WO2017003149A1 - Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same - Google Patents

Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same Download PDF

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Publication number
WO2017003149A1
WO2017003149A1 PCT/KR2016/006882 KR2016006882W WO2017003149A1 WO 2017003149 A1 WO2017003149 A1 WO 2017003149A1 KR 2016006882 W KR2016006882 W KR 2016006882W WO 2017003149 A1 WO2017003149 A1 WO 2017003149A1
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Prior art keywords
powder
jade
composite powder
impregnated
poly
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PCT/KR2016/006882
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French (fr)
Korean (ko)
Inventor
이현석
백동현
조가영
김형준
정해진
장동혁
김용진
권이경
이존환
최성욱
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(주)아모레퍼시픽
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Priority claimed from KR1020160080232A external-priority patent/KR102116545B1/en
Application filed by (주)아모레퍼시픽 filed Critical (주)아모레퍼시픽
Priority to EP16818182.4A priority Critical patent/EP3318243B1/en
Priority to JP2017559068A priority patent/JP6796082B2/en
Priority to CN201680035773.0A priority patent/CN108040466B/en
Priority to US15/576,125 priority patent/US10238583B2/en
Publication of WO2017003149A1 publication Critical patent/WO2017003149A1/en
Priority to US16/271,399 priority patent/US10624822B2/en

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin

Definitions

  • the present invention relates to a composite powder of jade powder and a porous polymer, and more particularly, jade powder particles prepared by spraying a dispersion in which the jade powder is dispersed in a solution in which the porous polymer is dissolved in a single step is porous. It relates to a composite powder (Jade sphere) impregnated in a polymer, a cosmetic composition containing the same and a method for producing the same.
  • a powder particle (A) serving as a mother is produced, and then the surface is coated with other powder particles (B).
  • the method of manufacturing is common, but this technique has a problem that the procedure of the two-step manufacturing process is not only complicated, and the characteristics of each of the two or more powders are not properly exhibited.
  • the composite powder is prepared by applying the spray drying process and the electrospray process, the powder powder (B) is uniformly dispersed and penetrated between the inside of the powder particles (A), which is a parent, and thus the granulated powder is collected in a single process. There are differences that can be made.
  • Spray drying technology is a method of spraying a substance in a dissolved state composed of raw material powder, a solvent, a binder, or the like with a spraying unit such as a nozzle, a rotating disk, or the like to instantly dry with hot air. More specifically, spray drying increases the surface area by increasing the surface area by atomizing liquid raw materials such as solution, emulsion, dispersion, suspension and slurry. As a technique of immediately drying in direct contact with hot air streams to obtain a powdery product directly from a liquid raw material, dry powdering is performed in a single step.
  • Korean Patent Publication No. 2002-0091779 in order to prepare a ceramic powder having excellent dispersibility and filling ability to a resin, a spray drying process of spraying a slurry containing raw material powder to form droplets and then drying to obtain ceramic granule powder is carried out.
  • Korean Patent Publication No. 2014-0110439 discloses a method for producing spherical boron nitride powder having a certain particle size using a spray drying method.
  • electro-spraying technology is a method of preparing microparticles by injecting a polymer solution having a certain degree of electrical conductivity and viscosity into a capillary, and then applying an electrostatic force.
  • a polymer solution having a certain degree of electrical conductivity and viscosity into a capillary, and then applying an electrostatic force.
  • gravity and the surface tension of the polymer solution are balanced at the end of the nozzle to form a hemispherical drop.
  • charge or dipole orientation is induced at the interface of the air layer and the solution on the surface of the hemispherical droplet, and a force opposite to the surface tension is generated by the repulsive force of the electric or dipole.
  • the hemispherical surface at the nozzle tip extends into a conical surface called the Taylor cone, and the charged polymer solution is released from the Taylor cone when the repulsion of the electric or dipoles exceeds the force to overcome the surface tension.
  • the polymer solution having a low viscosity is sprayed into fine droplets due to the surface tension.
  • Electrospraying like spray drying, also powders in a single step.
  • Electrospray is easy to manufacture due to the simple form and structure of the device, and the particles produced can have a monodispersion distribution and are useful for producing particles of various sizes ranging from tens of nanometers to hundreds of micrometers. It has been widely used in the fields such as coating of ethylene, mass spectrometry and structural analysis of proteins and biochemicals.
  • Korean Patent No. 10-1471280 in order to improve the absorption rate of poorly soluble drugs in the body, after dissolving a poorly soluble substance in an organic solvent, It is known to produce ultrafine, poorly soluble material nanopowders by electrospraying a poorly soluble material solution prepared by dispersing a surfactant.
  • the present inventors pay attention to the fact that the spray drying and electrospraying technology can granulate the liquid raw material in a single process, the particle size of the granules can be easily controlled, and spherical particles can be produced.
  • the present invention leads to a technique of evenly impregnating amorphous coarse jade powder particles into a porous polymer.
  • Jade powder particles are known to be included in the cosmetic composition for the purpose of skin moisturizing or whitening effect, etc., but when formulated and applied to the skin, the surface of the jade powder is rough, thereby reducing the feeling of use. In addition, cloudiness occurs due to agglomeration of the jade powder particles, and when the makeup cosmetics are included, the whiteness is reduced due to the turbid saturation of the jade itself.
  • a composite powder hereinafter, jade impregnated powder, Jade sphere
  • jade powder particles are uniformly impregnated in a porous polymer
  • a cosmetic composition containing the same a method of preparing the same.
  • the particles of the jade powder is 10000 ⁇ 20000 mesh, it may be impregnated with 10 to 90% by weight, preferably 50 to 90% by weight relative to the total weight of the composite powder.
  • the porous polymer is polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)] and poly It is preferably selected from the group -L-lactic acid [PLLA: Poly- (L-Lactic Acid)].
  • the jade impregnated powder in which the jade powder particles of the present invention are evenly impregnated with the porous polymer is formulated as a cosmetic composition
  • the blue powder blocking effect of the jade powder and sebum adsorption capacity of the porous polymer are higher than those of the cosmetic containing the jade powder alone.
  • the makeup persistence is improved.
  • the spreadability, spreadability and softness is improved, the aggregation phenomenon is eliminated to prevent turbidity and whiteness is improved.
  • SEM scanning electron microscope
  • Figure 2 is a scanning electron microscope (SEM) image
  • (a) is an image of the surface of the jade impregnated powder of the present invention
  • (b) is an image of the cut surface.
  • Figure 7 is the result of the percent reflectance (%) test of the visible light region of the formulation containing the jade impregnated powder of the present invention.
  • the present invention relates to a composite powder of jade powder and a porous polymer, and more particularly, after the jade powder is dispersed in a solution in which the porous polymer is dissolved, a single process of spray drying or electrospraying
  • the present invention relates to a composite powder (hereinafter, jade impregnated powder, Jade sphere) in which impregnation of jade powder particles is uniformly impregnated into a porous polymer by spraying a dispersion solution (One-step), a cosmetic composition comprising the same, and a manufacturing method thereof.
  • the term 'impregnation' means a state in which other powder particles are uniformly dispersed and penetrated between the inside of the powder particles to be a mother, and in the past, the surface of the powder particles is coated with other powder particles or supported by the pores of the powder surface. It is different from.
  • the present invention will be described in detail.
  • Jade is generally classified into jadeite and nephrite jade, and jadeite, unlike sodium and aluminum in jadeite, has three minerals that are beneficial to the human body. That is, calcium (Ca), iron (Fe), and magnesium (Mg) are the main components. Therefore, the jade powder which can be applied to the present invention is not limited in kind, but more preferably uses jade.
  • the Chuncheon Jade used in the present invention is a kind of purgatory, which is a high-quality nephrite Jade produced in Chuncheon, Gangwon-do, and is a variant mineral of Tremolite and Actinolite of Amphibole group. It is a mineral with dense, fine, tough wool texture.
  • jade is used by grinding and processing into a powder
  • the particle size distribution of the particles of the jade powder that can be used as a cosmetic composition in the present invention is preferably processed to be 10000 ⁇ 20000 mesh. If the amount exceeds 20000 mesh, the effect of the jade powder is inadequate, and if it is less than 10000 mesh, the surface of the spherical jade impregnated powder becomes rough and the use of the skin is deteriorated.
  • the porous polymer impregnated with the jade powder particles is a spherical powder having oil absorption and sebum adsorption, for example, polymethyl methacrylate (PMMA: poly (methyl methacrylate)), but in addition to poly Vinyl pyrrolidone [PVP: poly (vinyl pyrrolidone)], polycaprolactone [PCL: poly (caprolactone)] and poly-L-lactic acid [PLLA: Poly (L-Lactic Acid)]
  • PMMA poly (methyl methacrylate)
  • PVP poly (vinyl pyrrolidone)
  • PCL poly (caprolactone)
  • PLLA Poly (L-Lactic Acid)
  • the porous polymer is spherical in shape, it is easy to mix when manufacturing various cosmetic formulations, and the spherical fine particles are rolled on the skin, thereby providing excellent feeling of application such as spreadability when applying the skin and having characteristics of a spherical surface. Due to light scattering prevention effect and improvement of makeup persistence, it is commonly used in basic cosmetics for sebum control and makeup products for skin tone correction.
  • the content of the jade powder may be impregnated with 10 to 90% by weight relative to the total jade impregnated powder weight, more preferably 50 to It may be impregnated at 90% by weight.
  • the average particle diameter of the jade impregnated powder may be 5 ⁇ 20 ⁇ m. This feature is suitable for application as a cosmetic in terms of effects due to jade powder and usability in skin application.
  • the present invention provides a jade impregnated powder by spray drying or electrospraying a porous polymer dispersion in which jade powder is dispersed in a porous polymer solution to prepare jade impregnated powder in one step. It is possible to impregnate the polymer evenly. At this time, it is preferable to exclude the emulsifier for the super water-repellent implementation of the porous polymer.
  • porous powders produced by the same method as emulsion polymerization have inevitable use of emulsifiers, which makes it impossible to completely remove the emulsifiers in the future, causing skin irritation, and drying skin because it absorbs moisture as well as skin oils. There was this.
  • the porous polymer solution dissolves polymethylmethacrylate (PMMA) in a mixed solvent of dichloromethane (DCM) and hexanol, and the mixing ratio (weight ratio) of dichloromethane (DCM) and hexanol (Hexanol) is 9 : 1 to 7: 3 can be selected. Since hexanol plays a role of forming pores of porous polymers, if the proportion of hexanol is less than 10% by weight of the total solvent, the pore size is too small. .
  • the jade impregnated powder can control the pore characteristics according to the manufacturing process conditions.
  • Controllable pore characteristics include average pore size, porosity and total pore area.
  • the average pore size may be 15 to 800 nm, more preferably 250 to 600 nm, and the porosity may be 40 to 85%, and more preferably 50 to 75%.
  • the total pore area may be 1 to 100 m 2 / g, more preferably 5 to 80 m 2 / g.
  • Jade impregnated powder having such a feature may cause an oil absorption increase effect due to its pore size and porosity.
  • the oil absorption amount can be explained by the intrusion volume of mercury described later.
  • the mercury penetration volume of the jade impregnated powder according to the invention is measured in the range of 0.5 to 5 cm 3 / g, which can be regarded as oil absorption with a high confidence level.
  • Pore Channel is formed due to the structure of Micro + Meso + Macro, which is much more advantageous for oil absorption by capillary action.
  • the jade impregnated powder can be applied as a cosmetic composition, wherein the jade impregnated powder is preferably included 0.1 to 5.0% by weight relative to the total cosmetic weight.
  • the content of the jade powder is excessive, not only the inherent properties and softness of the cosmetic raw material and the feeling of use when applying the skin, but also because the jade is expensive, the product cost rises.
  • the content of the jade powder is small, the effect due to the jade powder can not be expected is not preferable.
  • cosmetic composition of the present invention in addition to jade powder, skin wrinkle improvement, skin whitening improvement, skin elasticity improvement, facial sagging improvement, skin moisturization improvement, skin gloss improvement, skin aging prevention (for example, skin wrinkle formation by photo aging and skin curing) Inhibition), functional additives for skin improvement such as dark circle improvement and skin exfoliation, or functional additives for blocking UV rays, or ingredients included in a general cosmetic composition may be further included.
  • the functional additive for improving the skin may include a component selected from the group consisting of water-soluble vitamins, fat-soluble vitamins, polymer peptides, polymer polysaccharides, sphingolipids, natural extracts and fermented substances.
  • a functional additive for UV protection it is possible to further include inorganic powders such as titanium dioxide (TiO 2 : Titanium dioxide), zinc oxide (ZnO: Zinc oxide), cerium oxide (CeO 2 : Cerium oxide).
  • titanium dioxide TiO 2 : Titanium dioxide
  • ZnO Zinc oxide
  • CeO 2 Cerium oxide
  • oils and fats In addition to the other components included, oils and fats, moisturizers, emollients, surfactants, organic and inorganic pigments, organic powders, ultraviolet absorbers, preservatives, fungicides, antioxidants, plant extracts, pH adjusters, alcohols, pigments, flavorings, blood circulation Accelerators, cooling agents, limiting agents, purified water, and the like, but is not limited thereto.
  • the cosmetic composition containing the jade impregnated powder may be any one of skin, lotion, cream, serum, emulsion, essence, powder, foundation, spray, sunscreen, mask pack, gel, more preferably mask pack, sheet pack. It may be formulated as a sleeping pack, wash off pack, peel off pack, and the like, but is not particularly limited in the formulation, and may be appropriately selected and changed as desired.
  • Example 1 To prepare the following Example 1 and Example 2, the following Table 1 was prepared.
  • Jade powder Chuncheon Jade
  • Oxane production Poly methyl methacrylate
  • DCM Dichloromethane anhydrous
  • Table 1 was prepared to prepare jade impregnated powder (hereinafter referred to as jade sphere) according to the following spray drying method.
  • Table 1 was prepared to prepare jade impregnated powder (hereinafter referred to as jade sphere) according to the following electrospray method.
  • Electrospray Electro Spraying
  • FIG. 1 is a scanning electron microscope (SEM) image of the jade powder of Comparative Example 1
  • Figure 2 is a jade impregnated powder of Example 1 in which the jade powder is impregnated evenly inside the polymethyl methacrylate (PMMA) particles of the porous polymer Scanning electron microscope (SEM) images of the surface (a) and the cut surface (b) of.
  • PMMA polymethyl methacrylate
  • SEM scanning electron microscope
  • FIG. 3 is an image quantitatively and qualitatively analyzed by an energy dispersive X-ray (EDX) analyzer, and each element included in the jade impregnated powder (a) and the jade impregnated powder of Example 1 are represented as points.
  • EDX energy dispersive X-ray
  • the jade powder of Comparative Example 1 and the jade-impregnated powder of Example 1 exhibited higher reflectances in the visible light band (380 to 710 nm), but in particular, the jade of Example 1 from a longer wavelength range than 380 nm.
  • the impregnated powder showed higher reflectance than the jade powder of Comparative Example 1.
  • the difference in reflectance is large, and it can be seen that the jade impregnated powder of Example 1 exhibits a higher blue light blocking rate than the jade powder of Comparative Example 1.
  • Whiteness is a numerical value representing the whiteness of a color in one dimension, and the whiteness index was derived through the following formula based on the XYZ color difference value of the entire visible light region in the reflectance test.
  • WI Y + 800 (x n -x) + 1700 (y n -y) ⁇ CIE Whiteness>
  • the whiteness of the jade impregnated powder of Example 1 was 94%, and the whiteness of the jade powder of Comparative Example 1 was 10% improved from the whiteness of 84%.
  • 'Total Intrusion Volume' is the amount of mercury penetrated per gram
  • 'Total Pore Area' is the total pore area represented by the cylindrical area
  • 'Average Pore Diameter' is the average value of the total pore size
  • the oil absorption of the jade impregnated powder of Example 1 was 1.7 mL / g, which is very similar to the total intrusion volume 1.6797 mL / g of mercury in the above 3. porosity measurement test. It is a result demonstrating the reliability of the measurement result, and it can also be confirmed that the oil absorption amount increased by at least 5 times compared to the jade powder. This is an effect generated by maintaining a large pore size and a high porosity, although the jade impregnated powder of Example 1 contains 50 wt% of jade powder.
  • Example 1 The following jade impregnated powder prepared in Example 1 was formulated in an emulsion form (mask pack) according to the composition (% by weight) described in the following [Table 5] to perform an itemized test.
  • Comparative Formulation Examples 1, 2 and Formulation Example 1 of the present invention 30 women aged 25 to 35 years old were used twice a day for one month, and then adhesiveness, spreadability, softness, particle aggregation, and cosmetic sustainability were used. By comparing the items to the usability as a cosmetic was evaluated to 1 to 5 points, the results are shown in the following [Table 6].
  • the jade impregnated powder of the present invention showed excellent results in the softness caused by the spherical shape and the cosmetic persistence caused by sebum absorption due to high porosity. In addition, it was confirmed that the particle aggregation, which was the biggest problem of Comparative Formulation Example 2 including jade powder, was greatly improved to prevent cloudiness.
  • Whiteness of the formulation is a numerical value representing the whiteness of the color in one dimension, and the whiteness index was derived through the following formula based on the XYZ color difference value of the entire visible light region in the reflectance test of the formulation.
  • WI Y + 800 (x n -x) + 1700 (y n -y) ⁇ CIE Whiteness>
  • Example 9 The following contained 5.0 wt% of the jade impregnated powder prepared in Example 1, and prepared a massage cream in a conventional manner according to the composition (wt%) shown in the following [Table 9].

Abstract

The present invention relates to a composite powder of jade powder and a porous polymer, and more specifically relates to a composite powder (jade sphere) in which jade powder particles are impregnated in a porous polymer, the composite powder being produced by spraying, in one step, a dispersion in which jade powder has been dispersed in a solution that dissolves porous polymers, and to a cosmetic composition containing the composite powder, and to a manufacturing method for the composite powder.

Description

옥 분말 입자가 다공성 고분자에 함침된 복합분체, 이를 함유하는 화장료 조성물 및 이의 제조방법Composite powder impregnated with the jade powder particles in a porous polymer, a cosmetic composition containing the same, and a preparation method thereof
본 출원은 2015년 6월 30일자 한국 특허 출원 제10-2015-0092868호와 2016년 6월 27일자 한국 특허 출원 제10-2016-0080232호에 기초한 우선권의 이익을 주장하며, 해당 한국 특허 출원의 문헌에 개시된 모든 내용은 본 명세서의 일부로서 포함한다.This application claims the benefit of priority based on Korean Patent Application No. 10-2015-0092868 dated June 30, 2015 and Korean Patent Application No. 10-2016-0080232 dated June 27, 2016. All content disclosed in the literature is included as part of this specification.
본 발명은 옥 분말과 다공성 고분자의 복합분체에 관한 것으로, 보다 상세하게는 다공성 고분자를 용해시킨 용액에 옥 분말을 분산시킨 분산액을 단일공정(One-step)으로 분무하여 제조되는 옥 분말 입자가 다공성 고분자에 함침된 복합분체(Jade sphere), 이를 함유하는 화장료 조성물 및 이의 제조방법에 관한 것이다.The present invention relates to a composite powder of jade powder and a porous polymer, and more particularly, jade powder particles prepared by spraying a dispersion in which the jade powder is dispersed in a solution in which the porous polymer is dissolved in a single step is porous. It relates to a composite powder (Jade sphere) impregnated in a polymer, a cosmetic composition containing the same and a method for producing the same.
유기분체와 무기분체의 결합체와 같이, 2종 이상의 분체가 결합된 복합분체 제조시, 모체가 되는 분체 입자(A)를 제조한 후, 그 표면을 다른 분체 입자(B)가 코팅하는 공정을 통하여 제조하는 방법이 일반적이나, 이러한 기술은 2단계 제조공정으로 절차가 복잡할 뿐만 아니라, 2종 이상의 분체 각각의 특성이 제대로 발휘되지 않는 문제점이 있었다. 반면 분말화 방법 중 분무 건조 공정과 전기 분무 공정을 적용하여 복합분체를 제조하게 되면, 모체가 되는 분체 입자(A) 내부 사이로 다른 분체 입자(B)가 고르게 분산되어 침투되면서 단일 공정으로 과립 분말을 제조할 수 있는 차이가 있다.When manufacturing a composite powder in which two or more powders are combined, such as a combination of an organic powder and an inorganic powder, a powder particle (A) serving as a mother is produced, and then the surface is coated with other powder particles (B). The method of manufacturing is common, but this technique has a problem that the procedure of the two-step manufacturing process is not only complicated, and the characteristics of each of the two or more powders are not properly exhibited. On the other hand, when the composite powder is prepared by applying the spray drying process and the electrospray process, the powder powder (B) is uniformly dispersed and penetrated between the inside of the powder particles (A), which is a parent, and thus the granulated powder is collected in a single process. There are differences that can be made.
분무 건조(Spray Drying) 기술은, 원료 분말, 용매 및 바인더 등에 의해 구성되는 용해 상태의 물질을 노즐이나 회전 디스크 등의 분무부에 의해 분무하여, 열풍으로 순간적으로 건조시키는 방법이다. 좀 더 구체적으로 설명하면, 분무 건조는 용액(Solution), 에멀젼(Emulsion), 분산액(Dispersion), 현탁액(Suspension), 슬러리(Slurry) 등의 액상원료를 미립화하여 표면적을 증가시켜 수열면적을 크게 한 후 열풍기류와 직접 접촉함에 따라 순간적으로 건조되어 액상원료로부터 곧바로 분립상의 제품을 얻는 기술로서, 건조 분말화가 단일 단계에서 이루어지는 특징이 있다.Spray drying technology is a method of spraying a substance in a dissolved state composed of raw material powder, a solvent, a binder, or the like with a spraying unit such as a nozzle, a rotating disk, or the like to instantly dry with hot air. More specifically, spray drying increases the surface area by increasing the surface area by atomizing liquid raw materials such as solution, emulsion, dispersion, suspension and slurry. As a technique of immediately drying in direct contact with hot air streams to obtain a powdery product directly from a liquid raw material, dry powdering is performed in a single step.
따라서 제품이 열에 접촉되는 시간이 수초 내로 이루어져 제품의 물성에 비교적 적은 영향을 미친다는 장점과 생산된 제품의 취급이 용이한 등의 이유로 파인 세라믹스, 분유, 의약품, 식품류, 염료 및 안료 등의 제조시, 천연추출물 등을 건조하고 과립을 얻기 위하여 광범위하게 사용되고 있다.Therefore, in the manufacture of fine ceramics, powdered milk, pharmaceuticals, foodstuffs, dyes and pigments due to the advantage that the product is in contact with heat within a few seconds, which has a relatively small influence on the physical properties of the product and the handling of the produced product is easy. It is widely used to dry natural extracts and to obtain granules.
한국공개특허 제2002-0091779호에는 수지에 대한 분산성, 충진성이 우수한 세라믹스 분말을 제조하기 위하여 원료 분체를 포함하는 슬러리를 분무하여 액적을 형성한 후 건조하여 세라믹스 과립분을 얻는 분무 건조 공정에 대해서 공지되어 있으며, 한국공개특허 제2014-0110439호에는 분무 건조 공법을 이용하여 일정 입도를 가지는 구형의 질화붕소 분말을 제조하는 방법이 공지되어 있다.In Korean Patent Publication No. 2002-0091779, in order to prepare a ceramic powder having excellent dispersibility and filling ability to a resin, a spray drying process of spraying a slurry containing raw material powder to form droplets and then drying to obtain ceramic granule powder is carried out. For example, Korean Patent Publication No. 2014-0110439 discloses a method for producing spherical boron nitride powder having a certain particle size using a spray drying method.
한편 전기 분무(Electro-Spraying) 기술은 어느 정도의 전기 전도도와 점도를 가지는 고분자 용액 등을 모세관에 주입시킨 후, 정전기력을 부과하여 미세입자를 제조하는 방법이다. 일반적으로 수직으로 위치한 노즐을 통해 고분자 용액을 분사시키면 노즐 끝에는 중력과 고분자 용액의 표면장력이 균형을 이루어 반구형 방울을 형성하며 매달리게 된다. 이때 전기장이 가해지면 이 반구형 방울 표면에 전하 또는 쌍극자 배향이 공기층과 용액의 계면에 유도되고, 이러한 전하나 쌍극자의 반발력으로 표면장력과 반대되는 힘이 발생된다. 따라서 노즐 끝의 반구형 표면은 테일러 원뿔(Taylor cone)이라 부르는 원추형 표면으로 늘어 나게 되고 전하나 쌍극자들의 반발력이 표면장력을 극복할 만한 힘 이상이 되면 하전된 고분자 용액이 테일러 원뿔에서부터 방출된다. 이때 점도가 낮은 고분자 용액의 경우에는 표면장력으로 인해 미세 방울로 분사되게 된다. 전기 분무 또한 분무 건조와 마찬가지로 분말화가 단일 단계에서 이루어진다.On the other hand, electro-spraying technology is a method of preparing microparticles by injecting a polymer solution having a certain degree of electrical conductivity and viscosity into a capillary, and then applying an electrostatic force. In general, when the polymer solution is sprayed through a vertically located nozzle, gravity and the surface tension of the polymer solution are balanced at the end of the nozzle to form a hemispherical drop. At this time, when an electric field is applied, charge or dipole orientation is induced at the interface of the air layer and the solution on the surface of the hemispherical droplet, and a force opposite to the surface tension is generated by the repulsive force of the electric or dipole. Thus, the hemispherical surface at the nozzle tip extends into a conical surface called the Taylor cone, and the charged polymer solution is released from the Taylor cone when the repulsion of the electric or dipoles exceeds the force to overcome the surface tension. In this case, the polymer solution having a low viscosity is sprayed into fine droplets due to the surface tension. Electrospraying, like spray drying, also powders in a single step.
전기 분무는 장치의 형태와 구조가 간단하여 제작이 용이하고 발생된 입자들이 단분산 분포를 가질 수 있을 뿐 아니라 수십 나노부터 수백 마이크로미터까지 다양한 크기의 입자를 제조하기에 유용하여 박막부착이나 금속표면에의 코팅, 단백질과 생화학 물질 등의 질량 분석이나 구조해석 등의 분야에 널리 이용되어 왔다.Electrospray is easy to manufacture due to the simple form and structure of the device, and the particles produced can have a monodispersion distribution and are useful for producing particles of various sizes ranging from tens of nanometers to hundreds of micrometers. It has been widely used in the fields such as coating of ethylene, mass spectrometry and structural analysis of proteins and biochemicals.
최근에는 약물 전달 분야에서 약물을 포함한 입자 생성에 적용하려는 연구가 진행되고 있으며, 한국등록특허 제10-1471280호에는 난용성 약물의 체내 흡수율을 향상시키기 위하여, 난용성 물질을 유기용매에 용해한 후, 계면활성제를 분산시켜 제조된 난용성 물질 용액을 전기 분무하여 초미립자 난용성 물질 나노분체를 제조하는 방법이 공지되어 있다.Recently, research is being conducted to apply to the production of particles including drugs in the field of drug delivery. In Korean Patent No. 10-1471280, in order to improve the absorption rate of poorly soluble drugs in the body, after dissolving a poorly soluble substance in an organic solvent, It is known to produce ultrafine, poorly soluble material nanopowders by electrospraying a poorly soluble material solution prepared by dispersing a surfactant.
본 발명자들은 상기 분무 건조 및 전기 분무 기술은 단일 공정으로 액상원료를 과립화할 수 있으며, 과립의 입도 조절이 용이할 뿐 아니라 구형의 입자를 제조할 수 있다는 점에 착안하여, 분무 건조 및 전기 분무 공정을 이용하여 다공성 고분자에 무정형의 거친 옥 분말 입자를 고르게 함침시키는 기술인 본 발명에 이르게 되었다.The present inventors pay attention to the fact that the spray drying and electrospraying technology can granulate the liquid raw material in a single process, the particle size of the granules can be easily controlled, and spherical particles can be produced. The present invention leads to a technique of evenly impregnating amorphous coarse jade powder particles into a porous polymer.
[선행문헌] 한국등록특허 제10-1015386호 "분무 건조기(Spray Dryer)"[Previous Document] Korean Patent No. 10-1015386 "Spray Dryer"
옥 분말 입자는 피부 보습이나 미백 효과 등을 목적으로 화장료 조성물에 포함되는 기술이 공지되어 있으나, 제형화하여 피부에 도포하게 되면, 그 표면이 거칠기 때문에 사용감을 저하시키게 된다. 또한 옥 분말 입자의 뭉침으로 인하여 백탁현상이 발생하고, 메이크업 화장료 포함 시 옥 자체의 탁한 채도로 인하여 백색도가 저하되는 문제점이 있었다.Jade powder particles are known to be included in the cosmetic composition for the purpose of skin moisturizing or whitening effect, etc., but when formulated and applied to the skin, the surface of the jade powder is rough, thereby reducing the feeling of use. In addition, cloudiness occurs due to agglomeration of the jade powder particles, and when the makeup cosmetics are included, the whiteness is reduced due to the turbid saturation of the jade itself.
이러한 문제점을 해결하기 위하여 본 발명에서는 다공성 고분자를 용해시킨 용액에 옥 분말을 분산시킨 후, 분무 건조(Spray Drying) 또는 전기 분무(Electro-Spraying)의 단일공정(One-step)으로 분산액을 분무함으로써 옥 분말 입자를 다공성 고분자에 고르게 함침(Impregnation)시킨 복합분체(이하 옥 함침 분체, Jade sphere), 이를 함유하는 화장료 조성물 및 이의 제조방법을 개시한다.In order to solve this problem, in the present invention, by dispersing jade powder in a solution in which the porous polymer is dissolved, by spraying the dispersion solution by one-step spray spraying or electro-spraying Disclosed is a composite powder (hereinafter, jade impregnated powder, Jade sphere) in which jade powder particles are uniformly impregnated in a porous polymer, a cosmetic composition containing the same, and a method of preparing the same.
상기 옥 분말의 입자는 10000 ~ 20000 mesh이며, 전체 복합분체 중량 대비 10 ~ 90 중량%, 바람직하게는 50 ~ 90 중량%로 함침될 수 있다. The particles of the jade powder is 10000 ~ 20000 mesh, it may be impregnated with 10 to 90% by weight, preferably 50 to 90% by weight relative to the total weight of the composite powder.
상기 다공성 고분자는 폴리메틸메타크릴레이트[PMMA: poly-(methyl methacrylate)], 폴리비닐피롤리돈[PVP: poly-(vinyl pyrrolidone)], 폴리카프로락톤[PCL: poly-(caprolactone)] 및 폴리-L-락틱산[PLLA: Poly-(L-Lactic Acid)] 군으로부터 선택되는 것이 바람직하다.The porous polymer is polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)] and poly It is preferably selected from the group -L-lactic acid [PLLA: Poly- (L-Lactic Acid)].
본 발명의 옥 분말 입자를 다공성 고분자에 고르게 함침시킨 옥 함침 분체(Jade sphere)를 화장료 조성물로서 제형화시키면, 옥 분말이 단독 함유된 화장료보다 옥 분말의 블루 라이트 차단 효과와 다공성 고분자의 피지 흡착력으로 인한 화장 지속성이 향상된다.When the jade impregnated powder (Jade sphere) in which the jade powder particles of the present invention are evenly impregnated with the porous polymer is formulated as a cosmetic composition, the blue powder blocking effect of the jade powder and sebum adsorption capacity of the porous polymer are higher than those of the cosmetic containing the jade powder alone. The makeup persistence is improved.
또한 거친 무정형의 옥 분말을 구형의 다공성 고분자 내부에 함침시킴으로써 발림성, 퍼짐성 및 부드러움성이 개선되고, 뭉침현상을 해소하여 백탁현상이 방지되며, 백색도가 개선되는 효과가 있다.In addition, by impregnating the coarse amorphous jade powder into the spherical porous polymer, the spreadability, spreadability and softness is improved, the aggregation phenomenon is eliminated to prevent turbidity and whiteness is improved.
도 1은 본 발명에 적용되는 옥 분말의 주사전자현미경(SEM) 이미지이다.1 is a scanning electron microscope (SEM) image of jade powder applied to the present invention.
도 2는 주사전자현미경(SEM) 이미지로서, (a)는 본 발명의 옥 함침 분체의 표면의 이미지이고, (b)는 절단면의 이미지이다.Figure 2 is a scanning electron microscope (SEM) image, (a) is an image of the surface of the jade impregnated powder of the present invention, (b) is an image of the cut surface.
도 3의 에너지 분산형 X선(EDX: Energy Dispersive X-ray) 분석장치로 정량 및 정성 분석한 이미지로서, (a)는 본 발명의 옥 함침 분체의 표면 이미지이고, (b)는 옥 함침 분체에 포함된 각 원소를 가시화한 이미지이다.Quantitative and qualitative analysis by the energy dispersive X-ray (EDX) analyzer of Figure 3, (a) is the surface image of the jade impregnated powder of the present invention, (b) is jade impregnated powder This is a visualized image of each element included in.
도 4는 본 발명의 옥 함침 분체의 가시광선 영역대별 반사율(%) 테스트 결과이다.4 is a test result of reflectance (%) of visible light region of jade impregnated powder according to the present invention.
도 5는 본 발명의 옥 함침 분체의 백색도(whiteness, %R) 테스트 결과이다.5 is a result of the whiteness (% R) test of the jade impregnated powder of the present invention.
도 6은 본 발명의 옥 함침 분체의 흡유량(mL/g) 테스트 결과이다.6 is a result of oil absorption (mL / g) test of jade impregnated powder of the present invention.
도 7은 본 발명의 옥 함침 분체를 포함하는 제형의 가시광선 영역대별 반사율(%) 테스트 결과이다. Figure 7 is the result of the percent reflectance (%) test of the visible light region of the formulation containing the jade impregnated powder of the present invention.
도 8은 본 발명의 옥 함침 분체를 포함하는 제형의 백색도(whiteness, %R) 테스트 결과이다.8 is a result of the whiteness (% R) test of the formulation containing the jade impregnated powder of the present invention.
본 발명은 옥 분말과 다공성 고분자의 복합분체에 관한 것으로, 보다 상세하게는 다공성 고분자를 용해시킨 용액에 옥 분말을 분산시킨 후, 분무 건조(Spray Drying) 또는 전기 분무(Electro-Spraying)의 단일공정(One-step)으로 분산액을 분무함으로써 옥 분말 입자를 다공성 고분자에 고르게 함침(Impregnation)시킨 복합분체(이하 옥 함침 분체, Jade sphere), 이를 포함하는 화장료 조성물 및 이의 제조방법에 관한 것이다. 본 발명에서 '함침'의 의미는 모체가 되는 분체 입자 내부 사이로 다른 분체 입자가 고르게 분산되어 침투된 상태를 의미하는 것으로 종래에 분체 입자 표면을 다른 분체 입자가 코팅하거나 분체 표면의 기공 사이로 담지된 형태와는 차이가 있다. 이하 본 발명을 상세히 설명한다.The present invention relates to a composite powder of jade powder and a porous polymer, and more particularly, after the jade powder is dispersed in a solution in which the porous polymer is dissolved, a single process of spray drying or electrospraying The present invention relates to a composite powder (hereinafter, jade impregnated powder, Jade sphere) in which impregnation of jade powder particles is uniformly impregnated into a porous polymer by spraying a dispersion solution (One-step), a cosmetic composition comprising the same, and a manufacturing method thereof. In the present invention, the term 'impregnation' means a state in which other powder particles are uniformly dispersed and penetrated between the inside of the powder particles to be a mother, and in the past, the surface of the powder particles is coated with other powder particles or supported by the pores of the powder surface. It is different from. Hereinafter, the present invention will be described in detail.
옥(Jade)Jade
일반적으로 옥(玉, Jade)은 경옥(Jadeite jade)과 연옥(Nephrite jade)으로 분류되며, 연옥은 경옥에 있어서의 나트륨(Na)과 알루미늄(Al) 조성분과는 달리, 인체에 유익한 3가지 광물 즉, 칼슘(Ca), 철분(Fe), 마그네슘(Mg)을 주성분으로 하고 있다. 따라서 본 발명에 적용 가능한 옥 분말은 그 종류에 제한이 있는 것은 아니나, 보다 바람직하게는 연옥을 사용한다.Jade is generally classified into jadeite and nephrite jade, and jadeite, unlike sodium and aluminum in jadeite, has three minerals that are beneficial to the human body. That is, calcium (Ca), iron (Fe), and magnesium (Mg) are the main components. Therefore, the jade powder which can be applied to the present invention is not limited in kind, but more preferably uses jade.
또한 본 발명에서 사용되는 춘천옥은 연옥의 일종으로, 강원도 춘천지역에서 생산되는 양질의 연옥(Nephrite Jade)으로서, 각섬석(Amphibole) 그룹의 투섬석(Tremolite)과 양기석(Actinolite)의 변종 광물로 그 조직이 치밀 섬세하고, 인성이 강한 양모상 조직을 가지는 광물이다.In addition, the Chuncheon Jade used in the present invention is a kind of purgatory, which is a high-quality nephrite Jade produced in Chuncheon, Gangwon-do, and is a variant mineral of Tremolite and Actinolite of Amphibole group. It is a mineral with dense, fine, tough wool texture.
본 발명에서 옥은 연마하여 분말로 가공된 것을 사용하며, 당업자가 실시하는 통상의 방법으로서 연옥의 분말화 방법에는 제한이 없다. 다만 본 발명에서 화장료 조성물로서 사용 가능한 옥 분말의 입자의 입도 분포는 10000 ~ 20000 mesh가 되도록 가공하는 것이 바람직하다. 20000 mesh가 초과되면 옥 분말의 효과가 미비하고, 10000 mesh 미만이면 구형의 옥 함침 분체 표면이 거칠어져 피부 적용시 사용감이 저하되기 때문이다.In the present invention, jade is used by grinding and processing into a powder, there is no limitation in the method of powdering purgatory as a common method performed by those skilled in the art. However, the particle size distribution of the particles of the jade powder that can be used as a cosmetic composition in the present invention is preferably processed to be 10000 ~ 20000 mesh. If the amount exceeds 20000 mesh, the effect of the jade powder is inadequate, and if it is less than 10000 mesh, the surface of the spherical jade impregnated powder becomes rough and the use of the skin is deteriorated.
다공성 고분자(Porous Polymer)Porous Polymer
본 발명에서 상기 옥 분말 입자가 함침되는 다공성 고분자는 오일 흡유력과 피지 흡착력이 있는 구형(Sphere) 분말상으로서, 예컨대 폴리메틸메타크릴레이트[PMMA: poly (methyl methacrylate)]를 적용하였으나, 이 외에도 폴리비닐피롤리돈[PVP: poly (vinyl pyrrolidone)], 폴리카프로락톤[PCL: poly (caprolactone)] 및 폴리-L-락틱산[PLLA: Poly (L-Lactic Acid)] 군으로부터 선택할 수 있으며, 이에 제한되지 않음은 물론이다.In the present invention, the porous polymer impregnated with the jade powder particles is a spherical powder having oil absorption and sebum adsorption, for example, polymethyl methacrylate (PMMA: poly (methyl methacrylate)), but in addition to poly Vinyl pyrrolidone [PVP: poly (vinyl pyrrolidone)], polycaprolactone [PCL: poly (caprolactone)] and poly-L-lactic acid [PLLA: Poly (L-Lactic Acid)] Of course, it is not limited.
이러한 다공성 고분자는 입자의 형상이 구형이기 때문에 다양한 화장료 제형의 제조시에 배합이 용이하고, 피부 위에서 구형상 미립자가 롤링(Rolling)됨으로써 피부 도포시 발림성 등의 사용감이 우수하며, 구형 표면의 특성인 광 산란을 이용한 피부 번들거림 방지 효과와 화장 지속성 향상 효과로 인해, 통상 피지 컨트롤을 위한 기초화장품과 피부톤 보정을 위한 메이크업 제품에 많이 사용된다.Since the porous polymer is spherical in shape, it is easy to mix when manufacturing various cosmetic formulations, and the spherical fine particles are rolled on the skin, thereby providing excellent feeling of application such as spreadability when applying the skin and having characteristics of a spherical surface. Due to light scattering prevention effect and improvement of makeup persistence, it is commonly used in basic cosmetics for sebum control and makeup products for skin tone correction.
옥 jade 함침Impregnation 분체Powder
본 발명의 옥 함침 분체, 즉 옥 분말 입자가 다공성 고분자에 고르게 함침된 복합분체에서, 옥 분말의 함량은 전체 옥 함침 분체 중량 대비 10 ~ 90 중량%로 함침될 수 있으며, 보다 바람직하게는 50 ~ 90 중량%로 함침될 수 있다. 또한 옥 함침 분체의 평균 입경은 5 ~ 20 ㎛일 수 있다. 이러한 특징은 옥 분말로 인한 효과와 피부 적용 시 사용감에 있어서 화장료로 적용하기에 적절하다.In the jade impregnated powder of the present invention, that is, the composite powder in which the jade powder particles are evenly impregnated into the porous polymer, the content of the jade powder may be impregnated with 10 to 90% by weight relative to the total jade impregnated powder weight, more preferably 50 to It may be impregnated at 90% by weight. In addition, the average particle diameter of the jade impregnated powder may be 5 ~ 20 ㎛. This feature is suitable for application as a cosmetic in terms of effects due to jade powder and usability in skin application.
본 발명은 옥 분말을 다공성 고분자 용액에 분산시킨 다공성 고분자 분산액을 분무 건조(Spray Drying) 또는 전기 분무(Electro-Spraying)하여 단일 공정(One-step)으로 옥 함침 분체를 제조함으로써, 옥 분말을 다공성 고분자 내부에 고르게 함침시키는 것이 가능하다. 이때 다공성 고분자의 초발수성 구현을 위해 유화제는 배제하는 것이 바람직하다. 종래에 유화중합과 같은 방법으로 생산되는 다공성 분체는 유화제의 사용이 불가피하여, 차후 유화제의 완전한 제거가 불가능하기 때문에 피부의 자극이 있으며, 피부의 유분뿐만 아니라 수분 또한 흡수하기 때문에 피부가 건조해지는 문제점이 있었다. 그러나 본 발명에 따르면, 유화제로 인한 피부 자극이 없으며, 초발수성을 구현하여 유분만을 선택적으로 흡수하고 화장지속력을 높일 수 있다.The present invention provides a jade impregnated powder by spray drying or electrospraying a porous polymer dispersion in which jade powder is dispersed in a porous polymer solution to prepare jade impregnated powder in one step. It is possible to impregnate the polymer evenly. At this time, it is preferable to exclude the emulsifier for the super water-repellent implementation of the porous polymer. Conventionally, porous powders produced by the same method as emulsion polymerization have inevitable use of emulsifiers, which makes it impossible to completely remove the emulsifiers in the future, causing skin irritation, and drying skin because it absorbs moisture as well as skin oils. There was this. However, according to the present invention, there is no skin irritation due to an emulsifier, and by implementing super water repellency, it is possible to selectively absorb only oil and increase makeup persistence.
또한 다공성 고분자 용액은 폴리메틸메타크릴레이트(PMMA)를 디클로로메탄(DCM)과 헥산올(Hexanol)의 혼합 용매에 용해시키며, 디클로로메탄(DCM)과 헥산올(Hexanol)의 혼합비(중량비)는 9 : 1 ~ 7 : 3 내에서 선택할 수 있다. 헥산올은 다공성 고분자의 포어(Pore)를 형성하는 역할을 하기 때문에, 헥산올의 비율이 전체 용매의 10 중량% 미만이면 포어 사이즈가 너무 작고, 30 중량% 이상이면 포어 사이즈가 너무 커서 적합하지 못하다.In addition, the porous polymer solution dissolves polymethylmethacrylate (PMMA) in a mixed solvent of dichloromethane (DCM) and hexanol, and the mixing ratio (weight ratio) of dichloromethane (DCM) and hexanol (Hexanol) is 9 : 1 to 7: 3 can be selected. Since hexanol plays a role of forming pores of porous polymers, if the proportion of hexanol is less than 10% by weight of the total solvent, the pore size is too small. .
본 발명에서 옥 함침 분체는 제조 공정 조건에 따라 기공 특성의 제어가 가능하다. 제어 가능한 기공 특성으로는 평균 기공 사이즈, 공극률 및 총 기공의 면적 등이 있다. 구체적으로 평균 기공 사이즈는 15 ~ 800nm, 보다 바람직하게는 250 ~ 600nm인 것일 수 있으며, 공극률은 40 ~ 85%, 보다 바람직하게는 50 ~ 75%일 수 있다. 또한 총 기공의 면적은 1 ~ 100m2/g, 보다 바람직하게는 5 ~ 80m2/g일 수 있다.In the present invention, the jade impregnated powder can control the pore characteristics according to the manufacturing process conditions. Controllable pore characteristics include average pore size, porosity and total pore area. Specifically, the average pore size may be 15 to 800 nm, more preferably 250 to 600 nm, and the porosity may be 40 to 85%, and more preferably 50 to 75%. In addition, the total pore area may be 1 to 100 m 2 / g, more preferably 5 to 80 m 2 / g.
이러한 특징을 가지는 옥 함침 분체는 그 기공 사이즈 및 공극률로 인하여 흡유량 증대 효과를 야기할 수 있다. 흡유량은 후술하는 수은의 침투 부피(Intrusion Volume)로 설명 가능하다. 본 발명에 따른 옥 함침 분체의 수은 침투 부피는 0.5 ~ 5cm3/g 범위로 측정되며, 이 수치는 높은 신뢰 수준으로 흡유량으로 간주될 수 있다.Jade impregnated powder having such a feature may cause an oil absorption increase effect due to its pore size and porosity. The oil absorption amount can be explained by the intrusion volume of mercury described later. The mercury penetration volume of the jade impregnated powder according to the invention is measured in the range of 0.5 to 5 cm 3 / g, which can be regarded as oil absorption with a high confidence level.
종래의 다공성 고분자는 단일크기의 메조포러스(Meso-Porous)한 구조로 인해 비표면적은 상대적으로 크나 평균 기공 사이즈와 공극률이 낮은 반면에, 본 발명의 옥 함침 분체의 경우는 멀티포러스(Multi-Porous, Micro+Meso+Macro) 구조로 인해 포어채널(Pore Channel)이 형성되어 모세관 현상에 의해 오일을 흡유하는데 훨씬 유리하다.Conventional porous polymers have a relatively large specific surface area due to a single-size meso-porous structure but a low average pore size and porosity, whereas the jade impregnated powder of the present invention is multi-porous. Pore Channel is formed due to the structure of Micro + Meso + Macro, which is much more advantageous for oil absorption by capillary action.
화장료Cosmetics 조성물 Composition
상기 옥 함침 분체는 화장료 조성물로서 적용하는 것이 가능하며, 이때 상기 옥 함침 분체는 전체 화장료 중량 대비 0.1 ~ 5.0 중량% 포함하는 것이 바람직하다. 옥 분말의 함량이 과다하면, 화장 원료 고유의 성질이나 연성 및 피부 적용시의 사용감이 저하될 뿐 아니라, 옥이 고가이기 때문에 제품 단가가 상승하는 문제점이 발생한다. 반면 옥 분말의 함량이 적으면, 옥 분말로 인한 효과를 기대할 수 없으므로 바람직하지 못하다.The jade impregnated powder can be applied as a cosmetic composition, wherein the jade impregnated powder is preferably included 0.1 to 5.0% by weight relative to the total cosmetic weight. When the content of the jade powder is excessive, not only the inherent properties and softness of the cosmetic raw material and the feeling of use when applying the skin, but also because the jade is expensive, the product cost rises. On the other hand, if the content of the jade powder is small, the effect due to the jade powder can not be expected is not preferable.
또한 본 발명의 화장료 조성물에는 옥 분말 이외에 피부 주름 개선, 피부 미백 개선, 피부 탄력 개선, 안면 처짐 개선, 피부 보습 개선, 피부 윤기 개선, 피부 노화 방지(예컨대, 광 노화에 의한 피부 주름 형성 및 피부 경화 억제), 다크써클 개선 및 피부 각질 개선과 같은 피부 개선을 위한 기능성 첨가물이나 자외선 차단을 위한 기능성 첨가물 또는 일반적인 화장료 조성물에 포함되는 성분이 추가로 포함될 수 있다.In addition, in the cosmetic composition of the present invention, in addition to jade powder, skin wrinkle improvement, skin whitening improvement, skin elasticity improvement, facial sagging improvement, skin moisturization improvement, skin gloss improvement, skin aging prevention (for example, skin wrinkle formation by photo aging and skin curing) Inhibition), functional additives for skin improvement such as dark circle improvement and skin exfoliation, or functional additives for blocking UV rays, or ingredients included in a general cosmetic composition may be further included.
상기 피부 개선을 위한 기능성 첨가물로서, 수용성 비타민, 지용성 비타민, 고분자 펩티드, 고분자 다당, 스핑고 지질, 천연 추출물 및 발효물질로 이루어진 군에서 선택된 성분을 포함할 수 있다. 또한 자외선 차단을 위한 기능성 첨가물로서, 이산화티탄(TiO2: Titanium dioxide), 산화아연(ZnO: Zinc oxide), 산화세륨(CeO2: Cerium oxide)과 같은 무기분체를 더 포함하는 것이 가능하다. 이에 추가적으로 상기 기능성 첨가물과 더불어 필요에 따라 일반적인 화장료 조성물에 포함되는 성분을 배합할 수 있다. As the functional additive for improving the skin, it may include a component selected from the group consisting of water-soluble vitamins, fat-soluble vitamins, polymer peptides, polymer polysaccharides, sphingolipids, natural extracts and fermented substances. In addition, as a functional additive for UV protection, it is possible to further include inorganic powders such as titanium dioxide (TiO 2 : Titanium dioxide), zinc oxide (ZnO: Zinc oxide), cerium oxide (CeO 2 : Cerium oxide). In addition to these functional additives may be blended with the components included in the general cosmetic composition as needed.
이외에 포함되는 배합 성분으로서는 유지 성분, 보습제, 에몰리엔트제, 계면 활성제, 유기 및 무기 안료, 유기 분체, 자외선 흡수제, 방부제, 살균제, 산화 방지제, 식물 추출물, pH 조정제, 알콜, 색소, 향료, 혈행 촉진제, 냉감제, 제한제, 정제수 등을 들 수 있으나, 이에 제한하지 아니함은 물론이다.In addition to the other components included, oils and fats, moisturizers, emollients, surfactants, organic and inorganic pigments, organic powders, ultraviolet absorbers, preservatives, fungicides, antioxidants, plant extracts, pH adjusters, alcohols, pigments, flavorings, blood circulation Accelerators, cooling agents, limiting agents, purified water, and the like, but is not limited thereto.
상기 옥 함침 분체가 포함된 화장료 조성물을 스킨, 로션, 크림, 세럼, 에멀젼, 에센스, 파우더, 파운데이션, 스프레이, 자외선차단제, 마스크팩, 젤 중 어느 하나의 형태, 보다 바람직하게는 마스크팩, 시트팩, 수면팩, 워시오프팩, 필오프팩 등으로 제형화할 수 있으나, 제형에 있어서 특별히 한정되지 않으며, 목적하는 바에 따라 적절히 선택하여 변경할 수 있다.The cosmetic composition containing the jade impregnated powder may be any one of skin, lotion, cream, serum, emulsion, essence, powder, foundation, spray, sunscreen, mask pack, gel, more preferably mask pack, sheet pack. It may be formulated as a sleeping pack, wash off pack, peel off pack, and the like, but is not particularly limited in the formulation, and may be appropriately selected and changed as desired.
이하, 본 발명을 실시예 및 도면에 의해 보다 상세히 설명하고자 한다. 하지만, 본 발명은 하기 실시예에 의해 한정되는 것은 아니며, 본 발명의 기술 사상 범위 내에서 여러 가지 변형 또는 수정할 수 있음은 이 분야에 통상의 지식을 가진 자에게는 명백한 것이다.Hereinafter, the present invention will be described in more detail with reference to examples and drawings. However, the present invention is not limited by the following examples, and it can be apparent to those skilled in the art that various changes or modifications can be made within the technical idea of the present invention.
하기 실시예 1 및 실시예 2를 제조하기 위하여, 다음의 [표 1]을 준비하였다.To prepare the following Example 1 and Example 2, the following Table 1 was prepared.
옥 분말(춘천옥)Jade powder (Chuncheon Jade) 옥산가 제조Oxane production
폴리메틸메타크릴레이트(PMMA, poly(methyl methacrylate))Poly (methyl methacrylate) (PMMA) LG PMMA 제조LG PMMA Manufacturer
디클로로메탄(DCM, Dichloromethane anhydrous)Dichloromethane anhydrous (DCM) Sigma-Aldrich 제조, 순도 > 99.8%Manufactured by Sigma-Aldrich, Purity> 99.8%
헥산올(Hexanol, 1-hexanol)Hexanol (1-hexanol) Sigma-Aldrich 제조, 순도 > 99%Manufactured by Sigma-Aldrich, Purity> 99%
<< 실시예Example 1> 1>
상기 [표 1]을 준비하여 하기 분무 건조의 방법에 따라 옥 함침 분체(이하 Jade Sphere)를 제조하였다.Table 1 was prepared to prepare jade impregnated powder (hereinafter referred to as jade sphere) according to the following spray drying method.
분무 건조(Spray-Drying)Spray-Drying
1) PMMA 40g을 용매(DCM : Hexanol = 9 : 1, wt%) 1L에 용해시켰다.1) 40 g of PMMA was dissolved in 1 L of a solvent (DCM: Hexanol = 9: 1, wt%).
2) 옥 분말 40g을 PMMA 용액에 넣은 후 균질기(Homogenizer)를 사용하여 분산시켰다.2) 40 g of jade powder was added to a PMMA solution and dispersed using a homogenizer.
3) 옥 분말이 분산된 PMMA 용액을 하기 [표 2]의 조건에서 분무 건조하였다.3) The PMMA solution in which the jade powder was dispersed was spray dried under the conditions of the following [Table 2].
내부 습도Internal humidity 30% 이상30% or more
내부 온도Internal temperature 실온 유지Keep at room temperature
내부 압력Internal pressure 20atm20atm
Feed rateFeed rate 20%20%
AspiratorAspirator 70%70%
4) 옥 분말이 분산된 PMMA 용액은 분무 건조 중에 지속적으로 교반기를 통하여 교반시켰다.4) The PMMA solution in which the jade powder was dispersed was continuously stirred through the stirrer during spray drying.
5) 분무 건조된 옥 분말/PMMA 복합분체 입자를 충분히 세척한 후, 동결건조하여 잔존 용매를 완전히 제거한 후 수득했다.5) The spray dried jade powder / PMMA composite powder particles were sufficiently washed and then lyophilized to completely remove the remaining solvent.
<< 실시예Example 2> 2>
상기 [표 1]을 준비하여 하기 전기 분무의 방법에 따라 옥 함침 분체(이하 Jade Sphere)를 제조하였다.Table 1 was prepared to prepare jade impregnated powder (hereinafter referred to as jade sphere) according to the following electrospray method.
전기 분무(Electrospray ( ElectroElectro Spraying) Spraying)
1) PMMA 0.4g을 용매(DCM : Hexanol = 9 : 1, wt%) 10mL에 용해시켰다.1) 0.4 g of PMMA was dissolved in 10 mL of a solvent (DCM: Hexanol = 9: 1, wt%).
2) 옥 분말 0.4g을 PMMA 용액에 넣은 후 초음파분쇄기(Sonicator)를 사용하여 분산시켰다.2) 0.4 g of jade powder was added to a PMMA solution and dispersed using a sonicator.
3) 옥 분말이 분산된 PMMA 용액을 하기 [표 3]의 조건에서 전기 분무하였다.3) PMMA solution in which jade powder was dispersed was electrosprayed under the conditions of the following [Table 3].
내부 습도Internal humidity 30% 이상30% or more
내부 온도Internal temperature 실온 유지Keep at room temperature
DistanceDistance 15cm15 cm
Feed rateFeed rate 20%20%
VoltageVoltage 10kV10 kV
4) 전기 분무된 옥 분말/PMMA 복합분체 입자를 충분히 세척한 후, 동결건조하여 잔존 용매를 완전히 제거한 후 수득했다.4) The electrosprayed jade powder / PMMA composite powder particles were sufficiently washed and then lyophilized to completely remove the remaining solvent.
<< 비교예Comparative example 1> 1>
상기 [표 1]의 옥 분말을 단독으로 적용하였다.The jade powder of [Table 1] was applied alone.
도 1은 비교예 1의 옥 분말의 주사전자현미경(SEM) 이미지이고, 도 2는 이러한 옥 분말이 다공성 고분자인 폴리메틸메타크릴레이트(PMMA) 입자 내부에 고르게 함침된 실시예 1의 옥 함침 분체의 표면(a) 및 절단면(b)의 주사전자현미경(SEM) 이미지이다. 도 1에 도시된 바와 같이, 무정형의 거친 구조를 가진 입자인 옥 분말을 분무 건조 및 전기 분무 방식을 적용하여, 도 2에서와 같이 폴리메틸메타크릴레이트(PMMA) 입자 내부에 고르게 함침시키는 것이 가능하다.1 is a scanning electron microscope (SEM) image of the jade powder of Comparative Example 1, Figure 2 is a jade impregnated powder of Example 1 in which the jade powder is impregnated evenly inside the polymethyl methacrylate (PMMA) particles of the porous polymer Scanning electron microscope (SEM) images of the surface (a) and the cut surface (b) of. As shown in FIG. 1, it is possible to impregnate the inside of polymethyl methacrylate (PMMA) particles as shown in FIG. 2 by applying spray drying and electrospray method to jade powder which is particles having an amorphous coarse structure. Do.
도 3은 에너지 분산형 X선(EDX: Energy Dispersive X-ray) 분석장치로 정량 및 정성분석한 이미지로서, 실시예 1의 옥 함침 분체(a)와 옥 함침 분체에 포함된 각 원소를 포인트로 가시화(b)한 이미지이다. 본 발명에서 적용된 춘천옥의 주 성분인 칼슘(Ca, Red point), 마그네슘(Mg, Blue point) 이온을 확인할 수 있으며, 이로 인해 옥 분말이 폴리메틸메타크릴레이트(PMMA) 전체에 고르게 함침되어 분포되었음을 확인할 수 있다.FIG. 3 is an image quantitatively and qualitatively analyzed by an energy dispersive X-ray (EDX) analyzer, and each element included in the jade impregnated powder (a) and the jade impregnated powder of Example 1 are represented as points. This image is visualized (b). Calcium (Ca, Red point), Magnesium (Mg, Blue point) ions, which are the main components of Chuncheon jade applied in the present invention, can be identified, which causes jade powder to be uniformly impregnated and distributed throughout polymethyl methacrylate (PMMA). You can check it.
항목별 테스트Itemized Test
이하에서는 분무 건조 방법으로 제조된 옥 함침 분체의 항목별 테스트를 실시하였다.Hereinafter, an item-specific test of the jade impregnated powder prepared by the spray drying method was performed.
<< 실험예Experimental Example 1> 반사율 테스트 1> reflectance test
색차계(ColorMate, (주)신코, 대한민국)를 이용하여 실험대상의 360 ~ 740nm 반사율 스펙트럼을 측정하였다. 그리고 반사율 측정하기 위해 PC 소프트웨어인 ColorMaster를 사용하였다. 반사율을 측정하여 해당 영역에서의 차단율을 계산하였다.Using a color difference meter (ColorMate, Shinko, Korea) was measured the reflectance spectrum of 360 ~ 740nm of the test subject. ColorMaster, a PC software, was used to measure reflectance. The reflectance was measured to calculate the blocking rate in that area.
도 4에 나타난 바와 같이, 비교예 1의 옥 분말과 실시예 1의 옥 함침 분체 모두 가시광선 영역대(380 ~ 710nm)의 반사율이 높게 나타났으나, 특히 380nm보다 장파장 영역부터는 실시예 1의 옥 함침 분체가 비교예 1의 옥 분말보다 더 높은 반사율을 나타내었다. 특히 블루 라이트 영역인 380 ~ 500nm에서는 이러한 반사율의 격차가 큰 것으로 보아 실시예 1의 옥 함침 분체가 비교예 1의 옥 분말보다 더 높은 블루 라이트 차단율을 나타내는 것을 알 수 있다.As shown in FIG. 4, the jade powder of Comparative Example 1 and the jade-impregnated powder of Example 1 exhibited higher reflectances in the visible light band (380 to 710 nm), but in particular, the jade of Example 1 from a longer wavelength range than 380 nm. The impregnated powder showed higher reflectance than the jade powder of Comparative Example 1. In particular, in the blue light region of 380 to 500 nm, the difference in reflectance is large, and it can be seen that the jade impregnated powder of Example 1 exhibits a higher blue light blocking rate than the jade powder of Comparative Example 1.
<< 실험예Experimental Example 2> 백색도(Whiteness,  2> Whiteness %R% R ) 테스트) Test
백색도는 색의 흰 정도를 1차원적으로 나타낸 수치로서, 상기 반사율 테스트에서 전체 가시광선 영역의 XYZ 색차값을 바탕으로 다음과 같은 계산식을 통해 백색도 지수를 도출하였다.Whiteness is a numerical value representing the whiteness of a color in one dimension, and the whiteness index was derived through the following formula based on the XYZ color difference value of the entire visible light region in the reflectance test.
WI = Y + 800(xn - x) + 1700(yn - y) < CIE Whiteness >WI = Y + 800 (x n -x) + 1700 (y n -y) <CIE Whiteness>
Xn = 0.3101, Yn = 0.3162(C/2º), Xn = 0.3138, Yn = 0.3309(C/2º) X n = 0.3101, Y n = 0.3162 (C / 2º), X n = 0.3138, Y n = 0.3309 (C / 2º)
도 5에 나타난 바와 같이, 실시예 1의 옥 함침 분체의 백색도가 94%로 비교예 1의 옥 분말의 백색도 84%보다 백색도가 10% 개선된 결과를 나타내었다.As shown in FIG. 5, the whiteness of the jade impregnated powder of Example 1 was 94%, and the whiteness of the jade powder of Comparative Example 1 was 10% improved from the whiteness of 84%.
<< 실험예Experimental Example 3> 공극률 측정 테스트 3> Porosity Measurement Test
실시예 1의 옥 함침 분체의 기공 특성을 분석하기 위해서 수은(Hg) 침투법 분석을 실시하였다. Porosimeter (Autopore IV 9500, Micrometrics, Londonderry, NH, USA)를 이용하여 수은의 침투 부피(Intrusion Volume), 평균 기공크기(4V/A, V: volume, A: area) 및 공극률(Porosity)을 측정하여 [표 4]에 나타내었다. In order to analyze the pore characteristics of the jade impregnated powder of Example 1, analysis of mercury (Hg) penetration method was performed. The porosimeter (Autopore IV 9500, Micrometrics, Londonderry, NH, USA) was used to measure the intrusion volume, average pore size (4V / A, V: volume, A: area) and porosity of mercury. It is shown in [Table 4].
Total Intrusion VolumeTotal Intrusion Volume 1.6797 mL/g1.6797 mL / g
Total Pore Area Total Pore Area 15.125 m2/g15.125 m 2 / g
Average Pore Diameter (4V/A) Average Pore Diameter (4V / A) 444.2 nm444.2 nm
Bulk Density at 0.20 psiaBulk Density at 0.20 psia 0.3832 g/mL0.3832 g / mL
PorosityPorosity 64.37%64.37%
상기 'Total Intrusion Volume'은 단위 그램당 침투되는 수은의 양, 'Total Pore Area'는 원통형의 면적으로 나타낸 총 기공의 면적, 'Average Pore Diameter'는 총 기공 사이즈의 평균값, 'Bulk Density at 0.20 psia'는 0.20 psia에서 샘플의 기공을 포함한 실제 밀도를 의미한다.'Total Intrusion Volume' is the amount of mercury penetrated per gram, 'Total Pore Area' is the total pore area represented by the cylindrical area, 'Average Pore Diameter' is the average value of the total pore size, and 'Bulk Density at 0.20 psia 'Means the actual density including the pores of the sample at 0.20 psia.
결과 실시예 1의 옥 함침 분체의 경우 444.2nm의 평균 기공 크기와 64.37%의 높은 공극률을 확인할 수 있었다. As a result, in the jade impregnated powder of Example 1, an average pore size of 444.2 nm and a high porosity of 64.37% were confirmed.
<< 실험예Experimental Example 4>  4> 흡유량Oil absorption 테스트 Test
저울과 페트리 접시(Petri dish)를 이용하여 실시예 1의 옥 함침 분체를 1g 측량한 후, 스포이트를 이용하여 인체의 피지와 유사한 물성을 갖는 트리글리세리드(Triglyceride) 오일을 떨어뜨려 실시예 1의 옥 함침 분체가 촉촉히 젖을 때까지 소요된 흡유량을 측정하였다. 이때 스패츌러(Spatular)를 이용하여 오일이 잘 젖을 수 있도록 믹싱한다. 1 g of the jade impregnated powder of Example 1 was measured using a balance and a Petri dish, and then triglyceride oil having physical properties similar to sebum of the human body was dropped using a dropper to impregnate the jade of Example 1 The amount of oil absorption required until the powder was wet was measured. At this time, use a spatula to mix the oil so that it is well wet.
도 6에 도시된 바와 같이, 실시예 1의 옥 함침 분체의 흡유량은 1.7mL/g로서 상기 3. 공극률 측정 테스트에서 수은의 침투 부피(Total Intrusion Volume) 1.6797mL/g과 매우 유사하며 이는 곧 흡유량 측정 결과의 신뢰성을 입증하는 결과이며, 또한 옥 분말에 비해 최대 5배 이상 흡유량이 증가한 것을 확인할 수 있다. 이는 실시예 1의 옥 함침 분체가 옥 분말을 50 중량% 포함하고 있음에도 불구하고, 큰 기공 사이즈와 높은 공극률을 유지함으로써 발생하는 효과이다.As shown in FIG. 6, the oil absorption of the jade impregnated powder of Example 1 was 1.7 mL / g, which is very similar to the total intrusion volume 1.6797 mL / g of mercury in the above 3. porosity measurement test. It is a result demonstrating the reliability of the measurement result, and it can also be confirmed that the oil absorption amount increased by at least 5 times compared to the jade powder. This is an effect generated by maintaining a large pore size and a high porosity, although the jade impregnated powder of Example 1 contains 50 wt% of jade powder.
이하는 상기 실시예 1에서 제조된 옥 함침 분체를 다음의 [표 5]에 기재된 조성(중량%)에 따라 에멀젼 형태(마스크팩)로 제형화하여 항목별 테스트를 실시하였다.The following jade impregnated powder prepared in Example 1 was formulated in an emulsion form (mask pack) according to the composition (% by weight) described in the following [Table 5] to perform an itemized test.
구분division 성분ingredient 비교제형예 1Comparative Formulation Example 1 비교제형예 2Comparative Formulation Example 2 제형예 1Formulation Example 1
유상파트Paid Part 세테아릴알코올Cetearyl Alcohol 4.004.00 4.004.00 4.004.00
스테아릭애씨드Stearic acid 0.500.50 0.500.50 0.500.50
팔미틱애씨드Palmitic Acid 0.500.50 0.500.50 0.500.50
하이드로제네이티드레시친Hydrogenated Dressin 1.001.00 1.001.00 1.001.00
글리세릴스테아레이트Glyceryl Stearate 1.501.50 1.501.50 1.501.50
트리에칠헥사노인Triethylhexanoin 3.003.00 3.003.00 3.003.00
펜타에리스리틸테트라에칠헥사노에이트Pentaerythritol tetraethylhexanoate 4.004.00 4.004.00 4.004.00
트리실록산Trisiloxane 2.002.00 2.002.00 2.002.00
디메치콘Dimethicone 2.002.00 2.002.00 2.002.00
수상파트Water Part 향료Spices 적량Quantity 적량Quantity 적량Quantity
정제수Purified water 적량Quantity 적량Quantity 적량Quantity
디소듐 이디티에이Disodium ID 0.050.05 0.050.05 0.050.05
글리세린glycerin 4.004.00 4.004.00 4.004.00
프로판디올Propanediol 10.0010.00 10.0010.00 10.0010.00
기타 점증제, 중화제Other thickeners, neutralizers 적량Quantity 적량Quantity 적량Quantity
방부제antiseptic 적량Quantity 적량Quantity 적량Quantity
춘천옥Chuncheon Jade 0.000.00 1.001.00 0.000.00
Jade SphereJade sphere 0.000.00 0.000.00 1.001.00
<< 실험예Experimental Example 5> 사용성 평가 테스트 5> Usability Test
본 발명의 비교 제형예 1, 2 및 제형예 1에 대해 25 ~ 35세의 여성 30명을 대상으로 1일 2회씩 한 달간 사용하게 한 후, 밀착성, 퍼짐성, 부드러움성, 입자뭉침, 화장지속성 등의 항목에 대해 비교함으로써 화장료로서의 사용성을 1 ~ 5 점까지 평가하게 하였고, 그 결과를 하기 [표 6]에 나타내었다.For the Comparative Formulation Examples 1, 2 and Formulation Example 1 of the present invention, 30 women aged 25 to 35 years old were used twice a day for one month, and then adhesiveness, spreadability, softness, particle aggregation, and cosmetic sustainability were used. By comparing the items to the usability as a cosmetic was evaluated to 1 to 5 points, the results are shown in the following [Table 6].
구분division 밀착성Adhesiveness 퍼짐성Spreadability 부드러움성Softness 입자뭉침Particle aggregation 화장지속성Toilet paper
비교제형예 1Comparative Formulation Example 1 55 55 55 1One 33
비교제형예 2Comparative Formulation Example 2 22 33 22 55 22
제형예 1Formulation Example 1 44 44 55 22 55
상기 [표 6]을 보면, 춘천옥 분말을 포함한 비교 제형예 2의 경우에는 옥 분말을 전혀 포함하지 않는 비교 제형예 1에 비하여 입자뭉침 현상이 크고, 밀착성, 퍼짐성, 부드러움성 및 화장지속성의 전 항목에 대하여 낮은 평가치를 나타낸다. 반면, 옥 함침 분체를 포함한 제형예 1에서는 춘천옥 분말을 포함한 비교 제형예 2에 비하여 입자뭉침이 크게 줄어들고 밀착성, 퍼짐성이 개선되었으며, 부드러움성과 화장지속성이 비교 제형예 1과 비슷하거나 향상된 수준으로 나타났다. [Table 6], in the case of Comparative Formulation Example 2 containing Chuncheon jade powder compared to Comparative Formulation Example 1 containing no jade powder, the particle aggregation phenomenon is larger, and all items of adhesion, spreadability, softness and makeup persistence Low evaluation of the On the other hand, in Formulation Example 1 containing jade impregnated powder, compared to Comparative Formulation Example 2 containing Chuncheon Jade powder, particle aggregation was greatly reduced, adhesion and spreadability were improved, and softness and makeup persistence were similar or improved to those of Comparative Formulation Example 1.
따라서 본 발명의 옥 함침 분체는 구형의 형상에서 기인되는 부드러움성과 높은 공극률에 의한 피지흡유에서 기인되는 화장지속성에서도 우수한 결과를 보였다. 또한 옥 분말을 포함하는 비교 제형예 2의 가장 큰 문제점이었던 입자뭉침을 크게 개선하여 백탁현상을 방지할 수 있음을 확인하였다.Therefore, the jade impregnated powder of the present invention showed excellent results in the softness caused by the spherical shape and the cosmetic persistence caused by sebum absorption due to high porosity. In addition, it was confirmed that the particle aggregation, which was the biggest problem of Comparative Formulation Example 2 including jade powder, was greatly improved to prevent cloudiness.
<< 실험예Experimental Example 6> 제형의 반사율 테스트 6> Reflectance test of formulation
상기 비교 제형예 1, 2 및 제형예 1의 제형의 가시광선 영역내 차단율을 측정하기 위하여, 색차계(ColorMate, (주)신코, 대한민국)를 이용하여 실험대상의 360 ~ 740nm 반사율 스펙트럼을 측정하였다. 그리고 반사율 측정하기 위해 PC 소프트웨어인 ColorMaster를 사용하였다.In order to measure the blocking rate in the visible light region of the formulations of Comparative Formulation Examples 1 and 2 and Formulation Example 1, a 360-740 nm reflectance spectrum of the test subject was measured using a color difference meter (ColorMate, Shinco, Korea). . ColorMaster, a PC software, was used to measure reflectance.
도 7에 도시된 바와 같이, 제형화된 비교 제형예 1, 2 및 제형예 1 모두 분말 상태의 반사율 테스트 결과와 유사하게 나타났으나, 특히 블루 라이트 영역의 단파장의 빛일수록 옥 함침 분체를 포함한 제조예 1의 반사율의 격차가 큰 것으로 보아 옥 함침 분체를 제형화하여도 높은 블루 라이트 차단율을 나타내는 것을 알 수 있다.As shown in FIG. 7, the formulated Comparative Formulation Examples 1, 2 and Formulation Example 1 all appeared similar to the reflectance test results in the powder state, but in particular, the short wavelength light in the blue light region was prepared including jade impregnated powder. The large difference in reflectance of Example 1 shows that the blue light blocking rate is high even when the jade impregnated powder is formulated.
<< 실험예Experimental Example 7> 제형의 백색도(Whiteness,  7> Whiteness of the formulation %R% R ) 테스트) Test
제형의 백색도는 색의 흰 정도를 1차원적으로 나타낸 수치로서, 상기 제형의 반사율 테스트에서 전체 가시광선 영역의 XYZ 색차값을 바탕으로 다음과 같은 계산식을 통해 백색도 지수를 도출하였다.Whiteness of the formulation is a numerical value representing the whiteness of the color in one dimension, and the whiteness index was derived through the following formula based on the XYZ color difference value of the entire visible light region in the reflectance test of the formulation.
WI = Y + 800(xn - x) + 1700(yn - y) < CIE Whiteness >WI = Y + 800 (x n -x) + 1700 (y n -y) <CIE Whiteness>
Xn = 0.3101, Yn = 0.3162(C/2º), Xn = 0.3138, Yn = 0.3309(C/2º) X n = 0.3101, Y n = 0.3162 (C / 2º), X n = 0.3138, Y n = 0.3309 (C / 2º)
도 8에 나타난 바와 같이, 옥 분말을 포함하지 않은 비교 제형예 1에 비하여 옥 분말 또는 옥 함침 분체를 포함한 비교 제형예 2 및 제형예 1의 백색도가 유의적으로 향상되었음을 알 수 있으며, 미세하지만 제형예 1인 옥 함침 분체의 백색도가 가장 높은 수준인 것을 확인하였다.As shown in FIG. 8, it can be seen that the whiteness of Comparative Formulation Example 2 and Formulation Example 1 containing jade powder or jade impregnated powder was significantly improved compared to Comparative Formulation Example 1 without jade powder. It was confirmed that the whiteness of the jade impregnated powder of Example 1 was the highest level.
<< 제형예Formulation example 2> 2>
이하는 상기 실시예 1에서 제조된 옥 함침 분체를 0.1 중량% 함유하고, 다음의 [표 7]에 기재된 조성(중량 %)에 따라 통상적인 방법으로 영양 화장수를 제조하였다.The following contained 0.1 wt% of the jade impregnated powder prepared in Example 1, and prepared a nutritional lotion by a conventional method according to the composition (wt%) described in the following [Table 7].
성분ingredient 함량(중량%)Content (% by weight)
정제수Purified water 잔량Remaining amount
글리세린glycerin 8.08.0
부틸렌글리콜Butylene glycol 4.04.0
히알루론산 추출물Hyaluronic acid extract 5.05.0
베타글루칸Beta Glucan 7.07.0
카보머Carbomer 0.10.1
글루코세라마이드 & 7,8,4'-트리하이드록시이소플라본Glucoceramide & 7,8,4'-trihydroxyisoflavones 0.050.05
카프릴릭/카프릭 트리글리세라이드Caprylic / Capric Triglycerides 8.08.0
스쿠알란Squalane 5.05.0
세테아릴 글루코사이드Cetearyl Glucoside 1.51.5
소르비탄 스테아레이트Sorbitan stearate 0.40.4
세테아릴 알코올Cetearyl Alcohol 1.01.0
트리에탄올아민Triethanolamine 0.10.1
Jade SphereJade sphere 0.10.1
<< 제형예Formulation example 3> 3>
이하는 상기 실시예 1에서 제조된 옥 함침 분체를 3.0 중량% 함유하고, 다음의 [표 8]에 기재된 조성(중량 %)에 따라 통상적인 방법으로 영양 크림을 제조하였다.The following contained 3.0 wt% of the jade impregnated powder prepared in Example 1, and prepared a nutritious cream in a conventional manner according to the composition (wt%) shown in the following [Table 8].
성분ingredient 함량(중량%)Content (% by weight)
정제수Purified water 잔량Remaining amount
글리세린glycerin 3.03.0
부틸렌글리콜Butylene glycol 3.03.0
유동파라핀Liquid paraffin 7.07.0
베타글루칸Beta Glucan 7.07.0
카보머Carbomer 0.10.1
글루코세라마이드 & 7,8,4'-트리하이드록시이소플라본Glucoceramide & 7,8,4'-trihydroxyisoflavones 3.03.0
카프릴릭/카프릭 트리글리세라이드Caprylic / Capric Triglycerides 3.03.0
스쿠알란Squalane 5.05.0
세테아릴 글루코사이드Cetearyl Glucoside 1.51.5
소르비탄 스테아레이트Sorbitan stearate 0.40.4
폴리솔베이트 60Polysorbate 60 1.21.2
트리에탄올아민Triethanolamine 0.10.1
Jade SphereJade sphere 3.03.0
<< 제형예Formulation example 4> 4>
이하는 상기 실시예 1에서 제조된 옥 함침 분체를 5.0 중량% 함유하고, 다음의 [표 9]에 기재된 조성(중량 %)에 따라 통상적인 방법으로 마사지 크림를 제조하였다.The following contained 5.0 wt% of the jade impregnated powder prepared in Example 1, and prepared a massage cream in a conventional manner according to the composition (wt%) shown in the following [Table 9].
성분ingredient 함량(중량%)Content (% by weight)
정제수Purified water 잔량Remaining amount
글리세린glycerin 8.08.0
부틸렌글리콜Butylene glycol 4.04.0
유동파라핀Liquid paraffin 45.045.0
베타글루칸Beta Glucan 7.07.0
카보머Carbomer 0.10.1
글루코세라마이드 & 7,8,4'-트리하이드록시이소플라본Glucoceramide & 7,8,4'-trihydroxyisoflavones 1.01.0
카프릴릭/카프릭 트리글리세라이드Caprylic / Capric Triglycerides 3.03.0
밀납Beeswax 4.04.0
세테아릴 글루코사이드Cetearyl Glucoside 1.51.5
세스퀴올레인산 소르비탄Sesquioleic acid sorbitan 0.90.9
바세린Vaseline 3.03.0
파라핀paraffin 1.51.5
Jade SphereJade sphere 5.05.0

Claims (13)

  1. 옥(Jade) 분말 입자가 다공성 고분자에 함침(Impregnation)된 복합분체.Jade powder particles impregnated in the porous polymer (Impregnation) composite powder.
  2. 제1항에 있어서,The method of claim 1,
    상기 옥 분말은 전체 복합분체 중량 대비 50 ~ 90 중량%로 함침되는 것을 특징으로 하는 복합분체.The jade powder is a composite powder, characterized in that impregnated with 50 to 90% by weight relative to the total weight of the composite powder.
  3. 제1항에 있어서,The method of claim 1,
    상기 다공성 고분자는 폴리메틸메타크릴레이트[PMMA: poly-(methyl methacrylate)], 폴리비닐피롤리돈[PVP: poly-(vinyl pyrrolidone)], 폴리카프로락톤[PCL: poly-(caprolactone)] 및 폴리-L-락틱산[PLLA: Poly-(L-Lactic Acid)] 군으로부터 선택되는 1종 이상인 것을 특징으로 하는 복합분체.The porous polymer is polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)] and poly -L-lactic acid [PLLA: Poly- (L-Lactic Acid)] Complex powder, characterized in that at least one member selected from the group.
  4. 제1항에 있어서,The method of claim 1,
    상기 복합분체의 평균 입경은 5 ~ 20 ㎛인 것을 특징으로 하는 복합분체.The composite powder, characterized in that the average particle diameter of the composite powder is 5 ~ 20 ㎛.
  5. 제1항에 있어서,The method of claim 1,
    상기 복합분체의 평균 기공 사이즈는 15 ~ 800nm인 것을 특징으로 하는 복합분체.The composite powder, characterized in that the average pore size of the composite powder is 15 ~ 800nm.
  6. 제1항에 있어서,The method of claim 1,
    상기 복합분체의 공극률은 40 ~ 85%인 것을 특징으로 하는 복합분체.Porosity of the composite powder is a composite powder, characterized in that 40 to 85%.
  7. 제1항 내지 제6항 중 어느 한 항의 복합분체를 포함하는 화장료 조성물.Cosmetic composition containing the composite powder of any one of Claims 1-6.
  8. 제7항에 있어서,The method of claim 7, wherein
    상기 복합분체는 전체 화장료 중량 대비 0.1 ~ 5.0 중량% 포함되는 것을 특징으로 하는 화장료 조성물.The composite powder is a cosmetic composition, characterized in that contained 0.1 to 5.0% by weight relative to the total weight of the cosmetic.
  9. 제7항에 있어서,The method of claim 7, wherein
    상기 화장료 조성물은 스킨, 로션, 크림, 세럼, 에멀젼, 에센스, 파우더, 파운데이션, 스프레이, 자외선차단제, 마스크팩, 젤 중에서 어느 하나의 형태로 제형화되는 것을 특징으로 하는 화장료 조성물.The cosmetic composition is a cosmetic composition, characterized in that it is formulated in any one form of skin, lotion, cream, serum, emulsion, essence, powder, foundation, spray, sunscreen, mask pack, gel.
  10. 다공성 고분자 용액에 옥 분말을 분산시킨 분산액을 분무 건조(Spray Drying)하여 제조하는 것을 특징으로 하는 옥 분말 입자가 다공성 고분자에 함침된 복합분체의 제조방법.A method for producing a composite powder in which jade powder particles are impregnated into a porous polymer, characterized in that the dispersion is prepared by spray drying a dispersion in which jade powder is dispersed in a porous polymer solution.
  11. 다공성 고분자 용액에 옥 분말을 분산시킨 분산액을 전기 분무(Electro-Spraying)하여 제조하는 것을 특징으로 하는 옥 분말 입자가 다공성 고분자에 함침된 복합분체의 제조방법.A method for producing a composite powder in which jade powder particles are impregnated into a porous polymer, characterized in that the dispersion is prepared by electrospraying a dispersion in which jade powder is dispersed in a porous polymer solution.
  12. 제10항 또는 제11항에 있어서,The method according to claim 10 or 11, wherein
    상기 다공성 고분자 용액은 폴리메틸메타크릴레이트[PMMA: poly-(methyl methacrylate)], 폴리비닐피롤리돈[PVP: poly-(vinyl pyrrolidone)], 폴리카프로락톤[PCL: poly-(caprolactone)] 및 폴리-L-락틱산[PLLA: Poly-(L-Lactic Acid)] 군으로부터 선택되는 1종 이상의 고분자를 용매에 용해시킨 것으로,The porous polymer solution is polymethyl methacrylate [PMMA: poly- (methyl methacrylate)], polyvinylpyrrolidone [PVP: poly- (vinyl pyrrolidone)], polycaprolactone [PCL: poly- (caprolactone)] and One or more polymers selected from the group of poly-L-lactic acid [PLLA: Poly- (L-Lactic Acid)] are dissolved in a solvent,
    상기 용매는 디클로로메탄과 헥산올의 혼합 용매인 것을 특징으로 하는 복합분체의 제조방법.The solvent is a method for producing a composite powder, characterized in that a mixed solvent of dichloromethane and hexanol.
  13. 제12항에 있어서,The method of claim 12,
    상기 디클로로메탄과 헥산올의 중량비는 9 : 1 ~ 7 : 3인 것을 특징으로 하는 복합분체의 제조방법.Method for producing a composite powder, characterized in that the weight ratio of the dichloromethane and hexanol is 9: 1 to 7: 3.
PCT/KR2016/006882 2015-06-30 2016-06-28 Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same WO2017003149A1 (en)

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JP2017559068A JP6796082B2 (en) 2015-06-30 2016-06-28 A composite powder in which jade powder particles are impregnated in a porous polymer, a cosmetic composition containing the composite powder, and a method for producing the same.
CN201680035773.0A CN108040466B (en) 2015-06-30 2016-06-28 Composite powder of jade powder particles impregnated in porous polymer, cosmetic composition containing the same, and preparation method thereof
US15/576,125 US10238583B2 (en) 2015-06-30 2016-06-28 Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same
US16/271,399 US10624822B2 (en) 2015-06-30 2019-02-08 Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020065959A (en) * 2001-02-08 2002-08-14 주식회사 코리아나화장품 Cosmetics containing gem powder
KR20040039501A (en) * 2002-10-28 2004-05-12 주식회사 태평양 Composition for external application to the skin containing an anti-oxidant nano-sized emulsion composites
US20070009560A1 (en) * 2003-09-30 2007-01-11 Coty B.V. Cosmetic and dermatological agent containing magnetic particles production thereof and use of the same
KR20070057333A (en) * 2005-12-01 2007-06-07 주식회사 엘지생활건강 Powder with lustrous coating layer and color cosmetic containing the same
KR20110046619A (en) * 2009-10-29 2011-05-06 서범구 Cosmetic composition comprising kaolin, colostrum and fermented oriental medicinal active liquid, and method of preparing the same

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20020065959A (en) * 2001-02-08 2002-08-14 주식회사 코리아나화장품 Cosmetics containing gem powder
KR20040039501A (en) * 2002-10-28 2004-05-12 주식회사 태평양 Composition for external application to the skin containing an anti-oxidant nano-sized emulsion composites
US20070009560A1 (en) * 2003-09-30 2007-01-11 Coty B.V. Cosmetic and dermatological agent containing magnetic particles production thereof and use of the same
KR20070057333A (en) * 2005-12-01 2007-06-07 주식회사 엘지생활건강 Powder with lustrous coating layer and color cosmetic containing the same
KR20110046619A (en) * 2009-10-29 2011-05-06 서범구 Cosmetic composition comprising kaolin, colostrum and fermented oriental medicinal active liquid, and method of preparing the same

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