A kind of gel frosting for beauty instrument and preparation method thereof
Through the composite structure of aluminum nitride-coated chitosan and Ag nanowires/hydroxyapatite microspheres, the thermal conductivity and antibacterial properties of beauty instrument gel are improved, solving the problem of insufficient thermal conductivity and antibacterial properties of existing materials, and is suitable for high-end beauty instruments.
Patent Information
- Application Number
- CN202510678364.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-26
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2045-05-26
AI Technical Summary
Existing beauty instrument frosting materials have deficiencies in thermal conductivity and antibacterial properties, making it difficult to meet the needs of efficient heat conduction and long-term safe use.
A composite system of aluminum nitride-coated chitosan composite nanospheres and Ag nanowires/hydroxyapatite microspheres is used to improve the thermal conductivity and antibacterial properties of the material by constructing a porous structure and the synergistic effect of precious metal nanowires.
It significantly improves the thermal conductivity and antibacterial properties of the gel, and is suitable for high-end beauty equipment. It solves the problems of poor thermal conductivity and weak antibacterial properties of existing materials and is suitable for high-end beauty equipment.
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Figure CN120189356B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the field of frosting, and in particular to a frosting for beauty equipment and a preparation method thereof. Background Art
[0002] With the widespread adoption of high-tech beauty devices in skin care, facial firming, and anti-aging, the delivery media in these devices are gradually evolving from traditional creams or gels to functional gels. During use, gels, acting as an intermediary between the skin and the device, must not only possess excellent tactile feel and lubricity, but also meet the dual functional requirements of efficient thermal conductivity and antibacterial properties. On the one hand, beauty devices such as radiofrequency, microcurrent, and thermal conductivity devices generate heat during operation. Gels must possess excellent thermal conductivity to achieve efficient energy transfer and ensure even heat distribution across the skin, thereby enhancing device efficiency and user experience. On the other hand, since gels directly apply to facial skin, they are susceptible to bacterial growth and contamination during use. Therefore, antibacterial properties are crucial for ensuring product safety and extending product life. Against this backdrop, developing a gel specifically for beauty devices that combines excellent thermal conductivity with good antibacterial properties would not only significantly enhance the overall efficacy of the device but also expand its applicability to high-standard applications such as medical aesthetics and home care. This is crucial for promoting the development and upgrading of functional skincare materials.
[0003] Despite the recent expansion of functional gels in beauty devices, most current gel products still face challenges with insufficient thermal conductivity and antimicrobial properties, making them difficult to meet the dual requirements of high-frequency heat transfer and long-term safety. Conventional gel formulations often utilize a hydrogel matrix and an oil emulsifier system. While these systems offer excellent tactile properties and fluidity, they exhibit limited thermal conductivity, making them incapable of achieving the rapid heat transfer required for efficient energy output in beauty devices. Furthermore, preservatives or inefficient antimicrobial components introduced to enhance product stability often fail to provide a sustained and mild antimicrobial effect in actual use, particularly after repeated contact with the skin or exposure to air, leading to the risk of microbial growth. Some research has attempted to improve performance by incorporating functional particles into gels. For example, Chinese patent application number CN101002725A discloses a beauty gel intended to enhance skin nutrition and reduce surface moisture loss. However, these gels still suffer from suboptimal thermal conductivity and a limited duration of antimicrobial efficacy. These issues stem from uneven dispersion and uncontrolled release of the functional components within the system, as well as a lack of synergistic structural design. Therefore, there is an urgent need to develop a new type of frosting material with a reasonable structure, synergistic composite functions, and significantly improved performance in thermal conductivity and antibacterial properties, so as to meet the higher requirements of high-end beauty equipment for functional introduction media. Summary of the Invention
[0004] (1) Technical problems solved
[0005] The purpose of the present invention is to provide a gel frosting for beauty instruments and a preparation method thereof, so as to solve the problem that the existing gel frosting has insufficient thermal conductivity and antibacterial properties.
[0006] (2) Technical solution
[0007] In order to achieve the above object, the present invention provides the following technical solutions:
[0008] A gel cream for a beauty instrument, comprising the following raw materials in parts by weight: 4.0-8.0 parts of aluminum nitride-coated chitosan composite nanospheres, 3.5-8.0 parts of Ag nanowire / hydroxyapatite microspheres, 40.0-60.0 parts of sodium hyaluronate hydrogel, 4.0-8.0 parts of cetyl palmitate, 2.0-5.0 parts of polyglycerol-10 stearate, 20.0-40.0 parts of a mixed solvent of glycerol and deionized water, 0.5-2.0 parts of carbomer 940, and 0.2-0.5 parts of triethanolamine;
[0009] The aluminum nitride-coated chitosan composite nanospheres are composed of porous aluminum nitride hollow microspheres and chitosan coated in their inner cavities; wherein the outer surface of the porous aluminum nitride hollow microspheres is uniformly distributed with a through-hole structure, which is used to achieve the sustained release of chitosan;
[0010] In the mixed solvent of glycerol and deionized water, the volume ratio of glycerol to water is 1:1 to 3:1;
[0011] The Ag nanowire / hydroxyapatite microspheres are composed of hydroxyapatite microspheres and Ag nanowires loaded on the surface thereof; wherein the Ag nanowires are evenly distributed and stably loaded on the surface of the hydroxyapatite microspheres.
[0012] Furthermore, the preparation method of the aluminum nitride-coated chitosan composite nanospheres is as follows: in parts by weight, 0.5-0.6 parts of chitosan with a deacetylation degree of ≥85% and a molecular weight of 50-100 kDa, 11.5-12.5 parts of glacial acetic acid and 87.0-89.0 parts of deionized water are mixed, stirred at 25-30°C with a magnetic stirring rate of 500-700 rpm for 4.0-6.0 hours, and filtered through a 0.45 μm filter membrane to prepare a chitosan solution; 95-105 parts of pre-dried porous aluminum nitride hollow microspheres are mixed with 48-52 parts of the chitosan solution, and ultrasonically treated at 40-45°C with an ultrasonic frequency of 38-42 kHz, a power of 190-210 W, and a time of 10-20 minutes, and then filtered under a vacuum degree of 0.04-0.06 MPa for 18-22 minutes. min, and continue to stir at 20-25°C for 1.5-2.5 hours to form a composite microsphere suspension; 0.48-0.52 parts of a 25 wt% glutaraldehyde aqueous solution are added dropwise to the suspension, the pH is adjusted to 5.5-6.0 with a 0.01-0.03 wt.% hydrochloric acid aqueous solution, and the mixture is stirred at 200-300 rpm for 14-16 minutes. After washing with deionized water, the mixture is centrifuged at a speed of 4800-5200 rpm for 4.5-5.5 minutes. The precipitate is collected and pre-frozen at -80--70°C for 11-13 hours, and then transferred to a vacuum freeze dryer and dried at a pressure of ≤10 Pa for 24-50 hours to obtain white to light yellow powdery aluminum nitride-coated chitosan composite nanospheres.
[0013] Furthermore, the preparation method of the porous aluminum nitride hollow microspheres is as follows: in parts by weight, 0.9-1.1 parts of polystyrene template microspheres with a particle size of 300-500 nm are dispersed in 48-52 parts of a mixed solvent of ethanol and deionized water in a volume ratio of 6.5:3.5-7.5:2.5, 0.09-0.11 parts of polyvinyl pyrrolidone are added, and then dispersed for 8-12 minutes under ultrasonic frequency of 40-45 kHz and power of 80-100 W to form a stable suspension; 2.8-3.2 parts of aluminum isopropanol are dissolved in 18-22 parts of anhydrous ethanol and controlled hydrolysis is carried out by dropwise addition of 1.8-2.2 parts of deionized water, and 0.01-0.03 wt.% nitric acid solution is added to adjust the pH to 4.3-5.7 to form an aluminum sol precursor; the aluminum sol is precipitated at 0.5-1.5 The template dispersion system was added dropwise at a rate of 400-600 rpm, and the sol-gel coating reaction was carried out for 110-130 min, followed by standing for aging for 11-13 h; the supernatant was discarded by centrifugation at a speed of 3500-4500 rpm and the precipitate was collected, and dried for 11-13 h under vacuum conditions of -0.08-0.10 MPa and a temperature of 58-62°C to obtain porous aluminum nitride hollow precursor microspheres; the precursor was placed in a tube furnace, and the temperature was increased to 900-1100°C at a rate of 4-6°C / min, and then ammonia flow rate of 280-320 mL / min was introduced for nitridation treatment, and the temperature was kept for 115-125 The aluminum oxide was completely converted into an aluminum nitride shell for 10 min, and the polystyrene template was pyrolyzed at 420-480°C to form a hollow structure. The obtained hollow microspheres were dispersed in a 28-32% hydrogen peroxide solution, oxidized and etched at 40-50°C for 40-50 min, and then washed with deionized water until neutral, finally obtaining porous aluminum nitride hollow microspheres.
[0014] Furthermore, the average diameter of the aluminum nitride-coated chitosan composite nanospheres is 350-550 nm; the average pore diameter of the porous aluminum nitride hollow microspheres is 18-30 nm;
[0015] Furthermore, the mass ratio of the porous aluminum nitride hollow microspheres to chitosan in the aluminum nitride-coated chitosan composite nano-microspheres is 8:1-12:1.
[0016] The present invention adopts the preparation of aluminum nitride-coated chitosan composite nano-microspheres, which is mainly used to enhance the performance of the frost system with thermal conductivity and antibacterial properties. The core of its design is to achieve a synergistic improvement of material functions through the composite structure of porous aluminum nitride hollow microspheres and chitosan. In this technical solution, porous aluminum nitride microspheres with hollow structures and through-holes are first constructed by the polystyrene template method, which provides a high specific surface area and a good interface carrier for the subsequent coating of functional components; then chitosan with a high degree of deacetylation and an appropriate molecular weight is used to form a uniform solution in a glacial acetic acid solution, and then subjected to ultrasonic treatment, filtration dispersion and glutaraldehyde cross-linking to achieve effective coating and structural fixation in the inner cavity of the porous aluminum nitride. As an inorganic material with excellent thermal conductivity, aluminum nitride's hollow, porous structure not only provides channels for heat transfer but also increases the specific surface area of the overall material, facilitating uniform distribution with other components. Chitosan, with its natural polymer biocompatibility and antibacterial properties, introduces mild and effective antimicrobial properties to the gel system, while also improving the system's stability and release behavior by regulating its coating and cross-linking levels. By optimizing the ratio of the two materials, they form stable composite microspheres at the microscopic level, enhancing both fundamental thermal conductivity and antibacterial properties. Furthermore, through structural complementarity and interfacial interactions, they achieve comprehensive performance superior to that of a single material, providing reliable support for the high-standard functional delivery media required in beauty devices.
[0017] Furthermore, the preparation method of the Ag nanowire / hydroxyapatite microspheres is as follows: in parts by weight, 0.9-1.1 parts of hydroxyapatite microspheres are dispersed in 18-22 parts of anhydrous ethylene glycol, 0.045-0.055 parts of polyvinyl pyrrolidone are added, and then treated under ultrasonic frequency of 38-42 kHz and power of 180-220 W for 8-12 minutes to form a surface activated dispersion system, and the stirring speed is maintained at 300-400 rpm and the temperature is maintained at 25-30°C for 25-35 minutes to complete the surface modification; 0.16-0.18 parts of silver nitrate, 0.28-0.32 parts of polyvinyl pyrrolidone and a concentration of 0.095-0.105 are sequentially added to the dispersion system. 0.09-0.11 parts of a mol / L ferric chloride solution were transferred to a three-necked flask and heated to a reaction temperature of 120-140°C at a heating rate of 4-6°C / min. An in-situ reduction reaction was carried out at a stirring rate of 500-700 rpm for 60-90 min to promote the directional growth of silver ions on the hydroxyapatite surface. After the reaction, the solution was naturally cooled to 20-25°C. The supernatant containing unreacted silver nitrate, free polyvinylpyrrolidone, and by-products was separated by centrifugation at a speed of 5800-6200 rpm. The precipitate was collected and washed repeatedly with an ethanol / water mixture with a volume ratio of 0.95:1.05-1.05:0.95 for 2-4 times. Finally, the solution was freeze-dried at a temperature of -50--45°C and a vacuum degree of ≤10 Pa for 10-14 h to prepare Ag nanowire / hydroxyapatite microspheres.
[0018] Furthermore, the preparation method of the hydroxyapatite microspheres is as follows: in parts by weight, 0.8-1.2 parts of calcium nitrate tetrahydrate are dissolved in 45-55 parts of deionized water to form a calcium source solution, and 0.4-0.6 parts of diammonium hydrogen phosphate are dissolved in 45-55 parts of deionized water to form a phosphorus source solution, and the phosphorus source solution is added dropwise to the calcium source solution at a stirring rate of 400-600 rpm at a dropwise addition rate of 1-2 mL / min, and ammonia water is simultaneously added to adjust the pH to 9.5-10.5 and maintain the temperature at 25-30°C to perform a coprecipitation reaction. After the dropwise addition is completed, stirring is continued for 120-180 minutes to form a hydroxyapatite precursor suspension, which is then transferred to a high-pressure reactor for hydrothermal treatment at a heating rate of 3-5°C / min to a reaction temperature of 120-130°C. During the hydrothermal treatment stage, the pressure in the reactor is maintained at 0.15-0.25 MPa and the holding time is 3.5-4.5 h to crystallize the precursor into hydroxyapatite microspheres. After the reaction, the supernatant was removed by centrifugation at a speed of 3000-4000 rpm and the precipitate was collected. The precipitate was washed alternately with deionized water and anhydrous ethanol for 3-5 times and then placed in a vacuum drying oven for 6-8 h at a drying temperature of 50-70°C and a vacuum degree of -0.08-0.10 MPa to obtain hydroxyapatite microspheres.
[0019] Furthermore, the mass ratio of Ag nanowires to hydroxyapatite microspheres in the Ag nanowire / hydroxyapatite microspheres is 1:10 to 1:5;
[0020] Furthermore, the average diameter of the Ag nanowire / hydroxyapatite microspheres is 350-600 nm.
[0021] The present invention uses Ag nanowire / hydroxyapatite microspheres to enhance the thermal conductivity and antibacterial performance of the frost-forming system. Its design is based on the antibacterial activity of precious metal nanostructures and the structural stability of inorganic bioceramic materials. By constructing a composite microsphere, multiple functions are synergistically enhanced. In this scheme, calcium nitrate tetrahydrate and diammonium hydrogen phosphate are first coprecipitated under alkaline conditions to form a hydroxyapatite precursor. Then, under controlled temperature and pressure conditions, hydrothermal treatment is performed to obtain hydroxyapatite microspheres with stable crystal form and uniform particle size. Such microspheres have good biocompatibility and dispersibility, and provide a high specific surface area for the subsequent directional growth of silver nanowires. Subsequently, the microspheres are dispersed in anhydrous ethylene glycol and modified and activated with polyvinyl pyrrolidone to form a reaction environment on the surface that is conducive to the adsorption and reduction of silver ions. By gradually introducing silver nitrate and ferric chloride solutions into the system, silver ions are reduced in situ on the hydroxyapatite surface under elevated temperature conditions and self-assemble to form a silver nanowire structure with a high specific surface area. The formation of silver nanowires not only significantly enhances the material's antibacterial properties, but also helps improve the thermal conductivity of the de-icing medium through their excellent electronic and thermal conductivity properties. Hydroxyapatite microspheres provide a stable carrier while ensuring the uniform distribution and structural stability of the silver nanowires, reducing the risk of agglomeration and migration. The close structural integration and complementary performance of these two components enable the composite microspheres to demonstrate superior thermal conductivity and antibacterial properties compared to either single material, providing new insights and technical support for the development of high-performance delivery media for beauty devices.
[0022] The present invention also discloses a method for preparing gel frosting for a beauty instrument, comprising the following steps:
[0023] S1. Pre-disperse the sodium hyaluronate hydrogel in a clean container at a stirring rate of 300-500 rpm and a temperature of 20-30°C for 10-20 minutes to obtain a uniform and fluid sodium hyaluronate hydrogel base system.
[0024] S2. Add a mixed solvent of glycerol and deionized water to the base system described in S1, along with Carbomer 940. Stir continuously at 400-600 rpm for 20-30 minutes to fully disperse and pre-swell the Carbomer. Then, let the mixture stand for 5-10 minutes to eliminate air bubbles and stabilize the system structure.
[0025] S3. Cetyl palmitate and polyglyceryl-10 stearate were mixed and heated to melt at 65-75 ° C for 10-15 min under magnetic stirring at a rate of 200-400 rpm to form a uniform emulsion phase. The emulsion phase was then added to the system obtained in S2 at a dropwise addition rate of 1-2 mL / min. The stirring rate was maintained at 600-800 rpm and the emulsification was carried out for 15-25 min to form a primary emulsion system.
[0026] S4. The aluminum nitride-coated chitosan composite nanospheres were added to the primary emulsification system described in S3 and dispersed at a temperature of 30 to 40 ° C and a stirring rate of 500 to 700 rpm for 15 to 25 min;
[0027] S5. Add the Ag nanowires / hydroxyapatite microspheres to the dispersion obtained in S4. Maintain stirring at 400–600 rpm and 25–35°C for 20–30 min.
[0028] S6. Triethanolamine is added dropwise to the mixture obtained in S5. The mixture is stirred at a stirring rate of 300-500 rpm for 10-15 minutes. The mixture is then degassed under a vacuum of 0.05-0.08 MPa for 10-20 minutes. The mixture is finally cooled to 20-25°C to form a homogeneous and stable frosted product.
[0029] This invention effectively enhances the thermal conductivity and antibacterial properties of the de-icing material by constructing a composite system of Ag nanowires / hydroxyapatite microspheres and aluminum nitride-coated chitosan composite nanospheres. The Ag nanowires grow directionally on the surface of the hydroxyapatite microspheres, providing not only efficient antibacterial activity but also forming localized heat conduction pathways at the microscopic scale through their linear conductive structure. Hydroxyapatite acts as a stabilizing carrier, enhancing its dispersibility and biocompatibility. The aluminum nitride hollow microspheres possess excellent thermal conductivity and a porous structure, enabling the formation of continuous heat flow channels, significantly improving the efficiency of heat conduction in the de-icing. The chitosan coating not only enhances the dispersion stability of the composite microspheres in aqueous systems but also achieves mild antibacterial properties through its cationic properties, forming a charge interaction with bacterial cell membranes. The two types of functional components form a synergistic mechanism in terms of structural configuration, interfacial interaction and functional properties. The strong bactericidal effect of Ag nanowires and the sustained-release antibacterial effect of chitosan complement each other. The rapid thermal conduction of aluminum nitride and the microscale heat flow regulation of the silver structure promote each other, achieving dual optimization of thermal conductivity and antibacterial properties while ensuring material stability and biosafety.
[0030] (3) Beneficial technical effects
[0031] 1. This invention significantly improves the thermal conductivity and antibacterial properties of frost through the structural synergy of aluminum nitride and chitosan, overcoming the problems of poor thermal conductivity and weak antibacterial properties of existing materials, and has good application prospects.
[0032] 2. This invention significantly enhances the thermal conductivity and antibacterial properties of the gel through the structural complementarity of silver nanowires and hydroxyapatite microspheres, addressing the challenges of poor antibacterial durability and low thermal conductivity efficiency of existing materials. It is suitable for high-end beauty applications, demonstrating excellent synergistic advantages and promising application prospects. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 This is a morphology diagram of the porous aluminum nitride hollow microspheres prepared in Example 1 of the present invention.
[0034] Figure 2 This is a morphology diagram of the aluminum nitride-coated chitosan composite nanospheres prepared in Example 1 of the present invention.
[0035] Figure 3 This is the XRD phase analysis diagram of the aluminum nitride-coated chitosan composite nanospheres prepared in Example 1 of the present invention.
[0036] Figure 4 This is a morphology diagram of the hydroxyapatite microspheres prepared in Example 1 of the present invention.
[0037] Figure 5 This is the XRD phase analysis diagram of the hydroxyapatite microspheres prepared in Example 1 of the present invention.
[0038] Figure 6 This is a morphology diagram of the Ag nanowire / hydroxyapatite microspheres prepared in Example 1 of the present invention.
[0039] Figure 7 This is the XRD phase analysis diagram of the Ag nanowire / hydroxyapatite microspheres prepared in Example 1 of the present invention. DETAILED DESCRIPTION
[0040] To make the objectives, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
[0041] Example 1
[0042] A gel cream for a beauty instrument, comprising the following raw materials in parts by weight: 4.0 parts of aluminum nitride-coated chitosan composite nanospheres, 3.5 parts of Ag nanowire / hydroxyapatite microspheres, 40.0 parts of sodium hyaluronate hydrogel, 4.0 parts of cetyl palmitate, 2.0 parts of polyglycerol-10 stearate, 20.0 parts of a mixed solvent of glycerin and deionized water, 0.5 parts of carbomer 940, and 0.2 parts of triethanolamine;
[0043] The aluminum nitride-coated chitosan composite nanospheres are composed of porous aluminum nitride hollow microspheres and chitosan coated in their inner cavities. The outer surface of the porous aluminum nitride hollow microspheres is uniformly distributed with through-hole structures, which are used to achieve the sustained release of chitosan.
[0044] In the mixed solvent of glycerol and deionized water, the volume ratio of glycerol to water is 1:1;
[0045] The Ag nanowire / hydroxyapatite microspheres are composed of hydroxyapatite microspheres and Ag nanowires loaded on the surface thereof; wherein the Ag nanowires are uniformly distributed and stably loaded on the surface of the hydroxyapatite microspheres.
[0046] The preparation method of the aluminum nitride-coated chitosan composite nanospheres of the present embodiment is as follows: in parts by weight, 0.5 parts of chitosan with a deacetylation degree of ≥85% and a molecular weight of 50 kDa, 11.5 parts of glacial acetic acid and 87.0 parts of deionized water are mixed, stirred at a magnetic stirring rate of 500 rpm at 25°C for 4.0 hours, and filtered through a 0.45 μm filter membrane to prepare a chitosan solution; 95 parts of pre-dried porous aluminum nitride hollow microspheres are mixed with 48 parts of the chitosan solution, ultrasonically treated at 40°C with an ultrasonic frequency of 38 kHz, a power of 190 W, and a time of 10 minutes, followed by suction filtration at a vacuum degree of 0.04 MPa for 18 minutes, and continued to stand and stir at 20°C for 1.5 hours to form a composite microsphere suspension; 0.48 parts of a 25 wt% aqueous solution of glutaraldehyde are added dropwise to the suspension, the pH is adjusted to 5.5 with a 0.01 wt.% aqueous solution of hydrochloric acid, and the mixture is heated at 200°C. The mixture was stirred at 4800 rpm for 14 min, washed with deionized water and then centrifuged at 4800 rpm for 4.5 min. The precipitate was collected and pre-frozen at -80°C for 11 h, and then transferred to a vacuum freeze dryer and dried at a pressure of ≤10 Pa for 24 h to obtain aluminum nitride-coated chitosan composite nanospheres in the form of white to light yellow powder.
[0047] The preparation method of the porous aluminum nitride hollow microspheres of this embodiment is as follows: 0.9 parts of polystyrene template microspheres with a particle size of 300 nm are dispersed in 48 parts of a mixed solvent of ethanol and deionized water in a volume ratio of 6.5:3.5, 0.09 parts of polyvinyl pyrrolidone are added, and then dispersed for 8 minutes under ultrasonic frequency of 40 kHz and power of 80 W to form a stable suspension; 2.8 parts of aluminum isopropanol are dissolved in 18 parts of anhydrous ethanol and controlled hydrolyzed by dropwise addition of 1.8 parts of deionized water, and 0.01 wt.% nitric acid solution is added to adjust the pH to 4.3 to form an aluminum sol precursor; the aluminum sol is added dropwise to the template dispersion system at a rate of 0.5 mL / min, and the stirring speed is maintained at 400 rpm for sol-gel coating reaction for 110 minutes, followed by standing for aging for 11 hours; the supernatant is discarded by centrifugation at a speed of 3500 rpm and the precipitate is collected, and the vacuum degree is -0.08 MPa and a temperature of 58°C for 11 h to obtain porous aluminum nitride hollow precursor microspheres; the precursor was placed in a tube furnace, and the temperature was raised to 900°C at a rate of 4°C / min, and then an ammonia flow rate of 280 mL / min was introduced for nitridation treatment. The heat preservation time was 115 min to completely convert the aluminum oxide into an aluminum nitride shell. At the same time, the polystyrene template was pyrolyzed at 420°C to form a hollow structure; the obtained hollow microspheres were dispersed in a 28% by mass hydrogen peroxide solution, oxidized and etched at a temperature of 40°C for 40 min, and then washed with deionized water until neutral, finally obtaining porous aluminum nitride hollow microspheres.
[0048] The average diameter of the aluminum nitride-coated chitosan composite nanospheres in this example is 350 nm;
[0049] The average pore diameter of the porous aluminum nitride hollow microspheres is 18 nm;
[0050] The mass ratio of the porous aluminum nitride hollow microspheres to chitosan in the aluminum nitride-coated chitosan composite nano-microspheres of this embodiment is 8:1.
[0051] The preparation method of Ag nanowire / hydroxyapatite microspheres of this embodiment is as follows: 1.0 part of hydroxyapatite microspheres is dispersed in 19 parts of anhydrous ethylene glycol, 0.048 parts of polyvinyl pyrrolidone is added, and then treated under ultrasonic frequency of 39 kHz and power of 192 W for 9 minutes to form a surface-activated dispersion system, and the surface modification is completed by maintaining the stirring speed at 330 rpm and the temperature at 27°C for 28 minutes; 0.17 parts of silver nitrate, 0.29 parts of polyvinyl pyrrolidone and 0.10 parts of 0.098 mol / L ferric chloride solution are added to the dispersion system in sequence, and the mixture is transferred to a three-necked flask, heated to a reaction temperature of 126°C at a heating rate of 5°C / min, and subjected to an in situ reduction reaction at a stirring rate of 560 rpm. min, promoting the directional growth of silver ions nanowires on the surface of hydroxyapatite; after the reaction, it was naturally cooled to 21°C, and the supernatant containing unreacted silver nitrate, free polyvinylpyrrolidone and by-products was separated and removed by centrifugation at a speed of 5920 rpm. The precipitate was collected and washed repeatedly three times with an ethanol / water mixture with a volume ratio of 0.98:1.02, and finally dehydrated at a freeze-drying temperature of -49°C and a vacuum degree of ≤10 Pa for 11 h to obtain Ag nanowire / hydroxyapatite microspheres.
[0052] The preparation method of hydroxyapatite microspheres in this embodiment is as follows: in parts by weight, 0.9 parts of calcium nitrate tetrahydrate are dissolved in 48 parts of deionized water to form a calcium source solution, and 0.5 parts of diammonium hydrogen phosphate are dissolved in 48 parts of deionized water to form a phosphorus source solution. The phosphorus source solution is added dropwise to the calcium source solution at a dropping speed of 1.3 mL / min under a stirring rate of 460 rpm. Ammonia water is simultaneously added to adjust the pH to 9.8 and the temperature is maintained at 27°C to perform a coprecipitation reaction. After the dropwise addition is completed, stirring is continued for 138 minutes to form a hydroxyapatite precursor suspension, which is then transferred to a high-pressure reactor for hydrothermal treatment at a heating rate of 3.6°C / min to a reaction temperature of 123°C. During the hydrothermal treatment stage, the pressure in the reactor is maintained at 0.18 MPa and the holding time is 3.8 hours to allow the precursor to crystallize into hydroxyapatite microspheres. After the reaction is completed, the suspension is centrifuged at a speed of 3300. The supernatant was removed by rpm separation and the precipitate was collected. It was washed alternately with deionized water and anhydrous ethanol for 4 times and then placed in a vacuum drying oven. Hydroxyapatite microspheres were obtained by treatment at a drying temperature of 56°C and a vacuum degree of -0.086 MPa for 7 h.
[0053] The mass ratio of Ag nanowires to hydroxyapatite microspheres in the Ag nanowire / hydroxyapatite microspheres of this embodiment is 1:8.5;
[0054] The average diameter of the Ag nanowire / hydroxyapatite microspheres in this example is 425 nm;
[0055] A method for preparing a gel frosting for a beauty instrument according to this embodiment includes the following steps:
[0056] S1. The sodium hyaluronate hydrogel was placed in a clean container and pre-dispersed at a stirring rate of 360 rpm, maintaining a temperature of 23 ° C, and stirring for 13 min to obtain a uniform and fluid sodium hyaluronate hydrogel base system;
[0057] S2. A mixture of glycerol and deionized water was added to the base system described in S1, along with Carbomer 940. Stirring was continued at 460 rpm for 23 minutes to allow the Carbomer to fully disperse and pre-swell. The mixture was then allowed to stand for 7 minutes to eliminate air bubbles and stabilize the system structure.
[0058] S3. Cetyl palmitate and polyglyceryl-10 stearate were mixed and heated to melt at 68 ° C for 12 min under magnetic stirring at a rate of 260 rpm to form a uniform emulsion phase. The emulsion phase was then added to the system obtained in S2 at a dropwise addition rate of 1.3 mL / min. The stirring rate was maintained at 660 rpm and the emulsification was carried out for 18 min to form a primary emulsion system.
[0059] S4. The aluminum nitride-coated chitosan composite nanospheres were added to the primary emulsification system of S3 and dispersed at a temperature of 33 ° C and a stirring rate of 560 rpm for 18 min;
[0060] S5. Add the Ag nanowires / hydroxyapatite microspheres to the dispersion obtained in S4, maintain the stirring rate at 460 rpm and the temperature at 28°C, and continue stirring for 23 min.
[0061] S6. Triethanolamine was added dropwise to the system obtained in S5, and the mixture was stirred at a stirring rate of 360 rpm for 12 min. The mixture was then degassed under a vacuum degree of 0.059 MPa for 13 min, and finally cooled to 21°C to form a homogeneous and stable frosted product.
[0062] Depend on Figure 1 and Figure 2 It can be seen that the porous aluminum nitride hollow microspheres prepared in Example 1 have a regular spherical structure as a whole, and have evenly distributed through-holes on the surface. The composite nano-microspheres formed after chitosan coating maintain a good spherical morphology and a denser surface structure, indicating that chitosan achieves effective loading and structural stability in the inner cavity of the aluminum nitride hollow microspheres. Figure 3 The XRD patterns further verified the existence of aluminum nitride crystal structure in the composite microspheres, and no impurity peaks appeared, indicating that the chitosan coating process did not change the crystal phase composition of aluminum nitride; Figure 4 and Figure 6The composite morphologies of hydroxyapatite microspheres and their loaded Ag nanowires are shown respectively. The former has uniform particle size and smooth surface, while the latter has uniformly distributed silver nanowire structures on its surface, indicating that silver has achieved directional growth on the hydroxyapatite surface. Figure 5 and Figure 7 XRD analysis shows that hydroxyapatite has typical hexagonal crystal structure characteristics, and the introduction of Ag nanowires does not destroy its crystal phase. At the same time, the characteristic diffraction peaks of silver can be clearly detected, proving that silver nanowires have been successfully generated and stably exist on the surface of hydroxyapatite. In summary, the two functional microspheres used in the present invention have clear structure, clear composition, and good interface bonding, providing a structural and material basis for the thermal conductivity and antibacterial properties of the subsequent defrost system.
[0063] Example 2
[0064] A gel cream for a beauty instrument, comprising the following raw materials in parts by weight: 5.0 parts of aluminum nitride-coated chitosan composite nanospheres, 4.9 parts of Ag nanowire / hydroxyapatite microspheres, 46.0 parts of sodium hyaluronate hydrogel, 5.0 parts of cetyl palmitate, 3.0 parts of polyglycerol-10 stearate, 26.0 parts of a mixed solvent of glycerin and deionized water, 1.0 part of carbomer 940, and 0.3 part of triethanolamine;
[0065] The aluminum nitride-coated chitosan composite nanospheres are composed of porous aluminum nitride hollow microspheres and chitosan coated in their inner cavities. The outer surface of the porous aluminum nitride hollow microspheres is uniformly distributed with through-hole structures, which are used to achieve the sustained release of chitosan.
[0066] In the mixed solvent of glycerol and deionized water, the volume ratio of glycerol to water is 1.6:1;
[0067] The Ag nanowire / hydroxyapatite microspheres are composed of hydroxyapatite microspheres and Ag nanowires loaded on the surface thereof; wherein the Ag nanowires are uniformly distributed and stably loaded on the surface of the hydroxyapatite microspheres.
[0068] The preparation method of the aluminum nitride-coated chitosan composite nanospheres of the present embodiment is as follows: in parts by weight, 0.5 parts of chitosan with a deacetylation degree of 85% or more and a molecular weight of 65 kDa, 11.8 parts of glacial acetic acid and 87.7 parts of deionized water are mixed, stirred at a magnetic stirring rate of 560 rpm at 26°C for 4.6 hours, and filtered through a 0.45 μm filter membrane to prepare a chitosan solution; 98 parts of pre-dried porous aluminum nitride hollow microspheres are mixed with 49 parts of the chitosan solution, and ultrasonically treated at 41°C with an ultrasonic frequency of 39 kHz, a power of 196 W, and a time of 13 minutes, followed by suction filtration under a vacuum degree of 0.046 MPa for 19 minutes, and continued to stand and stir at 21°C for 1.8 hours to form a composite microsphere suspension; 25 0.49 parts of wt% glutaraldehyde aqueous solution was adjusted to pH 5.7 with 0.016wt.% hydrochloric acid aqueous solution and stirred at 230 rpm for 15 min. After washing with deionized water, the mixture was centrifuged at 4920 rpm for 4.8 min. The precipitate was collected and pre-frozen at -77°C for 12 h, and then transferred to a vacuum freeze dryer and dried at a pressure of ≤10 Pa for 32 h to obtain white to light yellow powdery aluminum nitride-coated chitosan composite nanospheres.
[0069] The preparation method of the porous aluminum nitride hollow microspheres of this embodiment is as follows: 1.0 part of polystyrene template microspheres with a particle size of 360 nm is dispersed in 49 parts of a mixed solvent of ethanol and deionized water in a volume ratio of 6.8:3.2, 0.10 parts of polyvinyl pyrrolidone is added, and the mixture is dispersed for 9 minutes under ultrasonic frequency of 42 kHz and power of 86 W to form a stable suspension; 2.9 parts of aluminum isopropanol are dissolved in 19 parts of anhydrous ethanol and controlled hydrolyzed by adding 1.9 parts of deionized water dropwise, and 0.016 wt.% nitric acid solution is added to adjust the pH to 4.7 to form an aluminum sol precursor; the aluminum sol is added dropwise to the template dispersion system at a rate of 0.8 mL / min, and the stirring speed is maintained at 460 rpm for sol-gel coating reaction for 116 minutes, followed by standing and aging for 12 hours; the supernatant is discarded by centrifugation at a speed of 3800 rpm and the precipitate is collected, and the vacuum degree is -0.086 MPa and a temperature of 60°C for 12 h to obtain porous aluminum nitride hollow precursor microspheres; the precursor was placed in a tube furnace, and the temperature was raised to 960°C at a rate of 5°C / min, and then an ammonia flow rate of 292 mL / min was introduced for nitridation treatment. The heat preservation time was 118 min to completely convert the aluminum oxide into an aluminum nitride shell. At the same time, the polystyrene template was pyrolyzed at 438°C to form a hollow structure; the obtained hollow microspheres were dispersed in a 29% by mass hydrogen peroxide solution, oxidized and etched at a temperature of 43°C for 43 min, and then washed with deionized water until neutral, finally obtaining porous aluminum nitride hollow microspheres.
[0070] The average diameter of the aluminum nitride-coated chitosan composite nanospheres in this example is 410 nm;
[0071] The average pore diameter of the porous aluminum nitride hollow microspheres is 22 nm;
[0072] The mass ratio of the porous aluminum nitride hollow microspheres to chitosan in the aluminum nitride-coated chitosan composite nano-microspheres of this embodiment is 9:1.
[0073] The preparation method of Ag nanowire / hydroxyapatite microspheres of this embodiment is as follows: in parts by weight, 0.9 parts of hydroxyapatite microspheres are dispersed in 18 parts of anhydrous ethylene glycol, 0.045 parts of polyvinyl pyrrolidone is added, and the mixture is treated under ultrasonic conditions of 38 kHz and 180 W for 8 min to form a surface-activated dispersion system, and the surface modification is completed by maintaining a stirring speed of 300 rpm and a temperature of 25°C for 25 min; 0.16 parts of silver nitrate, 0.28 parts of polyvinyl pyrrolidone, and 0.09 parts of a 0.095 mol / L ferric chloride solution are sequentially added to the dispersion system, and the mixture is transferred to a three-necked flask, heated to a reaction temperature of 120°C at a heating rate of 4°C / min, and subjected to an in-situ reduction reaction at a stirring rate of 500 rpm for 60 min. min, promoting the directional growth of silver ions nanowires on the surface of hydroxyapatite; after the reaction, it was naturally cooled to 20°C, and the supernatant containing unreacted silver nitrate, free polyvinyl pyrrolidone and by-products was separated and removed by centrifugation at a speed of 5800 rpm. The precipitate was collected and washed twice with an ethanol / water mixture with a volume ratio of 0.95:1.05, and finally dehydrated at a freeze-drying temperature of -50°C and a vacuum degree of ≤10 Pa for 10 h to obtain Ag nanowire / hydroxyapatite microspheres.
[0074] The preparation method of hydroxyapatite microspheres in this embodiment is as follows: in parts by weight, 0.8 parts of calcium nitrate tetrahydrate are dissolved in 45 parts of deionized water to form a calcium source solution, and 0.4 parts of diammonium hydrogen phosphate are dissolved in 45 parts of deionized water to form a phosphorus source solution. The phosphorus source solution is added dropwise to the calcium source solution at a dropping speed of 1 mL / min under a stirring rate of 400 rpm, and ammonia water is simultaneously added to adjust the pH to 9.5 and maintain the temperature at 25°C to perform a coprecipitation reaction. After the dropwise addition is completed, stirring is continued for 120 minutes to form a hydroxyapatite precursor suspension, which is then transferred to a high-pressure reactor for hydrothermal treatment at a heating rate of 3°C / min to a reaction temperature of 120°C. During the hydrothermal treatment stage, the pressure in the reactor is maintained at 0.15 MPa and the holding time is 3.5 hours to allow the precursor to crystallize into hydroxyapatite microspheres. After the reaction is completed, the suspension is centrifuged at a speed of 3000. The supernatant was removed by rpm separation and the precipitate was collected. It was washed alternately with deionized water and anhydrous ethanol three times and then placed in a vacuum drying oven. Hydroxyapatite microspheres were obtained by treatment at a drying temperature of 50°C and a vacuum degree of -0.08 MPa for 6 h.
[0075] The mass ratio of Ag nanowires to hydroxyapatite microspheres in the Ag nanowire / hydroxyapatite microspheres of this embodiment is 1:10;
[0076] The average diameter of the Ag nanowire / hydroxyapatite microspheres in this example is 350 nm;
[0077] A method for preparing a gel frosting for a beauty instrument according to this embodiment includes the following steps:
[0078] S1. The sodium hyaluronate hydrogel was placed in a clean container and pre-dispersed at a stirring rate of 300 rpm, maintained at a temperature of 20 ° C, and stirred for 10 min to obtain a uniform and fluid sodium hyaluronate hydrogel base system;
[0079] S2. A mixture of glycerol and deionized water was added to the base system described in S1, along with Carbomer 940. The mixture was stirred at 400 rpm for 20 minutes to allow the Carbomer to fully disperse and pre-swell. The mixture was then allowed to stand for 5 minutes to eliminate bubbles and stabilize the system structure.
[0080] S3. Cetyl palmitate and polyglyceryl-10 stearate were mixed and heated to melt at 65 ° C for 10 min under magnetic stirring at a rate of 200 rpm to form a uniform emulsion phase. The emulsion phase was then added to the system obtained in S2 at a dropwise addition rate of 1 mL / min. The stirring rate was maintained at 600 rpm and the emulsification was carried out for 15 min to form a primary emulsion system.
[0081] S4. The aluminum nitride-coated chitosan composite nanospheres were added to the primary emulsification system of S3 and dispersed at a temperature of 30 ° C and a stirring rate of 500 rpm for 15 min;
[0082] S5. Add the Ag nanowires / hydroxyapatite microspheres to the dispersion obtained in S4, maintain the stirring rate at 400 rpm and the temperature at 25°C, and continue stirring for 20 min.
[0083] S6. Triethanolamine was added dropwise to the system obtained in S5, and the mixture was stirred at a stirring rate of 300 rpm for 10 min. The mixture was then degassed under a vacuum degree of 0.05 MPa for 10 min, and finally cooled to 20°C to form a homogeneous and stable frosted product.
[0084] Example 3
[0085] A gel cream for a beauty instrument, comprising the following raw materials in parts by weight: 8.0 parts of aluminum nitride-coated chitosan composite nanospheres, 8.0 parts of Ag nanowire / hydroxyapatite microspheres, 60.0 parts of sodium hyaluronate hydrogel, 8.0 parts of cetyl palmitate, 5.0 parts of polyglycerol-10 stearate, 40.0 parts of a mixed solvent of glycerin and deionized water, 2.0 parts of carbomer 940, and 0.5 parts of triethanolamine;
[0086] The aluminum nitride-coated chitosan composite nanospheres are composed of porous aluminum nitride hollow microspheres and chitosan coated in their inner cavities. The outer surface of the porous aluminum nitride hollow microspheres is uniformly distributed with through-hole structures, which are used to achieve the sustained release of chitosan.
[0087] In the mixed solvent of glycerol and deionized water, the volume ratio of glycerol to water is 3:1;
[0088] The Ag nanowire / hydroxyapatite microspheres are composed of hydroxyapatite microspheres and Ag nanowires loaded on the surface thereof; wherein the Ag nanowires are uniformly distributed and stably loaded on the surface of the hydroxyapatite microspheres.
[0089] The preparation method of the aluminum nitride-coated chitosan composite nanospheres of the present embodiment is as follows: in parts by weight, 0.6 parts of chitosan with a deacetylation degree of 85% or higher and a molecular weight of 100 kDa, 12.5 parts of glacial acetic acid and 89.0 parts of deionized water are mixed, stirred at 30°C with a magnetic stirring rate of 700 rpm for 6.0 hours, and filtered through a 0.45 μm filter membrane to prepare a chitosan solution; 105 parts of pre-dried porous aluminum nitride hollow microspheres are mixed with 52 parts of the chitosan solution, and ultrasonically treated at 45°C with an ultrasonic frequency of 42 kHz, a power of 210 W, and a time of 20 minutes, followed by suction filtration under a vacuum degree of 0.06 MPa for 22 minutes, and continued to stand and stir at 25°C for 2.5 hours to form a composite microsphere suspension; 25 0.52 parts of wt% glutaraldehyde aqueous solution was adjusted to pH 6.0 with 0.03wt.% hydrochloric acid aqueous solution and stirred at 300 rpm for 16 min. After washing with deionized water, the mixture was centrifuged at a speed of 5200 rpm for 5.5 min. The precipitate was collected and pre-frozen at -70°C for 13 h, and then transferred to a vacuum freeze dryer and dried at a pressure of ≤10 Pa for 50 h to obtain white to light yellow powdery aluminum nitride-coated chitosan composite nanospheres.
[0090] The preparation method of the porous aluminum nitride hollow microspheres of this embodiment is as follows: 1.1 parts of polystyrene template microspheres with a particle size of 500 nm are dispersed in 52 parts of a mixed solvent of ethanol and deionized water in a volume ratio of 7.5:2.5, 0.11 parts of polyvinyl pyrrolidone are added, and then dispersed for 12 minutes under ultrasonic frequency of 45 kHz and power of 100 W to form a stable suspension; 3.2 parts of aluminum isopropanol are dissolved in 22 parts of anhydrous ethanol and controlled hydrolyzed by adding 2.2 parts of deionized water dropwise, and 0.03 wt.% nitric acid solution is added to adjust the pH to 5.7 to form an aluminum sol precursor; the aluminum sol is added dropwise to the template dispersion system at a rate of 1.5 mL / min, and the stirring speed is maintained at 600 rpm for sol-gel coating reaction for 130 minutes, followed by standing and aging for 13 hours; the supernatant is discarded by centrifugation at a speed of 4500 rpm and the precipitate is collected, and the vacuum degree is -0.10 MPa and a temperature of 62°C for 13 h to obtain porous aluminum nitride hollow precursor microspheres; the precursor was placed in a tube furnace, and the temperature was raised to 1100°C at a rate of 6°C / min, and then an ammonia flow rate of 320 mL / min was introduced for nitridation treatment. The heat preservation time was 125 min to completely convert the aluminum oxide into an aluminum nitride shell. At the same time, the polystyrene template was pyrolyzed at 480°C to form a hollow structure; the obtained hollow microspheres were dispersed in a 32% by mass hydrogen peroxide solution, oxidized and etched at a temperature of 50°C for 50 min, and then washed with deionized water until neutral, finally obtaining porous aluminum nitride hollow microspheres.
[0091] The average diameter of the aluminum nitride-coated chitosan composite nanospheres in this example is 550 nm;
[0092] The average pore diameter of the porous aluminum nitride hollow microspheres is 30 nm;
[0093] The mass ratio of the porous aluminum nitride hollow microspheres to chitosan in the aluminum nitride-coated chitosan composite nano-microspheres of this embodiment is 12:1.
[0094] The preparation method of Ag nanowires / hydroxyapatite microspheres in this embodiment is as follows: 1.0 parts of hydroxyapatite microspheres are dispersed in 20 parts of anhydrous ethylene glycol, 0.051 parts of polyvinyl pyrrolidone are added, and the mixture is treated under ultrasonic frequency of 40 kHz and power of 204 W for 10 min to form a surface activated dispersion system, and the surface modification is completed by maintaining the stirring speed at 360 rpm and the temperature at 28°C for 31 min; 0.17 parts of silver nitrate, 0.30 parts of polyvinyl pyrrolidone and 0.10 parts of 0.101 mol / L ferric chloride solution are added to the dispersion system in sequence, and the mixture is transferred to a three-necked flask and heated to a reaction temperature of 132°C at a heating rate of 5°C / min and subjected to an in-situ reduction reaction at a stirring rate of 620 rpm for 78 min to promote the directional growth of silver ions on the surface of hydroxyapatite nanowires; after the reaction is completed, the mixture is naturally cooled to 23°C and centrifuged at a speed of 6040 The supernatant containing unreacted silver nitrate, free polyvinylpyrrolidone and by-products was removed by rpm separation. The precipitate was collected and washed three times with an ethanol / water mixture with a volume ratio of 1.01:0.99. Finally, it was freeze-dried at -48°C and vacuum ≤10 Pa for 12 h to obtain Ag nanowire / hydroxyapatite microspheres.
[0095] The preparation method of hydroxyapatite microspheres in this embodiment is as follows: in parts by weight, 1.0 part of calcium nitrate tetrahydrate is dissolved in 50 parts of deionized water to form a calcium source solution, and 0.5 part of diammonium hydrogen phosphate is dissolved in 50 parts of deionized water to form a phosphorus source solution. The phosphorus source solution is added dropwise to the calcium source solution at a dropping speed of 1.6 mL / min under a stirring rate of 520 rpm. Ammonia water is simultaneously added to adjust the pH to 10.1 and the temperature is maintained at 28°C to perform a coprecipitation reaction. After the dropwise addition is completed, stirring is continued for 156 minutes to form a hydroxyapatite precursor suspension, which is then transferred to a high-pressure reactor for hydrothermal treatment at a heating rate of 4.2°C / min to a reaction temperature of 126°C. During the hydrothermal treatment stage, the pressure in the reactor is maintained at 0.21 MPa and the holding time is 4.1 hours to allow the precursor to crystallize into hydroxyapatite microspheres. After the reaction is completed, the suspension is centrifuged at a speed of 3600 rpm. The supernatant was removed by rpm separation and the precipitate was collected. It was washed alternately with deionized water and anhydrous ethanol for 4 times and then placed in a vacuum drying oven. Hydroxyapatite microspheres were obtained by treatment at a drying temperature of 62°C and a vacuum degree of -0.092 MPa for 7 h.
[0096] The mass ratio of Ag nanowires to hydroxyapatite microspheres in the Ag nanowire / hydroxyapatite microspheres of this embodiment is 1:7;
[0097] The average diameter of the Ag nanowire / hydroxyapatite microspheres in this example is 500 nm;
[0098] A method for preparing a gel frosting for a beauty instrument according to this embodiment includes the following steps:
[0099] S1. The sodium hyaluronate hydrogel was placed in a clean container and pre-dispersed at a stirring rate of 420 rpm, maintained at a temperature of 26 ° C, and stirred for 16 min to obtain a uniform and fluid sodium hyaluronate hydrogel base system;
[0100] S2. A mixture of glycerol and deionized water was added to the base system described in S1, along with Carbomer 940. Stirring was continued at 520 rpm for 26 minutes to allow the Carbomer to fully disperse and pre-swell. The mixture was then allowed to stand for 8 minutes to eliminate air bubbles and stabilize the system structure.
[0101] S3. Cetyl palmitate and polyglyceryl-10 stearate were mixed and heated to melt at 71 ° C for 13 min under magnetic stirring at a rate of 320 rpm to form a uniform emulsion phase. The emulsion phase was then added to the system obtained in S2 at a dropwise addition rate of 1.6 mL / min. The stirring rate was maintained at 720 rpm and the emulsification was carried out for 21 min to form a primary emulsion system.
[0102] S4. The aluminum nitride-coated chitosan composite nanospheres were added to the primary emulsification system described in S3 and dispersed at a temperature of 36 ° C and a stirring rate of 620 rpm for 21 min;
[0103] S5. Add the Ag nanowires / hydroxyapatite microspheres to the dispersion obtained in S4, maintain the stirring rate at 520 rpm and the temperature at 31°C, and continue stirring for 26 min.
[0104] S6. Triethanolamine was added dropwise to the system obtained in S5, and the mixture was stirred at a stirring rate of 420 rpm for 13 min. The mixture was then degassed under a vacuum degree of 0.068 MPa for 16 min, and finally cooled to 23°C to form a homogeneous and stable frosted product.
[0105] Example 4
[0106] A gel cream for a beauty instrument, comprising the following raw materials in parts by weight: 6.0 parts of aluminum nitride-coated chitosan composite nanospheres, 6.2 parts of Ag nanowire / hydroxyapatite microspheres, 52.0 parts of sodium hyaluronate hydrogel, 6.0 parts of cetyl palmitate, 4.0 parts of polyglycerol-10 stearate, 32.0 parts of a mixed solvent of glycerin and deionized water, 1.0 part of carbomer 940, and 0.4 part of triethanolamine;
[0107] The aluminum nitride-coated chitosan composite nanospheres are composed of porous aluminum nitride hollow microspheres and chitosan coated in their inner cavities. The outer surface of the porous aluminum nitride hollow microspheres is uniformly distributed with through-hole structures, which are used to achieve the sustained release of chitosan.
[0108] In the mixed solvent of glycerol and deionized water, the volume ratio of glycerol to water is 2.2:1;
[0109] The Ag nanowire / hydroxyapatite microspheres are composed of hydroxyapatite microspheres and Ag nanowires loaded on the surface thereof; wherein the Ag nanowires are uniformly distributed and stably loaded on the surface of the hydroxyapatite microspheres.
[0110] The preparation method of the aluminum nitride-coated chitosan composite nanospheres of the present embodiment is as follows: in parts by weight, 0.6 parts of chitosan with a deacetylation degree of 85% or higher and a molecular weight of 80 kDa, 12.1 parts of glacial acetic acid and 88.3 parts of deionized water are mixed, stirred at a magnetic stirring rate of 620 rpm at 28°C for 5.2 hours, and filtered through a 0.45 μm filter membrane to prepare a chitosan solution; 101 parts of pre-dried porous aluminum nitride hollow microspheres are mixed with 50 parts of the chitosan solution, and ultrasonically treated at 43°C with an ultrasonic frequency of 41 kHz, a power of 202 W, and a time of 16 minutes, followed by suction filtration under a vacuum degree of 0.052 MPa for 20 minutes, and continued to stand and stir at 23°C for 2.1 hours to form a composite microsphere suspension; 25 0.50 parts of wt% glutaraldehyde aqueous solution was adjusted to pH 5.8 with 0.022wt.% hydrochloric acid aqueous solution and stirred at 260 rpm for 15 min. After washing with deionized water, the mixture was centrifuged at a speed of 5040 rpm for 5.1 min. The precipitate was collected and pre-frozen at -74°C for 12 h, and then transferred to a vacuum freeze dryer and dried at a pressure of ≤10 Pa for 40 h to obtain white to light yellow powdery aluminum nitride-coated chitosan composite nanospheres.
[0111] The preparation method of the porous aluminum nitride hollow microspheres of this embodiment is as follows: 1.0 part of polystyrene template microspheres with a particle size of 420 nm is dispersed in 50 parts of a mixed solvent of ethanol and deionized water in a volume ratio of 7.1:2.9, 0.10 part of polyvinyl pyrrolidone is added, and the mixture is dispersed for 10 min under ultrasonic frequency of 43 kHz and power of 92 W to form a stable suspension; 3.0 parts of aluminum isopropanol are dissolved in 20 parts of anhydrous ethanol and controlled hydrolyzed by adding 2.0 parts of deionized water dropwise, and 0.022 wt.% nitric acid solution is added to adjust the pH to 5.1 to form an aluminum sol precursor; the aluminum sol is added dropwise to the template dispersion system at a rate of 1.1 mL / min, and the stirring speed is maintained at 520 rpm for sol-gel coating reaction for 122 min, followed by standing and aging for 12 h; the supernatant is discarded by centrifugation at a speed of 4100 rpm and the precipitate is collected, and the vacuum degree is -0.092 MPa and a temperature of 60°C for 12 h to obtain porous aluminum nitride hollow precursor microspheres; the precursor was placed in a tube furnace, and the temperature was raised to 1020°C at a rate of 5°C / min, and then an ammonia flow rate of 304 mL / min was introduced for nitridation treatment. The heat preservation time was 121 min to completely convert the aluminum oxide into an aluminum nitride shell. At the same time, the polystyrene template was pyrolyzed at 456°C to form a hollow structure; the obtained hollow microspheres were dispersed in a 30% by mass hydrogen peroxide solution, oxidized and etched at a temperature of 46°C for 46 min, and then washed with deionized water until neutral, finally obtaining porous aluminum nitride hollow microspheres.
[0112] The average diameter of the aluminum nitride-coated chitosan composite nanospheres in this example is 470 nm;
[0113] The average pore diameter of the porous aluminum nitride hollow microspheres is 25 nm;
[0114] The mass ratio of the porous aluminum nitride hollow microspheres to chitosan in the aluminum nitride-coated chitosan composite nano-microspheres of this embodiment is 10:1.
[0115] The preparation method of Ag nanowires / hydroxyapatite microspheres of this embodiment is as follows: 1.1 parts of hydroxyapatite microspheres are dispersed in 22 parts of anhydrous ethylene glycol, 0.055 parts of polyvinyl pyrrolidone is added, and the mixture is treated under ultrasonic frequency of 42 kHz and power of 220 W for 12 min to form a surface activated dispersion system, and the surface modification is completed by maintaining a stirring speed of 400 rpm and a temperature of 30°C for 35 min; 0.18 parts of silver nitrate, 0.32 parts of polyvinyl pyrrolidone and 0.11 parts of ferric chloride solution with a concentration of 0.105 mol / L are added to the dispersion system in sequence, and the mixture is transferred to a three-necked flask and heated to a reaction temperature of 140°C at a heating rate of 6°C / min and subjected to an in-situ reduction reaction for 90 min under a stirring rate of 700 rpm to promote the directional growth of silver ions on the surface of hydroxyapatite nanowires; after the reaction is completed, the mixture is naturally cooled to 25°C and centrifuged at a speed of 6200 The supernatant containing unreacted silver nitrate, free polyvinylpyrrolidone and by-products was removed by rpm separation. The precipitate was collected and washed four times with an ethanol / water mixture of a volume ratio of 1.05:0.95. Finally, it was freeze-dried at -45°C and a vacuum degree of ≤10 Pa for 14 h to obtain Ag nanowire / hydroxyapatite microspheres.
[0116] The preparation method of hydroxyapatite microspheres in this embodiment is as follows: in parts by weight, 1.2 parts of calcium nitrate tetrahydrate are dissolved in 55 parts of deionized water to form a calcium source solution, and 0.6 parts of diammonium hydrogen phosphate are dissolved in 55 parts of deionized water to form a phosphorus source solution. The phosphorus source solution is added dropwise to the calcium source solution at a dropping speed of 2 mL / min under a stirring rate of 600 rpm, and ammonia water is simultaneously added to adjust the pH to 10.5 and maintain the temperature at 30°C to perform a coprecipitation reaction. After the dropwise addition is completed, stirring is continued for 180 minutes to form a hydroxyapatite precursor suspension, which is then transferred to a high-pressure reactor for hydrothermal treatment at a heating rate of 5°C / min to a reaction temperature of 130°C. During the hydrothermal treatment stage, the pressure in the reactor is maintained at 0.25 MPa and the holding time is 4.5 hours to allow the precursor to crystallize into hydroxyapatite microspheres. After the reaction is completed, the suspension is centrifuged at a speed of 4000. The supernatant was removed by rpm separation and the precipitate was collected. It was washed alternately with deionized water and anhydrous ethanol for 5 times and then placed in a vacuum drying oven. Hydroxyapatite microspheres were obtained by treatment at a drying temperature of 70°C and a vacuum degree of -0.10 MPa for 8 h.
[0117] The mass ratio of Ag nanowires to hydroxyapatite microspheres in the Ag nanowire / hydroxyapatite microspheres of this embodiment is 1:5;
[0118] The average diameter of the Ag nanowire / hydroxyapatite microspheres in this example is 600 nm;
[0119] A method for preparing a gel frosting for a beauty instrument according to this embodiment includes the following steps:
[0120] S1. The sodium hyaluronate hydrogel was placed in a clean container and pre-dispersed at a stirring rate of 500 rpm, maintained at a temperature of 30 ° C, and stirred for 20 min to obtain a uniform and fluid sodium hyaluronate hydrogel base system;
[0121] S2. A mixture of glycerol and deionized water was added to the base system described in S1, along with Carbomer 940. The mixture was stirred at 600 rpm for 30 min to allow the Carbomer to fully disperse and pre-swell. The mixture was then allowed to stand for 10 min to eliminate bubbles and stabilize the system structure.
[0122] S3. Cetyl palmitate and polyglyceryl-10 stearate were mixed and heated to melt at 75 ° C for 15 min under magnetic stirring at a rate of 400 rpm to form a uniform emulsion phase. The emulsion phase was then added to the system obtained in S2 at a dropwise addition rate of 2 mL / min. The stirring rate was maintained at 800 rpm and the emulsification was carried out for 25 min to form a primary emulsion system.
[0123] S4. The aluminum nitride-coated chitosan composite nanospheres were added to the primary emulsification system of S3 and dispersed at a temperature of 40 ° C and a stirring rate of 700 rpm for 25 min;
[0124] S5. Add the Ag nanowires / hydroxyapatite microspheres to the dispersion obtained in S4, maintain the stirring rate at 600 rpm and the temperature at 35°C, and continue stirring for 30 min.
[0125] S6. Triethanolamine was added dropwise to the system obtained in S5, and the mixture was stirred at a stirring rate of 500 rpm for 15 min. The mixture was then degassed under a vacuum degree of 0.08 MPa for 20 min, and finally cooled to 25°C to form a homogeneous and stable frosted product.
[0126] Comparative Example 1
[0127] The method is basically the same as Example 1, except that during the preparation of aluminum nitride-coated chitosan composite nanospheres, glutaraldehyde aqueous solution is not used for cross-linking. Instead, the porous aluminum nitride hollow microspheres are directly mixed with the chitosan solution and then dried, resulting in the chitosan not being firmly coated in the inner cavity of the aluminum nitride hollow microspheres.
[0128] Comparative Example 2
[0129] The method is basically the same as Example 1, except that in the preparation method of the porous aluminum nitride hollow microspheres, polyvinyl pyrrolidone is not used as a dispersant, but the polystyrene template microspheres are directly dispersed in the mixed solvent.
[0130] Comparative Example 3
[0131] The method is basically the same as Example 1, except that during the preparation of the porous aluminum nitride hollow microspheres, the nitriding temperature is 800° C., which results in the failure to completely convert the aluminum oxide into the aluminum nitride shell.
[0132] Comparative Example 4
[0133] The method is basically the same as Example 1, except that during the preparation of Ag nanowires / hydroxyapatite microspheres, ferric chloride solution was not added as an auxiliary reducing agent, and only silver nitrate and polyvinyl pyrrolidone were used for the reaction, resulting in the inability of silver ions to effectively grow into nanowire structures on the hydroxyapatite surface.
[0134] Comparative Example 5
[0135] The method is basically the same as Example 1, except that the porous aluminum nitride hollow microspheres are not coated with chitosan.
[0136] Comparative Example 6
[0137] The method is basically the same as Example 1, except that silver nanowires are not prepared on the surface of the hydroxyapatite microspheres.
[0138] Comparative Example 7
[0139] The method is basically the same as Example 1, except that the porous aluminum nitride hollow microspheres are not coated with chitosan, and the two are added separately.
[0140] Performance testing:
[0141] Frost thermal conductivity: The thermal conductivity of frost is measured using the heat flow method (ASTM D5470). Frost is evenly applied between two parallel copper plates. The upper plate is heated while the lower plate is maintained at a constant temperature. The steady-state heat flux and temperature gradient are measured, and the thermal conductivity (λ = Q × d / (A × ΔT)) is calculated.
[0142] Antibacterial properties: Staphylococcus aureus (ATCC 6538) and Escherichia coli (ATCC 25922) were selected, and bacterial suspensions (10^6 CFU / mL) were prepared and evenly spread on Mueller-Hinton agar plates. Frost samples (50 mg) were filled into Oxford cups, and the diameters of the inhibition zones were measured after incubation at 37°C for 24 hours.
[0143] Silver ion release kinetics: Frost samples (1 g) were immersed in deionized water (10 mL) and shaken at 37°C in the dark. Samples were collected at 0, 6, 24, and 48 h, filtered through a 0.22 μm filter, and the amount of Ag+ released was quantified by inductively coupled plasma mass spectrometry (ICP-MS).
[0144] Rheological properties: A rotational rheometer was used to measure the viscosity-shear rate curve (0.1-100 s^-1) and the storage modulus (G')-loss modulus (G'') of the gel at 25°C as a function of frequency.
[0145] The frosting properties of Examples 1 to 4 and Comparative Examples 1 to 7 are summarized in Table 1.
[0146] Table 1 Summary of the performance of frosting in Examples 1 to 4 and Comparative Examples 1 to 7
[0147]
[0148] As can be seen from Table 1, the degree of nitridation of aluminum nitride directly determines the construction integrity of its thermal conductivity path. Incomplete nitridation will lead to a decrease in the thermal conductivity of the ceramic shell. Whether chitosan is cross-linked and coated affects its fixation and sustained-release properties in the microsphere structure, thereby affecting the stability and release efficiency of the antibacterial component. The formation of silver nanowires depends on the presence of an auxiliary reducing agent. The absence of an auxiliary reducing agent will result in the inability of silver ions to be directionally reduced to a linear structure, affecting the formation of an efficient thermal conductivity and antibacterial pathway. The structural uniformity and surface activation degree of hydroxyapatite determine the loading density and distribution uniformity of silver nanowires, thereby affecting the release behavior of silver and the synergistic thermal conductivity effect. The use or non-use of a dispersant such as polyvinyl pyrrolidone directly affects the nucleation of the nanostructure. and dispersion stability, affecting the integrity of the microsphere structure and interface bonding; whether aluminum nitride and chitosan form an effective composite structure is related to the synergistic realization of the material's thermal conductivity and antibacterial functions, and structural separation will lead to a weakening of the synergistic effect; the simultaneous presence of silver nanowires and chitosan makes the antibacterial mechanism have a dual path of fast-acting and sustained-release, and the absence of any component will make the antibacterial effect show a staged or unstable performance; the integrity of the porous structure determines the specific surface area of the microspheres and the uniformity of component distribution, thereby affecting the heat-mass synergistic transfer ability and mechanical stability of the overall system; the uniformity of the spatial distribution of components in the system and the interface compatibility determine the network structure and rheological behavior of the frost, thereby affecting its film-forming and stability in use.
[0149] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that any equivalent structural transformations made within the scope of the present invention using the contents of the present invention's description and drawings should be included within the scope of protection of the claims of the present invention.
Claims
1. A gel frosting for beauty equipment, characterized in that: The invention comprises the following raw materials in parts by weight: 4.0-8.0 parts of aluminum nitride-coated chitosan composite nanospheres, 3.5-8.0 parts of Ag nanowires / hydroxyapatite microspheres, 40.0-60.0 parts of sodium hyaluronate hydrogel, 4.0-8.0 parts of cetyl palmitate, 2.0-5.0 parts of polyglycerol-10 stearate, 20.0-40.0 parts of a mixed solvent of glycerol and deionized water, 0.5-2.0 parts of carbomer 940, and 0.2-0.5 parts of triethanolamine; The aluminum nitride-coated chitosan composite nanospheres are composed of porous aluminum nitride hollow microspheres and chitosan coated in their inner cavities; wherein the outer surface of the porous aluminum nitride hollow microspheres is uniformly distributed with a through-hole structure, which is used to achieve the sustained release of chitosan; In the mixed solvent of glycerol and deionized water, the volume ratio of glycerol to water is 1:1 to 3:1; The Ag nanowire / hydroxyapatite microspheres are composed of hydroxyapatite microspheres and Ag nanowires loaded on their surfaces; wherein the Ag nanowires are evenly distributed and stably loaded on the surfaces of the hydroxyapatite microspheres; The aluminum nitride-coated chitosan composite nanospheres are prepared by preparing a solution of chitosan with a deacetylation degree of 85% or higher, treating the solution with pre-dried porous aluminum nitride hollow microspheres at an ultrasonic frequency of 38 to 42 kHz at 40 to 45° C. for 10 to 20 minutes, vacuum filtering, cross-linking with glutaraldehyde, and then freeze-drying. The porous aluminum nitride hollow microspheres are coated with a sol-gel in an ethanol-water mixed solvent containing polyvinyl pyrrolidone using a polystyrene template method, heating the solution to 900 to 1100° C. at a heating rate of 4 to 6° C. / min, introducing ammonia at a flow rate of 280 to 320 mL / min, and finally etching with hydrogen peroxide to obtain the prepared nanospheres. The Ag nanowire / hydroxyapatite microspheres are prepared by surface-activating the hydroxyapatite microspheres in anhydrous ethylene glycol, then adding silver nitrate, polyvinyl pyrrolidone, and ferric chloride solution, and performing an in-situ reduction reaction at 120-140°C for 60-90 minutes. The hydroxyapatite microspheres are prepared by coprecipitating calcium nitrate tetrahydrate with diammonium hydrogen phosphate, followed by crystallization by hydrothermal treatment at 120-130°C for 3.5-4.5 hours.
2. The gel frosting for beauty equipment according to claim 1, characterized in that: The preparation method of the aluminum nitride-coated chitosan composite nanospheres is as follows: in parts by weight, 0.5-0.6 parts of chitosan with a molecular weight of 50-100 kDa, 11.5-12.5 parts of glacial acetic acid and 87.0-89.0 parts of deionized water are mixed, stirred at 25-30°C with a magnetic stirring rate of 500-700 rpm for 4.0-6.0 hours, and filtered through a 0.45 μm filter membrane to prepare a chitosan solution; 95-105 parts of pre-dried porous aluminum nitride hollow microspheres are mixed with 48-52 parts of the chitosan solution, and ultrasonically treated at 40-45°C with an ultrasonic frequency of 38-42 kHz, a power of 190-210 W, and a time of 10-20 minutes, and then filtered under a vacuum degree of 0.04-0.06 MPa for 18-22 minutes. min, and continue to stir at 20-25°C for 1.5-2.5 hours to form a composite microsphere suspension; 0.48-0.52 parts of a 25wt% glutaraldehyde aqueous solution were added dropwise to the suspension, the pH was adjusted to 5.5-6.0 with a 0.01-0.03wt.% hydrochloric acid aqueous solution, and the suspension was stirred at 200-300 rpm for 14-16 minutes. After washing with deionized water, the suspension was centrifuged at a speed of 4800-5200 rpm for 4.5-5.5 minutes. The precipitate was collected and pre-frozen at -80--70°C for 11-13 hours, and then transferred to a vacuum freeze dryer and dried at a pressure of ≤10 Pa for 24-50 hours to obtain white to light yellow powdery aluminum nitride-coated chitosan composite nanospheres.
3. The gel frosting for beauty equipment according to claim 1, characterized in that: The porous aluminum nitride hollow microspheres are prepared by dispersing, by weight, 0.9 to 1.1 parts of polystyrene template microspheres having a particle size of 300 to 500 nm in 48 to 52 parts of a mixed solvent having a volume ratio of ethanol to deionized water of 6.5:3.5 to 7.5:2.5, adding 0.09 to 0.11 parts of polyvinyl pyrrolidone, and performing a dispersion treatment under ultrasonic conditions of 40 to 45 kHz and 80 to 100 W for 8 to 12 minutes to form a stable suspension. 2.8-3.2 parts of aluminum isopropoxide were dissolved in 18-22 parts of anhydrous ethanol and controlled hydrolysis was carried out by dropwise addition of 1.8-2.2 parts of deionized water, and 0.01-0.03 wt.% nitric acid solution was added to adjust the pH to 4.3-5.7 to form an aluminum sol precursor; the aluminum sol was added dropwise at a rate of 0.5-1.5 mL / min to the template dispersion system, and the stirring speed was maintained at 400-600 rpm to carry out the sol-gel coating reaction for 110-130 min, followed by standing and aging for 11-13 h; the supernatant was discarded by centrifugation at a speed of 3500-4500 rpm and the precipitate was collected and dried under vacuum of -0.08-0.10 MPa and a temperature of 58-62°C for 11-13 h. h to obtain porous aluminum nitride hollow precursor microspheres; placing the precursor in a tube furnace for nitridation treatment to completely convert aluminum oxide into an aluminum nitride shell, and simultaneously pyrolyzing the polystyrene template at 420-480°C to form a hollow structure; the obtained hollow microspheres are dispersed in a 28-32% by mass hydrogen peroxide solution, subjected to oxidative etching treatment at a temperature of 40-50°C for 40-50 min, and then washed with deionized water until neutral, to finally obtain porous aluminum nitride hollow microspheres.
4. The gel frosting for beauty equipment according to claim 1, characterized in that: The average diameter of the aluminum nitride-coated chitosan composite nanospheres is 350-550 nm; the average pore diameter of the porous aluminum nitride hollow microspheres is 18-30 nm.
5. The gel frosting for beauty equipment according to claim 1, characterized in that: The mass ratio of the porous aluminum nitride hollow microspheres to chitosan in the aluminum nitride-coated chitosan composite nano-microspheres is 8:1-12:
1.
6. The gel frosting for beauty equipment according to claim 1, characterized in that: The preparation method of the Ag nanowire / hydroxyapatite microspheres is as follows: in parts by weight, 0.9-1.1 parts of hydroxyapatite microspheres are dispersed in 18-22 parts of anhydrous ethylene glycol, 0.045-0.055 parts of polyvinyl pyrrolidone are added, and then treated under ultrasonic frequency of 38-42 kHz and power of 180-220 W for 8-12 minutes to form a surface activated dispersion system, and the stirring speed is maintained at 300-400 rpm and the temperature is maintained at 25-30°C for 25-35 minutes to complete the surface modification; 0.16-0.18 parts of silver nitrate, 0.28-0.32 parts of polyvinyl pyrrolidone and a concentration of 0.095-0.105 are sequentially added to the dispersion system. 0.09-0.11 parts of a mol / L ferric chloride solution were transferred to a three-necked flask and heated to a reaction temperature of 120-140°C at a heating rate of 4-6°C / min. An in-situ reduction reaction was carried out at a stirring rate of 500-700 rpm for 60-90 min to promote the directional growth of silver ions on the hydroxyapatite surface. After the reaction, the solution was naturally cooled to 20-25°C. The supernatant containing unreacted silver nitrate, free polyvinylpyrrolidone, and by-products was separated by centrifugation at a speed of 5800-6200 rpm. The precipitate was collected and washed repeatedly with an ethanol / water mixture with a volume ratio of 0.95:1.05-1.05:0.95 for 2-4 times. Finally, the solution was freeze-dried at a temperature of -50--45°C and a vacuum degree of ≤10 Pa for 10-14 h to prepare Ag nanowire / hydroxyapatite microspheres.
7. The gel frosting for beauty equipment according to claim 6, characterized in that: The preparation method of the hydroxyapatite microspheres is as follows: in parts by weight, 0.8-1.2 parts of calcium nitrate tetrahydrate are dissolved in 45-55 parts of deionized water to form a calcium source solution, and 0.4-0.6 parts of diammonium hydrogen phosphate are dissolved in 45-55 parts of deionized water to form a phosphorus source solution. The phosphorus source solution is added dropwise to the calcium source solution at a stirring rate of 400-600 rpm at a dropwise addition rate of 1-2 mL / min. Ammonia water is simultaneously added to adjust the pH to 9.5-10.5 and the temperature is maintained at 25-30°C to perform a coprecipitation reaction. After the dropwise addition is completed, stirring is continued for 120-180 minutes to form a hydroxyapatite precursor suspension, which is then transferred to a high-pressure reactor for hydrothermal treatment at a heating rate of 3-5°C / min to a reaction temperature of 120-130°C. During the hydrothermal treatment stage, the pressure in the reactor is maintained at 0.15-0.25 MPa and the holding time is 3.5-4.5 h to crystallize the precursor into hydroxyapatite microspheres. After the reaction, the supernatant was removed by centrifugation at a speed of 3000-4000 rpm and the precipitate was collected. The precipitate was washed alternately with deionized water and anhydrous ethanol for 3-5 times and then placed in a vacuum drying oven for 6-8 h at a drying temperature of 50-70°C and a vacuum degree of -0.08-0.10 MPa to obtain hydroxyapatite microspheres.
8. The gel frosting for beauty equipment according to claim 1, characterized in that: The mass ratio of the Ag nanowires to the hydroxyapatite microspheres in the Ag nanowire / hydroxyapatite microspheres is 1:10 to 1:
5.
9. The gel frosting for beauty equipment according to claim 1, characterized in that: The average diameter of the Ag nanowire / hydroxyapatite microspheres is 350-600 nm.
10. The method for preparing gel frosting for beauty equipment according to claim 1, wherein: The following steps are involved: S1. Pre-disperse the sodium hyaluronate hydrogel in a clean container at a stirring rate of 300-500 rpm and a temperature of 20-30°C for 10-20 minutes to obtain a uniform and fluid sodium hyaluronate hydrogel base system. S2. Add a mixed solvent of glycerol and deionized water to the base system described in S1, along with Carbomer 940. Stir continuously at 400-600 rpm for 20-30 minutes to fully disperse and pre-swell the Carbomer. Then, let the mixture stand for 5-10 minutes to eliminate air bubbles and stabilize the system structure. S3. Cetyl palmitate and polyglyceryl-10 stearate were mixed and heated to melt at 65-75°C for 10-15 min under magnetic stirring at 200-400 rpm to form a uniform emulsion. This emulsion was then added to the mixture obtained in S2 at a dropwise rate of 1-2 mL / min. The mixture was stirred at 600-800 rpm for 15-25 min to form a primary emulsion. S4. The aluminum nitride-coated chitosan composite nanospheres were added to the primary emulsification system described in S3 and dispersed at a temperature of 30 to 40 ° C and a stirring rate of 500 to 700 rpm for 15 to 25 min; S5. The Ag nanowires / hydroxyapatite microspheres were added to the dispersion obtained in S4, and the stirring rate was maintained at 400-600 rpm and the temperature was maintained at 25-35 ° C. The stirring was continued for 20-30 min. S6. Triethanolamine is added dropwise to the mixture obtained in S5. The mixture is stirred at a stirring rate of 300-500 rpm for 10-15 minutes. The mixture is then degassed under a vacuum of 0.05-0.08 MPa for 10-20 minutes. The mixture is finally cooled to 20-25°C to form a homogeneous and stable frosted product.
Citation Information
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