WO2016199997A1 - Cosmetic composition provided with ultraviolet protection function, and method for preparing same - Google Patents

Cosmetic composition provided with ultraviolet protection function, and method for preparing same Download PDF

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Publication number
WO2016199997A1
WO2016199997A1 PCT/KR2015/013715 KR2015013715W WO2016199997A1 WO 2016199997 A1 WO2016199997 A1 WO 2016199997A1 KR 2015013715 W KR2015013715 W KR 2015013715W WO 2016199997 A1 WO2016199997 A1 WO 2016199997A1
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Prior art keywords
graphene quantum
weight
cosmetic composition
quantum dot
sunscreen
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PCT/KR2015/013715
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French (fr)
Korean (ko)
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전석우
윤혜원
송성호
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한국과학기술원
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Publication of WO2016199997A1 publication Critical patent/WO2016199997A1/en

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/04Topical preparations for affording protection against sunlight or other radiation; Topical sun tanning preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin

Definitions

  • the present invention relates to a cosmetic composition imparted with the sunscreen function and a method for producing the same. More specifically, the present invention relates to a cosmetic composition capable of absorbing ultraviolet rays and given a UV blocking function and a method of manufacturing the same.
  • UVC ultraviolet rays reaching the ground surface are classified into UVC (about 200 nm to about 280 nm), UVB (about 280 to about 320 nm), and UVA (about 320 nm to about 400 nm), depending on the wavelength band. Since UVC is mostly absorbed in the ozone layer, a sunscreen is required to effectively block ultraviolet rays in the UVA and UVB regions.
  • the sunscreen may include an inorganic UV scattering agent such as titanium dioxide having an ultraviolet scattering function, and an organic UV absorber including an organic compound that chemically absorbs ultraviolet light.
  • an inorganic UV scattering agent such as titanium dioxide having an ultraviolet scattering function
  • an organic UV absorber including an organic compound that chemically absorbs ultraviolet light.
  • Patent Literature 1 discloses a sunscreen containing titanium dioxide.
  • One object of the present invention is to provide a cosmetic composition having excellent chemical properties and endowed with excellent sunscreen function.
  • One object of the present invention is to provide a method for producing a cosmetic composition which has excellent chemical properties and is provided with a sunscreen function excellent in human applicability.
  • the problem to be solved by the present invention is not limited to the above-mentioned problem, and may be variously expanded within a range without departing from the spirit and scope of the present invention.
  • Cosmetic composition according to the exemplary embodiments of the present invention for achieving the above object of the present invention includes a graphene quantum dot and may have a sunscreen function.
  • the cosmetic composition may include the graphene quantum dots, an inorganic ultraviolet scattering agent, an organic ultraviolet absorber and an emulsion.
  • the composition comprises about 0.5% to about 5% by weight of the graphene quantum dots, about 5% to about 10% by weight of the inorganic ultraviolet scattering agent, about 3 to about 7.5 Weight percent of the organic ultraviolet absorbent, and from about 78 weight percent to about 91 weight percent of the emulsion.
  • the inorganic ultraviolet scattering agent may include rutile titanium dioxide.
  • the organic ultraviolet absorbent may be ethylhexyl methoxycinnamate, ethylhexyl salicylate, 4-methylbenzylidene camphor, isoamyl p-methoxycinnamate, octocrylene, phenylbenzimidazole Sulfonic acids, homosalates, synoxates, ethylhexyltrizone, polysilicon-15, tie-salicylates, popba (PABA), ethylhexyldimethylpava or glycerylpava. These may be used alone or in combination of two or more.
  • a graphene quantum dot powder A mixture of the graphene quantum dot powder and the inorganic ultraviolet scattering agent is prepared. The mixture is heat treated to form a composite pigment. An organic ultraviolet absorbent and an emulsion are mixed with the composite pigment.
  • a graphene quantum dot dispersion may be prepared by removing metal ions from a graphite interlayer compound in which metal ions are inserted into a graphite layer.
  • the graphene quantum dot dispersion in preparing the graphene quantum dot powder, may be dried at a temperature of about 100 ° C to about 130 ° C.
  • the heat treatment of the mixture may be performed at a temperature of about 100 °C to about 200 °C.
  • rutile titanium dioxide and ethylhexyl methoxycinnamate may be used as the inorganic UV scattering agent and the organic UV absorbing agent, respectively.
  • about 0.5% to about 5% by weight of the graphene quantum dot powder, about 5% to about 10% by weight of the inorganic UV scattering agent, about 3 to about the total weight of the sunscreen About 7.5% by weight of the organic ultraviolet absorbent and about 78% to about 91% by weight of the emulsion can be combined.
  • graphene quantum dots having an ultraviolet absorbing function may be included in the cosmetic composition.
  • an inorganic UV scattering agent such as titanium dioxide and an organic UV absorber
  • the application of affinity to the skin is remarkably improved by reducing the skin spreadability and the clouding phenomenon caused by the inorganic material.
  • the photocatalytic reaction by titanium dioxide can be suppressed, and the wavelength range and absorption intensity which can absorb ultraviolet rays can be expanded.
  • the graphene quantum dots can be produced by a standardized process at low cost, the economics of the cosmetic composition can also be improved.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a cosmetic composition according to exemplary embodiments.
  • FIG. 3 is a UV / VIS graph of measuring ultraviolet absorbing ability using the compositions according to Experimental Example 1.
  • FIG. 4 is a UV / VIS graph of measuring ultraviolet absorbing ability using the compositions according to Experimental Example 2.
  • FIG. 4 is a UV / VIS graph of measuring ultraviolet absorbing ability using the compositions according to Experimental Example 2.
  • FIG. 5 is a UV / VIS graph of measuring ultraviolet absorbing ability using a skin toner according to Experimental Example 3.
  • FIG. 5 is a UV / VIS graph of measuring ultraviolet absorbing ability using a skin toner according to Experimental Example 3.
  • FIG. 6 is a photograph for comparing color development of a cosmetic composition according to exemplary embodiments.
  • FIG. 7 is a photograph showing skin spreadability of a cosmetic composition according to exemplary embodiments.
  • FIG. 8 is a photograph showing skin stability of a cosmetic composition according to exemplary embodiments.
  • the cosmetic composition may include graphene quantum dots (GQD).
  • GQD graphene quantum dots
  • the cosmetic composition may have a UV absorbing function and, accordingly, may be provided as various cosmetics and beauty products having a UV blocking function.
  • the graphene quantum dots may be prepared in the form of a finally dried powder (see FIG. 2).
  • the graphene quantum dots may have a diameter of about 20 nm or less, for example, for the efficiency of ultraviolet absorption function.
  • graphene quantum dots having a diameter of about 10 nm to about 20 nm can be used.
  • the cosmetic composition may be provided as a sunscreen.
  • the sunscreen agent may include an emulsion, an inorganic UV scattering agent, an organic UV absorber, and the graphene quantum dot.
  • the emulsion may be a base formulation for imparting applicability and skin applicability of the sunscreen.
  • the emulsion may include materials known in the art of various organic series, and the composition thereof is not particularly limited.
  • titanium dioxide may be used as the inorganic ultraviolet scattering agent.
  • rutile titanium dioxide nanoparticles having a diameter of about 100 nm or less may be used as the inorganic ultraviolet scattering agent.
  • active species such as radicals can be generated, and the rutile titanium dioxide nanoparticles can be used.
  • an organic compound capable of absorbing ultraviolet rays in the UVB region may be used.
  • ethylhexyl methoxycinnamate for example, 2-Ethylhexyl 4-methoxycinnamate
  • ethylhexyl salicylate 4-methylbenzylidene camphor
  • isoamyl p-methoxycinnamate Octocrylene
  • phenylbenzimidazolesulfonic acid homosalate, synoxate, ethylhexyltrizone, polysilicone-15, tie-salicylate, popba (PABA), ethylhexyldimethylpava, glycerylpava, etc.
  • PABA popba
  • ethylhexyldimethylpava glycerylpava, etc.
  • ethylhexyl methoxycinnamate may be used as the organic ultraviolet absorber.
  • the sunscreen is about 0.5% to about 5% by weight of the graphene quantum dots, about 5% to about 10% by weight of the inorganic UV scattering agent, about 3 to about 7.5% by weight of the organic ultraviolet absorbent, and the balance of the emulsion.
  • the emulsion may be included in an amount of about 78% by weight to about 91% by weight based on the total weight of the sunscreen.
  • the ultraviolet absorber (eg, absorption wavelength region and absorption intensity) of the sunscreen may be further enhanced by the addition of the graphene quantum dots.
  • the content of the inorganic UV scattering agent and the organic UV absorber may be reduced than the allowable limit for human application.
  • the content of the inorganic ultraviolet scattering agent such as titanium dioxide, which is poor in skin spreadability and can cause a photocatalytic reaction, can be reduced.
  • sunscreens with improved human affinity and / or suitability can be obtained without causing side effects such as skin diseases.
  • the unique color of the brown system of the graphene quantum dots may be mixed with white titanium dioxide, thereby enabling natural skin color expression.
  • applicable sunscreens can be obtained without the addition of additional pigments, pigments.
  • Cosmetic compositions according to exemplary embodiments are not limited to the sunscreen.
  • the cosmetic composition may be made of various cosmetic products such as a whitening lotion, a moisturizer, a skin, etc., including the graphene quantum dots, and may be provided as a functional composition to which UV absorption ability is given.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a cosmetic composition according to exemplary embodiments.
  • FIG. 1 illustrates a method for preparing a sunscreen added with graphene quantum dots.
  • 2 is a photograph of dried powdery graphene quantum dots.
  • step S10 graphene quantum dot powder may be prepared.
  • the graphene quantum dots may be prepared by removing metal ions from a graphite interlayer compound in which metal ions are inserted into the graphite layer.
  • the method of manufacturing the graphene quantum dot may refer to the present applicant's publication No. 2015-0044326 (published on May 4, 2015, application number 2013-0127275), which is incorporated herein by reference.
  • the graphene quantum dots may be prepared as an aqueous dispersion having a diameter of about 20 nm or less.
  • the graphene quantum dots dispersed in water may be dried at a temperature of, for example, about 100 ° C. to about 130 ° C. to obtain graphene quantum dot powder as shown in FIG. 2.
  • the graphene quantum dots may be obtained from various carbon precursors in addition to the graphite interlayer compound.
  • step S20 a mixture of the graphene quantum dot powder and the inorganic ultraviolet scattering agent may be prepared.
  • rutile titanium dioxide can be used as the inorganic ultraviolet scattering agent.
  • the mixture may be prepared by inducing the graphene quantum dot powder and rutile titanium dioxide and mixing / stirring evenly using a mortar and pestle.
  • step S30 the mixture may be heat treated to form a composite pigment.
  • the heat treatment the crystal structures of the graphene quantum dot powder and rutile titanium dioxide included in the composite pigments may be stabilized.
  • the heat treatment may be performed at a temperature of about 150 ° C to about 200 ° C.
  • the cosmetic composition according to the exemplary embodiments may be prepared by mixing the organic UV absorber and the emulsion in the composite pigment.
  • an organic compound having a UVB region ultraviolet absorbing function such as ethylhexyl methoxycinnamate can be used as the organic ultraviolet absorbent.
  • the prepared cosmetic composition comprises about 0.5% to about 5% by weight of the graphene quantum dots, about 5% to about 10% by weight of the inorganic ultraviolet scattering agent, about 3 to about total weight About 7.5% by weight of the organic ultraviolet absorbent, and about 78% to about 91% by weight of the emulsion.
  • compositions having compositions according to Table 1 below were prepared. Specifically, rutile titanium dioxide (rutile TiO 2 ) was used as an inorganic ultraviolet scattering agent, and 2-ethylhexyl 4-methoxycinnamate (OMC) was used as an organic ultraviolet absorber.
  • rutile TiO 2 rutile TiO 2
  • OMC 2-ethylhexyl 4-methoxycinnamate
  • FIG. 3 is a UV / VIS graph of measuring ultraviolet absorbance using the compositions according to Experimental Example 1 (compositions in Table 1).
  • FIG. 3 is a UV / VIS graph of measuring ultraviolet absorbance using the compositions according to Experimental Example 1 (compositions in Table 1).
  • the composition 2 including the OMC absorbs UV in the region of about 320 nm to about 340 nm, and the intensity of absorption becomes stronger as graphene quantum dots are added as in composition 6. have. Therefore, it can be seen that the graphene quantum dot acts as an ultraviolet absorption enhancer.
  • composition 5 including OMC and TiO 2
  • UV absorbing ability was shown in a wider wavelength range
  • graphene quantum dots were added as in composition 8, the absorption wavelength region and the intensity of absorption were enhanced. have.
  • the range of wavelengths absorbed by the addition of TiO 2 can be further expanded, and it can be predicted that the intensity of absorption is enhanced as graphene quantum dots are added.
  • compositions having compositions according to Table 2 were prepared.
  • FIG. 4 is a UV / VIS graph of measuring ultraviolet absorbing capacity using the compositions according to Experimental Example 2 (compositions in Table 2).
  • FIG. 4 is a UV / VIS graph of measuring ultraviolet absorbing capacity using the compositions according to Experimental Example 2 (compositions in Table 2).
  • composition 3 As graphene quantum dots were added in Composition 2 (composition 3), the overall UV absorption intensity increased, particularly in the range of about 340 nm or more. In addition, as the graphene quantum dots were further increased (composition 4), the UV absorption intensity was further increased.
  • Graphene quantum dots were added to commercially available skin toner products according to Table 3 below to evaluate ultraviolet absorption characteristics.
  • FIG. 5 is a UV / VIS graph of measuring ultraviolet absorbing ability using a skin toner according to Experimental Example 3.
  • FIG. 5 is a UV / VIS graph of measuring ultraviolet absorbing ability using a skin toner according to Experimental Example 3.
  • the general skin toner does not substantially exhibit absorption in the wavelength range of about 300 nm or more, but the absorption intensity increases in the UV region of the wavelength of about 300 nm or more as the amount of graphene quantum dots increases. It can be seen.
  • graphene quantum dots can be added to give a sunscreen function to not only a sunscreen but also a general cosmetic product.
  • FIG. 6 is a photograph for comparing color development of a cosmetic composition according to exemplary embodiments. Specifically, Figure 6 is a photograph showing the color development of Composition 2, Composition 3 and Composition 4 (see Table 2) of Experimental Example 2.
  • Figure 7 is a photograph showing skin spreadability of a cosmetic composition according to exemplary embodiments. Specifically, Figure 7 is a photograph showing a process of applying the composition 8 (see Table 1) of Experimental Example 1 to the skin.
  • the sunscreen according to the exemplary embodiments including the graphene quantum dots is applied in substantially the same color as the skin color without the cloudiness and the lifting phenomenon.
  • FIG. 8 is a photograph showing skin stability of a cosmetic composition according to exemplary embodiments. Specifically, FIG. 8 includes photographs taken 24 hours after applying Composition 4 (see Table 2) of Experimental Example 2 to the skin.
  • the cosmetic composition according to the above-described exemplary embodiments includes graphene quantum dots, and may have improved skin affinity, applicability, and retain sunscreen functionality.
  • the cosmetic composition may be provided in various cosmetic products such as skin, lotion and the like with sunscreen as well as sunscreen.

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Abstract

Provided is a cosmetic composition which contains graphene quantum dots (GQD) and has an ultraviolet protection function. Ultraviolet absorption capacity can be strengthened as skin affinity is improved according to addition of the GQD.

Description

자외선 차단 기능이 부여된 화장료 조성물 및 이의 제조 방법Cosmetic composition imparted with the sun protection function and a method of manufacturing the same
본 발명은 자외선 차단 기능이 부여된 화장료 조성물 및 이의 제조 방법에 관한 것이다. 보다 상세하게는, 본 발명은 자외선 흡수가 가능하며 자외선 차단 기능이 부여된 화장료 조성물 및 이의 제조 방법에 관한 것이다.The present invention relates to a cosmetic composition imparted with the sunscreen function and a method for producing the same. More specifically, the present invention relates to a cosmetic composition capable of absorbing ultraviolet rays and given a UV blocking function and a method of manufacturing the same.
환경 오염에 따라 자외선 노출 우려도 증가하고 있으며, 자외선 차단제의 수요 역시 함께 증가하고 있다. 예를 들면, 지표면에 도달하는 자외선은 파장대에 따라 UVC(약 200 nm 내지 약 280 nm), UVB(약 280 내지 약 320 nm) 및 UVA(약 320 nm 내지 약 400 nm)으로 분류되며, 이 중 UVC는 오존층에서 대부분 흡수되므로, UVA 및 UVB 영역의 자외선을 효과적으로 동시에 차단하기 위한 자외선 차단제가 필요하다. There is an increasing concern about UV exposure due to environmental pollution, and the demand for sunscreens is also increasing. For example, ultraviolet rays reaching the ground surface are classified into UVC (about 200 nm to about 280 nm), UVB (about 280 to about 320 nm), and UVA (about 320 nm to about 400 nm), depending on the wavelength band. Since UVC is mostly absorbed in the ozone layer, a sunscreen is required to effectively block ultraviolet rays in the UVA and UVB regions.
상기 자외선 차단제는 자외선 산란 기능을 갖는 이산화티탄과 같은 무기 계열 자외선 산란제, 및 화학적으로 자외선을 흡수하는 유기 화합물을 포함하는 유기 계열 자외선 흡수제를 포함할 수 있다.The sunscreen may include an inorganic UV scattering agent such as titanium dioxide having an ultraviolet scattering function, and an organic UV absorber including an organic compound that chemically absorbs ultraviolet light.
예를 들면, 특허문헌 1은 이산화티탄을 포함한 자외선 차단제를 개시하고 있다.For example, Patent Literature 1 discloses a sunscreen containing titanium dioxide.
<선행기술문헌><Preceding technical literature>
<특허문헌><Patent Documents>
1. 대한민국 공개특허공보 제2015-0035126호(2015.04.06)1. Republic of Korea Patent Publication No. 2015-0035126 (2015.04.06)
본 발명의 일 과제는 우수한 화학적 특성을 가지며 인체 적용성이 우수한 자외선 차단 기능이 부여된 화장료 조성물을 제공하는 것이다. One object of the present invention is to provide a cosmetic composition having excellent chemical properties and endowed with excellent sunscreen function.
본 발명의 일 과제는 우수한 화학적 특성을 가지며 인체 적용성이 우수한 자외선 차단 기능이 부여된 화장료 조성물을 제조 방법을 제공하는 것이다.One object of the present invention is to provide a method for producing a cosmetic composition which has excellent chemical properties and is provided with a sunscreen function excellent in human applicability.
다만, 본 발명이 해결하고자 하는 과제는 상기 언급된 과제에 한정되는 것이 아니며, 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위에서 다양하게 확장될 수 있을 것이다.However, the problem to be solved by the present invention is not limited to the above-mentioned problem, and may be variously expanded within a range without departing from the spirit and scope of the present invention.
상술한 본 발명의 일 과제를 달성하기 위한 본 발명의 예시적인 실시예들에 따른 화장료 조성물은 그래핀 양자점을 포함하며 자외선 차단 기능을 가질 수 있다.Cosmetic composition according to the exemplary embodiments of the present invention for achieving the above object of the present invention includes a graphene quantum dot and may have a sunscreen function.
예시적인 실시예들에 따르면, 상기 화장료 조성물은 상기 그래핀 양자점, 무기 자외선 산란제, 유기 자외선 흡수제 및 에멀젼을 포함할 수 있다.According to exemplary embodiments, the cosmetic composition may include the graphene quantum dots, an inorganic ultraviolet scattering agent, an organic ultraviolet absorber and an emulsion.
예시적인 실시예들에 따르면, 상기 조성물은 총 중량 대비 약 0.5 중량% 내지 약 5 중량%의 상기 그래핀 양자점, 약 5 중량% 내지 약 10 중량%의 상기 무기 자외선 산란제, 약 3 내지 약 7.5 중량%의 상기 유기 자외선 흡수제, 및 약 78 중량% 내지 약 91 중량%의 상기 에멀젼을 포함할 수 있다.According to exemplary embodiments, the composition comprises about 0.5% to about 5% by weight of the graphene quantum dots, about 5% to about 10% by weight of the inorganic ultraviolet scattering agent, about 3 to about 7.5 Weight percent of the organic ultraviolet absorbent, and from about 78 weight percent to about 91 weight percent of the emulsion.
예시적인 실시예들에 따르면, 상기 무기 자외선 산란제는 금홍석(rutile) 이산화티탄을 포함할 수 있다. According to exemplary embodiments, the inorganic ultraviolet scattering agent may include rutile titanium dioxide.
예시적인 실시예들에 따르면, 상기 유기 자외선 흡수제는 에틸헥실 메톡시신나메이트, 에틸헥실살리실레이트, 4-메틸벤질리덴캠퍼, 이소아밀 p-메톡시신나메이트, 옥토크릴렌, 페닐벤즈이미다졸설포닉산, 호모살레이트, 시녹세이트, 에틸헥실트리아존, 폴리실리콘-15, 티이에이-살리실레이트, 팝바(PABA), 에틸헥실디메틸파바 또는 글리세릴파바를 포함할 수 있다. 이들은 단독으로 혹은 2 이상이 조합되어 사용될 수 있다.According to exemplary embodiments, the organic ultraviolet absorbent may be ethylhexyl methoxycinnamate, ethylhexyl salicylate, 4-methylbenzylidene camphor, isoamyl p-methoxycinnamate, octocrylene, phenylbenzimidazole Sulfonic acids, homosalates, synoxates, ethylhexyltrizone, polysilicon-15, tie-salicylates, popba (PABA), ethylhexyldimethylpava or glycerylpava. These may be used alone or in combination of two or more.
상술한 본 발명의 일 과제를 달성하기 위한 본 발명의 예시적인 실시예들에 따른 자외선 차단제의 제조 방법에 따르면 그래핀 양자점 분말을 준비한다. 상기 그래핀 양자점 분말 및 무기 자외선 산란제의 혼합물을 제조한다. 상기 혼합물을 열처리하여 복합 안료를 형성한다. 상기 복합 안료에 유기 자외선 흡수제 및 에멀젼을 혼합한다. According to the method of manufacturing the sunscreen according to the exemplary embodiments of the present invention for achieving the above object of the present invention to prepare a graphene quantum dot powder. A mixture of the graphene quantum dot powder and the inorganic ultraviolet scattering agent is prepared. The mixture is heat treated to form a composite pigment. An organic ultraviolet absorbent and an emulsion are mixed with the composite pigment.
예시적인 실시예들에 따르면, 상기 그래핀 양자점 분말을 준비함에 있어서, 금속 이온이 그래파이트 층에 삽입된 그래파이트 층간 화합물로부터 금속 이온을 제거하여 그래핀 양자점 수분산체를 제조할 수 있다.According to exemplary embodiments, in preparing the graphene quantum dot powder, a graphene quantum dot dispersion may be prepared by removing metal ions from a graphite interlayer compound in which metal ions are inserted into a graphite layer.
예시적인 실시예들에 따르면, 상기 그래핀 양자점 분말을 준비함에 있어서 상기 그래핀 양자점 수분산체를 약 100℃ 내지 약 130℃의 온도에서 건조시킬 수 있다. According to exemplary embodiments, in preparing the graphene quantum dot powder, the graphene quantum dot dispersion may be dried at a temperature of about 100 ° C to about 130 ° C.
예시적인 실시예들에 따르면, 상기 혼합물을 열처리하는 단계는 약 100℃ 내지 약 200℃의 온도에서 수행될 수 있다.According to exemplary embodiments, the heat treatment of the mixture may be performed at a temperature of about 100 ℃ to about 200 ℃.
예시적인 실시예들에 따르면, 상기 무기 자외선 산란제 및 상기 유기 자외선 흡수제로서 각각 금홍석 이산화티탄 및 에틸헥실 메톡시신나메이트를 사용할 수 있다.According to exemplary embodiments, rutile titanium dioxide and ethylhexyl methoxycinnamate may be used as the inorganic UV scattering agent and the organic UV absorbing agent, respectively.
예시적인 실시예들에 따르면, 상기 자외선 차단제의 총 중량 대비 약 0.5 중량% 내지 약 5 중량%의 상기 그래핀 양자점 분말, 약 5 중량% 내지 약 10 중량%의 상기 무기 자외선 산란제, 약 3 내지 약 7.5 중량%의 상기 유기 자외선 흡수제, 및 약 78 중량% 내지 약 91 중량%의 상기 에멀젼이 조합될 수 있다. According to exemplary embodiments, about 0.5% to about 5% by weight of the graphene quantum dot powder, about 5% to about 10% by weight of the inorganic UV scattering agent, about 3 to about the total weight of the sunscreen About 7.5% by weight of the organic ultraviolet absorbent and about 78% to about 91% by weight of the emulsion can be combined.
상술한 바와 같이 본 발명의 예시적인 실시예들에 따르면, 자외선 흡수 기능을 갖는 그래핀 양자점을 화장료 조성물에 포함시킬 수 있다. 예를 들어, 그래핀 양자점이 이산화티탄과 같은 무기계열 자외선 산란제 및 유기 계열 자외선 흡수제와 함께 사용되는 경우, 상기 무기 물질에 의한 피부 발림성 저하, 백탁 현상 등을 현저히 개선하여 피부에의 친화성을 증가시킬 수 있다. 또한, 이산화티탄에 의한 광촉매 반응을 억제하고, 자외선 흡수 가능한 파장 영역 및 흡수 세기를 확장시킬 수 있다.As described above, according to exemplary embodiments of the present invention, graphene quantum dots having an ultraviolet absorbing function may be included in the cosmetic composition. For example, when graphene quantum dots are used together with an inorganic UV scattering agent such as titanium dioxide and an organic UV absorber, the application of affinity to the skin is remarkably improved by reducing the skin spreadability and the clouding phenomenon caused by the inorganic material. Can be increased. In addition, the photocatalytic reaction by titanium dioxide can be suppressed, and the wavelength range and absorption intensity which can absorb ultraviolet rays can be expanded.
상기 그래핀 양자점은 저비용으로 표준화된 공정에 의해 생산될 수 있으므로, 화장료 조성물의 경제성 역시 향상될 수 있다.Since the graphene quantum dots can be produced by a standardized process at low cost, the economics of the cosmetic composition can also be improved.
도 1은 예시적인 실시예들에 따른 화장료 조성물의 제조 방법을 설명하기 위한 순서도이다.1 is a flowchart illustrating a method of manufacturing a cosmetic composition according to exemplary embodiments.
도 2는 건조된 분말상의 그래핀 양자점의 사진이다.2 is a photograph of dried powdery graphene quantum dots.
도 3은 실험예 1에 따른 조성물들을 사용하여 자외선 흡수능을 측정한 UV/VIS 그래프이다.3 is a UV / VIS graph of measuring ultraviolet absorbing ability using the compositions according to Experimental Example 1. FIG.
도 4는 실험예 2에 따른 조성물들을 사용하여 자외선 흡수능을 측정한 UV/VIS 그래프이다.4 is a UV / VIS graph of measuring ultraviolet absorbing ability using the compositions according to Experimental Example 2. FIG.
도 5는 실험예 3에 따른 스킨 토너를 사용하여 자외선 흡수능을 측정한 UV/VIS 그래프이다.5 is a UV / VIS graph of measuring ultraviolet absorbing ability using a skin toner according to Experimental Example 3. FIG.
도 6은 예시적인 실시예들에 따른 화장료 조성물의 발색을 비교하기 위한 사진들이다.6 is a photograph for comparing color development of a cosmetic composition according to exemplary embodiments.
도 7은 예시적인 실시예들에 따른 화장료 조성물의 피부 발림성을 나타내는 사진들이다.7 is a photograph showing skin spreadability of a cosmetic composition according to exemplary embodiments.
도 8은 예시적인 실시예들에 따른 화장료 조성물의 피부 안정성을 나타내는 사진들이다.8 is a photograph showing skin stability of a cosmetic composition according to exemplary embodiments.
이하, 첨부한 도면을 참조하여 본 발명의 실시예에 대해 상세히 설명한다. 본 발명은 다양한 변경을 가할 수 있고 여러 가지 형태를 가질 수 있는 바, 특정 실시예들을 예시하고 본문에 상세하게 설명하고자 한다. 그러나 이는 본 발명을 특정한 개시 형태에 대해 한정하려는 것이 아니며, 본 발명의 사상 및 기술 범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. 첨부된 도면에 있어서, 구조물들의 치수는 본 발명의 명확성을 기하기 위하여 실제보다 확대하여 도시한 것이다. Hereinafter, with reference to the accompanying drawings will be described in detail an embodiment of the present invention. As the inventive concept allows for various changes and numerous modifications, particular embodiments will be illustrated and described in detail in the text. However, this is not intended to limit the present invention to a specific disclosed form, it should be understood to include all modifications, equivalents, and substitutes included in the spirit and scope of the present invention. In the accompanying drawings, the dimensions of the structures are shown in an enlarged scale than actual for clarity of the invention.
본 출원에서 사용한 용어는 단지 특정한 실시예를 설명하기 위해 사용된 것으로, 본 발명을 한정하려는 의도가 아니다. 단수의 표현은 문맥상 명백하게 다르게 뜻하지 않는 한, 복수의 표현을 포함한다. 본 출원에서, "포함하다" 또는 "가지다" 등의 용어는 명세서상에 기재된 특징, 숫자, 단계, 동작, 구성요소 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 숫자, 단계, 동작, 구성요소 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다.The terminology used herein is for the purpose of describing particular example embodiments only and is not intended to be limiting of the present invention. Singular expressions include plural expressions unless the context clearly indicates otherwise. In this application, the terms "comprise" or "having" are intended to indicate that there is a feature, number, step, operation, component, or a combination thereof described in the specification, but one or more other features or numbers. It is to be understood that the present invention does not exclude in advance the possibility of the presence or the addition of steps, actions, components, or a combination thereof.
다르게 정의되지 않는 한, 기술적이거나 과학적인 용어를 포함해서 여기서 사용되는 모든 용어들은 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자에 의해 일반적으로 이해되는 것과 동일한 의미를 가지고 있다. 일반적으로 사용되는 사전에 정의되어 있는 것과 같은 용어들은 관련 기술의 문맥 상 가지는 의미와 일치하는 의미를 가지는 것으로 해석되어야 하며, 본 출원에서 명백하게 정의하지 않는 한, 이상적이거나 과도하게 형식적인 의미로 해석되지 않는다.Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art. Terms such as those defined in the commonly used dictionaries should be construed as having meanings consistent with the meanings in the context of the related art and shall not be construed in ideal or excessively formal meanings unless expressly defined in this application. Do not.
화장료 조성물Cosmetic composition
예시적인 실시예들에 따르면, 화장료 조성물은 그래핀 양자점(Graphene Quantum Dots: GQD)을 포함할 수 있다. 상기 그래핀 양자점이 포함됨에 따라 상기 화장료 조성물은 자외선 흡수 기능을 가지며 이에 따라, 자외선 차단 기능이 부여된 각종 화장품, 미용 제품으로 제공될 수 있다.According to exemplary embodiments, the cosmetic composition may include graphene quantum dots (GQD). As the graphene quantum dots are included, the cosmetic composition may have a UV absorbing function and, accordingly, may be provided as various cosmetics and beauty products having a UV blocking function.
상기 그래핀 양자점은 최종적으로 건조된 분말 상으로 제조될 수 있다(도 2 참조). 일부 실시예들에 있어서, 상기 그래핀 양자점은 자외선 흡수 기능의 효율을 위해 예를 들면 약 20 nm이하의 직경을 갖는 것을 사용할 수 있다. 일 실시예에 있어서, 약 10 nm 내지 약 20 nm의 직경을 갖는 그래핀 양자점을 사용할 수 있다.The graphene quantum dots may be prepared in the form of a finally dried powder (see FIG. 2). In some embodiments, the graphene quantum dots may have a diameter of about 20 nm or less, for example, for the efficiency of ultraviolet absorption function. In one embodiment, graphene quantum dots having a diameter of about 10 nm to about 20 nm can be used.
일부 예시적인 실시예들에 따르면, 상기 화장료 조성물은 자외선 차단제로 제공될 수 있다. 예시적인 실시예들에 따르면, 상기 자외선 차단제는 에멀젼, 무기 자외선 산란제, 유기 자외선 흡수제 및 상기 그래핀 양자점을 포함할 수 있다.According to some exemplary embodiments, the cosmetic composition may be provided as a sunscreen. In example embodiments, the sunscreen agent may include an emulsion, an inorganic UV scattering agent, an organic UV absorber, and the graphene quantum dot.
상기 에멀젼은 상기 자외선 차단제의 도포성, 피부 적용성을 부여하기 위한 베이스 제제일 수 있다. 상기 에멀젼은 다양한 유기 계열의 당해 기술 분야에서 공지된 물질을 포함할 수 있으며, 특별히 그 조성이 한정되는 것은 아니다.The emulsion may be a base formulation for imparting applicability and skin applicability of the sunscreen. The emulsion may include materials known in the art of various organic series, and the composition thereof is not particularly limited.
예시적인 실시예들에 따르면, 상기 무기 자외선 산란제로서 이산화티탄(TiO2)을 사용할 수 있다. 일부 실시예들에 있어서, 상기 무기 자외선 산란제로서 예를 들면, 약 100 nm 이하의 직경을 갖는 금홍석(rutile) 이산화티탄 나노입자를 사용할 수 있다. 아나타제(anatase) 형태의 이산화티탄 나노입자를 사용하는 경우, 자외선에 의해 광촉매 반응이 활성화되어 라디칼과 같은 활성종이 다량 생성될 수 있으므로, 금홍석 형태의 이산화티탄 나노입자를 사용할 수 있다.According to exemplary embodiments, titanium dioxide (TiO 2 ) may be used as the inorganic ultraviolet scattering agent. In some embodiments, for example, rutile titanium dioxide nanoparticles having a diameter of about 100 nm or less may be used as the inorganic ultraviolet scattering agent. In the case of using the titanium dioxide nanoparticles in the anatase form, since the photocatalytic reaction is activated by ultraviolet light, a large amount of active species such as radicals can be generated, and the rutile titanium dioxide nanoparticles can be used.
상기 유기 자외선 흡수제로서 UVB 영역의 자외선을 흡수할 수 있는 유기 화합물을 사용할 수 있다. 예를 들면, 상기 유기 자외선 흡수제로서 에틸헥실 메톡시신나메이트(예를 들면, 2-Ethylhexyl 4-methoxycinnamate), 에틸헥실살리실레이트, 4-메틸벤질리덴캠퍼, 이소아밀 p-메톡시신나메이트, 옥토크릴렌, 페닐벤즈이미다졸설포닉산, 호모살레이트, 시녹세이트, 에틸헥실트리아존, 폴리실리콘-15, 티이에이-살리실레이트, 팝바(PABA), 에틸헥실디메틸파바, 글리세릴파바 등을 사용할 수 있다. 이들은 단독으로 또는 2 이상이 조합되어 사용될 수 있다.As the organic ultraviolet absorber, an organic compound capable of absorbing ultraviolet rays in the UVB region may be used. For example, ethylhexyl methoxycinnamate (for example, 2-Ethylhexyl 4-methoxycinnamate), ethylhexyl salicylate, 4-methylbenzylidene camphor, isoamyl p-methoxycinnamate, Octocrylene, phenylbenzimidazolesulfonic acid, homosalate, synoxate, ethylhexyltrizone, polysilicone-15, tie-salicylate, popba (PABA), ethylhexyldimethylpava, glycerylpava, etc. Can be used. These may be used alone or in combination of two or more.
일부 예시적인 실시예들에 있어서, 상기 유기 자외선 흡수제로서 에틸헥실 메톡시신나메이트를 사용할 수 있다.In some exemplary embodiments, ethylhexyl methoxycinnamate may be used as the organic ultraviolet absorber.
예시적인 실시예들에 있어서, 상기 자외선 차단제는 총 중량 대비 약 0.5 중량% 내지 약 5 중량%의 상기 그래핀 양자점, 약 5 중량% 내지 약 10 중량%의 상기 무기 자외선 산란제, 약 3 내지 약 7.5 중량%의 상기 유기 자외선 흡수제, 및 잔량의 상기 에멀젼을 포함할 수 있다. 예를 들면, 상기 에멀젼은 상기 자외선 차단제의 총 중량 대비 약 78 중량% 내지 약 91 중량%의 함량으로 포함될 수 있다.In exemplary embodiments, the sunscreen is about 0.5% to about 5% by weight of the graphene quantum dots, about 5% to about 10% by weight of the inorganic UV scattering agent, about 3 to about 7.5% by weight of the organic ultraviolet absorbent, and the balance of the emulsion. For example, the emulsion may be included in an amount of about 78% by weight to about 91% by weight based on the total weight of the sunscreen.
상술한 바와 같이, 예시적인 실시예들에 따르면, 상기 그래핀 양자점의 첨가에 의해 상기 자외선 차단제의 자외선 흡수능력(예를 들면, 흡수 파장 영역 및 흡수 세기)이 보다 강화될 수 있다. As described above, according to exemplary embodiments, the ultraviolet absorber (eg, absorption wavelength region and absorption intensity) of the sunscreen may be further enhanced by the addition of the graphene quantum dots.
추가적으로, 상기 자외선 차단제에 자외선 흡수 기능을 갖는 상기 그래핀 양자점이 포함되므로, 상기 무기 자외선 산란제 및 상기 유기 자외선 흡수제의 함량이 인체 적용을 위한 허용 한도보다 감소될 수 있다. 예를 들면, 피부 발림성이 약하고, 광촉매 반응을 유발할 수 있는 이산화티탄과 같은 상기 무기 자외선 산란제의 함량이 감소될 수 있다. 따라서, 피부 질환과 같은 부작용을 야기하지 않으면서 인체 친화도 및/또는 적합성이 향상된 자외선 차단제가 수득될 수 있다. Additionally, since the graphene quantum dots having ultraviolet absorbing function are included in the sunscreen, the content of the inorganic UV scattering agent and the organic UV absorber may be reduced than the allowable limit for human application. For example, the content of the inorganic ultraviolet scattering agent, such as titanium dioxide, which is poor in skin spreadability and can cause a photocatalytic reaction, can be reduced. Thus, sunscreens with improved human affinity and / or suitability can be obtained without causing side effects such as skin diseases.
또한, 상기 그래핀 양자점의 갈색 계통의 고유한 색상이 백색의 이산화티탄과 혼합되어, 자연스러운 피부색 발현이 가능할 수 있다. 따라서, 추가적인 색소, 안료의 첨가 없이도 적용 가능한 자외선 차단제가 수득될 수 있다.In addition, the unique color of the brown system of the graphene quantum dots may be mixed with white titanium dioxide, thereby enabling natural skin color expression. Thus, applicable sunscreens can be obtained without the addition of additional pigments, pigments.
예시적인 실시예들에 따른 화장료 조성물은 상기 자외선 차단제에 제한되는 것은 아니다. 예를 들면, 상기 화장료 조성물은 상기 그래핀 양자점이 포함된 미백용 로션, 보습제, 스킨 등과 같은 다양한 화장료 제품으로 제조되어 자외선 흡수능이 부여된 기능성 조성물로 제공될 수 있다.Cosmetic compositions according to exemplary embodiments are not limited to the sunscreen. For example, the cosmetic composition may be made of various cosmetic products such as a whitening lotion, a moisturizer, a skin, etc., including the graphene quantum dots, and may be provided as a functional composition to which UV absorption ability is given.
도 1은 예시적인 실시예들에 따른 화장료 조성물의 제조 방법을 설명하기 위한 순서도이다. 예를 들면, 도 1은 그래핀 양자점이 첨가된 자외선 차단제의 제조 방법을 설명하고 있다. 한편, 도 2는 건조된 분말상의 그래핀 양자점의 사진이다.1 is a flowchart illustrating a method of manufacturing a cosmetic composition according to exemplary embodiments. For example, FIG. 1 illustrates a method for preparing a sunscreen added with graphene quantum dots. 2 is a photograph of dried powdery graphene quantum dots.
도 1 및 도 2를 참조하면, 단계 S10에서, 그래핀 양자점 분말을 준비할 수 있다. 1 and 2, in step S10, graphene quantum dot powder may be prepared.
일부 실시예들에 있어서, 상기 그래핀 양자점은 금속 이온이 그래파이트 층에 삽입된 그래파이트 층간 화합물로부터 금속 이온을 제거함으로써 제조될 수 있다. 상기 그래핀 양자점의 제조 방법은 예를 들면, 본 출원에 참조로서 병합되는 본 출원인의 공개특허공보 제2015-0044326호(공개일 2015.05.04, 출원번호 2013-0127275)를 참조할 수 있다. 예를 들면, 상기 그래핀 양자점은 약 20 nm 이하의 직경을 갖는 수분산체로서 제조될 수 있다. In some embodiments, the graphene quantum dots may be prepared by removing metal ions from a graphite interlayer compound in which metal ions are inserted into the graphite layer. For example, the method of manufacturing the graphene quantum dot may refer to the present applicant's publication No. 2015-0044326 (published on May 4, 2015, application number 2013-0127275), which is incorporated herein by reference. For example, the graphene quantum dots may be prepared as an aqueous dispersion having a diameter of about 20 nm or less.
이후, 물에 분산된 상기 그래핀 양자점을 예를 들면, 약 100℃ 내지 약 130℃의 온도에서 건조시켜 도 2에 도시된 바와 같은 그래핀 양자점 분말을 수득할 수 있다.Thereafter, the graphene quantum dots dispersed in water may be dried at a temperature of, for example, about 100 ° C. to about 130 ° C. to obtain graphene quantum dot powder as shown in FIG. 2.
그러나, 상기 그래핀 양자점은 상기 그래파이트 층간 화합물 외에 다양한 탄소 전구체들로부터 수득될 수도 있다.However, the graphene quantum dots may be obtained from various carbon precursors in addition to the graphite interlayer compound.
다시 도 1을 참조하면, 단계 S20에서, 상기 그래핀 양자점 분말 및 무기 자외선 산란제의 혼합물을 제조할 수 있다.Referring back to FIG. 1, in step S20, a mixture of the graphene quantum dot powder and the inorganic ultraviolet scattering agent may be prepared.
상술한 바와 같이, 상기 무기 자외선 산란제로서 금홍석 이산화티탄을 사용할 수 있다. 예를 들면, 상기 그래핀 양자점 분말 및 금홍석 이산화티탄을 유발 및 막자사발을 이용하여 고르게 혼합/교반하여 상기 혼합물을 제조할 수 있다.As described above, rutile titanium dioxide can be used as the inorganic ultraviolet scattering agent. For example, the mixture may be prepared by inducing the graphene quantum dot powder and rutile titanium dioxide and mixing / stirring evenly using a mortar and pestle.
단계 S30에서, 상기 혼합물을 열처리하여 복합 안료를 형성할 수 있다.In step S30, the mixture may be heat treated to form a composite pigment.
예시적인 실시예들에 따르면, 약 100℃ 내지 약 200℃의 온도에서 상기 혼합물을 수분 내지 수백분 동안 가열하여 상기 그래핀 양자점 분말 및 금홍석 이산화티탄이 고르게 분포되어 실질적으로 균일상으로 형성된 복합 안료가 제조될 수 있다. 상기 열처리에 의해 상기 복합 안료들에 포함된 상기 그래핀 양자점 분말 및 금홍석 이산화티탄의 결정 구조가 안정화될 수 있다. 일부 실시예들에 있어서, 상기 열처리는 약 150℃ 내지 약 200℃의 온도에서 수행될 수 있다.According to exemplary embodiments, the composite pigment formed by heating the mixture at a temperature of about 100 ° C. to about 200 ° C. for several minutes to several hundred minutes to uniformly distribute the graphene quantum dot powder and rutile titanium dioxide to form a substantially uniform phase. Can be prepared. By the heat treatment, the crystal structures of the graphene quantum dot powder and rutile titanium dioxide included in the composite pigments may be stabilized. In some embodiments, the heat treatment may be performed at a temperature of about 150 ° C to about 200 ° C.
이후, 단계 S40에서, 상기 복합 안료에 유기 자외선 흡수제 및 에멀젼을 혼합하여 예시적인 실시예들에 따른 화장료 조성물이 제조될 수 있다.Thereafter, in step S40, the cosmetic composition according to the exemplary embodiments may be prepared by mixing the organic UV absorber and the emulsion in the composite pigment.
상술한 바와 같이, 상기 유기 자외선 흡수제로서 에틸헥실 메톡시신나메이트와 같은 UVB 영역 자외선 흡수 기능을 갖는 유기 화합물을 사용할 수 있다.As described above, an organic compound having a UVB region ultraviolet absorbing function such as ethylhexyl methoxycinnamate can be used as the organic ultraviolet absorbent.
일부 실시예들에 따르면, 제조된 상기 화장료 조성물은 총 중량 대비 약 0.5 증량% 내지 약 5 중량%의 상기 그래핀 양자점, 약 5 중량% 내지 약 10 중량%의 상기 무기 자외선 산란제, 약 3 내지 약 7.5 중량%의 상기 유기 자외선 흡수제, 및 약 78 중량% 내지 약 91 중량%의 상기 에멀젼을 포함할 수 있다.According to some embodiments, the prepared cosmetic composition comprises about 0.5% to about 5% by weight of the graphene quantum dots, about 5% to about 10% by weight of the inorganic ultraviolet scattering agent, about 3 to about total weight About 7.5% by weight of the organic ultraviolet absorbent, and about 78% to about 91% by weight of the emulsion.
이하에서는, 구체적인 실험예를 참조로 예시적인 실시예들에 따른 화장료 조성물의 특성에 대해 보다 상세히 설명한다.Hereinafter, the characteristics of the cosmetic composition according to exemplary embodiments will be described in more detail with reference to specific experimental examples.
실험예 1: 그래핀 양자점 추가에 따른 자외선 흡수능 평가Experimental Example 1 Evaluation of UV Absorption Capacity by Adding Graphene Quantum Dots
도 1을 참조로 설명한 제조 방법에 따라, 하기의 표 1에 따른 조성을 갖는 조성물들을 제조하였다. 구체적으로, 무기 자외선 산란제로서 금홍석 이산화티탄(rutile TiO2)을 사용하였고, 유기 자외선 흡수제로서 2-에틸헥실 4-메톡시신나메이트(OMC)를 사용하였다. 그래핀 양자점은 GQD로 표시된다According to the preparation method described with reference to FIG. 1, compositions having compositions according to Table 1 below were prepared. Specifically, rutile titanium dioxide (rutile TiO 2 ) was used as an inorganic ultraviolet scattering agent, and 2-ethylhexyl 4-methoxycinnamate (OMC) was used as an organic ultraviolet absorber. Graphene quantum dots are represented by GQD
Figure PCTKR2015013715-appb-T000001
Figure PCTKR2015013715-appb-T000001
도 3은 실험예 1에 따른 조성물들(표 1의 조성물들)을 사용하여 자외선 흡수능을 측정한 UV/VIS 그래프이다.FIG. 3 is a UV / VIS graph of measuring ultraviolet absorbance using the compositions according to Experimental Example 1 (compositions in Table 1). FIG.
표 1 및 도 3을 참조하면, OMC를 포함한 조성물 2의 경우 약 320 nm 내지 약 340 nm 영역의 UV를 흡수하며, 조성물 6과 같이 그래핀 양자점이 추가됨에 따라 흡수의 세기가 보다 강해짐을 알 수 있다. 따라서, 상기 그래핀 양자점이 자외선 흡수 강화제로서 작용함을 알 수 있다.Referring to Table 1 and FIG. 3, the composition 2 including the OMC absorbs UV in the region of about 320 nm to about 340 nm, and the intensity of absorption becomes stronger as graphene quantum dots are added as in composition 6. have. Therefore, it can be seen that the graphene quantum dot acts as an ultraviolet absorption enhancer.
한편, OMC 및 TiO2가 함께 포함된 조성물 5의 경우 보다 넓은 파장 범위에서 UV 흡수능이 나타났으며, 조성물 8과 같이 그래핀 양자점이 추가됨에 따라 흡수 파장 영역 및 흡수의 세기가 보다 강화됨을 알 수 있다.Meanwhile, in the case of the composition 5 including OMC and TiO 2 , UV absorbing ability was shown in a wider wavelength range, and as the graphene quantum dots were added as in composition 8, the absorption wavelength region and the intensity of absorption were enhanced. have.
따라서, TiO2의 첨가에 따라 흡수되는 파장의 범위가 보다 확대될 수 있으며, 그래핀 양자점이 첨가되면서 흡수의 세기가 강화됨을 예측할 수 있다.Therefore, the range of wavelengths absorbed by the addition of TiO 2 can be further expanded, and it can be predicted that the intensity of absorption is enhanced as graphene quantum dots are added.
실험예 2: 그래핀 양자점 함량에 따른 자외선 흡수능 평가Experimental Example 2: Evaluation of UV Absorption Capacity According to Graphene Quantum Dot Content
도 1 및 실험예 1을 참조로 설명한 제조 방법에 따라, 하기의 표 2에 따른 조성을 갖는 조성물들을 제조하였다. According to the preparation method described with reference to FIG. 1 and Experimental Example 1, compositions having compositions according to Table 2 were prepared.
Figure PCTKR2015013715-appb-T000002
Figure PCTKR2015013715-appb-T000002
도 4는 실험예 2에 따른 조성물들(표 2의 조성물들)을 사용하여 자외선 흡수능을 측정한 UV/VIS 그래프이다.FIG. 4 is a UV / VIS graph of measuring ultraviolet absorbing capacity using the compositions according to Experimental Example 2 (compositions in Table 2). FIG.
표 2 및 도 4를 참조하면, 조성물 2에서 그래핀 양자점이 추가됨에 따라(조성물 3) 전체적으로 UV 흡수 세기가 증가하였으며, 특히 약 340 nm 이상의 범위에서 이러한 경향이 확인되었다. 또한, 그래핀 양자점이 더욱 증가됨에 따라(조성물 4) UV 흡수 세기가 추가적으로 증가되었다.Referring to Table 2 and FIG. 4, as graphene quantum dots were added in Composition 2 (composition 3), the overall UV absorption intensity increased, particularly in the range of about 340 nm or more. In addition, as the graphene quantum dots were further increased (composition 4), the UV absorption intensity was further increased.
실험예 3: 그래핀 양자점이 첨가된 스킨 토너의 자외선 흡수능 평가Experimental Example 3: Evaluation of UV Absorption Capacity of Skin Toner Added with Graphene Quantum Dots
상업적으로 시판되는 스킨 토너 제품에 그래핀 양자점을 아래의 표 3에 따라 첨가하여 자외선 흡수 특성을 평가하였다. Graphene quantum dots were added to commercially available skin toner products according to Table 3 below to evaluate ultraviolet absorption characteristics.
Figure PCTKR2015013715-appb-T000003
Figure PCTKR2015013715-appb-T000003
도 5는 실험예 3에 따른 스킨 토너를 사용하여 자외선 흡수능을 측정한 UV/VIS 그래프이다.5 is a UV / VIS graph of measuring ultraviolet absorbing ability using a skin toner according to Experimental Example 3. FIG.
표 3 및 도 5를 참조하면, 일반 스킨 토너는 약 300 nm 이상의 파장 범위에서는 실질적으로 흡수능을 보이지 않으나, 그래핀 양자점의 양이 증가함에 따라 약 300 nm 이상의 파장의 UV 영역에서 흡수 세기가 증가함을 알 수 있다.Referring to Table 3 and FIG. 5, the general skin toner does not substantially exhibit absorption in the wavelength range of about 300 nm or more, but the absorption intensity increases in the UV region of the wavelength of about 300 nm or more as the amount of graphene quantum dots increases. It can be seen.
따라서, 자외선 차단제 뿐만 아니라 일반 화장료 제품에도 자외선 차단 기능을 부여하기 위해 그래핀 양자점을 첨가할 수 있음을 확인할 수 있다.Therefore, it can be seen that graphene quantum dots can be added to give a sunscreen function to not only a sunscreen but also a general cosmetic product.
도 6은 예시적인 실시예들에 따른 화장료 조성물의 발색을 비교하기 위한 사진들이다. 구체적으로 도 6은 실험예 2의 조성물 2, 조성물 3 및 조성물 4(표 2 참조)의 발색을 나타내는 사진들이다.6 is a photograph for comparing color development of a cosmetic composition according to exemplary embodiments. Specifically, Figure 6 is a photograph showing the color development of Composition 2, Composition 3 and Composition 4 (see Table 2) of Experimental Example 2.
도 6을 참조하면, 에멀젼, OMC 및 이산화티탄만을 포함하는 조성물 2의 경우 백색을 나타내나, 그래핀 양자점이 추가되면서 피부색에 가까운 색상으로 변화함을 확인할 수 있다.Referring to FIG. 6, in the case of the composition 2 including the emulsion, OMC, and titanium dioxide only, white is shown, but it can be confirmed that the graphene quantum dot is changed to a color close to the skin color.
도 7은 예시적인 실시예들에 따른 화장료 조성물의 피부 발림성을 나타내는 사진들이다. 구체적으로, 도 7은 실험예 1의 조성물 8(표 1 참조)을 피부에 도포하는 과정을 나타내는 사진들이다.7 is a photograph showing skin spreadability of a cosmetic composition according to exemplary embodiments. Specifically, Figure 7 is a photograph showing a process of applying the composition 8 (see Table 1) of Experimental Example 1 to the skin.
도 7을 참조하면, 그래핀 양자점을 포함하는 예시적인 실시예들에 따른 자외선 차단제는 백탁 현상, 들뜸 현상 없이 실질적으로 피부색과 동일한 색상으로 도포됨을 확인할 수 있다.Referring to FIG. 7, it can be seen that the sunscreen according to the exemplary embodiments including the graphene quantum dots is applied in substantially the same color as the skin color without the cloudiness and the lifting phenomenon.
도 8은 예시적인 실시예들에 따른 화장료 조성물의 피부 안정성을 나타내는 사진들이다. 구체적으로, 도 8은 실험예 2의 조성물 4(표 2 참조)을 피부에 적용시킨 후 24시간 이후에 촬영된 사진을 포함하고 있다.8 is a photograph showing skin stability of a cosmetic composition according to exemplary embodiments. Specifically, FIG. 8 includes photographs taken 24 hours after applying Composition 4 (see Table 2) of Experimental Example 2 to the skin.
도 8을 참조하면, 그래핀 양자점을 포함하는 예시적인 실시예들에 따른 자외선 차단제를 적용 후, 장시간이 지난 경우에도 두드러기, 피부 변색 등과 같은 부작용이 관찰되지 않았다.Referring to FIG. 8, even after a long time after application of the sunscreen according to the exemplary embodiments including graphene quantum dots, no side effects such as hives and skin discoloration were observed.
전술한 예시적인 실시예들에 따른 화장료 조성물은 그래핀 양자점을 포함하며, 향상된 피부 친화도, 적용성을 가지며 자외선 차단 기능성을 보유할 수 있다. 상기 화장료 조성물은 자외선 차단제 뿐만 아니라 자외선 차단성이 부가된 스킨, 로션 등 다양한 화장료 제품으로 제공될 수 있다.The cosmetic composition according to the above-described exemplary embodiments includes graphene quantum dots, and may have improved skin affinity, applicability, and retain sunscreen functionality. The cosmetic composition may be provided in various cosmetic products such as skin, lotion and the like with sunscreen as well as sunscreen.
이상에서는 본 발명의 실시예들을 참조하여 설명하였지만, 해당 기술 분야의 숙련된 당업자는 하기의 특허 청구의 범위에 기재된 본 발명의 사상 및 영역으로부터 벗어나지 않는 범위 내에서 본 발명을 다양하게 수정 및 변경시킬 수 있음을 이해할 수 있을 것이다.Although the above has been described with reference to the embodiments of the present invention, those skilled in the art will be able to variously modify and change the present invention without departing from the spirit and scope of the present invention as set forth in the claims below. It will be appreciated.

Claims (11)

  1. 그래핀 양자점(Graphene Quantum Dots: GQD)을 포함하며 자외선 차단 기능을 갖는 화장료 조성물.A cosmetic composition comprising graphene quantum dots (GQD) and having a sunscreen function.
  2. 제1항에 있어서, 상기 조성물은 상기 그래핀 양자점, 무기 자외선 산란제, 유기 자외선 흡수제 및 에멀젼을 포함하는 화장료 조성물.The cosmetic composition of claim 1, wherein the composition comprises the graphene quantum dots, an inorganic ultraviolet scatterer, an organic ultraviolet absorber, and an emulsion.
  3. 제2항에 있어서, 상기 조성물은 총 중량 대비 0.5 중량% 내지 5 중량%의 상기 그래핀 양자점, 5 중량% 내지 10 중량%의 상기 무기 자외선 산란제, 3 내지 7.5 중량%의 상기 유기 자외선 흡수제, 및 78 중량% 내지 91 중량%의 상기 에멀젼을 포함하는 화장료 조성물.According to claim 2, wherein the composition is 0.5% to 5% by weight of the graphene quantum dots, 5% to 10% by weight of the inorganic ultraviolet scattering agent, 3 to 7.5% by weight of the organic ultraviolet absorber, And 78 wt% to 91 wt% of the emulsion.
  4. 제2항에 있어서, 상기 무기 자외선 산란제는 금홍석(rutile) 이산화티탄을 포함하는 화장료 조성물.The cosmetic composition of claim 2, wherein the inorganic ultraviolet scattering agent comprises rutile titanium dioxide.
  5. 제2항에 있어서, 상기 유기 자외선 흡수제는 에틸헥실 메톡시신나메이트, 에틸헥실살리실레이트, 4-메틸벤질리덴캠퍼, 이소아밀 p-메톡시신나메이트, 옥토크릴렌, 페닐벤즈이미다졸설포닉산, 호모살레이트, 시녹세이트, 에틸헥실트리아존, 폴리실리콘-15, 티이에이-살리실레이트, 팝바(PABA), 에틸헥실디메틸파바 및 글리세릴파바로 구성된 그룹에서 선택된 적어도 하나를 포함하는 화장료 조성물.The method of claim 2, wherein the organic ultraviolet absorber is ethylhexyl methoxycinnamate, ethylhexyl salicylate, 4-methylbenzylidene camphor, isoamyl p-methoxycinnamate, octocrylene, phenylbenzimidazole sulfonic acid Cosmetic composition comprising at least one selected from the group consisting of homosalate, synoxate, ethylhexyltrizone, polysilicone-15, tie-salicylate, popbar (PABA), ethylhexyldimethylpava and glyceryl pava.
  6. 그래핀 양자점 분말을 준비하는 단계;Preparing a graphene quantum dot powder;
    상기 그래핀 양자점 분말 및 무기 자외선 산란제의 혼합물을 제조하는 단계;Preparing a mixture of the graphene quantum dot powder and an inorganic ultraviolet scattering agent;
    상기 혼합물을 열처리하여 복합 안료를 형성하는 단계; 및Heat treating the mixture to form a composite pigment; And
    상기 복합 안료에 유기 자외선 흡수제 및 에멀젼을 혼합하는 단계를 포함하는 자외선 차단제의 제조 방법Method for producing a sunscreen comprising the step of mixing an organic UV absorber and an emulsion in the composite pigment
  7. 제6항에 있어서, 상기 그래핀 양자점 분말을 준비하는 단계는 금속 이온이 그래파이트 층에 삽입된 그래파이트 층간 화합물로부터 금속 이온을 제거하여 그래핀 양자점 수분산체를 제조하는 단계를 포함하는 자외선 차단제의 제조 방법.The method of claim 6, wherein preparing the graphene quantum dot powder includes preparing a graphene quantum dot water dispersion by removing metal ions from a graphite interlayer compound in which metal ions are inserted into the graphite layer. .
  8. 제7항에 있어서, 상기 그래핀 양자점 분말을 준비하는 단계는 상기 그래핀 양자점 수분산체를 100℃ 내지 130℃의 온도에서 건조시키는 단계를 더 포함하는 자외선 차단제의 제조 방법.8. The method of claim 7, wherein preparing the graphene quantum dot powder further comprises drying the graphene quantum dot water dispersion at a temperature of 100 ° C. to 130 ° C. 9.
  9. 제6항에 있어서, 상기 혼합물을 열처리하는 단계는 100℃ 내지 200℃의 온도에서 수행되는 자외선 차단제의 제조 방법.The method of claim 6, wherein the heat treatment of the mixture is performed at a temperature of 100 ° C. to 200 ° C. 8.
  10. 제6항에 있어서, 상기 무기 자외선 산란제 및 상기 유기 자외선 흡수제로서 각각 금홍석 이산화티탄 및 에틸헥실 메톡시신나메이트를 사용하는 자외선 차단제의 제조 방법.The method for producing a sunscreen according to claim 6, wherein rutile titanium dioxide and ethylhexyl methoxycinnamate are used as the inorganic ultraviolet scattering agent and the organic ultraviolet absorber, respectively.
  11. 제6항에 있어서, 상기 자외선 차단제의 총 중량 대비 0.5 중량% 내지 5 중량%의 상기 그래핀 양자점 분말, 5 중량% 내지 10 중량%의 상기 무기 자외선 산란제, 3 내지 7.5 중량%의 상기 유기 자외선 흡수제, 및 78 중량% 내지 91 중량%의 상기 에멀젼이 조합되는 자외선 차단제의 제조 방법.According to claim 6, 0.5 to 5% by weight of the graphene quantum dot powder, 5 to 10% by weight of the inorganic ultraviolet scattering agent, 3 to 7.5% by weight of the organic ultraviolet ray relative to the total weight of the sunscreen A method of making a sunscreen comprising a water absorbent and 78% to 91% by weight of said emulsion.
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