5~7.0. After drying, it was mixed with 3% silane coupling agent KH-570 solution at a solid-liquid ratio of 1:8 g / mL, ultrasonically dispersed for 30 min at a power of 400 W and a frequency of 20 kHz, and dried in an oven at 80℃ to obtain modified diatomaceous earth.
[0040] (2) Preparation of composite carrier: Montmorillonite and modified diatomite were mixed at a mass ratio of 2:1 to obtain a composite mixture. The mixture was added to deionized water at a solid-liquid ratio of 1:15 g / mL and ultrasonically dispersed for 1 h at a power of 400 W and a frequency of 20 kHz. Then, polyethylene glycol 6000, accounting for 5% of the mass of the composite mixture, was added and stirred evenly. Spray drying was carried out at an inlet air temperature of 180℃, an outlet air temperature of 90℃, and a feed rate of 6 mL / min to obtain a composite carrier with a particle size of 0.5~3 μm. The carrier was then sealed and stored in a desiccator.
[0041] Step 3: Preparation of Blend Spinning Solution (1) Pretreatment of viscose stock solution: Viscose stock solution was prepared by conventional viscose preparation process, with the cellulose content controlled at 9.5% and the total alkali content at 6%. After filtration, it was placed in a constant temperature environment of 25~30℃ for 12~16 h to mature.
[0042] (2) Blending: 3% of the viscose stock solution mass of peony microcapsule powder and 1.5% of composite carrier were added. The mixture was initially dispersed at 150 rpm for 10 min under 60℃ conditions, and then stirred at 400 rpm for 30 min. The mixture was filtered through a 15μm metal filter and degassed under a vacuum of -0.08 MPa. After maturing at 38℃ for 8 h, the blended spinning solution was obtained.
[0043] Step 4: Spinning and Post-processing (1) Spinning: The blended spinning solution is extruded into the coagulation bath through the spinneret. The coagulation bath consists of 130 g / L sulfuric acid, 360 g / L sodium sulfate, and 18 g / L zinc sulfate. The spinning temperature is controlled at 45℃, the spinning speed is 80 m / min, and the immersion length is 0.7 m. The nascent filament bundle is cut after being stretched by 0.35 times and plasticized and shaped to obtain short fibers.
[0044] (2) Post-treatment: The short fibers are successively subjected to a desulfurization bath of 10 g / L sulfide, water washing, and oil bath treatment of 15 g / L oil agent concentration, and then dried in an oven at 100℃ to constant weight, finally obtaining viscose fiber containing peony active ingredients. Example 3
[0045] A method for preparing viscose fiber containing peony active ingredients includes the following steps: Step 1: Extraction and Modification of Active Ingredients from Peony (1) Raw material pretreatment: Select fresh peony petals, rinse them with deionized water, dry them in a vacuum drying oven at 65℃ to constant weight, grind them through a 120-mesh sieve to obtain peony flower powder; place the powder in a plasma treatment instrument, use nitrogen as the working gas, control the treatment power at 400 W and the time at 15 min, and activate the active sites on the powder surface.
[0046] (2) Extraction: The pretreated peony flower powder was added to a 50% ethanol solution at a solid-liquid ratio of 1:25 g / mL. The mixture was ultrasonically extracted for 2 h at 55℃, ultrasonic power of 400 W and frequency of 25 kHz. The filtrate was collected by filtering through a 300-mesh filter cloth. The residue was extracted twice under the same conditions. The two filtrates were combined and concentrated by vacuum distillation to 1 / 5 of the original volume to obtain peony active concentrate.
[0047] (3) Microcapsule preparation: β-cyclodextrin was added to deionized water, heated to 60°C and stirred to dissolve, and a β-cyclodextrin solution with a mass concentration of 8% was prepared. The concentrate was added dropwise to the β-cyclodextrin solution at a mass ratio of 5:1 (β-cyclodextrin to peony active concentrate) at a rate of 2 mL / min. The solution was stirred at 60°C for 2 h, cooled to room temperature, and then refrigerated at 4°C for 6 h. After filtration, the precipitate was washed three times with anhydrous ethanol. The precipitate was then freeze-dried under vacuum at -20°C and a vacuum degree of 300 Pa for 26 h to obtain peony microcapsule powder.
[0048] Step 2: Preparation of the composite carrier (1) Preparation of modified diatomaceous earth: The diatomaceous earth was crushed and passed through a 200-mesh sieve, placed in a calcining furnace at 550℃ for 2 h, cooled to room temperature, and then soaked in 12% hydrochloric acid solution at a solid-liquid ratio of 1:10 g / mL for 6 h. It was then washed with deionized water at a speed of 3000 rpm until the pH of the washing solution was 6.5~7.0. After drying, it was mixed with 4% silane coupling agent KH-570 solution at a solid-liquid ratio of 1:8 g / mL, ultrasonically dispersed for 30 min at a power of 400 W and a frequency of 20 kHz, and dried in an oven at 80℃ to obtain modified diatomaceous earth.
[0049] (2) Preparation of composite carrier: Montmorillonite and modified diatomite were mixed at a mass ratio of 3:1 to obtain a composite mixture. The mixture was added to deionized water at a solid-liquid ratio of 1:15 g / mL and ultrasonically dispersed for 1 h at a power of 400 W and a frequency of 20 kHz. Then, polyethylene glycol 6000, accounting for 8% of the mass of the composite mixture, was added and stirred evenly. Spray drying was carried out at an inlet air temperature of 180℃, an outlet air temperature of 90℃, and a feed rate of 6 mL / min to obtain a composite carrier with a particle size of 0.5~3 μm. The carrier was then sealed and stored in a desiccator.
[0050] Step 3: Preparation of Blend Spinning Solution (1) Pretreatment of viscose stock solution: Viscose stock solution was prepared by conventional viscose preparation process, with the cellulose content controlled at 9.0% and the total alkali content at 4%. After filtration, it was placed in a constant temperature environment of 25~30℃ for 12~16 h to mature.
[0051] (2) Blending: 1% of the viscose stock solution mass of peony microcapsule powder and 0.5% of the composite carrier were added. The mixture was initially dispersed at 100 rpm for 10 min under 20℃ conditions, and then stirred at 350 rpm for 40 min. The mixture was filtered through a 5 μm metal filter and degassed under a vacuum of -0.08 MPa. After maturing at 20℃ for 30 h, the blended spinning solution was obtained.
[0052] Step 4: Spinning and Post-processing (1) Spinning: The blended spinning solution is extruded into the coagulation bath through the spinneret. The coagulation bath consists of 95 g / L sulfuric acid, 280 g / L sodium sulfate, and 8.5 g / L zinc sulfate. The spinning temperature is controlled at 20℃, the spinning speed at 15 m / min, and the immersion length at 0.5 m. The nascent filament bundle is cut after being stretched twice and plasticized to obtain short fibers.
[0053] (2) Post-treatment: The short fibers are successively subjected to a desulfurization bath with 3 g / L sulfide, water washing, and oil bath treatment with an oil concentration of 8 g / L. They are then dried in an oven at 100℃ to constant weight, and finally viscose fibers containing peony active ingredients are obtained. Comparative Example 1
[0054] The difference between this and Example 1 is that in step one, plasma treatment of peony flower powder is not used; instead, peony active concentrate is extracted directly from sieved peony flower powder. Comparative Example 2
[0055] The difference between this and Example 1 is that in step one, β-cyclodextrin is not used to encapsulate the peony active concentrate. Instead, the filtrate from the two combined extractions in (2) is dried under reduced pressure to obtain peony active powder, and this peony active powder is used to replace the peony microcapsule powder added in the blending in step three (2). Comparative Example 3
[0056] The difference between this and Example 1 is that in step two, the diatomaceous earth is not modified, and conventional diatomaceous earth is used instead of modified diatomaceous earth when preparing the composite carrier. Comparative Example 4
[0057] The difference between this and Example 1 is that no composite carrier is prepared, and in step (2) of the third step, the viscose solution and peony microcapsule powder are directly dispersed and mixed. Comparative Example 5
[0058] The difference between it and Example 1 is that in step (2) of the third step, the two-stage gradient dispersion is not used, but only a single dispersion is carried out by stirring at 350 rpm for 50 min.
[0059] The viscose fibers obtained in Examples 1-3 and Comparative Examples 1-5 were tested for their properties, and the results are shown in the table below: Referring to GB / T 45178-2024 "Determination of Antioxidant Activity of Chemical Fibers by DPPH and ABTS Methods", the ABTS method was used to test the free radical scavenging rate, reflecting the antioxidant performance of the fiber. After 50 standard washes, the antioxidant performance degradation rate of the fiber was obtained by calculating the ratio of the difference in free radical scavenging rate before and after washing to the free radical scavenging rate before washing.
[0060] Referring to GB / T 14337-2022 "Test Method for Tensile Properties of Chemical Fibers (Short Fibers)," the dry breaking strength, wet breaking strength, and elongation at break of the fibers were tested.
[0061] Free radical scavenging rate % Dry fracture strength cN / dtex Wet fracture strength cN / dtex Elongation at break % Antioxidant performance degradation rate % Example 1 77.5 3.12 1.78 20.5 6.8 Example 2 76.3 3.05 1.72 19.8 7.3 Example 3 75.6 2.98 1.65 18.7 7.9 Comparative Example 1 65.2 3.08 1.75 20.2 8.5 Comparative Example 2 60.4 3.01 1.68 19.5 18.2 Comparative Example 3 70.8 2.76 1.52 17.3 9.4 Comparative Example 4 68.4 2.63 1.45 16.8 10.7 Comparative Example 5 71.2 2.81 1.55 17.6 8.8 Test results show that: Antioxidant performance: The free radical scavenging rates of Examples 1-3 were all above 75%, significantly higher than those of Comparative Examples 1-5, indicating that the synergistic effect of plasma pretreatment, β-cyclodextrin inclusion, and composite carrier loading of the present invention can effectively retain the antioxidant function of peony active ingredients; Comparative Example 1 did not undergo plasma treatment, resulting in a lower extraction yield of active ingredients and a lower free radical scavenging rate; Comparative Example 2 did not use β-cyclodextrin inclusion, and the active ingredients were partially degraded during spinning, resulting in a significant decrease in both antioxidant performance and durability.
[0062] Mechanical properties: The dry breaking strength of Examples 1-3 is above 2.98 cN / dtex, the wet breaking strength is above 1.65 cN / dtex, and the elongation at break is above 18.7%, indicating stable mechanical properties. Comparative Examples 3 and 4 have poor or missing carrier performance, resulting in loose internal fiber structure and significantly reduced mechanical properties. Comparative Example 5 also has reduced mechanical properties due to improper dispersion method, which caused the active ingredients and carrier to agglomerate.
[0063] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Any other modifications or equivalent substitutions made by those skilled in the art to the technical solutions of the present invention, as long as they do not depart from the spirit and scope of the technical solutions of the present invention, should be covered within the scope of the claims of the present invention.
Claims
1. A method for preparing viscose fiber containing peony active ingredients, characterized in that, Includes the following steps: S100. Add the concentrated active peony extract dropwise to the β-cyclodextrin solution for inclusion. After inclusion, filter and wash the precipitate, and then freeze-dry to obtain peony microcapsule powder. S200. Montmorillonite and modified diatomaceous earth are mixed at a mass ratio of 2:1 to 3:1 to obtain a composite mixture. Then, deionized water is added at a solid-liquid ratio of 1:15 g / mL. The mixture is ultrasonically dispersed, and 5-8% of polyethylene glycol 6000 by mass of the composite mixture is added. The mixture is stirred evenly and spray-dried to obtain a composite carrier with a particle size of 0.5-3 μm. S300: Mix the viscose solution, peony microcapsule powder and composite carrier, disperse in a two-stage gradient, filter, degas and mature to obtain a blended spinning solution. S400. The blended spinning solution is extruded into the coagulation bath through a spinneret for spinning. The nascent filament is drawn, plasticized and shaped and then cut to obtain short fibers. The short fibers are then treated in sequence by a desulfurization bath, water washing and oil bath, and then dried to constant weight to obtain viscose fibers containing peony active ingredients. The preparation methods for modified diatomaceous earth include: S210. Pulverize, sieve, calcine, and cool to room temperature in sequence. Then soak in hydrochloric acid solution. After soaking, wash with deionized water until neutral. S220. After washing, the diatomaceous earth is dried, mixed with a silane coupling agent, ultrasonically dispersed, and then dried to obtain modified diatomaceous earth.
2. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, In step S100, the preparation of the peony active concentrate includes: S110. Fresh peony petals are washed, dried, crushed and sieved in sequence to obtain peony flower powder; plasma treatment is used to activate the active sites on the surface of the peony flower powder to obtain pretreated peony flower powder. S120. Add the pretreated peony flower powder to a 50-60% ethanol solution at a solid-liquid ratio of 1:20~1:30 g / mL, extract by ultrasonication, filter, extract the residue a second time under the same conditions and filter, combine the two filtrates, and distill under reduced pressure to 1 / 5 of the original volume to obtain the peony active concentrate.
3. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, In step S100, the inclusion is as follows: Add β-cyclodextrin to deionized water and stir to dissolve at 60-70℃ to prepare a β-cyclodextrin aqueous solution with a mass concentration of 5-8%. Add peony active concentrated solution dropwise to the β-cyclodextrin aqueous solution at a rate of 1-2 mL / min, keep the temperature constant at 60-70℃ and stir, then cool to room temperature and refrigerate and stand. The mass ratio of β-cyclodextrin to peony active concentrate is 3:1 to 5:
1.
4. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, The preparation of modified diatomaceous earth specifically includes: The diatomaceous earth was crushed and passed through a 200-mesh sieve, calcined at 500-550℃ for 2-3 hours, cooled to room temperature, and then soaked in 10-15% hydrochloric acid solution at a solid-liquid ratio of 1:10 g / mL for 4-6 hours. Wash with deionized water by centrifugation until the pH of the washing solution is 6.5-7.
0. After drying, mix with 3-5% silane coupling agent at a solid-liquid ratio of 1:8 g / mL, disperse by ultrasonication, and then dry to obtain the final product.
5. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, In step S300, the viscose raw solution has a cellulose content of 9.0-9.5% and a total alkali content of 2.8-6.0%, and is cured at a constant temperature after filtration.
6. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, In step S300, the mass ratio of viscose stock solution: peony microcapsule powder: composite carrier is 100:(1~3):(0.5~1.5).
7. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, In step S300, the two-stage gradient dispersion is as follows: under conditions of 20~60℃, stir at 100~150 rpm for 10 min for initial dispersion, and then stir at 300~400 rpm for 30~40 min.
8. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, In step S400, the coagulation bath includes 95~130 g / L sulfuric acid, 280~360 g / L sodium sulfate, and 8.5~18.5 g / L zinc sulfate. The spinning temperature is controlled at 20~45℃, the spinning speed at 10~85 m / min, the immersion length at 0.5~1.0 m, and the nascent filament bundle is drawn at 0.35~2.0 times.
9. The method for preparing viscose fiber containing peony active ingredients according to claim 1, characterized in that, In step S400, the short fibers are successively subjected to a desulfurization bath of 3~10 g / L sulfide, water washing, and oil bath treatment of 8~15 g / L, and then dried at 100~105℃ to constant weight.
10. The method for preparing viscose fiber containing peony active ingredients according to claim 2, characterized in that, In step S110, the peony petals are crushed and passed through a 100-120 mesh sieve; in step S120, after ultrasonic extraction, they are filtered through a 300 mesh sieve; in step S300, after two-stage dispersion, they are filtered through a 5-15 μm metal filter.