Collagen mask base material and preparation method thereof
Through plasma treatment, etherification reaction and microwave-ultrasound combined treatment, the binding strength of collagen and mask substrate is improved, the problem of collagen loss is solved, and the skin care effect of the mask is significantly improved.
Patent Information
- Application Number
- CN202510053765.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-14
- Publication Date
- 2025-02-21
AI Technical Summary
The binding force between the existing collagen mask substrate and the mask substrate is weak, which makes collagen easy to detach during use, reducing the skin care effect of the mask.
Modified mask substrate was treated by plasma, etherification was introduced to increase hydrophilic and lipophilic groups, followed by mixing with collagen solution and microwave-ultrasound combined to enhance binding.
It significantly improves the binding force between collagen and the mask substrate, enhances the moisturizing properties and skin care effects of the mask, and reduces the loss of collagen.
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Figure CN119488438A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of facial mask base materials, and in particular to a collagen facial mask base material and a preparation method thereof. Background Art
[0002] Collagen is one of the main components of the skin, with multiple functions such as moisturizing, repairing, and tightening. Adding collagen to the mask base material can significantly improve the skin care effect of the mask. Collagen molecules can closely combine with skin cells, providing long-lasting moisturizing and nourishing for the skin, while promoting the regeneration and repair of skin cells.
[0003] At present, the combination of collagen and mask substrate mostly adopts physical methods (such as dipping, spraying) or simple chemical methods (such as cross-linking reaction). Although these methods can achieve the combination of collagen and mask substrate, the binding force is often weak, which leads to the collagen easily detaching from the mask substrate during the use of the mask, especially when the mask is soaked in water, resulting in the loss of collagen and reducing the skin care effect of the mask. Summary of the invention
[0004] The present application provides a collagen mask substrate and a preparation method thereof to solve the following technical problem: how to improve the bonding force between collagen and the mask substrate.
[0005] In a first aspect, the present application provides a method for preparing a collagen mask substrate, the method comprising the following steps:
[0006] S1, subjecting the facial mask substrate to plasma treatment to obtain a modified facial mask substrate;
[0007] S2, subjecting the modified facial mask substrate to an etherification reaction with an etherifying agent to introduce hydrophilic and lipophilic groups into the structure of the modified facial mask substrate to obtain an etherified facial mask substrate;
[0008] S3, mixing the etherified facial mask base material with the collagen solution to obtain a mixed liquid;
[0009] S4, subjecting the mixed liquid to a microwave-ultrasound combined treatment, and then drying to obtain a collagen mask substrate.
[0010] Optionally, the plasma treatment includes the following parameters: the plasma gas is oxygen, the power is 10 to 30 W, the time is 30 s to 180 s, and the gas flow rate is 10 to 30 sccm.
[0011] Optionally, the etherifying agent consists of ethylene glycol butyl ether and ethylene oxide, and the mass ratio of the ethylene glycol butyl ether to the ethylene oxide is (3-8):1.
[0012] Optionally, the etherification reaction includes the following parameters: reaction temperature is 60-80° C., and time is 3-6 hours.
[0013] Optionally, the collagen solution consists of the following components, measured by mass: 1 to 5 parts of fish skin collagen, 1 to 2 parts of quaternized sodium alginate, 0.5 to 1 part of hyaluronic acid, 0.1 to 0.5 parts of citric acid, 0.1 to 0.5 parts of glutathione, 0.5 to 1 part of polyvinyl alcohol, 0.5 to 1 part of polysorbate and 85 to 96 parts of deionized water.
[0014] Optionally, the microwave-ultrasound combined treatment includes the following parameters: microwave power is 50-150 W, ultrasonic power is 200-300 W, and combined treatment time is 10 s to 90 s.
[0015] Optionally, the fiber raw material of the mask substrate is biological fiber, and the preparation method of the biological fiber comprises the following steps:
[0016] S101, inoculating xylindracenacetobacillus and bacillus cereus into a culture medium for fermentation, and performing laser irradiation-ultrasound combined treatment during the fermentation process to obtain a fermentation liquid containing fiber;
[0017] S102, taking out the cellulose in the fermentation liquid, washing and drying it, and obtaining the biofiber.
[0018] Optionally, the culture medium includes the following chemical components, measured by mass concentration: 10-20 g of glucose, 5-15 g of yeast extract, 5-10 g of peptone, 1.5-3 g of potassium dihydrogen phosphate, 0.5-1 g of caffeine, and 1000 mL of deionized water.
[0019] Optionally, the inoculation rate of the xylinacetobacter is 6-8%, and the inoculation rate of the Bacillus cereus is 10-20%; and / or,
[0020] The laser irradiation-ultrasound combined treatment includes the following parameters: ultrasonic power is 200-300W, laser irradiation intensity is 5-15mW / cm², and time is 15-30s / h; and / or,
[0021] The fermentation temperature is 28-30°C, and the fermentation time is 7-10 days; and / or,
[0022] The deposit number of the Gluconacetobacter xylinus is ATCC 23767; and / or,
[0023] The deposit number of the Bacillus cereus is CICC 23828.
[0024] In a second aspect, the present application provides a collagen mask substrate prepared by the preparation method of the collagen mask substrate described in any one of the first aspects.
[0025] The above technical solution provided by the embodiment of the present application has the following advantages compared with the prior art:
[0026] The present application provides a method for preparing a collagen mask substrate. First, the surface of the mask substrate is etched by plasma treatment to form conical or spherical protrusions, thereby increasing the surface roughness of the mask substrate, which helps to improve the binding force between the mask substrate and the collagen macromolecules; secondly, through etherification reaction, hydrophilic and lipophilic groups can be introduced into the structure of the mask substrate, and these groups can enhance the interaction between the mask substrate and the collagen, thereby improving the binding force; finally, through microwave-ultrasound combined treatment, the uniform distribution and penetration of collagen in the mask substrate is promoted, and the binding force between collagen and the mask substrate is enhanced. Thereby improving the binding force between collagen and the mask substrate. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.
[0028] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative labor.
[0029] Figure 1 A schematic flow chart of a method for preparing a collagen mask substrate provided in an embodiment of the present application. DETAILED DESCRIPTION
[0030] In order to make the purpose, technical solution and advantages of the embodiments of the present application clearer, the technical solution in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application.
[0031] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in this application can be purchased from the market or prepared by existing methods.
[0032] Figure 1 A schematic flow chart of a method for preparing a collagen mask substrate provided in an embodiment of the present application.
[0033] like Figure 1 As shown, the present application provides a method for preparing a collagen mask substrate, the method comprising the following steps:
[0034] S1, subjecting the facial mask substrate to plasma treatment to obtain a modified facial mask substrate;
[0035] It should be noted that plasma is an electrically neutral gas composed of electrons, ions, free radicals and excited molecules, in which high-speed electrons collide with gas molecules and atoms in the reaction chamber, transferring energy to these molecules and atoms. When the energy is large enough, these molecules and atoms will be excited or ionized to produce new ions, electrons, metastable particles or free radicals and other active species. These active species react with the surface of the mask substrate, or react with the functional groups opened on the surface of the material itself, thereby changing the properties of the surface of the material.
[0036] The plasma treatment operation process is as follows: Preparation stage: Place the mask substrate in the plasma generator to ensure good contact between the substrate and the plasma generator so that the plasma can act on the surface of the substrate. Parameter adjustment: Adjust the plasma parameters such as power, gas type, treatment time, etc. according to the material and modification requirements of the mask substrate. The adjustment of these parameters has an important influence on the effect of plasma treatment. Treatment stage: Start the plasma generator to form a thin plasma layer on the surface of the mask substrate. The high-energy particles in this plasma layer will continuously bombard the surface of the substrate, causing physical or chemical changes. Subsequent treatment: After the plasma treatment is completed, the mask substrate is removed from the plasma generator and necessary cleaning and drying are carried out to remove residual plasma components and impurities.
[0037] In some embodiments, the plasma treatment includes the following parameters: the plasma gas is oxygen, the power is 10 to 30 W, the time is 30 s to 180 s, and the gas flow rate is 10 to 30 sccm.
[0038] Plasma treatment can etch the surface of the mask substrate to form conical or spherical protrusions, thereby increasing the surface roughness. This increase in roughness helps to improve the binding force between the mask substrate and biomacromolecules such as collagen. At the same time, plasma treatment can introduce new functional groups (such as hydroxyl, carboxyl, etc.) to the surface of the mask substrate, which can form hydrogen bonds with water molecules, thereby increasing the hydrophilicity of the substrate. The increase in hydrophilicity helps the mask substrate to better absorb and retain moisture, and also helps the penetration and adsorption of active ingredients such as collagen. In addition, plasma treatment can produce strong chemical reactions and physical bombardment, thereby removing pollutants and impurities on the surface of the mask substrate. The removal of these pollutants and impurities helps to improve the purity and hygiene of the mask substrate, and also helps to improve its binding force with biomacromolecules such as collagen.
[0039] S2, subjecting the modified facial mask substrate to an etherification reaction with an etherifying agent to introduce hydrophilic and lipophilic groups into the structure of the modified facial mask substrate to obtain an etherified facial mask substrate;
[0040] It should be noted that, in the modification process of the mask substrate, the etherification reaction of the modified mask substrate with the etherifying agent is a key step. The purpose of this step is to introduce more hydrophilic and lipophilic groups into the structure of the mask substrate.
[0041] Hydrophilic groups can enhance the water absorption and water retention capacity of the mask substrate, making it fit the skin better and helping the skin absorb active ingredients. At the same time, introducing more hydrophilic groups not only improves the moisturizing properties of the mask substrate, but also facilitates its combination with active ingredients such as collagen. The presence of hydrophilic groups can increase the interaction between the mask substrate and collagen molecules, making the combination tighter and more stable. This helps the uniform distribution and release of collagen in the mask substrate, thereby improving the skin care effect of the mask.
[0042] At the same time, the introduction of lipophilic groups enables it to have a great improvement on oily skin and effectively remove facial oil. At the same time, due to the presence of lipophilic groups, the essence formula can be more flexible, oily ingredients can be added to the essence, and it can be stably absorbed by the mask base material.
[0043] In addition, the etherification reaction can change the chemical structure of the surface of the mask substrate, making it easier to interact with biomacromolecules such as collagen, thereby enhancing the binding force, helping the mask to better fit the skin and release active ingredients. The etherification reaction can lead to changes in the surface morphology of the mask substrate, forming a rougher surface, which helps to increase the friction with the skin and make the mask less likely to slip. In addition, the etherification reaction can make the chemical structure of the mask substrate more stable, thereby improving its weather resistance, heat resistance, and chemical corrosion resistance.
[0044] In some embodiments, the etherifying agent is composed of ethylene glycol butyl ether and ethylene oxide, and the mass ratio of the ethylene glycol butyl ether to the ethylene oxide is (3-8):1.
[0045] Ethylene glycol butyl ether is a green and environmentally friendly solvent with dual characteristics of hydrophilicity and hydrophobicity. The ether bond in its molecular structure is lipophilic, while the hydroxyl group is hydrophilic. This dual characteristic makes ethylene glycol butyl ether an effective ingredient in the etherification reaction, which can introduce hydrophilic groups and maintain a certain hydrophobic balance. In the etherification reaction, the hydroxyl group of ethylene glycol butyl ether can react with the hydroxyl group or other active groups in the mask substrate to form a new ether bond, thereby introducing the hydrophilic group into the mask substrate.
[0046] Ethylene oxide is an active compound, and the epoxy group in its molecule can react with the hydroxyl group in the mask base material to form an ether bond. This reaction can not only introduce hydrophilic groups, but also increase the cross-linking degree of the mask base material, thereby improving its stability and durability.
[0047] In addition, ethylene oxide can also copolymerize with ethylene glycol butyl ether to form an etherifying agent with a more complex structure, further enriching the performance of the mask substrate. The mass ratio of ethylene glycol butyl ether to ethylene oxide is selected in the range of (3-8):1. This ratio is intended to balance the amount of hydrophilic and lipophilic groups introduced to meet the dual requirements of the mask substrate for moisturizing performance and stability. By adjusting this ratio, the performance of the mask substrate can be optimized to make it more suitable for different skin types and usage environments.
[0048] In some embodiments, the etherification reaction includes the following parameters: reaction temperature is 60-80° C., and time is 3-6 hours.
[0049] S3, mixing the etherified facial mask base material with the collagen solution to obtain a mixed liquid;
[0050] In some embodiments, the collagen solution is composed of the following components, measured by mass: 1 to 5 parts of fish skin collagen, 1 to 2 parts of quaternized sodium alginate, 0.5 to 1 part of hyaluronic acid, 0.1 to 0.5 parts of citric acid, 0.1 to 0.5 parts of glutathione, 0.5 to 1 part of polyvinyl alcohol, 0.5 to 1 part of polysorbate and 85 to 96 parts of deionized water.
[0051] In the process of mixing the mask base material and the collagen liquid, the various components of the collagen liquid play an important role, as follows:
[0052] Fish skin collagen: As the main source of collagen, fish skin collagen has the effect of deeply moisturizing the skin, increasing skin elasticity, and improving fine lines and wrinkles. It can be closely combined with the mask base material to provide rich collagen nutrition for the skin and promote skin firming and repair.
[0053] Quaternized sodium alginate: Quaternized sodium alginate is a natural polysaccharide extracted from seaweed, which has excellent moisturizing and repairing properties. It can form a protective film on the skin surface to prevent moisture loss and enhance the skin's barrier function. After combining with collagen, it can further improve the moisturizing and fit of the mask, keeping the skin moisturized and soft. In addition, quaternized sodium alginate has significant antibacterial properties and can effectively kill or inhibit the growth of a variety of bacteria.
[0054] Hyaluronic acid: Hyaluronic acid (HA), also known as hyaluronic acid, is a linear, naturally occurring polysaccharide that belongs to the class of glycosaminoglycan biological compounds and is widely found in the epithelium and connective tissue of vertebrates. Due to its high molecular weight and unique biochemical and mechanical properties, hyaluronic acid can enhance the connection between collagen molecules, forming a tighter network structure, thereby improving its binding force with the mask substrate. At the same time, hyaluronic acid can provide lasting moisture to the skin, improve the physiological conditions of the skin, provide a superior external environment for the synthesis of dermal collagen and elastic fibers, strengthen the supply of nutrients, and achieve the effect of skin care and beauty.
[0055] Citric acid: As a buffer and acid-base regulator, citric acid can adjust the pH value of the mask, making it gentler and safer. At the same time, citric acid can also accelerate the renewal of keratin, promote the exfoliation of melanin in the skin, and help improve dark spots and roughness of the skin. After combining with collagen, it can further enhance the whitening and moisturizing effects of the mask.
[0056] Glutathione: Glutathione is a highly effective antioxidant that can remove free radicals in the body and protect cells from oxidative damage. It can also inhibit the formation of melanin and accelerate the decomposition of melanin, thereby promoting skin whitening. After combining with collagen, it can form a dual barrier of antioxidant and moisturizing to protect the skin from damage by the external environment.
[0057] Polyvinyl alcohol: As a film-forming agent, polyvinyl alcohol has the function of bonding and film-forming. It can improve the adhesion and fit of the mask, making the collagen liquid more evenly distributed on the mask base. At the same time, polyvinyl alcohol can also enhance the elasticity and toughness of the mask, improving the use experience of the mask.
[0058] Polysorbate: Polysorbate is an emulsifier that can improve the texture and stability of the mask. It can make the components of the collagen solution more evenly dispersed in the mask base material, improving the permeability and absorption of the mask. At the same time, polysorbate can also enhance the moisturizing and nourishing properties of the mask, making the skin softer and smoother.
[0059] S4, subjecting the mixed liquid to a microwave-ultrasound combined treatment, and then drying to obtain a collagen mask substrate.
[0060] It should be noted that microwaves and ultrasound differ in the properties of activation energy. When used together, they can play their respective advantages in improving heating and energy transfer. Microwaves heat materials mainly through dipole rotation and ion conduction mechanisms, and have the characteristics of strong penetration, uniform heating, and fast speed. Ultrasound processes materials through mechanisms such as cavitation, mechanical effects, and chemical effects, which can promote material exchange and reaction rate.
[0061] In the production process of collagen mask, the mixed liquid is subjected to microwave-ultrasound combined treatment and then dried to obtain a mask base material with excellent performance and stability. This mask base material not only has better moisturizing and functionality, but also can improve the bonding strength and uniformity between collagen and the mask base material.
[0062] In some embodiments, the microwave-ultrasound combined treatment includes the following parameters: microwave power is 50-150 W, ultrasonic power is 200-300 W, and combined treatment time is 10 s to 90 s.
[0063] Microwave-ultrasound combined treatment can utilize the mechanical effect and stirring action of ultrasound to promote the mixing and uniform distribution of the components in the collagen liquid. This helps to improve the uniformity of the combination of the mask base material and collagen. At the same time, it improves permeability: the penetrating power of microwaves can make it easier for the functional components in the collagen liquid to penetrate into the mask base material, while the cavitation effect of ultrasound can further promote the diffusion and distribution of these components in the base material. This helps to improve the moisturizing and functionality of the mask. In addition, microwave-ultrasound combined treatment can also change the molecular structure and arrangement of the collagen liquid, making it more conducive to combining with the mask base material. This structural change helps to improve the elasticity and toughness of the mask.
[0064] In some embodiments, the fiber raw material of the mask substrate is biological fiber, and the preparation method of the biological fiber comprises the following steps:
[0065] S101, inoculating xylindracenacetobacillus and bacillus cereus into a culture medium for fermentation, and performing laser irradiation-ultrasound combined treatment during the fermentation process to obtain a fermentation liquid containing fiber;
[0066] S102, taking out the cellulose in the fermentation liquid, washing and drying it, and obtaining the biofiber.
[0067] When biofiber is selected as the fiber raw material of the mask substrate, the biofiber mask substrate has good wet flexibility, water absorption and water retention, and contains rich hydrophilic groups, which has many advantages, as follows:
[0068] (1) Good biocompatibility. The ingredients of biofiber masks are natural and mild, and have good biocompatibility with human skin. This means that biofiber masks can easily fit the skin, are not likely to cause allergies or irritation, and are suitable for people of all skin types. This good biocompatibility provides a good foundation for the combination of biofiber and collagen, allowing the two to interact more effectively.
[0069] (2) Strong permeability. The fiber structure of the biofiber mask is compact and soft, with excellent breathability and fit. When applied to the face, the biofiber mask can closely fit the skin texture, forming a thin and breathable film. This high degree of fit allows the collagen in the mask to more easily penetrate into the deep layers of the skin, improving the skin's absorption efficiency of nutrients.
[0070] (3) Promote collagen absorption. Biofiber masks not only have good permeability, but also promote the skin's absorption of collagen. Collagen is an important component of the skin, which has the function of maintaining skin elasticity, moisture and radiance. The fiber structure in the biofiber mask helps to evenly release collagen to the skin surface and send it into the deep layers of the skin through penetration, thereby enhancing the skin's elasticity and firmness.
[0071] (4) Moisturizing and nourishing. Biofiber masks have strong water absorption and can fully absorb essence and release it evenly onto the skin surface. This allows the mask to provide sufficient moisture and nutrition to the skin during application, helping the skin to remain moisturized and nourished. At the same time, the collagen in the biofiber mask can also provide additional nourishment and moisturizing effects to the skin, making it more hydrated and smooth.
[0072] (5) Promote skin repair and regeneration. The ingredients in the biofiber mask can help soothe skin discomfort, relieve redness, swelling, sensitivity and other problems. At the same time, it can also promote skin self-repair and regeneration, and improve skin texture and gloss. Collagen, as one of the important components of the skin, also has the function of promoting skin repair and regeneration. Therefore, the combination of biofiber mask and collagen can further enhance this effect, making the skin healthier and younger.
[0073] The present application embodiment can utilize the complementary advantages of xyloglucanacetobacter and Bacillus cereus to achieve the synthesis of complex compounds and reduce the metabolic burden, thereby increasing the yield of bacterial cellulose by co-culturing xyloglucanacetobacter and Bacillus cereus. Studies have found that acetoin and 2,3-butanediol produced by Bacillus cereus are key factors in increasing the yield of bacterial cellulose. These two substances can increase the specific activity of acetoin dehydrogenase and the content of adenosine triphosphate (ATP) and acetyl-CoA, thereby promoting the growth and energy supply of xyloglucanacetobacter.
[0074] At the same time, co-cultivation can increase the structural density of bacterial cellulose, making it tougher and more durable. Moreover, through co-cultivation, the crystallinity of bacterial cellulose is improved, which helps to improve its physical and chemical properties, such as strength, heat resistance and chemical corrosion resistance. In addition, co-cultivation can also improve the mechanical properties of bacterial cellulose, such as tensile strength and elongation at break, making it more suitable for application areas such as facial mask substrates.
[0075] In some embodiments, the culture medium includes the following chemical components, measured by mass concentration: 10-20 g glucose, 5-15 g yeast extract, 5-10 g peptone, 1.5-3 g potassium dihydrogen phosphate, 0.5-1 g caffeine, and 1000 mL deionized water.
[0076] Adding the synergistic factor caffeine to the culture medium can help increase the production of bacterial cellulose. The mechanism of action of caffeine is to inhibit the activity of phosphodiesterase (PDE-A) and increase cyclic guanosine monophosphate (c-di-GMP), which is an activator of cellulose synthase, thereby increasing cellulose production.
[0077] In some embodiments, the inoculation rate of the xylinacetobacter is 6-8%, and the inoculation rate of the Bacillus cereus is 10-20%; and / or,
[0078] The laser irradiation-ultrasound combined treatment includes the following parameters: ultrasonic power is 200-300W, laser irradiation intensity is 5-15mW / cm², and time is 15-30s / h; and / or,
[0079] The fermentation temperature is 28-30°C, and the fermentation time is 7-10 days; and / or,
[0080] The deposit number of the Gluconacetobacter xylinus is ATCC 23767; and / or,
[0081] The deposit number of the Bacillus cereus is CICC 23828.
[0082] Xylindracenacetobacillus and Bacillus cereus are inoculated into a culture medium for fermentation culture, and laser irradiation-ultrasound combined treatment is performed during the fermentation process. The time of laser irradiation-ultrasound combined treatment is 15 to 30 s / h, that is, laser irradiation-ultrasound combined treatment is required for 15 to 30 s for every 1 hour of fermentation time.
[0083] Ultrasonic treatment can produce tiny cavitation effects and mechanical vibrations, which can stimulate bacterial cells and promote their metabolism and growth rate. And through ultrasonic treatment, the fermentation environment can be optimized, so that the bacteria can obtain better nutrition and growth conditions, thereby enhancing their reproductive capacity. At the same time, ultrasonic treatment can enhance the material exchange in the fermentation broth, including the diffusion of oxygen, nutrients and metabolites, which helps the bacteria to better utilize nutrients and improve fermentation efficiency. In addition, ultrasonic treatment can destroy the cell wall of the bacteria and release enzymes and other active substances in the cells, which can participate in the fermentation process and improve the purity and quality of the product.
[0084] As a non-contact energy transfer method, laser has unique physical properties, such as coherence, directionality and monochromaticity. These properties allow laser to act precisely on the target area without significantly affecting the surrounding environment. In the biological field, laser has been widely used to stimulate cell growth, induce gene expression, and promote metabolic processes.
[0085] When laser light is irradiated on fermentation liquid containing fiber synthase, its energy can be absorbed by the enzyme molecules. This energy absorption can trigger physical processes such as vibration, rotation or electronic transition inside the enzyme molecules, thereby changing the conformation and activity state of the enzyme molecules. In particular, laser light can activate the active sites of fiber synthase, which are usually the key areas on the enzyme molecules responsible for binding to the substrate and catalyzing the reaction.
[0086] The activation of active sites can accelerate the interaction between enzymes and substrates and improve catalytic efficiency. Therefore, under laser irradiation, the activity of fiber synthase is significantly improved, thereby accelerating the synthesis rate of cellulose. In this process, laser not only improves the catalytic efficiency of the enzyme, but also promotes the effective contact and reaction between the enzyme and the substrate, further increasing the yield of cellulose.
[0087] Based on a general inventive concept, the present application provides a collagen mask substrate prepared by the method described in any one of the above embodiments.
[0088] The collagen mask base material provided in the embodiments of the present application includes the following forms of collagen in the mask base material:
[0089] (1) Penetration and filling effect. During the microwave-ultrasound combined treatment process, the collagen liquid can further penetrate into the tiny pores or fiber gaps of the mask base. This penetration and filling effect not only strengthens the structure of the mask base, but also improves its moisturizing performance and fit. The filling of collagen makes the mask base tighter and reduces water loss, thus ensuring that the skin can obtain a long-lasting moisturizing effect when applying the mask.
[0090] (2) Physical adsorption or chemical bonding. After plasma treatment and etherification reaction, more active groups are introduced on the surface or inside of the mask substrate, which can physically adsorb or chemically bond with the collagen molecules in the collagen solution. This combination ensures that collagen can be evenly distributed in the mask substrate, providing comprehensive moisturizing and nourishing effects for the skin. The combination of physical adsorption and chemical bonding also enhances the interaction between collagen and the mask substrate, making the mask fit the skin better when applied and less likely to slip off.
[0091] (3) Cross-linking and curing. Using hyaluronic acid as a cross-linking agent and through an etherification reaction, a stable chemical bond can be formed between collagen and the mask base material. This form of cross-linking and curing not only improves the stability and durability of the collagen mask base material, but also enhances its moisturizing and nourishing effects. Cross-linking and curing makes the collagen molecules in the mask base material more tightly combined, reducing water loss, while improving the elasticity and toughness of the mask, making it more suitable for the needs of different skin types and usage environments.
[0092] At the same time, the collagen mask substrate provided in the embodiment of the present application can be used alone after absorbing water, or combined with essence. Users can choose the appropriate usage method according to their skin needs and skin care goals, and enjoy a more personalized and efficient skin care experience.
[0093] On the one hand, when the collagen mask substrate provided in the embodiment of the present application is used alone, it only needs to be soaked in an appropriate amount of water, and it can be applied to the face after it fully absorbs water. This method is easy to operate, does not require additional essence or skin care products, and is very suitable for use when busy or traveling. At the same time, the collagen mask substrate itself is rich in collagen and has good moisturizing properties. After absorbing water, the mask can fit the facial skin closely, provide a lasting moisturizing effect for the skin, and improve problems such as dry skin and tightness. In addition, for users with good skin condition or only basic moisturizing, using the collagen mask substrate alone is enough to meet daily skin care needs.
[0094] On the other hand, the collagen mask substrate provided in the embodiment of the present application can be used in combination with an essence to further enhance the efficacy of the mask. The active ingredients in the essence can penetrate deep into the skin and work together with collagen to improve various skin problems, such as fine lines, dullness, sagging, etc. At the same time, the essence has multiple functions, such as whitening, anti-wrinkle, repair, etc. Users can choose the appropriate essence and use it in combination with the collagen mask substrate according to their skin needs and skin care goals to achieve a personalized skin care plan.
[0095] The present application will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are intended only to illustrate the present application and are not intended to limit the scope of the present application. The experimental methods for which specific conditions are not specified in the following examples are usually measured according to industry standards. If there is no corresponding industry standard, then the conditions recommended by the manufacturer are followed.
[0096] Example 1
[0097] like Figure 1 As shown, this embodiment provides a method for preparing a collagen mask substrate, and the method may include the following steps:
[0098] S11, subjecting the facial mask substrate to plasma treatment to obtain a modified facial mask substrate;
[0099] The plasma treatment includes the following parameters: the plasma gas is oxygen, the power is 20 W, the time is 60 s, and the gas flow rate is 20 sccm;
[0100] The fiber raw material of the mask substrate is biological fiber, and the preparation method of the biological fiber includes the following steps: S1101, inoculating gluconic acid acetobacter and bacillus cereus into a culture medium for fermentation culture, and performing laser irradiation-ultrasound combined treatment during the fermentation culture to obtain a fermentation liquid containing fiber; S1102, taking out the cellulose in the fermentation liquid, and then washing and drying it to obtain the biological fiber.
[0101] Among them, the culture medium includes the following chemical components, measured by mass concentration: 15g glucose, 10g yeast extract, 7g peptone, 2g potassium dihydrogen phosphate, 0.7g caffeine, and 1000mL deionized water; the inoculation rate of the xylinobacter is 7%, and the inoculation rate of the cereus is 15%; the laser irradiation-ultrasound combined treatment includes the following parameters: the ultrasonic power is 250W, the irradiation intensity of the laser irradiation is 10mW / cm², and the time is 20s / h; the fermentation culture temperature is 28°C, and the fermentation culture time is 10d; the preservation number of the xylinobacter is ATCC 23767; the preservation number of the cereus is CICC 23828.
[0102] S21, mixing the modified facial mask substrate with an etherifying agent for an etherification reaction, so as to introduce hydrophilic and lipophilic groups into the structure of the modified facial mask substrate to obtain an etherified facial mask substrate;
[0103] Wherein, the etherifying agent is composed of ethylene glycol butyl ether and ethylene oxide, and the mass ratio of the ethylene glycol butyl ether to the ethylene oxide is 5:1;
[0104] The etherification reaction includes the following parameters: reaction temperature is 70°C, time is 4h;
[0105] S31, mixing the etherified facial mask base material with the collagen solution to obtain a mixed liquid;
[0106] Wherein, the collagen solution is composed of the following components, measured by mass: 4 parts of fish skin collagen (model QN0534 Biolab), 1.5 parts of quaternized sodium alginate, 1 part of hyaluronic acid (small molecule level, 99% purity), 0.3 parts of citric acid, 0.3 parts of glutathione (purity of 99%, molecular formula C10H17NO6S2), 0.8 parts of polyvinyl alcohol (straight chain PVA0588), 0.6 parts of polysorbate (Tween 80) and 91.5 parts of deionized water;
[0107] The preparation method of the quaternized sodium alginate is as follows: dissolve sodium alginate (Shanghai Aladdin Biochemical Technology Co., Ltd., viscosity 200±20 mPa·s) in deionized water and stir thoroughly until completely dissolved, add 2,3-epoxypropyltrimethylammonium chloride and stir thoroughly, place the reaction in a 60°C stirrer in the dark for 24 hours. Adjust the pH value to 7 as follows, and then place it at room temperature. Add excess ethanol for precipitation, collect the product and dry it to obtain quaternized sodium alginate.
[0108] S41, subjecting the mixed liquid to a microwave-ultrasound combined treatment, and then drying to obtain a collagen mask substrate.
[0109] The microwave-ultrasound combined treatment includes the following parameters: microwave power is 100W, ultrasonic power is 250W, and combined treatment time is 60s.
[0110] Example 2
[0111] This embodiment provides a method for preparing a collagen mask substrate, which may include the following steps:
[0112] S11, subjecting the facial mask substrate to plasma treatment to obtain a modified facial mask substrate;
[0113] The plasma treatment includes the following parameters: the plasma gas is oxygen, the power is 10 W, the time is 180 s, and the gas flow rate is 10 sccm;
[0114] The fiber raw material of the mask substrate is biological fiber, and the preparation method of the biological fiber includes the following steps: S1101, inoculating gluconic acid acetobacter and bacillus cereus into a culture medium for fermentation culture, and performing laser irradiation-ultrasound combined treatment during the fermentation culture to obtain a fermentation liquid containing fiber; S1102, taking out the cellulose in the fermentation liquid, and then washing and drying it to obtain the biological fiber.
[0115] Among them, the culture medium includes the following chemical components, measured by mass concentration: 10g glucose, 5g yeast extract, 5g peptone, 1.5g potassium dihydrogen phosphate, 0.5g caffeine, and 1000mL deionized water; the inoculation rate of the xylinobacter is 6%, and the inoculation rate of the cereus is 10%; the laser irradiation-ultrasound combined treatment includes the following parameters: the ultrasonic power is 200W, the irradiation intensity of the laser irradiation is 5mW / cm², and the time is 30s / h; the fermentation culture temperature is 28°C, and the fermentation culture time is 7d; the preservation number of the xylinobacter is ATCC 23767; the preservation number of the cereus is CICC 23828.
[0116] S21, mixing the modified facial mask substrate with an etherifying agent for an etherification reaction, so as to introduce hydrophilic and lipophilic groups into the structure of the modified facial mask substrate to obtain an etherified facial mask substrate;
[0117] Wherein, the etherifying agent is composed of ethylene glycol butyl ether and ethylene oxide, and the mass ratio of the ethylene glycol butyl ether to the ethylene oxide is 3:1;
[0118] The etherification reaction includes the following parameters: reaction temperature is 60°C, time is 6h;
[0119] S31, mixing the etherified facial mask base material with the collagen solution to obtain a mixed liquid;
[0120] Wherein, the collagen solution is composed of the following components, measured by mass: 1 part of fish skin collagen (model QN0534 Biolab), 1 part of quaternized sodium alginate, 0.6 parts of hyaluronic acid (small molecule level, 99% purity), 0.2 parts of citric acid, 0.2 parts of glutathione (purity of 99%, molecular formula C10H17NO6S2), 0.5 parts of polyvinyl alcohol (straight chain PVA0588), 0.5 parts of polysorbate (Tween 80) and 96 parts of deionized water;
[0121] The preparation method of the quaternized sodium alginate is as follows: dissolve sodium alginate (Shanghai Aladdin Biochemical Technology Co., Ltd., viscosity 200±20 mPa·s) in deionized water and stir thoroughly until completely dissolved, add 2,3-epoxypropyltrimethylammonium chloride and stir thoroughly, place the reaction in a 60°C stirrer in the dark for 24 hours. Adjust the pH value to 7 as follows, and then place it at room temperature. Add excess ethanol for precipitation, collect the product and dry it to obtain quaternized sodium alginate.
[0122] S41, subjecting the mixed liquid to a microwave-ultrasound combined treatment, and then drying to obtain a collagen mask substrate.
[0123] The microwave-ultrasound combined treatment includes the following parameters: microwave power is 50W, ultrasonic power is 200W, and combined treatment time is 90s.
[0124] Example 3
[0125] The present application provides a method for preparing a collagen mask substrate, which may include the following steps:
[0126] S11, subjecting the facial mask substrate to plasma treatment to obtain a modified facial mask substrate;
[0127] The plasma treatment includes the following parameters: the plasma gas is oxygen, the power is 30 W, the time is 30 s, and the gas flow rate is 30 sccm;
[0128] The fiber raw material of the mask substrate is biological fiber, and the preparation method of the biological fiber includes the following steps: S1101, inoculating gluconic acid acetobacter and bacillus cereus into a culture medium for fermentation culture, and performing laser irradiation-ultrasound combined treatment during the fermentation culture to obtain a fermentation liquid containing fiber; S1102, taking out the cellulose in the fermentation liquid, and then washing and drying it to obtain the biological fiber.
[0129] Among them, the culture medium includes the following chemical components, measured by mass concentration: 20g glucose, 15g yeast extract, 10g peptone, 3g potassium dihydrogen phosphate, 1g caffeine, and 1000mL deionized water; the inoculation rate of the xylinobacter is 8%, and the inoculation rate of the cereus is 20%; the laser irradiation-ultrasound combined treatment includes the following parameters: the ultrasonic power is 300W, the irradiation intensity of the laser irradiation is 15mW / cm², and the time is 15s / h; the fermentation culture temperature is 28°C, and the fermentation culture time is 7d; the preservation number of the xylinobacter is ATCC 23767; the preservation number of the cereus is CICC 23828.
[0130] S21, mixing the modified facial mask substrate with an etherifying agent for an etherification reaction, so as to introduce hydrophilic and lipophilic groups into the structure of the modified facial mask substrate to obtain an etherified facial mask substrate;
[0131] Wherein, the etherifying agent is composed of ethylene glycol butyl ether and ethylene oxide, and the mass ratio of the ethylene glycol butyl ether to the ethylene oxide is 8:1;
[0132] The etherification reaction includes the following parameters: reaction temperature is 80°C, time is 3h;
[0133] S31, mixing the etherified facial mask base material with the collagen solution to obtain a mixed liquid;
[0134] Wherein, the collagen solution is composed of the following components, measured by mass: 5 parts of fish skin collagen (model QN0534 Biolab), 2 parts of quaternized sodium alginate, 1 part of hyaluronic acid (small molecule level, 99% purity), 0.5 parts of citric acid, 0.5 parts of glutathione (purity of 99%, molecular formula C10H17NO6S2), 1 part of polyvinyl alcohol (straight chain PVA0588), 1 part of polysorbate (Tween 80) and 89 parts of deionized water;
[0135] The preparation method of the quaternized sodium alginate is as follows: dissolve sodium alginate (Shanghai Aladdin Biochemical Technology Co., Ltd., viscosity 200±20 mPa·s) in deionized water and stir thoroughly until completely dissolved, add 2,3-epoxypropyltrimethylammonium chloride and stir thoroughly, place the reaction in a 60°C stirrer in the dark for 24 hours. Adjust the pH value to 7 as follows, and then place it at room temperature. Add excess ethanol for precipitation, collect the product and dry it to obtain quaternized sodium alginate.
[0136] S41, subjecting the mixed liquid to a microwave-ultrasound combined treatment, and then drying to obtain a collagen mask substrate.
[0137] The microwave-ultrasound combined treatment includes the following parameters: microwave power is 150W, ultrasonic power is 300W, and combined treatment time is 10s.
[0138] Comparative Example 1
[0139] This comparative example is modified as follows based on Example 1:
[0140] The mask substrate is not subjected to plasma treatment in step S11.
[0141] Comparative Example 2
[0142] This comparative example is modified as follows based on Example 1:
[0143] The mask base material does not undergo etherification reaction in step S21.
[0144] Comparative Example 3
[0145] This comparative example is modified as follows based on Example 1:
[0146] In step S31, hyaluronic acid is not added to the collagen solution.
[0147] Comparative Example 4
[0148] This comparative example is modified as follows based on Example 1:
[0149] In step S41, the microwave-ultrasound combined treatment includes the following parameters: microwave power is 100 W, ultrasonic power is 250 W, and the combined treatment time is 5 s.
[0150] Comparative Example 5
[0151] This comparative example is modified as follows based on Example 1:
[0152] In step S31, no quaternized sodium alginate is added to the collagen solution.
[0153] Comparative Example 6
[0154] This comparative example is modified as follows based on Example 1:
[0155] In step S41, the microwave-ultrasound combined treatment is not performed.
[0156] Comparative Example 7
[0157] This comparative example is modified as follows based on Example 1:
[0158] In step S41, microwave treatment is performed alone.
[0159] Comparative Example 8
[0160] This comparative example is modified as follows based on Example 1:
[0161] Ultrasonic treatment is performed separately in step S41.
[0162] Comparative Example 9
[0163] The preparation method of the collagen mask substrate of this comparative example is:
[0164] The mask base material is directly immersed in the collagen solution, and then dried to obtain the collagen mask base material;
[0165] Wherein, the collagen solution is composed of the following components, measured by mass: 5 parts of fish skin collagen (model QN0534 Biolab) and 95 parts of deionized water.
[0166] The mask substrates obtained in Examples 1 to 3 and Comparative Examples 1 to 9 were subjected to performance tests, and the results are shown in Table 1. The test standard for surface density (g / m2) is GB / T24218-2010, the test standard for air permeability is GB / T5453-2007, and the calculation formula for liquid holdup is: liquid holdup = (m2-m1) / m1 × 100%, m1 is the initial weight of the sample, and m2 is the final weight of the sample after being immersed in deionized water for 10 seconds and suspended for 1 minute. The test standard for wet breaking strength is GB / T6529-2008.
[0167] Table 1 Properties of the mask substrates obtained in Examples 1 to 3 and Comparative Examples 1 to 9
[0168]
[0169] It can be seen from Table 1 that the surface density of the collagen mask substrate obtained in Examples 1 to 3 of the present application is 42.5 to 43.5 g / m2, the liquid holding rate is ≥1490%, the air permeability is ≥2750 mm / s, and the wet breaking strength is ≥31.5N.
[0170] The degree of binding between the collagen in the collagen mask substrate obtained in Examples 1 to 3 and Comparative Examples 1 to 9 and the mask substrate is determined, and the results are shown in Table 2. The specific determination method is as follows: the collagen in the collagen mask substrate is separated from the mask substrate by enzymatic hydrolysis, and then the content of the separated collagen is determined to obtain the original collagen content W1. Then, the collagen mask substrate is soaked in deionized water for 1 hour, and then the collagen content in the soaking liquid is determined to obtain the original collagen content W2. The calculation formula of the collagen loss rate is: collagen loss rate = W2 / W1×100%.
[0171] Table 2 The loss rate of collagen in the collagen mask base material after immersion for 1 hour
[0172]
[0173] It can be seen from Table 2 that the collagen loss rate of the collagen mask base materials obtained in Examples 1 to 3 of the present application after immersion for 1 hour is ≤6%.
[0174] Six volunteers aged 25 to 45 were selected to try the collagen mask substrate of Example 1, and the collagen mask substrate was soaked in deionized water for 5 minutes to obtain a collagen mask. The moisturizing performance and physical cooling performance of the collagen mask were then tested, and the test results are shown in Table 3.
[0175] The moisturizing performance test method is: first test the moisture content of the volunteers' facial skin before using the mask, and control it at about 35% to ensure the validity of the comparison results. Then apply the collagen mask on the volunteers' cheeks in the correct way, and measure the moisture content of the skin in the same area on both sides after 20 minutes of application. Each volunteer tests 3 areas and takes the average value.
[0176] The physical cooling performance test method is: first measure the facial temperature of the volunteers when no mask is used, then apply the collagen mask on the cheeks according to the correct method, measure the facial temperature 20 minutes after application, and test 3 areas on the left and right faces of each volunteer, and take the average value.
[0177] Table 3 Moisturizing and physical cooling properties of collagen mask
[0178]
[0179] As shown in Table 3, the collagen mask substrate prepared in this application has excellent moisturizing, hydrating and physical cooling properties. After the collagen mask substrate is soaked in deionized water, it can replenish about 25-35% of the moisture of the facial skin, and has excellent hydrating and moisturizing effects; at the same time, after the collagen mask substrate is soaked in deionized water, it can play an effective physical cooling role after being applied to the face, with an average cooling of 5°C, which improves the coolness and comfort of the face.
[0180] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity, and should not be understood as a rigid limitation on the scope of the present application; therefore, the range description should be considered to have specifically disclosed all possible sub-ranges and single numerical values within the range. For example, the range description from 1 to 6 should be considered to have specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any cited number (fractional or integer) within the indicated range.
[0181] The above description is only a specific implementation of the present application, so that those skilled in the art can understand or implement the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest range consistent with the principles and novel features applied for herein.
Claims
1. A method for preparing a collagen mask substrate, characterized in that: The method comprises the following steps: S1, subjecting the facial mask substrate to plasma treatment to obtain a modified facial mask substrate; S2, subjecting the modified facial mask substrate to an etherification reaction with an etherifying agent to introduce hydrophilic and lipophilic groups into the structure of the modified facial mask substrate to obtain an etherified facial mask substrate; S3, mixing the etherified facial mask base material with the collagen solution to obtain a mixed liquid; S4, subjecting the mixed liquid to a microwave-ultrasound combined treatment, and then drying to obtain a collagen mask substrate.
2. The method for preparing the collagen mask substrate according to claim 1, characterized in that: The plasma treatment includes the following parameters: the plasma gas is oxygen, the power is 10-30 W, the time is 30 s-180 s, and the gas flow rate is 10-30 sccm.
3. The method for preparing the collagen mask substrate according to claim 1, characterized in that: The etherifying agent is composed of ethylene glycol butyl ether and ethylene oxide, and the mass ratio of the ethylene glycol butyl ether to the ethylene oxide is (3-8):
1.
4. The method for preparing the collagen mask substrate according to claim 1, characterized in that: The etherification reaction includes the following parameters: reaction temperature is 60-80° C., and time is 3-6 hours.
5. The method for preparing the collagen mask substrate according to claim 1, characterized in that: The collagen solution is composed of the following components in parts by mass: 1 to 5 parts of fish skin collagen, 1 to 2 parts of quaternized sodium alginate, 0.5 to 1 part of hyaluronic acid, 0.1 to 0.5 part of citric acid, 0.1 to 0.5 part of glutathione, 0.5 to 1 part of polyvinyl alcohol, 0.5 to 1 part of polysorbate and 85 to 96 parts of deionized water.
6. The method for preparing the collagen mask substrate according to claim 1, characterized in that: The microwave-ultrasound combined treatment includes the following parameters: microwave power is 50-150W, ultrasonic power is 200-300W, and combined treatment time is 10s-90s.
7. The method for preparing the collagen mask substrate according to claim 1, characterized in that: The fiber raw material of the mask substrate is biological fiber, and the preparation method of the biological fiber comprises the following steps: S101, inoculating xylindracenacetobacillus and bacillus cereus into a culture medium for fermentation, and performing laser irradiation-ultrasound combined treatment during the fermentation process to obtain a fermentation liquid containing fiber; S102, taking out the cellulose in the fermentation liquid, washing and drying it, and obtaining the biofiber.
8. The method for preparing the collagen mask substrate according to claim 7, characterized in that: In terms of mass concentration, the culture medium includes the following chemical components: 10-20 g of glucose, 5-15 g of yeast extract, 5-10 g of peptone, 1.5-3 g of potassium dihydrogen phosphate, 0.5-1 g of caffeine, and 1000 mL of deionized water.
9. The method for preparing the collagen mask substrate according to claim 7, characterized in that: The inoculation rate of the xylinacetobacter is 6-8%, and the inoculation rate of the Bacillus cereus is 10-20%; and / or, The laser irradiation-ultrasound combined treatment includes the following parameters: ultrasonic power is 200-300W, laser irradiation intensity is 5-15mW / cm², and time is 15-30s / h; and / or, The fermentation temperature is 28-30°C, and the fermentation time is 7-10 days; and / or, The deposit number of the xylinacetobacter is ATCC 23767; and / or, The deposit number of the Bacillus cereus is CICC 23828.
10. A collagen mask base material prepared by the preparation method of the collagen mask base material according to any one of claims 1 to 9.
Citation Information
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