Composite powder in which jade powder particles are impregnated in porous polymer, cosmetic composition containing same and manufacturing method for same
10624822 ยท 2020-04-21
Assignee
Inventors
- Hyun Suk Lee (Yongin-si, KR)
- Dong-Hyun Paik (Siheung-si, KR)
- Ga Young Cho (Yongin-si, KR)
- Hyoung June KIM (Yongin-si, KR)
- Hae Jin Jung (Yongin-si, KR)
- Dong Hyuk Jang (Yongin-si, KR)
- Yong Jin Kim (Yongin-si, KR)
- Lee Kyoung Kwon (Yongin-si, KR)
- John Hwan LEE (Yongin-si, KR)
- Sung-Wook Choi (Bucheon-si, KR)
Cpc classification
A61K8/8147
HUMAN NECESSITIES
A61K8/0245
HUMAN NECESSITIES
A61K8/8152
HUMAN NECESSITIES
A61K2800/654
HUMAN NECESSITIES
A61K2800/83
HUMAN NECESSITIES
A61K8/8176
HUMAN NECESSITIES
International classification
A61K8/81
HUMAN NECESSITIES
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.
Claims
1. A composite powder in which jade powder particles are impregnated in a porous polymer, wherein the jade powder particles are impregnated at a content of 50 to 90% by weight, based on the total weight of the composite powder; the porous polymer is selected from the group consisting of poly(vinyl pyrrolidone) (PVP), poly(caprolactone) (PCL), poly(L-lactic acid) (PLLA), and a mixture thereof; the composite powder has an average pore size of 250 to 600 nm; and the composite powder has a porosity of 40 to 85%.
2. The composite powder of claim 1, wherein the composite powder has an average particle diameter of 5 to 20 m.
3. A cosmetic composition comprising the composite powder of claim 1.
4. The cosmetic composition of claim 3, wherein the composite powder is included at a content of 0.1 to 5.0% by weight, based on the total weight of the cosmetic composition.
5. The cosmetic composition of claim 3, wherein the cosmetic composition is formulated into any one form selected from the group consisting of a toner, a lotion, a cream, a serum, an emulsion, a nourishing serum, a powder, a foundation, a spray, a sunscreen agent, a mask pack, and a gel.
6. A method for manufacturing a composite powder according to claim 1 in which jade powder particles are impregnated in a porous polymer, comprising: spray-drying or electro-spraying a dispersion in which jade powder is dispersed in the porous polymer solution to manufacture the composite powder, wherein the porous polymer comprises poly(vinyl pyrrolidone) (PVP), poly(caprolactone) (PCL), or and poly(L-lactic acid) (PLLA).
7. The method of claim 6, wherein the porous polymer solution is obtained by dissolving the porous polymer in a mixed solvent of dichloromethane and hexanol.
8. The method of claim 7, wherein the dichloromethane and the hexanol are present at a weight ratio of 9:1 to 7:3.
9. A method for manufacturing a composite powder in which jade powder particles are impregnated in a porous polymer, comprising: spray-drying or electro-spraying a dispersion in which jade powder is dispersed in the porous polymer solution to manufacture the composite powder, wherein, the jade powder particles are impregnated at a content of 50 to 90% by weight, based on the total weight of the composite powder; the porous polymer is selected from the group consisting of poly(vinyl pyrrolidone) (PVP), poly(caprolactone) (PCL), poly(L-lactic acid) (PLLA), and a mixture thereof; the composite powder has an average pore size of 250 to 600 nm; and the composite powder has a porosity of 40 to 85%.
Description
DESCRIPTION OF DRAWINGS
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BEST MODE
(9) The present invention relates to a composite powder including jade powder and a porous polymer, and more particularly, to a composite powder (hereinafter referred to as a jade sphere) in which jade powder particles are uniformly impregnated in a porous polymer by dispersing jade powder in a solution in which a porous polymer is dissolved, and then spraying the dispersion using a one-step spray drying or electro-spraying process, a cosmetic composition containing the same, and a manufacturing method for the same. In the present invention, the term impregnation refers to a situation in which other powder particles are uniformly dispersed in underlying powder particles so that the other powder particles permeate into the underlying powder particles. In this case, such a configuration differs from a configuration in which surfaces of powder particles are coated with other powder particles or a configuration in which powder particles are supported between pores on surfaces of other powder particles, as known in the art. Hereinafter, the present invention will be described in detail.
(10) Jade
(11) Generally, jade is divided into jadeite jade and nephrite jade. Nephrite jade contains three minerals beneficial to the human body, that is, calcium (Ca), iron (Fe), magnesium (Mg) as main components unlike minor components such as sodium (Na) and aluminum (Al) contained in jadeite jade. Therefore, types of the jade powder applicable to the present invention are not limited. More preferably, the nephrite jade is used.
(12) Also, Chuncheon jade used in the present invention is a kind of nephrite jade, that is, high-quality nephrite jade produced in the Chuncheon area of Gangwon-do. In this case, Chuncheon jade is an altered mineral of tremolite and actinolite of the amphibole family, which has a compact and delicate texture and also has a pilotoxitic texture with strong toughness.
(13) In the present invention, jade is ground into powder, which is then used as the jade powder. As a conventional method performed by a person having ordinary skill in the art, a method of grinding nephrite jade into powder is not limited. However, the jade powder that may be used for a cosmetic composition according to the present invention is processed so that the jade powder particles have a particle size distribution of 10,000 to 20,000 meshes. When the particle size distribution is greater than 20,000 meshes, an effect of the jade powder may be not significant. On the other hand, when the particle size distribution is less than 10,000 meshes, a sense of feeling in use upon application to the skin may be degraded due to a coarse surface of the spherical jade sphere.
(14) Porous Polymer
(15) In the present invention, a porous polymer in which the jade powder particles are impregnated is in a spherical powdery phase having oil absorption and sebum absorption powder. For example, poly(methyl methacrylate) (PMMA) is used as the porous polymer. In addition, the porous polymer may be selected from the group consisting of poly(vinyl pyrrolidone) (PVP), poly(caprolactone) (PCL), and poly(L-lactic acid) (PLLA), but the prevent invention is not limited thereto.
(16) Such a porous polymer is easily blended in the manufacture of various cosmetic formulations because the porous polymer has a spherical particle shape, and has excellent senses of feeling in use thereof, such as applicability, and the like because spherical particulates are rolled on the skin when the cosmetic formulations are applied onto the skin. Therefore, the porous polymer is generally often used in fundamental cosmetics for controlling sebum and make-up cosmetics for modifying a color tone of the skin due to surface characteristics of the spherical particulates, such as an effect of preventing greasiness of the skin using light scattering, and an effect of improving cosmetic durability.
(17) Jade Sphere
(18) In the jade sphere of the present invention, that is, a composite powder in which jade powder particles are uniformly impregnated in a porous polymer, the jade powder may be impregnated at a content of 10 to 90% by weight, more preferably impregnated at a content of 50 to 90% by weight, based on the total weight of the jade sphere. Also, the jade sphere may have an average particle diameter of 5 to 20 m. Such characteristics of the jade sphere make the composite powder suitable for use as a cosmetic material in terms of an effect of the jade powder and a sense of feeling in use thereof upon application to the skin.
(19) According to the present invention, the jade powder may be uniformly impregnated in the porous polymer by spray-drying or electro-spraying a porous polymer dispersion, in which the jade powder is dispersed in a porous polymer solution, to manufacture a jade sphere using a one-step process. In this case, an emulsifying agent is preferably excluded so that super-water repellency of the porous polymer can be achieved. The porous powder produced by a method known in the art, such as emulsion polymerization, has drawbacks in that the emulsifying agent irritates the skin because the use of the emulsifying agent is inevitable but the subsequent complete removal of the emulsifying agent is impossible, and the skin may get dry because the porous powder absorbs sebum of the skin as well as moisture. However, according to the present invention, there is no skin irritation caused by the emulsifying agent, only the sebum may be selectively absorbed due to super-water repellency, and cosmetic durability may be enhanced.
(20) Also, the porous polymer solution may be obtained by dissolving poly(methyl methacrylate) (PMMA) in a mixed solvent of dichloromethane (DCM) and hexanol. In this case, a mixing ratio (weight ratio) of the dichloromethane (DCM) and hexanol may be chosen in a range of 9:1 to 7:3. In this case, the hexanol serves to form pores in the porous polymer. Therefore, it is not desirable because the size of the pores may be too small when the ratio of the hexanol is less than 10% by weight of the total solvent, whereas the size of the pores may be too high when the ratio of the hexanol is greater than 30% by weight of the total solvent.
(21) In the present invention, porosity characteristics of the jade sphere may be controlled depending on conditions for a manufacturing process. The controllable porosity characteristics may include an average pore size, porosity, the total area of the pores, and the like. Specifically, the average pore size may be in a range of 15 to 800 nm, more preferably 250 to 600 nm, and the porosity may be in a range of 40 to 85%, more preferably 50 to 75%. Also, the total area of the pores may be in a range of 1 to 100 m.sup.2/g, more preferably 5 to 80 m.sup.2/g.
(22) The jade sphere having such characteristics may be effective in enhancing an oil absorption rate due to the pore size and porosity. The oil absorption rate may be expressed as an intrusion volume of mercury to be described below. The intrusion volume of mercury in the jade sphere according to the present invention may be measured to be in a range of 0.5 to 5 cm.sup.3/g, the value of which is at a reliable level so that the intrusion volume of mercury may be expressed as the oil absorption rate.
(23) Conventional porous polymers have a relatively larger specific surface area but have a smaller average pore size and porosity due to a single-sized mesoporous structure, but the jade sphere of the present invention is much more advantageous in absorbing oils through a capillary action because pore channels are formed due to a multiporous (Micro+Meso+Macro) structure.
(24) Cosmetic Composition
(25) The jade sphere may be applied as a cosmetic composition. In this case, the jade sphere is preferably included at a content of 0.1 to 5.0% by weight, based on the total weight of the cosmetics. When the jade powder is present at an excessive content, the inherent natures or softness of raw materials for cosmetics, and a sense of feeling in use upon application to the skin may be degraded, and an increase in unit price of products may also be caused due to expensive jade. On the other hand, when the jade powder is present at a very small content, it is undesirable because it is impossible to expect effects caused by the jade powder.
(26) Also, in addition to the jade powder, the cosmetic composition of the present invention may further include functional additives for improvement of skin conditions, such as improvement of skin wrinkles, improvement of skin whitening, improvement of skin elasticity, improvement of facial skin sagging, improvement of skin moisturizing, skin gloss improvement, skin aging prevention (e.g., inhibition of skin wrinkle formation and dermatosclerosis caused by photoaging), improvement of dark circles, and improvement of horny skin; functional additives for blocking ultraviolet (UV) rays; or components included in typical cosmetic compositions.
(27) The functional additives for improvement of skin conditions may include components selected from the group consisting of water-soluble vitamins, fat-soluble vitamins, high-molecular-weight peptides, high-molecular-weight polysaccharides, sphingolipids, natural extracts, and fermented materials. Also, the functional additive for blocking UV rays may further include inorganic powders such as titanium dioxide (TiO.sub.2), zinc oxide (ZnO), cerium oxide (CeO.sub.2), and the like. In addition, the components included in the typical cosmetic compositions may be further blended together with the functional additives, when necessary.
(28) Blending components included in addition to the aforementioned components may include oily components, moisturizing agents, emollients, surfactants, organic and inorganic pigments, organic powders, UV absorbing agents, preservatives, disinfectants, antioxidants, plant extracts, pH regulators, alcohols, dyes, fragrances, blood flow stimulants, cooling agents, anhydrotics, purified water, and the like, but the present invention is not limited thereto.
(29) The cosmetic composition including the jade sphere may be formulated into any one form selected from toners, lotions, creams, sera, emulsions, nourishing sera, powders, foundations, sprays, sunscreen agents, mask packs, gels, and the like, more preferably may be formulated into mask packs, sheet packs, sleeping packs, wash-off packs, peel-off packs, and the like, but is not limited to the formulations. In this case, such formulations may be properly chosen and changed depending on a purpose.
MODE FOR INVENTION
(30) Hereinafter, the present invention will be described in further detail with reference to specific embodiments thereof and the accompanying drawings. However, it will be apparent to those skilled in the art that the present invention is not limited to the embodiments disclosed below, but various modifications and changes can be made to the aforementioned embodiments of the present invention.
(31) Components listed in the following Table 1 were prepared to manufacture composite powders of Examples 1 and 2 below.
(32) TABLE-US-00001 TABLE 1 Jade powder (Chuncheon jade) Manufactured by Oksanga Co., Ltd. Poly(methyl methacrylate) Manufactured by LG PMMA (PMMA) Dichloromethane anhydrous Manufactured by Sigma-Aldrich (DCM) (Purity: >99.8%) Hexanol (or 1-hexanol) Manufactured by Sigma-Aldrich (Purity: >99%)
Example 1
(33) The components listed in Table 1 were prepared, and a jade sphere was manufactured according to the following spray drying method.
(34) Spray Drying
(35) 1) 40 g of PMMA was dissolved in 1 L of a solvent (DCM:hexanol=9:1 (% by weight)).
(36) 2) 40 g of jade powder was added to the PMMA solution, and then dispersed using a homogenizer.
(37) 3) The PMMA solution in which the jade powder was dispersed was spray-dried according to the conditions listed in the following Table 2.
(38) TABLE-US-00002 TABLE 2 Inside moisture 30% or more Inside temperature Maintained at room temperature Inside pressure 20 atm Feed rate 20% Aspirator 70%
(39) 4) The PMMA solution in which the jade powder was dispersed was continuously stirred during the spray drying using a stirring machine.
(40) 5) The spray-dried jade powder/PMMA composite powder particles were thoroughly washed, and then freeze-dried to completely remove a residual solvent, thereby obtaining the jade powder/PMMA composite powder.
Example 2
(41) The components listed in Table 1 were prepared, and a jade sphere was then manufactured according to the following electro-spraying method.
(42) Electro-Spraying
(43) 1) 0.4 g of PMMA was dissolved in 10 mL of a solvent (DCM:hexanol=9:1 (% by weight)).
(44) 2) 0.4 g of jade powder was added to the PMMA solution, and then dispersed using a sonicator.
(45) 3) The PMMA solution in which the jade powder was dispersed was electro-sprayed according to the conditions listed in the following Table 3.
(46) TABLE-US-00003 TABLE 3 Inside moisture 30% or more Inside temperature Maintained at room temperature Distance 15 cm Feed rate 20% Voltage 10 kV
(47) 4) The electro-sprayed jade powder/PMMA composite powder particles were thoroughly washed, and then freeze-dried to completely remove a residual solvent, thereby obtaining the powder/PMMA composite powder.
Comparative Example 1
(48) The jade powder listed in Table 1 was applied alone.
(49)
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(51) Tests on Items
(52) Hereinafter, tests on items of the jade sphere manufactured by the spray drying method were carried out.
(53) The reflectance spectra of subjects for tests were measured at a wavelength range of 360 to 740 nm using a color difference meter (ColorMate commercially available from Scinco Co., Ltd., Korea). Then, PC software, ColorMaster, was used to measure the reflectance. The reflectance was measured to calculate a light blocking rate in the corresponding spectrum.
(54) As shown in
(55) Whiteness is a value that one-dimensionally represents a degree of white color. In the reflectance test, a whiteness index was calculated based on XYZ color difference values in the entire visible light spectrum using the following equation.
WI=Y+800(x.sub.nx)+1,700(y.sub.ny)
X.sub.n=0.3101, Y.sub.n=0.3162 (C/2), X.sub.n=0.3138, Y.sub.n=0.3309 (C/2)<CIE Whiteness>
(56) As shown in
(57) To analyze porosity characteristics of the jade sphere of Example 1, a mercury (Hg) intrusion assay was performed. The intrusion volume of mercury, average pore size (4V/A, V: volume, and A: area) and porosity were measured using a porosimeter (Autopore IV 9500, Micrometrics, Londonderry, N.H., USA). The results are listed in Table 4.
(58) TABLE-US-00004 TABLE 4 Total intrusion volume 1.6797 mL/g Total pore area 15.125 m.sup.2/g Average pore diameter (4 V/A) 444.2 nm Bulk density at 0.20 psia 0.3832 g/mL Porosity 64.37%
(59) The term total intrusion volume refers to an amount of mercury intruded per unit gram, the term total pore area refers to a total pore area expressed as a cylindrical area, the term average pore diameter refers to an average value of the total pore sizes, and the term bulk density at 0.20 psia refers to a true density of a sample including pores at 0.20 psia.
(60) As a result, it can be seen that the jade sphere of Example 1 had an average pore size of 444.2 nm and a high porosity of 64.37%.
(61) One gram of the jade sphere of Example 1 was weighed using a scale and a Petri dish, and an absorption rate of oil required until the jade sphere of Example 1 got wet by dropping triglyceride oil having physical properties similar to the human sebum using a spuit was measured. In this case, the oil was stirred with a spatula so that the jade sphere of Example 1 was sufficiently wet with the oil.
(62) As shown in
(63) Hereinafter, the jade sphere manufactured in Example 1 was formulated into the form of an emulsion (for mask packs) based on the compositions (% by weight) listed in the following Table 5, and tests on items was then performed.
(64) TABLE-US-00005 TABLE 5 Comparative Comparative Formulation Formulation Formulation Items Component Example 1 Example 2 Example 1 Oily phase Cetearyl alcohol 4.00 4.00 4.00 part Stearic acid 0.50 0.50 0.50 Palmitic acid 0.50 0.50 0.50 Hydrogenated lecithin 1.00 1.00 1.00 Glyceryl stearate 1.50 1.50 1.50 Triethylhexanoin 3.00 3.00 3.00 Pentaerythrityl 4.00 4.00 4.00 tetraethylhexanoate Trisiloxane 2.00 2.00 2.00 Dimethicone 2.00 2.00 2.00 Aqueous fragrance Proper amount Proper amount Proper amount phase part purified water Proper amount Proper amount Proper amount Disodium EDTA 0.05 0.05 0.05 Glycerin 4.00 4.00 4.00 Propanediol 10.00 10.00 10.00 Other thickening and Proper amount Proper amount Proper amount neutralizing agents preservative Proper amount Proper amount Proper amount Chuncheon jade 0.00 1.00 0.00 Jade Sphere 0.00 0.00 1.00
(65) Thirty women of age from 25 to 35 years used the formulations of Comparative Formulation Examples 1 and 2 and Formulation Example 1 of the present invention twice a day for a month. Thereafter, the usability of the formulations as the cosmetics was evaluated in scores ranging from 1 to 5 by comparing the items such as adhesion, spreadability, softness, particle lumping, cosmetic durability, and the like. The results are listed in the following Table 6.
(66) TABLE-US-00006 TABLE 6 Particle Cosmetic Items Adhesion Spreadability Softness lumping durability Comparative 5 5 5 1 3 Formulation Example 1 Comparative 2 3 2 5 2 Formulation Example 2 Formulation 4 4 5 2 5 Example 1
(67) Looking at Table 6, it was revealed that the formulation of Comparative Formulation Example 2 including the Chuncheon jade powder had higher particle lumping and lower estimation values for all the items including adhesion, spreadability, softness and cosmetic durability, compared to the formulation of Comparative Formulation Example 1 including no jade powder. On the other hand, it was revealed that the formulation of Formulation Example 1 including the jade sphere had significantly reduced particle lumping and improved adhesion and spreadability, compared to the formulation of Comparative Formulation Example 2 including the Chuncheon jade powder, and had similar or improved softness and cosmetic durability, compared to the formulation of Comparative Formulation Example 1.
(68) Therefore, the jade sphere of the present invention had excellent outcomes such as softness derived from the spherical shape thereof, and cosmetic durability derived from the oil absorption of sebum caused due to high porosity thereof. Also, it can be seen that a white cast may be prevented by significantly improving the particle lumping which had been considered as the biggest problem of the formulation of Comparative Formulation Example 2 including the jade powder.
(69) To measure light-blocking rates of the formulations of Comparative Formulation Examples 1 and 2 and Formulation Example 1 in the visible light spectrum, the reflectance spectra of subjects for tests were measured at a wavelength range of 360 to 740 nm using a color difference meter (ColorMate commercially available from Scinco Co., Ltd., Korea). Then, PC software, ColorMaster, was used to measure the reflectance.
(70) As shown in
(71) Whiteness of a formulation is a value that one-dimensionally represents a degree of white color. In the reflectance test of the formulation, a whiteness index was calculated based on XYZ color difference values in the entire visible light spectrum using the following equation.
WI=Y+800(x.sub.nx)+1,700(y.sub.ny)
X.sub.n=0.3101, Y.sub.n=0.3162(C/2), X.sub.n=0.3138, Y.sub.n=0.3309(C/2)<CIE Whiteness>
(72) As shown in
Formulation Example 2
(73) Hereinafter, a face lotion containing 0.1% by weight of the jade sphere manufactured in Example 1 was manufactured based on the compositions (% by weight) listed in the following Table 7 using a conventional method.
(74) TABLE-US-00007 TABLE 7 Component content (% by weight) Purified water Balance Glycerin 8.0 Butylene glycol 4.0 Hyaluronic acid extract 5.0 -Glucan 7.0 Carbomer 0.1 Glucoceramide & 7,8,4-trihydroxyisoflavone 0.05 Caprylic/capric triglyceride 8.0 Squalane 5.0 Cetearyl glucoside 1.5 Sorbitan stearate 0.4 Cetearyl alcohol 1.0 Triethanolamine 0.1 Jade Sphere 0.1
Formulation Example 3
(75) Hereinafter, a nourishing cream containing 3.0% by weight of the jade sphere manufactured in Example 1 was manufactured based on the compositions (% by weight) listed in the following Table 8 using a conventional method.
(76) TABLE-US-00008 TABLE 8 Component Content (% by weight) Purified water Balance Glycerin 3.0 Butylene glycol 3.0 Liquid paraffin 7.0 B-glucan 7.0 Carbomer 0.1 Glucoceramide & 7,8,4-trihydroxyisoflavone 3.0 Caprylic/capric triglyceride 3.0 Squalane 5.0 Cetearyl glucoside 1.5 Sorbitan stearate 0.4 Polysorbate 60 1.2 Triethanolamine 0.1 Jade sphere 3.0
Formulation Example 4
(77) Hereinafter, a massage cream containing 5.0% by weight of the jade sphere manufactured in Example 1 was manufactured based on the compositions (% by weight) listed in the following Table 9 using a conventional method.
(78) TABLE-US-00009 TABLE 9 Component Content (% by weight) Purified water Balance Glycerin 8.0 Butylene glycol 4.0 Liquid paraffin 45.0 B-glucan 7.0 Carbomer 0.1 Glucoceramide & 7,8,4-trihydroxyisoflavone 1.0 Caprylic/capric triglyceride 3.0 Wax 4.0 Cetearyl glucoside 1.5 Sorbitan sesquioleate 0.9 Vaseline 3.0 Paraffin 1.5 Jade sphere 5.0