Hydrogel mask fiber base cloth containing centella asiatica component and preparation method of hydrogel mask fiber base cloth

Abstract

The invention discloses hydrogel mask fiber base cloth containing centella asiatica and a preparation method of the hydrogel mask fiber base cloth, relates to the technical field of functional fiber base cloth, and belongs to the patent publication number D06M15 / 13. The method comprises the following steps: firstly, encapsulating a centella asiatica extract in a microcapsule, blending the centella asiatica extract with sodium alginate and the like to prepare a spinning solution, carrying out wet spinning to obtain calcium alginate-zinc nascent fibers, then carrying out plasma treatment on the fibers, and sequentially carrying out silane coupling agent treatment, clathrate grafting and carboxymethyl hyaluronic acid / chitosan composite modification to obtain the calcium alginate-zinc composite fiber. And finally, carding, spunlace and hot-rolling shaping are performed to obtain the mask base cloth. The fiber base cloth prepared by the method has good moisturizing performance, and has relatively high loading capacity on active ingredients of centella asiatica.

Description

Technical Field

[0001] This invention relates to the field of functional fiber base fabric technology, belonging to patent publication number D06M15 / 13, specifically to a hydrogel mask fiber base fabric containing Centella asiatica and its preparation method. Background Technology

[0002] In today's rapidly developing beauty and skincare industry, consumers have higher demands for the efficacy, safety, and user experience of skincare products. As a highly efficient and intensive skincare product, the performance of the mask base fabric, the core carrier of a face mask, directly determines the carrying efficiency of skincare essence, skin absorption, and overall user experience. The mask base fabric not only needs excellent essence-carrying capacity but also needs to consider moisturizing and water-locking properties, skin compatibility, and the stable release of active ingredients, becoming a crucial bridge connecting skincare ingredients and the skin. Among these, hydrogel mask base fabrics, with their unique three-dimensional network structure, have a much higher liquid absorption rate than traditional non-woven fabrics. They can efficiently carry large amounts of water-soluble essences and active ingredients, while their soft texture and good skin-adhesion allow them to closely conform to the skin's texture, reducing essence loss and promoting the penetration and absorption of effective ingredients. Therefore, they have become one of the research hotspots and mainstream products in the mask base fabric field in recent years.

[0003] Alginate fiber, a polysaccharide fiber extracted from natural seaweed, is a preferred raw material for preparing hydrogel mask base fabrics due to its green and environmentally friendly origin, excellent biocompatibility, and abundant hydrophilic groups in its molecular chain, resulting in outstanding hygroscopicity. However, single alginate fiber base fabrics still face several technical bottlenecks in practical applications: Firstly, its moisturizing performance suffers from the problem of absorbing a lot of moisture but not locking it in. Although it can quickly absorb water and essence, the lack of a stable water-locking mechanism in its molecular structure leads to rapid water evaporation, resulting in insufficient moisturizing duration and difficulty in meeting the skin's long-term hydration needs. Secondly, the stability of active ingredient loading is poor. The adsorption of alginate fiber is mostly physical, lacking specific binding sites, resulting in a low loading of added active ingredients. Summary of the Invention

[0004] The purpose of this invention is to provide a hydrogel mask fiber base fabric containing Centella asiatica and its preparation method, so as to solve the technical problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution:

[0006] A method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract includes the following steps:

[0007] S1. Weigh gelatin and gum arabic and dissolve them in deionized water. Heat and stir until dissolved. Add centella asiatica extract and stir to emulsify. Add sodium sulfate solution and cool down. Add formaldehyde solution to crosslink and solidify. Centrifuge, wash and dry to obtain centella asiatica extract microcapsules.

[0008] S2. Weigh out sodium alginate and dissolve it in deionized water to obtain sodium alginate aqueous solution. Add Centella asiatica extract microcapsules and polyethylene glycol, continue to stir at high speed and let stand to degas, and obtain spinning solution.

[0009] S3. Prepare a composite coagulation bath of calcium chloride and zinc chloride, extrude the spinning solution through the spinneret, control the stretching rate and elongation, and let the filament stay in the coagulation bath to complete the coagulation and shape, and collect the calcium alginate-zinc primary fiber.

[0010] S4. The calcium alginate-zinc nascent fibers are laid flat and placed into the plasma treatment equipment. Using oxygen as the gas source, plasma treatment is carried out to obtain plasma-treated nascent fibers.

[0011] S5. Weigh γ-cyclodextrin-methacrylate and dissolve it in deionized water. After heating and stirring to dissolve, add asiaticoside, stir and cool, then refrigerate and stand. Filter, wash and dry to obtain the inclusion complex. Dissolve silane coupling agent in ethanol aqueous solution, adjust pH and hydrolyze to obtain treatment solution. Immerse plasma-treated nascent fibers in the treatment solution, take them out and pre-dry them, then immerse the fibers in an aqueous solution containing the above inclusion complex. Add ammonium persulfate as an initiator and react under nitrogen protection to obtain fiber intermediate.

[0012] S6. Mix carboxymethyl hyaluronic acid and chitosan, dissolve in acetic acid aqueous solution and stir until dissolved to form a mixed aqueous solution. Add EDC and NHS and stir to dissolve. Then add sodium glycerophosphate to obtain a composite modified solution. Immerse the fiber intermediate in the composite modified solution and continue the reaction by heating. After the reaction, take out the fiber, soak it in sodium bicarbonate aqueous solution, wash and dry it to obtain hydrogel mask fiber.

[0013] S7. The hydrogel mask fibers are combed to form a fiber web, then hydroentangled to make the fibers intertwine, and then hot rolled to shape, thus obtaining the final product.

[0014] In this invention, the moisturizing performance of the fiber base fabric is improved synergistically from two aspects: Firstly, the γ-cyclodextrin-methacrylate molecule is rich in a large number of hydrophilic groups. After grafting onto the surface of the fiber pretreated by plasma, it can significantly increase the density of hydrophilic sites on the fiber, enhance the fiber's adsorption affinity for water and essence, and promote the rapid adhesion and penetration of water into the fiber interior. Its unique cavity structure can not only encapsulate asiaticoside, but also store some water through physical action, reducing the direct contact between water and the external environment, reducing the instantaneous evaporation rate, and achieving initial water retention. At the same time, plasma pretreatment significantly improves the grafting rate and distribution uniformity of the inclusion complexes formed on the fiber surface, allowing all areas of the fiber to efficiently perform the functions of moisture absorption and water storage, thereby constructing a basic and stable moisturizing system for the fiber base fabric and improving the initial moisturizing effect and the ability to retain moisture in a short period of time. On the other hand, carboxymethyl hyaluronic acid has extremely strong water absorption properties, which can quickly capture moisture and essence in the environment, and use the hydrophilicity of the molecular chain to firmly adsorb moisture into the fiber structure, greatly increasing the total water absorption of the fiber; chitosan has good moisture absorption and film-forming properties, which can form a breathable film structure on the fiber surface and inside, effectively preventing internal moisture from diffusing and losing to the outside, and playing a water-locking barrier role. The two form a three-dimensional network structure in the fiber inside and on the fiber through composite cross-linking, which, together with the moisturizing effect of sodium glycerophosphate, constructs a synergistic mechanism of efficient water absorption, stable water storage and long-lasting water locking: the three-dimensional network can not only accommodate more water, but also reduce water evaporation through spatial barrier effect, further improving the moisturizing performance of the fiber base fabric.

[0015] Furthermore, the active ingredients of Centella asiatica can be stably retained in the fiber base fabric, and are not easily detached or lost. First, Centella asiatica extract microcapsules are prepared by complex coagulation method, and the Centella asiatica extract is physically embedded for the first time using a composite wall material formed by gelatin and gum arabic, avoiding direct exposure of the active ingredients to the external environment. Then, γ-cyclodextrin-methacrylate encapsulates Centella asiatica glycosides a second time through a cavity structure, further fixing the active ingredients. At the same time, γ-cyclodextrin-methacrylate forms a covalent graft with the fiber surface with the activation effect of silane coupling agent, so that the molecules of the encapsulated active ingredients are firmly bound to the fiber, rather than simply physically adsorbed. Finally, a three-dimensional cross-linked network of carboxymethyl hyaluronic acid-chitosan further locks the Centella asiatica extract microcapsules and the inclusion complexes grafted on the fiber into the network structure, forming a three-dimensional fixation effect. Whether during storage, transportation, or during application and contact with the skin, friction, or moisture, the active ingredients can remain stably in the fiber base fabric, effectively preventing detachment and loss, and ensuring the continuous performance of efficacy.

[0016] Preferably, in step S1, the mass ratio of gelatin to gum arabic is 10:(12-15).

[0017] Preferably, in step S1, the mass ratio of gelatin to Centella asiatica extract is 10:(4-6).

[0018] Preferably, in step S2, the mass ratio of sodium alginate to Centella asiatica extract microcapsules is 20:(15-20).

[0019] Preferably, in step S5, the preparation method of γ-cyclodextrin-methacrylate includes the following steps:

[0020] γ-Cyclodextrin was added to N,N-dimethylformamide, followed by p-toluenesulfonic acid and hydroquinone. The mixture was heated and stirred, then methacrylate was added, and the mixture was heated to react. After the reaction was completed, the mixture was cooled to room temperature and poured into a precipitant to precipitate a white precipitate. After washing and drying, the product was obtained.

[0021] Preferably, in step S5, the mass ratio of γ-cyclodextrin-methacrylate to asiaticoside is 15:(3-6).

[0022] Preferably, in step S6, the mass ratio of carboxymethyl hyaluronic acid to chitosan is 10:(4-6).

[0023] Preferably, in step S6, the fiber intermediate undergoes pretreatment, including the following steps:

[0024] Sodium dihydrogen phosphate-citric acid buffer, polyglycerol-3, and silane coupling agent KH-550 were added to deionized water and stirred to dissolve, thus obtaining a treatment solution. The fiber intermediate was then immersed in the treatment solution for soaking treatment, and the product was obtained.

[0025] In the technical solution of this invention, the research and development team discovered through in-depth research that after the plasma-grown fibers are grafted with γ-cyclodextrin-methacrylate containing asiaticoside, the dense grafted layer formed on the surface will block the fiber pores. This will cause the composite modification liquid to have difficulty effectively penetrating into the fiber interior during the cross-linking of carboxymethyl hyaluronic acid-chitosan, resulting in a problem of penetration-cross-linking imbalance, leading to weak internal water storage, loose cross-linking network, and ultimately affecting the moisturizing performance. To further address this technical problem, this invention pre-treats the fiber intermediates. A sodium dihydrogen phosphate-citric acid buffer solution provides a weakly acidic environment, gently eroding the dense areas of the grafted layer. This creates micro-nano scale penetration channels without disrupting the structure of the γ-cyclodextrin-methacrylate asiaticoside inclusion complex, opening pathways for the composite modified liquid to penetrate deep into the fiber. Polyglycerol-3, acting as a hydrophilic bridging component, can simultaneously form hydrogen bonds with the hydroxyl groups of the grafted material, the carboxyl groups of carboxymethyl hyaluronic acid, and the amino groups of chitosan. This eliminates the hydrophilic competition between the two groups and reduces the surface tension of the modified liquid, further promoting wetting and penetration. The silane coupling agent KH560, acting as an interface anchoring component, forms hydroxyl groups after hydrolysis that can combine with the active groups on the fiber surface and the grafted material, providing more anchoring points for the crosslinking network. This ensures that the modified liquid, after penetrating deep into the fiber, can fully combine with the fiber body and grafted components, forming a globally synergistic three-dimensional crosslinking network. This solves the penetration-crosslinking imbalance problem and further improves the moisture retention performance of the fiber base fabric.

[0026] Preferably, in step S7, the hot rolling temperature is 100-105℃ and the pressure is 0.3-0.4MPa.

[0027] A hydrogel mask fiber base fabric containing Centella asiatica extract is prepared by the method described above.

[0028] Compared with the prior art, the beneficial effects of the present invention are:

[0029] 1. By grafting γ-cyclodextrin-methacrylate, the hydrophilic sites on the fiber surface are greatly increased, enhancing the water adsorption and storage capacity. Then, by constructing a three-dimensional cross-linked network covering the entire fiber inside and out through carboxymethyl hyaluronic acid and chitosan, a synergistic mechanism of efficient water absorption, stable water storage, and long-lasting water locking is formed, which significantly improves the overall moisture retention durability and stability of the fiber base fabric.

[0030] 2. The active ingredients of Centella Asiatica are encapsulated layer by layer and firmly fixed in the fiber structure, which effectively prevents the active ingredients from falling off and being lost due to friction or soaking during storage, transportation and use, ensuring that they can exert their skin care effects continuously and stably during use. Attached Figure Description

[0031] Figure 1 This is a SEM image of the hydrogel mask fiber substrate prepared in Example 1 of the present invention. Detailed Implementation

[0032] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0033] Example 1

[0034] A method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract includes the following steps:

[0035] Step 1: Weigh 10g of gelatin and 14g of gum arabic and dissolve them in 400mL of deionized water (50℃). Adjust the pH to 4.2. Add 5.5g of Centella asiatica extract, emulsify at 600r / min for 40min, add 30mL of 10% sodium sulfate solution and stir for 18min. Cool to 8℃, adjust the pH to 8.2, and add 5mL of 37% formaldehyde for crosslinking for 25min. Centrifuge at 8000r / min for 10min, wash the precipitate three times with anhydrous ethanol, and vacuum dry at 45℃ for 5h to obtain microcapsules.

[0036] Step 2: Weigh 20g of sodium alginate and dissolve it in 300mL of deionized water. Stir at 1300r / min for 35min to obtain sodium alginate solution. Add 18g of microcapsules and 0.08g of polyethylene glycol 400. Stir for 25min and let stand for 30h to remove bubbles to obtain spinning solution.

[0037] Step 3: Prepare a composite aqueous solution of calcium chloride (4% by mass) and zinc chloride (0.8% by mass) as a coagulation bath. Extrude the spinning solution through a 0.12mm spinneret at a draw rate of 6m / min and an elongation of 45%. Let the filaments stay in the coagulation bath for 18min and collect the calcium alginate-zinc nascent fibers.

[0038] Step 4: Place the calcium alginate-zinc nascent fibers flat into the plasma treatment equipment, using oxygen as the plasma source; set the plasma power to 100W, the treatment time to 4min, and adjust the equipment vacuum to 65Pa to obtain plasma-treated nascent fibers.

[0039] Step 5: Add 12g of γ-cyclodextrin to 150mL of DMF, start magnetic stirring (300r / min) and purge with nitrogen for 15min; then add 0.5g of p-toluenesulfonic acid and 0.05g of hydroquinone, heat to 50℃ and stir for 30min until the γ-cyclodextrin is completely dissolved. Maintain 50℃, nitrogen protection and stirring at 300r / min, add 6.2g of methacrylate dropwise, and after the addition is complete, heat to 65℃, maintain stirring at 300r / min and nitrogen protection, and react at this temperature for 9 hours. After the reaction solution cools to room temperature, add 300mL of anhydrous ethanol and stir to precipitate crystals. Centrifuge at 5000r / min for 10min to collect the white precipitate; wash the precipitate three times with 100mL of anhydrous ethanol, and finally dry the precipitate under vacuum at 60℃ and -0.09MPa for 6 hours to obtain γ-cyclodextrin-methacrylate.

[0040] Weigh 15g of γ-cyclodextrin-methacrylate and dissolve it in 300mL of deionized water (65℃). Add 5g of asiaticoside and stir for 75min. Let it stand at room temperature for 15h. After filtration, wash the precipitate three times with anhydrous ethanol and dry it under vacuum at 45℃ for 5h to obtain the inclusion complex. Dissolve 6mL of KH550 in 294mL of 65% ethanol aqueous solution, adjust the pH to 4.0, and hydrolyze for 35min to obtain the hydrolysate. Immerse the plasma-treated nascent fibers in the hydrolysate (soak at 50℃ for 75min), remove and pre-dry at 85℃ for 30min. Then immerse the fibers in 300mL of aqueous solution containing 12g of the inclusion complex, add 0.12g of ammonium persulfate, react at 65℃ under nitrogen protection for 135min, and wash with deionized water until clear to obtain the fiber intermediate.

[0041] Step 6: Immerse the fiber intermediate in a composite treatment solution containing 2% sodium dihydrogen phosphate-citric acid buffer (pH=4.5), 3% polyglycerol-3, and 0.5% silane coupling agent KH560, using deionized water as the solvent. Static soak for 30 minutes at 35°C. After removal, gently squeeze the fiber with sterile gauze to remove the free treatment solution on the surface, while retaining the treatment solution adsorbed inside the fiber, to obtain the pretreated fiber intermediate.

[0042] 10g of carboxymethyl hyaluronic acid and 5.5g of chitosan were dissolved in 450mL of 1% acetic acid aqueous solution to obtain a mixture. 1.35g of EDC, 0.675g of NHS, and 9g of sodium glycerophosphate were added to the mixture, and the pH was adjusted to 5.0 to obtain a modified solution. The pretreated fiber intermediate was immersed in the modified solution and soaked at 32℃ for 165min, then heated to 48℃ and reacted for 105min. After removal, it was soaked in 6% sodium bicarbonate aqueous solution for 12min, washed four times with deionized water, and dried to obtain hydrogel mask fibers.

[0043] Step 7: The hydrogel mask fibers are combed into a web and treated with 90 bar pressure three times in a hydroentangling machine; the hydroentangled fabric is then shaped in a hot rolling mill (103℃, 0.35MPa, 6m / min) to obtain a hydrogel mask fiber base fabric containing Centella asiatica.

[0044] Example 2

[0045] A method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract includes the following steps:

[0046] Step 1: Weigh 10g of gelatin and 13g of gum arabic and dissolve them in 400mL of deionized water (50℃). Adjust the pH to 4.2. Add 4.5g of Centella asiatica extract, emulsify at 600r / min for 40min, add 30mL of 10% sodium sulfate solution and stir for 18min. Cool to 8℃, adjust the pH to 8.2, and add 5mL of 37% formaldehyde for crosslinking for 25min. Centrifuge at 8000r / min for 10min, wash the precipitate three times with anhydrous ethanol, and vacuum dry at 45℃ for 5h to obtain microcapsules.

[0047] Step 2: Weigh 20g of sodium alginate and dissolve it in 300mL of deionized water. Stir at 1300r / min for 35min to obtain sodium alginate solution. Add 16g of microcapsules and 0.08g of polyethylene glycol 400. Stir for 25min and let stand for 30h to remove bubbles to obtain spinning solution.

[0048] Step 3: Prepare a composite aqueous solution of calcium chloride (4% by mass) and zinc chloride (0.8% by mass) as a coagulation bath. Extrude the spinning solution through a 0.12mm spinneret at a draw rate of 6m / min and an elongation of 45%. Let the filaments stay in the coagulation bath for 18min and collect the calcium alginate-zinc nascent fibers.

[0049] Step 4: Place the calcium alginate-zinc nascent fibers flat into the plasma treatment equipment, using oxygen as the plasma source; set the plasma power to 100W, the treatment time to 4min, and adjust the equipment vacuum to 65Pa to obtain plasma-treated nascent fibers.

[0050] Step 5: Add 12g of γ-cyclodextrin to 150mL of DMF, start magnetic stirring (300r / min) and purge with nitrogen for 15min; then add 0.5g of p-toluenesulfonic acid and 0.05g of hydroquinone, heat to 50℃ and stir for 30min until the γ-cyclodextrin is completely dissolved. Maintain 50℃, nitrogen protection and stirring at 300r / min, add 6.2g of methacrylate dropwise, and after the addition is complete, heat to 65℃, maintain stirring at 300r / min and nitrogen protection, and react at this temperature for 9 hours. After the reaction solution cools to room temperature, add 300mL of anhydrous ethanol and stir to precipitate crystals. Centrifuge at 5000r / min for 10min to collect the white precipitate; wash the precipitate three times with 100mL of anhydrous ethanol, and finally dry the precipitate under vacuum at 60℃ and -0.09MPa for 6 hours to obtain γ-cyclodextrin-methacrylate.

[0051] Weigh 15g of γ-cyclodextrin-methacrylate and dissolve it in 300mL of deionized water (65℃). Add 4g of asiaticoside and stir for 75min. Let it stand at room temperature for 15h. After filtration, wash the precipitate three times with anhydrous ethanol and dry it under vacuum at 45℃ for 5h to obtain the inclusion complex. Dissolve 6mL of KH550 in 294mL of 65% ethanol aqueous solution, adjust the pH to 4.0, and hydrolyze for 35min to obtain the hydrolysate. Immerse the plasma-treated nascent fibers in the hydrolysate (soak at 50℃ for 75min), remove and pre-dry at 85℃ for 30min. Then immerse the fibers in 300mL of aqueous solution containing 12g of the inclusion complex, add 0.12g of ammonium persulfate, react at 65℃ under nitrogen protection for 135min, and wash with deionized water until clear to obtain the fiber intermediate.

[0052] Step 6: Immerse the fiber intermediate in a composite treatment solution containing 2% sodium dihydrogen phosphate-citric acid buffer (pH=4.5), 3% polyglycerol-3, and 0.5% silane coupling agent KH560, using deionized water as the solvent. Static soak for 30 minutes at 35°C. After removal, gently squeeze the fiber with sterile gauze to remove the free treatment solution on the surface, while retaining the treatment solution adsorbed inside the fiber, to obtain the pretreated fiber intermediate.

[0053] 10g of carboxymethyl hyaluronic acid and 4.5g of chitosan were dissolved in 450mL of 1% acetic acid aqueous solution to obtain a mixture. 1.35g of EDC, 0.675g of NHS, and 9g of sodium glycerophosphate were added to the mixture, and the pH was adjusted to 5.0 to obtain a modified solution. The pretreated fiber intermediate was immersed in the modified solution and soaked at 32℃ for 165min, then heated to 48℃ and reacted for 105min. After removal, it was soaked in 6% sodium bicarbonate aqueous solution for 12min, washed four times with deionized water, and dried to obtain hydrogel mask fibers.

[0054] Step 7: The hydrogel mask fibers are combed into a web and treated with 90 bar pressure three times in a hydroentangling machine; the hydroentangled fabric is then shaped in a hot rolling mill (103℃, 0.35MPa, 6m / min) to obtain a hydrogel mask fiber base fabric containing Centella asiatica.

[0055] Example 3

[0056] A method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract includes the following steps:

[0057] Step 1: Weigh 10g of gelatin and 13.5g of gum arabic and dissolve them in 400mL of deionized water (50℃), adjust the pH to 4.2; add 5g of Centella asiatica extract, emulsify at 600r / min for 40min, add 30mL of 10% sodium sulfate solution and stir for 18min, cool to 8℃, adjust the pH to 8.2, add 5mL of 37% formaldehyde and crosslink for 25min; centrifuge at 8000r / min for 10min, wash the precipitate three times with anhydrous ethanol, and vacuum dry at 45℃ for 5h to obtain microcapsules.

[0058] Step 2: Weigh 20g of sodium alginate and dissolve it in 300mL of deionized water. Stir at 1300r / min for 35min to obtain sodium alginate solution. Add 17g of microcapsules and 0.08g of polyethylene glycol 400. Stir for 25min and let stand for 30h to remove bubbles to obtain spinning solution.

[0059] Step 3: Prepare a composite aqueous solution of calcium chloride (4% by mass) and zinc chloride (0.8% by mass) as a coagulation bath. Extrude the spinning solution through a 0.12mm spinneret at a draw rate of 6m / min and an elongation of 45%. Let the filaments stay in the coagulation bath for 18min and collect the calcium alginate-zinc nascent fibers.

[0060] Step 4: Place the calcium alginate-zinc nascent fibers flat into the plasma treatment equipment, using oxygen as the plasma source; set the plasma power to 100W, the treatment time to 4min, and adjust the equipment vacuum to 65Pa to obtain plasma-treated nascent fibers.

[0061] Step 5: Add 12g of γ-cyclodextrin to 150mL of DMF, start magnetic stirring (300r / min) and purge with nitrogen for 15min; then add 0.5g of p-toluenesulfonic acid and 0.05g of hydroquinone, heat to 50℃ and stir for 30min until the γ-cyclodextrin is completely dissolved. Maintain 50℃, nitrogen protection and stirring at 300r / min, add 6.2g of methacrylate dropwise, and after the addition is complete, heat to 65℃, maintain stirring at 300r / min and nitrogen protection, and react at this temperature for 9 hours. After the reaction solution cools to room temperature, add 300mL of anhydrous ethanol and stir to precipitate crystals. Centrifuge at 5000r / min for 10min to collect the white precipitate; wash the precipitate three times with 100mL of anhydrous ethanol, and finally dry the precipitate under vacuum at 60℃ and -0.09MPa for 6 hours to obtain γ-cyclodextrin-methacrylate.

[0062] Weigh 15g of γ-cyclodextrin-methacrylate and dissolve it in 300mL of deionized water (65℃). Add 4.5g of asiaticoside and stir for 75min. Let it stand at room temperature for 15h. After filtration, wash the precipitate three times with anhydrous ethanol and dry it under vacuum at 45℃ for 5h to obtain the inclusion complex. Dissolve 6mL of KH550 in 294mL of 65% ethanol aqueous solution, adjust the pH to 4.0, and hydrolyze for 35min to obtain the hydrolysate. Immerse the plasma-treated nascent fibers in the hydrolysate (soak at 50℃ for 75min), remove and pre-dry at 85℃ for 30min. Then immerse the fibers in 300mL of aqueous solution containing 12g of the inclusion complex, add 0.12g of ammonium persulfate, react at 65℃ under nitrogen protection for 135min, and wash with deionized water until clear to obtain the fiber intermediate.

[0063] Step 6: Immerse the fiber intermediate in a composite treatment solution containing 2% sodium dihydrogen phosphate-citric acid buffer (pH=4.5), 3% polyglycerol-3, and 0.5% silane coupling agent KH560, using deionized water as the solvent. Static soak for 30 minutes at 35°C. After removal, gently squeeze the fiber with sterile gauze to remove the free treatment solution on the surface, while retaining the treatment solution adsorbed inside the fiber, to obtain the pretreated fiber intermediate.

[0064] 10g of carboxymethyl hyaluronic acid and 5g of chitosan were dissolved in 450mL of 1% acetic acid aqueous solution to obtain a mixture. 1.35g of EDC, 0.675g of NHS, and 9g of sodium glycerophosphate were added to the mixture, and the pH was adjusted to 5.0 to obtain a modified solution. The pretreated fiber intermediate was immersed in the modified solution and soaked at 32℃ for 165min, then heated to 48℃ and reacted for 105min. After removal, it was soaked in 6% sodium bicarbonate aqueous solution for 12min, washed four times with deionized water, and dried to obtain hydrogel mask fibers.

[0065] Step 7: The hydrogel mask fibers are combed into a web and treated with 90 bar pressure three times in a hydroentangling machine; the hydroentangled fabric is then shaped in a hot rolling mill (103℃, 0.35MPa, 6m / min) to obtain a hydrogel mask fiber base fabric containing Centella asiatica.

[0066] Example 4

[0067] A method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract includes the following steps:

[0068] Step 1: Weigh 10g of gelatin and 15g of gum arabic and dissolve them in 400mL of deionized water (50℃). Adjust the pH to 4.2. Add 6g of Centella asiatica extract, emulsify at 600r / min for 40min, add 30mL of 10% sodium sulfate solution and stir for 18min. Cool to 8℃, adjust the pH to 8.2, and add 5mL of 37% formaldehyde for crosslinking for 25min. Centrifuge at 8000r / min for 10min, wash the precipitate three times with anhydrous ethanol, and vacuum dry at 45℃ for 5h to obtain microcapsules.

[0069] Step 2: Weigh 20g of sodium alginate and dissolve it in 300mL of deionized water. Stir at 1300r / min for 35min to obtain sodium alginate solution. Add 20g of microcapsules and 0.08g of polyethylene glycol 400. Stir for 25min and let stand for 30h to remove bubbles to obtain spinning solution.

[0070] Step 3: Prepare a composite aqueous solution of calcium chloride (4% by mass) and zinc chloride (0.8% by mass) as a coagulation bath. Extrude the spinning solution through a 0.12mm spinneret at a draw rate of 6m / min and an elongation of 45%. Let the filaments stay in the coagulation bath for 18min and collect the calcium alginate-zinc nascent fibers.

[0071] Step 4: Place the calcium alginate-zinc nascent fibers flat into the plasma treatment equipment, using oxygen as the plasma source; set the plasma power to 100W, the treatment time to 4min, and adjust the equipment vacuum to 65Pa to obtain plasma-treated nascent fibers.

[0072] Step 5: Add 12g of γ-cyclodextrin to 150mL of DMF, start magnetic stirring (300r / min) and purge with nitrogen for 15min; then add 0.5g of p-toluenesulfonic acid and 0.05g of hydroquinone, heat to 50℃ and stir for 30min until the γ-cyclodextrin is completely dissolved. Maintain 50℃, nitrogen protection and stirring at 300r / min, add 6.2g of methacrylate dropwise, and after the addition is complete, heat to 65℃, maintain stirring at 300r / min and nitrogen protection, and react at this temperature for 9 hours. After the reaction solution cools to room temperature, add 300mL of anhydrous ethanol and stir to precipitate crystals. Centrifuge at 5000r / min for 10min to collect the white precipitate; wash the precipitate three times with 100mL of anhydrous ethanol, and finally dry the precipitate under vacuum at 60℃ and -0.09MPa for 6 hours to obtain γ-cyclodextrin-methacrylate.

[0073] Weigh 15g of γ-cyclodextrin-methacrylate and dissolve it in 300mL of deionized water (65℃). Add 6g of asiaticoside and stir for 75min. Let it stand at room temperature for 15h. After filtration, wash the precipitate three times with anhydrous ethanol and dry it under vacuum at 45℃ for 5h to obtain the inclusion complex. Dissolve 6mL of KH550 in 294mL of 65% ethanol aqueous solution, adjust the pH to 4.0, and hydrolyze for 35min to obtain the hydrolysate. Immerse the plasma-treated nascent fibers in the hydrolysate (soak at 50℃ for 75min), remove and pre-dry at 85℃ for 30min. Then immerse the fibers in 300mL of aqueous solution containing 12g of the inclusion complex, add 0.12g of ammonium persulfate, react at 65℃ under nitrogen protection for 135min, and wash with deionized water until clear to obtain the fiber intermediate.

[0074] Step 6: Immerse the fiber intermediate in a composite treatment solution containing 2% sodium dihydrogen phosphate-citric acid buffer (pH=4.5), 3% polyglycerol-3, and 0.5% silane coupling agent KH560, using deionized water as the solvent. Static soak for 30 minutes at 35°C. After removal, gently squeeze the fiber with sterile gauze to remove the free treatment solution on the surface, while retaining the treatment solution adsorbed inside the fiber, to obtain the pretreated fiber intermediate.

[0075] 10g of carboxymethyl hyaluronic acid and 6g of chitosan were dissolved in 450mL of 1% acetic acid aqueous solution to obtain a mixture. 1.35g of EDC, 0.675g of NHS, and 9g of sodium glycerophosphate were added to the mixture, and the pH was adjusted to 5.0 to obtain a modified solution. The pretreated fiber intermediate was immersed in the modified solution and soaked at 32℃ for 165min, then heated to 48℃ and reacted for 105min. After removal, it was soaked in 6% sodium bicarbonate aqueous solution for 12min, washed four times with deionized water, and dried to obtain hydrogel mask fibers.

[0076] Step 7: The hydrogel mask fibers are combed into a web and treated with 90 bar pressure three times in a hydroentangling machine; the hydroentangled fabric is then shaped in a hot rolling mill (105℃, 0.4MPa, 6m / min) to obtain a hydrogel mask fiber base fabric containing Centella asiatica.

[0077] Example 5

[0078] A method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract includes the following steps:

[0079] Step 1: Weigh 10g of gelatin and 12g of gum arabic and dissolve them in 400mL of deionized water (50℃). Adjust the pH to 4.2. Add 4g of Centella asiatica extract, emulsify at 600r / min for 40min, add 30mL of 10% sodium sulfate solution and stir for 18min. Cool to 8℃, adjust the pH to 8.2, and add 5mL of 37% formaldehyde for crosslinking for 25min. Centrifuge at 8000r / min for 10min, wash the precipitate three times with anhydrous ethanol, and vacuum dry at 45℃ for 5h to obtain microcapsules.

[0080] Step 2: Weigh 20g of sodium alginate and dissolve it in 300mL of deionized water. Stir at 1300r / min for 35min to obtain sodium alginate solution. Add 15g of microcapsules and 0.08g of polyethylene glycol 400. Stir for 25min and let stand for 30h to remove bubbles to obtain spinning solution.

[0081] Step 3: Prepare a composite aqueous solution of calcium chloride (4% by mass) and zinc chloride (0.8% by mass) as a coagulation bath. Extrude the spinning solution through a 0.12mm spinneret at a draw rate of 6m / min and an elongation of 45%. Let the filaments stay in the coagulation bath for 18min and collect the calcium alginate-zinc nascent fibers.

[0082] Step 4: Place the calcium alginate-zinc nascent fibers flat into the plasma treatment equipment, using oxygen as the plasma source; set the plasma power to 100W, the treatment time to 4min, and adjust the equipment vacuum to 65Pa to obtain plasma-treated nascent fibers.

[0083] Step 5: Add 12g of γ-cyclodextrin to 150mL of DMF, start magnetic stirring (300r / min) and purge with nitrogen for 15min; then add 0.5g of p-toluenesulfonic acid and 0.05g of hydroquinone, heat to 50℃ and stir for 30min until the γ-cyclodextrin is completely dissolved. Maintain 50℃, nitrogen protection and stirring at 300r / min, add 6.2g of methacrylate dropwise, and after the addition is complete, heat to 65℃, maintain stirring at 300r / min and nitrogen protection, and react at this temperature for 9 hours. After the reaction solution cools to room temperature, add 300mL of anhydrous ethanol and stir to precipitate crystals. Centrifuge at 5000r / min for 10min to collect the white precipitate; wash the precipitate three times with 100mL of anhydrous ethanol, and finally dry the precipitate under vacuum at 60℃ and -0.09MPa for 6 hours to obtain γ-cyclodextrin-methacrylate.

[0084] Weigh 15g of γ-cyclodextrin-methacrylate and dissolve it in 300mL of deionized water (65℃). Add 3g of asiaticoside and stir for 75min. Let it stand at room temperature for 15h. After filtration, wash the precipitate three times with anhydrous ethanol and dry it under vacuum at 45℃ for 5h to obtain the inclusion complex. Dissolve 6mL of KH550 in 294mL of 65% ethanol aqueous solution, adjust the pH to 4.0, and hydrolyze for 35min to obtain the hydrolysate. Immerse the plasma-treated nascent fibers in the hydrolysate (soak at 50℃ for 75min), remove and pre-dry at 85℃ for 30min. Then immerse the fibers in 300mL of aqueous solution containing 12g of the inclusion complex, add 0.12g of ammonium persulfate, react at 65℃ under nitrogen protection for 135min, and wash with deionized water until clear to obtain the fiber intermediate.

[0085] Step 6: Immerse the fiber intermediate in a composite treatment solution containing 2% sodium dihydrogen phosphate-citric acid buffer (pH=4.5), 3% polyglycerol-3, and 0.5% silane coupling agent KH560, using deionized water as the solvent. Static soak for 30 minutes at 35°C. After removal, gently squeeze the fiber with sterile gauze to remove the free treatment solution on the surface, while retaining the treatment solution adsorbed inside the fiber, to obtain the pretreated fiber intermediate.

[0086] 10g of carboxymethyl hyaluronic acid and 4g of chitosan were dissolved in 450mL of 1% acetic acid aqueous solution to obtain a mixture. 1.35g of EDC, 0.675g of NHS, and 9g of sodium glycerophosphate were added to the mixture, and the pH was adjusted to 5.0 to obtain a modified solution. The pretreated fiber intermediate was immersed in the modified solution and soaked at 32℃ for 165min, then heated to 48℃ and reacted for 105min. After removal, it was soaked in 6% sodium bicarbonate aqueous solution for 12min, washed four times with deionized water, and dried to obtain hydrogel mask fibers.

[0087] Step 7: The hydrogel mask fibers are combed into a web and treated with 90 bar pressure three times in a hydroentangling machine; the hydroentangled fabric is then shaped in a hot rolling mill (100℃, 0.3MPa, 6m / min) to obtain a hydrogel mask fiber base fabric containing Centella asiatica.

[0088] Comparative Example 1: The difference between Comparative Example 1 and Example 1 is that step 1 is omitted in the preparation of the fiber base fabric, and the microcapsules in step 2 are replaced with an equal mass of Centella asiatica extract.

[0089] Comparative Example 2: The difference between Comparative Example 1 and Example 1 is that step 5 is omitted in the preparation of the fiber base fabric, that is, the plasma-treated nascent fibers do not undergo γ-cyclodextrin-methacrylate grafting treatment.

[0090] Comparative Example 3: The difference between Comparative Example 3 and Example 1 is that step 6 is omitted in the preparation of the fiber base fabric, that is, the fiber intermediate is not cross-linked with carboxymethyl hyaluronic acid and chitosan.

[0091] Comparative Example 4: The difference between Comparative Example 4 and Example 1 is that in step 6, the fiber intermediate is not pretreated by soaking in the composite treatment solution.

[0092] Performance testing:

[0093] 1. Liquid Absorption Rate Test: Take base fabric samples (cut to 5cm × 5cm) from each example and comparative example, and vacuum dry them at 105℃ to constant weight (recorded as m0). Completely immerse the dried samples in deionized water at 25℃, let them stand for 30 minutes, then remove them and gently squeeze them with sterile gauze until no liquid drips. Weigh them immediately (recorded as m1). The liquid absorption rate is calculated using the formula: Liquid Absorption Rate (%) = (m1 - m0) / m0 × 100%. Each group of samples was tested in triplicate, and the average value was taken. The test results are shown in Table 1.

[0094] 2. Moisture retention test: A constant temperature and humidity chamber was used to control environmental conditions (temperature 25℃±1℃, relative humidity 50%±2%). A sample of the base fabric saturated with liquid (denoted as m2) was placed in the above environment and weighed after 24 hours (denoted as m). n The formula for calculating moisture retention rate is: Moisture retention rate (%) = (m n (-m0) / (m2-m0)×100%, each group of samples was tested in parallel 3 times, and the average value was taken. The test results are shown in Table 1.

[0095] 3. Aspartic acid loading test: High performance liquid chromatography (HPLC) was used. The chromatographic conditions were: C18 column (250 mm × 4.6 mm, 5 μm), mobile phase: methanol-water (60:40, v / v), detection wavelength: 205 nm, column temperature: 30 ℃, flow rate: 1.0 mL / min. 0.5 g of each base fabric sample was added to 25 mL of methanol and extracted ultrasonically for 30 min. The supernatant was centrifuged, filtered through a 0.45 μm filter membrane, and 20 μL was injected. The aspartic acid content was calculated using the standard curve method. The loading formula was: loading (mg / g) = mass of aspartic acid in the extract (mg) / mass of the sample (g). Each group was tested in triplicate, and the average value was taken. The test results are shown in Table 1.

[0096] 4. Tensile strength and elongation at break test: A universal testing machine was used. The base fabric sample was cut into standard strips of 50mm × 10mm, with a clamping distance of 30mm and a tensile rate of 10mm / min. The maximum force (tensile strength) and elongation at break were recorded. The elongation at break was calculated using the formula: Elongation at break (%) = (Elongation at break / Clamping distance) × 100%. Each group of samples was tested in parallel for 5 times, and the average value was taken. The test results are shown in Table 1.

[0097] Table 1:

[0098] Liquid absorption rate (%) Moisture retention rate (%) Centella asiatica glycoside loading (mg / g) Fracture strength (N) Elongation at break (%) Example 1 539.7 47.1 0.81 8.7 32.8 Example 2 534.5 45.6 0.75 8.4 31.6 Example 3 537.2 46.5 0.78 8.6 32.0 Example 4 542.6 47.8 0.86 8.9 33.2 Example 5 529.8 45.0 0.71 8.1 31.1 Comparative Example 1 518.4 41.6 0.26 5.3 21.3 Comparative Example 2 421.5 28.3 0.38 6.2 24.5 Comparative Example 3 352.1 17.9 0.45 5.8 23.1 Comparative Example 4 453.7 33.7 0.58 7.2 27.8

[0099] 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 a hydrogel mask fiber base fabric containing Centella asiatica extract, characterized in that, Includes the following steps: S1. Weigh gelatin and gum arabic and dissolve them in deionized water. Heat and stir until dissolved. Add centella asiatica extract and stir to emulsify. Add sodium sulfate solution and cool down. Add formaldehyde solution to crosslink and solidify. Centrifuge, wash and dry to obtain centella asiatica extract microcapsules. S2. Weigh out sodium alginate and dissolve it in deionized water to obtain sodium alginate aqueous solution. Add Centella asiatica extract microcapsules and polyethylene glycol, continue to stir at high speed and let stand to degas, and obtain spinning solution. S3. Prepare a composite coagulation bath of calcium chloride and zinc chloride, extrude the spinning solution through the spinneret, control the stretching rate and elongation, and let the filament stay in the coagulation bath to complete the coagulation and shape, and collect the calcium alginate-zinc primary fiber. S4 The calcium alginate-zinc nascent fibers were laid flat and placed into a plasma treatment device. Using oxygen as the gas source, plasma treatment was carried out to obtain plasma-treated nascent fibers. S5. Weigh γ-cyclodextrin-methacrylate and dissolve it in deionized water. After heating and stirring to dissolve, add asiaticoside, stir and cool, then refrigerate and stand. Filter, wash and dry to obtain the inclusion complex. Dissolve silane coupling agent in ethanol aqueous solution, adjust pH and hydrolyze to obtain treatment solution. Immerse plasma-treated nascent fibers in the treatment solution, take them out and pre-dry them, then immerse the fibers in an aqueous solution containing the above inclusion complex. Add ammonium persulfate as an initiator and react under nitrogen protection to obtain fiber intermediate. S6. Mix carboxymethyl hyaluronic acid and chitosan, dissolve in acetic acid aqueous solution and stir until dissolved to form a mixed aqueous solution. Add EDC and NHS and stir to dissolve. Then add sodium glycerophosphate to obtain a composite modified solution. Immerse the fiber intermediate in the composite modified solution and continue the reaction by heating. After the reaction, take out the fiber, soak it in sodium bicarbonate aqueous solution, wash and dry it to obtain hydrogel mask fiber. S7. The hydrogel mask fibers are combed to form a fiber web, then hydroentangled to make the fibers intertwine, and then hot rolled to shape, thus obtaining the final product.

2. The method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S1, the mass ratio of gelatin to gum arabic is 10:(12-15).

3. The method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S1, the mass ratio of gelatin to Centella asiatica extract is 10:(4-6).

4. The method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S2, the mass ratio of sodium alginate to Centella asiatica extract microcapsules is 20:(15-20).

5. The method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S5, the preparation method of γ-cyclodextrin-methacrylate includes the following steps: γ-Cyclodextrin was added to N,N-dimethylformamide, followed by p-toluenesulfonic acid and hydroquinone. The mixture was heated and stirred, then methacrylate was added, and the mixture was heated to react. After the reaction was completed, the mixture was cooled to room temperature and poured into a precipitant to precipitate a white precipitate. After washing and drying, the product was obtained.

6. The method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S5, the mass ratio of γ-cyclodextrin-methacrylate to asiaticoside is 15:(3-6).

7. A method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S6, the mass ratio of carboxymethyl hyaluronic acid to chitosan is 10:(4-6).

8. The method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S6, the fiber intermediate undergoes pretreatment, including the following steps: Sodium dihydrogen phosphate-citric acid buffer, polyglycerol-3, and silane coupling agent KH-550 were added to deionized water and stirred to dissolve, thus obtaining a treatment solution. The fiber intermediate was then immersed in the treatment solution for soaking treatment, and the product was obtained.

9. The method for preparing a hydrogel mask fiber base fabric containing Centella asiatica extract according to claim 1, characterized in that, In step S7, the hot rolling temperature is 100-105℃ and the pressure is 0.3-0.4MPa.

10. A hydrogel mask fiber base fabric containing Centella asiatica extract, characterized in that, It is prepared by the method described in any one of claims 1 to 9 above.

Images