CN114948762A

CN114948762A - Fullerene powder material and preparation method and application thereof

Info

Publication number: CN114948762A
Application number: CN202111681972.8A
Authority: CN
Inventors: 许哲; 李慧
Original assignee: Chifeng Funakang Biotechnology Co ltd; Beijing Fullcan Biotechnology Co ltd
Current assignee: Beijing Rensheng Zefa Biotechnology Co ltd; Chifeng Renze Cosmetics Co ltd; Suzhou Rensheng Zefa Biotechnology Co ltd
Priority date: 2021-12-31
Filing date: 2021-12-31
Publication date: 2022-08-30

Abstract

The disclosure relates to a fullerene powder material and a preparation method thereof, wherein the fullerene powder material comprises fullerene and a dispersing material, and the disclosure also relates to a cosmetic powder material or a cosmetic containing the fullerene powder material.

Description

Fullerene powder material and preparation method and application thereof

Technical Field

The disclosure relates to the technical field of material chemistry, in particular to a preparation method of a fullerene powder material, and a compounding method and application of the fullerene powder material and other raw materials.

Background

C60 fullerene was discovered by scientists Kroto, Smalley, Curl, et al in 1985 when studying carbon elements deep in space, and three people gained a Nobel prize for chemistry in 1996. Fullerene is an allotrope of carbon, as well as diamond and graphite. C60 is a spherical molecule consisting of 60 carbon atoms, consisting of 12 pentagons and 20 hexagons, each carbon atom and the adjacent three carbon atoms hybridized into bonds by SP2, and is called football since it resembles football.

The fullerene has strong electron accepting capacity due to a large pi bond conjugated system formed by a plurality of P orbitals, has excellent free radical scavenging performance due to unique structure and physicochemical properties, is called as free radical sponge, and simultaneously shows excellent oxidation resistance. So that it has attracted much attention in the fields of cosmetic materials, biomedicines, and the like.

By embedding C60 in the surfactant, C60 can eliminate reactive oxygen species in the cell, inhibit mitochondrial depolarization, activation of cysteine protease, exposure of phosphatidylserine on the cell membrane, and DNA division, and C60 exhibits the effect of protecting cells from oxidative apoptosis. The C60 liposome complex exerts an antioxidant effect by protecting the skin structure, nucleus and collagen fibers from UVA damage and penetration into human skin tissue, is several hundred times higher than vitamin C, and quenches free radicals. The fullerene is used as a nonpolar molecule, has a strong ultraviolet absorption effect, and can remove free radicals generated by the skin, thereby having the effects of resisting light damage, whitening and the like.

Professor withani withasa long engaged in the study of the properties of C60, as the first person to study fullerene dissolved in olive oil, they found that fullerene had a long life-prolonging health-care function by feeding mice 10-17 months once every two weeks (4 mg fullerene per kg body weight), the control group mice died 17-38 months, and the test group had prolonged life to 59-66 months. No abnormality exists in physiological performance regardless of body weight, and C60 is not found to be toxic or biogenetic, but C60 in a certain amount has the performance of scavenging free radicals, so that animals are protected from harm caused by excessive free radicals.

As external products, fullerene-related products such as C60-PVP have been reported in patents: 200480005008.1, 200580049615.2, due to the limitation of the preparation process and the compounding property of PVP and C60, the content of C60 in the compound is not more than 1%. 201810871219.7, when compounded with a polymer composition, it can hinder the performance of certain cosmetics after being coated on the surface of skin. C60-squalane, application No. 201510427642.4, but C60 has limited solubility in squalane, while squalane is an oil solution, making the use of this series of products limited.

In the preparation of fullerene composite materials, the existing commercial products can not fully exert the efficacy of the fullerene composite products, can not effectively combine the fullerene composite products, and are easy to phase-split.

Disclosure of Invention

In order to solve the problems in the prior art, an object of the present disclosure is to provide a fullerene powder material including fullerene and a dispersion material, and a method for preparing the same. The fullerene powder material is directly used as a raw material to be added and used in the using process without modification or optimization.

The present disclosure also aims to provide a cosmetic powder material containing the fullerene powder material of the present disclosure, and use thereof in preparing cosmetics.

In one aspect of the present disclosure, a fullerene powder material is provided, wherein the fullerene powder material comprises a fullerene and a dispersing material.

In one aspect of the disclosure, the fullerene is selected from C ₆₀ Fullerene, C ₇₀ One or more of a fullerene or a metallofullerene.

In one aspect of the present disclosure, the dispersed material comprises a mesoporous dispersed material.

In one aspect of the disclosure, the mass ratio of the fullerene to the dispersed material is 0.01% to 10%.

In another aspect of the disclosure, the mass ratio of the fullerene to the dispersed material is 0.01% to 5%.

In another aspect of the disclosure, the mass ratio of the fullerene to the dispersed material is 0.01% to 2%.

In one aspect of the disclosure, the dispersing material is selected from one or more of silica, titanium dioxide, talc, mica, sericite, kaolin.

In one aspect of the present disclosure, the dispersion material is selected from one or more of mesoporous silica, mesoporous titanium dioxide, talc, sericite.

In another aspect of the present disclosure, the silica is mesoporous silica.

In another aspect of the present disclosure, the titanium dioxide is mesoporous titanium dioxide.

In one aspect of the disclosure, the particle size of the fullerene powder material is 0.1 μm to 10 μm.

In another aspect of the disclosure, the fullerene powder material has a particle size of 0.5 μm to 5 μm.

A fullerene powder material for cosmetics, characterized by comprising a fullerene and silicon dioxide and/or titanium dioxide.

A fullerene powder material for cosmetics is characterized by comprising fullerene, and mesoporous silica and/or mesoporous titania.

In one aspect of the present disclosure, a method for preparing a fullerene powder material is provided, the method comprising the steps of preparing a dispersion material, and mixing the dispersion material with a fullerene solution.

In one aspect of the disclosure, a preparation method of a fullerene powder material is provided, and the preparation method comprises the following steps:

s1: preparing a dispersion material;

s2: mixing the dispersion material with a fullerene solution, and then stirring and centrifuging to obtain a precipitate and a supernatant;

s3: adding the fullerene solution into the supernatant again, and repeating the steps of stirring and centrifuging until the supernatant becomes colorless to obtain a precipitate;

s4: subjecting the precipitate obtained at S2 and the precipitate obtained at S3 to washing to obtain a total precipitate;

s5: and drying and dehydrating the total precipitate to obtain the fullerene powder material.

In a specific embodiment of the present disclosure, the dispersed material comprises a mesoporous dispersed material.

In a specific embodiment of the present disclosure, the dispersion material comprises mesoporous silica and/or mesoporous titania.

In one embodiment of the present disclosure, the mesoporous silica and/or mesoporous titania is prepared by a hydrothermal method.

In one particular embodiment of the present disclosure, the preparation method comprises the steps of:

s1: preparing mesoporous silicon dioxide and/or mesoporous titanium dioxide in equipment by a hydrothermal method;

s2: mixing the mesoporous silicon dioxide and/or mesoporous titanium dioxide with a fullerene solution, and stirring and centrifuging to obtain a precipitate and a supernatant;

In one aspect of the present disclosure, in step S1, the apparatus is selected from one or more of a glass reaction kettle or a stainless steel reaction kettle.

In one aspect of the present disclosure, in step S1, the temperature of the heating process of the hydrothermal method is selected from 10 ℃, 20 ℃, 40 ℃, 60 ℃, 80 ℃, 100 ℃, 120 ℃.

In another aspect of the present disclosure, in step S1, the temperature of the heating process of the hydrothermal method is 60 ℃.

In another aspect of the present disclosure, in step S1, the temperature of the heating process of the hydrothermal method is 120 ℃.

In one aspect of the present disclosure, in step S1, the heating process of the hydrothermal process is performed for a time selected from 1 hour, 2 hours, 4 hours, 5 hours, 6 hours.

In another aspect of the disclosure, in step S1, the heating process of the hydrothermal process has a time of 4 hours.

In another aspect of the present disclosure, in step S1, the heating process of the hydrothermal method is performed for a period of 5 hours.

In another aspect of the present disclosure, in step S2 and step S3, the stirring rate of the stirring process is selected from 500r/min, 750r/min, 1000r/min, 1500 r/min.

In another aspect of the present disclosure, in step S2 and step S3, the stirring rate of the stirring process is selected from 1000r/min to 1500 r/min;

in one aspect of the present disclosure, in steps S2 and S3, the centrifuged device is selected from one or more of a tube centrifuge, a plate filter, or a bench filter.

In one aspect of the present disclosure, in step S6, the drying device is selected from one or more of a rotary evaporator, a freeze dryer, a spray dryer, or a thin film evaporator.

In one aspect of the disclosure, a fullerene powder material is provided, which is characterized by being prepared by any one of the preparation methods.

In one aspect of the present disclosure, a powder material for cosmetics is provided, which is characterized by containing the fullerene powder material according to the present disclosure.

In one aspect of the disclosure, a cosmetic powder material is provided, which further comprises other cosmetic adjuvants.

In one aspect of the present disclosure, the cosmetic auxiliary material is selected from one or more of mica powder, titanium white powder, talc powder, sericite powder, silica.

In one aspect of the disclosure, the weight percentage of the fullerene powder material to the cosmetic auxiliary material is 1:200 to 1: 1.

In another aspect of the disclosure, the weight percentage of the fullerene powder material to the auxiliary material for cosmetics is 1:100 to 1: 5.

In one aspect of the disclosure, the disclosure provides the fullerene powder material and the use of the powder material for cosmetics in preparing cosmetics.

In another aspect of the disclosure, there is provided a use of any one of the fullerene powder materials described above in the preparation of a cosmetic.

In another aspect of the present disclosure, there is provided a use of any one of the aforementioned cosmetic powder materials in the preparation of a cosmetic.

In one aspect of the present disclosure, the cosmetic includes, but is not limited to, any of a solution, suspension, emulsion, ointment, gel, cream, emulsion, powder, soap, surfactant-containing cleanser, oil, powder foundation, emulsion, foundation, wax foundation, spray, liniment, paste, and poultice.

In another aspect of the present disclosure, the cosmetic includes, for example, loose powders, creams, multiple emulsions, anhydrous compositions, aqueous dispersions, oils, emulsions, balms, foams, lotions, gels, cream gels, hydroalcoholic solutions, hydroglycolic solutions, liniments, saline solutions, soaps, shampoos, conditioners, slurries, salves, mousses, ointments, powders, sticks, pencils, sprays, aerosols, capsules, gelatin capsules, tablets, powders, particulate forms, chewing gums, solutions, suspensions, emulsions, syrups, polysaccharide films, jellies, gelatins, ointments, creams, soft lotions, nutritional lotions, masks, essences, pilatory agents, shampoos, rinses, hair conditioners, skin lotions, skin softeners, skin lotions, astringents, emulsions, milk emulsions, lotions, creams, gels, lotions, creams, gels, lotions, creams, gels, lotions, gels, lotions, creams, gels, lotions, creams, gels, lotions, creams, gels, lotions, creams, gels, creams, lotions, creams, gels, lotions, gels, lotions, gels, creams, gels, lotions, creams, gels, lotions, gels, lotions, gels, lotions, creams, gels, creams, gels, creams, gels, lotions, creams, or the like, A nourishing lotion, a massage cream, a nourishing cream, a moisturizing cream, a hand cream, a foundation cream, a nourishing essence, a sun cream, a soap, a cleansing foam, a cleansing milk, a cleansing cream, a body lotion and a body cleanser, an under-eye pouch remover, a makeup foundation, a makeup remover lotion, an eye shadow, a lipstick, a lip gloss, and a lip powder.

In another aspect of the present disclosure, the effects of the cosmetic or toiletry product include, but are not limited to: whitening skin, improving pigmentation, treating acne, improving wrinkle, improving pachylosis, improving oily skin, improving dry skin, shrinking pore, treating scar, treating flush complexion, treating alopecia, promoting hair growth, treating burn, killing bacteria and mite, improving skin pit, and preventing acne and haze.

In one aspect of the disclosure, the materials of the present disclosure may also be used with other adjuvants including hyaluronic acid, greases, surfactants, preservatives, fragrances, binders, thickeners, complexing agents, PH adjusters.

In one aspect of the present disclosure, the materials of the present disclosure may be used with a surfactant selected from the group consisting of: at least one of anionic surfactant, cationic surfactant, amphoteric surfactant, lipophilic nonionic surfactant, hydrophilic nonionic surfactant, and natural surfactant.

Drawings

Fig. 1 is an Electron Paramagnetic Resonance (EPR) spectrum of the ability of the fullerene powder material to quench hydroxyl radicals of the present disclosure.

Fig. 2 is a photograph of the fullerene powder material after ultrasonic treatment.

FIG. 3 is a photograph of a conventional product (Veil Fullerene, Mitsubishi, Japan) after ultrasonic treatment.

FIG. 4 is an ultraviolet absorption spectrum of the fullerene powder material disclosed by the invention.

Fig. 5 is a photograph of the oxidation resistance of the fullerene powder material of the present disclosure.

Fig. 6 is a scanning electron microscope image of the fullerene powder material of the present disclosure.

Detailed Description

Based on the above disclosure, other modifications, substitutions and alterations can be made without departing from the basic technical concept of the present disclosure as it is known and customary in the art.

Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.

I. Detailed description of the preferred embodiments

In one embodiment, a fullerene soot material is provided, wherein the fullerene soot material comprises a fullerene and a dispersing material.

In one embodiment, wherein the fullerene is selected from C ₆₀ Fullerene, C ₇₀ One or more of a fullerene or a metallofullerene.

In one embodiment, the dispersed material comprises a mesoporous dispersed material.

In one embodiment, the mass ratio of the fullerene to the dispersed material is 0.01% to 10%.

In one embodiment, the mass ratio of the fullerene to the dispersed material is 0.01% to 5%.

In one embodiment, the mass ratio of the fullerene to the dispersed material is 0.01% to 2%.

In one embodiment, the dispersing material is selected from one or more of silica, titanium dioxide, talc, mica, sericite, kaolin.

In one aspect of the present disclosure, the dispersion material is selected from one or more of mesoporous silica, mesoporous titanium dioxide, talc, and sericite.

In one embodiment, the silica is mesoporous silica.

In one embodiment, the titanium dioxide is mesoporous titanium dioxide.

In one embodiment, the fullerene powder material has a particle size of 0.1 μm to 10 μm.

In one embodiment, the fullerene powder material has a particle size of 0.5 μm to 5 μm.

In one embodiment, the present disclosure provides a preparation method of a fullerene powder material, which includes controlling a process of reacting a mixed solution at different reaction temperatures.

In one embodiment, the reaction temperature of the mixture is 10 ℃, 20 ℃, 40 ℃, 60 ℃, 80 ℃, 100 ℃, 120 ℃, preferably 60 ℃ or 120 ℃.

In one embodiment, the reaction time of the mixed solution is 1 hour, 2 hours, 4 hours, 5 hours, 6 hours, preferably 4 hours or 5 hours.

In one embodiment, the mixed solution is reacted in a device such as a glass reaction vessel or a stainless steel reaction vessel.

In one embodiment, the present disclosure provides a preparation method of a fullerene powder material, which includes a process of subjecting a mixed solution to a plurality of high-speed centrifugation processes in an apparatus to obtain a mesoporous dispersion material precipitate.

In one embodiment, the present disclosure provides a preparation method of a fullerene powder material, the preparation method comprising a process of mixing the mesoporous dispersion material precipitate with a fullerene solution, and obtaining a precipitate and a supernatant through a centrifugal process after a stirring process.

In one embodiment, the present disclosure provides a preparation method of a fullerene powder material, including a process of adding the fullerene solution to the supernatant again, and performing a centrifugal process after a stirring process until the supernatant becomes colorless to obtain a precipitate.

In one embodiment, the stirring rate of the stirring process is 500r/min, 750r/min, 1000r/min, 1500 r/min; preferably 1000r/min to 1500 r/min.

In one embodiment, the present disclosure provides a method for preparing a fullerene powder material, the method comprising a process of washing the obtained precipitate with ethanol.

In one embodiment, the present disclosure provides a method for preparing a fullerene powder material, the method comprising drying the washed precipitate to obtain the fullerene powder material.

In one embodiment, the present disclosure provides a method for preparing a fullerene powder material, the method comprising the steps of:

s1: mixing a silicon-containing raw material, short-chain alcohol and water, heating to 60 ℃ in equipment, and simultaneously stirring at the stirring speed of 1000r/min for 4 hours until no precipitate is generated to obtain a mixed solution;

s2: obtaining a dispersion material by subjecting the mixed solution to multiple high-speed centrifugation processes in equipment;

s3: mixing the dispersion material with the fullerene solution, stirring at the stirring speed of 1000r/min for 2 hours, and centrifuging to obtain a precipitate and a supernatant;

s4: adding the fullerene solution into the supernatant again, stirring at the stirring speed of 1000r/min, and centrifuging until the supernatant becomes colorless to obtain a precipitate;

s5: washing the precipitate obtained at S3 and the precipitate obtained at S4 with ethanol;

s6: and drying the washed precipitate to obtain the titanium dioxide fullerene material.

In one embodiment, the present disclosure provides a preparation method of a fullerene powder material, the preparation method comprising a step of preparing mesoporous silica, preferably, the preparation method comprises a process of mixing silicon-containing raw materials such as n-silane ethyl ester, water and different short-chain alcohols to form a mixed solution.

In one embodiment, the short chain alcohol is selected from the group consisting of ethanol, butanediol, propanediol, isopropanol, n-hexane, pentanediol, preferably isopropanol.

s1: mixing a titanium-containing raw material and water, heating the mixture to 120 ℃ in equipment, reacting for 5 hours, and cooling to obtain a dispersed material;

s2: mixing the dispersion material with the fullerene solution, stirring at the stirring speed of 1000r/min, and centrifuging to obtain a precipitate and a supernatant;

s3: adding the fullerene solution into the supernatant again, stirring at the stirring speed of 1000r/min, and centrifuging until the supernatant becomes colorless to obtain a precipitate;

s4: washing the precipitate obtained at S3 and the precipitate obtained at S4 with ethanol;

s5: and drying the washed precipitate to obtain the titanium dioxide fullerene material.

In one aspect, the present disclosure provides a fullerene powder material, characterized by being prepared by any one of the aforementioned preparation methods.

In one embodiment, the present disclosure provides a cosmetic powder material comprising the fullerene powder material described above.

In one embodiment, the present disclosure provides a cosmetic powder material further comprising other cosmetic adjuvants.

In one embodiment, the present disclosure provides a cosmetic powder material comprising other cosmetic auxiliary materials selected from one or more of mica powders, titanium white powders, talc powders, sericite powders, silica and silicon-treated powders.

In one embodiment, the present disclosure provides a loose powder material, wherein the weight percentage of the fullerene powder material to other cosmetic auxiliary materials is 1:200 to 1: 1.

In one embodiment, the present disclosure provides a use of a fullerene powder material in the preparation of a cosmetic.

In one embodiment, the cosmetic includes, but is not limited to, solutions, suspensions, emulsions, ointments, gels, creams, emulsions, powders, soaps, surfactant-containing cleansers, oils, powdered foundations, emulsions, foundations, wax foundations, sprays, liniments, pastes and poultices in any dosage form, such as loose powders, creams, multiple emulsions, anhydrous compositions, dispersions, oils, emulsions, balsams, foams, lotions, gels, cream gels, hydroalcoholic solutions, hydroglycolic solutions, liniments, saline solutions, soaps, shampoos, conditioners, slurries, salves, mousses, ointments, powders, sticks, pencils, sprays, aerosols, capsules, gelatin capsules, tablets, dragees, powders, granular forms, chewing gums, solutions, suspensions, emulsions, syrups, polysaccharide films, jellies, gelatins, solutions, suspensions, lotions, creams, lotions, creams, lotions, anhydrous compositions, water dispersions, oil, creams, foams, lotions, creams, hydroalcoholic solutions, liniments, lotions, creams, gels, creams, ointments, creams, gels, gelatins, solutions, creams, lotions, creams, lotions, creams, gels, solutions, gels, pastes, gels, pastes, and cataplasms, pastes, and pastes, and pastes, ointments, creams, softening lotions, nourishing lotions, masks, essences, pilatory, shampoos, rinses, conditioners, hair conditioners, gels, skin lotions, skin softeners, fresheners, astringents, lotions, milk lotions, moisturizing lotions, nourishing lotions, massage creams, nourishing creams, moisturizing creams, hand creams, foundation creams, nourishing essences, sun screens, soaps, cleansing foams, cleansing milks, cleansing creams, body lotions, and body cleansers, pouch removers, cosmetic foundations, make-up removers, eye shadows, lipsticks, lip gloss, and lip powders; the effects of the cosmetic or toiletry product include, but are not limited to: whitening skin, improving pigmentation, treating acne, improving wrinkle, improving pachylosis, improving oily skin, improving dry skin, shrinking pore, treating scar, treating flush complexion, treating alopecia, promoting hair growth, treating burn, killing bacteria and mite, improving skin pit, and preventing acne and haze.

In one embodiment, the materials of the present disclosure may also be used with other adjuvants including hyaluronic acid, greases, surfactants, preservatives, fragrances, binders, thickeners, complexing agents, PH adjusters.

In one embodiment, the materials of the present disclosure may be used with a surfactant selected from the group consisting of: at least one of anionic surfactant, cationic surfactant, amphoteric surfactant, lipophilic nonionic surfactant, hydrophilic nonionic surfactant, and natural surfactant.

Example II

The disclosure is further illustrated with reference to the following examples. The description of the specific exemplary embodiments of the present disclosure has been presented for purposes of illustration and description. These descriptions are not intended to limit the disclosure to the precise form disclosed, and obviously many modifications and variations are possible in light of the teaching of this specification. The exemplary embodiments were chosen and described in order to explain certain principles of the disclosure and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the disclosure and various alternatives and modifications thereof.

The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.

Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.

Example 1: preparation of Fullerene powder material

Mixing ethyl orthosilicate, isopropanol and water, and stirring for 4 hours in equipment at the temperature of 60 ℃ to obtain a mixed solution; centrifuging the mixed solution in equipment for many times at a high speed to obtain a mesoporous silica precipitate;

mixing the mesoporous silica precipitate with a fullerene solution, stirring at the speed of 500r/min, and centrifuging to obtain precipitate and supernatant;

taking out the precipitate, adding the fullerene solution into the supernatant again, continuing to stir at the speed of 1500r/min, and centrifuging until the supernatant becomes colorless to obtain the precipitate;

and washing the precipitate obtained in the two steps with ethanol, and drying the washed precipitate to obtain silicon dioxide fullerene.

Example 2: preparation of Fullerene powder material

200mL of tetrabutyl titanate is weighed briefly and poured into the inner liner of the reaction kettle, 2L of distilled water is weighed according to the volume ratio of 1:10, and the distilled water is poured into the inner liner and mixed with tetrabutyl titanate and then placed into an oven. The reaction temperature is 120 ℃ and the reaction time is 5 h. After the sample is naturally cooled, the sample is cooled by distilled water and absolute ethyl alcohol to obtain a mesoporous titanium dioxide material;

mixing a mesoporous titanium dioxide material with a fullerene solution, stirring at the speed of 1000r/min, and centrifuging to obtain a precipitate and a supernatant;

taking out the precipitate, adding the fullerene solution into the supernatant again, continuing to stir at the speed of 1000r/min, and centrifuging until the supernatant becomes colorless to obtain the precipitate;

and washing the precipitate obtained in the two steps by using ethanol, and drying the washed precipitate to obtain the titanium dioxide fullerene.

Example 3: preparation of Fullerene powder material

Simply weighing 100mL of tetrabutyl titanate, pouring the tetrabutyl titanate into an inner liner of a reaction kettle, weighing 1L of distilled water according to the volume ratio of 1:5, pouring the distilled water into the inner liner and mixing the tetrabutyl titanate, putting the mixture into an oven, naturally cooling a sample at 120 ℃ for 4 hours, and cooling the sample with distilled water and absolute ethyl alcohol to obtain a mesoporous titanium dioxide material;

mixing a mesoporous titanium dioxide material, talcum powder and a fullerene solution, stirring at the speed of 1000r/min, and centrifuging to obtain a precipitate and a supernatant;

and washing the precipitate obtained in the two steps with ethanol, and drying the washed precipitate to obtain the composite powder fullerene.

Example 4: preparation of Fullerene powder material

Mixing ethyl orthosilicate, n-butanol and water, and stirring for 2 hours in equipment at the temperature of 60 ℃ to obtain a mixed solution; centrifuging the mixed solution in equipment for many times at a high speed to obtain a mesoporous silica precipitate;

mixing mesoporous silica, talcum powder, sericite and fullerene solution, stirring at the speed of 1500r/min, centrifuging to obtain precipitate and supernatant, and taking out the precipitate;

adding the fullerene solution into the supernatant again, continuing stirring at the speed of 1500r/min, and centrifuging until the supernatant becomes colorless to obtain a precipitate;

Example 5: the disclosed fullerene powder material free radical quenching experiment

Detection of quenching free radical effect of fullerene powder material through Electron Paramagnetic Resonance (EPR) test

The experimental principle is as follows: under Ultraviolet (UV) irradiation, H ₂ O ₂ A large number of hydroxyl radicals are generated and immediately captured by DMPO to form DMPO-OH, which is detected by Electron Paramagnetic Resonance (EPR). The spin trapping method is to utilize the short-lived free radicals and a special compound to act to generate relatively stable free radicals, so as to utilize the ESR method to detect the short-lived free radicals.

1. Preparing DMPO solution: add 5.5. mu.L of DMPO mother liquor to 250. mu.L of ultrapure water;

2. and (3) detection sample preparation: 20mg of the product of example 1 and the control (Veil Fullerene, Mitsubishi, Japan) were ultrasonically dispersed in 1000. mu.L of ultrapure water, and 25. mu.L of the mixture was immediately transferred to 25. mu.L of L H ₂ O ₂ After being mixed uniformly (100mM), 10 mu L of DPMO solution is added;

3. the solution was irradiated with 500W uv light for 4 minutes and then the X-band EPR spectrum was recorded in the dark.

And (4) conclusion: as shown in fig. 1, it can be observed that the fullerene powder material of the present disclosure has a significant radical quenching effect, which is stronger than that of the control, and it is also confirmed that only fullerene capable of being dispersed in water can exert the effect of quenching radicals.

Example 6: the disclosed fullerene powder material stability experiment and hydrophilicity experiment

Respectively taking 1.25g of the product of the example 2 and a reference substance (Veil Fullerene, a product of Mitsubishi Japan), adding 25g of deionized water into a 100mL volumetric flask, and shaking up; and (3) putting the mixture into an ultrasonic machine for 30 minutes of ultrasonic treatment, standing the mixture after ultrasonic treatment, and observing the state of the solution, wherein the product of example 2 and the stability thereof are shown in figure 2, and the product of a reference product and the stability thereof are shown in figure 3.

And respectively adding 20ml of toluene solution into two triangular flasks, extracting precipitated substances, performing rotary evaporation, and weighing to finally obtain the weight of the precipitated substances.

And (4) conclusion: as shown in fig. 2-3, due to the strong ultrasonic effect, the fullerene in the product can be separated from other auxiliary materials, but the fullerene split material disclosed by the invention can be uniformly and stably dispersed in water, the solution is beige, and no fullerene precipitation is found in the solution; and a large amount of black particles are separated out from the reference product, so that the product stability is poor. Therefore, the fullerene material disclosed by the invention has better hydrophilicity and stability.

Example 7: the disclosed fullerene powder material is subjected to ultraviolet absorption experiment

2.5g of the product obtained in example 4 is taken, 50g of toluene is added into a 100mL volumetric flask, and the mixture is shaken up; and (3) putting the mixture into an ultrasonic machine for ultrasonic treatment for 30 minutes, standing the mixture after ultrasonic treatment, taking supernatant for detection, and detecting the absorption effect of the product on ultraviolet rays by using an ultraviolet-visible absorption spectrum (UV-Vis), wherein the experimental result is shown in figure 4.

And (4) conclusion: as can be seen from FIG. 4, the fullerene powder material disclosed by the invention has a better ultraviolet absorption effect, and the ultraviolet absorbance of 10ppm reaches 0.7, which shows that the fullerene powder material disclosed by the invention has a strong ultraviolet damage resistance effect.

Example 8: the disclosed fullerene powder material is used for oxidation resistance experiment

2.49g KI solid and 0.75g example 1 or control (Veil Fullerene, Mitsubishi, Japan) were taken, and 26.76g deionized water was added to a 50mL beaker; dropping 3 drops of hydrogen peroxide solution into the solution by using a dropper, shaking up, standing and observing the color change of the solution, wherein the color change of the solution is shown in figure 5.

And (4) conclusion: as can be seen from fig. 5, after 8 hours of dropping hydrogen peroxide, the color of the solution added with the fullerene powder material of the present disclosure is not changed, which proves that the fullerene powder material of the present disclosure still has strong oxidation resistance after 8 hours; the reference substance has no oxidation resistance no matter 5 minutes or 8 hours after the hydrogen peroxide is dripped. Therefore, the fullerene powder material disclosed by the invention has more excellent oxidation resistance, and meanwhile, the oxidation resistance also verifies that the fullerene powder material disclosed by the invention has good dispersibility in water.

Example 9: experiments on waterproof and oilproof effects of cosmetics prepared from fullerene powder material

Compounding loose powder products: the fullerene powder material or the reference substance in the embodiment 1-3 is respectively compounded with 600g of mica, 120g of pearl powder, 10g of lycopene, 6g of zinc oxide, 12g of titanium dioxide powder, 40g of magnesium stearate, 8g of talcum powder, 10g of hydrophobic film-forming agent and 10g of natural pigment to form a loose powder product.

Selecting 30 volunteers, randomly dividing into 3 groups, each group containing 10 volunteers, dyeing skin with ink, applying fullerene loose powder on the dyed part of the skin of each group of volunteers, washing the tested part with clear water and water containing oil alternately, and observing the color of the tested part. Professional testers score the color of the product, the color of the product is 0 point when the product has no color, the color of the product is 10 points as before the product is washed, then the average score of each group is calculated, and the darker the color of the tested part is, the better the water and oil resistance of the product is, and the stronger the protection effect on the skin is. The test results are shown in table 1 below.

[ Table 1]

And (4) conclusion: the loose powder products prepared from the products of examples 1 to 3 have excellent hydrophobicity and oleophobicity, and can prevent sweat or oil secreted from the skin from destroying the effects of the cosmetics prepared therefrom.

Example 10: the experiment on the use effect of the cosmetics prepared from the fullerene powder material

Compounding loose powder products: the fullerene powder material or the reference substance in the embodiment 1-3 is respectively compounded with 550g of mica, 100g of pearl powder, 10g of lycopene, 10g of zinc oxide, 10g of titanium dioxide powder, 40g of magnesium stearate, 5g of ferric oxide, 8g of talcum powder, 10g of hydrophobic film-forming agent and 10g of natural pigment to form a loose powder product.

60 volunteers aged 25-35 were selected and randomly divided into 3 groups of 20 each, and the 3 groups of volunteers used the loose powder products of examples 1-3 respectively, with a service cycle of 3 months, and used once per person on average. A satisfaction test is carried out, wherein the standard of satisfaction to the use effect is that the foundation has good smoothness and spreadability and no stimulation to the skin when being applied; after the use, the user feels comfortable, breathable and natural, and the dry line phenomenon cannot occur; effectively keep the makeup-free, and have whitening effect after being used for a period of time. The results of the satisfaction test are shown in table 2 below:

[ Table 2]

Sample to be tested	Example 1	Example 2	Example 3	Reference substance
					Degree of satisfaction	84％	87％	95％	76％

And (4) conclusion: the loose powder products prepared from the fullerene powder materials of examples 1-3 have no stimulation to skin, smooth hand feeling, good skin-attaching property and air permeability, good spreadability and natural makeup, can effectively keep no makeup, and have a certain whitening effect after long-term use.

Example 11: topography testing of products

The product of example 1 was dispersed with ethanol, and the dispersion was dipped onto a silicon wafer using a capillary, and after the ethanol naturally volatilized, a scanning electron microscope test was performed, and the results are shown in fig. 6.

And (4) conclusion: the fullerene-silicon dioxide composite material is spherical, and the particle size is about 200 nm.

The above embodiments are merely illustrative of specific embodiments of the present disclosure, and are not intended to limit the scope of the present disclosure, and those skilled in the art can make various modifications and changes based on the prior art, and various changes and modifications made to the technical solution of the present disclosure by those skilled in the art should be within the scope of the present disclosure as defined by the claims.

Claims

1. A fullerene powder material for cosmetics, characterized by comprising a fullerene and a dispersing material, wherein the fullerene is selected from C ₆₀ Fullerene, C ₇₀ One or more of fullerenes or metallofullerenes, the dispersion material comprising a mesoporous dispersion material。

2. A fullerene powder material according to claim 1 wherein the mass ratio of fullerene to the dispersed material is 0.01% to 10%, preferably 0.01% to 5%, more preferably 0.01% to 2%.

3. A fullerene powder material according to claim 1 or 2 wherein the dispersing material is selected from one or more of silica, titanium dioxide, talc, mica, sericite, kaolin; preferably, the silica is mesoporous silica; preferably, the titanium dioxide is mesoporous titanium dioxide; preferably, the dispersion material is selected from one or more of mesoporous silica, mesoporous titanium dioxide, talcum powder and sericite.

4. A fullerene powder material according to any one of claims 1-3 wherein the fullerene powder material has a particle size of 0.1 to 10 μm, preferably 0.5 to 5 μm.

5. A method of producing a fullerene powder material according to any one of claims 1-4, comprising the steps of preparing a dispersion material, and mixing the dispersion material with a fullerene solution.

6. A method of preparing a fullerene powder material according to any one of claims 1-4, comprising the steps of:

s1: preparing a dispersed material in an apparatus;

s2: mixing the dispersion material with a fullerene solution, and stirring and centrifuging to obtain a precipitate and a supernatant;

7. The method according to claim 6, wherein in step S1, the apparatus is selected from one of a glass reaction kettle or a stainless steel reaction kettle;

preferably, in step S1, the dispersion material comprises mesoporous silica and/or mesoporous titania, and the mesoporous silica and/or mesoporous titania is preferably prepared by a hydrothermal method;

preferably, the temperature of the heating process of the hydrothermal method is selected from 10 ℃, 20 ℃, 40 ℃, 60 ℃, 80 ℃, 100 ℃, 120 ℃, preferably 60 ℃ or 120 ℃;

preferably, the heating process of the hydrothermal method is carried out for a time selected from 1 hour, 2 hours, 4 hours, 5 hours, 6 hours, preferably 4 hours or 5 hours;

preferably, in step S2 and step S3, the stirring speed of the stirring process is selected from 500r/min, 750r/min, 1000r/min, 1500r/min, preferably 1000r/min to 1500 r/min;

preferably, in steps S2 and S3, the centrifuged device is selected from one or more of a tube centrifuge, a plate filter or a bench filter;

preferably, in step S5, the drying device is selected from one or more of a rotary evaporator, a freeze dryer, a spray dryer, or a thin film evaporator.

8. A powder material for cosmetics, characterized by comprising the fullerene powder material according to any one of claims 1 to 4.

9. The cosmetic powder material according to claim 8, further comprising one or more cosmetic adjuvants selected from mica powders, titanium white powders, talc powders, sericite powders and silica, preferably, the weight percentage of the fullerene powder material to the cosmetic adjuvants is 1:200 to 1:1, preferably 1:100 to 1: 5.

10. A fullerene powder material according to any one of claims 1 to 4, or a cosmetic powder material according to any one of claims 8 to 9, for use in the preparation of a cosmetic.