A skin-adhering, long-lasting makeup composition, its preparation method, and its application.

Abstract

This invention discloses a skin-adhering, long-lasting makeup composition, its preparation method, and its applications, relating to the field of cosmetic technology. The preparation method includes: mixing polydimethylsiloxane, squalane, ethylhexyl palmitate, and polyglycerol-3 diisostearate to form an oil phase; adding the oil phase to a tin-antimony-containing solution, adding ammonia for hydrolysis and precipitation, followed by centrifugation, and removing the upper oil phase composition; adding the powder matrix to the oil phase composition in multiple batches, stirring and mixing with a gradually increasing rotation speed after each addition; adding a stabilizer; and then vacuum degassing, filling, and sealing. This invention significantly improves the dispersion effect of the powder matrix and the oil phase, resulting in a skin-adhering, long-lasting makeup composition that is free of particles, has a silky smooth feel, and a more sophisticated makeup effect. The high interfacial bonding strength between the powder and the matrix greatly delays sedimentation and oil phase separation caused by gravity, resulting in better stability. Furthermore, it also has higher hiding power and color rendering, making it widely applicable to the preparation of various cosmetics.

Description

Technical Field

[0001] This invention relates to the field of cosmetic technology, and more specifically, to a skin-adhering, long-lasting makeup composition, its preparation method, and its application. Background Technology

[0002] As consumers' demands for foundation products to achieve a three-in-one effect of "lightweight and skin-adhering, long-lasting makeup, and skin-nourishing and repairing," the beauty industry is facing a critical stage of technological challenges in formula system reconstruction and functional integration. Modern makeup has gradually evolved from a single function of concealing and correcting imperfections to a complex carrier system that integrates skin physiological adaptability, environmental tolerance, and the ability to deliver active ingredients. Among these, skin adherence depends on the biomimetic matching degree between film-forming substances and sebum structure, makeup staying power depends on the stability and anti-migration ability of the oil phase system in a dynamic sebum environment, and skin-nourishing effects require active ingredients to maintain a high encapsulation rate and sustained-release activity in a complex matrix. Currently, most mainstream products use silicone elastomers or acrylate film-forming agents to construct the makeup-holding framework, supplemented by moisturizers to improve skin feel. However, their rigid film structure is prone to misalignment with skin texture, leading to powder settling and creasing. At the same time, high molecular weight film-forming agents are prone to phase separation due to sebum penetration in high temperature and high humidity environments, causing localized makeup fading and patchiness, and the makeup-holding time is generally difficult to exceed the 6-hour critical value.

[0003] Among them, the technology route based on polydimethylsiloxane alcohol to construct a biomimetic skin-adhesive film layer is considered a key direction to overcome the limitations of traditional film-forming agents due to its excellent softness, breathability, and wide temperature range stability. This ingredient can self-assemble into a nanoscale continuous film on the skin surface. The flexible oscillating properties of its molecular chain segments can dynamically conform to the micro-undulation structure of the skin, while maintaining the opening of sweat channels and avoiding the stuffy feeling caused by traditional film-forming agents. However, a single siloxane system is difficult to trigger the "silicone oil bursting" effect on skin with low sebum secretion, which prevents makeup-enhancing ingredients from effectively migrating to the surface to form a secondary protection, resulting in a decrease in anti-migration performance.

[0004] While existing technologies can improve adherence to the skin in the short term by siliconizing pigments or adding hyaluronic acid, they cannot solve the fundamental contradiction of the imbalance between the film structure and the dynamic interaction of sebum. Using high-concentration film-forming agents prolongs makeup wear time but sacrifices skin comfort and the skin's ability to breathe freely. Directly adding free antioxidants faces multiple bottlenecks, including poor stability, low permeability, and high irritation. Especially under the combined stress of temperatures above 35°C and relative humidity of 60%, commercially available products generally exhibit a chain reaction of failures, including film embrittlement, oil phase leakage, and deactivation of active ingredients, resulting in a decrease in makeup integrity of more than 35% within 8 hours. Therefore, there is an urgent need to develop a cosmetic composition system that can dynamically respond to the sebum environment, precisely control the migration path of silicone oil, and achieve low-temperature, high-efficiency encapsulation of active ingredients to overcome the technical challenge of synergistically optimizing adherence, makeup wear, and skin-nourishing effects.

[0005] In view of this, the present invention is proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a skin-adhering makeup composition, its preparation method, and its application.

[0007] This invention is implemented as follows:

[0008] In a first aspect, the present invention provides a method for preparing a skin-adhering makeup composition, comprising:

[0009] S1, Pre-crosslinked matrix: Polydimethylsiloxane and squalane are mixed under a first temperature and a first rotation speed to form a pre-crosslinked matrix;

[0010] S2. Homogenization: The pre-crosslinked matrix is ​​cooled to a second temperature, and ethylhexyl palmitate and polyglycerol-3 diisostearate are added and mixed while maintaining the second temperature and the second rotation speed to form an oil phase;

[0011] S3. Sample solution: At room temperature, dissolve tin tetrachloride pentahydrate and antimony trichloride in anhydrous ethanol by stirring. Heat the solution to 40-50℃ and stir until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0012] S4. Oil phase addition: The oil phase is added to the tin-antimony containing solution to obtain a mixture;

[0013] S5. Hydrolysis and precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 6.8-7.2 to obtain a hydrolyzed mixture;

[0014] S6. Centrifugation: Centrifuge the hydrolyzed mixture. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0015] S7. Powder dispersion: Under the protection of a protective gas, the powder matrix is ​​added to the oil phase composition in multiple portions, and the mixture is stirred and mixed with a gradually increasing rotation speed after each addition to obtain a dispersion.

[0016] S8. Finished product: The dispersion is added to a stabilizer, and then vacuum degassed, filled and sealed.

[0017] In an optional embodiment, the multiple times include 2-4 times, and the gradient increasing speed includes an initial speed of 400-600 rpm, an increase of 200-600 rpm each time, a mixing time of 10-15 min each time, and a total mixing time of 30-45 min.

[0018] In an optional embodiment, the first temperature is 55-65°C, the first rotation speed is 200-400 rpm, and the mixing time is 20-40 min;

[0019] And / or, the second temperature is 35-45℃, the second rotation speed is 400-500rpm, and the mixing time is 10-30min.

[0020] In an optional embodiment, the vacuum degassing temperature is 25-35℃, the vacuum degree is -0.1~-0.05MPa, and the degassing time is 10-20min.

[0021] In an optional embodiment, the mass ratio of the polydimethylsiloxane, the squalane, the ethylhexyl palmitate, and the polyglycerol-3 diisostearate is 10-15:3-5:10-20:3-15;

[0022] And / or, the mass-to-volume ratio of the tin tetrachloride pentahydrate, the antimony trichloride, and the anhydrous ethanol is 3-11:6-13:4-13;

[0023] And / or, the mass ratio of the tin-antimony-containing solution to the oil phase is 3-10:5-20;

[0024] And / or, the centrifugation speed is 8000-12000 r / min, and the time is 8-12 min.

[0025] In an optional embodiment, the mass ratio of the oil phase composition, the powder matrix, and the stabilizer is 1:(0.45~0.96):(0.03~0.06).

[0026] In an optional embodiment, the powder matrix includes at least one of titanium dioxide and iron oxide;

[0027] And / or, the stabilizer includes at least one of hydrogenated polyisobutylene, octanoic acid / decanoic acid triglyceride, and hydrogenated polydecene.

[0028] Secondly, the present invention provides a skin-adhering makeup composition, which is prepared by the method for preparing a skin-adhering makeup composition as described in any of the foregoing embodiments.

[0029] Thirdly, the present invention provides the application of the skin-adhering makeup composition as described in the foregoing embodiments in the preparation of skin-adhering makeup cosmetics, wherein the amount of the skin-adhering makeup composition added to the cosmetics is 0.01-15 wt%.

[0030] In an optional embodiment, the cosmetic includes at least one of sunscreen, BB cream, makeup base, sunscreen BB cream, and tone-up cream.

[0031] The present invention has the following beneficial effects:

[0032] The preparation method of the skin-adhering makeup composition provided by this invention involves first mixing polydimethylsiloxane and squalane to form a pre-crosslinked matrix, then cooling and adding ethylhexyl palmitate and polyglycerol-3 diisostearate to form an oil phase. The oil phase is then mixed with a tin-antimony solution and subjected to hydrolysis and precipitation, which effectively disperses the oil phase. The upper oil phase composition is then collected by centrifugation, avoiding the introduction of components from the tin-antimony solution into the oil phase composition. The oil phase composition is then mixed with a powder matrix. Dispersion is achieved by adding the powder matrix multiple times with increasing rotation speed each time, significantly improving the dispersion effect of the powder matrix and the oil phase. Because the powder matrix is ​​completely dispersed and encapsulated, the product experiences minimal resistance during application, has no grainy feel, and a silky smooth texture. Uniform powder dispersion means more consistent light reflection, resulting in a uniform and delicate makeup color with a high-end matte or satin finish, avoiding "spots" or "white marks" caused by agglomeration. This invention achieves layered coating of powder at different rotation speeds, resulting in high interfacial bonding strength between the powder and the matrix. The resulting three-dimensional network structure is more stable, significantly delaying sedimentation and oil phase separation caused by gravity. The product maintains its original texture, color, and performance throughout its shelf life, without deterioration due to increased powder agglomeration. Fully dispersed powder means more effectively covered particles per unit area, with uniform distribution, achieving better coverage with less powder. The pigment powder is fully dispersed and wetted, exhibiting its purest and most saturated color, avoiding whitening, dullness, or unevenness caused by agglomeration and air bubbles. Attached Figure Description

[0033] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0034] Figure 1 This is a statistical chart showing the results of the in vitro waterproofing and sweat-resistant test provided in Experimental Example 1 of the present invention;

[0035] Figure 2 This is a statistical chart of the subjective evaluation results of the subjects provided in Experiment Example 3 of the present invention;

[0036] Figure 3 This is a statistical chart of the L* value results of the objective quantitative evaluation of the subjects - makeup holding test provided in Experiment Example 3 of the present invention;

[0037] Figure 4 This is a statistical chart of the ITA value results of the objective quantitative evaluation of the subjects - the makeup holding test provided in Experimental Example 3 of the present invention. Detailed Implementation

[0038] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0039] This invention provides a method for preparing a skin-adhering, long-lasting makeup composition, comprising:

[0040] S1. Pre-crosslinked matrix: Polydimethylsiloxane and squalane are mixed under the conditions of a first temperature and a first rotation speed to form a pre-crosslinked matrix.

[0041] The mass ratio of polydimethylsiloxane to squalane is 10-15:3-5, with a first temperature of 55-65℃, a first rotation speed of 200-400 rpm, and a mixing time of 20-40 min. By mixing polydimethylsiloxane and squalane at the above temperature and rotation speed, pre-crosslinking of polydimethylsiloxane and squalane can be achieved. Polydimethylsiloxane forms a three-dimensional network elastic framework in the composition, and its hydroxyl functional groups associate with the isoprene units of squalane through hydrogen bonds, forming a dynamically reversible intermolecular crosslinking structure. This structure temporarily dissociates under shear force during application, allowing the powder to spread evenly on the skin surface; under static conditions, the crosslinking network recovers, anchoring the powder in the grooves of the stratum corneum, achieving a biomimetic skin-adhesive effect. Squalane serves a dual function: First, as a natural sebum mimic, its carbon chain length and saturation are highly matched with the squalene metabolites in human sebum, allowing it to penetrate the stratum corneum gap to form a biomimetic lipid barrier, reduce transepidermal water loss, maintain skin hydration, and thus inhibit powder peeling caused by dryness; Second, its unsaturated double bond structure can capture free radicals, block lipid peroxidation chain reactions, and endow the composition with antioxidant and skin-nourishing effects.

[0042] S2. Homogenization: Cool the pre-crosslinked matrix to a second temperature, and add ethylhexyl palmitate and polyglycerol-3 diisostearate. Mix under the conditions of the second temperature and the second rotation speed to form an oil phase.

[0043] The mass ratio of polydimethylsiloxane, squalane, ethylhexyl palmitate, and polyglycerol-3 diisostearate is 10-15:3-5:10-20:3-15. The second temperature is 35-45℃, the second rotation speed is 400-500 rpm, and the mixing time is 10-30 min.

[0044] In this invention, by lowering the temperature and increasing the rotation speed, the dynamically reversible intermolecular cross-linked structure composed of polydimethylsiloxane and squalane can undergo temporary dissociation at a rotation speed of 400-500 rpm, thereby facilitating uniform mixing with ethylhexyl palmitate and polyglycerol-3 diisostearate. Ethylhexyl palmitate, as a low-viscosity ester solvent, has a viscosity of approximately 10-15 mPa at 25°C. s, its chemical formula is C 24 H 48 O2, formed by the esterification of palmitic acid and isooctyl alcohol, contains long-chain alkyl groups in its molecular structure. Palmitic acid corresponds to a sixteen-carbon straight-chain alkyl group (a long-chain alkyl group with a carbon chain length far exceeding C8), and this long-chain alkyl group has a 2-ethylhexyl branched alkyl group. This "straight-chain long-chain alkyl + branched alkyl" structure reduces intermolecular entanglement and weakens intermolecular forces, allowing ethylhexyl palmitate to maintain a low viscosity despite containing long-chain alkyl groups. The molecular chain of ethylhexyl palmitate can insert into the interstitial spaces of the polydimethylsiloxane alcohol backbone, reducing the system's cohesive force and improving its spreadability. Simultaneously, its long-chain alkyl groups are structurally similar to triglycerides in sebum, preferentially fusing with sebum during secretion and preventing makeup from becoming patchy due to oil migration.

[0045] Polyglycerol-3 diisostearate, as a nonionic emulsifier, provides hydrophilic anchors with its polyglycerol backbone and embeds its diisostearate side chains into the oil phase, forming an interfacial tension gradient field. This allows the powder particles to be dispersed in a monolayer state in the oil phase, avoiding agglomeration and sedimentation, and ensuring the uniformity of the makeup surface.

[0046] S3. Sample solution: At room temperature, dissolve tin tetrachloride pentahydrate and antimony trichloride in anhydrous ethanol by stirring. Heat the solution to 40-50℃ and stir until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0047] Tin tetrachloride pentahydrate and antimony trichloride are dissolved in anhydrous ethanol to form a clear homogeneous solution, providing an ionic dispersion core precursor for subsequent mixing with the oil phase and precipitation reaction.

[0048] The mass-volume ratio of tin tetrachloride pentahydrate, antimony trichloride and anhydrous ethanol is 3-11:6-13:4-13;

[0049] S4. Oil phase addition: Add the oil phase to the tin-antimony solution to obtain a mixture;

[0050] The oil phase consists of polydimethylsiloxane, squalane, ethylhexyl palmitate, and polyglycerol-3 diisostearate, all of which are non-water-soluble, oil-soluble organic compounds. It forms an oil-water mixture with the aqueous phase (containing ethanol, ammonia, and tin-antimony ions). The mass ratio of the tin-antimony-containing solution to the oil phase is 3-10:5-20.

[0051] When the oil phase is added to the tin-antimony alcohol solution, the system is a coarse dispersion system in which oil droplets are dispersed in an alcohol-water mixed medium. The oil droplets are dispersed only by stirring. Without the presence of a stabilizer, they are prone to agglomeration and stratification, resulting in poor dispersion stability.

[0052] S5. Hydrolysis and precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 6.8-7.2 to obtain a hydrolyzed mixture;

[0053] Ammonia provides OH - This process hydrolyzes tin and antimony ions, forming hydroxide precipitates. Simultaneously, ammonia, being a weak base, ensures complete hydrolysis at pH 7.0. Tin tetrachloride pentahydrate and antimony trichloride undergo complete hydrolysis in the alkaline environment provided by ammonia, generating Sn(OH)4 and Sb(OH)3 solid precipitates, which is crucial for improving the uniformity of oil phase dispersion.

[0054] Specifically, tin-antimony hydroxide precipitates as colloidal particles with a large specific surface area and high surface activity. These particles spontaneously adsorb onto the interface between oil droplets and the medium, forming a "precipitate particle adsorption layer." The colloidal particles adsorbed on the oil droplet surface create steric hindrance between the droplets, hindering their collision and aggregation, thus transforming the originally easily stratified coarse dispersion system into a stable colloidal dispersion system. The stirring operation during the ammonia addition process ensures that the colloidal precipitate is evenly distributed throughout the system, further guaranteeing that the oil droplets are fully coated by the precipitate particles and preventing localized oil phase aggregation.

[0055] S6. Centrifugation: Centrifuge the hydrolyzed mixture. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Remove the oil phase composition.

[0056] The centrifugation speed is 8000-12000 r / min and the time is 8-12 min. In this invention, high-speed centrifugation can effectively separate the three phases in the hydrolyzed mixture, thereby separating the components in the oil phase to form an oil phase composition without introducing components such as tin, antimony and ammonia into the oil phase composition, ensuring that the components of the oil phase composition are clean and evenly dispersed.

[0057] In this invention, the core objective of steps S3-S6 is to fully and uniformly disperse the oil phase without introducing other components, ensuring that the oil phase composition contains only polydimethylsiloxane, squalane, ethylhexyl palmitate, and polyglycerol-3 diisostearate.

[0058] S7. Powder dispersion: Under the protection of protective gas, the powder matrix is ​​added to the oil phase composition in multiple portions. After each addition, the mixture is stirred and mixed at a gradually increasing speed to obtain a dispersion.

[0059] In this invention, the mass ratio of the oil phase composition to the powder matrix is ​​1:(0.45~0.96). The method of adding the powder multiple times with a gradient increase in rotation speed significantly improves the mixing uniformity of the powder and oil phase, ensuring that the powder particles are dispersed in a single layer within the oil phase, preventing agglomeration and sedimentation, and guaranteeing a uniform makeup finish.

[0060] In this invention, the powder matrix includes, but is not limited to, at least one of titanium dioxide and iron oxide. The powder matrix is ​​added to the oil phase composition in multiple steps, for example, 2-4 steps. The gradually increasing rotation speed includes an initial speed of 400-600 rpm, with each step increasing by 200-600 rpm. Each stirring and mixing time is 10-15 min, and the total mixing time is 30-45 min.

[0061] Because in this invention, polydimethylsiloxane alcohol and the isoprene unit of squalane are associated through hydrogen bonds to form a dynamically reversible intermolecular cross-linking structure, and its polyglycerol backbone provides hydrophilic anchors, while the diisostearate side chain is embedded in the oil phase to form an interfacial tension gradient field, it can achieve different interfacial tensions at different rotation speeds and undergo temporary dissociation under shear force, thus achieving a monolayer dispersion state of the powder matrix. Subsequently, increasing the rotation speed will form a new interfacial tension, which will again make the powder matrix present a monolayer dispersion state, avoiding agglomeration and sedimentation, and ensuring the uniformity of the makeup surface.

[0062] S8. Finished product: The dispersant is added to the stabilizer, and then vacuum degassed, filled and sealed.

[0063] In this invention, the mass ratio of oil phase to stabilizer is 1:(0.03~0.06). By adding stabilizer to the dispersion, the uniformity of the powder matrix and oil phase in the dispersion can be maintained, the powder matrix can be kept in a monolayer dispersion state, powder agglomeration and sedimentation can be inhibited, and the long-term stability of the system can be ensured. The stabilizer includes, but is not limited to, at least one of hydrogenated polyisobutylene, octanoic acid / decanoic acid triglyceride, and hydrogenated polydecene.

[0064] Subsequent vacuum degassing removes air bubbles from the system, improving product density and stability. The vacuum degassing temperature is 25-35℃, the vacuum level is -0.1~-0.05MPa, and the degassing time is 10-20 minutes. Filling and sealing after vacuum degassing ensures precise metering and shape retention, isolates external interference, and extends shelf life.

[0065] The skin-adhering makeup composition prepared by the above-mentioned method has good stability, significantly improved skin adherence and makeup-holding power, and also has certain skin-nourishing effects.

[0066] The above-mentioned skin-adhering and long-lasting makeup composition can be widely used in the preparation of skin-adhering and long-lasting cosmetics. The amount of the skin-adhering and long-lasting makeup composition added to the cosmetic is 0.01-15 wt%, preferably 8-12 wt%.

[0067] Among them, cosmetics include, but are not limited to, at least one of sunscreen, BB cream, makeup base, sunscreen BB cream and BB cream.

[0068] The features and performance of the present invention will be further described in detail below with reference to embodiments.

[0069] Example 1

[0070] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0071] S1. Pre-crosslinked matrix formation: At 60°C, 10 parts of polydimethylsiloxane alcohol and 3 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0072] S2. Homogenization: Cool to 40°C, add 20 parts of ethylhexyl palmitate and 5 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0073] S3, Sample solution: At room temperature, 4 parts of tin tetrachloride pentahydrate and 8 parts of antimony trichloride are dissolved in 10 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0074] S4. Oil phase addition: Add the oil phase to the tin-antimony solution. The mass ratio of the tin-antimony solution to the oil phase is 7:15 to obtain a mixture.

[0075] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0076] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0077] S7. Powder Dispersion: Under nitrogen protection, the total 25 parts of powder matrix (titanium dioxide) are divided into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 500 rpm for 10 minutes. Second addition: Add the second part of powder and increase the stirring speed to 1000 rpm for 10 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1500 rpm for 15 minutes. Ensure the total dispersion time is at least 35 minutes.

[0078] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0079] Example 2

[0080] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0081] S1. Pre-crosslinked matrix formation: At 60°C, 10 parts of polydimethylsiloxane alcohol and 3 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0082] S2. Homogenization: Cool to 40°C, add 20 parts of ethylhexyl palmitate and 5 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0083] S3, Sample solution: At room temperature, 6 parts of tin tetrachloride pentahydrate and 9 parts of antimony trichloride are dissolved in 13 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0084] S4. Oil phase addition: Add the oil phase to the tin-antimony solution. The mass ratio of the tin-antimony solution to the oil phase is 5:17 to obtain a mixture.

[0085] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0086] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0087] S7. Powder Dispersion: Under nitrogen protection, the total 25 parts of powder matrix (titanium dioxide) are divided into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 600 rpm for 10 minutes. Second addition: Add the second part of powder and increase the stirring speed to 1200 rpm for 10 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1800 rpm for 15 minutes. Ensure the total dispersion time is at least 35 minutes.

[0088] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0089] Example 3

[0090] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0091] S1. Pre-crosslinked matrix formation: At 60°C, 10 parts of polydimethylsiloxane alcohol and 3 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0092] S2. Homogenization: Cool to 40°C, add 20 parts of ethylhexyl palmitate and 5 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0093] S3, Sample solution: At room temperature, 7 parts of tin tetrachloride pentahydrate and 12 parts of antimony trichloride are dissolved in 13 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0094] S4. Oil phase addition: Add the oil phase to the tin-antimony-containing solution. The mass ratio of the tin-antimony-containing solution to the oil phase is 4:11 to obtain a mixture.

[0095] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0096] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0097] S7. Powder Dispersion: Under nitrogen protection, the total 25 parts of powder matrix (titanium dioxide) are divided into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 400 rpm for 10 minutes. Second addition: Add the second part of powder and increase the stirring speed to 800 rpm for 10 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1200 rpm for 15 minutes. Ensure the total dispersion time is at least 35 minutes.

[0098] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0099] Example 4

[0100] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0101] S1. Pre-crosslinked matrix formation: At 60°C, 10 parts of polydimethylsiloxane alcohol and 3 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0102] S2. Homogenization: Cool to 40°C, add 20 parts of ethylhexyl palmitate and 5 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0103] S3, Sample solution: At room temperature, 11 parts of tin tetrachloride pentahydrate and 13 parts of antimony trichloride are dissolved in 13 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0104] S4. Oil phase addition: Add the oil phase to the tin-antimony solution. The mass ratio of the tin-antimony solution to the oil phase is 9:20 to obtain a mixture.

[0105] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0106] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0107] S7. Powder Dispersion: Under nitrogen protection, the total 25 parts of powder matrix (titanium dioxide) are divided into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 600 rpm for 20 minutes. Second addition: Add the second part of powder and increase the stirring speed to 1200 rpm for 20 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1800 rpm for 25 minutes. Ensure the total dispersion time is at least 65 minutes.

[0108] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0109] Example 5

[0110] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0111] S1. Pre-crosslinked matrix formation: At 60°C, 15 parts of polydimethylsiloxane alcohol and 3 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0112] S2. Homogenization: Cool to 40°C, add 10 parts of ethylhexyl palmitate and 15 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0113] S3, Sample solution: At room temperature, 11 parts of tin tetrachloride pentahydrate and 7 parts of antimony trichloride are dissolved in 13 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0114] S4. Oil phase addition: Add the oil phase to the tin-antimony solution, with a mass ratio of 9:5 between the tin-antimony solution and the oil phase, to obtain a mixture;

[0115] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0116] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0117] S7. Powder Dispersion: Under nitrogen protection, the total 25 parts of powder matrix (titanium dioxide) are divided into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 600 rpm for 10 minutes. Second addition: Add the second part of powder and increase the stirring speed to 1200 rpm for 10 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1800 rpm for 15 minutes. Ensure the total dispersion time is at least 35 minutes.

[0118] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0119] Example 6

[0120] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0121] S1. Pre-crosslinked matrix formation: At 60°C, 15 parts of polydimethylsiloxane alcohol and 5 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0122] S2. Homogenization: Cool to 40°C, add 20 parts of ethylhexyl palmitate and 5 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0123] S3, Sample solution: At room temperature, 9 parts of tin tetrachloride pentahydrate and 9 parts of antimony trichloride are dissolved in 10 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0124] S4. Oil phase addition: Add the oil phase to the tin-antimony solution, with a mass ratio of 7:9 between the tin-antimony solution and the oil phase, to obtain a mixture;

[0125] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0126] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0127] S7. Powder Dispersion: Under nitrogen protection, divide the total 25 parts of powder matrix (titanium dioxide) into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 600 rpm for 10 minutes. Second addition: Add the second part of powder and increase the stirring speed to 1200 rpm, stirring for 10 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1800 rpm, stirring for 15 minutes. Ensure the total dispersion time is at least 35 minutes.

[0128] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0129] Example 7

[0130] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0131] S1. Pre-crosslinked matrix formation: At 60°C, 15 parts of polydimethylsiloxane alcohol and 5 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0132] S2. Homogenization: Cool to 40°C, add 20 parts of ethylhexyl palmitate and 5 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0133] S3, Sample solution: At room temperature, 5 parts of tin tetrachloride pentahydrate and 9 parts of antimony trichloride are dissolved in 10 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0134] S4. Oil phase addition: Add the oil phase to the tin-antimony solution. The mass ratio of the tin-antimony solution to the oil phase is 6:11 to obtain a mixture.

[0135] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0136] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0137] S7. Powder Dispersion: Under nitrogen protection, the total 25 parts of powder matrix (titanium dioxide) are divided into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 500 rpm for 10 minutes. Second addition: Add the second part of powder and increase the stirring speed to 1000 rpm for 10 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1200 rpm for 15 minutes. Ensure the total dispersion time is at least 35 minutes.

[0138] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0139] Example 8

[0140] This embodiment provides a skin-adhering, long-lasting makeup composition, the preparation method of which includes:

[0141] S1. Pre-crosslinked matrix formation: At 60°C, 15 parts of polydimethylsiloxane alcohol and 3 parts of squalane are mixed and stirred at 300 rpm for 30 minutes.

[0142] S2. Homogenization: Cool to 40°C, add 15 parts of ethylhexyl palmitate and 3 parts of polyglycerol-3 diisostearate in sequence, maintain 40°C and stir at 500 rpm for 20 minutes to form a homogeneous oil phase;

[0143] S3. Sample solution: At room temperature, 6 parts of tin tetrachloride pentahydrate and 7 parts of antimony trichloride are dissolved in 10 parts of anhydrous ethanol by stirring. The solution is heated to 40°C and stirred until the solution is clear and transparent to obtain a tin-antimony containing solution.

[0144] S4. Addition of oil phase: Add oil phase to tin-antimony solution, with a mass ratio of tin-antimony solution to oil phase of 4:7, to obtain a mixture;

[0145] S5. Hydrolysis precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 7.0 to obtain the hydrolyzed mixture;

[0146] S6. High-speed centrifugation: Centrifuge the hydrolysate mixture at a speed of 10000 r / min for 10 min. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition.

[0147] S7. Powder Dispersion: Under nitrogen protection, the total 25 parts of powder matrix (titanium dioxide) are divided into three equal parts. First addition: Add the first part of powder to the oil phase composition and stir at 500 rpm for 10 minutes. Second addition: Add the second part of powder and increase the stirring speed to 1000 rpm for 10 minutes. Third addition: Add the last part of powder and further increase the stirring speed to 1200 rpm for 15 minutes. Ensure the total dispersion time is at least 35 minutes.

[0148] S8. Finished product: Add 1.5 parts of auxiliary stabilizer (hydrogenated polyisobutylene), perform vacuum degassing treatment at 30°C (-0.09 MPa) for 15 minutes, and then fill and seal.

[0149] Comparative Example 1: Powder was added all at once, and stirring was performed using a gradient speed increase.

[0150] This comparative example is basically the same as Example 1, except for step S7. In this comparative example, in step S7, all 25 parts of powder matrix are added to the oil phase composition at once. The stirring strategy is still the same as in Example 1: first stir at 500 rpm for 10 minutes, then increase to 1000 rpm for 10 minutes, and finally stir at 1500 rpm for 15 minutes.

[0151] Comparative Example 2: The powder was added in three batches, but the mixing was done at a low speed throughout.

[0152] This comparative example is basically the same as Example 1, except for step S7. In this comparative example, the powder matrix is ​​added to the oil phase composition in three parts in step S7 (same as Example 1), but the low-speed stirring of 500 rpm is maintained throughout the process, and the total dispersion time is the same.

[0153] Comparative Example 3: The powder was added in three batches, but high-speed stirring was used throughout the process.

[0154] This comparative example is basically the same as Example 1, except for step S7. In this comparative example, the powder matrix is ​​added to the oil phase composition in three parts in step S7 (same as Example 1), but high-speed stirring at 1500 rpm is used from the first addition of powder until the dispersion is completed.

[0155] Comparative Example 4: Add the powder all at once and stir at low speed throughout.

[0156] This comparative example is basically the same as Example 1, except for step S7. In this comparative example, in step S7, all the powder matrix is ​​added to the oil phase composition at once, and the entire process is stirred at a low speed of 500 rpm.

[0157] Comparative Example 5

[0158] This comparative example is basically the same as Example 1, except that in this comparative example, polydimethylsiloxane, squalane, ethylhexyl palmitate and polyglycerol-3 diisostearate are mixed together and mixed at 60°C and 500 rpm for 50 min.

[0159] Comparative Example 6

[0160] This comparative example is basically the same as Example 1, except that squalane is replaced with jojoba oil in this comparative example.

[0161] Comparative Example 7

[0162] This comparative example is basically the same as Example 1, except that ethylhexyl palmitate is replaced with isododecane in this comparative example.

[0163] Comparative Example 8

[0164] This comparative example is basically the same as Example 1, except that polyglycerol-3 diisostearate is replaced with cetyl PEG / PPG-10 / 1 polydimethylsiloxane in this comparative example.

[0165] Comparative Example 9

[0166] This comparative example is basically the same as Example 1, except that the mass ratio of polydimethylsiloxane, squalane, ethylhexyl palmitate and polyglycerol-3 diisostearate in this comparative example is 3:3:3:1.

[0167] Comparative Example 10

[0168] This comparative example is basically the same as Example 1, except that the mass ratio of polydimethylsiloxane, squalane, ethylhexyl palmitate and polyglycerol-3 diisostearate in this comparative example is 4:2:3:1.

[0169] Comparative Example 11

[0170] This comparative example is basically the same as Example 1, except that steps S3-S6 are omitted in this comparative example, and the powder matrix is ​​directly added to the oil phase prepared in step S2.

[0171] Comparative Example 12

[0172] This comparative example is basically the same as Example 1, except that steps S3-S6 are omitted in this comparative example, and all 25 parts of powder matrix are directly added to the oil phase prepared in step S2 at once. The stirring strategy is still the same as in Example 1: first stir at 500 rpm for 10 minutes, then increase to 1000 rpm for 10 minutes, and finally stir at 1500 rpm for 15 minutes.

[0173] Experiment Example 1: External Waterproofing and Sweat Resistance Test

[0174] Test method: Cut leather samples of different colors into 9cm × 18cm sizes. Mark two 4cm × 5cm test areas on the leather. Apply the skin-adhering makeup composition samples obtained in the examples and comparative examples evenly to the test areas at a dosage of (2.00±0.05) mg / cm. Place the leather in an oven at 45 ℃ for 2 hours, remove and cool to room temperature. Use a skin color meter to test the skin color at 5 points in each marked area. L 1*、 a 1*、 b 1* value, calculate the average value. The leather slabs with the applied samples were completely immersed in artificial sweat at 35–37°C and clean water for 2 hours respectively. The leather slabs were then removed and dried in a 45°C oven. Skin color analysis was performed on 5 sites in each marked area using a skin color analyzer. L 2*、 a 2*、 b The average value was calculated using the 2* value. The leather color difference ΔE was calculated based on the ΔL*, Δa*, and Δb* values ​​of the leather after coating and after treatment with sweat / water. Each sample was tested in parallel three times.

[0175] The formula for calculating ΔE is:

[0176] ;

[0177] Where, Δ L *=L2*-L1*,Δ a *= a 2*- a 1*, Δ b *= b 2*- b 1*.

[0178] Please refer to the test results. Figure 1 ,from Figure 1It can be seen that in the water treatment group and the sweat treatment group, the leather color difference ΔE of Examples 1-8 of this application is significantly smaller than that of Comparative Examples 1-12, which proves that the solution of this application has excellent external waterproof and sweat-resistant performance. Comparative Examples 1-4 changed the way the powder was added or stirred, which caused the powder particles to be unable to be dispersed in a monolayer state in the oil phase, resulting in a certain amount of agglomeration and sedimentation, poor makeup uniformity, and poor waterproof and sweat-resistant effect. Comparative Example 5 changed the mixing method of the oil phase, which also led to poor pre-crosslinking and homogenization of the oil phase, resulting in poor dispersion of the powder, and therefore poor waterproof and sweat-resistant effect. Comparative Examples 6-10 changed the selection of components and the proportion of the oil phase, which also led to poor waterproof and sweat-resistant effect. Comparative Example 11 omitted steps S3-S6, which led to poor uniformity of oil phase component dispersion, and therefore poor waterproof and sweat-resistant effect. In Comparative Example 12, not only were steps S3-S6 omitted, but all the powder matrix was also added at once, which resulted in poor uniformity of oil phase dispersion and significantly worse dispersion of oil phase and powder matrix. Its effect was significantly worse than that of Comparative Example 1 and Comparative Example 11, which fully demonstrates that the steps of this application are interconnected and have some synergistic effects.

[0179] Experimental Example 2: External Coverage Test

[0180] The samples prepared in Examples 1-8 and Comparative Examples 1-12 were subjected to external opacity tests. Their external opacity was evaluated by measuring the contrast ratio (CR) of the samples on black and white cardstock.

[0181] The test method includes: taking black and white cardstock, clearly distinguishing between the black and white areas, and using a pipette to transfer an appropriate amount of the sample to be tested above the black and white areas, adding it in a long strip; using a wire rod film stretcher, spreading the sample evenly on the black and white areas to form a uniform coating with a size of 10cm×8cm; placing the black and white cardstock with the spread sample in a 45℃ oven and baking for 2 hours; after baking, removing the black and white cardstock and cooling it to room temperature for later use.

[0182] A skin color meter was used to test the black and white areas of the black and white cardstock. Nine different sites were selected for measurement in each test area (black and white) and the test data of each site were recorded. The average value of the test data of the nine sites in the black area and the nine sites in the white area was calculated. The contrast ratio (CR) of the sample was calculated based on the above measurement results. This test needs to be performed in parallel three times.

[0183] Please refer to the test results. Figure 2 .

[0184] Experimental Example 3: Skin-adhering and Long-lasting Makeup Composition Foundation

[0185] This experimental example provides a foundation containing the skin-adhering and long-lasting makeup composition provided in Example 1, the formulation of which is shown in Table 1:

[0186] Table 1. Formulation of Skin-Adhering and Long-Lasting Foundation

[0187]

[0188] Its preparation methods include:

[0189] (1) Weigh the A phase raw material and grind it into a homogenized state using a homogenizer;

[0190] (2) Add phase B raw material to phase A and continue to homogenize it evenly using a homogenizer;

[0191] (3) Add phase C to phase A+B and continue to homogenize and disperse it evenly;

[0192] (4) During the stirring process, slowly add phase D to the beaker. After adding the phase, homogenize for a period of time and continue stirring until homogeneous.

[0193] The anti-wrinkle efficacy of the prepared foundation cream was evaluated before and after product use.

[0194] (1) Volunteers: 33 healthy Chinese female subjects aged 30 to 55 years;

[0195] (2) Preparation before the test: No products should be used on the test site on the day of the test. Before the test, the subject needs to clean their face and the flexor surface of the forearm and dry them with a dry tissue. They should sit quietly for 30 minutes in the human efficacy evaluation room (temperature: 20℃~22℃, humidity: 40%~60%), during which time they should not drink water or beverages. The subject should remain relaxed, with their face and the flexor surface of the forearm exposed, and avoid touching them. Before the test, the subject should be given an explanation of the test and sign an informed consent form. The test areas are the face and the flexor surface of the forearm. For the makeup retention test, the flexor surface of the forearm is divided into two measurement areas, each with an area of ​​16 square centimeters (4cm×4cm). The tester divides the area into a water treatment area and an artificial sweat treatment area according to a random table. For the moisturizing test, the flexor surface of the forearm is divided into two measurement areas, each with an area of ​​30 square centimeters (5cm×6cm). The tester divides the area into a product area and a blank control area according to a random table.

[0196] (3) Product usage method: For daily use, after basic skin care, take an appropriate amount of product and apply it evenly to the face. It is recommended to use about 1g each time, and then pat gently until even. Use at least once a day for 4 consecutive weeks. During the trial, subjects are prohibited from using other similar preparations or other makeup; subjects are prohibited from ingesting preparations that may affect the test through infusion, injection, oral administration or other forms; subjects should mainly engage in indoor activities and avoid prolonged exposure to outdoor sunlight.

[0197] (4) Moisturizing test: The tester uses a disposable latex finger cot to apply the test product evenly to the designated test area at a dosage of (2.0±0.1) mg / cm. No product is used in the blank control area.

[0198] (5) Subjective evaluation: Subjects used the product for 7 and 28 consecutive days, and were treated with water / artificial sweat daily. They evaluated their facial condition in the human efficacy laboratory using a mirror and recorded their scores. A 7-point rating method was used to rate the product in four aspects: skin feel, effect, gentleness, and user satisfaction. The results were then judged. Please refer to Table 2 for the evaluation results.

[0199] Table 2. Scoring criteria and statistical results of subjective evaluations by test takers

[0200]

[0201] (6) Objective quantitative evaluation - makeup holding test

[0202] Pre-use measurements: After 30 minutes of cleansing, facial images were captured using the VISIA-CR facial image analyzer, and the skin L* and ITA° values ​​at the center of the test area on each arm were measured using the CL400. These measurements were used as the baseline values ​​(T0).

[0203] Product Use: The tester used disposable latex finger cots to apply approximately 1g of the test product evenly to each test area on the arm in a single application. A suitable amount of product was also applied evenly to the cheeks and forehead, then gently patted out with a powder puff, applying in small amounts multiple times until the skin tone was even. Subjects were emphasized that they should not touch the test areas during the test.

[0204] Post-use measurement (T0'): After using the product and waiting for the film to form, the same index as T0 needs to be tested, and the measured value is used as the initial value (T0').

[0205] Purified water / artificial sweat treatment: According to the random table, the tester sprayed purified water and artificial sweat 10 times (about 1.2g) onto the water-treated area and artificial sweat-treated area of ​​the subject's arm, respectively. The spray bottle was perpendicular to the arm and about 10cm away. The tester observed whether the makeup was removed from the test area.

[0206] Post-treatment measurement (T0*): After air drying, the skin L* value and ITA° value at the center of the test area of ​​each arm were measured using a CL400.

[0207] Simultaneously, the skin L* and ITA° values ​​at the center of the test area of ​​each arm were detected using a CL400 at 8h and 12h after treatment.

[0208] (7) Statistical analysis

[0209] Statistical analysis was performed on the measured values ​​of each test area, including quantity, mean, standard deviation, standard error, minimum, median, and maximum.

[0210] If the test data is normally distributed, an independent t-test is used for statistical analysis; if the test data is not normally distributed, a rank-sum test is used. The difference between the initial values ​​of each test area and the values ​​measured at other time points is calculated, and then this difference is used to statistically analyze the differences between the product area and the blank control area at different time points. Two-tailed tests are used for all statistical methods, with a significance level of α=0.05. Statistical software is used for data analysis. When significant differences occur, they are marked with *<0.05 and **p<0.01, respectively. p<0.05 indicates a significant difference. If there are no significant differences in the values ​​of various indicators in the test areas, the product is judged to have makeup-holding, waterproof, and sweat-proof effects.

[0211] (8) Test results

[0212] Please refer to Table 2 for the results of the subjects' subjective evaluations. As shown in Table 2, during the trial, 33 subjects were enrolled, 0 dropped out, and all 33 subjects ultimately met the protocol requirements, constituting valid cases. All subjects were female, with a mean age of 32.42 ± 7.74 years; this population was used for statistical analysis in this study. Regarding the product's feel on the skin, all scores had a mean of 6.2 or higher, and statistically, over 50% of the subjects gave positive evaluations of the product's feel. Specifically, "easy to apply evenly and with good spreadability," "lightweight and adherent without caking or flaking," "hydrating and clear without feeling heavy," and "natural and clear without looking fake" all received 96.97% agreement on day 7; "the product is gentle and non-irritating" received 100.00% agreement on both day 7 and day 28; and "the product is suitable for sensitive skin" received 100.00% agreement on day 28.

[0213] For objective quantitative evaluation - please refer to the results of the makeup holding test. Figure 3 and Figure 4 ,from Figure 3 and Figure 4 The analysis of arm skin brightness (L*) and skin ITA° values ​​shows that the L* value was not significantly different immediately after treatment with purified water and artificial sweat compared to the immediate time after product application. The skin ITA° value showed an increasing trend immediately after product application, immediately after treatment with purified water / artificial sweat, at 8 hours, and at 12 hours, all showing significant differences compared to baseline. There were no significant differences immediately after treatment with purified water, immediately after treatment with artificial sweat, and at 8 hours compared to the immediate time after product application.

[0214] In summary, the preparation method of the skin-adhering makeup composition provided by this invention involves first mixing polydimethylsiloxane and squalane to form a pre-crosslinked matrix, then cooling and adding ethylhexyl palmitate and polyglycerol-3 diisostearate to form an oil phase. The oil phase is then mixed with a tin-antimony solution and subjected to hydrolysis and precipitation, which effectively disperses the oil phase. The upper oil phase composition is then collected by centrifugation, avoiding the introduction of components from the tin-antimony solution into the oil phase composition. The oil phase composition is then mixed with a powder matrix. Dispersion is achieved by adding the powder matrix multiple times with increasing rotation speed each time, significantly improving the dispersion effect of the powder matrix and the oil phase. Because the powder matrix is ​​completely dispersed and encapsulated, the product experiences minimal resistance during application, has no grainy feel, and a silky smooth texture. Uniform powder dispersion means more consistent light reflection, resulting in a uniform and delicate makeup color with a high-end matte or satin finish, avoiding "spots" or "white marks" caused by agglomeration. This invention achieves layered coating of powder at different rotation speeds, resulting in high interfacial bonding strength between the powder and the matrix. The resulting three-dimensional network structure is more stable, significantly delaying sedimentation and oil phase separation caused by gravity. The product maintains its original texture, color, and performance throughout its shelf life, without deterioration due to increased powder agglomeration. Fully dispersed powder means more effectively covered particles per unit area, with uniform distribution, achieving better coverage with less powder. The pigment powder is fully dispersed and wetted, exhibiting its purest and most saturated color, avoiding whitening, dullness, or unevenness caused by agglomeration and air bubbles.

[0215] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for preparing a skin-adhering, long-lasting makeup composition, characterized in that, It includes: S1, Pre-crosslinked matrix: Polydimethylsiloxane and squalane are mixed under a first temperature and a first rotation speed to form a pre-crosslinked matrix; The first temperature is 55-65℃, the first rotation speed is 200-400rpm, and the mixing time is 20-40min; S2. Homogenization: The pre-crosslinked matrix is ​​cooled to a second temperature, and ethylhexyl palmitate and polyglycerol-3 diisostearate are added. The mixture is then maintained at the second temperature and the second rotation speed to form an oil phase. The mass ratio of polydimethylsiloxane, squalane, ethylhexyl palmitate, and polyglycerol-3 diisostearate is 10-15:3-5:10-20:3-15. The second temperature is 35-45℃, the second rotation speed is 400-500 rpm, and the mixing time is 10-30 min. S3. Sample solution: At room temperature, tin tetrachloride pentahydrate and antimony trichloride are dissolved in anhydrous ethanol by stirring. The solution is heated to 40-50°C and stirred until the solution is clear and transparent to obtain a tin-antimony solution. The mass ratio of tin tetrachloride pentahydrate, antimony trichloride and anhydrous ethanol is 3-11:6-13:4-13. S4. Oil phase addition: The oil phase is added to the tin-antimony-containing solution to obtain a mixture, wherein the mass ratio of the tin-antimony-containing solution to the oil phase is 3-10:5-20. S5. Hydrolysis and precipitation: Add ammonia water dropwise to the mixture and stir until the pH stabilizes at 6.8-7.2 to obtain a hydrolyzed mixture; S6. Centrifugation: Centrifuge the hydrolyzed mixture. After centrifugation, the system is divided into an upper oil phase composition, a middle aqueous phase, and a bottom precipitate. Take out the oil phase composition. S7. Powder dispersion: Under the protection of a protective gas, the powder matrix is ​​added to the oil phase composition in multiple batches, and the mixture is stirred and mixed with a gradually increasing speed after each addition to obtain a dispersion. The multiple batches include 2-4 batches, and the gradually increasing speed includes an initial speed of 400-600 rpm, with an increase of 200-600 rpm each time. The stirring and mixing time for each batch is 10-20 min, and the total mixing time is 30-65 min. S8. Finished product: The dispersion is added to a stabilizer, and then vacuum degassed, filled and sealed.

2. The method for preparing the skin-adhering and long-lasting makeup composition according to claim 1, characterized in that, The vacuum degassing temperature is 25-35℃, the vacuum degree is -0.1~-0.05MPa, and the degassing time is 10-20min.

3. The method for preparing the skin-adhering makeup composition according to claim 1, characterized in that, The centrifugation speed is 8000-12000 r / min, and the time is 8-12 min.

4. The method for preparing the skin-adhering and long-lasting makeup composition according to claim 1, characterized in that, The mass ratio of the oil phase composition, the powder matrix, and the stabilizer is 1:(0.45~0.96):(0.03~0.06).

5. The method for preparing the skin-adhering and long-lasting makeup composition according to claim 1, characterized in that, The powder matrix includes at least one of titanium dioxide and iron oxide; And / or, the stabilizer includes at least one of hydrogenated polyisobutylene, octanoic acid / decanoic acid triglyceride, and hydrogenated polydecene.

6. A skin-adhering, long-lasting makeup composition, characterized in that, It is prepared by the method of preparing the skin-adhering and long-lasting makeup composition as described in any one of claims 1-5.

7. The application of the skin-adhering and long-lasting makeup composition as described in claim 6 in the preparation of skin-adhering and long-lasting cosmetics, characterized in that, The amount of the skin-adhering and long-lasting makeup composition added to the cosmetic is 0.01-15 wt%.

8. The application according to claim 7, characterized in that, The cosmetics include at least one of sunscreen, BB cream, makeup base, and tone-up cream.

Images