Freeze-dried blusher composition and preparation method thereof

Abstract

The invention discloses a freeze-dried blusher composition and a preparation method thereof, and belongs to the technical field of cosmetics. The composition comprises a filler, a water phase, an emollient and an emulsifier, the filling agent is one or more of modified starch, synthetic fluorophlogopite, boron nitride and the like; the water phase is deionized water, a humectant and the like; the emollient is a polydimethylsiloxane derivative, jojoba oil and the like; and the emulsifier is sorbitan stearate and the like. The preparation method comprises the following steps: weighing the raw materials, crushing and mixing the filler into a phase A, heating a water phase into a phase B, and dissolving the emollient and the emulsifier into a phase C; emulsifying, homogenizing and cooling the phase C and the phase B into a phase D, and mixing and pressing the phase A and the phase D; performing vacuum freeze drying, including pre-freezing, sublimation drying and heating drying, and finally performing constant-temperature and constant-humidity storage. The embodiment shows that the water loss rate of the composition is 2.5-4%, the hardness is low, the stability is high, the smoothness, the ductility, the skin fitting degree and the coloring property are superior to those of a contrast, the preparation time is 12.87-17.7 h, the energy consumption is reasonable, and the composition has a good market prospect.

Description

Technical Field

[0001] This invention belongs to the field of cosmetic technology, specifically, it relates to a freeze-dried blush composition and its preparation method. Background Technology

[0002] As an important part of the global consumer goods market, the cosmetics industry has always pursued softness, skin-adherence, and long-lasting color in powder makeup. However, due to limitations in natural raw materials and technology, the products are fragile and have poor stability.

[0003] With the advent of the Industrial Revolution, cosmetics entered a modern era in the late 19th and early 20th centuries. Western brands such as Max Factor and Elizabeth Arden introduced synthetic pigments and oil-based formulas, driving the shift from handmade preparation to large-scale production of powder products. In China, Xie Fuchun was founded in 1829, specializing in duck egg powder and face powder, becoming a pioneer of domestic products; in 1862, Kong Fengchun's goose egg powder was even selected as a royal tribute, marking the rise of domestic powder cosmetics. In the 1930s, Shanghai Guang Sheng Hang (the predecessor of Shanghai Jahwa) launched the Shuangmei brand powder compact and Ya Shuang cream, and Bai Que Ling's skin care balm also became popular. These products were based on mineral powders such as talc and mica, realizing the transformation from traditional rouge to modern pressed powder. After World War II, the development of petrochemicals ushered in the "mineral oil era" (1940s-1970s). Mineral oil and synthetic thickeners were added to powder cosmetics, reducing costs but highlighting safety issues, such as frequent lead poisoning incidents. In the 1980s, the "era of natural ingredients" emerged. The Japanese melanosis incident prompted the industry to turn to plant extracts, but the immature technology of natural powder mixing led to products that were prone to causing allergies and had limited efficacy. From the 1990s to the early 21st century, the "era of antioxidants" arrived. Powder products incorporated active ingredients such as vitamins C and E to target free radical aging, but still faced challenges such as powder fallout and hard texture.

[0004] In recent years, with consumers' increasing demands for makeup quality, powder makeup products have become increasingly diverse in variety and texture, including pressed powder, baked powder, wet powder, and aerosol powder. These innovations stem from consumers' needs for convenient, multi-functional, and personalized makeup looks: younger consumers seek natural blending and long-lasting wear, while mid-to-high-end users prioritize lightweight and environmentally friendly ingredients. For example, pressed powder achieves portability through high-pressure molding but is fragile; baked powder enhances density through high-temperature baking but sacrifices softness; wet powder adds a water-oil phase for moisturizing but has a short shelf life. In the blush market, as the core of facial makeup, products need to balance even color application, comfortable feel, and stability to create a sculpted facial contour. Global brands such as L'Oréal and Shiseido dominate the market, launching numerous innovative blushes, but domestic brands such as Perfect Diary and Florasis are rapidly gaining market share through traditional Chinese design and natural powders.

[0005] Despite significant advancements in powder makeup, traditional pressed powder blushes still suffer from a problem of excessive fallout. The pressing process relies on mechanically pressing powder and binders (such as mica, talc, and magnesium stearate) together, but the weak friction between powder particles means that even slight bumps during use cause dust to scatter. This not only results in waste but also pollutes the air and clothing, affecting makeup evenness, especially in dry or windy environments where fallout is exacerbated. Studies show that traditional pressed powder can have a fallout rate of 10-20%, causing irritation or allergies for users with sensitive skin. Furthermore, the color payoff of pressed powder depends on the pigment ratio, but it is prone to oxidation and discoloration, with a lasting effect of only 4-6 hours, insufficient for all-day makeup needs. Consumer feedback indicates that over 60% of users complain about the inconvenience of using pressed powder, requiring additional tools and reducing portability.

[0006] In contrast, while baked powder blush is less prone to fallout, its texture is harder and the surface is prone to crusting, making it difficult to pick up and resulting in a poor user experience. The baking process involves baking moist powder at medium to high temperatures (40-70℃) to form a dense, blocky structure, reducing dust shedding. However, the high temperature causes the powder to sinter, increasing its hardness to a Shore A of 20-30, far exceeding the ideal 10-15. This makes it difficult to pick up powder evenly with a brush, easily pulling on the skin or causing patchy makeup. The crusting on the surface stems from uneven moisture evaporation and binder polymerization, worsening after several months of storage, affecting adherence and spreadability. Tests show that baked powder blush scores only 3-4 out of 5 in spreadability, requiring multiple layers for application, wasting product and prolonging makeup time. Furthermore, the heat treatment of baking powder may damage active ingredients such as vitamins, reducing moisturizing effects and leading to dry lines or makeup fading. In high-temperature and high-humidity environments, baked powder is unstable, easily softening or cracking, resulting in a market return rate as high as 5%.

[0007] Wet powder and aerosol powder, as emerging forms, attempt to address the aforementioned shortcomings, but limitations remain. Wet powder uses a water-oil emulsion matrix to encapsulate powder, providing a silky feel, but its high water content (20-30%) makes it prone to bacterial growth, resulting in a shelf life of only 6-12 months, and it is prone to cracking after drying. Aerosol powder utilizes spray technology to achieve contactless makeup application, facilitating blending, but the uneven powder fineness easily clogs the nozzle, and it poses a high risk of environmental pollution (containing propellants). While these products improve softness, they do not fundamentally solve the balance between stability and color payoff, resulting in a consumer satisfaction rate of only 70%. Overall, current powder blushes struggle to simultaneously meet the demands for softness and smoothness, adherence without feeling heavy, even color application, and resistance to fading, especially in a fast-paced lifestyle where users expect products to "blend instantly with a single swipe and last forever with a single touch."

[0008] To address these challenges, the industry is exploring new drying technologies such as spray drying and freeze-drying. Spray drying rapidly evaporates moisture, forming microsphere powders and improving flowability, but it consumes a lot of energy and the particles are prone to agglomeration, affecting uniformity. Freeze-drying (vacuum freeze-drying), as a low-temperature vacuum sublimation technology, has been used in food and pharmaceuticals since the mid-20th century and has recently expanded to cosmetics. Freeze-drying preserves the porous structure of powders, improving softness and absorbency, reducing heat damage, and is suitable for protecting active ingredients. In the foundation and eyeshadow fields, freeze-dried products have achieved water loss control of 3-5%, a 20% reduction in hardness, and a 15% improvement in color payoff. However, in blush applications, the freeze-drying process parameters (such as pre-freezing temperature and sublimation pressure) are not sufficiently optimized, resulting in products that are brittle or contain too much water, leading to poor stability. Existing freeze-dried blushes are mostly simple transplants of food processes, without adjustments for the oil-water emulsification of color cosmetics, resulting in long preparation times (over 20 hours), high energy consumption, and uneconomical production. Summary of the Invention

[0009] The problem to be solved

[0010] The technical problem this invention aims to solve is that existing powder-based makeup products, especially traditional pressed and baked powder blushes, have significant shortcomings in terms of softness, skin adherence, color payoff, and stability, failing to fully meet consumers' demands for high-quality makeup. Specifically, while traditional pressed powder blushes are convenient to carry and shape, the weak bonding between powder particles easily leads to fallout, resulting in significant dust dispersion during use. This not only wastes the product but can also pollute the air and clothing, affecting makeup evenness and environmental hygiene. Especially in dry or windy conditions, the fallout rate can reach 10-20%, easily causing irritation or allergic reactions in sensitive skin. Furthermore, the color payoff of pressed powder blush depends on the pigment ratio, but it is prone to oxidation and discoloration, with a lasting effect of only 4-6 hours. Its poor spreadability prevents natural blending, leading to low consumer satisfaction. On the other hand, baked powder blush reduces fallout through high-temperature baking, but its texture is relatively hard (Shore hardness 20-30), the surface is prone to crusting, making it difficult to pick up the powder. It requires vigorous brushing during application, which can pull on the skin, causing discomfort or patchy makeup. The skin feel is rough, and its spreadability and adherence score is only 3-4 out of 5. The high-temperature process may also damage active ingredients such as vitamins and moisturizers, leading to dryness and brittleness. After several months of storage, stability decreases, with a breakage rate exceeding 30% in drop tests, and a shortened shelf life. Emerging wet powder and aerosol powders attempt to improve softness, but their high water content (20-30%) makes them prone to bacterial growth, resulting in a shelf life of only 6-12 months. After drying, they are prone to cracking or fading. Aerosol powder sprays are convenient to apply, but uneven particle size can clog nozzles, and the presence of propellants poses a high risk of environmental pollution. While these products improve some aspects of the skin feel, they do not solve core problems such as unstable oil-water emulsification, difficulty in controlling water content, and high energy consumption. Their long preparation time (over 20 hours) and high cost make them unsuitable for large-scale production. In the application of freeze-drying technology, current methods are mostly adapted from the food industry and have not been optimized for pigment filling and moisturizing phases in makeup. They face technical challenges such as pre-freezing ice crystals damaging the powder structure, uneven sublimation pressure leading to porous collapse, and excessive residual water during baking. The water loss rate is difficult to control within the ideal range of 2.5-4%, resulting in high hardness, low color a* value (<25), poor stability, brittleness, or microbial growth. Furthermore, existing freeze-dried blushes neglect the supporting and luminous balance of fillers (such as mica and boron nitride), the soft retention of moisturizers (such as glycerin), and the uniform dispersion of emulsifiers (such as sorbitan stearate). This leads to products that are not soft to the touch, have poor skin adhesion, and uneven color application, resulting in overall performance inferior to traditional products and limited market application. These problems not only affect the consumer experience but also hinder the innovative development of domestic makeup brands, urgently requiring a new solution that comprehensively combines softness, stability, and economy.

[0011] Technical solution

[0012] To solve the above problems, the present invention adopts the following technical solution.

[0013] A freeze-dried blush composition, by weight, comprises 40-70 parts filler, 30-40 parts aqueous phase, 4-10 parts emollient, and 1-4 parts emulsifier; wherein the aqueous phase is selected from one or more combinations of deionized water, moisturizer, plant fermentation broth, and plant flower water; wherein the emollient is selected from one or more combinations of polydimethylsiloxane and its derivatives, triglycerides and their derivatives, jojoba oil, sunflower seed oil, castor oil, coconut oil, grape seed oil, shea butter, meadowfoam seed oil, macadamia nut oil, olive oil, palm oil, squalane, cocoa butter, jojoba butter, glycolipid, octyl dodecanol, caprylic / capric triglyceride, and cocoyl alcohol-caprylic / capric triglyceride.

[0014] Preferably, the filler is selected from one or more combinations of modified starch, synthetic fluorophlogopite, sericite, talc, silica, lake, polymethyl methacrylate, polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer, vinyl polydimethylsiloxane / polymethylsiloxysilsesquioxane cross-linked polymer, polydimethylsiloxane cross-linked polymer, boron nitride, organosilicon elastomer, calcium carbonate, pearl powder, silk powder, zinc stearate, aluminum stearate, lauroyl lysine, polymethylsilsesquioxane, kaolin, nylon-12, diamond powder, zinc oxide, barium sulfate, hydroxyapatite, aluminum oxide, bismuth oxychloride, aluminum hydroxide, magnesium myristate, and nephrite powder.

[0015] Preferably, the moisturizer is selected from one or more combinations of glycerin, sodium hyaluronate, 1,3-propanediol, 1,2-hexanediol, cetyl alcohol, and trehalose.

[0016] Preferably, the emulsifier is selected from one or more combinations of sorbitan stearate, sorbitan isostearate, sorbitan sesquioleate, and polysorbate-60.

[0017] A method for preparing the freeze-dried blush composition as described above includes the following steps: A. Weighing filler, aqueous phase, emollient, and emulsifier according to the mass ratio; B. Grinding and mixing the filler in a pulverizer until uniformly mixed to obtain phase A; C. Mixing the aqueous phase and emollient in an emulsifying pot until uniformly mixed, and heating to 80-90℃ for later use, which is phase B; D. Heating the emollient and emulsifier to 80℃ until the solid is completely dissolved and stirred uniformly, which is phase C; E. Adding phase C to the emulsifying pot and emulsifying and homogenizing it with phase B, the emulsification temperature is 75-85℃, the homogenization speed is 2000-4000 rpm, the time is 3-8 min, and then cooling to 25℃ to obtain phase B. Phase D; F. Mix Phase A and Phase D evenly, and press them onto a plastic tray using a mold to obtain a freeze-dried blush composition; G. Place the composition in a freeze dryer for vacuum freeze-drying, including pre-freezing, sublimation drying, and temperature drying. Pre-freezing is freezing at -30℃ to -50℃ for 0.5h to 3h; sublimation drying is freezing and sublimation at -30℃ to -40℃ and negative pressure of 1Pa to 50Pa for 0.5h to 3h, and then slowly heating to 20℃ and holding at pressure for 6-9h; temperature drying is baking at 20℃ to 55℃ under negative pressure for 3.5-6h; finally, remove the composition and store it in a constant temperature and humidity environment to obtain the freeze-dried blush composition.

[0018] Preferably, the filler in step B consists of 20.9 parts mica, 14.5 parts synthetic fluorophlogopite, 0.9 parts boron nitride, 1.6 parts kaolin, 8.8 parts silica, 3.3 parts polymethylsilsesquioxane, 1.7 parts CI15850, 1.9 parts CI77491, and 1.5 parts CI77007.

[0019] Preferably, the aqueous phase in step C consists of 36.3 parts deionized water, and the humectant consists of 0.32 parts dipropylene glycol and 1.3 parts glycerin.

[0020] Preferably, the emollient in step D consists of 1.7 parts hydrogenated polydecene, 0.9 parts bis-diglyceride polyacryloyl adipate-2, 1.5 parts caprylic / capric triglyceride, and 0.72 parts ethylhexylglycerin / caprylyl glycol. The emulsifier consists of 0.27 parts C12-20 acid PEG-8 ester, 0.14 parts cetyl alcohol, 0.45 parts sorbitan isostearate, and 1.3 parts sorbitan stearate.

[0021] Beneficial effects

[0022] The beneficial effects of this invention lie in its optimization of the formulation ratio of the freeze-dried blush composition and the vacuum freeze-drying process parameters. This significantly solves the problems of traditional pressed powder blush (prone to powder fallout), baked powder blush (hard texture and difficult to pick up), and existing freeze-dried products (poor stability and uneven color application). The invention achieves a comprehensive improvement in product softness and smoothness against the skin, even and long-lasting color application, mechanical stability, and microbial safety. The preparation process is highly efficient and economical, offering significant technical and market advantages. Compared to existing technologies, the water loss rate of the product in this invention is controlled within the ideal range of 2.5-4%, avoiding the risks of insufficient moisture due to excessively low water loss or excessive water content and microbial growth due to excessively high water loss. This ensures a shelf life extended to 18-24 months, suitable for various skin types, especially sensitive skin. Specifically, in Examples 1-3, the water loss rates are 3.8%, 3.5%, and 3.3%, respectively, far superior to 1.2% (too dry and brittle) in Comparative Example 1 and 6.4% (high water content and instability) in Comparative Example 4, thus maintaining the soft texture and integrity of the active ingredients.

[0023] Regarding skin softness and firmness, this invention employs the synergistic effect of fillers (such as a combination of synthetic fluorophlogopite and boron nitride) and emollients (such as hydrogenated polydecene and caprylic / capric triglycerides), combined with negative pressure sublimation drying to form a porous structure. The product's Shore hardness is reduced to 10-15, more than 30% lower than traditional baked powder (20-30). Shore hardness testing shows the lowest hardness in this embodiment, resulting in a softer, smoother feel and avoiding surface crusting and difficulty in powder application. Hardness comparison charts confirm that maintaining negative pressure during temperature drying effectively reduces hardness and improves user experience. The hardness curve of this embodiment is stable with no abrupt peak changes, indicating a uniform and dense structure. This makes the product easy to brush, blending seamlessly with a single stroke, naturally adhering to the skin without pulling or feeling stuffy, suitable for both everyday and professional makeup.

[0024] Stability is another outstanding advantage of this invention. By precisely controlling pre-freezing (-30 to -50℃, 0.5-3h) and sublimation drying (negative pressure 1-50Pa, gradually increasing temperature to 20℃ and holding for 6-9h), the product forms a stable porous network with excellent resistance to mechanical shock. In a 30cm drop test, the product of the example remained intact without damage, while Comparative Example 1 was severely damaged, Comparative Example 3 was slightly damaged, and Comparative Example 2 was stable but had an excessively long preparation time (20.2h). This proves that the process parameters of this invention (such as the total sublimation time of 4.67h) achieve a balance between stability and efficiency, reducing the breakage rate to 0%, which is far superior to the 5-30% of traditional products. In addition, after constant temperature and humidity storage, the product did not shrink or break, and the microbial limit test met the cosmetic standards (total bacterial count <100CFU / g), indicating high safety and suitability for high temperature and high humidity environments.

[0025] In terms of color payoff and sensory performance, this invention optimizes the aqueous moisturizer (such as glycerin and 1,3-propanediol) and emulsifier (such as sorbitan stearate) to ensure uniform dispersion of pigments (such as CI 15850 and CI 77491). This results in a significant improvement in Lab values ​​after makeup application: the a* value (redness) increases to 32.89 (Example 1), a 31% increase compared to 25.03 in Comparative Example 1; the L* value (lightness) decreases to 45.61, providing strong coverage; and the b* value remains stable at 9.03, presenting a natural, rosy makeup effect without yellowing. The bar chart shows that Example 1 exhibits the best color payoff, with a more vibrant and long-lasting color, maintaining its color for 8-12 hours without oxidation or discoloration, superior to the 26.9 a* value of Comparative Example 3. Sensory evaluation further confirmed that smoothness, spreadability, and skin-fit were all scored out of 5, with an average score of 5.0, which is 20-50% higher than Comparative Example 1's 3.3 and Comparative Example 3's 4.2. Smoothness refers to the delicate feel, spreadability to the skin, and skin-fit to the skin. The average score from 1 to 5 was used. The full score in the example reflects the product's silky smoothness, non-suffocating texture, and easy and even application. The testing method was a blind evaluation by a professional sensory panel, confirming its practical advantages.

[0026] In terms of preparation efficiency and economy, the process of this invention shortens the total time to 12.87-17.7 hours, with Example 3 taking only 12.87 hours, a 36% reduction compared to Comparative Example 2's 20.2 hours. While Comparative Example 4's 11.77 hours was shorter, its high water loss rate resulted in a failure to meet standards. The equipment operating time is moderate, reducing energy consumption by 20-30%. Vacuum freeze-drying combined with emulsification homogenization (2000-4000 rpm, 3-8 min) avoids energy waste and component damage from high-temperature baking, keeping costs below 80% of traditional baking methods, facilitating industrial production. Simultaneously, it boasts high raw material utilization, efficient filler pulverization and mixing (phase A) and oil-water emulsification (phase D) steps, requires no additional protective agents, simplifies the process, and is suitable for domestic cosmetic companies.

[0027] In summary, the freeze-dried blush composition and its preparation method of the present invention are superior to existing technologies in terms of softness (low hardness, porous and soft), skin adhesion (smooth and spreadable 5 points), color payoff (increased a*, decreased L*), and stability (no damage, low microorganisms). Furthermore, they optimize preparation time and energy consumption, filling a technological gap in freeze-dried cosmetics and possessing broad market application prospects. Especially among young consumers seeking "zero-burden, natural and long-lasting" makeup, they can enhance brand competitiveness and drive the cosmetics industry towards sustainable innovation. Attached Figure Description

[0028] Figure 1 This is a diagram showing the situation after the 30cm drop three times in Example 1.

[0029] Figure 2 This is a comparison image showing the situation after three drops from 30cm.

[0030] Figure 3 A diagram of the drop platform used in the example and comparative drop tests.

[0031] Figure 4 Hardness charts obtained using a Shore hardness tester for both examples and comparative cases.

[0032] Figure 5 A bar chart comparing Lab values ​​measured using a Cutometer dual MPA 580 (color test probe - CL 440) instrument for both examples and comparative examples. Detailed Implementation

[0033] The present invention will be further described below with reference to specific embodiments. These embodiments are intended to illustrate the feasibility, operational details, and practical application effects of the present invention, but are not intended to limit the scope of protection of the present invention.

[0034] The following examples use a preferred formulation of the composition: The filler comprises 20.9 parts mica, 14.5 parts synthetic fluorophlogopite, 0.9 parts boron nitride, 1.6 parts kaolin, 8.8 parts silica, 3.3 parts polymethylsilsesquioxane, 1.7 parts CI 15850, 1.9 parts CI 77491, and 1.5 parts CI 77007; the aqueous phase comprises 36.3 parts deionized water, 0.32 parts dipropylene glycol, and 1.3 parts glycerin; the emollient comprises 1.7 parts hydrogenated polydecene and bis-diglyceride polyacryladiate-2. 0.9 parts, caprylic / capric triglyceride 1.5 parts, ethylhexylglycerin / caprylyl glycol 0.72 parts; emulsifiers include C12-20 acid PEG-8 ester 0.27 parts, cetyl alcohol 0.14 parts, sorbitan isostearate 0.45 parts, and sorbitan stearate 1.3 parts. Before preparation, all utensils and equipment were sterilized at 120℃ for 20 min to ensure a sterile environment. The general steps AF are as follows: A. Weigh the raw materials according to the mass ratio; B. Crush and mix the filler to obtain phase A; C. Heat the aqueous phase and moisturizer to 80-90℃ to obtain phase B; D. Heat the emollient and emulsifier to 80℃ to dissolve to obtain phase C; E. Emulsify and homogenize phase C and phase B (75-85℃, 2000-4000rpm, 3-8min), cool to 25℃ to obtain phase D; F. Mix phase A and phase D, and press into a plastic tray using a mold to obtain the freeze-dried blush composition. Step G is a variant of vacuum freeze drying, using an industrial-grade freeze dryer with precise negative pressure control.

[0035] Example 1

[0036] I. Pre-freezing: Place the pressed composition in a freeze dryer and freeze at -40°C for 2 hours to form a uniform ice crystal structure, avoiding damage to the powder by large ice crystals. II. Sublimation drying: Freeze-sublimate at -40°C under vacuum, maintaining a negative pressure of 30 Pa (not exceeding 50 Pa) for 1.5 hours; then slowly and gradually raise the temperature to -20°C over 10 minutes, holding for 1.5 hours; starting from -20°C, heat in 10°C increments to 20°C, each increment lasting 1 hour, for a total duration of approximately 4.67 hours, ensuring uniform sublimation of moisture and the formation of a porous network. III. Heating drying: Slowly and gradually raise the temperature to 30°C over 10 minutes, holding for 1.5 hours; then slowly raise the temperature to 45°C over 12 minutes, holding for 3 hours, controlling the residual moisture content to <4%. IV. Storage: Remove the composition from the freeze dryer and store it in a constant temperature (25°C) and constant humidity (RH 50%) environment to obtain Example 1. The total preparation time was 14.7 hours, the water loss rate was 3.8%, and the product was soft, stable, and free from breakage.

[0037] Example 2

[0038] 1. Pre-freezing: Place the pressed composition into a freeze dryer and freeze at -30℃ for 3 hours until the ice crystals are fine and uniform.

[0039] 2. Sublimation drying: freeze-sublimate at -30℃ and vacuum under negative pressure of 30Pa for 2 hours; slowly and gradually raise the temperature to -20℃ within 10 minutes and hold at the temperature and pressure for 2 hours; starting from -20℃, heat in steps of 10℃ for 1 hour each, for a total duration of about 4.67 hours.

[0040] III. Heating and Drying: Slowly and gradually increase the temperature to 30°C over 10 minutes, and hold at this temperature and pressure for 2 hours for sublimation; then slowly increase the temperature to 40°C over 12 minutes, and hold at this temperature and pressure for 3.5 hours for sublimation. IV. Storage: Remove the composition from the freeze dryer and store it in a constant temperature and humidity environment to obtain Example 2. The total preparation time was 17.7 hours, the water loss rate was 3.5%, the composition had a soft texture, and the coloring was uniform.

[0041] Example 3

[0042] I. Pre-freezing: The pressed composition was placed in a freeze dryer and frozen at -50°C for 1 hour to rapidly freeze and minimize ice crystal size. II. Sublimation drying: Sublimation was carried out at -50°C under vacuum and a negative pressure of 30 Pa for 1 hour; the temperature was then slowly and gradually increased to -35°C over 10 minutes, and held at this temperature and pressure for 1 hour; the temperature was then slowly and gradually increased to -20°C over 10 minutes, and held at this temperature and pressure for 1 hour; starting from -20°C, the temperature was increased in 10°C increments, each increment lasting 1 hour, for a total duration of approximately 4.67 hours. III. Heating drying: The temperature was slowly and gradually increased to 40°C over 10 minutes, and held at this temperature and pressure for 1.5 hours; the temperature was then slowly increased to 55°C over 12 minutes, and held at this temperature and pressure for 2 hours. IV. Storage: The composition was removed from the freeze dryer and stored in a constant temperature and humidity environment to obtain Example 3. The total preparation time was 12.87 hours, the water loss rate was 3.3%, the hardness was the lowest, and the extensibility was the best.

[0043] Comparative Example 1

[0044] I. Oven Baking: The pressed composition (same as the formulation in the example) was placed in an oven at 50°C for 12 hours. No freeze-drying step was performed. The high temperature resulted in a dense and hardened structure. II. Storage: The powder was removed from the oven and stored in a constant temperature and humidity environment to obtain Comparative Example 1. The total time was 12 hours, with a water loss rate of 1.2%. The product was too dry and brittle, with high hardness (Shore > 25) and poor stability.

[0045] Comparative Example 2

[0046] 1. Pre-freezing: Place the pressed composition into a freeze dryer and freeze at -40℃ for 2 hours.

[0047] II. Sublimation Drying: Freeze-dry at -40℃ and 30Pa for 3 hours; then slowly raise the temperature to -20℃ within 10 minutes and hold for 3 hours; starting from -20℃, increase the temperature in 10℃ increments to 20℃, each increment lasting 1 hour, for a total duration of approximately 4.67 hours. Excessive sublimation time leads to over-drying. III. Heating Drying: Raise the temperature to 30℃ within 10 minutes and hold for 3 hours; then raise the temperature to 45℃ within 12 minutes and hold for 4 hours. IV. Storage: Remove the composition from the freeze dryer and store in a constant temperature and humidity environment to obtain Comparative Example 2. The total time was 20.2 hours, with a water loss rate of 3.3%. Although the composition was soft, it was energy-intensive and economically inefficient.

[0048] Comparative Example 3

[0049] 1. Pre-freezing: Place the pressed composition into a freeze dryer and freeze at -40℃ for 2 hours.

[0050] II. Sublimation Drying: Freeze-dry at -40℃ and 30Pa for 1.5 hours; then raise the temperature to -20℃ within 10 minutes and hold for 1.5 hours; starting from -20℃, increase the temperature in 10℃ increments to 20℃, for a total duration of approximately 4.67 hours. III. Oven Baking: Remove the powder from the freeze dryer and bake in an oven at 45℃ for 6 hours. Due to process variations, the results were uneven. IV. Storage: Remove the composition from the oven and store it in a constant temperature and humidity environment to obtain Comparative Example 3. The total time was 15.83 hours, with a water loss rate of 2.8%, indicating moderate stability and susceptibility to slight breakage.

[0051] Comparative Example 4

[0052] 1. Pre-freezing: Place the pressed composition into a freeze dryer and freeze at -50℃ for 1 hour.

[0053] II. Sublimation Drying: Freeze-sublimate at -50℃ and negative pressure 30Pa for 0.8h; raise the temperature to -35℃ within 10min and hold for 0.8h; raise the temperature to -20℃ within 10min and hold for 0.8h; starting from -20℃, increase the temperature in 10℃ increments, with a total duration of approximately 4.67h. If the time is too short, the residual water will be high.

[0054] 3. Heating and drying: Heat to 40℃ within 10 minutes and hold at the same temperature and pressure for 1.5 hours for sublimation; heat to 55℃ within 12 minutes and hold at the same temperature and pressure for 1.5 hours for sublimation.

[0055] IV. Storage: The composition was removed from the freeze dryer and stored in a constant temperature and humidity environment to obtain Comparative Example 4. The total time was 11.77 hours, and the water loss rate was 6.4%. Due to excessive water content, subsequent tests were not conducted, as it was prone to microbial growth.

[0056] Performance Comparison

[0057] Comparative Example 1 only involved baking, resulting in high product hardness and easy powder flying; Comparative Example 2 required a long baking time and consumed a lot of energy; Comparative Example 3 combined baking and had weak stability; Comparative Example 4 had a short baking time and a high water loss rate. The water loss rate of the examples was 2.5-4%, within the ideal range, avoiding excessive drying or microbial risks. Testing was conducted in a temperature-controlled laboratory, using equipment including a Shore hardness tester, a Cutometer dual MPA 580 (CL 440 probe), and a drop platform (…). Figure 3 ).

[0058] Table 1 Preparation time

[0059] Group Time / h Example 1 14.7 Example 2 17.7 Example 3 12.87 Comparative Example 1 12 Comparative Example 2 20.2 Comparative Example 3 15.83

[0060] The longer the equipment runs, the higher the energy consumption; the best balance is achieved in the implementation example.

[0061] Table 2 Water Loss Rate

[0062] Group Water loss rate % Example 1 3.8 Example 2 3.5 Example 3 3.3 Comparative Example 1 1.2 Comparative Example 2 3.3 Comparative Example 3 2.8

[0063] The example has a moderate water loss rate, good product wettability, and strong stability.

[0064] Figure 1 (After being dropped 30cm three times in the example) it showed to be intact and undamaged; Figure 2 (Comparative examples) show that Comparative Example 1 is severely damaged, Comparative Example 3 is slightly damaged, and Comparative Example 2 is stable but not excellent. Figure 3 To ensure consistency during drop testing. Figure 4 (Shore hardness test) shows that the hardness of Example 1 and Comparative Example 2 is lower, while Example 1 is better, and negative pressure heating drying is the key.

[0065] Table 3 Sensory Comparison

[0066] Testing items Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Smoothness / min 5 5 5 3.5 5 4.1 Extensibility / points 5 5 5 3 5 4 Adhesion to skin / point 5 5 5 3.7 5 4.4 Average score 5 5 5 3.3 5 4.2

[0067] Smoothness: delicate touch; Spreadability: ease of blending; Adhesion to skin: skin fit; Rating from 1 to 5 points, take the average value, all examples are excellent.

[0068] Table 4 Lab values ​​(Cutometer dual MPA 580, CL 440 probe, inner forearm test)

[0069] Inner side of forearm L* Avg a* Avg b* Avg Blank group 61.34 3.71 9.14 Example 1 45.61 32.89 9.03 Comparative Example 1 50.33 25.03 10.34 Comparative Example 2 44.58 33.09 9.6

[0070] L*: Brightness (low value, strong coverage); a*: Redness (high value, good color payoff); b*: Yellowness; In this example, a is the highest and L is the lowest, resulting in a rosy color and excellent coverage. Test: Apply the product to the forearm in three clockwise circles with your fingertip and measure with an instrument. Figure 5 The bar chart confirms that the coloring of the example is optimal.

[0071] Combining Table 3 and Table 4, Figure 5 The smoothness, spreadability, skin-adherence, and coloring of the embodiment are superior to those of Comparative Examples 1 and 3; Comparative Example 2 has a good skin feel but takes a long time, so the embodiment is the best. Figure 1-5 Tables 1-4 show that the embodiments exhibit strong stability, softness, good color application, spreadability, and skin adhesion, with reasonable time and energy consumption, superior to traditional baking and pressing powders, and have market potential. The above content provides a further detailed description of the invention in conjunction with specific embodiments. It should not be construed that the specific implementation of the invention is limited to these descriptions. For those skilled in the art of cosmetics, several simple deductions or substitutions can be made without departing from the concept of the invention, and all such modifications or substitutions should be considered within the scope of protection defined by the claims submitted herein.

Claims

1. A freeze-dried blush composition, characterized in that: By weight, it comprises 40-70 parts filler, 30-40 parts aqueous phase, 4-10 parts emollient, and 1-4 parts emulsifier; the aqueous phase is selected from one or more combinations of deionized water, moisturizer, plant fermentation liquid, and plant flower water; the emollient is selected from one or more combinations of polydimethylsiloxane and its derivatives, triglycerides and their derivatives, jojoba oil, sunflower seed oil, castor oil, coconut oil, grape seed oil, shea butter, meadowfoam seed oil, macadamia nut oil, olive oil, palm oil, squalane, cocoa butter, jojoba butter, glycolipid, octyl dodecanol, caprylic / capric triglyceride, and cocoyl alcohol-caprylic / capric triglyceride.

2. The freeze-dried blush composition according to claim 1, characterized in that: The filler is selected from one or more combinations of modified starch, synthetic fluorophlogopite, sericite, talc, silica, lake, polymethyl methacrylate, polydimethylsiloxane / vinyl polydimethylsiloxane cross-linked polymer, vinyl polydimethylsiloxane / polymethylsiloxysilsesquioxane cross-linked polymer, polydimethylsiloxane cross-linked polymer, boron nitride, organosilicon elastomer, calcium carbonate, pearl powder, silk powder, zinc stearate, aluminum stearate, lauroyl lysine, polymethylsilsesquioxane, kaolin, nylon-12, diamond powder, zinc oxide, barium sulfate, hydroxyapatite, aluminum oxide, bismuth oxychloride, aluminum hydroxide, magnesium myristate, and nephrite powder.

3. The freeze-dried blush composition according to claim 1, characterized in that: The moisturizer is selected from one or more combinations of glycerin, sodium hyaluronate, 1,3-propanediol, 1,2-hexanediol, cetyl alcohol, and trehalose.

4. The freeze-dried blush composition according to claim 1, characterized in that: The emulsifier is selected from one or more combinations of sorbitan stearate, sorbitan isostearate, sorbitan sesquioleate, and polysorbate-60.

5. A method for preparing the freeze-dried blush composition according to any one of claims 1-4, characterized in that: Includes the following steps: A. Weigh the filler, aqueous phase, emollient, and emulsifier according to the mass ratio; B. Put the filler into a pulverizer and pulverize and mix it until homogeneous to obtain phase A; C. Put the aqueous phase and emollient into an emulsifying pot and mix them evenly, then heat to 80-90℃ for later use, this is phase B; D. Heat the emollient and emulsifier to 80℃ until the solids are completely dissolved and stirred evenly, this is phase C; E. Add phase C to the emulsifying pot and emulsify and homogenize it with phase B at an emulsification temperature of 75-85℃, a homogenization speed of 2000-4000 rpm, and a time of 3-8 minutes, then cool to 25℃ to obtain phase D; F. Mix phase A and phase D evenly. G. Press the mixture evenly onto a plastic tray using a mold to obtain a freeze-dried blush composition; G. Place the composition in a freeze dryer for vacuum freeze-drying, including pre-freezing, sublimation drying, and temperature drying. Pre-freezing is performed at -30℃ to -50℃ for 0.5-3 hours; sublimation drying is performed at -30℃ to -40℃ and a negative pressure of 1Pa to 50Pa for 0.5-3 hours, followed by slow temperature increase to 20℃ and holding at pressure for 6-9 hours; temperature drying is performed at 20℃ to 55℃ and a negative pressure for 3.5-6 hours; finally, the composition is removed and stored in a constant temperature and humidity environment to obtain the freeze-dried blush composition.

6. The preparation method according to claim 5, characterized in that: The specific composition of the filler in step B is as follows: 20.9 parts mica, 14.5 parts synthetic fluorophlogopite, 0.9 parts boron nitride, 1.6 parts kaolin, 8.8 parts silica, 3.3 parts polymethylsilsesquioxane, 1.7 parts CI15850, 1.9 parts CI77491, and 1.5 parts CI77007.

7. The preparation method according to claim 5, characterized in that: In step C, the aqueous phase consists of 36.3 parts deionized water, and the humectant consists of 0.32 parts dipropylene glycol and 1.3 parts glycerin.

8. The preparation method according to claim 5, characterized in that: The emollient in step D consists of 1.7 parts hydrogenated polydecene, 0.9 parts bis-diglyceride polyacryloyl adipate-2, 1.5 parts caprylic / capric triglyceride, and 0.72 parts ethylhexylglycerin / caprylyl glycol. The emulsifier consists of 0.27 parts C12-20 acid PEG-8 ester, 0.14 parts cetyl alcohol, 0.45 parts sorbitan isostearate, and 1.3 parts sorbitan stearate.

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