Preparation method and application of oil-control and anti-dullness cosmetic composition

CN121533924BActive Publication Date: 2026-11-03MEISHANG(GZ)COSMETICS CO LTD
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Patent Information

Application Number
CN202511904146.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-12-17
Publication Date
2026-11-03
Estimated Expiration
2045-12-17

AI Technical Summary

Technical Problem

但这类材料仍存在一些不可忽视的问题:当皮脂分泌过多时,妆容仍容易脱落,甚至出现“油光”现象

Benefits of technology

本发明先以合成氟金云母为基底,再嫁接有机硅交联聚合物,后使用生育酚乙酸酯包覆,加入羟基磷灰石,最后以三乙氧基辛基硅烷进行改性,制备出控油抗暗沉的化妆品组合物,使组合物兼顾丝滑绵柔肤感与不易脱落的优势,达成控油和柔焦效果,并有效避免有机硅粉体快速吸油及油脂氧化导致的暗沉,高效吸附并凝胶化皮肤不饱和脂肪酸以强化控油,尤为适用于定妆产品中,减少皮脂分泌对妆容的影响,使妆容持久清爽。

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Abstract

The present application relates to the technical field of cosmetics, more specifically, it relates to a preparation method and application of an oil-controlling and anti-dullness cosmetic composition, and technical scheme points are as follows: S1, using wet chain transfer technology, grafting silicone cross-linked polymer on the surface of synthetic fluormica to obtain grafted powder; S2, using tocopherol acetate to coat the surface of the grafted powder to obtain coated powder; S3, mixing the coated powder and hydroxyapatite to obtain composite powder; S4, using triethoxysilane to perform surface modification treatment on the composite powder to obtain a product. The present application combines various components to prepare an oil-controlling and anti-dullness cosmetic composition, to provide a smooth and soft skin feel, enhance oil control and soft focus effect, and prevent oil oxidation and dullness.
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Description

Technical Field

[0001] This invention relates to the technical field of cosmetics, and more specifically, to a method for preparing and applying a cosmetic composition for controlling oil and combating dullness. Background Technology

[0002] Nowadays, almost every woman, and some men, wear makeup when going out or attending important events. However, as makeup wears on, it often becomes difficult to maintain its perfection. The main reason for this problem is that the skin naturally secretes oil, especially in summer or in humid and hot environments. Excessive sebum can easily cause makeup to smudge or become less effective. Therefore, consumers often use pressed powder or loose powder to absorb excess oil from the skin's surface.

[0003] Currently, most setting products on the market use porous powders to achieve oil control, such as porous silica, porous polymethyl methacrylate (PMMA), or certain metal salts with strong oil-absorbing capabilities. However, these materials still have some significant problems: when sebum secretion is excessive, makeup is still prone to fading and even results in a "shine" appearance. Specifically, porous silica not only absorbs oil but also draws away moisture, leading to dry skin; porous PMMA has limited oil-absorbing capacity; and metal salts have poor spreadability, feeling rough when used, and poor water resistance, making them prone to peeling. Furthermore, when these materials mix with sebum secreted by the skin, they can also cause makeup to melt or become dull. Summary of the Invention

[0004] In view of the shortcomings of the existing technology, the purpose of this invention is to provide a method for preparing an oil-controlling and anti-dullness cosmetic composition, which has the advantages of targeted absorption and flocculation and solidification of oils.

[0005] The above-mentioned technical objective of the present invention is achieved through the following technical solution: a method for preparing an oil-controlling and anti-dullness cosmetic composition, comprising the following steps: S1. Using wet chain transfer technology, organosilicon crosslinked polymers are grafted onto the surface of synthetic fluorophlogopite to obtain grafted powder; S2. Coating the surface of the grafting powder with tocopheryl acetate to obtain coated powder; S3. Mix the coated powder with hydroxyapatite to obtain a composite powder; S4. The composite powder is surface modified using triethoxyoctylsilane to obtain the target product.

[0006] In one embodiment, the specific steps of S1 include: S11. Dissolve the organosilicon crosslinked polymer in a solvent to prepare a first treatment solution; S12. The synthesized fluorophlogopite is added to a high-speed mixer, and the first treatment liquid is sprayed in during high-speed mixing for thorough mixing. Then, it is heated, air-jet pulverized, and surface-treated to obtain the grafted powder.

[0007] In one embodiment, the specific steps of S4 include: S41. Disperse the triethoxyoctylsilane using a 70% aqueous ethanol solution to prepare a second treatment solution; S42. The composite powder is added to a high-speed mixer, and the second treatment liquid is sprayed in during high-speed mixing for thorough mixing. Then, it is heated, air-jet pulverized, and surface treated to obtain the target product.

[0008] In one embodiment, the organosilicon crosslinking polymer includes one or more of polydimethylsiloxane / vinyl polydimethylsiloxane crosslinking polymer, polymethylsilsesquioxane, and vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinking polymer.

[0009] In one embodiment, the particle size of the organosilicon crosslinked polymer, the synthetic fluorophlogopite, and the hydroxyapatite are all 5-12 μm.

[0010] An oil-controlling and anti-dullness cosmetic composition is prepared by the above-described preparation method.

[0011] In one embodiment, the cosmetic composition comprises the following raw materials in parts by weight: 10-40 parts of organosilicon crosslinking polymer, 45-60 parts of synthetic fluorophlogopite, 0.5-1 part of tocopheryl acetate, 10-20 parts of hydroxyapatite, and 1-3 parts of triethoxyoctylsilane.

[0012] An oil-controlling and anti-dullness cosmetic, comprising the above-mentioned cosmetic composition and excipients; The excipients include at least one of the following: preservatives, chelating agents, fragrances, humectants, emollients, thickeners, colorants, emulsifiers, antioxidants, and skin conditioning agents.

[0013] In one embodiment, the cosmetic is a foundation. The excipients include deionized water, polydimethylsiloxane, titanium dioxide, butylene glycol, dioctyl carbonate, lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane, glycerin, caprylic / capric triglyceride, diisostearyl malate, PEG-10 polydimethylsiloxane, phenyl polytrimethylsiloxane, polymethyl methacrylate, HDI / trimethylolhexyl lactone crosspolymer, trimethylsiloxysilicate, 1,2-hexanediol, lithium distearate dimethylammonium montmorillonite, sodium chloride, magnesium stearate, ethylhexylglycerin, sodium hyaluronate, bisabolol, dipotassium glycyrrhizate, aloe vera leaf extract, tea leaf extract, centella asiatica extract, Ganoderma lucidum stem extract, ginseng root extract, licorice root extract, fragrance, disodium EDTA, and colorant.

[0014] In one embodiment, the oil-controlling and anti-dullness cosmetic composition is present in the cosmetic at a mass percentage of 3-5%.

[0015] The preparation method of the above-mentioned oil-controlling and anti-dullness cosmetic composition has the following beneficial effects: This invention first uses synthetic fluorophlogopite as a base, then grafts an organosilicon cross-linked polymer, followed by encapsulation with tocopheryl acetate, the addition of hydroxyapatite, and finally modification with triethoxyoctylsilane to prepare an oil-controlling and anti-dullness cosmetic composition. This composition combines the advantages of a silky smooth and soft feel with resistance to fading, achieving oil control and a soft-focus effect. It effectively avoids the dullness caused by rapid oil absorption and oil oxidation of organosilicon powder, and efficiently adsorbs and gels unsaturated fatty acids in the skin to enhance oil control. It is especially suitable for setting products, reducing the impact of sebum secretion on makeup and making makeup last longer and fresher. Attached Figure Description

[0016] Figure 1 This is a flowchart of the steps of the present invention. Detailed Implementation

[0017] The present invention will be further described in detail below with reference to embodiments. It should be noted that the embodiments described below are intended to facilitate understanding of the present invention and are not intended to limit it in any way. Unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. In case of any conflict, the definitions in this specification shall prevail.

[0018] As used herein, the terms “prepared from” and “comprising” are synonymous. The terms “comprising,” “including,” “having,” “containing,” or any other variations thereof, as used herein, are intended to cover non-exclusive inclusion. For example, a composition, step, method, article, or apparatus that includes the listed elements is not necessarily limited to those elements, but may include other elements not expressly listed or elements inherent to such composition, step, method, article, or apparatus.

[0019] The conjunction "composed of..." excludes any unspecified elements, steps, or components. If used in a claim, this phrase makes the claim closed, excluding materials other than those described, except for associated conventional impurities. When the phrase "composed of..." appears in a clause of the body of a claim rather than immediately following it, it limits only the elements described in that clause; other elements are not excluded from the claim as a whole.

[0020] When a quantity, concentration, or other value or parameter is expressed as a range, a preferred range, or a range defined by a series of upper and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pair of any upper or preferred value with any lower or preferred value, regardless of whether the range is disclosed individually. For example, when the range “1 to 5” is disclosed, the described range should be interpreted as including the ranges “1 to 4”, “1 to 3”, “1 to 2”, “1 to 2 and 4 to 5”, “1 to 3 and 5”, etc. When numerical ranges are described herein, unless otherwise stated, the range is intended to include its endpoints and all integers and fractions within that range.

[0021] A method for preparing an oil-controlling and anti-dullness cosmetic composition, such as... Figure 1 As shown, it includes the following steps: S1. Using wet chain transfer technology, organosilicon crosslinked polymers are grafted onto the surface of synthetic fluorophlogopite to obtain grafted powder; The specific steps of S1 are as follows: S11. Dissolve the organosilicon crosslinked polymer in a solvent to prepare a first treatment solution; S12. The synthetic fluorophlogopite is added to a high-speed mixer, and the first treatment liquid is sprayed in during high-speed mixing for thorough mixing. Then, it is heated, air-jet pulverized, and surface treated to obtain grafted powder. In practical applications, the solvent is a raw material that can dissolve organosilicon crosslinked polymers and has good volatility, such as isododecane and low-viscosity volatile silicone oil. The high-speed mixer used has a liquid atomizing device, which sprays the first treatment liquid into the synthetic fluorophlogopite while it is being stirred at high speed. This ensures that the organosilicon crosslinked polymer can be uniformly combined with the surface of the synthetic fluorophlogopite, enhancing its oil control and adsorption capabilities and improving the dispersibility of the powder. The key role of this step is to improve the performance of the powder, enabling it to have a high efficiency in oil adsorption and giving the final product a silky feel. In addition, in this step, heat treatment can effectively remove the previously added volatile solvents.

[0022] Furthermore, if the two raw materials are simply mixed by stirring, the flake-like synthetic fluorophlogopite and the spherical organosilicon crosslinked polymer are initially in a loose, dispersed state. However, as the standing time increases, the flake-like synthetic fluorophlogopite tends to aggregate, and the spherical organosilicon crosslinked polymer also tends to agglomerate, failing to achieve the silky smoothness and makeup-holding effect required by the composition. This mixing method also leads to uneven subsequent surface coating treatments, failing to achieve the desired oil control, makeup-holding, and anti-dullness effects.

[0023] S2. Coating the surface of the grafting powder with tocopheryl acetate to obtain coated powder; In practical applications, a high-speed mixer with an atomizing liquid device can still be used. Under high-speed mixing conditions, tocopheryl acetate is "atomized" and sprayed onto the surface of the grafting powder for coating. This ensures that tocopheryl acetate can be effectively coated, preventing the darkening phenomenon caused by oil adsorption, and allowing it to exert its moisturizing and antioxidant effects on the skin, avoiding the dryness or irritation caused by oil-controlling ingredients.

[0024] S3. Mix the coated powder with hydroxyapatite to obtain a composite powder; Hydroxyapatite and coated powder were mechanically and physically mixed at room temperature by stirring, which further enhanced the oil control effect by leveraging its properties of directional oil absorption and sebum solidification.

[0025] S4. The composite powder was surface modified using triethoxyoctylsilane to obtain the target product. The specific steps of S4 include: S41. Disperse triethoxyoctylsilane using a 70% aqueous ethanol solution to prepare a second treatment solution; S42. Add the composite powder to a high-speed mixer, and spray the second treatment liquid into it during high-speed mixing to mix it thoroughly. Then, heat it, air jet mill it, and surface treat it to obtain the target product. In practical applications, besides 70% ethanol, other solvents with good volatility can be used to disperse triethoxyoctylsilane, which can then be removed by subsequent heating. Surface modification with triethoxyoctylsilane imparts stronger hydrophobicity and water resistance to the powder, ensuring its long-term stable oil control effect while maintaining high-efficiency anti-dulling properties when exposed to moisture.

[0026] This invention first utilizes the ultra-high aspect ratio of synthetic fluorophlogopite as the base of the composite powder, giving the powder a natural and translucent makeup feel that is neither too white nor too pale, yet still brightens the complexion. The lamellar structure of fluorophlogopite provides excellent adhesion for the composite powder. Based on this, spherical organosilicon powder is grafted onto the mica surface. Combining the smoothness of the spherical powder with the adhesion of mica, the powder is silky smooth and does not easily fall off, while also possessing oil control and a soft-focus effect.

[0027] Next, the surface of the grafted powder is coated with tocopheryl acetate (VE). Tocopheryl acetate has good antioxidant properties, which can effectively prevent the silicone powder from absorbing the skin's secreted oil too quickly and avoid dullness caused by oil oxidation.

[0028] Subsequently, hydroxyapatite is added to the surface of the coated powder. Hydroxyapatite can efficiently adsorb unsaturated fatty acids (such as oleic acid) secreted by the skin and gel them in a short time, enhancing the oil-controlling effect. In addition, the calcium ions in hydroxyapatite help regulate the lipid arrangement of the stratum corneum, enhance the skin barrier function, and reduce moisture loss. Its porous structure can also adsorb moisture, forming a moisturizing barrier and effectively improving dry skin problems.

[0029] Finally, the composite powder was modified by secondary surface coating using triethoxyoctylsilane. By utilizing its hydrophobicity to water and oil, the powder's anti-sweat and anti-oil properties were improved, thereby enhancing the makeup-holding and anti-dulling effects of the composite powder.

[0030] Specifically, the silicone crosslinking polymers include one or more of polydimethylsiloxane / vinyl polydimethylsiloxane crosslinking polymers, polymethylsilsesquioxane, and vinyl polydimethylsiloxane / polymethylsiloxane silsesquioxane crosslinking polymers. In practical applications, polydimethylsiloxane / vinyl polydimethylsiloxane crosslinking polymers, polymethylsilsesquioxane, and vinyl polydimethylsiloxane / polymethylsilsesquioxane silsesquioxane crosslinking polymers are all spherical powders, which can effectively achieve oil control, soft-focus, and velvety makeup effects.

[0031] Furthermore, the particle sizes of the organosilicon crosslinking polymer, synthetic fluorophlogopite, and hydroxyapatite are all 5-12 μm. In practical applications, the particle size D50 of hydroxyapatite is 11.46 μm. By controlling the particle size of the powder raw materials, the obtained cosmetic composition can achieve better oil control, soft-focus, and velvety effects.

[0032] An oil-controlling and anti-dullness cosmetic composition is prepared by the above-described preparation method.

[0033] Furthermore, the oil-controlling and anti-dullness cosmetic composition consists of the following raw materials in parts by weight: 10-40 parts of organosilicon crosslinking polymer, 45-60 parts of synthetic fluorophlogopite, 0.5-1 part of tocopheryl acetate, 10-20 parts of hydroxyapatite, and 1-3 parts of triethoxyoctylsilane.

[0034] Traditional silica, with its porous structure, can absorb sebum and moisture from the skin and cosmetics. However, due to its spherical shape, the absorbed moisture merely adheres to the skin surface and cannot participate in the stratum corneum arrangement. It cannot form a barrier on the skin's surface or prevent moisture from flowing from within the skin into the porous interior of the silica spheres, resulting in continuous moisture loss from the skin. Furthermore, its pores lack a highly ordered structure, preventing the absorbed moisture and moisturizing ingredients from penetrating and being absorbed into the skin layers. This fails to achieve controlled-release and sustained-release effects, thus creating a "drying" sensation.

[0035] This invention utilizes hydroxyapatite, which exhibits high adsorption capacity for unsaturated fatty acids (oleic acid). Compared to other powders, it can gel oleic acid in a short time. Furthermore, the calcium ions in hydroxyapatite participate in the lipid arrangement of the stratum corneum, enhancing the skin barrier function and reducing moisture loss from the skin. Its porous structure can adsorb moisture from cosmetics, forming a moisturizing barrier. In addition, hydroxyapatite possesses a highly ordered pore structure, which can fix adsorbed moisture and oil within its pores, facilitating the penetration and absorption of moisturizing ingredients into the skin layer. This improves the permeability and absorption of cosmetics, achieving controlled-release and sustained-release effects without causing dryness.

[0036] In practical applications, if the hydroxyapatite content is less than 10 parts, it can easily lead to insufficient absorption and solidification of the oils secreted by human skin; while if the content exceeds 20 parts, it will not only fail to fully exert the effect of the raw material, but will also significantly increase the cost.

[0037] An oil-controlling and anti-dullness cosmetic, comprising the above-mentioned cosmetic composition and excipients; The excipients include at least one of the following: preservatives, chelating agents, fragrances, humectants, emollients, thickeners, colorants, emulsifiers, antioxidants, and skin conditioning agents.

[0038] Furthermore, the aforementioned oil-controlling and anti-dullness cosmetics are foundation liquids; in practical applications, these cosmetics can also be foundation creams, makeup primers, cushion BB creams, or concealer liquids. The excipients include 30-40% deionized water, 10-20% polydimethylsiloxane, 8-15% titanium dioxide, 3-8% butanediol, 3-5% dioctyl carbonate, 2-4% lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane, 2-4% glycerol, 2-4% caprylic / capric triglyceride, 2-4% diisostearyl malate, 1-3% PEG-10 polydimethylsiloxane, 1-6% phenyl polytrimethylsiloxane, 1-3% polymethyl methacrylate, 1-3% HDI / trimethylolhexyl lactone crosspolymer, 3-8% trimethylsiloxysilicate, 1-2% 1,2-hexanediol, 0.8-1.5% distearate dimethylammonium lithium montmorillonite, and 0.8-1. 5% sodium chloride, 0.3-1.0% magnesium stearate, 0.1-0.5% polydimethylsiloxane / vinyl polydimethylsiloxane crosspolymer, 0.1-0.5% ethylhexylglycerin, 0.02-0.1% sodium hyaluronate, 0.02-0.1% bisabolol, 0.02-0.1% dipotassium glycyrrhizate, 0.01-0.1% aloe vera leaf extract, 0.01-0.1% tea extract, 0.01-0.1% centella asiatica extract, 0.01-0.1% Ganoderma lucidum stem extract, 0.01-0.1% ginseng root extract, 0.01-0.1% licorice root extract, 0.01-0.1% fragrance, 0.01-0.1% disodium EDTA and appropriate amount of color powder.

[0039] Furthermore, the oil-controlling and anti-dullness cosmetic composition accounts for 3-5% of the cosmetic's mass percentage.

[0040] In practical applications, the above-mentioned foundation liquid is prepared through the following steps: (1) Polydimethylsiloxane, polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer and trimethylsiloxysilicate are premixed and dispersed evenly to form phase B; (2) The above-mentioned oil-controlling and anti-dullness cosmetic composition, titanium dioxide, triethoxyoctylsilane, pigment, HDI / trimethylolhexyl lactone crosspolymer, polymethyl methacrylate and magnesium stearate are evenly dispersed in a powder homogenizer to form phase C; (3) Add deionized water, butanediol, sodium chloride, disodium EDTA, glycerol, sodium hyaluronate and dipotassium glycyrrhizate to the aqueous phase pot in sequence to form phase D. Stir and heat to 80-85℃ until completely dissolved and homogeneous. (4) Add the components of diisostearyl malate, caprylic / capric triglyceride, dioctyl carbonate, phenyl polytrimethylsiloxane, lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane, PEG-10 polydimethylsiloxane and distearate dimethylammonium lithium montmorillonite to the emulsification pot in sequence to form phase A, stir and heat to 80-85℃, and completely melt and homogenize; Add the pre-dispersed phase C to phase A, homogenize and stir until uniform, heat to 80-85℃, add the pre-dispersed phase B before emulsification, stir until uniform, vacuum the emulsification pot (-0.05MPa), and use the negative pressure to slowly draw the material in the aqueous phase pot into the emulsification pot through the filter screen for emulsification. At the same time, start homogenization and stirring at 3000rpm for 15-20min. Then turn on the circulating water to cool down and maintain vacuum to defoam. (5) Cool down to 60°C, add 1,2-hexanediol and ethylhexylglycerin, stir and homogenize for 3-5 min; (6) Cool down to 45°C, add Aloe vera leaf extract, tea extract, Centella asiatica extract, Ganoderma lucidum stem extract, ginseng root extract, Glycyrrhiza glabra root extract and flavoring in sequence, stir well, and vacuum degas. (7) Continue to cool down to 38℃, and discharge the material after passing the inspection.

[0041] The following examples and comparative examples provide further explanation: Examples 1-3 and Comparative Examples 1-3 respectively provide cosmetic compositions for oil control and anti-dullness, and the specific components are shown in Table 1:

[0042] Table 1

[0043] The specific preparation steps for Examples 1-3 are as follows: S1. Weigh the organosilicon crosslinking polymer according to the proportion and dissolve it in 2 times the amount of isododecane to prepare the first treatment solution; The synthetic fluorophlogopite was weighed out in proportion and added to a high-speed mixer. The first treatment liquid was sprayed into the mixer under high-speed mixing conditions to fully mix the synthetic fluorophlogopite with the first treatment liquid. Then, it was heated and dried at 80°C, and after air jet pulverization and surface treatment, grafted powder was obtained. S2. Add the grafting powder obtained in S1 into a high-speed mixer. Under high-speed mixing conditions, spray tocopheryl acetate into the mixer in proportion to coat the surface of the grafting powder and obtain coated powder. S3. The powder obtained in S2 is put into a high-speed mixer, and an appropriate amount of hydroxyapatite is added in proportion. The mixture is mechanically and physically mixed at room temperature to obtain composite powder. S4. Weigh out triethoxyoctylsilane according to the proportion, disperse it with 2 times the amount of 70% ethanol aqueous solution, and prepare the second treatment solution. The composite powder obtained in S3 is added to a high-speed mixer, and a second treatment liquid is sprayed in under high-speed stirring conditions to fully mix the second treatment liquid with the composite powder. Then, it is heated and dried at 80°C, followed by air jet pulverization and surface treatment to obtain the target product.

[0044] Unlike Example 1, the preparation steps for Comparative Example 1 are as follows: Tocopheryl acetate and triethoxyoctylsilane were mixed in advance to prepare a mixture; Then, the organosilicon crosslinking polymer, synthetic fluorophlogopite, and hydroxyapatite were sequentially added to a high-speed mixer. During high-speed mixing, the mixture of tocopheryl acetate and triethoxyoctylsilane was atomized and sprayed onto the powder. After high-speed mixing, the mixture and powder were fully mixed to obtain the target product.

[0045] Unlike Example 2, the preparation steps for Comparative Example 2 are as follows: S1. Weigh the organosilicon crosslinking polymer according to the proportion and dissolve it in 2 times the amount of isododecane to prepare the first treatment solution; The synthetic fluorophlogopite was weighed out in proportion and added to a high-speed mixer. The first treatment liquid was sprayed into the mixer under high-speed mixing conditions to fully mix the synthetic fluorophlogopite with the first treatment liquid. Then, it was heated and dried at 80°C, and after air jet pulverization and surface treatment, grafted powder was obtained. S2. Weigh out triethoxyoctylsilane according to the proportion, disperse it with 2 times the amount of 70% aqueous ethanol solution, and prepare the second treatment solution. The grafted powder obtained in S1 was added to a high-speed mixer, and a second treatment liquid was sprayed in under high-speed mixing conditions to fully mix the second treatment liquid with the composite powder. Then, it was heated and dried at 80°C, and after air jet pulverization and surface treatment, the first composite powder was obtained. S3. The first composite powder obtained in S2 is put into a high-speed mixer, and an appropriate amount of hydroxyapatite is added in proportion. The mixture is mechanically and physically mixed at room temperature to obtain the second composite powder. S4. Add the second composite powder obtained in S3 into a high-speed mixer. Under high-speed mixing conditions, spray tocopheryl acetate into the mixer in proportion to coat the surface of the second composite powder and obtain the target product.

[0046] Unlike Example 3, the preparation steps for Comparative Example 3 are as follows: S1. Weigh out synthetic fluorophlogopite and hydroxyapatite in proportion, and mix them mechanically and physically at room temperature to obtain composite powder. S2. Weigh the organosilicon crosslinking polymer according to the proportion and dissolve it in 2 times the amount of isododecane to prepare the first treatment solution; The composite powder obtained in S1 is added to a high-speed mixer. Under high-speed mixing conditions, the first treatment liquid is sprayed into the mixer to fully mix the synthetic fluorophlogopite with the first treatment liquid. Then, it is heated and dried at 80°C, and after air jet pulverization and surface treatment, the grafted powder is obtained. S3. Add the grafting powder obtained in S2 into a high-speed mixer. Under high-speed mixing conditions, spray tocopheryl acetate into the mixer in proportion to coat the surface of the grafting powder and obtain coated powder. S4. Weigh out triethoxyoctylsilane according to the proportion, disperse it with 2 times the amount of 70% ethanol aqueous solution, and prepare the second treatment solution. The coated powder obtained in S3 is added to a high-speed mixer, and a second treatment liquid is sprayed in under high-speed mixing conditions to fully mix the second treatment liquid with the coated powder. Then, it is heated and dried at 80°C, and the target product is obtained by air jet milling and surface treatment.

[0047] Efficacy test comparison: As shown in Table 2, Examples 1-3, Comparative Examples 1-3, and the purchased silica raw material were used as Comparative Example 4 in the preparation of cosmetics to obtain foundation liquids using Examples 1-3 and Comparative Examples 1-4. A control group was set up simultaneously to conduct relevant efficacy tests.

[0048]

[0049] Table 2

[0050] The specific preparation steps for the foundation liquids used in the control group, Application Examples 1-3, and Application Comparative Examples 1-4 are as follows: (1) Weigh phase B according to the proportion, and mix and disperse it evenly for later use; (2) Weigh phase C according to the proportion, disperse it evenly using a powder homogenizer, and set aside; (3) Weigh phase D according to the proportion and add it to the aqueous phase pot. Stir and heat to 80-85℃ to make it completely dissolved and homogeneous. (4) Weigh phase A according to the proportion and add it to the emulsification pot to form phase A. Stir and heat to 80-85℃ to make it completely melt and uniform. Then add the pre-dispersed phase C, homogenize and stir evenly, and heat to 80-85℃. Before emulsification, add the pre-dispersed phase B and stir evenly. Vacuum the emulsification pot (-0.05MPa). Use the negative pressure to slowly draw phase D in the aqueous phase pot into the emulsification pot through the filter screen for emulsification. At the same time, turn on the homogenizer and stir at 3000rpm for 15-20min. Then turn on the circulating water to cool down and maintain the vacuum to defoam. (5) Cool down to 60℃, add phase E in proportion, stir and homogenize for 3-5 minutes; (6) Cool down to 45°C, add phase F in proportion, stir evenly, and degas under vacuum; (7) Continue to cool down to 38℃, and discharge the material after passing the inspection.

[0051] The performance of the foundation liquids used in the control group, Examples 1-3, and Comparative Examples 1-4 was compared using relevant performance tests. The test items and methods are as follows: Test 1: Patch test.

[0052] Participants: A total of 30 participants, including 16 males and 14 females, aged 20 to 40 years, who met the inclusion criteria for the study volunteers.

[0053] Test materials: control group and foundation liquids used in Examples 1-3, with a blank group also included.

[0054] Test method: Select qualified patch testing equipment and use the closed patch test method. Place about 0.020g-0.025g of the mixed test substance in the patch testing device, apply it to the back of the subject with hypoallergenic adhesive tape, remove the test substance after 24 hours, and observe the skin reaction at 0.5, 24 and 48 hours after removal. Record the results according to the skin reaction grading standard in the "Cosmetic Safety Technical Specifications" (2015 edition) (Table 3).

[0055]

[0056] Table 3

[0057]

[0058] Table 4

[0059] The test results are shown in Table 4. The oil-controlling and anti-dullness cosmetic composition prepared by this invention is unlikely to cause allergic or irritating reactions, and all test groups showed negative skin reactions at different time points. This result indicates that the foundation prepared using the product of this invention has good safety and adaptability on the skin, does not cause adverse reactions, and is suitable for all skin types.

[0060] Test 2: Skin oil content test.

[0061] Test substances: foundation liquids used in Examples 1-3 and Comparative Examples 1-4.

[0062] Participants: A total of 70 participants, including 16 males and 54 females, aged 18–35 years, with a forehead oil content greater than 120 µg / cm². 2 Those who meet the selection criteria for the trial volunteers are divided into 7 groups of 10 people each.

[0063] Test environment: Temperature 21±1℃, relative humidity 50%+10%.

[0064] Test Principle: The internationally recognized SEBUMETER method for oil content testing is used. This method is based on the principle of photometry. A special matte adhesive tape with a thickness of 0.1mm absorbs the oil on human skin, forming a semi-transparent tape. The amount of oil in the skin is measured by the change in light transmittance. The more oil absorbed, the greater the light transmittance. This is an indirect method for measuring sebum secretion. The results can be used to distinguish different skin types and accurately understand the changes in sebum production caused by internal and external factors. The biggest advantage of this method is its ease of use and the fact that the test site is not limited.

[0065] Test method: Before the test, cleanse your face. Then, sit quietly in an indoor environment with an ambient temperature of 21±1℃ and a relative humidity of 50%+10% for 30 minutes. Test and record the oil content on your forehead as the initial oil content. Then, use one product for each group and test the oil content 2 hours and 4 hours after using the product.

[0066]

[0067] Table 5

[0068]

[0069] Table 6

[0070] The results are shown in Tables 5 and 6. The test data show that, under the premise that all raw material components are the same, comparing the application of Examples 1-3 with Comparative Examples 1-3, the oil-controlling and anti-dullness compositions of Examples 1-3 exhibit significantly better oil-controlling effects and durability than those of Comparative Examples 1-3. Furthermore, the oil-controlling effects and durability of Examples 1-3 are also significantly better than those of Comparative Example 4 (which uses silica, a commonly used oil-controlling raw material).

[0071] Test 3: Consumer Reviews.

[0072] Test substances: foundation liquids used in Examples 1-3 and Comparative Examples 1-4.

[0073] Subjects: A total of 140 participants, including 33 males and 107 females, aged 18 to 40 years, with oily and combination skin, etc., meeting the inclusion criteria for the subjects, with 20 participants in each group.

[0074] Testing Method: Volunteers used the foundation for 4 weeks (1mL each time after cleansing, morning and evening). Each volunteer provided an objective evaluation of the foundation. Questionnaires were collected and the results were analyzed. The questionnaire included evaluations of five aspects: the foundation's gentleness, its ability to control oil secretion, its oil-controlling and makeup-holding time, its improvement of skin condition, and personal preference. A 10-point scale was used for evaluation. Volunteers scored based on their own experiences, with higher scores indicating stronger characteristic features of the item. The average of the collected data was used for analysis.

[0075]

[0076] Table 7

[0077] Table 7 shows consumer reviews of the oil-controlling and anti-dullness effects of different foundations. Among them, the oil-controlling and anti-dullness long-lasting foundations of Examples 1-3 (the oil-controlling and anti-dullness compositions of Examples 1-3) received higher ratings than the foundations of Comparative Examples 1-4 in terms of gentleness, ability to control sebum secretion, oil-controlling and makeup-lasting time, improvement of skin condition, and personal preference. In particular, the oil-controlling and anti-dullness long-lasting foundation of Example 1 (the oil-controlling and anti-dullness composition of Example 1) received the highest scores in all aspects.

[0078] In addition, regarding the oil control and anti-dullness effect of the foundation, the evaluators assessed the makeup of the volunteers 8 hours after using the foundation, according to the evaluation criteria in Table 8. The results are shown in Table 9.

[0079]

[0080] Table 8

[0081]

[0082] Table 9

[0083] Table 9 shows the oil-control and anti-dullness effects of the foundation after 8 hours of use, and the percentage of people in different categories is statistically analyzed. The effects of applications in Examples 1-3 (virtually no dullness and / or significantly no dullness and / or noticeably effective no dullness) were superior to those in Comparative Examples 1-4, with Example 1 showing the best results. The product prepared by this invention showed strong oil-control and anti-dullness effects in all test results across different examples, especially Example 1, which exhibited the best effect among all examples. The foundation of Example 1 has excellent makeup-holding and oil-control effects, demonstrating significant advantages in all tests, making it particularly suitable for consumers who need to maintain a perfect makeup look for a long time. Furthermore, the oil-control and anti-dullness composition prepared by this invention is gentle and non-irritating, and has broad application prospects in cosmetics.

[0084] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention. Therefore, the scope of protection of this patent should be determined by the appended claims.

Claims

1. A method for preparing an oil-controlling and anti-dullness cosmetic composition, characterized in that, Includes the following steps: S1. Using wet chain transfer technology, organosilicon crosslinked polymers are grafted onto the surface of synthetic fluorophlogopite to obtain grafted powder; S2. Coating the surface of the grafting powder with tocopheryl acetate to obtain coated powder; S3. Mix the coated powder with hydroxyapatite to obtain a composite powder; S4. The composite powder is surface modified using triethoxyoctylsilane to obtain the target product; The amounts of each raw material, by weight, are as follows: 10-40 parts of the organosilicon crosslinking polymer, 45-60 parts of the synthetic fluorophlogopite, 0.5-1 part of the tocopherol acetate, 10-20 parts of the hydroxyapatite, and 1-3 parts of the triethoxyoctylsilane. The specific steps of S1 include: S11. Dissolve the organosilicon crosslinked polymer in a solvent to prepare a first treatment solution; S12. The synthesized fluorophlogopite is added to a high-speed mixer, and the first treatment liquid is sprayed in during high-speed mixing for thorough mixing. Then, it is heated, air-jet pulverized, and surface treated to obtain the grafted powder. The organosilicon crosslinked polymer is one or more of polydimethylsiloxane / vinyl polydimethylsiloxane crosslinked polymer, polymethylsilsesquioxane, and vinyl polydimethylsiloxane / polymethylsilsesquioxane crosslinked polymer.

2. The method for preparing an oil-controlling and anti-dullness cosmetic composition according to claim 1, characterized in that, The specific steps of S4 include: S41. Disperse the triethoxyoctylsilane using a 70% aqueous ethanol solution to prepare a second treatment solution; S42. The composite powder is added to a high-speed mixer, and the second treatment liquid is sprayed in during high-speed mixing for thorough mixing. Then, it is heated, air-jet pulverized, and surface treated to obtain the target product.

3. The method for preparing an oil-controlling and anti-dullness cosmetic composition according to claim 1, characterized in that: The particle size of the organosilicon crosslinked polymer, the synthetic fluorophlogopite, and the hydroxyapatite are all 5-12 μm.

4. A cosmetic composition for controlling oil and combating dullness, characterized in that, The cosmetic composition for oil control and anti-dullness is prepared according to any one of claims 1-3.

5. The oil-controlling and anti-dullness cosmetic composition according to claim 4, characterized in that, It is composed of the following raw materials in parts by weight: 10-40 parts of organosilicon crosslinking polymer, 45-60 parts of synthetic fluorophlogopite, 0.5-1 part of tocopheryl acetate, 10-20 parts of hydroxyapatite, and 1-3 parts of triethoxyoctylsilane.

6. A cosmetic product for controlling oil and combating dullness, characterized in that: Includes the cosmetic composition and excipients as described in claim 4; The excipients include at least one of the following: preservatives, chelating agents, fragrances, humectants, emollients, thickeners, colorants, emulsifiers, antioxidants, and skin conditioning agents.

7. A cosmetic product for controlling oil and preventing dullness according to claim 6, characterized in that: The cosmetic product is a liquid foundation; The excipients include deionized water, polydimethylsiloxane, titanium dioxide, butylene glycol, dioctyl carbonate, lauryl PEG-9 polydimethylsiloxane ethyl polydimethylsiloxane, glycerin, caprylic / capric triglyceride, diisostearyl malate, PEG-10 polydimethylsiloxane, phenyl polytrimethylsiloxane, polymethyl methacrylate, HDI / trimethylolhexyl lactone crosspolymer, trimethylsiloxysilicate, 1,2-hexanediol, lithium distearate dimethylammonium montmorillonite, sodium chloride, magnesium stearate, ethylhexylglycerin, sodium hyaluronate, bisabolol, dipotassium glycyrrhizate, aloe vera leaf extract, tea leaf extract, centella asiatica extract, Ganoderma lucidum stem extract, ginseng root extract, licorice root extract, fragrance, disodium EDTA, and colorant.

8. A cosmetic product for controlling oil and preventing dullness according to claim 6, characterized in that: The oil-controlling and anti-dullness cosmetic composition has a mass percentage of 3-5% in the cosmetic.

Citation Information

Patent Citations

  • Makeup-keeping and oil-controlling composition as well as preparation method and application thereof

    CN116687803A

  • Primary makeup product with efficient makeup maintaining effect and preparation method

    CN118948664A