KR20100047799A - Plate-like brown pigment - Google Patents

Plate-like brown pigment Download PDF

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KR20100047799A
KR20100047799A KR1020090100020A KR20090100020A KR20100047799A KR 20100047799 A KR20100047799 A KR 20100047799A KR 1020090100020 A KR1020090100020 A KR 1020090100020A KR 20090100020 A KR20090100020 A KR 20090100020A KR 20100047799 A KR20100047799 A KR 20100047799A
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South Korea
Prior art keywords
plate
pigment
acid
extract
brown pigment
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KR1020090100020A
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Korean (ko)
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아키코 스미요시
다카유키 구메이
다쿠미 다나카
겐지 니시모토
츠기오 사토
슈 인
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가부시키가이샤환케루
고쿠리츠다이가쿠호진 도호쿠다이가쿠
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Publication of KR20100047799A publication Critical patent/KR20100047799A/en

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36Compounds of titanium
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0216Solid or semisolid forms
    • A61K8/022Powders; Compacted Powders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241Containing particulates characterized by their shape and/or structure
    • A61K8/0254Platelets; Flakes
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/02Preparations containing skin colorants, e.g. pigments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/42Colour properties
    • A61K2800/43Pigments; Dyes

Abstract

PURPOSE: A plate-type brown pigment and a cosmetic material containing thereof is provided to improve protecting effect for the skin of a user from ultraviolet light, the polishing ability, and to prevent color changes by wetting. CONSTITUTION: A plate-type brown pigment has a structure marked as the chemical formula: K_(3x+y)Li_xTi_(2-x-y)Fe_yO_4. X and Y in the formula is in the range of 0.2<=x<=0.3, 0.05<=y<=0.5, respectively. The average thickness of the pigment is 0.1~1 microns. The average large diameter of the pigment is 10~100 microns. A cosmetic material and a powder cosmetic material contain the plate-type brown pigment.

Description

판상 갈색계 안료{Plate-like brown pigment}Plate-like brown pigment

본 발명은 판상 갈색계 안료 및 그것을 함유하는 화장료에 관한 것이다.The present invention relates to a plate-like brown pigment and a cosmetic containing the same.

화장료에는 각종 착색 안료가 사용되고 있다. 예를 들면, 색 불균일이 없고, 미끄러짐성(滑性)이 좋은 산화철을 피복한 판상 황산바륨(특허문헌 1: 일본국 특허공개 제2000-265154호 공보), 자외선 차폐효과가 우수하고, 전착성(展着性), 배향성(配向性), 은폐성이 우수한 금속화합물을 저결정성의 실리카에 의해 내포해서 복합화한 입자(특허문헌 2: 일본국 특허공개 평11-11927호 공보), 사용시에 색조의 거무칙칙함 등이 없고, 색조의 선명함을 유지할 수 있는 불소화합물로 표면처리한 착색료(특허문헌 3: 일본국 특허공개 평3-246210호 공보), 백색 안료와 유색 안료의 색 분리 방지를 개선한 철 함유 이산화티탄(특허문헌 4: 일본국 특허공개 평7-69636호 공보) 등이 사용되고 있다.Various coloring pigments are used for cosmetics. For example, plate-shaped barium sulfate coated with iron oxide having no slippage and good slipperiness (Patent Document 1: Japanese Patent Laid-Open No. 2000-265154), excellent ultraviolet shielding effect, and electrodeposition property Particles incorporating and compounding a metal compound excellent in exhibition property, orientation, and concealability with low crystalline silica (Patent Document 2: Japanese Patent Application Laid-open No. Hei 11-11927), color tone at the time of use A colorant surface-treated with a fluorine compound that can maintain the vividness of color without the dullness and the like (Patent Document 3: Japanese Patent Application Laid-Open No. 3-246210), improving the prevention of color separation of white and colored pigments. Iron containing titanium dioxide (patent document 4: Unexamined-Japanese-Patent No. 7-69636) etc. are used.

한편, 레피도크로사이트형(Lepidocrocite-type) 판상 티탄산에 대해서 발명자 등은 연구 개발을 계속해서 실시하고 있으며, 자외선 차폐효과가 우수하고, 미끄러짐성이 좋은 레피도크로사이트형 판상 티탄산으로서 특허문헌 5(일본국 특허공개 제2006-316107호 공보), 광휘성(光輝性) 안료로서 특허문헌 6(일본국 특허공개 제2008-162971호 공보)을 제안하고 있다. 또한, 제조방법으로서 특허문헌 7, 8(일본국 특허 제3062497호 공보, 일본국 특허 제4091337호 공보)이 알려져 있다. 레피도크로사이트형 판상 티탄산에 대해서, 착색 안료로서의 응용은 이루어지고 있지 않다.On the other hand, the inventors, etc., continue to carry out research and development on the lepidocrocite-type plate-like titanic acid, and the patent document 5 as a lepidocrocite-type plate-like titanic acid having excellent ultraviolet shielding effect and good slipperiness. (Japanese Patent Laid-Open No. 2006-316107) and Patent Document 6 (Japanese Patent Laid-Open No. 2008-162971) have been proposed as a bright pigment. Moreover, patent document 7, 8 (Japanese Patent No. 3062497 and Japanese Patent No. 4091337) is known as a manufacturing method. The application as a coloring pigment is not made about the lepidocrocite plate-like titanic acid.

[특허문헌 1] 일본국 특허공개 제2000-265154호 공보[Patent Document 1] Japanese Unexamined Patent Publication No. 2000-265154

[특허문헌 2] 일본국 특허공개 평11-11927호 공보[Patent Document 2] Japanese Patent Application Laid-Open No. 11-11927

[특허문헌 3] 일본국 특허공개 평3-246210호 공보[Patent Document 3] Japanese Patent Application Laid-Open No. 3-246210

[특허문헌 4] 일본국 특허공개 평7-69636호 공보[Patent Document 4] Japanese Patent Application Laid-Open No. 7-69636

[특허문헌 5] 일본국 특허공개 제2006-316107호 공보[Patent Document 5] Japanese Patent Publication No. 2006-316107

[특허문헌 6] 일본국 특허공개 제2008-162971호 공보[Patent Document 6] Japanese Patent Publication No. 2008-162971

[특허문헌 7] 일본국 특허 제3062497호 공보[Patent Document 7] Japanese Patent No. 3062497

[특허문헌 8] 일본국 특허 제4091337호 공보[Patent Document 8] Japanese Patent No. 4091337

레피도크로사이트형 판상 티탄산을 사용한 안료 및 그것을 함유하는 화장료를 제공하는 것을 목적으로 한다.It is an object to provide a pigment using a lepidocrocite plate-like titanic acid and a cosmetic containing the same.

상기 과제를 해결하기 위해 본 발명은 이하의 구성을 구비하고 있다.MEANS TO SOLVE THE PROBLEM In order to solve the said subject, this invention is equipped with the following structures.

(1) 화학식 K3x + yLixTi2 -x- yFeyO4(단, 0.2≤x≤0.3, 0.05≤y≤0.5)의 판상 갈색계 안료.(1) A plate-like brown pigment of the formula K 3x + y Li x Ti 2 -x- y Fe y O 4 (0.2≤x≤0.3, 0.05≤y≤0.5).

(2) 색조가 L*a*b* 표색계에 있어서 a*=4~15, b*=15~26인 것을 특징으로 하는 (1)에 기재된 판상 갈색계 안료.(2) The plate-like brown pigment according to (1), wherein the color tone is a * = 4 to 15 and b * = 15 to 26 in an L * a * b * color system.

(3) 입자의 평균 두께가 0.1 ㎛~1 ㎛, 평균 장경(長徑)이 10 ㎛~100 ㎛인 것을 특징으로 하는 (1) 또는 (2)에 기재된 판상 갈색계 안료.(3) The plate-shaped brown pigment as described in (1) or (2) whose average thickness of particle | grains is 0.1 micrometer-1 micrometer, and average long diameter is 10 micrometers-100 micrometers.

(4) (1) 내지 (3) 중 어느 하나에 기재된 판상 갈색계 안료를 함유하는 화장료.(4) Cosmetics containing the plate-like brown pigment as described in any one of (1)-(3).

(5) (1) 내지 (3) 중 어느 하나에 기재된 판상 갈색계 안료를 함유하는 분말 화장료.(5) Powder cosmetics containing the plate-like brown pigment as described in any one of (1)-(3).

자외선 차폐효과를 갖고, 미끄러짐성이 우수하며, 광택성이 우수하고, 젖음에 의한 색조 변화가 적은 레피도크로사이트형 판상 티탄산을 사용한 안료를 실현할 수 있었다. 그리고, 그것을 함유하는 화장료를 제공할 수 있다. 색은 갈색계이다.The pigment using the lepidocrocite-type plate titanic acid which has the ultraviolet-ray shielding effect, is excellent in slipperiness | lubricacy, is excellent in glossiness, and has little change in the color tone by wetness can be achieved. And the cosmetics containing it can be provided. The color is brown.

본 발명의 안료는, 화학식 K3x+yLixTi2-x-yFeyO4(단, 0.2≤x≤0.3, 0.05≤y≤0.5)의 레피도크로사이트형 판상 티탄산 결정입자가 유용한 판상 갈색계 안료이다. L*a*b* 표색계에 있어서 a*=4~15, b*=15~26인 착색 안료를 제공할 수 있다. 평균 두께가 0.1 ㎛~1 ㎛, 평균 장경이 10 ㎛~100 ㎛로서, 매끄러워 우수한 미끄러짐성을 발휘할 수 있다.The pigment of the present invention is a plate-like brown in which the repidocrosite-type plate titanic acid crystal particles of the general formula K 3x + y Li x Ti 2-xy Fe y O 4 (0.2≤x≤0.3, 0.05≤y≤0.5) are useful. Pigments. A colored pigment whose a * = 4-15 and b * = 15-26 can be provided in a L * a * b * color system. 0.1 micrometer-1 micrometer of average thickness, and 10 micrometers-100 micrometers of average long diameters are smooth and can exhibit the outstanding slipperiness | lubricacy.

이와 같은 안료는, 자외선 차폐성이 양호하고, 젖음에 의한 색 변화가 적으며, 피부 도포성능이 양호하기 때문에, 화장료용 안료로서 우수하고, 분말 화장료로서 적합하다. 정상적인 피부색을 나타내는 착색 안료로서 배합하는 것이 적합하다.Such a pigment is excellent as a pigment for cosmetics and is suitable as a powder cosmetic since it has good ultraviolet shielding property, little color change by wetness, and good skin coating performance. It is suitable to mix | blend as a coloring pigment which shows normal skin color.

본 발명의 판상 갈색계 안료는 레피도크로사이트형(Lepidocrocite-type) 판상 티탄산 결정입자로서, 다음의 화학식으로 표시된다. K3x+yLixTi2-x-yFeyO4(단, 0.2≤x≤0.3, 0.05≤y≤0.5).The plate-like brown pigment of the present invention is a lepidocrocite-type plate-shaped titanic acid crystal grain, and is represented by the following formula. K 3x + y Li x Ti 2-xy Fe y O 4 , provided 0.2 ≦ x ≦ 0.3, 0.05 ≦ y ≦ 0.5.

본 발명의 판상 갈색계 안료는 옅은 갈색 내지 짙은 갈색이고, 색조가 L*a*b* 표색계에 있어서 a*=4~15, b*=15~26인 것이 바람직하다.It is preferable that the plate-shaped brown pigment of this invention is light brown to dark brown, and a hue is a * = 4-15 and b * = 15-26 in L * a * b * color system.

본 발명의 판상 갈색계 안료는 평균 두께가 0.1 ㎛~1 ㎛, 평균 장경이 10 ㎛~100 ㎛인 것이 바람직하다.It is preferable that the plate-shaped brown pigment of this invention is 0.1 micrometer-1 micrometer in average thickness, and 10 micrometer-100 micrometers in average long diameter.

본 발명의 판상 갈색계 안료의 지름의 측정은 이하의 방법에 의한다. 주사형 전자현미경 관찰에 의해, 그 입자의 판상면에 있어서 최장부분의 길이의 평균값을 평균 장경, 그 입자의 두께방향의 최장의 평균값을 평균 두께로 하였다.The diameter of the plate-shaped brown pigment of the present invention is measured by the following method. By scanning electron microscope observation, the average value of the longest part and the longest average value in the thickness direction of the particle | grains were made into the average thickness in the plate-shaped surface of the particle | grains.

본 발명의 판상 갈색계 안료는, 예를 들면 소정비의 K2CO3, Li2CO3, TiO2, FeCl2 등의 주원료와 플럭스로서 예를 들면 K2MoO4, NaCl, KCl 등을 혼합하여 900℃~1100℃에서 수시간 반응시킨 후, 플럭스성분을 세정하여 얻을 수 있으나, 보다 안정된 형상의 입자를 형성하기 위해서는, 바람직하게는 KCl을 플럭스로 하는 것이 좋다.The plate-like brown pigment of the present invention is mixed with, for example, K 2 MoO 4 , NaCl, KCl, etc. as a main raw material such as K 2 CO 3 , Li 2 CO 3 , TiO 2 , FeCl 2 , and the flux at a predetermined ratio. After the reaction at 900 ° C to 1100 ° C for several hours, the flux component may be washed and obtained. However, in order to form particles having a more stable shape, KCl is preferably used as the flux.

본 발명의 판상 갈색계 안료는, 유제나 물로의 친화성을 향상시키거나, 화장료에 내수성, 내유성을 부여하기 위해서 일반유제처리, 금속비누처리, 실리콘화합물처리, 알킬인산처리, 퍼플루오로알킬기를 갖는 화합물처리, 아미노산처리, 레시틴처리, 콜라겐처리 등의 표면처리를 한 후에 사용해도 된다.The plate-like brown pigment of the present invention has a general emulsion treatment, a metal soap treatment, a silicon compound treatment, an alkyl phosphate treatment, a perfluoroalkyl group in order to improve affinity to an oil or water, or to impart water resistance and oil resistance to a cosmetic. You may use after surface treatment, such as a compound treatment which has a compound, an amino acid treatment, a lecithin treatment, and a collagen treatment.

본 발명의 화장료에는, 식물유와 같은 유지류, 고급지방산, 고급알코올, 실리콘, 음이온 계면활성제, 양이온 계면활성제, 양성 계면활성제, 비이온 계면활성제, 방부제, 당류, 금속이온봉쇄제, 수용성 고분자와 같은 고분자, 증점제, 분체성분, 자외선 흡수제, 자외선 차단제, 히알루론산과 같은 보습제, 향료, pH 조정제 등을 함유시킬 수 있다. 비타민류, 피부 부활제(賦活劑), 혈행촉진제, 상재균 컨트롤제, 활성산소 소거제, 항염증제, 미백제, 살균제 등의 다른 약효성분, 생리활성성분을 함유시키는 것도 가능하다.The cosmetics of the present invention include polymers such as fats and oils such as vegetable oils, higher fatty acids, higher alcohols, silicones, anionic surfactants, cationic surfactants, amphoteric surfactants, nonionic surfactants, preservatives, sugars, metal ion blocking agents, and water-soluble polymers. , Thickeners, powder components, ultraviolet absorbers, sunscreens, moisturizers such as hyaluronic acid, fragrances, pH adjusters and the like. It is also possible to contain other active ingredients such as vitamins, skin activators, blood stimulators, fungus control agents, active oxygen scavengers, anti-inflammatory agents, whitening agents, fungicides, and physiologically active ingredients.

유지류로서, 예를 들면, 동백 기름, 달맞이꽃 기름, 마카다미아너트 오일, 올리브유, 평지씨유, 옥수수유, 참기름, 호호바유, 배아유, 소맥배아유, 트리옥탄 산글리세린 등의 액체유지, 카카오버터, 야자유, 경화야자유, 팜유, 팜핵유, 목랍, 목랍 핵유, 경화유, 경화피마자유 등의 고체유지, 밀랍, 칸델릴라왁스, 면왁스, 쌀겨왁스, 라놀린, 초산라놀린, 액상라놀린, 사탕수수왁스 등의 왁스류를 들 수 있다. 탄화수소류로서, 예를 들면, 유동파라핀, 스쿠알렌, 스쿠알란, 마이크로크리스탈린왁스 등을 들 수 있다.As fats and oils, For example, liquid oils, such as camellia oil, evening primrose oil, macadamia nut oil, olive oil, rapeseed oil, corn oil, sesame oil, jojoba oil, germ oil, wheat germ oil, and triglycerol acid triglyceride, Solid oils such as palm oil, hardened palm oil, palm oil, palm kernel oil, wax, wax core oil, hardened oil, hardened castor oil, beeswax, candelilla wax, cotton wax, rice bran wax, lanolin, lanolin acetate, liquid lanolin, sugar cane wax Waxes are mentioned. Examples of the hydrocarbons include liquid paraffin, squalene, squalane, microcrystalline wax, and the like.

고급지방산으로서, 예를 들면, 라우르산, 미리스트산, 팔미트산, 스테아르산, 올레산, 리놀산, 리놀렌산, 도코사헥사엔산(DHA), 에이코사펜타엔산(EPA) 등을 들 수 있다.Examples of higher fatty acids include lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid, docosahexaenoic acid (DHA), eicosapentaenoic acid (EPA), and the like. have.

고급알코올로서, 예를 들면, 라우릴알코올, 스테아릴알코올, 세틸알코올, 세토스테아릴알코올 등의 직쇄 알코올, 모노스테아릴글리세린에테르, 라놀린알코올, 콜레스테롤, 피토스테롤, 옥틸도데칸올 등의 분지쇄 알코올 등을 들 수 있다.As the higher alcohol, for example, straight chain alcohols such as lauryl alcohol, stearyl alcohol, cetyl alcohol, cetostearyl alcohol, monostearyl glycerin ether, lanolin alcohol, branched chain alcohols such as cholesterol, phytosterol and octyldodecanol Etc. can be mentioned.

실리콘으로서, 예를 들면, 쇄상 폴리실록산의 디메틸폴리실록산, 메틸페닐폴리실록산 등, 환상 폴리실록산의 데카메틸시클로펜타실록산 등을 들 수 있다.As silicone, decamethyl cyclopentasiloxane of cyclic polysiloxane, etc. are mentioned, for example, dimethyl polysiloxane of linear polysiloxane, and methylphenyl polysiloxane.

음이온 계면활성제로서, 예를 들면, 라우르산나트륨 등의 지방산염, 라우릴황산나트륨 등의 고급알킬황산에스테르염, POE 라우릴황산트리에탄올아민 등의 알킬에테르황산에스테르염, N-아실살콕신산, 설포숙신산염, N-아실아미노산염 등을 들 수 있다.As an anionic surfactant, For example, fatty acid salts, such as sodium laurate, higher alkyl sulfate ester salts, such as sodium lauryl sulfate, alkyl ether sulfate ester salts, such as POE lauryl sulfate triethanolamine, N-acylsulfonic acid, and sulfo Succinate, N-acylamino acid salt, etc. are mentioned.

양이온 계면활성제로서, 예를 들면, 염화스테아릴트리메틸암모늄 등의 알킬트리메틸암모늄염, 염화벤잘코늄, 염화벤제토늄 등을 들 수 있다.As a cationic surfactant, alkyltrimethylammonium salts, such as stearyl trimethylammonium chloride, benzalkonium chloride, benzetonium chloride, etc. are mentioned, for example.

양성 계면활성제로서, 예를 들면, 알킬베타인, 아미도베타인 등의 베타인계 계면활성제 등을 들 수 있다.As amphoteric surfactant, betaine-type surfactant, such as alkylbetaine and amidobetaine, etc. are mentioned, for example.

비이온 계면활성제로서, 예를 들면, 소르비탄모노올레에이트 등의 소르비탄지방산에스테르류, 경화피마자유 유도체 등을 들 수 있다.As a nonionic surfactant, sorbitan fatty acid esters, such as sorbitan monooleate, a hardened castor oil derivative, etc. are mentioned, for example.

방부제로서, 예를 들면, 메틸파라벤, 에틸파라벤 등을 들 수 있다.As a preservative, methyl paraben, ethyl paraben, etc. are mentioned, for example.

금속이온봉쇄제로서, 예를 들면, 에틸렌디아민사초산이나트륨, 에데트산, 에데트산나트륨염 등의 에데트산염을 들 수 있다.As a metal ion blocking agent, edetate salts, such as ethylenediamine disodium tetraacetate, edetic acid, a sodium edate salt, are mentioned, for example.

고분자로서, 예를 들면, 아라비아검, 트래거캔스검, 갈락탄, 구아검, 카라기난, 펙틴, 한천, 퀸스시드, 덱스트란, 플루란, 카르복시메틸전분, 콜라겐, 카제인, 젤라틴, 메틸셀룰로오스, 메틸히드록시프로필셀룰로오스, 히드록시에틸셀룰로오스, 카르복시메틸셀룰로오스나트륨(CMC), 알긴산나트륨, 카르복시비닐폴리머(CARBOPOL 등) 등의 비닐계 고분자 등을 들 수 있다.As the polymer, for example, gum arabic, tragacanth gum, galactan, guar gum, carrageenan, pectin, agar, queen's seed, dextran, pullulan, carboxymethyl starch, collagen, casein, gelatin, methylcellulose, methylhydride And vinyl polymers such as hydroxypropyl cellulose, hydroxyethyl cellulose, sodium carboxymethyl cellulose (CMC), sodium alginate, and carboxyvinyl polymer (such as CARBOPOL).

증점제로서, 카라기난, 트래거캔스검, 퀸스시드, 카제인, 덱스트린, 젤라틴, CMC, 히드록시에틸셀룰로오스, 히드록시프로필셀룰로오스, 구아검, 크산탄검, 벤토나이트 등을 들 수 있다.Examples of the thickener include carrageenan, tragacanth gum, queen's seed, casein, dextrin, gelatin, CMC, hydroxyethyl cellulose, hydroxypropyl cellulose, guar gum, xanthan gum and bentonite.

분말성분으로서, 예를 들면, 탈크, 카올린, 마이카, 실리카, 제올라이트, 폴리에틸렌 분말, 폴리스티렌 분말, 셀룰로오스 분말, 무기 백색 안료, 무기 적색계 안료, 산화티탄 코티드 마이카, 산화티탄 코티드 탈크, 착색산화티탄 코티드 마이카 등의 펄 안료, 적색 201호, 적색 202호 등의 유기 안료를 들 수 있다.As the powder component, for example, talc, kaolin, mica, silica, zeolite, polyethylene powder, polystyrene powder, cellulose powder, inorganic white pigment, inorganic red pigment, titanium oxide coated mica, titanium oxide coated talc, colored titanium oxide Pearl pigments, such as a coated mica, Organic pigments, such as red 201 and red 202, are mentioned.

자외선 흡수제로서, 예를 들면, 파라아미노안식향산, 살리실산페닐, 파라메톡시계피산이소프로필, 파라메톡시계피산옥틸, 2,4-디히드록시벤조페논 등을 들 수 있다.As a ultraviolet absorber, paraamino benzoic acid, phenyl salicylate, isopropyl paramethoxy cinnamic acid, octyl paramethoxy cinnamic acid, 2, 4- dihydroxy benzophenone, etc. are mentioned, for example.

자외선 차단제로서, 예를 들면, 산화티탄, 탈크, 카민, 벤토나이트, 카올린, 산화아연 등을 들 수 있다.As a sunscreen agent, titanium oxide, talc, carmine, bentonite, kaolin, zinc oxide, etc. are mentioned, for example.

보습제로서, 예를 들면, 폴리에틸렌글리콜, 프로필렌글리콜, 디프로필렌글리콜, 1,3-부틸렌글리콜, 1,2-펜탄디올, 글리세린, 디글리세린, 폴리글리세린, 크실리톨, 말티톨, 말토오스, 소르비톨, 포도당, 과당, 콘드로이틴황산나트륨, 히알루론산나트륨, 젖산나트륨, 피롤리돈카르복실산, 시클로덱스트린 등을 들 수 있다.As the humectant, for example, polyethylene glycol, propylene glycol, dipropylene glycol, 1,3-butylene glycol, 1,2-pentanediol, glycerin, diglycerin, polyglycerine, xylitol, maltitol, maltose, sorbitol, Glucose, fructose, sodium chondroitin sulfate, sodium hyaluronate, sodium lactate, pyrrolidone carboxylic acid, cyclodextrin, etc. are mentioned.

약효성분으로서, 예를 들면, 비타민 A유, 레티놀 등의 비타민 A류, 리보플라빈 등의 비타민 B2류, 피리독신 염산염 등의 B6류, L-아스코르브산, L-아스코르브산 인산에스테르, L-아스코르브산 모노팔미트산에스테르, L-아스코르브산 디팔미트산에스테르, L-아스코르브산-2-글루코시드 등의 비타민 C류, 판토텐산칼슘 등의 판토텐산류, 비타민 D2, 콜레칼시페롤 등의 비타민 D류, α-토코페롤, 초산토코페롤, 니코틴산 DL-α-토코페롤 등의 비타민 E류 등의 비타민류를 들 수 있다.Examples of the active ingredient include vitamin A oils such as vitamin A oil and retinol, vitamin B 2 such as riboflavin, B 6 such as pyridoxine hydrochloride, L-ascorbic acid, L-ascorbic acid phosphate ester and L-ascorb. Vitamin C such as acid monopalmitic acid ester, L-ascorbic acid dipalmitate, L-ascorbic acid-2-glucoside, pantothenic acid such as calcium pantothenate, vitamin D 2 such as vitamin D 2 and cholecalciferol And vitamins such as vitamin E, such as α-tocopherol, tocopherol acetate, and nicotinic acid DL-α-tocopherol.

플라센타 추출물, 글루타티온, 범의귀 추출물 등의 미백제, 로열젤리, 너도밤나무 추출물 등의 피부 부활제, 캡사이신, 진게론, 칸타리스팅크, 이크타몰, 카페인, 탄닌산, γ-오리자놀 등의 혈행촉진제, 글리시리진산 유도체, 글리시레틴산 유도체, 아줄렌 등의 소염제, 알기닌, 세린, 류신, 트립토판 등의 아미노산류, 상재균 컨트롤제의 말토오스 수크로오스 축합물, 염화리소자임 등을 들 수 있다.Whitening agents such as placenta extract, glutathione and panaxanthus extract, skin activators such as royal jelly and beech extract, blood stimulants such as capsaicin, gingeron, canthalistine, iktamol, caffeine, tannic acid, γ-orizanol, and glycyrrhizin derivatives And anti-inflammatory agents such as glycyrrhetinic acid derivatives and azulene, amino acids such as arginine, serine, leucine and tryptophan, maltose sucrose condensates of the fungus control agent, and lysozyme chloride.

또한, 카밀레 추출물, 파슬리 추출물, 와인효모 추출물, 그레이프후르츠 추 출물, 인동 추출물, 쌀 추출물, 포도 추출물, 홉 추출물, 쌀겨 추출물, 비파 추출물, 황벽나무 추출물, 의이인 추출물, 자주쓴풀 추출물, 멜리로트 추출물, 버치 추출물, 감초 추출물, 작약 추출물, 비누풀 추출물, 수세미외 추출물, 고추 추출물, 레몬 추출물, 겐티아나 추출물, 차조기 추출물, 알로에 추출물, 로즈마리 추출물, 세이지 추출물, 타임 추출물, 차 추출물, 해조 추출물, 오이 추출물, 정향 추출물, 인삼 추출물, 마로니에 추출물, 하마멜리스 추출물, 뽕나무 추출물 등의 각종 추출물을 들 수 있다.In addition, chamomile extract, parsley extract, wine yeast extract, grapefruit extract, honeysuckle extract, rice extract, grape extract, hop extract, rice bran extract, loquat extract, rhubarb extract, oyster extract, barberry extract, melilot extract, birch Extract, Licorice Extract, Peony Extract, Soap Extract, Scrubber Extract, Pepper Extract, Lemon Extract, Gentian Extract, Perilla Extract, Aloe Extract, Rosemary Extract, Sage Extract, Thyme Extract, Tea Extract, Seaweed Extract, Cucumber Extract, Clove Various extracts, such as extract, ginseng extract, horse chestnut extract, hamamelis extract, and mulberry extract, are mentioned.

실시예Example

[실시예 1]Example 1

TiO2: 3.4054 g, Li2CO3: 0.24 g, K2CO3: 1.355 g, KCl: 5 g, FeCl2·4H2O: 0.34 g을 칭량(稱量)하고, 유발(乳鉢)을 사용해서, 약 10분간 혼합하였다. 1000℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 분체를 80℃의 온수에서 추가적으로 약 15분간 교반하였다. 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0 .835Li0 .256Ti1 .677Fe0 .067O4이다.TiO 2 : 3.4054 g, Li 2 CO 3 : 0.24 g, K 2 CO 3 : 1.355 g, KCl: 5 g, FeCl 2 · 4H 2 O: 0.34 g were weighed, and the trigger was used. The mixture was mixed for about 10 minutes. It baked at 1000 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration, and the powder was further stirred for about 15 minutes in warm water at 80 ° C. The powder was separated by filtration and dried at 150 ° C for 1 hour. The composition formula of the obtained plate-like brown pigments is K 0 .835 Li 0 .256 Ti 1 .677 Fe 0 .067 O 4.

[실시예 2][Example 2]

TiO2: 6.81 g, Li2CO3: 0.48 g, K2CO3: 2.71 g, KCl: 11.388 g, Fe(No3)3·9H2O: 1.388 g을 칭량하고, 유발을 사용해서, 약 30분간 혼합하였다. 950℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 3시간 교반하였다. 얻어진 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0 .835Li0 .256Ti1 .677Fe0 .067O4이다.TiO 2 : 6.81 g, Li 2 CO 3 : 0.48 g, K 2 CO 3 : 2.71 g, KCl: 11.388 g, Fe (No 3 ) 3 .9H 2 O: 1.388 g, were weighed and used in a mortar to Mix for 30 minutes. It baked at 950 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 3 hours. The obtained powder was separated by filtration and dried at 150 ° C. for 1 hour. The composition formula of the obtained plate-like brown pigments is K 0 .835 Li 0 .256 Ti 1 .677 Fe 0 .067 O 4.

[실시예 3]Example 3

TiO2: 6.81 g, Li2CO3: 0.48 g, K2CO3: 2.71 g, KCl: 11.388 g, Fe(No3)3·9H2O: 1.388 g을 칭량하고, 유발을 사용해서, 약 30분간 혼합하였다. 1100℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 3시간 교반하였다. 얻어진 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0 .835Li0 .256Ti1 .677Fe0 .067O4이다.TiO 2 : 6.81 g, Li 2 CO 3 : 0.48 g, K 2 CO 3 : 2.71 g, KCl: 11.388 g, Fe (No 3 ) 3 .9H 2 O: 1.388 g, were weighed and used in a mortar to Mix for 30 minutes. It calcined at 1100 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 3 hours. The obtained powder was separated by filtration and dried at 150 ° C. for 1 hour. The composition formula of the obtained plate-like brown pigments is K 0 .835 Li 0 .256 Ti 1 .677 Fe 0 .067 O 4.

[실시예 4]Example 4

TiO2: 3.405 g, Li2CO3: 0.24 g, K2CO3: 1.355 g, KCl: 5.6068 g, Fe(CH3COCHCOCH3)3: 0.6068 g을 칭량하고, 유발을 사용해서, 약 30분간 혼합하였다. 950℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 3시간 교반하였다. 얻어진 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0 .835Li0 .256Ti1 .677Fe0 .067O4이다.TiO 2 : 3.405 g, Li 2 CO 3 : 0.24 g, K 2 CO 3 : 1.355 g, KCl: 5.6068 g, Fe (CH 3 COCHCOCH 3 ) 3 : 0.6068 g was weighed, and used for the firing, about 30 minutes Mixed. It baked at 950 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 3 hours. The obtained powder was separated by filtration and dried at 150 ° C. for 1 hour. The composition formula of the obtained plate-like brown pigments is K 0 .835 Li 0 .256 Ti 1 .677 Fe 0 .067 O 4.

[실시예 5]Example 5

TiO2: 3.405 g, Li2CO3: 0.24 g, K2CO3: 1.355 g, KCl: 5.6068 g, Fe(CH3COCHCOCH3)3: 0.6068 g을 칭량하고, 유발을 사용해서, 약 30분간 혼합하였다. 1100℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 3시간 교반하였다. 얻어진 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0 .835Li0 .256Ti1 .677Fe0 .067O4이다.TiO 2 : 3.405 g, Li 2 CO 3 : 0.24 g, K 2 CO 3 : 1.355 g, KCl: 5.6068 g, Fe (CH 3 COCHCOCH 3 ) 3 : 0.6068 g was weighed, and used for the firing, about 30 minutes Mixed. It calcined at 1100 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 3 hours. The obtained powder was separated by filtration and dried at 150 ° C. for 1 hour. The composition formula of the obtained plate-like brown pigments is K 0 .835 Li 0 .256 Ti 1 .677 Fe 0 .067 O 4.

[실시예 6]Example 6

TiO2: 3.405 g, Li2CO3: 0.24 g, K2CO3: 1.355 g, KCl: 6.7278 g, Fe(CH3COCHCOCH3)3: 1.7278 g을 칭량하고, 유발을 사용해서, 약 30분간 혼합하였다. 950℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0 .90Li0 .24Ti1 .58Fe0 .18O4이다.TiO 2 : 3.405 g, Li 2 CO 3 : 0.24 g, K 2 CO 3 : 1.355 g, KCl: 6.7278 g, Fe (CH 3 COCHCOCH 3 ) 3 : 1.7278 g was weighed, and the mortar was used for about 30 minutes. Mixed. It baked at 950 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration and dried at 150 ° C. for 1 hour. The composition formula of the obtained plate-like brown pigments is K 0 .90 Li 0 .24 Ti 1 .58 Fe 0 .18 O 4.

[실시예 7]Example 7

TiO2: 3.405 g, Li2CO3: 0.24 g, K2CO3: 1.355 g, KCl: 9.1965 g, Fe(CH3COCHCOCH3)3: 4.1965 g을 칭량하고, 유발을 사용해서, 약 30분간 혼합하였다. 950℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K1 .02Li0 .21Ti1 .40Fe0 .39O4이다.TiO 2 : 3.405 g, Li 2 CO 3 : 0.24 g, K 2 CO 3 : 1.355 g, KCl: 9.1965 g, Fe (CH 3 COCHCOCH 3 ) 3 : 4.1965 g was weighed, and the mortar was used for about 30 minutes. Mixed. It baked at 950 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration and dried at 150 ° C. for 1 hour. The composition formula of the obtained plate-like brown pigments is K 1 .02 Li 0 .21 Ti 1 .40 Fe 0 .39 O 4.

[실시예 8]Example 8

TiO2: 136.2 g, Li2CO3: 9.6 g, K2CO3: 54.2 g, KCl: 215.8 g, 적산화철(α- Fe2O3, 순분(純分): Fe2O3로서 99.2%): 15.8 g을 칭량하고, 교반혼합기에서 20분간 혼합하여, 해머 밀을 사용해서 분쇄하였다. 950℃에서 3시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 130℃에서 12시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0.90Li0.24Ti1.58Fe0.18O4이다.TiO 2 : 136.2 g, Li 2 CO 3 : 9.6 g, K 2 CO 3 : 54.2 g, KCl: 215.8 g, Iron red oxide (α-Fe 2 O 3 , Pure content: 99.2% as Fe 2 O 3 ) ): 15.8 g was weighed, mixed for 20 minutes in a stirred mixer, and ground using a hammer mill. It baked at 950 degreeC for 3 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration and dried at 130 ° C. for 12 hours. The composition formula of the obtained plate-like brown pigment is K 0.90 Li 0.24 Ti 1.58 Fe 0.18 O 4 .

[실시예 9]Example 9

TiO2: 136.2 g, Li2CO3: 9.6 g, K2CO3: 54.2 g, KCl: 217.7 g, 황산화철(α-FeOOH, 순분: Fe2O3로서 88.9%): 17.7 g을 칭량하고, 교반혼합기에서 20분간 혼합하여, 해머 밀을 사용해서 분쇄하였다. 950℃에서 3시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 130℃에서 12시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0.90Li0.24Ti1.58Fe0.18O4이다.TiO 2 : 136.2 g, Li 2 CO 3 : 9.6 g, K 2 CO 3 : 54.2 g, KCl: 217.7 g, iron sulfate (α-FeOOH, pure content: 88.9% as Fe 2 O 3 ): 17.7 g was weighed The mixture was mixed for 20 minutes in a stirring mixer, and ground using a hammer mill. It baked at 950 degreeC for 3 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration and dried at 130 ° C. for 12 hours. The composition formula of the obtained plate-like brown pigment is K 0.90 Li 0.24 Ti 1.58 Fe 0.18 O 4 .

[실시예 10]Example 10

TiO2: 136.2 g, Li2CO3: 9.6 g, K2CO3: 54.2 g, KCl: 215.7 g, 흑산화철((FeO)x(Fe2O3)y, 순분: Fe2O3로서 99.8%): 15.7 g을 칭량하고, 교반혼합기에서 20분간 혼합하여, 해머 밀을 사용해서 분쇄하였다. 950℃에서 3시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 130℃에서 12시간 건조하였다. 얻어진 판상 갈색계 안료의 조성식은 K0.90Li0.24Ti1.58Fe0.18O4이다.TiO 2 : 136.2 g, Li 2 CO 3 : 9.6 g, K 2 CO 3 : 54.2 g, KCl: 215.7 g, black iron oxide ((FeO) x (Fe 2 O 3 ) y , pure content: 99.8 as Fe 2 O 3 %): 15.7 g was weighed, mixed for 20 minutes in a stirring mixer, and ground using a hammer mill. It baked at 950 degreeC for 3 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration and dried at 130 ° C. for 12 hours. The composition formula of the obtained plate-like brown pigment is K 0.90 Li 0.24 Ti 1.58 Fe 0.18 O 4 .

[비교예 1] 철을 함유하지 않는 판상 티탄산Comparative Example 1 A plate-shaped titanic acid containing no iron

TiO2: 5.675 g, Li2CO3: 0.40 g, K2CO3: 2.26 g, KCl: 8.35 g을 칭량하고, 유발을 사용해서, 약 30분간 혼합하였다. 1000℃에서 3시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 판상 티탄산의 조성식은 K0 .81Li0 .27Ti1 .73O4이다.TiO 2 : 5.675 g, Li 2 CO 3 : 0.40 g, K 2 CO 3 : 2.26 g, KCl: 8.35 g were weighed and mixed for about 30 minutes using a mortar. It baked at 1000 degreeC for 3 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration and dried at 150 ° C. for 1 hour. The composition formula of the flaky titanic acid obtained is K 0 .81 Li 0 .27 Ti 1 .73 O 4.

[비교예 2] 철 대신에 크롬을 함유시킨 안료Comparative Example 2 A Pigment Containing Chromium Instead of Iron

TiO2: 3.4054 g, Li2CO3: 0.24 g, K2CO3: 1.355 g, KCl: 5 g, Cr(NO3)3·9H2O: 0.69 g을 칭량하고, 유발을 사용해서, 약 10분간 혼합하였다. 1000℃에서 5시간 소성하고, 80℃의 온수 중에 소성물을 투입하여, 약 1시간 교반하였다. 얻어진 분체를 여과 분별하고, 분체를 80℃의 온수에서 추가적으로 약 15분간 교반하였다. 분체를 여과 분별하고, 150℃에서 1시간 건조하였다. 얻어진 안료의 조성식은 K0.835Li0.256Ti1.677Cr0.067O4이다.TiO 2 : 3.4054 g, Li 2 CO 3 : 0.24 g, K 2 CO 3 : 1.355 g, KCl: 5 g, Cr (NO 3 ) 3 .9H 2 O: 0.69 g, were weighed, and the mortar was used to weigh Mix for 10 minutes. It baked at 1000 degreeC for 5 hours, the baked material was put into 80 degreeC warm water, and it stirred for about 1 hour. The obtained powder was separated by filtration, and the powder was further stirred for about 15 minutes in warm water at 80 ° C. The powder was separated by filtration and dried at 150 ° C for 1 hour. The composition formula of the obtained pigment is K 0.835 Li 0.256 Ti 1.677 Cr 0.067 O 4 .

실시예 1~10의 판상 갈색계 안료의 평균 장경, 평균 두께를 주사형 전자현미경 관찰로 확인한 결과, 모두 평균 두께가 0.1 ㎛~1 ㎛, 평균 장경이 10 ㎛~100 ㎛의 범위 내였다.As a result of confirming the average long diameter and average thickness of the plate-shaped brown pigment of Examples 1-10 by the scanning electron microscope observation, the average thickness of all was in the range of 0.1 micrometer-1 micrometer, and the average long diameter of 10 micrometers-100 micrometers.

색조의 육안평가Visual evaluation of color tone

실시예 1~10의 판상 갈색계 안료는 옅은 갈색 내지 짙은 갈색이었다. 한편, 비교예 1의 판상 티탄산 및 비교예 2의 철 대신에 크롬을 함유하는 안료는 백색으로, 착색 안료로서는 부적합하였다.The plate-like brown pigments of Examples 1 to 10 were pale brown to dark brown. On the other hand, the pigment containing chromium instead of the plate-like titanic acid of the comparative example 1 and iron of the comparative example 2 was white, and was unsuitable as a coloring pigment.

분광측색계에On the spectrophotometer 의한 색조 측정 Color measurement

실시예 2, 7의 판상 갈색계 안료의 색조를 분광측색계에 의해 측정하였다.The color tone of the plate-shaped brown pigment of Examples 2 and 7 was measured with the spectrophotometer.

장치: 코니카 미놀타사제 CM-2600dDevice: Konica Minolta CM-2600d

시료 조제방법: 3M사제 Scotch 투명 미색(美色)(점착 테이프) 24 mm×35 m를 5 cm 잘라내어, 실시예 2, 7의 판상 갈색계 안료를 기모(起毛) 퍼프로 점착 테이프면에 균일하게 도포하였다.Sample preparation method: 3 mm Scotch transparent off-white (adhesive tape) 24 mm x 35 m was cut out by 5 cm, and the plate-like brown pigments of Examples 2 and 7 were evenly brushed on the adhesive tape surface with brushed puffs. Applied.

결과: 결과를 표 1에 나타낸다.Results: Table 1 shows the results.

Figure 112009064307395-PAT00001
Figure 112009064307395-PAT00001

SCI: 정반사광 포함, SCE: 정반사광 제거SCI: with specular reflection, SCE: specular reflection

실시예 2, 7의 a*, b*의 범위는, 측정모드 SCI의 값을 하한으로 하고, 측정모드 SCE의 값을 상한으로 하면, a*=4~15, b*=15~26의 범위였다.The ranges of a * and b * in Examples 2 and 7 are in the range of a * = 4 to 15 and b * = 15 to 26 when the value of the measurement mode SCI is the lower limit and the value of the measurement mode SCE is the upper limit. It was.

매끄러움의 관능평가Sensory Evaluation of Smoothness

실시예 1과 비교예 1, 2의 매끄러움을 관능평가하였다.Sensory evaluation of the smoothness of Example 1 and Comparative Examples 1 and 2 was carried out.

안료를 피부 위에 올리고, 안료를 펼쳤을 때의 매끄러움을 이하의 기준에 의해 평가하였다.The smoothness when the pigment was placed on the skin and the pigment was spread was evaluated by the following criteria.

○: 매우 매끄럽다.(Circle): It is very smooth.

△: 매끄러우나 조금 까슬까슬하다.(Triangle | delta): Although it is smooth, it is a little blackish.

×: 까슬까슬하다.×: It is black.

결과를 표 2에 나타낸다.The results are shown in Table 2.

Figure 112009064307395-PAT00002
Figure 112009064307395-PAT00002

실시예 1, 비교예 1은 매끄러웠으나, 비교예 2는 까슬까슬했다. 실시예 1, 비교예 1, 2의 주사형 전자현미경 사진을 도 1~3에 나타낸다. 도 1, 2는 매끄러운 판상 결정이지만, 도 3에는 침상(針狀) 결정이 포함되어 있어, 그 결과, 비교예 2의 안료는 까슬까슬한 것으로 생각된다.Example 1 and Comparative Example 1 were smooth, but Comparative Example 2 was black. The scanning electron micrographs of Example 1 and Comparative Examples 1 and 2 are shown in FIGS. 1 and 2 are smooth plate crystals, but needles are included in FIG. 3, and as a result, the pigment of Comparative Example 2 is considered to be black.

젖음에 의한 색조 변화의 평가Evaluation of Tone Change by Wetting

실시예 2, 7의 판상 갈색계 안료와, 색조를 유사하게 한 혼합 안료에 대해, 스쿠알란으로 적시기 전후의 색조를 측정하여, 젖음에 의한 색조 변화를 측정하였다.About the plate-like brown pigment of Examples 2 and 7, and the mixed pigment which made the color tone similar, the color tone before and behind soaking with squalane was measured, and the color tone change by wetness was measured.

먼저, 안료의 색조를 상기 「분광측색계에 의한 색조 측정」에 기재한 방법으로 측정하였다(젖기 전).First, the color tone of the pigment was measured by the method described in "measurement of color tone by spectrophotometer" (before wet).

이어서, 안료에 스쿠알란을 적하하고, 유동성이 나타났을 때 적하를 멈췄다. 그 상태에서 측색하였다(젖은 후).Subsequently, squalane was dripped at the pigment, and dripping was stopped when fluidity appeared. Coloring was carried out in that state (after wet).

또한, 측정모드는 「SCE」로 하였다.In addition, the measurement mode was set to "SCE".

실시예 2와 실시예 2와 유사한 색조의 혼합 안료의 측정결과를 표 3에, 실시예 7과 실시예 7과 유사한 색조의 혼합 안료의 측정결과를 표 4에 나타낸다.Table 3 shows the measurement results of the mixed pigments having similar color hues as those of Example 2 and Example 2, and the results of the measurement of the mixed pigments having similar hues to Examples 7 and 7.

Figure 112009064307395-PAT00003
Figure 112009064307395-PAT00003

Figure 112009064307395-PAT00004
Figure 112009064307395-PAT00004

표 3, 표 4에 있어서, 혼합 안료의 성분은 이하와 같다.In Table 3 and Table 4, the component of a mixed pigment is as follows.

탈크: 아사다제분제 탈크 JA-46RTalc: Asada Powder Talc JA-46R

황산화철: 티탄공업제 LL-XLOIron sulfate: titanium LL-XLO

벵갈라: 티탄공업제 R-516-LBengala: T-Industrial R-516-L

황산Ba: 사카이화학공업제 판상 황산바륨 H-LFSulfuric acid Ba: Plate-like barium sulfate H-LF made by Sakai Chemical Co., Ltd.

흑산화철: 티탄공업제 BL-100Black oxide: titanium BL-100

표 3, 표 4에 나타낸 바와 같이, 실시예 2, 7의 판상 갈색계 안료는, 색조를 유사하게 한 혼합 안료에 비해, 스쿠알란에 의한 젖음 전후에서의 색조 변화가 작은 것을 알 수 있다.As shown in Table 3 and Table 4, it can be seen that the plate-brown pigments of Examples 2 and 7 have a smaller change in color tone before and after wetting by squalane compared to the mixed pigments having similar color tone.

자외선 차폐효과UV shielding effect

실시예 2와 비교예 1의 자외선 차폐효과를 비교하였다. 자외선은 UVB와 UVA의 경계파장인 320 nm로 측정하였다.The ultraviolet shielding effect of Example 2 and Comparative Example 1 was compared. Ultraviolet light was measured at 320 nm, the boundary wavelength between UVB and UVA.

1. 도막용 시료의 조제1. Preparation of coating film sample

샘플 0.2 g에 피마자유 0.2 g을 첨가하고, 휴버 뮬러(hoover muller)로 50회전, 3회 혼련을 행하였다. 그 용액에 쿠리야 래커((주)엔도화학공업제) 1.8 g을 첨가하여, 도막용 시료의 조제를 행하였다.0.2 g of castor oil was added to 0.2 g of the sample, and the mixture was kneaded 50 times and three times with a hover muller. 1.8 g of Kuriya lacquer (the Endo Chemical Co., Ltd. product) was added to this solution, and the sample for coating films was prepared.

2. 도막 제작방법2. Coating method

상기에서 제작한 도막용 시료를 투명 펫 필름(파낙(주)제 루미러 100-T60) 상에 2~3방울 적하하고, 도막 제작용 어플리케이터(간격 0.100 mm)로 도막을 제작하였다.The sample for coating film produced above was dripped 2-3 drops on the transparent pet film (Lanmir 100-T60 by Panak Co., Ltd.), and the coating film was produced with the applicator (0.100 mm spacing) for coating film production.

3. 투과율의 측정3. Measurement of transmittance

상기에서 제작한 도막의 320 nm 투과율을, 자외 가시 분광광도계(니혼분코주식회사제, 형식: V-570형)로 측정하였다.The 320 nm transmittance | permeability of the coating film produced above was measured with the ultraviolet visible spectrophotometer (The Nippon Bunko Corporation make, model: V-570 type).

4. 결과4. Results

결과를 표 5에 나타낸다.The results are shown in Table 5.

Figure 112009064307395-PAT00005
Figure 112009064307395-PAT00005

표 5에 나타낸 바와 같이, 실시예 2의 320 nm 투과율은 62%로, 자외선 차폐효과가 확인되었다.As shown in Table 5, the 320 nm transmittance of Example 2 was 62%, confirming the ultraviolet shielding effect.

[실시예 11]Example 11

파우더 파운데이션Powder foundation

성분 배합량(질량%)Ingredient compounding amount (mass%)

1. 실시예 1의 판상 갈색계 안료 201.Plate brown pigment 20 of Example 1

2. 실리콘처리 탈크 23.42. Siliconized Talc 23.4

3. 불소처리 산화티탄 103. Fluorinated titanium oxide 10

4. 아미노산처리 세리사이트 254. Amino Acid Treatment Sericite 25

5. 실리콘처리 황산화철 55. Siliconized Iron Sulfate 5

6. 실리콘처리 벵갈라 2.56. Siliconized Bengala 2.5

7. 실리콘처리 흑산화철 0.17. Silicon-treated black iron oxide 0.1

8. 메틸폴리실록산(100 cst) 118. Methylpolysiloxane (100 cst) 11

9. 사과산 디이소스테아릴 39. Malic Acid Diisostearyl 3

성분 1~7을 헨셀믹서로 5분간 교반한 후, 잘 혼합된 8, 9를 서서히 첨가하고, 해머 밀로 분쇄한다. 그 후, 중간 접시에 프레스한다.After stirring components 1-7 with a Henschel mixer for 5 minutes, the well mixed 8 and 9 are added gradually, and it grind | pulverizes with a hammer mill. After that, it is pressed to an intermediate plate.

[실시예 12]Example 12

아이섀도Eye shadow

성분 배합량(질량%)Ingredient compounding amount (mass%)

1. 실시예 2의 판상 갈색계 안료 151.Plate brown pigment of Example 2 15

2. 아미노산처리 산화티탄 72. Amino Acid Treatment Titanium Oxide 7

3. 실리콘처리 마이카 253. Siliconized Mica 25

4. 아미노산처리 세리사이트 104. Amino Acid Treatment Sericite 10

5. 나일론파우더 105. Nylon Powder 10

6. 불소처리 황산화철 56. Fluorinated Iron Sulfate 5

7. 불소처리 벵갈라 107. Fluorinated Bengala 10

8. 실리콘처리 군청 38. Silicon treatment county 3

9. 메틸페닐폴리실록산 89. Methylphenylpolysiloxane 8

10. 2-에틸헥산산세틸 710.Cetyl 2-ethylhexanoate 7

성분 1~8을 헨셀믹서로 5분간 교반한 후, 잘 혼합된 9, 10을 서서히 첨가하고, 해머 밀로 분쇄하였다. 그 후, 중간 접시에 프레스한다.The components 1-8 were stirred with a Henschel mixer for 5 minutes, and the well mixed 9 and 10 were added gradually, and it grind | pulverized with the hammer mill. After that, it is pressed to an intermediate plate.

[실시예 13]Example 13

크림 파운데이션Cream foundation

성분 배합량(질량%)Ingredient compounding amount (mass%)

1. 실시예 3의 판상 갈색계 안료 101. Plate-like brown pigment 10 of Example 3

2. 실리콘처리 산화티탄 9.42. Siliconized Titanium Oxide 9.4

3. 실리콘처리 황산화철 53. Siliconized Iron Sulfate 5

4. 실리콘처리 벵갈라 2.54. Siliconized Bengala 2.5

5. 실리콘처리 흑산화철 0.15. Silicon-treated black iron oxide 0.1

6. 시클로메티콘 306. Cyclomethicone 30

7. 메틸페닐폴리실록산 107. Methylphenylpolysiloxane 10

8. 디메티콘코폴리올 58. Dimethicone Copolyol 5

9. 정제수 209. Purified Water 20

10. 1,3-부틸렌글리콜 510. 1,3-butylene glycol 5

11. 글리세린 311.Glycerin 3

성분 1~8을 균일하게 혼합한다. 성분 8~11을 균일하게 혼합한 후, 성분 1~8에 첨가하고, 유화 혼합한다.The components 1-8 are mixed uniformly. After mixing components 8-11 uniformly, it adds to components 1-8 and emulsifies and mixes.

[실시예 14]Example 14

선스크린Sunscreen 크림 cream

성분 배합량(질량%)Ingredient compounding amount (mass%)

1. 실시예 4의 판상 갈색계 안료 101.Plate brown pigment 10 of Example 4

2. 데카메틸시클로펜타실록산 102. Decamethylcyclopentasiloxane 10

3. 실리콘처리 미립자 산화티탄 53. Siliconized fine particle titanium oxide 5

4. 실리콘처리 미립자 산화아연 54. Siliconized fine particle zinc oxide 5

5. 메틸페닐폴리실록산 55. Methylphenylpolysiloxane 5

6. 이소노난산 이소트리데실 56. Isononanosan Isotridecyl 5

7. 디이소스테아르산 폴리글리세릴-3 17. Diisostearic Acid Polyglyceryl-3 1

8. 디메티콘코폴리올 18. Dimethicone Copolyol 1

9. 베헤닐알코올 29. Behenyl Alcohol 2

10. 폴리메타크릴산메틸 510. Methyl Polymethacrylate 5

11. 트리메틸실록시규산 111.Trimethylsiloxysilicate 1

12. 1,3-부틸렌글리콜 512. 1,3-butylene glycol 5

13. 염화나트륨 0.513.Sodium Chloride0.5

14. 정제수 잔여14. Purified water residual

A: 성분 2~9를 80℃로 가열하고, 균일하게 혼합한다.A: The components 2-9 are heated at 80 degreeC, and it mixes uniformly.

B: 성분 1, 10, 11을 A성분에 첨가해서 혼합한다.B: Components 1, 10 and 11 are added to A component and mixed.

C: 성분 12~14를 80℃로 가열하고, 균일하게 혼합한 후, 이것을 B성분에 첨가해서 유화 혼합하여 실온까지 냉각한다.C: The components 12-14 are heated at 80 degreeC, and it mixes uniformly, adds this to B component, emulsifies and mixes and cools to room temperature.

도 1은 실시예 1의 주사형 전자현미경 사진을 나타내는 도면이다.1 is a view showing a scanning electron micrograph of Example 1.

도 2는 비교예 1의 판상 티탄산의 주사형 전자현미경 사진을 나타내는 도면이다.FIG. 2 is a view showing a scanning electron micrograph of plate-like titanic acid of Comparative Example 1. FIG.

도 3은 비교예 2의 크롬 함유 주사형 전자현미경 사진을 나타내는 도면이다.3 is a view showing a chromium-containing scanning electron microscope photograph of Comparative Example 2. FIG.

Claims (5)

화학식 K3x + yLixTi2 -x- yFeyO4(단, 0.2≤x≤0.3, 0.05≤y≤0.5)의 판상 갈색계 안료.A plate-like brown pigment of the formula K 3x + y Li x Ti 2 -x- y Fe y O 4 (0.2≤x≤0.3, 0.05≤y≤0.5). 제1항에 있어서,The method of claim 1, 색조가 L*a*b* 표색계에 있어서 a*=4~15, b*=15~26인 것을 특징으로 하는 판상 갈색계 안료.The color tone is a plate-like brown pigment, which is a * = 4-15 and b * = 15-26 in L * a * b * color system. 제1항 또는 제2항에 있어서,The method according to claim 1 or 2, 입자의 평균 두께가 0.1 ㎛~1 ㎛, 평균 장경이 10 ㎛~100 ㎛인 것을 특징으로 하는 판상 갈색계 안료.A plate-shaped brown pigment, wherein the average thickness of the particles is 0.1 μm to 1 μm and the average long diameter is 10 μm to 100 μm. 제1항 내지 제3항 중 어느 한 항의 판상 갈색계 안료를 함유하는 화장료.Cosmetics containing the plate-like brown pigment of any one of Claims 1-3. 제1항 내지 제3항 중 어느 한 항의 판상 갈색계 안료를 함유하는 분말 화장료.Powder cosmetic containing the plate-like brown pigment of any one of Claims 1-3.
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