WO2023173671A1 - Oil-control composite material and preparation method therefor, and cosmetic - Google Patents

Abstract

The present invention provides an oil-control composite material, obtained by performing high-pressure homogenization on a mixture. The mixture comprises: 0.0001-6 parts by mass of fullerene; 1-50 parts by mass of hydroxyapatite; 0.1-30 parts by mass of zinc oxide; and 30-90 parts by mass of a base material, the base material being selected from at least one of synthetic fluorphlogopite, silica, aluminum oxide, and silicone powder. The present invention also provides a preparation method for the oil-control composite material. The present invention further provides a cosmetic. The oil-control composite material provided by the present invention has the functions of selectively adsorbing sebum, flocculating sebum, and preventing sebum oxidation, and a closed loop from selective adsorption of sebum to flocculation of sebum and to prevention of sebum oxidation can be formed, thereby completely solving the influence of sebum on makeup. In addition, the oil-control composite material provided by the present application further has low cytotoxicity and has the effect of reducing ultraviolet transmittance and the like.

Description

Oil control composite material, preparation method thereof and cosmetics

This application claims priority to the Chinese patent application filed with the China Patent Office on March 14, 2022, with the application number 202210246508.4 and the invention title "An oil-control composite material, its preparation method and cosmetics", the entire content of which is incorporated by reference. in this application.

Technical field

The invention relates to the technical field of daily cosmetics, specifically an oil-controlling composite material, its preparation method and cosmetics.

Background technique

When the oil secretion of facial skin is strong, even the most delicate makeup will become greasy and dirty. Therefore, oil control is one of the core issues that base makeup products need to solve. Most of the common oil-controlling powders on the market are mesoporous materials, which are not selective in the adsorption of various types of oils and are prone to excessive oil control. Excessive oil control will lead to difficulty in applying base makeup, inconsistent application, makeup sticking, and a drying feeling. A series of questions.

Hydroxyapatite has good biological activity and biocompatibility, and has been widely studied in biology and medicine. Bone and teeth are typical biomineralized tissues, and their inorganic components are hydroxyapatite. Hydroxyapatite is a hexagonal crystal system, and its microcrystalline surface has several possible surface states: (1) When OH is located on the crystal surface, OH is connected to two Ca(Ⅱ) ions, and the OH position on this surface is at least in a certain Momentarily vacant, because the two Ca(II) ions are positively charged, a positively charged adsorption site is formed, which can adsorb PO ₄ ^3- or phosphate groups or carboxyl groups on macromolecules. (2) When Ca ions are located on the surface of the crystal, since Ca(Ⅰ) is connected to 6 negatively charged O atoms, when the Ca(Ⅰ) position on the surface is vacant at a certain moment, it will be formed at the Ca(Ⅰ) position. The stronger adsorption site can adsorb cations such as Sr ³⁺ and K ⁺ and groups of protein molecules, while a weaker adsorption site is formed at the Ca(II) position. Hydroxyapatite has certain selective adsorption properties due to its crystal surface structure characteristics.

Patent CN112741775A provides a composite mica powder for cosmetics with oil-controlling properties and a preparation method thereof. Zinc oxide and hydroxyapatite are used to coat the surface of cosmetic-grade mica powder. It has a certain directional oil absorption effect, but the material is harmful to the face. The oil secreted by the skin has poor adsorption effect.

Contents of the invention

In view of this, the object of the present invention is to provide an oil-controlling composite material, its preparation method and cosmetics. The oil-controlling composite material provided by the present invention has the functions of selectively adsorbing sebum, flocculating sebum, and preventing sebum oxidation, and has the effect of preventing sebum oxidation. Strong adsorption capacity.

The invention provides an oil-control composite material, which is obtained by high-pressure homogenization of a mixture;

The mixture includes:

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 base material;

The base material is selected from at least one selected from the group consisting of synthetic fluorphlogopite, silica, alumina and organic silicon powder.

The invention uses fullerene, hydroxyapatite, zinc oxide and at least one substrate selected from the group consisting of synthetic fluorphlogopite, silica, alumina and organic silicon powder as raw materials, and homogenizes the fullerene through high pressure. , hydroxyapatite and zinc oxide are embedded on the base material to obtain a composite material that is more uniform, has a relatively smooth surface and smoother corners, thus improving the oil control effect of the composite material.

The mixture provided by the invention includes fullerene, a large π bond conjugated system composed of multiple P orbitals of fullerene, which makes it have a strong ability to accept electrons. Because of its unique structure and physical and chemical properties, it has It has excellent free radical scavenging properties and is called a "free radical sponge". It also shows excellent antioxidant properties and has received widespread attention in cosmetic materials, biomedicine and other aspects. In this application, fullerene is compounded on the base material, thereby increasing the dispersion degree of fullerene, thereby improving the performance of the obtained composite material. In one embodiment, the amount of fullerene is 0.0001 to 6 parts by mass. In one embodiment, the amount of fullerene is 0.001 to 4 parts by mass. In one embodiment, the amount of fullerene is 0.01 to 2 parts by mass.

The mixture provided by the present invention includes hydroxyapatite, and hydroxyapatite has certain selective adsorption properties for oils due to its crystal surface structure characteristics. In one embodiment, the amount of hydroxyapatite is 1 to 50 parts by mass. In one embodiment, the amount of hydroxyapatite is 5 to 40 parts by mass. In one embodiment, the amount of hydroxyapatite is 10 to 30 parts by mass.

The mixture provided by the invention includes zinc oxide, which has astringent and drying functions. In one embodiment, the amount of zinc oxide is 0.1 to 30 parts by mass. In one embodiment, the amount of zinc oxide is 1 to 20 parts by mass. In one embodiment, the amount of zinc oxide is 5 to 15 parts by mass.

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

In one embodiment, the mixture includes:

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;

45 to 85 parts by mass of base material.

In one embodiment, the mixture includes:

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;

50 to 80 parts by mass of base material.

In the present invention, the oil control composite material is obtained by high-pressure homogenization of the above mixture. In one embodiment, the particle size of the oil control composite material is less than 300 mesh.

The oil-controlling composite material provided by the present invention has the function of selectively adsorbing sebum, flocculating sebum, and preventing sebum oxidation, forming a closed loop, thereby completely solving the impact of sebum on makeup, and can be widely used in oil-control cosmetics.

The invention also provides a method for preparing oil control composite materials, which includes the following steps:

Mix 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 the base material and 1000 to 5000 parts by mass of water. Obtain a mixture; wherein, the substrate is selected from at least one of synthetic fluorphlogopite, silica, alumina and organic silicon powder;

The mixture is sequentially subjected to high-pressure homogenization, filtration, drying and pulverization to obtain an oil-control composite material.

In the present invention, the above mixture is firstly mixed with water to form a mixture. In one embodiment, the above raw materials are mixed evenly with water under stirring conditions. In one embodiment, the stirring speed is 50 to 100 r/min.

In one embodiment, before performing high-pressure homogenization, the mixture is also pre-homogenized. In one embodiment, the pre-homogenization is performed under stirring. In one embodiment, the rotation speed of the pre-homogenization is 800-1500 r/min, and the time is 30-90 minutes.

After pre-homogenization, the resulting mixture is subjected to high-pressure homogenization in a high-pressure homogenizer. During the high-pressure homogenization process, the material is subjected to mechanical forces such as high-speed shearing, high-frequency oscillation, cavitation, and convection impact, which induce changes in the physical, chemical, and structural properties of the material, thereby making multiple materials fit together. Combine the ingredients into a whole.

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.

After the high-pressure homogenization is completed, the obtained mixed material is filtered, dried, pulverized, and sieved in order to obtain the oil-controlling composite material. Specifically, a plate and frame filter is first used to filter the solvent, and then the filter residue is vacuum-dried. The dried filter residue is crushed and passed through a sieve of less than 300 mesh to obtain a composite oil control material.

The oil-control composite material provided by the invention forms a closed loop from selectively adsorbing sebum to flocculating sebum, and then preventing sebum oxidation, thereby completely solving the impact of sebum on makeup. In addition, the oil-control composite material provided by this application also has the effects of lower cytotoxicity and lowering ultraviolet transmittance.

The present invention also provides a cosmetic composition, including the oil control composite material and gardenia fruit extract described in the above technical solution;

The mass ratio of the oil control composite material and the gardenia fruit extract is 90-99:0.1-10.

The gardenia fruit extract in the present invention refers to the blue powder obtained by refining and drying the gardenia fruit after hydrolysis. It has an antioxidant effect, can reduce the oxidation and dullness of oil, and has the effect of correcting yellow color. It is combined with the composite oil control material. Used in combination, it can effectively reduce the dullness of foundation makeup.

The gardenia fruit extract used in the present invention can be prepared according to the following process:

Crush the gardenia fruit, add ethanol-water solution for extraction, dry under reduced pressure to remove the ethanol, and obtain gardenia fruit pulp;

Carry out enzymatic hydrolysis of gardenia fruit pulp and filter;

Add amino acids to the filtrate to react;

The reaction mixture was purified using macroporous resin, then concentrated and dried to obtain gardenia fruit extract.

The extraction technology of the gardenia fruit extract of the present invention is mature at home and abroad and has been commercialized.

In one embodiment of the present invention, the selected gardenia fruit extract was purchased from Sensient Technologies Corp (China) Ltd., and the product code is GB618. After testing, 0.0125% gardenia fruit extract has an The DPPH free radical scavenging rate is 66.2%.

The present invention also provides a cosmetic, including the oil control composite material described in the above technical solution and the cosmetic composition described in the above technical solution.

The oil-control composite material provided by the invention can be used to prepare oil-control cosmetics, including but not limited to loose powder, powder cake, liquid foundation, foundation cream, BB cream, isolation cream, repair cream, concealer, concealer liquid, contour powder cake, and highlight powder cake. Or CC cream, etc.

The oil-controlling composite material provided by the invention can be used together with gardenia fruit extract to prepare cosmetics, has good antioxidant properties, and can reduce the dullness of base makeup.

In addition to the oil-controlling composite material, the above-mentioned cosmetics may also include other ingredients. Those skilled in the art can determine the types and dosages of other ingredients according to the functional needs of the cosmetics. This application will not repeat them here.

The present invention uses fullerene, hydroxyapatite, zinc oxide and at least one base material selected from synthetic fluorphlogopite, silica, alumina and organic silicon powder as raw materials. After high-pressure homogenization treatment, it will be processed under high-pressure During the homogenization process, the material is subjected to mechanical forces such as high-speed shearing, high-frequency oscillation, cavitation, and convection impact, which induce changes in the physical, chemical, and structural properties of the material, thereby causing multiple materials to fit together and making the raw materials Combined into a whole, a composite material is obtained that is more uniform, has a relatively smooth surface, and has smoother corners. The oil-control composite material provided by the invention has the functions of selectively adsorbing sebum, flocculating sebum and preventing sebum oxidation. It can form a closed loop from selectively adsorbing sebum to flocculating sebum and then preventing sebum oxidation, thereby completely solving the impact of sebum on makeup. . In addition, the oil-control composite material provided by this application also has the effects of lower cytotoxicity and lowering ultraviolet transmittance.

Description of the drawings

Figure 1 is a scanning electron microscope photograph of the material prepared in Example 8 of the present invention;

Figure 2 is a particle size distribution diagram of the material prepared in Example 8 of the present invention;

Figure 3 is a scanning electron microscope photo of the material prepared in Comparative Example 4 of the present invention;

Figure 4 is a photo of the dispersion stability of the material prepared in Example 7 of the present invention in water;

Figure 5 is a photo of the dispersion stability of the material prepared in Comparative Example 4 of the present invention in water;

Figure 6 is a Raman spectrum chart of the materials prepared according to the embodiments and comparative examples of the present invention;

Figure 7 is the free radical quenching test results of the materials provided by the embodiments and comparative examples of the present invention;

Figure 8 shows the test results of the cell viability of the materials provided in the embodiments and comparative examples of the present invention.

Detailed ways

The oil control composite material, its preparation method and cosmetics provided by the present invention will be described in detail below with reference to the examples.

Example 1

Mix 0.0001 parts of fullerene, 1 part of hydroxyapatite, 30 parts of zinc oxide, 50 parts of flaky alumina, and 3000 parts of deionized water, stir evenly at 60r/min, and then homogenize at 1000r/min. 60min, process the obtained slurry with a high-pressure homogenizer, repeat the process 4 times under 40MPa conditions, then use a plate and frame filter to filter out the solvent, vacuum dry the obtained filter residue, crush the dried filter residue, and screen it with 300 mesh Process to obtain composite oil control materials. The median particle size D50 of the composite oil control material is between 1 and 20 μm.

Example 2

Take 6 parts of fullerene, 50 parts of hydroxyapatite, 0.1 part of zinc oxide, 90 parts of synthetic fluorphlogopite, and 3000 parts of deionized water, mix them evenly at 60r/min, and then homogenize at 1000r/min. 60min, process the obtained slurry with a high-pressure homogenizer, repeat the process 4 times under 40MPa conditions, then use a plate and frame filter to filter out the solvent, vacuum dry the obtained filter residue, crush the dried filter residue, and screen it with 300 mesh Process to obtain composite oil control materials.

Example 3

Mix 0.001 parts of fullerene, 5 parts of hydroxyapatite, 20 parts of zinc oxide, 65 parts of organic silicon powder, and 3000 parts of deionized water, stir evenly at 60r/min, and then homogenize for 60min at 1000r/min. , the obtained slurry is treated with a high-pressure homogenizer, and the treatment is repeated 4 times under 40MPa conditions, and then a plate and frame filter is used to filter out the solvent, and the obtained filter residue is vacuum dried. The dried filter residue is crushed and screened with 300 mesh. , to obtain composite oil control materials.

Example 4

Mix 4 parts of fullerene, 40 parts of hydroxyapatite, 1 part of zinc oxide, 90 parts of silica, and 3000 parts of deionized water, stir evenly at 60r/min, and then homogenize at 1000r/min for 60 minutes. The obtained slurry is treated with a high-pressure homogenizer, and the treatment is repeated 4 times under 40MPa conditions, and then a plate and frame filter is used to filter out the solvent. The obtained filter residue is vacuum-dried, and the dried filter residue is crushed and screened with 300 mesh to obtain Composite oil control material.

Example 5

Take 0.01 parts of fullerene, 10 parts of hydroxyapatite, 1 part of zinc oxide, 40 parts of silica, 30 parts of alumina, and 3000 parts of deionized water, mix them, stir them evenly at 60r/min, and then mix them evenly at 1000r/min. Quality treatment for 60 minutes, the obtained slurry is treated with a high-pressure homogenizer, and the treatment is repeated 4 times under 40MPa conditions, and then a plate and frame filter is used to filter out the solvent, and the obtained filter residue is vacuum dried, and the dried filter residue is crushed into 300 mesh. After sieving, the composite oil control material is obtained.

Example 6

Take 2 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, mix them, stir evenly at 60r/min, and then stir at 1000r/min Rotate and homogenize for 60 minutes. Use a high-pressure homogenizer to process the obtained slurry. Repeat the treatment 4 times under 40MPa conditions. Then use a plate and frame filter to filter out the solvent. The resulting filter residue is vacuum dried and the dried filter residue is crushed. After 300 mesh sieving, a composite oil control material is obtained.

Example 7

Take 1 part of fullerene, 20 parts of hydroxyapatite, 5 parts of zinc oxide, 77.5 parts of synthetic fluorphlogopite, and 3000 parts of deionized water, mix them, stir evenly at 60r/min, and then homogenize at 1000r/min. 60min, process the obtained slurry with a high-pressure homogenizer, repeat the process 4 times under 40MPa conditions, then use a plate and frame filter to filter out the solvent, vacuum dry the obtained filter residue, crush the dried filter residue, and screen it with 300 mesh Process to obtain composite oil control materials.

Example 8

Take 0.02 parts of fullerene, 15 parts of hydroxyapatite, 5 parts of zinc oxide, 80 parts of synthetic fluorophlogopite, and 3000 parts of deionized water, mix them, stir evenly at 60r/min, and then homogenize at 1000r/min. 60min, process the obtained slurry with a high-pressure homogenizer, repeat the process 4 times under 40MPa conditions, then use a plate and frame filter to filter out the solvent, vacuum dry the obtained filter residue, crush the dried filter residue, and screen it with 300 mesh Process to obtain composite oil control materials.

The material obtained in Example 8 was observed under a scanning electron microscope. The results are shown in Figure 1. Figure 1 is a scanning electron microscope photograph of the material prepared in Example 8 of the present invention. It can be seen from Figure 1 that the material prepared by the embodiment of the present invention is in a uniform overall state, with a relatively flat surface and smoother corners, which improves skin feel.

The material obtained in Example 8 was subjected to a particle size distribution test. The results are shown in Figure 2. Figure 2 is a particle size distribution diagram of the material prepared in Example 8 of the present invention. It can be seen from Figure 2 that the median particle size D50 of the material prepared in the embodiment of the present invention is between 1 and 20 μm.

Comparative example 1

The preparation method is the same as in Example 8, except that synthetic fluorphlogopite is not added to the composite material.

Comparative example 2

The preparation method is the same as in Example 8, except that hydroxyapatite is not added to the composite material.

Comparative example 3

The preparation method is the same as in Example 8, except that zinc oxide is not added to the composite material.

Comparative example 4

Physically stir and mix 0.02 parts of fullerene, 15 parts of hydroxyapatite, 5 parts of zinc oxide, and 80 parts of synthetic fluorphlogopite.

The material obtained in Comparative Example 4 was observed under a scanning electron microscope, and the results 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 components of directly physically mixed materials appear separated under an electron microscope.

Experimental example 1

Mix oleic acid and water in a ratio of 2:1 to create a simple artificial sebum. Take 1.2g of the composite oil control materials prepared in Examples 1 to 8 and the samples prepared in Comparative Examples 1 to 4 and put them into 50ml beakers respectively. Add 7.2g of artificial sebum. After stirring evenly, tilt the beaker to observe its fluidity and calculate its The coagulation time was used to observe the sebum flocculation ability of the material. The results are shown in Table 1. Table 1 is the test results of the material's oil adsorption capacity and sebum flocculation ability provided by the embodiments and comparative examples of the present invention.

Experimental example 2

Oleic acid and silicone oil are oils secreted by the skin and commonly used oils in base makeup formulas respectively. Take 5g of the composite oil control materials prepared in Examples 1 to 8 and the samples prepared in Comparative Examples 1 to 4, respectively, with 50g of oleic acid and 50g of silicone oil. (10cst) mix well and leave at room temperature for 18 hours. Then add 100 mL of petroleum ether and stir for 30 minutes, filter and clean the filter residue, and repeat cleaning three times. After waiting for the petroleum ether to completely evaporate, weigh 1g of the residue into the crucible, put it into the muffle furnace, and burn it at 500℃±25℃ for 2 hours. Then take the crucible out and place it on the asbestos board outside the furnace to cool for 3 minutes before moving it to In the desiccator, cool to room temperature and weigh on a precision balance. Repeat this operation (the second and subsequent burning times are 30 minutes) until the mass difference between two consecutive times is less than 0.4 mg. Obtain the oil from the reduced weight. For the adsorption capacity, please refer to Table 1 for the results. Table 1 is the test results of the grease adsorption capacity and sebum flocculation ability of the materials provided by the embodiments and comparative examples of the present invention.

Table 1 Test results of material oil adsorption capacity and sebum flocculation ability

Experimental Example 3 Dispersion Stability Test of Composite Oil Control Material in Water

Weigh 1.25g of the materials of Comparative Example 4 and Example 7 respectively into a 100mL volumetric flask, add 35g of deionized water, shake well, ultrasonic for 30min, let stand for 2h, observe the solution, the results are shown in Figure 4 and Figure 5, Figure 4 Figure 5 is a photo of the dispersion stability of the material prepared in Example 7 of the present invention in water. Figure 5 is a photo of the dispersion stability of the material prepared in Comparative Example 4 of the present invention.

Pure fullerene powder is black, and appears light yellow when the fullerene is well dispersed. From Figure 4 and Figure 5, it can be found that after ultrasonic treatment of directly physically mixed materials, black particles precipitate at the bottom of the bottle. Take the black particles Testing of the substance confirmed that the black particles were fullerenes. However, the composite material prepared in Example 7 still appears in a uniform state after ultrasonic treatment, indicating that the composite material prepared by the present invention has good stability.

Experimental Example 4 Raman Spectroscopy Detection Experiment of Composite Oil Control Material

Take the samples of Comparative Example 4 and Example 8, Raw Material 1 (fullerene), and Raw Material 2 (a mixture of hydroxyapatite, zinc oxide, and synthetic fluorphlogopite) respectively on the solid substrate, and cover the surface of the sample with a layer Take a clean and flat sheet, press it gently to make the experimental surface smooth, and conduct Raman spectrum detection. The results are shown in Figure 6. Figure 6 is the Raman spectrum of the materials prepared in the embodiments and comparative examples of the present invention. Among them, the composite oil control material is The material prepared in Example 8, the raw materials were physically mixed into the material prepared in Comparative Example 4. It can be seen from Figure 6 that the composite oil control material prepared in the embodiment of the present invention has both the characteristic signal of raw material 1 and the characteristic signal of raw material 2, indicating that the original structure of the material has not been changed after compounding. However, compared with direct physical mixing, the Raman peaks of composite oil control materials are significantly different, proving that composite oil control materials are not simply mixed, but are combined with certain interactions.

Experimental Example 5 Antioxidation performance test of composite oil control materials

(1) Free radical quenching test: Take the samples prepared in Comparative Example 4 and Example 8, and detect the free radical quenching effect of the materials through electron paramagnetic resonance (EPR). Add 5.5ul of DMPO mother liquor to 250ul of ultrapure water to form a DMPO solution; weigh 20mg of the samples prepared in Ratio 4 and Example 8 respectively, add 1000ul of ultrapure water for ultrasonic dispersion, and immediately remove 25ul of the sample and 25ul of H2O2 (100mM), after mixing evenly, add 10ul of DPMO solution; first, irradiate the solution with 500W ultraviolet light for 4 minutes, and then record the X-band EPR spectrum in the dark. The results are shown in Figure 7, which shows the embodiments and comparative examples of the present invention. Free radical quenching test results for the materials provided. As can be seen from Figure 7, the material prepared in Comparative Example 4 has almost no quenching effect on free radicals. The antioxidant properties of fullerene are related to its dispersion. When the materials are directly physically mixed, the fullerene is not well dispersed. , so the antioxidant properties are weak. In the composite material prepared in Example 8, the fullerenes are uniformly attached to the surface of the material, and the antioxidant properties are fully effective.

(2) Anti-fat oxidation ability test: Add the material prepared in Example 8 to oleic acid at a ratio of 1.25%, place it under a UV lamp for 7 days to accelerate the oxidation of oleic acid, then centrifuge, and take the supernatant for testing For its peroxide value, please refer to Table 2 for the results. Table 2 is the test results of the anti-grease oxidation ability of the composite materials provided by the embodiments of the present invention.

Table 2 Test results of the anti-grease oxidation ability of composite materials provided by the embodiments of the present invention

Experimental Example 6 Cell Protection Experiment of Composite Oil Control Material

Weigh 5 mg of the material prepared in Example 8 and the material prepared in Comparative Example 4 respectively, add 1 mL of culture medium containing 10% FBS, mix well, place in a 37°C constant temperature incubator for 24 hours, and then filter to obtain a sample. Extract liquid.

For cells in the logarithmic growth phase, use DMEM colorless cell culture medium containing 10% fetal bovine serum to prepare a cell suspension of appropriate concentration, add 5ⅹ104 cells (100 μl) per well to a 96-well cell culture plate, and culture overnight. . The experiment was divided into 3 groups: blank group, Example 8 group and Comparative Example 4 group. 40 mg of sample extract was added to the Example 8 group and the Comparative Example 4 group respectively, and the blank group was used as a control. When the cells grow to 80% confluence, add the sample extract and culture in the incubator for 24 hours. Conduct CCK8 test on each group of HACAT cells. Detect the absorbance of HACAT cells at 450nm with a microplate reader to obtain the proliferation activity of each group of HACAT cells. For data

Represents; cell survival rate = dosing group value/blank group OD value × 100%. The results are shown in Figure 8. Figure 8 is the test results of the cell survival rate of the materials provided by the embodiments and comparative examples of the present invention. As can be seen from Figure 8, the cell survival rate of the composite oil control material group prepared in Example 8 is 99.2%, while the cell survival rate of the sample group of Comparative Example 4 is only 20.94%, proving that the composite oil control material prepared by the present invention has the effect of protecting cells.

Experimental Example 7 Composite oil control material grease selective adsorption test

Weigh about 0.11g of different types of fats, add 110mL of n-hexane to dissolve, and mix evenly. Weigh about 0.5g of the composite material prepared in Example 8 into an Erlenmeyer flask, add 50 mL of n-hexane containing oil, seal with a cap, shake for 1 hour, filter, analyze with GCMS, and calculate the content with the external standard method. The n-hexane content of the grease is 100%, 20%, 10%, 1% and 0.1% of the working curve. The results are shown in Table 3. Table 3 shows the adsorption results of the grease on the materials provided by the embodiments of the present invention.

Table 3 The adsorption results of grease on materials provided by the embodiments of the present invention

Grease type	Adsorption capacity(%)
Oleic acid	41.11
mineral oil	0
Silicone oil	2.84
Squalane	0
2-EHP	1.32
GTCC	0

It can be seen from Table 3 that the composite oil control material prepared in the embodiment of the present invention has the highest adsorption rate for oleic acid (the oil component secreted by the skin), and a small amount of adsorption of commonly used oils in base makeup formulas: silicone oil and isooctyl palmitate (2-EHP). There is almost no adsorption of mineral oil, squalane, and glyceryl caprylate (GTCC), which proves that the composite material has selective adsorption function.

Example 8

Prepare liquid foundation according to the formula shown in Table 4:

Table 4 The formula of liquid foundation provided in Example 8

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

The preparation steps include the following steps:

1. Add emulsifier, colorant, film-forming agent, emollient, skin texture regulator, and thickener into the beaker in sequence, stir and heat to 80°C, homogenize for 10 minutes, and keep warm for 10 minutes to obtain phase A material;

2. Add the humectant, inorganic salt, composite oil control material composition, preservative and water into the beaker in sequence, stir and heat to 80°C, and keep warm for 10 minutes to obtain phase B material;

3. Slowly add phase B material to phase A material and homogenize for 10 minutes, stir and cool down to

35℃, get liquid foundation

Configure olive oil: oleic acid: squalane into simple artificial sebum in a ratio of 2:2:1. Take 4g of liquid foundation and add 0.4g of artificial sebum. Stir evenly. Place it on a glass plate and apply it with an applicator. 90 μm film, use a colorimeter to measure the color of the foundation film, leave it at room temperature for 12 hours and test the color of the foundation film again, and calculate the color difference value. The results are shown in Table 5. Table 5 is the color difference value of the liquid foundation provided by the present invention.

Table 5 Color difference values of liquid foundation provided by the present invention

​	ΔL	Δa	Δb	ΔE
Experiment 1	-2.54	-0.20	-1.08	2.77
Experiment 2	-2.77	-0.19	-1.24	3.04
Experiment 3	-2.73	-0.61	-1.82	3.34
Experiment 4	-2.99	-0.73	-2.69	4.09

It can be seen from Table 5 that the color difference value ΔE of the liquid foundation added with the composite oil-control material composition is the smallest after 12 hours of application, indicating that the liquid foundation has the lightest discoloration and the best ability to resist dullness.

The above are only preferred specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any person familiar with the technical field can, within the technical scope disclosed in the present invention, implement the technical solutions of the present invention. Equivalent substitutions or changes of the inventive concept thereof shall be included in the protection scope of the present invention.

Claims (10)

1. An oil-control composite material is characterized in that it is obtained by high-pressure homogenization of a mixture;

   The mixture includes:

   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 base material;

   The base material is selected from at least one selected from the group consisting of synthetic fluorphlogopite, silica, alumina and organic silicon powder.
2. The oil control composite material according to claim 1, wherein the mixture includes:

   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;

   45 to 85 parts by mass of base material.
3. The oil control composite material according to claim 2, wherein the mixture includes:

   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;

   50 to 80 parts by mass of base material.
4. The oil control composite material according to any one of claims 1 to 3, characterized in that the particle size of the oil control composite material is 300 mesh or less.
5. A preparation method of oil control composite material, including the following steps:

   Mix 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, 30 to 90 parts by mass of the base material and 1000 to 5000 parts by mass of water. Obtain a mixture; wherein, the substrate is selected from at least one of synthetic fluorphlogopite, silica, alumina and organic silicon powder;

   The mixture is sequentially subjected to high-pressure homogenization, filtration, drying and pulverization to obtain an oil-control composite material.
6. The preparation method according to claim 5, characterized in that the mixture is subjected to high-pressure homogenization 1 to 8 times;

   The pressure of each high-pressure homogenization is 30~50MPa.
7. The preparation method according to claim 5, characterized in that the mixture is pre-homogenized before high-pressure homogenization, the rotation speed of the pre-homogenization is 800-1500 r/min, and the time is 30-90 min.
8. A cosmetic composition comprising the oil-controlling composite material according to any one of claims 1 to 4 and gardenia fruit extract;

   The mass ratio of the oil control composite material and the gardenia fruit extract is 90-99:0.1-10.
9. A cosmetic including the oil control composite material according to any one of claims 1 to 4 or the cosmetic composition according to claim 8.
10. The cosmetics according to claim 9, characterized in that the cosmetics are selected from the group consisting of loose powder, pressed powder, liquid foundation, foundation cream, BB cream, isolation cream, repair cream, concealer, liquid concealer, contouring powder, and high-gloss powder. Or CC cream.

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