An antibacterial herbal mask cloth and a method of preparing the same
Patent Information
- Application Number
- CN202610869438.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-06-16
- Publication Date
- 2026-10-30
AI Technical Summary
[0006]为了解决现有面膜布基材自身不具备功能活性、草本活性成分与基材结合力弱导致突释流失、各组分功效发挥不充分且利用率低、单层均质结构难以兼顾贴肤舒适性与储液缓释、抑蒸性能等问题,本发明提供了一种抗菌草本面膜布及其制备方法
1、三层功能梯度结构实现“释放-储液-抑蒸”协同:本发明的面膜布由内至外依次设置释放层、储液层和阻蒸层,三层通过水刺纤维缠结一体化成型,层间无胶粘界面。释放层以黄柏基纤维和小檗碱微胶囊作为功能组分,可以直接贴合皮肤,提供高效、持续的抗菌活性释放;储液层富含储液组合物,具有高吸液量和凝胶化缓释能力,可持续向释放层补给精华液;阻蒸层以高比例的莱赛尔纤维构建致密结构,可有效抑制精华液从背面蒸发散失。三层各司其职、功能互补,克服了现有单层均质面膜布无法同时兼顾贴肤舒适性、储液保持性和抑蒸性能的技术瓶颈。
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Abstract
Description
Technical Field
[0001] This invention relates to the field of mask substrate preparation technology, specifically to an antibacterial herbal mask fabric and its preparation method. Background Technology
[0002] The mask sheet is the core carrier of sheet mask products. Its function is to absorb and store the essence, and to continuously deliver the active ingredients to the skin during the application process. Currently, most mask sheet substrates only serve as inert liquid carriers, and all efficacy depends on the essence formula they contain.
[0003] There are two main methods for introducing herbal active ingredients in existing technologies: one is to add herbal extracts to the essence, which is then physically adsorbed by the mask sheet before use; the other is to coat the herbal extracts onto the surface of the finished mask sheet. In the former, the active ingredients are only loosely adsorbed to the substrate, resulting in a burst release at the initial application stage and thus low utilization. In the latter, the binding force is weak, making it easy for the ingredients to detach or dissolve rapidly during storage and use, and the uniformity of coating and batch stability are difficult to guarantee. Furthermore, existing technologies typically use herbal raw materials in the form of crude extracts or single active ingredients, failing to perform graded extraction and differentiated introduction based on the physicochemical differences of different types of active components. This makes it difficult for the components to fully exert their synergistic effects, resulting in low overall utilization of the raw materials.
[0004] In terms of structural design, most existing mask sheets are single-layer homogeneous structures, failing to simultaneously meet the three requirements of skin-friendly comfort, efficient liquid retention, and evaporation inhibition. While some existing technologies propose multi-layer structures, these are merely simple superpositions of a skin-friendly layer and a support layer, lacking a gradient design in pore size and function among the layers. Regarding antibacterial properties, some products impart antibacterial functionality to the substrate through chemical means such as adding silver ions and organic antibacterial agents, but these pose issues such as irritation to sensitive skin, safety concerns, and environmental residues. Furthermore, existing mask sheets generally lack an interactive response mechanism with the skin's microenvironment; the release of active ingredients is not regulated by physiological factors such as the skin's surface pH, preventing adaptive release and limiting precise skincare effects.
[0005] To address the aforementioned issues, this invention provides an antibacterial herbal facial mask fabric and its preparation method. Summary of the Invention
[0006] To address the problems of existing facial mask fabric substrates lacking functional activity, weak binding force between herbal active ingredients and substrate leading to burst release loss, insufficient efficacy and low utilization of each component, and difficulty in balancing skin comfort with liquid storage, slow release, and anti-evaporation performance in a single-layer homogeneous structure, this invention provides an antibacterial herbal facial mask fabric and its preparation method.
[0007] In a first aspect, the present invention provides an antibacterial herbal facial mask sheet, which adopts the following technical solution: An antibacterial herbal facial mask sheet, comprising, from the inside out, a release layer, a liquid storage layer, and an anti-evaporation layer; The release layer comprises the following raw materials in parts by weight: 2-4 parts of berberine-based fiber, 3-5 parts of ultrafine viscose fiber, and 1-2 parts of berberine microcapsules; The liquid storage layer comprises the following raw materials in parts by weight: 5-7 parts of ultrafine viscose fiber, 2-3 parts of liquid storage composition, and 1-2 parts of lyocell fiber; The vapor barrier layer comprises the following raw materials in parts by weight: 2-4 parts of ultrafine viscose fiber and 6-8 parts of lyocell fiber.
[0008] Preferably, the areal density of the release layer is 8-18 g / m²; the areal density of the liquid storage layer is 15-25 g / m²; and the areal density of the anti-evaporation layer is 8-15 g / m².
[0009] Preferably, the fineness of the ultrafine viscose fiber is 0.5-1.1 dtex; the fineness of the lyocell fiber is 1.0-1.7 dtex; and the fiber cutting length of both the ultrafine viscose fiber and the lyocell fiber is 35-45 mm.
[0010] Preferably, the method for preparing the phellodendron-based fiber is as follows: The dried bark of Phellodendron bark is crushed and sieved to obtain Phellodendron bark powder. The Phellodendron bark powder is added to hydrochloric acid aqueous solution for extraction, filtered, and the residue is obtained. The residue is added to ethanol aqueous solution for extraction, filtered, and a secondary residue is obtained. The secondary residue is boiled with alkali, washed with water, mechanically loosened, dried, and cut to obtain Phellodendron bark-based fiber.
[0011] Preferably, the specific preparation method of the phellodendron-based fiber is as follows: The dried bark of Phellodendron amurense is pulverized and passed through a 40-80 mesh sieve to obtain Phellodendron amurense powder. The Phellodendron amurense powder is mixed with a 1-2% hydrochloric acid aqueous solution at a solid-liquid ratio of 1:8-15 and extracted at 60-80℃ for 1-3 hours. After filtration, the residue is obtained. The residue is mixed with a 50-80% ethanol aqueous solution at a solid-liquid ratio of 1:6-12 and extracted at 60-70℃ for 1-2 hours. After filtration, a secondary residue is obtained. The secondary residue is added to a 2-6wt% sodium hydroxide solution and boiled at 90-100℃ for 1-3 hours. It is then washed with deionized water until neutral, mechanically loosened, dried at 60-80℃ until the moisture content is ≤10%, and cut into lengths of 35-45 mm to obtain Phellodendron amurense-based fibers.
[0012] Preferably, the berberine microcapsules are prepared by: Berberine hydrochloride was dissolved in acetate buffer to obtain a core solution; chitosan was dissolved in acetic acid solution to obtain a chitosan solution; the core solution and chitosan solution were mixed to obtain an inner phase; sodium alginate was dissolved in deionized water to obtain an outer phase; the inner phase was dispersed uniformly by high-speed shearing and then added dropwise to the outer phase to obtain a precapsule; the precapsule was added to a coagulation bath and stirred to react, filtered, washed, and freeze-dried to obtain berberine microcapsules.
[0013] Preferably, the specific preparation method of the berberine microcapsules is as follows: Berberine hydrochloride was dissolved in an acetate buffer solution (composed of 0.1-0.2 mol / L acetic acid solution and 0.1-0.2 mol / L sodium acetate solution in a volume ratio of 1:0.8-1.2) at a mass ratio of 1-2:100 to obtain the core solution; chitosan was dissolved in a 1-2 wt% acetic acid solution at a mass ratio of 2-3:100 to obtain the chitosan solution; the core solution and chitosan solution were mixed at a volume ratio of 1:1-3 to obtain the inner phase; sodium alginate was dissolved in deionized water at a mass ratio of 1-3:100 to obtain the outer phase; the reaction was carried out at room temperature. Under high-speed shear dispersion at 6000-10000 rpm for 5-15 min, the internal phase is then added dropwise to the external phase at a rate of 1-2 mL / min to obtain precapsules. The precapsules are added to a coagulation bath at a mass ratio of 1:6-10 and stirred at 30-50℃ and 100-200 rpm for 6-8 h. After filtration, the precapsules are washed 2-3 times with deionized water, pre-frozen at -40℃ to -80℃ for 8-12 h, and then freeze-dried at -50℃ to -60℃ and a vacuum degree ≤20 Pa for 24-48 h to obtain berberine microcapsules.
[0014] Preferably, the coagulation bath is composed of calcium chloride, genipin and deionized water in a mass ratio of 3-5:0.1-0.3:100.
[0015] Preferably, the storage liquid composition consists of sodium carboxymethyl cellulose, flavonoid extract of Phellodendron bark, and metal ion coordinating agent in a mass ratio of 4-6:3-5:0.06-0.1.
[0016] Preferably, the metal ion ligand is selected from one or two of aluminum chloride and ferric chloride.
[0017] Preferably, the specific preparation method of the Phellodendron chinense flavonoid extract is as follows: The dried bark of Phellodendron bark is pulverized and passed through a 40-80 mesh sieve to obtain Phellodendron bark powder. The Phellodendron bark powder is mixed with a 50-80% (v / v) ethanol aqueous solution at a solid-liquid ratio of 1:6-12 and extracted at 60-70℃ for 1-2 hours. After filtration, a flavonoid-rich solution is obtained. The flavonoid-rich solution is concentrated under reduced pressure at 40-60℃ and a vacuum degree ≤-0.08MPa to 20-30% of its original volume. Then, it is spray-dried at an inlet air temperature of 140-180℃ and an outlet air temperature of 70-90℃ until the moisture content is ≤10% to obtain the Phellodendron bark flavonoid extract.
[0018] Secondly, the present invention provides a method for preparing an antibacterial herbal facial mask sheet, using the following technical solution: A method for preparing an antibacterial herbal facial mask sheet includes the following steps: S1. Mix the raw materials of the release layer, the liquid storage layer and the anti-evaporation layer separately, loosen them and comb them into a web to obtain the release layer fiber web, the liquid storage layer fiber web and the anti-evaporation layer fiber web. S2. From bottom to top, the release layer fiber mesh, the liquid storage layer fiber mesh and the anti-evaporation layer fiber mesh are laid in sequence to obtain a three-layer composite fiber mesh. S3. The three-layer composite fiber web is pre-wetted and subjected to double-sided gradient hydroentangling, then dried with hot air and cut to obtain an antibacterial herbal facial mask fabric.
[0019] Preferably, in step S1, the cylinder speed for opening is 300-600 rpm, and the doffer speed for combing is 40-60 m / min.
[0020] Preferably, the parameters for the double-sided gradient hydroentangling treatment in step S3 include: hydroentangling pressure on the fiber web side of the release layer is 40-80 bar, hydroentangling pressure on the fiber web side of the anti-evaporation layer is 80-150 bar, hydroentangling head orifice diameter is 0.08-0.15 mm, and machine speed is 40-60 m / min; the drying temperature is 60-90℃, and drying is carried out until the moisture content is ≤8%.
[0021] Thirdly, the present invention provides an application of the above-mentioned antibacterial herbal mask fabric in the preparation of skin care masks, antibacterial dressings or acne care patch products.
[0022] In summary, the present invention has the following beneficial effects: 1. A three-layer functional gradient structure achieves synergistic "release-retention-anti-evaporation": The mask fabric of this invention consists of a release layer, a retention layer, and an anti-evaporation layer arranged sequentially from the inside out. These three layers are integrally formed by entanglement of hydroentangled fibers, with no adhesive interfaces between them. The release layer uses berberine-based fibers and berberine microcapsules as functional components, allowing it to directly adhere to the skin and provide efficient and continuous antibacterial activity release. The retention layer is rich in a retention composition, possessing high absorbency and gel-based sustained-release capabilities, continuously replenishing the essence to the release layer. The anti-evaporation layer, constructed with a high proportion of lyocell fibers to create a dense structure, effectively inhibits the evaporation and loss of essence from the back. Each of the three layers performs its specific function and complements the others, overcoming the technical bottleneck of existing single-layer homogeneous mask fabrics that cannot simultaneously achieve skin-friendly comfort, retention, and anti-evaporation performance.
[0023] 2. Phellodendron bark-based fibers endow the substrate with intrinsic antibacterial activity: This invention obtains Phellodendron bark-based fibers by graded extraction and alkali boiling treatment, which retain the natural fiber morphology and are rich in residual antibacterial components (such as berberine). This enables the mask fabric substrate to have antibacterial function on its own, which is different from the existing mask fabrics that rely entirely on external antibacterial agents. This fundamentally improves the functional activity and safety of the mask fabric substrate.
[0024] 3. Berberine Microcapsules Achieve pH-Responsive Controlled Release: This invention utilizes a chitosan-sodium alginate double-walled structure to encapsulate berberine hydrochloride, and uses genipin as a covalent cross-linking agent to cross-link and solidify the chitosan layer. During application, the resulting berberine microcapsules respond to the slightly acidic environment of the skin surface (pH 4.5-6.5), causing the chitosan layer to swell and increasing the permeability of the wall layer, thereby achieving on-demand release of berberine. This effectively avoids the sudden release loss and oxidative degradation of free berberine in the serum, significantly improving the bioavailability and duration of action of the antibacterial components.
[0025] 4. The reservoir composition constructs an in-situ gel-release system: After absorbing the essence, sodium carboxymethyl cellulose in the reservoir composition forms a hydrogel network. The flavonoid extract of Phellodendron amurense undergoes coordination cross-linking with metal ion coordinating agents through its phenolic hydroxyl groups, further enhancing the gel network density and achieving efficient retention and slow release of the essence. This system combines the dual functions of reservoir and efficacy release, significantly extending the effective utilization time of the essence compared to traditional mask sheets.
[0026] 5. Double-sided gradient hydroentangling constructs an asymmetric pore structure: This invention employs a double-sided gradient hydroentangling strategy in the hydroentangling reinforcement process, with low pressure on the release layer side and high pressure on the anti-evaporation layer side. Low-pressure hydroentangling maintains a large porosity and fluffiness in the release layer, facilitating the penetration and release of the essence towards the skin; high-pressure hydroentangling makes the fibers of the anti-evaporation layer highly entangled and dense, effectively inhibiting the evaporation of the essence from the back side. Gradient hydroentangling, while ensuring interlayer bonding, achieves an asymmetric pore size distribution in the thickness direction of the mask fabric, from loose to dense, which is a key process for synergistic "release-anti-evaporation" functions.
[0027] 6. All-natural herbal system with high safety: The functional active components in the mask fabric of this invention (such as berberine-based fiber, berberine hydrochloride, and berberine flavonoid extract) are all derived from the natural herb berberine. The microcapsule wall material (such as chitosan and sodium alginate) and cross-linking agent (such as genipin) are all natural polymer materials or natural cross-linking agents. The matrix fiber (such as viscose and lyocell) is regenerated cellulose fiber. The overall system is green and safe, and can be used in skin care masks, antibacterial dressings, acne care patches, and other product scenarios that come into direct contact with the skin. Detailed Implementation
[0028] The present invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are for illustrative purposes only and are not intended to limit the scope of the invention.
[0029] Where specific techniques or conditions are not specified in the examples, they shall be performed in accordance with the techniques or conditions described in the literature in this field, or in accordance with the product instructions. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased through legitimate channels.
[0030] Unless otherwise specified, the experimental methods used in the following embodiments are conventional methods. Unless otherwise specified, the experimental materials used in the following embodiments are commercially available products.
[0031] The ultrafine viscose fiber was purchased from Shandong Fuhui Textile Technology Co., Ltd. Lyocell fiber was purchased from Jiangsu Huasai New Material Technology Co., Ltd. Berberine hydrochloride was purchased from Shaanxi Angxu Biotechnology Co., Ltd., with a purity of 98%.
[0032] Example 1 An antibacterial herbal facial mask sheet, comprising, from the inside out, a release layer, a liquid storage layer, and an anti-evaporation layer; The release layer comprises the following raw materials in parts by weight: 2 parts of phellodendron bark fiber, 3 parts of ultrafine viscose fiber, and 1 part of berberine microcapsules; the areal density of the release layer is 8 g / m². The liquid storage layer comprises the following raw materials in parts by weight: 5 parts ultrafine viscose fiber, 2 parts liquid storage composition, and 1 part lyocell fiber; the areal density of the liquid storage layer is 15 g / m². The vapor barrier layer comprises the following raw materials in parts by weight: 2 parts ultrafine viscose fiber and 6 parts lyocell fiber; the areal density of the vapor barrier layer is 8 g / m².
[0033] The fineness of the ultrafine viscose fiber is 0.5 dtex, and the fineness of the lyocell fiber is 1 dtex; the fiber cut length of both ultrafine viscose fiber and lyocell fiber is 35 mm.
[0034] The reservoir composition consists of sodium carboxymethyl cellulose, flavonoid extract of Phellodendron bark, and aluminum chloride in a mass ratio of 4:3:0.06.
[0035] The specific preparation method of Phellodendron amurense-based fiber is as follows: The dried bark of Phellodendron amurense was pulverized and passed through a 40-mesh sieve to obtain Phellodendron amurense powder. The Phellodendron amurense powder was mixed with a 1% hydrochloric acid aqueous solution at a solid-liquid ratio of 1:8 and extracted at 60℃ for 1 hour. After filtration, the residue was obtained. The residue was mixed with a 50% ethanol aqueous solution at a solid-liquid ratio of 1:6 and extracted at 60℃ for 1 hour. After filtration, a secondary residue was obtained. The secondary residue was added to a 2wt% sodium hydroxide solution and boiled at 90℃ for 1 hour. It was washed with deionized water until neutral, mechanically loosened, dried at 60℃ to a moisture content of 10%, and cut to a length of 35 mm to obtain Phellodendron amurense-based fibers.
[0036] The specific preparation method of berberine microcapsules is as follows: Berberine hydrochloride was dissolved in an acetate buffer solution (composed of a 0.1 mol / L acetic acid solution and a 0.1 mol / L sodium acetate solution with a volume ratio of 1:0.8) at a mass ratio of 1:100 to obtain the core solution; chitosan was dissolved in a 1 wt% acetic acid solution at a mass ratio of 2:100 to obtain the chitosan solution; the core solution and chitosan solution were mixed at a volume ratio of 1:1 to obtain the inner phase; sodium alginate was dissolved in deionized water at a mass ratio of 1:100 to obtain the outer phase; the inner phase was then... The precapsules were dispersed by high-speed shearing at 6000 rpm for 5 min, and then added dropwise to the external phase at a rate of 1 mL / min to obtain precapsules. The precapsules were added to a coagulation bath (composed of calcium chloride, genipin and deionized water in a mass ratio of 3:0.1:100) at a mass ratio of 1:6, and stirred at 100 rpm for 6 h at 30 °C. After filtration, the precapsules were washed twice with deionized water, pre-frozen at -40 °C for 8 h, and then freeze-dried at -50 °C and 20 Pa under vacuum for 24 h to obtain berberine microcapsules.
[0037] The specific preparation method of Phellodendron bark flavonoid extract is as follows: The dried bark of Phellodendron bark was pulverized and passed through a 40-mesh sieve to obtain Phellodendron bark powder. The Phellodendron bark powder was mixed with a 50% ethanol aqueous solution at a solid-liquid ratio of 1:6 and extracted at 60℃ for 1 hour. After filtration, a flavonoid-rich solution was obtained. The flavonoid-rich solution was concentrated under reduced pressure at 40℃ and a vacuum degree of -0.08MPa to 20% of its original volume, and then spray-dried at an inlet air temperature of 140℃ and an outlet air temperature of 70℃ until the water content was 10% to obtain the Phellodendron bark flavonoid extract.
[0038] A method for preparing an antibacterial herbal facial mask sheet includes the following steps: S1. Mix the raw materials of the release layer, the liquid storage layer and the anti-evaporation layer evenly, open them once with an opening machine at a cylinder speed of 300 rpm and a feeding curtain speed of 1 m / min; then card them into a web with a carding machine at a doffer speed of 40 m / min and a cylinder to doffer linear speed ratio of 1.5:1 to obtain the release layer fiber web, the liquid storage layer fiber web and the anti-evaporation layer fiber web. S2. The release layer fiber mesh, the liquid storage layer fiber mesh and the anti-evaporation layer fiber mesh are laid sequentially from bottom to top, and then laid and stacked by a cross-laying machine to obtain a three-layer composite fiber mesh. S3. The three-layer composite fiber mesh is first pre-wetted at 5 bar and 20℃ once, and then subjected to double-sided gradient hydroentangling treatment: the release layer fiber mesh side is hydroentangled once at 40 bar, and the anti-evaporation layer fiber mesh side is hydroentangled twice at 80 bar. The hydroentangling head aperture is 0.08 mm, and the speed is 40 m / min. After hydroentangling, it is dried with hot air at 60℃ until the moisture content is 8%. Finally, it is cut according to the mask pattern to obtain the antibacterial herbal mask cloth.
[0039] Example 2 An antibacterial herbal facial mask sheet, comprising, from the inside out, a release layer, a liquid storage layer, and an anti-evaporation layer; The release layer comprises the following raw materials in parts by weight: 3 parts of phellodendron bark fiber, 4 parts of ultrafine viscose fiber, and 1.5 parts of berberine microcapsules; the areal density of the release layer is 12 g / m². The liquid storage layer comprises the following raw materials in parts by weight: 6 parts ultrafine viscose fiber, 2.5 parts liquid storage composition, and 1.5 parts lyocell fiber; the areal density of the liquid storage layer is 20 g / m². The vapor barrier layer comprises the following raw materials in parts by weight: 3 parts ultrafine viscose fiber and 7 parts lyocell fiber; the areal density of the vapor barrier layer is 12 g / m².
[0040] The fineness of the ultrafine viscose fiber is 0.67 dtex, and the fineness of the lyocell fiber is 1.5 dtex; the fiber cutting length of both ultrafine viscose fiber and lyocell fiber is 40 mm.
[0041] The reservoir composition consists of sodium carboxymethyl cellulose, flavonoid extract of Phellodendron bark, and aluminum chloride in a mass ratio of 5:4:0.08.
[0042] The specific preparation method of Phellodendron amurense-based fiber is as follows: The dried bark of Phellodendron amurense was pulverized and passed through a 60-mesh sieve to obtain Phellodendron amurense powder. The Phellodendron amurense powder was mixed with a 1.5% hydrochloric acid aqueous solution at a solid-liquid ratio of 1:12 and extracted at 70°C for 2 hours. After filtration, the residue was obtained. The residue was mixed with a 70% ethanol aqueous solution at a solid-liquid ratio of 1:9 and extracted at 65°C for 1.5 hours. After filtration, a secondary residue was obtained. The secondary residue was added to a 4wt% sodium hydroxide solution and boiled at 95°C for 2 hours. It was washed with deionized water until neutral, mechanically loosened, dried at 70°C until the moisture content was 10%, and cut to a length of 40 mm to obtain Phellodendron amurense-based fibers.
[0043] The specific preparation method of berberine microcapsules is as follows: Berberine hydrochloride was dissolved in acetate buffer (composed of 0.15 mol / L acetic acid solution and 0.15 mol / L sodium acetate solution in a 1:1 volume ratio) at a mass ratio of 1.5:100 to obtain the core solution; chitosan was dissolved in 1.5 wt% acetic acid solution at a mass ratio of 2.5:100 to obtain the chitosan solution; the core solution and chitosan solution were mixed at a volume ratio of 1:2 to obtain the inner phase; sodium alginate was dissolved in deionized water at a mass ratio of 2:100 to obtain the outer phase; the inner phase was then... The phase was dispersed by high-speed shearing at 8000 rpm for 10 min, and then added dropwise to the external phase at a rate of 1.5 mL / min to obtain precapsules. The precapsules were added to a coagulation bath (composed of calcium chloride, genipin and deionized water in a mass ratio of 4:0.2:100) at a mass ratio of 1:8, and stirred at 150 rpm for 7 h at 40 °C. After filtration, the mixture was washed twice with deionized water, pre-frozen at -60 °C for 10 h, and then freeze-dried at -55 °C and 20 Pa vacuum for 36 h to obtain berberine microcapsules.
[0044] The specific preparation method of Phellodendron bark flavonoid extract is as follows: The dried bark of Phellodendron bark was pulverized and passed through a 60-mesh sieve to obtain Phellodendron bark powder. The Phellodendron bark powder was mixed with a 70% ethanol aqueous solution at a solid-liquid ratio of 1:9 and extracted at 65℃ for 1.5 h. After filtration, a flavonoid-rich solution was obtained. The flavonoid-rich solution was concentrated under reduced pressure at 50℃ and a vacuum degree of -0.08 MPa to 25% of its original volume, and then spray-dried at an inlet air temperature of 160℃ and an outlet air temperature of 80℃ until the water content was 10% to obtain the Phellodendron bark flavonoid extract.
[0045] A method for preparing an antibacterial herbal facial mask sheet includes the following steps: S1. Mix the raw materials of the release layer, liquid storage layer and anti-evaporation layer evenly, open them twice with an opening machine at a cylinder speed of 500 rpm and a feeding curtain speed of 2 m / min; then card them into a web with a carding machine at a doffer speed of 50 m / min and a cylinder to doffer linear speed ratio of 2:1 to obtain the release layer fiber web, liquid storage layer fiber web and anti-evaporation layer fiber web. S2. The release layer fiber mesh, the liquid storage layer fiber mesh and the anti-evaporation layer fiber mesh are laid sequentially from bottom to top, and then laid and stacked by a cross-laying machine to obtain a three-layer composite fiber mesh. S3. The three-layer composite fiber mesh is first pre-wetted twice at 10 bar and 25°C, and then subjected to double-sided gradient hydroentangling: the release layer fiber mesh side is hydroentangled twice at 60 bar, and the anti-evaporation layer fiber mesh side is hydroentangled three times at 120 bar. The hydroentangling head aperture is 0.12 mm, and the machine speed is 50 m / min. After hydroentangling, it is dried with hot air at 80°C until the moisture content is 8%. Finally, it is cut according to the mask pattern to obtain the antibacterial herbal mask cloth.
[0046] Example 3 An antibacterial herbal facial mask sheet, comprising, from the inside out, a release layer, a liquid storage layer, and an anti-evaporation layer; The release layer comprises the following raw materials in parts by weight: 4 parts of phellodendron bark fiber, 5 parts of ultrafine viscose fiber, and 2 parts of berberine microcapsules; the areal density of the release layer is 18 g / m². The liquid storage layer comprises the following raw materials in parts by weight: 7 parts ultrafine viscose fiber, 3 parts liquid storage composition, and 2 parts lyocell fiber; the areal density of the liquid storage layer is 25 g / m². The vapor barrier layer comprises the following raw materials in parts by weight: 4 parts ultrafine viscose fiber and 8 parts lyocell fiber; the areal density of the vapor barrier layer is 15 g / m².
[0047] The fineness of the ultrafine viscose fiber is 1.1 dtex, and the fineness of the lyocell fiber is 1.7 dtex; the fiber cutting length of both ultrafine viscose fiber and lyocell fiber is 45 mm.
[0048] The reservoir composition consists of sodium carboxymethyl cellulose, flavonoid extract of Phellodendron bark, and aluminum chloride in a mass ratio of 6:5:0.1.
[0049] The specific preparation method of Phellodendron amurense-based fiber is as follows: The dried bark of Phellodendron amurense was pulverized and passed through an 80-mesh sieve to obtain Phellodendron amurense powder. The Phellodendron amurense powder was mixed with a 2% hydrochloric acid aqueous solution at a solid-liquid ratio of 1:15 and extracted at 80℃ for 3 hours. After filtration, the residue was obtained. The residue was mixed with an 80% ethanol aqueous solution at a solid-liquid ratio of 1:12 and extracted at 70℃ for 2 hours. After filtration, a secondary residue was obtained. The secondary residue was added to a 6wt% sodium hydroxide solution and boiled at 100℃ for 3 hours. It was washed with deionized water until neutral, mechanically loosened, dried at 80℃ to a moisture content of 10%, and cut to a length of 45 mm to obtain Phellodendron amurense-based fibers.
[0050] The specific preparation method of berberine microcapsules is as follows: Berberine hydrochloride was dissolved in acetate buffer (composed of 0.2 mol / L acetic acid solution and 0.2 mol / L sodium acetate solution in a volume ratio of 1:1.2) at a mass ratio of 2:100 to obtain the core solution; chitosan was dissolved in 2 wt% acetic acid solution at a mass ratio of 3:100 to obtain the chitosan solution; the core solution and chitosan solution were mixed at a volume ratio of 1:3 to obtain the inner phase; sodium alginate was dissolved in deionized water at a mass ratio of 3:100 to obtain the outer phase; the inner phase was then subjected to 14-day incubation at room temperature. The berberine microcapsules were dispersed by high-speed shearing at 0000 rpm for 15 min and then dropped into the external phase at a rate of 2 mL / min to obtain precapsules. The precapsules were added to a coagulation bath (composed of calcium chloride, genipin and deionized water in a mass ratio of 5:0.3:100) at a mass ratio of 1:10. The mixture was stirred at 200 rpm for 8 h at 50 °C. After filtration, the mixture was washed three times with deionized water, pre-frozen at -80 °C for 12 h, and then freeze-dried at -60 °C and 20 Pa under vacuum for 48 h to obtain berberine microcapsules.
[0051] The specific preparation method of Phellodendron bark flavonoid extract is as follows: The dried bark of Phellodendron bark was pulverized and passed through an 80-mesh sieve to obtain Phellodendron bark powder. The Phellodendron bark powder was mixed with an 80% ethanol aqueous solution at a solid-liquid ratio of 1:12 and extracted at 70℃ for 2 hours. After filtration, a flavonoid-rich solution was obtained. The flavonoid-rich solution was concentrated under reduced pressure at 60℃ and a vacuum degree of -0.08MPa to 30% of its original volume, and then spray-dried at an inlet air temperature of 180℃ and an outlet air temperature of 90℃ until the water content was 10% to obtain the Phellodendron bark flavonoid extract.
[0052] A method for preparing an antibacterial herbal facial mask sheet includes the following steps: S1. Mix the raw materials of the release layer, liquid storage layer and anti-evaporation layer evenly, open them twice with an opening machine at a cylinder speed of 600 rpm and a feeding curtain speed of 3 m / min; then card them into a web with a carding machine at a doffer speed of 60 m / min and a cylinder to doffer linear speed ratio of 2.5:1 to obtain the release layer fiber web, liquid storage layer fiber web and anti-evaporation layer fiber web. S2. The release layer fiber mesh, the liquid storage layer fiber mesh and the anti-evaporation layer fiber mesh are laid sequentially from bottom to top, and then laid and stacked by a cross-laying machine to obtain a three-layer composite fiber mesh. S3. The three-layer composite fiber mesh is first pre-wetted twice at 15 bar and 30℃, and then subjected to double-sided gradient hydroentangling: the release layer fiber mesh side is hydroentangled twice at 80 bar, and the anti-evaporation layer fiber mesh side is hydroentangled four times at 150 bar. The hydroentangling head aperture is 0.15 mm, and the machine speed is 60 m / min. After hydroentangling, it is dried with hot air at 90℃ until the moisture content is 8%. Finally, it is cut according to the mask pattern to obtain the antibacterial herbal mask cloth.
[0053] Comparative Example 1 This comparative example provides a mask sheet and its preparation method. The only difference from Example 2 is that: instead of setting a three-layer gradient structure, all raw materials are mixed to form a single-layer homogeneous mask sheet; the other types of raw materials, amounts, and preparation process parameters are completely consistent with Example 2.
[0054] Specifically: An antibacterial herbal facial mask sheet comprises the following raw materials in parts by weight: 3 parts of berberine-based fiber, 13 parts of ultrafine viscose fiber, 1.5 parts of berberine microcapsules, 2.5 parts of a liquid storage composition, and 8.5 parts of lyocell fiber; the surface density of the antibacterial herbal facial mask sheet is 44 g / m².
[0055] A method for preparing an antibacterial herbal facial mask sheet includes the following steps: S1. Mix all raw material components evenly, open them twice with an opening machine at a cylinder speed of 500 rpm and a feed curtain speed of 2 m / min; then card them into a web with a carding machine at a doffer speed of 50 m / min and a cylinder to doffer linear speed ratio of 2:1 to obtain a single-layer mixed fiber web. S2. The single-layer mixed fiber web is first pre-wetted twice at 10 bar and 25°C, and then subjected to double-sided gradient hydroentangling: two hydroentangling passes at 60 bar on one side and three hydroentangling passes at 120 bar on the other side, with a hydroentangling head aperture of 0.12 mm and a machine speed of 50 m / min. After hydroentangling, it is dried with hot air at 80°C until the moisture content is 8%. Finally, it is cut according to the mask pattern to obtain the antibacterial herbal mask cloth.
[0056] Comparative Example 2 This comparative example provides a mask fabric and its preparation method, which differs from Example 2 only in that: the phellodendron chinense fiber in the release layer is replaced with ultrafine viscose fiber; the other raw material types, amounts and preparation process parameters are completely consistent with Example 2.
[0057] Specifically: The release layer comprises the following raw materials in parts by weight: 7 parts ultrafine viscose fiber and 1.5 parts berberine microcapsules; the areal density of the release layer is 12 g / m².
[0058] Comparative Example 3 This comparative example provides a facial mask fabric and its preparation method. The only difference from Example 2 is that the berberine microcapsules in the release layer are replaced with berberine hydrochloride mixed powder; the other raw material types, amounts and preparation process parameters are completely consistent with Example 2.
[0059] The specific preparation method of the berberine hydrochloride mixed powder is as follows: Berberine hydrochloride was dissolved in an acetate buffer solution (composed of a 1:1 volume ratio of 0.15 mol / L acetic acid solution and 0.15 mol / L sodium acetate solution) at a mass ratio of 1.5:100 to obtain a berberine solution; chitosan was dissolved in a 1.5 wt% acetic acid solution at a mass ratio of 2.5:100 to obtain a chitosan solution; sodium alginate was dissolved in deionized water at a mass ratio of 2:100 to obtain a sodium alginate solution; the berberine solution, chitosan solution, and sodium alginate solution were mixed at a volume ratio of 1:2:5, stirred at 150 rpm for 7 h at 40 °C, pre-frozen at -60 °C for 10 h, and then freeze-dried at -55 °C and 20 Pa under vacuum for 36 h. The mixture was then ground through a 100-mesh sieve to obtain a mixed powder of berberine hydrochloride.
[0060] Comparative Example 4 This comparative example provides a facial mask fabric and its preparation method. The only difference from Example 2 is that the liquid storage composition consists of sodium carboxymethyl cellulose and flavonoid extract of Phellodendron bark in a mass ratio of 5.08:4; the other raw material types, amounts and preparation process parameters are completely consistent with Example 2.
[0061] Comparative Example 5 This comparative example provides a facial mask fabric and its preparation method. The only difference from Example 2 is that the liquid storage composition consists of sodium carboxymethyl cellulose and aluminum chloride in a mass ratio of 9:0.08; the other raw material types, amounts, and preparation process parameters are completely consistent with Example 2.
[0062] Comparative Example 6 This comparative example provides a mask fabric and its preparation method. The only difference from Example 2 is that in step S3, double-sided isobaric hydroentanglement is used instead of double-sided gradient hydroentanglement, that is, the same hydroentanglement pressure is used on the release layer side and the anti-evaporation layer side; the other raw material types, amounts and preparation process parameters are completely consistent with Example 2.
[0063] Specifically: S3. The three-layer composite fiber mesh is first pre-wetted twice at 10 bar and 25℃, and then subjected to double-sided isobaric hydroentangling: the release layer fiber mesh side is hydroentangled twice at 90 bar, and the anti-evaporation layer fiber mesh side is hydroentangled three times at 90 bar. The hydroentangling head aperture is 0.12mm, and the machine speed is 50m / min. After hydroentangling, it is dried with hot air at 80℃ until the moisture content is 8%. Finally, it is cut according to the mask pattern to obtain the antibacterial herbal mask cloth.
[0064] Performance verification The antibacterial herbal facial mask fabrics prepared in Examples 1-3 and Comparative Examples 1-6 were subjected to performance testing.
[0065] The specific testing items are as follows: (1) Liquid absorption rate (g / g) Take an antibacterial herbal mask sheet sample (10cm×10cm), dry it at 105℃ to constant weight, and record the mass as m0 (g); immerse the sample completely in simulated essence (prepared by 0.2wt% sodium hyaluronate, 5wt% glycerin and deionized water, 25℃) for 30min, remove it and hang it on a stainless steel rack to drip naturally for 60s, and record the mass as m1 (g); conduct 3 parallel tests for each group and take the average value.
[0066] The formula is: Absorption rate (g / g) = (m1-m0) / m0.
[0067] (2) Serum retention rate (30 min) The saturated antibacterial herbal mask sheet samples after the above absorption rate test (i.e., the samples after 60 seconds of dripping) were suspended in a constant temperature and humidity chamber at 37°C and 50% relative humidity. After 30 minutes, the weight was recorded as m2 (g). Each group was tested in parallel 3 times, and the average value was taken.
[0068] The liquid retention rate (%) is calculated using the formula: [(m2-m0) / (m1-m0)]×100%.
[0069] (3) Backside evaporation rate (30 min) After the absorbency test, the saturated antibacterial herbal mask sheet sample (i.e., the sample with a mass of m1 after 60 seconds of dripping) was attached to a 37℃ constant-temperature silicone simulated skin plate (release layer facing down), with the anti-evaporation layer / outer layer facing up, and exposed to an environment of 37℃ and 50% relative humidity. After 30 minutes, the mass was weighed and recorded as m3 (g). Each group was tested in triplicate, and the average value was taken. (Note: Comparative Example 1 is a single-layer homogeneous structure, with the low-pressure side of the spunlace material facing down attached to the skin plate and the high-pressure side facing up.) The formula is: Back evaporation rate (%) = [(m1-m3) / (m1-m0)] × 100%.
[0070] (4) Antibacterial rate (24h) Referring to GB / T 20944.3-2008 "Evaluation of Antimicrobial Properties of Textiles - Part 3: Shaking Method", the test strain was Staphylococcus aureus (… Staphylococcus aureus ATCC 6538) and Escherichia coli ( Escherichia coli (ATCC 8099).
[0071] Take 0.75g of antibacterial herbal facial mask sheet sample, cut it into small pieces, place it in a sterile Erlenmeyer flask, and add 70mL of 0.03mol / L PBS phosphate buffer (containing 1×10⁻⁶ test bacteria). 5 The cells were cultured at 24℃ and 150 rpm for 24 h with shaking (CFU / mL); the number of surviving colonies was counted using the plate count method.
[0072] Control sample setup: Pure viscose nonwoven fabric without any antibacterial components (area density of 44 g / m², fineness of 0.67 dtex, fiber length of 40 mm, hydroentangling process as in Example 2) was used as a uniform blank control sample; each group was tested in parallel 3 times and the average value was taken.
[0073] Calculated using the formula: Antibacterial rate (%) = [(C 对照 -C 样品 ) / C 对照 ]×100%; where C is the average number of colonies counted on the plate after 24 hours (CFU / mL).
[0074] The test results are shown in Table 1.
[0075] Table 1 Performance Verification Results The antibacterial herbal facial mask fabrics prepared in Examples 1-3 of this invention are superior to those in Comparative Examples 1-5 in all test indicators, with Example 2 showing the best performance.
[0076] Comparative Example 1: Compared with Example 2, the liquid absorption rate and liquid retention rate both decreased, the back-side evaporation rate increased, and the inhibition rates of Staphylococcus aureus and Escherichia coli both decreased. This indicates that the monolayer homogeneous structure cannot form a "release-storage-evaporation barrier" functional zone. The liquid storage composition is dispersed throughout the entire layer and cannot concentrate the liquid. Furthermore, there is no dense evaporation barrier layer to inhibit back-side evaporation, resulting in a comprehensive deterioration of all performance characteristics.
[0077] Comparative Example 2: Compared with Example 2, the antibacterial rates of Staphylococcus aureus and Escherichia coli both decreased, with the largest decrease among all comparative examples, while the changes in liquid absorption, liquid retention, and evaporation were relatively small. This indicates that the phellodendron chinense fiber provides the release layer with the intrinsic antibacterial activity of the fiber substrate, and is the main contributor to the high antibacterial rate of the mask fabric.
[0078] Comparative Example 3: Compared with Example 2, the antibacterial rates of Staphylococcus aureus and Escherichia coli both decreased. This indicates that when the berberine hydrochloride mixed powder does not have a core-shell coating structure, berberine hydrochloride will dissolve rapidly in a free state, resulting in severe initial burst release and insufficient active ingredients in the later stages, thus reducing its long-lasting antibacterial ability.
[0079] Comparative Example 4: Compared with Example 2, the liquid absorption rate and liquid retention rate both decreased significantly, the back-side evaporation rate increased significantly, while the antibacterial rate only decreased slightly. This indicates that Al³⁺ coordination crosslinking is the main framework for constructing a high-strength three-dimensional gel network in the liquid storage layer. After its removal, the thickening effect is only achieved by sodium carboxymethyl cellulose swelling and the hydrogen bonding assistance of berberine, which cannot maintain sufficient gel density, resulting in a significant deterioration in liquid retention capacity.
[0080] Comparative Example 5: Compared with Example 2, the decrease in physical properties was less than that of Comparative Example 4, but the decrease in antibacterial rate was significantly greater than that of Comparative Example 4. This indicates that the flavonoid extract of Phellodendron amurense plays a dual role: its polyphenolic hydroxyl groups form polyphenol-polysaccharide hydrogen bonds with sodium carboxymethyl cellulose, which helps to enhance gel elasticity; at the same time, its own polyphenolic antibacterial activity makes a significant contribution to the overall antibacterial performance, and the antibacterial ability decreases significantly after removal.
[0081] Comparative Example 6: Compared with Example 2, the back-side evaporation rate increased, while the liquid absorption rate and liquid retention rate decreased, and the antibacterial rate also decreased significantly. This indicates that the isobaric hydroentangling treatment caused the pores of the release layer to be over-compacted and the evaporation barrier layer to be insufficiently dense, resulting in the loss of the "loose inside and dense outside" asymmetric pore size gradient, and a simultaneous deterioration of both release efficiency and evaporation barrier capability.
[0082] This specific embodiment is merely an explanation of the present invention and is not intended to limit the invention. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they are within the scope of the claims of the present invention.
Claims
1. An antibacterial herbal facial mask sheet, characterized in that, From the inside out, it includes a release layer, a liquid storage layer, and an anti-evaporation layer; The release layer comprises the following raw materials in parts by weight: 2-4 parts of berberine-based fiber, 3-5 parts of ultrafine viscose fiber, and 1-2 parts of berberine microcapsules; The liquid storage layer comprises the following raw materials in parts by weight: 5-7 parts of ultrafine viscose fiber, 2-3 parts of liquid storage composition, and 1-2 parts of lyocell fiber; The vapor barrier layer comprises the following raw materials in parts by weight: 2-4 parts of ultrafine viscose fiber and 6-8 parts of lyocell fiber.
2. The antibacterial herbal facial mask sheet according to claim 1, characterized in that, The areal density of the release layer is 8-18 g / m²; the areal density of the liquid storage layer is 15-25 g / m²; and the areal density of the anti-evaporation layer is 8-15 g / m².
3. The antibacterial herbal facial mask sheet according to claim 1, characterized in that, The fineness of the ultrafine viscose fiber is 0.5-1.1 dtex; the fineness of the lyocell fiber is 1.0-1.7 dtex; and the fiber cutting length of both the ultrafine viscose fiber and the lyocell fiber is 35-45 mm.
4. The antibacterial herbal facial mask sheet according to claim 1, characterized in that, The preparation method of the phellodendron-based fiber is as follows: The dried bark of Phellodendron bark is crushed and sieved to obtain Phellodendron bark powder. The Phellodendron bark powder is added to hydrochloric acid aqueous solution for extraction, filtered, and the residue is obtained. The residue is added to ethanol aqueous solution for extraction, filtered, and a secondary residue is obtained. The secondary residue is boiled with alkali, washed with water, mechanically loosened, dried, and cut to obtain Phellodendron bark-based fiber.
5. The antibacterial herbal facial mask sheet according to claim 1, characterized in that, The preparation method of the berberine microcapsules is as follows: Berberine hydrochloride was dissolved in acetate buffer to obtain the core solution; chitosan was dissolved in acetate solution to obtain the chitosan solution; the core solution and chitosan solution were mixed to obtain the inner phase; sodium alginate was dissolved in deionized water to obtain the outer phase; the inner phase was dispersed uniformly by high-speed shearing and then added dropwise to the outer phase to obtain the precapsule; The pre-capsules were added to a coagulation bath and stirred to react. The mixture was then filtered, washed, and freeze-dried to obtain berberine microcapsules.
6. The antibacterial herbal facial mask sheet according to claim 5, characterized in that, The coagulation bath consists of calcium chloride, genipin, and deionized water in a mass ratio of 3-5:0.1-0.3:
100.
7. The antibacterial herbal facial mask sheet according to claim 1, characterized in that, The storage liquid composition consists of sodium carboxymethyl cellulose, flavonoid extract of Phellodendron bark, and metal ion coordinating agent in a mass ratio of 4-6:3-5:0.06-0.
1.
8. A method for preparing an antibacterial herbal facial mask sheet according to any one of claims 1-7, characterized in that, Includes the following steps: S1. Mix the raw materials of the release layer, the liquid storage layer and the anti-evaporation layer evenly, loosen them and comb them into a web to obtain the release layer fiber web, the liquid storage layer fiber web and the anti-evaporation layer fiber web. S2. From bottom to top, the release layer fiber mesh, the liquid storage layer fiber mesh and the anti-evaporation layer fiber mesh are laid in sequence to obtain a three-layer composite fiber mesh. S3. The three-layer composite fiber web is pre-wetted and subjected to double-sided gradient hydroentangling, then dried with hot air and cut to obtain an antibacterial herbal facial mask fabric.
9. The method for preparing the antibacterial herbal facial mask sheet according to claim 8, characterized in that, The parameters for the double-sided gradient hydroentangling treatment in step S3 include: hydroentangling pressure on the fiber web side of the release layer is 40-80 bar, hydroentangling pressure on the fiber web side of the anti-evaporation layer is 80-150 bar, hydroentangling head orifice diameter is 0.08-0.15 mm, and machine speed is 40-60 m / min; the drying temperature is 60-90℃, and drying is carried out until the moisture content is ≤8%.
10. The use of the antibacterial herbal mask sheet according to any one of claims 1-7 in the preparation of skin care masks, antibacterial dressings or acne care patch products.
