Oil-controlling composite material, its manufacturing method and cosmetics

A high-pressure homogenized composite material of fullerene, hydroxyapatite, and zinc oxide with a substrate, enhanced by gardenia fruit extract, addresses the issue of selective sebum adsorption and oxidation prevention, improving makeup performance and skin health.

JP7747876B2Active Publication Date: 2025-10-01INST OF CHEM CHINESE ACAD OF SCI
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Patent Information

Application Number
JP2024508106
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2022-03-14
Filing Date
2022-08-11
Publication Date
2025-10-01
Estimated Expiration
2042-08-11

AI Technical Summary

Technical Problem

Existing oil-control powders fail to selectively adsorb different types of oil, leading to over-control, difficulty in makeup application, uneven application, stickiness, and dryness, and insufficient adsorption of sebum.

Method used

A composite material composed of fullerene, hydroxyapatite, zinc oxide, and a substrate, homogenized under high pressure to form a uniform and smooth surface, selectively adsorbing sebum and preventing oxidation, with the addition of gardenia fruit extract for antioxidant properties.

Benefits of technology

The composite material effectively adsorbs and aggregates sebum, prevents oxidation, reduces cytotoxicity, and minimizes UV transmittance, while maintaining a smooth skin feel and reducing makeup dullness.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides an oil-control composite material obtained by high-pressure homogenization of a mixture containing 30-90 parts by mass of at least one base material selected from the group consisting of synthetic fluorphlogopite, silica, alumina, and organosilicon powder, 0.0001-6 parts by mass of fullerene, 1-50 parts by mass of hydroxyapatite, and 0.1-30 parts by mass of zinc oxide. The present invention also provides a method for producing the oil-control composite material. The present invention also provides a cosmetic. The oil-control composite material provided by the present invention has the functions of selectively adsorbing sebum, agglomerating sebum, and preventing oxidization of sebum, and can completely resolve the effect of sebum on makeup by forming a closed loop from selective adsorption of sebum to agglomeration of sebum and further prevention of oxidization of sebum. The oil-control composite material provided by the present application also has the effects of reducing cytotoxicity and ultraviolet light transmittance.
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Description

cross reference

[0001] This application claims priority to a Chinese patent application filed with the China Patent Office on March 14, 2022, with application number 202210246508.4, entitled "Oil-control composite material, its manufacturing method and cosmetics," the entire contents of which are incorporated herein by reference. [Technical Field]

[0002] The present invention relates to the technical field of daily cosmetics, and in particular to an oil-controlling composite material, its manufacturing method and cosmetic product. [Background technology]

[0003] Excessive oil secretion from facial skin can cause even the most delicate makeup to appear oily and smudge, making oil control one of the core problems that makeup base products aim to solve. Most commercially available oil-control powders are made of mesoporous materials, which are unable to selectively adsorb different types of oil and can over-control oil. Over-controlling oil can lead to a series of problems, including difficulty applying the makeup base, uneven application, makeup stickiness, and dryness.

[0004] Hydroxyapatite has good biological activity and biocompatibility and has been widely studied in biology and medicine. Bones and teeth are typical biomineralized tissues, and their inorganic components are all hydroxyapatite. Hydroxyapatite is a hexagonal crystal with microcrystalline structure and several possible surface states, as described below. (1) When OH groups are on the crystal surface, the positions of the surface OH groups that bind with two Ca(II) ions are vacant at least at some moment, and because the two Ca(II) ions are positively charged, the positively charged PO4 3- Or, adsorption sites that can adsorb phosphate or carboxyl groups on the polymer are formed. (2) When Ca ions are on the crystal surface, Ca(I) is bonded to six negatively charged O atoms. Therefore, if a Ca(I) site on the surface becomes vacant at a certain moment, Sr 3+, K. + Hydroxyapatite has a certain degree of selective adsorption due to the characteristics of its crystal surface structure.

[0005] CN112741775A provides a cosmetic composite mica powder with oil-controlling properties, which is made by coating the surface of cosmetic-grade mica powder with zinc oxide and hydroxyapatite, and a method for producing the same. This material has a certain directional oil absorption effect, but its adsorption effect on oil secreted from facial skin is insufficient. Summary of the Invention

[0006] The present invention has been made in view of the above circumstances, and aims to provide an oil-control composite material, a manufacturing method thereof, and a cosmetic product. The oil-control composite material provided by the present invention has the functions of selectively adsorbing sebum, aggregating sebum, and preventing sebum oxidation, and has a strong sebum adsorption ability.

[0007] The present invention provides 0.0001 to 6 parts by mass of fullerene; 1 to 50 parts by mass of hydroxyapatite; 0.1 to 30 parts by mass of zinc oxide, The oil-control composite material is obtained by high-pressure homogenizing a mixture containing synthetic fluorphlogopite, silica, alumina, and 40 to 90 parts by mass of at least one base material selected from the group consisting of organosilicon powder.

[0008] The present invention uses as raw materials at least one substrate selected from the group consisting of synthetic fluorphlogopite, silica, alumina, and organic silicon powder, fullerene, hydroxyapatite, and zinc oxide, and homogenizes under high pressure so that the fullerene, hydroxyapatite, and zinc oxide are interlocked with the substrate, thereby obtaining a composite material that is relatively uniform and has a relatively flat surface and smoother corners, thereby improving the oil control effect of the composite material.

[0009] The mixture provided by the present invention contains fullerenes with large π-bond conjugated systems composed of multiple P orbitals, which give them a strong electron-accepting ability. Furthermore, due to their unique structure and physicochemical properties, they exhibit excellent free radical scavenging properties, earning them the nickname "free radical sponge," as well as excellent antioxidant properties. Therefore, they have attracted widespread attention in the fields of cosmetic materials and biopharmaceuticals. In the present invention, by conjugating fullerenes to a substrate, the dispersion of fullerenes is improved, thereby improving the performance of the resulting composite material. In one embodiment, the amount of fullerene used is 0.0001 to 6 parts by mass. In one embodiment, the amount of fullerene used is 0.001 to 4 parts by mass. In one embodiment, the amount of fullerene used is 0.01 to 2 parts by mass.

[0010] The mixture provided by the present invention contains hydroxyapatite. Hydroxyapatite has a certain degree of selective adsorption ability for oils and fats due to the characteristics of its crystal surface structure. In one embodiment, the amount of hydroxyapatite used is 1 to 50 parts by mass. In one embodiment, the amount of hydroxyapatite used is 5 to 40 parts by mass. In one embodiment, the amount of hydroxyapatite used is 10 to 30 parts by mass.

[0011] The mixture provided by the present invention contains zinc oxide. Zinc oxide has astringent and drying functions. In one embodiment, the amount of zinc oxide used is 0.1 to 30 parts by mass. In one embodiment, the amount of zinc oxide used is 1 to 20 parts by mass. In one embodiment, the amount of zinc oxide used is 5 to 15 parts by mass.

[0012] The mixture provided by the present invention includes a substrate. The substrate is at least one selected from the group consisting of synthetic fluorphlogopite, silica, alumina, and organosilicon powder. In one embodiment, the amount of the substrate used is 40 to 90 parts by mass. In one embodiment, the amount of the substrate used is 45 to 85 parts by mass. In one embodiment, the amount of the substrate used is 50 to 80 parts by mass.

[0013] In one embodiment, the mixture comprises: 0.001 to 4 parts by mass of fullerene; 5 to 40 parts by mass of hydroxyapatite, 1 to 20 parts by mass of zinc oxide, and 45 to 85 parts by mass of the base material.

[0014] In one embodiment, the mixture comprises: 0.01 to 2 parts by mass of fullerene; 10 to 30 parts by mass of hydroxyapatite, 5 to 15 parts by mass of zinc oxide, and 50 to 80 parts by mass of the base material.

[0015] In the present invention, the oil-control composite material is obtained by high-pressure homogenizing the mixture. In one embodiment, the oil-control composite material has a particle size of 300 mesh or less.

[0016] The oil-control composite material provided by the present invention has the effects of selectively adsorbing sebum, agglomerating sebum, and preventing sebum oxidation, forming a closed loop that completely resolves the impact of sebum on makeup and can be widely used in oil-control cosmetics.

[0017] The present invention also provides a method for producing a powder of a fullerene, comprising the steps of: uniformly mixing 0.0001 to 6 parts by mass of fullerene, 1 to 50 parts by mass of hydroxyapatite, 0.1 to 30 parts by mass of zinc oxide, 40 to 90 parts by mass of a base material (wherein the base material is at least one selected from the group consisting of synthetic fluorphlogopite, silica, alumina, and organic silicon powder), and 1,000 to 5,000 parts by mass of water to obtain a mixture; and subjecting the mixture to high-pressure homogenization, filtration, drying and pulverization in sequence to obtain the oil-control composite material.

[0018] In the present invention, first, the mixture is uniformly mixed with water to form a mixture. In one embodiment, the raw materials are uniformly mixed with water under stirring conditions. In one embodiment, the rotation speed of the stirring is 50 to 100 r / min.

[0019] In one embodiment, the method further includes a step of pre-homogenizing the mixture before the high-pressure homogenization. In one embodiment, the pre-homogenization is carried out under stirring conditions. In one embodiment, the pre-homogenization is carried out at a rotation speed of 800 to 1500 r / min for 30 to 90 minutes.

[0020] After the pre-homogenization, the resulting mixture is subjected to high-pressure homogenization in a high-pressure homogenizer. During the high-pressure homogenization process, the materials are subjected to mechanical forces such as high-speed shear, high-frequency vibration, cavitation and convection impact, which induce changes in the physical, chemical and structural properties of the materials, thereby interlocking the materials together and binding them into a single whole.

[0021] In one embodiment, the mixture is subjected to high-pressure homogenization 1 to 8 times. In one embodiment, the mixture is subjected to high-pressure homogenization 3 to 6 times. In one embodiment, the pressure of each high-pressure homogenization is 30 to 50 MPa. In one embodiment, the pressure of each high-pressure homogenization is 35 to 55 MPa.

[0022] After high-pressure homogenization is complete, the resulting mixture is filtered, dried, crushed, and sieved to obtain the oil-control composite material. Specifically, the solvent is first filtered using a plate and frame filter, and the residue is then vacuum-dried. The dried residue is crushed and passed through a sieve of 300 mesh or smaller to obtain the composite oil-control material.

[0023] The oil-control composite material provided by the present invention completely resolves the effects of sebum on makeup by forming a closed loop from selective adsorption of sebum to aggregation and prevention of sebum oxidation. The oil-control composite material provided by the present invention also has the effects of reducing cytotoxicity and UV transmittance.

[0024] The present invention also provides a cosmetic composition containing the oil-control composite material and gardenia fruit extract in a mass ratio of 90-99:0.1-10.

[0025] The gardenia fruit extract in the present invention refers to a blue powder obtained by purifying and drying gardenia fruit after hydrolysis, and has antioxidant properties, can reduce oxidation and dullness of oils and fats, and has the effect of correcting yellow color.When used in combination with a composite oil-control material, it has the effect of effectively reducing the dullness of makeup bases.

[0026] The gardenia fruit extract used in the present invention can be prepared according to the following procedure. The gardenia fruit is crushed, leached with an ethanol-water solution, and dried under reduced pressure to remove the ethanol, thereby obtaining a gardenia fruit slurry; The gardenia fruit slurry is enzymatically hydrolyzed and filtered. Add amino acids to the filtrate and let it react. The reaction mixture is purified using a macroporous resin, then concentrated and dried to obtain the gardenia fruit extract.

[0027] The extraction technology of gardenia fruit extract described in this invention has been matured and commercialized both at home and abroad.

[0028] In one embodiment of the present invention, the gardenia fruit extract used is purchased from Sensient Technologies Corp (China) Ltd. and has the product code GB618. 0.0125% gardenia fruit extract was measured to have a DPPH free radical clearance of 66.2%.

[0029] The present invention also provides a cosmetic product comprising the oil-control composite material and the cosmetic composition.

[0030] The oil-control composite material provided in the present invention can be used to prepare oil-control cosmetics, including, but not limited to, loose powder, powder cake, liquid foundation, cream foundation, BB cream, isolation cream, skin repair cream, paste concealer, liquid concealer, contouring powder cake, highlighting powder cake, and CC cream, etc.

[0031] The oil-control composite material provided by the present invention can be used in combination with gardenia fruit extract to prepare cosmetics, which have good antioxidant properties and can reduce the dullness of makeup base.

[0032] The cosmetic product includes the oil-control complex material and may further include other ingredients, the types and amounts of which can be appropriately determined by those skilled in the art according to the functional requirements of the cosmetic product, and therefore the description thereof will be omitted.

[0033] The present invention uses as raw materials at least one substrate selected from the group consisting of synthetic fluorphlogopite, silica, alumina, and organosilicon powder, fullerene, hydroxyapatite, and zinc oxide, and performs high-pressure homogenization. During the high-pressure homogenization process, the materials are subjected to mechanical forces such as high-speed shear, high-frequency vibration, cavitation, and convective impact, which induce changes in the physical, chemical, and structural properties of the materials, thereby causing the materials to interlock and bond into a single whole, resulting in a relatively uniform composite material with a relatively flat surface and smoother corners. The oil-control composite material provided by the present invention has the functions of selectively adsorbing sebum, aggregating sebum, and preventing sebum oxidation. By forming a closed loop from selective sebum adsorption to sebum aggregating and preventing sebum oxidation, it can completely resolve the effects of sebum on makeup. The oil-control composite material provided by the present invention also has the effects of reduced cytotoxicity and reduced UV transmittance. [Brief explanation of the drawings]

[0034] [Figure 1] FIG. 1 is a scanning electron micrograph of the material prepared in Example 8 of the present invention. [Figure 2] FIG. 2 is a particle size distribution diagram of the material prepared in Example 8 of the present invention. [Figure 3] FIG. 3 is a scanning electron micrograph of the material prepared in Comparative Example 4 of the present invention. [Figure 4] FIG. 4 is a photograph of the dispersion stability in water of the material prepared in Example 7 of the present invention. [Figure 5] FIG. 5 is a photograph of the dispersion stability in water of the material prepared in Comparative Example 4 of the present invention. [Figure 6] FIG. 6 shows Raman spectra of the materials prepared in the examples of the present invention and the comparative examples. [Figure 7] FIG. 7 shows the test results of free radical quenching for the materials provided in the examples of the present invention and the comparative examples. [Figure 8] FIG. 8 shows the test results of cell viability using the materials provided in the examples of the present invention and the comparative examples. DETAILED DESCRIPTION OF THE INVENTION

[0035] The oil-control composite material, its manufacturing method, and cosmetic product provided by the present invention will be described in detail below with reference to examples.

[0036] Example 1 A mixture of 0.0001 parts fullerene, 1 part hydroxyapatite, 30 parts zinc oxide, 50 parts flaky alumina, and 3000 parts deionized water was stirred at 60 r / min and homogenized for 60 minutes at 1000 r / min. The resulting slurry was then processed in a high-pressure homogenizer. This process was repeated four times under 40 MPa, after which the solvent was filtered off using a plate-and-frame filter. The resulting filter residue was vacuum-dried, pulverized, and sieved through a 300-mesh sieve to obtain a composite oil-control material. The composite oil-control material had a median diameter D50 of 1-20 μm.

[0037] Example 2 6 parts of fullerene, 50 parts of hydroxyapatite, 0.1 parts of zinc oxide, 90 parts of synthetic fluorphlogopite, and 3000 parts of deionized water were mixed and stirred uniformly at a rotation speed of 60 r / min, and then homogenized for 60 minutes at a rotation speed of 1000 r / min. The resulting slurry was treated in a high-pressure homogenizer. This was repeated four times under 40 MPa conditions, and the solvent was then filtered off using a plate and frame filter. The resulting filter residue was vacuum dried, and the dried filter residue was pulverized and sieved through a 300 mesh screen to obtain a composite oil-control material.

[0038] Example 3 0.001 parts of fullerene, 5 parts of hydroxyapatite, 20 parts of zinc oxide, 65 parts of organosilicon powder, and 3000 parts of deionized water were mixed and stirred uniformly at a rotation speed of 60 r / min, and then homogenized for 60 minutes at a rotation speed of 1000 r / min. The resulting slurry was treated in a high-pressure homogenizer. This was repeated four times under 40 MPa conditions, and the solvent was then filtered off using a plate and frame filter. The resulting filter residue was vacuum dried, and the dried filter residue was pulverized and sieved through a 300 mesh screen to obtain a composite oil-control material.

[0039] Example 4 Four parts of fullerene, 40 parts of hydroxyapatite, 1 part of zinc oxide, 90 parts of silica, and 3,000 parts of deionized water were mixed and stirred uniformly at a rotation speed of 60 r / min, and then homogenized for 60 minutes at a rotation speed of 1,000 r / min. The resulting slurry was treated in a high-pressure homogenizer. This was repeated four times under 40 MPa conditions, and the solvent was then filtered off using a plate and frame filter. The resulting filter residue was vacuum dried, and the dried filter residue was pulverized and sieved through a 300 mesh screen to obtain a composite oil-control material.

[0040] Example 5 0.01 part fullerene, 10 parts hydroxyapatite, 1 part zinc oxide, 40 parts silica, 30 parts alumina, and 3000 parts deionized water were mixed and stirred uniformly at a rotation speed of 60 r / min, and then homogenized for 60 minutes at a rotation speed of 1000 r / min. The resulting slurry was treated in a high-pressure homogenizer. This was repeated four times under 40 MPa conditions, and the solvent was then filtered off using a plate and frame filter. The resulting filter residue was vacuum dried, and the dried filter residue was pulverized and sieved through a 300 mesh screen to obtain a composite oil-control material.

[0041] Example 6 Two parts of fullerene, 30 parts of hydroxyapatite, 10 parts of zinc oxide, 40 parts of silica, 45 parts of synthetic fluorphlogopite, and 3000 parts of deionized water were mixed and stirred uniformly at a rotation speed of 60 r / min, and then homogenized for 60 minutes at a rotation speed of 1000 r / min. The resulting slurry was treated in a high-pressure homogenizer. This was repeated four times under 40 MPa conditions, and the solvent was then filtered off using a plate and frame filter. The resulting filter residue was vacuum dried, and the dried filter residue was pulverized and sieved through a 300 mesh screen to obtain a composite oil-control material.

[0042] Example 7 One part fullerene, 20 parts hydroxyapatite, 5 parts zinc oxide, 77.5 parts synthetic fluorphlogopite, and 3000 parts deionized water were mixed and stirred uniformly at a rotation speed of 60 r / min, and then homogenized for 60 minutes at a rotation speed of 1000 r / min. The resulting slurry was treated in a high-pressure homogenizer and repeated four times under 40 MPa conditions. The solvent was then filtered off using a plate and frame filter, and the resulting filtration residue was vacuum dried. The dried filtration residue was pulverized and sieved through a 300 mesh screen to obtain a composite oil-control material.

[0043] Example 8 0.02 parts of fullerene, 15 parts of hydroxyapatite, 5 parts of zinc oxide, 80 parts of synthetic fluorphlogopite, and 3000 parts of deionized water were mixed and stirred uniformly at a rotation speed of 60 r / min, and then homogenized for 60 minutes at a rotation speed of 1000 r / min. The resulting slurry was treated in a high-pressure homogenizer. This was repeated four times under 40 MPa conditions, and the solvent was then filtered off using a plate and frame filter. The resulting filter residue was vacuum dried, and the dried filter residue was pulverized and sieved through a 300 mesh screen to obtain a composite oil-control material.

[0044] The results of observing the material obtained in Example 8 with a scanning electron microscope are shown in Figure 1. Figure 1 is a scanning electron microscope photograph of the material prepared in Example 8 of the present invention. As can be seen from Figure 1, the material prepared in this example of the present invention is in a uniform state overall, with a relatively flat surface and smoother corners, which is advantageous for improving the skin feel.

[0045] The results of a particle size distribution test on the material obtained in Example 8 are shown in Figure 2. Figure 2 is a particle size distribution diagram of the material prepared in Example 8 of the present invention. As can be seen from Figure 2, the median diameter D50 of the material prepared in this example of the present invention was 1 to 20 μm.

[0046] Comparative Example 1 The same preparation method as in Example 8 was employed, except that synthetic fluorphlogopite was not added to the composite material.

[0047] Comparative Example 2 The same manufacturing method as in Example 8 was used, except that hydroxyapatite was not added to the composite material.

[0048] Comparative Example 3 The same manufacturing method as in Example 8 was used, except that no zinc oxide was added to the composite material.

[0049] Comparative Example 4 0.02 parts of fullerene, 15 parts of hydroxyapatite, 5 parts of zinc oxide, and 80 parts of synthetic fluorphlogopite were mixed by physical stirring.

[0050] The results of observing the material obtained in Comparative Example 4 under a scanning electron microscope are shown in Figure 3. Figure 3 is a scanning electron microscope photograph of the material prepared in Comparative Example 4 of the present invention. As can be seen from Figure 3, the directly physically mixed material appeared to have each component separated under the electron microscope.

[0051] Experimental Example 1 Simple artificial sebum was prepared by mixing oleic acid and water in a 2:1 ratio. 1.2 g of each of the composite oil-control materials prepared in Examples 1 to 8 and the samples prepared in Comparative Examples 1 to 4 was placed in a 50 ml beaker, and 7.2 g of artificial sebum was added. After uniform stirring, the beaker was tilted to observe the fluidity, the solidification time was calculated, and the sebum coagulation ability of the material was observed. The results are shown in Table 1. Table 1 shows the test results for the oil adsorption capacity and sebum coagulation ability of the materials provided in the examples and comparative examples of the present invention.

[0052] Experimental Example 2 Oleic acid and silicone oil are oils secreted from the skin and oils commonly used in makeup base formulations, respectively. 5 g of the composite oil-control materials prepared in Examples 1-8 and 5 g of the samples prepared in Comparative Examples 1-4 were uniformly mixed with 50 g of oleic acid and 50 g of silicone oil (10 cst), respectively, and left at room temperature for 18 hours. Then, 100 mL of petroleum ether was added and stirred for 30 minutes. The mixture was filtered and the residue was washed. This washing process was repeated three times. After the petroleum ether was completely evaporated, 1 g of the residue was weighed into a crucible and placed in a muffle furnace and baked at 500°C ± 25°C for 2 hours. The crucible was then removed and placed on an asbestos plate outside the furnace. After cooling for 3 minutes, it was transferred to a dryer and cooled to room temperature. The result was then weighed on a precision balance. The above procedure was repeated until the mass difference between two consecutive weighings was less than 0.4 mg (the baking time from the second time onwards was 30 minutes). The oil adsorption amount was calculated from the weight loss. The results are shown in Table 1. Table 1 shows the test results of the oil adsorption capacity and sebum aggregation ability of the materials provided in the examples and comparative examples of the present invention.

[0053] [Table 1]

[0054] Experimental Example 3: Dispersion stability test of composite oil control material in water 1.25 g of each of the materials from Comparative Example 4 and Example 7 was weighed into a 100 mL volumetric flask, 35 g of deionized water was added, the mixture was shaken well, ultrasonicated for 30 minutes, and allowed to stand for 2 hours. The results of observing the solution are shown in Figures 4 and 5. Figure 4 is a photograph of the dispersion stability in water of the material prepared in Example 7 of the present invention. Figure 5 is a photograph of the dispersion stability in water of the material prepared in Comparative Example 4 of the present invention.

[0055] Pure fullerene powder is black, and when the fullerenes are well dispersed, they appear pale yellow. As can be seen from Figures 4 and 5, black particles precipitated at the bottom of the flask after ultrasonic treatment of the directly physically mixed materials. When these black particles were sampled and examined, they were confirmed to be fullerenes. In contrast, the composite material prepared in Example 7 remained homogeneous even after ultrasonic treatment, demonstrating the good stability of the composite material prepared in the present invention.

[0056] Experimental Example 4: Raman spectroscopic detection experiment of composite oil control material The samples of Comparative Example 4 and Example 8, Raw Material 1 (fullerene), and Raw Material 2 (mixed hydroxyapatite, zinc oxide, and synthetic fluorphlogopite) were each placed on a solid substrate. The sample surface was covered with a clean, flat sheet and gently pressed to flatten the experimental surface. Raman spectroscopy was performed, and the results are shown in Figure 6. Figure 6 shows the Raman spectra of the materials prepared in the examples of the present invention and the comparative examples. However, the composite oil-control material was the material prepared in Example 8, and the physically mixed raw material was the material prepared in Comparative Example 4. As can be seen from Figure 6, the composite oil-control material prepared in the examples of the present invention possesses the characteristic signals of both Raw Material 1 and Raw Material 2, indicating that the original structure of the materials was unchanged after mixing. However, compared to the direct physical mixture, the Raman peaks of the composite oil-control material were significantly different, demonstrating that the composite oil-control material is not simply mixed, but is combined with a certain interaction.

[0057] Experimental Example 5 Antioxidant performance test of composite oil control material (1) Free Radical Quenching Test: Samples obtained in Comparative Example 4 and Example 8 were collected and subjected to electron paramagnetic resonance (EPR) analysis to detect the free radical quenching activity of the materials. 5.5 μl of DMPO mother solution was added to 250 μl of ultrapure water to prepare a DMPO solution. 20 mg of each sample obtained in Comparative Example 4 and Example 8 was weighed, added to 1000 μl of ultrapure water, and ultrasonically dispersed. Immediately, 25 μl of the sample was transferred and uniformly mixed with 25 μl of HO (100 mM), followed by the addition of 10 μl of DPMO solution. The solution was first irradiated with 500 W UV light for 4 minutes, and then X-band EPR spectra were recorded in the dark. The results are shown in Figure 7. Figure 7 shows the free radical quenching test results for the materials provided in the examples and comparative examples of the present invention. As can be seen from Figure 7, the material prepared in Comparative Example 4 had almost no free radical quenching activity and exhibited weak antioxidant performance. This is because the antioxidant properties of fullerenes are related to their dispersibility, and when the materials are directly mixed physically, the fullerenes are not sufficiently dispersed. In contrast, in the composite material prepared in Example 8, the fullerenes were uniformly attached to the material surface, and the antioxidant properties were fully exhibited.

[0058] (2) Anti-oxidation test for oils and fats: The material prepared in Example 8 was added to oleic acid at a ratio of 1.25%, and then irradiated under a UV lamp for 7 days to promote the oxidation of oleic acid. After centrifugation, the supernatant was collected and the peroxide value was measured. The results are shown in Table 2. Table 2 shows the test results for the anti-oxidation ability of the composite materials provided in the examples of the present invention.

[0059] [Table 2]

[0060] Experimental Example 6: Cell protection experiment of composite oil control material 5 mg of the material prepared in Example 8 and 5 mg of the material prepared in Comparative Example 4 were weighed out, and 1 mL of medium containing 10% FBS was added to each, mixed well, and then left in a constant temperature incubator at 37°C for 24 hours, after which the material was filtered to obtain sample leachates.

[0061] Prepare a cell suspension of logarithmically growing cells at an appropriate concentration using DMEM colorless cell culture medium containing 10% fetal bovine serum, with 5 × 10 cells per well. 4 Cells (100 μl) were added to a 96-well cell culture plate and cultured overnight. For the experiment, the cells were divided into three groups: a blank group, an Example 8 group, and a Comparative Example 4 group. 40 mg of sample leachate was added to each of the Example 8 group and the Comparative Example 4 group, and the blank group served as a control. When the cells reached 80% confluence, the sample leachate was added and the cells were cultured in an incubator for 24 hours. A CCK8 test was performed on the HACAT cells of each group, and the absorbance of the HACAT cells at 450 nm was detected using a microplate reader to obtain the proliferation activity of the HACAT cells of each group, and the data was used for analysis. The results are shown in TIFF0007747876000003.tif9170. Cell viability was calculated as follows: cell viability = value of treatment group / OD value of blank group × 100%. The results are shown in Figure 8. Figure 8 shows the cell viability test results for the materials provided in the examples and comparative examples of the present invention. As can be seen from Figure 8, the cell viability of the composite oil-control material prepared in Example 8 was 99.2%, while the cell viability of the sample group of Comparative Example 4 was only 20.94%, demonstrating that the composite oil-control material prepared in this invention has the effect of protecting cells.

[0062] Experimental Example 7: Oil and fat selective adsorption test of composite oil control material Approximately 0.11 g of different types of oils were weighed and dissolved in 110 mL of n-hexane, then mixed uniformly. Approximately 0.5 g of the composite material prepared in Example 8 was weighed into an Erlenmeyer flask, 50 mL of n-hexane containing oil was added, the flask was sealed with a lid, shaken for 1 hour, filtered, and analyzed by GCMS. The content was calculated using the external standard method. A calibration curve was created using n-hexane containing oil at 100%, 20%, 10%, 1%, and 0.1% contents, and the results are shown in Table 3. Table 3 shows the adsorption results of the materials provided in the examples of the present invention to oils.

[0063] [Table 3]

[0064] As can be seen from Table 3, the composite oil-control material prepared in the example of the present invention had the highest adsorption rate for oleic acid (an oil component secreted by the skin), and among the oils commonly used in makeup base formulations, it had low adsorption for silicone oil and isooctyl palmitate (2-EHP), and almost no adsorption for mineral oil, squalane, and glyceryl caprate (GTCC), proving that this composite material has selective adsorption function.

[0065] Example 8 A liquid foundation was prepared according to the formulation shown in Table 4.

[0066] [Table 4]

[0067] Among them, gardenia fruit extract was purchased from Sensient Technologies Corp (China) Ltd. and had the product code GB618.

[0068] The preparation procedure includes the following steps: 1. Add emulsifier, colorant, film-forming agent, skin moisturizer, skin feel adjuster, and thickener to a beaker in that order, stir, heat to 80°C, homogenize for 10 minutes, and keep warm for 10 minutes to obtain Phase A material. 2. The moisturizer, inorganic salt, composite oil-control material composition, preservative, and water were added to a beaker in this order, stirred, heated to 80°C, and kept at this temperature for 10 minutes to obtain a B-phase material. 3. The B phase material was slowly added to the A phase material and homogenized for 10 minutes, stirred and cooled to 35°C to obtain the liquid foundation.

[0069] A simple artificial sebum was prepared by mixing olive oil, oleic acid, and squalane in a ratio of 2:2:1. 4 g of liquid foundation was taken, 0.4 g of artificial sebum was added, and the mixture was stirred uniformly. The mixture was placed on a glass plate and applied to a 90 μm film using a film applicator. The color of the foundation film was measured using a colorimeter, and the foundation film was left at room temperature for 12 hours, after which the color of the foundation film was measured again. The color difference values ​​were calculated and the results are shown in Table 5. Table 5 shows the color difference values ​​of the liquid foundation provided by the present invention.

[0070] [Table 5]

[0071] As can be seen from Table 5, the liquid foundation containing the composite oil-control material composition had the smallest color difference value ΔE after 12 hours of application, indicating that the liquid foundation had the least discoloration and the best ability to prevent dullness.

[0072] The above description is merely a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto, and any equivalent substitutions or modifications made by those skilled in the art based on the technology and inventive concept of the present invention within the technical scope disclosed in the present invention should all be included in the protection scope of the present invention.

Claims

1. a step of uniformly mixing 30 to 90 parts by mass of at least one base material selected from the group consisting of synthetic fluorphlogopite, silica, alumina, and organosilicon powder, 0.0001 to 6 parts by mass of fullerene, 1 to 50 parts by mass of hydroxyapatite, 0.1 to 30 parts by mass of zinc oxide, and 1,000 to 5,000 parts by mass of water to obtain a mixture; and subjecting the mixture to high-pressure homogenization, filtration, drying and pulverization in sequence to obtain an oil-control composite material.

2. The method according to claim 1, wherein the mixture is subjected to high-pressure homogenization at a pressure of 30 to 50 MPa for 1 to 8 times.

3. The method according to claim 1, characterized in that, before the high-pressure homogenization, the mixture is pre-homogenized at a rotation speed of 800-1500 r / min for 30-90 minutes.

4. The manufacturing method described in claim 1, characterized in that the oil control composite material has a median diameter D50 in the range of 1 to 20 μm.

5. A method for producing a cosmetic composition, comprising mixing the oil-control composite material obtained by the production method according to any one of claims 1 to 4 and gardenia fruit extract in a mass ratio of 90-99:0.1-10.

6. 6. The method for producing a cosmetic composition according to claim 5, wherein the cosmetic composition is selected from the group consisting of loose powder, powder cake, liquid foundation, cream foundation, BB cream, isolation cream, skin repair cream, paste concealer, liquid concealer, contouring powder cake, highlighting powder cake, and CC cream.

Citation Information

Patent Citations

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