TWI751992B - Emulsion type cosmetic composition comprising inorganic uv blocking agent and method for preparing same - Google Patents
Emulsion type cosmetic composition comprising inorganic uv blocking agent and method for preparing same Download PDFInfo
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Abstract
Description
本發明係關於含無機UV阻斷劑之一乳化型化妝品組成物及其製備方法。The invention relates to an emulsified cosmetic composition containing an inorganic UV blocking agent and a preparation method thereof.
用於UV阻斷化妝品之UV阻斷劑係被大致分類為有機UV阻斷劑及無機UV阻斷劑。雖然有機UV阻斷劑有優異之UV阻斷效果,其會導致黏性及由於滲透入皮膚之相關皮膚安全性問題。雖然無機UV阻斷劑主要係被用於將無機粉末分散在製劑中,不會導致黏性且顯示高皮膚安全性,由於無機粉末之聚結(coalescence)而引起白色渾濁(cloudy)現象且可提供乾燥使用感。為了防止無機UV阻斷劑粉末聚結之問題及將紫外線阻斷劑滲入(infiltration)製劑中,可能加入大量增稠劑及分散劑。然而,此可能引起製劑之黏性及皮膚刺激問題。UV blockers used in UV blocking cosmetics are roughly classified into organic UV blockers and inorganic UV blockers. Although organic UV blockers have excellent UV blocking effects, they can cause stickiness and related skin safety issues due to penetration into the skin. Although inorganic UV blockers are mainly used to disperse inorganic powders in formulations, do not cause stickiness and exhibit high skin safety, cause white cloudy phenomenon due to coalescence of inorganic powders and may Provides a dry feel. In order to prevent the problem of agglomeration of inorganic UV blocker powders and infiltration of the UV blocker into the formulation, it is possible to add large amounts of thickening and dispersing agents. However, this may cause stickiness and skin irritation problems of the formulation.
而且,考量持久性及防水性,常將UV阻斷化妝品組成物作為油包水(water-in-oil)製劑使用。如此之油包水製劑有油作為外相,因而不適合用於提供清爽(fresh)使用感。Furthermore, in consideration of durability and water repellency, UV blocking cosmetic compositions are often used as water-in-oil formulations. Such a water-in-oil formulation has oil as an external phase and is therefore not suitable for providing a fresh feeling in use.
含聚合物之球形微顆粒具有取決於其製備方法之大小及形狀,因此具有高適用性。例如,提供皮克林乳化(Pickering emulsion),其使用球形微顆粒以形成穩定之巨乳化顆粒。水相及油相間之接觸角(θ)隨著球形顆粒之親水性/疏水性而不同。當接觸角大於90°,形成O/W乳化顆粒。同時,當接觸角小於90°,形成W/O 乳化顆粒。The polymer-containing spherical microparticles have a size and shape that depends on the method of their preparation, and thus have high applicability. For example, Pickering emulsions are provided, which use spherical microparticles to form stable macroemulsion particles. The contact angle (θ) between the water phase and the oil phase varies with the hydrophilicity/hydrophobicity of the spherical particles. When the contact angle is greater than 90°, O/W emulsified particles are formed. Meanwhile, when the contact angle is less than 90°, W/O emulsified particles are formed.
此外,進行某些嘗試來賦予球形微顆粒兩親性之性質(即,親水性性質及疏水性性質二者)以獲得新穎異向性粉末。這可以用非對稱(Janus)球形顆粒來說明。然而,該球形顆粒由於其形態限制而有化學異向性之限制。換句話說,雖然該顆粒係形態異向性,其整體可為疏水性或親水性,因此具有有限之化學異向性。Furthermore, certain attempts were made to impart amphiphilic properties (ie, both hydrophilic and hydrophobic properties) to spherical microparticles to obtain novel anisotropic powders. This can be illustrated with asymmetric (Janus) spherical particles. However, the spherical particles are limited by their chemical anisotropy due to their morphological limitations. In other words, although the particles are morphologically anisotropic, they can be hydrophobic or hydrophilic as a whole, and thus have limited chemical anisotropy.
因此,進行某些嘗試來獲得表面活性異向性粉末,其係藉由控制幾何形狀及賦予化學異向性。然而,迄今仍未發展出大規模生產兩親性異向性粉末之方法,雖然該兩親性異向性粉末顯示高適用性。此外,難以在產業規模中大量地生產均勻兩親性異向性粉末,導致無法在實際中應用。Therefore, some attempts were made to obtain surface-active anisotropic powders by controlling the geometry and imparting chemical anisotropy. However, a method for mass production of amphiphilic anisotropic powders has not yet been developed, although the amphiphilic anisotropic powders show high applicability. In addition, it is difficult to mass-produce uniform amphiphilic anisotropic powder on an industrial scale, resulting in impossibility of practical application.
技術問題technical problem
本發明欲解決之一技術問題係在提供一乳化型化妝品組成物,其包含穩定分散其中之無機UV阻斷劑。One technical problem to be solved by the present invention is to provide an emulsified cosmetic composition comprising an inorganic UV blocking agent stably dispersed therein.
本發明欲解決之另一技術問題係在提供一乳化型化妝品組成物,其具有優異皮膚安全性。Another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition with excellent skin safety.
本發明欲解決之還另一技術問題係在提供一乳化型化妝品組成物,其能改善白色渾濁現象。Yet another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition, which can improve the white turbidity.
本發明欲解決之還另一技術問題係在提供一乳化型化妝品組成物,其不需使用過量增稠劑而可提供一高黏度製劑。Yet another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition, which can provide a high-viscosity formulation without using excessive thickener.
本發明欲解決之還另一技術問題係在提供一化妝用乳化型化妝品組成物,即使存在有高含量無機UV阻斷劑,其仍具有優異之隨時間推移製劑穩定性。Yet another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition for cosmetic use, which has excellent formulation stability over time even in the presence of a high content of inorganic UV blocking agents.
本發明欲解決之還另一技術問題係在提供一乳化型化妝品組成物,其具有優異之防水性及持久性。Yet another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition with excellent water resistance and durability.
本發明欲解決之又另一技術問題係在提供一乳化型化妝品組成物,其藉由乳化顆粒之摻水效果(watering effect)顯示出清爽使用感。 技術方案Yet another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition, which exhibits a refreshing use feeling through the watering effect of emulsified particles. Technical solutions
在一通常態樣中,提供含一無機UV阻斷劑及兩親性異向性粉末之一乳化型化妝品組成物,其中該無機UV阻斷劑係無機粉末,該兩親性異向性粉末包含一第一親水性聚合物球形體及一第二疏水性聚合物球形體,該第一聚合物球形體及該第二聚合物球形體係以一結構彼此結合,其中一聚合物球形體至少部分地貫穿入其他聚合物球形體,該第一聚合物球形體具有一核-殼結構,且該殼具有一官能基團。 有益效果In a general aspect, an emulsified cosmetic composition containing an inorganic UV blocking agent and an amphiphilic anisotropic powder is provided, wherein the inorganic UV blocking agent is an inorganic powder, and the amphiphilic anisotropic powder is provided. Including a first hydrophilic polymer sphere and a second hydrophobic polymer sphere, the first polymer sphere and the second polymer sphere system are combined with each other in a structure, wherein a polymer sphere is at least partially The first polymer sphere has a core-shell structure, and the shell has a functional group. beneficial effect
在一態樣中,本發明提供一乳化型化妝品組成物,其含有穩定分散於其中之無機UV阻斷劑。In one aspect, the present invention provides an emulsified cosmetic composition comprising an inorganic UV blocking agent stably dispersed therein.
在另一態樣中,本發明提供一乳化型化妝品組成物,其具有優異之皮膚安全性。In another aspect, the present invention provides an emulsified cosmetic composition with excellent skin safety.
在還另一態樣中,本發明提供一乳化型化妝品組成物,其改善白色渾濁現象。In yet another aspect, the present invention provides an emulsified cosmetic composition that improves white cloudiness.
在還另一態樣中,本發明提供一乳化型化妝品組成物,其不需使用過量增稠劑而可提供一高黏度製劑。In yet another aspect, the present invention provides an emulsified cosmetic composition that can provide a high-viscosity formulation without the use of excessive thickeners.
在還另一態樣中,本發明提供一乳化型化妝品組成物,即使存在有高含量無機UV阻斷劑,其仍具有優異之隨時間推移製劑穩定性。In yet another aspect, the present invention provides an emulsified cosmetic composition having excellent formulation stability over time even in the presence of high levels of inorganic UV blockers.
在還另一態樣中,本發明提供一乳化型化妝品組成物,其具有優異之防水性及持久性。In yet another aspect, the present invention provides an emulsified cosmetic composition having excellent water resistance and durability.
在還又一態樣中,本發明提供一乳化型化妝品組成物,其藉由乳化顆粒之摻水效果顯示出清爽使用感。In yet another aspect, the present invention provides an emulsified cosmetic composition, which exhibits a refreshing feeling of use through the water-incorporating effect of emulsified particles.
最佳實施例best practice
下文將參考附圖更充分地描述例示性具體實施例,其中該附圖顯示例示性具體實施例。然而,本揭露內容可以許多不同形式體現且不應被解釋為受限於列於其中之該等例示性具體實施例。相反地,此等具體實施例被提供以使得本揭露內容完全及完整,並向本領域技術人員充分傳達本發明之範圍。在圖式中,為了清楚起見,可能誇大圖式之形狀、尺寸及區域等。而且,儘管為了便於描述而顯示出部分構成元件,但本領域技術人員可容易地理解其餘部分。此外,本領域技術人員可理解在不悖離所附申請專利範圍定義之本揭露範圍之情況下,可對形式及細節進行各種改變。Illustrative embodiments will be described more fully hereinafter with reference to the accompanying drawings, in which illustrative embodiments are shown. However, the present disclosure may be embodied in many different forms and should not be construed as limited to the illustrative embodiments set forth therein. Rather, these specific embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. In the drawings, the shapes, sizes, regions, etc. of the drawings may be exaggerated for clarity. Also, although some constituent elements are shown for convenience of description, those skilled in the art can easily understand the remaining parts. Furthermore, it will be understood by those of ordinary skill in the art that various changes in form and details may be made therein without departing from the scope of the present disclosure as defined by the appended claims.
除非另有說明,本文所用之「經取代」意指至少本文所述之該官能基團之一氫原子係經以下取代:一鹵素原子(F、Cl、Br或I),羥基基團,硝基基團,亞胺基基團(=NH、=NR,其中R係C1-C10烷基基團),甲脒基基團,肼基或腙基基團,羧基基團,經取代或未經取代之C1-C20烷基基團,經取代或未經取代之C3-C30雜芳基基團,或經取代或未經取代之C2-C30雜環烷基基團。Unless otherwise stated, "substituted" as used herein means that at least one of the hydrogen atoms of the functional group described herein is substituted with: a halogen atom (F, Cl, Br or I), a hydroxyl group, a nitro group, imino group (=NH, =NR, wherein R is a C1-C10 alkyl group), formamidinyl group, hydrazine or hydrazone group, carboxyl group, substituted or unsubstituted A substituted C1-C20 alkyl group, a substituted or unsubstituted C3-C30 heteroaryl group, or a substituted or unsubstituted C2-C30 heterocycloalkyl group.
本文所用之「(甲基)丙烯醯基」意指丙烯醯基及/或甲基丙烯醯基。As used herein, "(meth)acryloyl" means acryl and/or methacryloyl.
本文所用之兩親性異向性粉末顆粒大小係被測定為最大長度,其係該粉末顆粒之最大長度。本文所用之存在於組成物中之兩親性異向性粉末顆粒之大小範圍意指至少95%該兩親性異向性粉末屬於此對應範圍。As used herein, amphiphilic anisotropic powder particle size is determined as the maximum length, which is the maximum length of the powder particle. As used herein, the size range of the amphiphilic anisotropic powder particles present in the composition means that at least 95% of the amphiphilic anisotropic powder falls within this corresponding range.
本文所用之乳化顆粒平均粒徑意指各顆粒之平均直徑。本文所用之乳化顆粒平均粒徑範圍意指至少95%該存在於組成物中之乳化顆粒屬於此對應範圍。The average particle size of the emulsified particles used herein means the average diameter of each particle. As used herein, the average particle size range of the emulsified particles means that at least 95% of the emulsified particles present in the composition fall within this corresponding range.
本文所用之無機粉末平均粒徑意指藉由計算基於顆粒大小分佈之體積平均獲得之體積平均粒徑,其係藉由已知用於確認顆粒大小分佈方法來確認,諸如觀察電子顯微影像、雷射繞射等。The average particle size of inorganic powders used herein means the volume average particle size obtained by calculating the volume average based on particle size distribution, which is confirmed by known methods for confirming particle size distribution, such as observation of electron microscopic images, Laser Diffraction, etc.
在一態樣中,提供一乳化型化妝品組成物,其包含一無機UV阻斷劑及兩親性異向性粉末。In one aspect, an emulsified cosmetic composition is provided comprising an inorganic UV blocker and an amphiphilic anisotropic powder.
根據一具體實施例,該無機UV阻斷劑可為能夠提供UV阻斷效果之無機粉末。According to an embodiment, the inorganic UV blocking agent may be an inorganic powder capable of providing UV blocking effect.
根據另一具體實施例,該無機粉末以該組成物組重為基礎可以下述之量使用:0.1 wt%或其以上、0.2 wt%或其以上、0.3 wt%或其以上、0.4 wt%或其以上、0.5 wt%或其以上、0.6 wt%或其以上、0.7 wt%或其以上、0.8 wt%或其以上、0.9 wt%或其以上、1.0 wt%或其以上、1.5 wt%或其以上、2.0 wt%或其以上、2.5 wt%或其以上、3.0 wt%或其以上、3.5 wt%或其以上、4.0 wt%或其以上、4.5 wt%或其以上、5.0 wt%或其以上、5.5 wt%或其以上、6.0 wt%或其以上、6.5 wt%或其以上、7.0 wt%或其以上、7.5 wt%或其以上、8.0 wt%或其以上、8.5 wt%或其以上、9.5 wt%或其以上、10.0 wt%或其以上、11.0 wt%或其以上、12.0 wt%或其以上、13.0 wt%或其以上、14.0 wt%或其以上、或15.0 wt%或其以上;及60 wt%或其以下、59 wt%或其以下、58 wt%或其以下、57 wt%或其以下、56 wt%或其以下、55 wt%或其以下、54 wt%或其以下、53 wt%或其以下、52 wt%或其以下、51 wt%或其以下、50 wt%或其以下、49 wt%或其以下、48 wt%或其以下、47 wt%或其以下、46 wt%或其以下、45 wt%或其以下、44 wt%或其以下、43 wt%或其以下、42 wt%或其以下、41 wt%或其以下、40 wt%或其以下、39 wt%或其以下、38 wt%或其以下、37 wt%或其以下、36 wt%或其以下、35 wt%或其以下、34 wt%或其以下、33 wt%或其以下、32 wt%或其以下、31 wt%或其以下、30 wt%或其以下、29 wt%或其以下、28 wt%或其以下、27 wt%或其以下、26 wt%或其以下、或25 wt%或其以下。舉例而言,該無機粉末以該組成物組重為基礎可以0.1 wt%-60 wt%、0.5 wt%-50 wt%、1 wt%-40 wt%或5 wt%-30 wt%之量使用。更特別為,該無機粉末可以30 wt%或其以上或40 wt%或其以上之高含量使用。可能在上述範圍內提供一UV阻斷效果及一優異使用感且保持一穩定乳化製劑。According to another embodiment, the inorganic powder may be used in the following amounts based on the composition weight: 0.1 wt% or more, 0.2 wt% or more, 0.3 wt% or more, 0.4 wt% or more 0.5 wt% or more, 0.6 wt% or more, 0.7 wt% or more, 0.8 wt% or more, 0.9 wt% or more, 1.0 wt% or more, 1.5 wt% or more Above, 2.0 wt% or more, 2.5 wt% or more, 3.0 wt% or more, 3.5 wt% or more, 4.0 wt% or more, 4.5 wt% or more, 5.0 wt% or more , 5.5 wt% or more, 6.0 wt% or more, 6.5 wt% or more, 7.0 wt% or more, 7.5 wt% or more, 8.0 wt% or more, 8.5 wt% or more, 9.5 wt% or more, 10.0 wt% or more, 11.0 wt% or more, 12.0 wt% or more, 13.0 wt% or more, 14.0 wt% or more, or 15.0 wt% or more; and 60 wt% or less, 59 wt% or less, 58 wt% or less, 57 wt% or less, 56 wt% or less, 55 wt% or less, 54 wt% or less, 53 wt% or less, 52 wt% or less, 51 wt% or less, 50 wt% or less, 49 wt% or less, 48 wt% or less, 47 wt% or less, 46 wt% or less, 45 wt% or less, 44 wt% or less, 43 wt% or less, 42 wt% or less, 41 wt% or less, 40 wt% or less, 39 wt% % or less, 38 wt% or less, 37 wt% or less, 36 wt% or less, 35 wt% or less, 34 wt% or less, 33 wt% or less, 32 wt% or less, 31 wt% or less, 30 wt% or less, 29 wt% or less, 28 wt% or less, 27 wt% or less, 26 wt% or less, or 25 wt% or below. For example, the inorganic powder may be used in an amount of 0.1 wt%-60 wt%, 0.5 wt%-50 wt%, 1 wt%-40 wt%, or 5 wt%-30 wt% based on the composition weight. . More particularly, the inorganic powder may be used in a high content of 30 wt% or more or 40 wt% or more. It is possible to provide a UV blocking effect and an excellent feeling in use within the above range while maintaining a stable emulsified formulation.
根據本發明之一具體實施例,該無機粉末憑藉著該兩親性異向性粉末穩固地保持該乳化顆粒之乳化界面,且巨乳化顆粒及該無機粉末係被緊密包在製劑中以提供高黏度之製劑。因而該無機粉末可被穩定分散在該製劑中。結果為,即使使用上述高含量之無機粉末,該粉末不會造成聚結且可改善白色渾濁現象及提供非乾燥及柔軟之使用感。According to an embodiment of the present invention, the inorganic powder firmly maintains the emulsification interface of the emulsified particles by virtue of the amphiphilic anisotropic powder, and the macroemulsified particles and the inorganic powder are tightly packed in the formulation to provide high Viscosity preparations. Thus the inorganic powder can be stably dispersed in the formulation. As a result, even if the above-mentioned high content of the inorganic powder is used, the powder does not cause agglomeration and can improve white cloudiness and provide a non-dry and soft feeling in use.
根據另一具體實施例,該無機粉末可為具有UV阻斷效果之粉末且慣用於美容領域中。舉例而言,該無機粉末可包含:二氧化鈦(TiO2 )、氧化鋅 (ZnO)、氧化鐵(Fe2 O3 )、氧化鋯(ZrO2 )、二氧化矽(SiO2 )、氧化錳(MnO)、氧化鋁(Al2 O3 )、氧化鈰(CeO3 )、雲母(mica)、矽土(silica)、滑石(talc)和高嶺土(kaolin)。According to another embodiment, the inorganic powder may be a powder with UV blocking effect and is conventionally used in the cosmetic field. For example, the inorganic powder may include: titanium dioxide (TiO 2 ), zinc oxide (ZnO), iron oxide (Fe 2 O 3 ), zirconium oxide (ZrO 2 ), silicon dioxide (SiO 2 ), manganese oxide (MnO) ), alumina (Al 2 O 3 ), cerium oxide (CeO 3 ), mica (mica), silica (silica), talc (talc) and kaolin (kaolin).
根據還另一具體實施例,該無機粉末存在於該乳化型組成物之油相中,可使用經表面疏水化處理之無機粉末。該表面疏水化處理可使用美容領域慣用方法進行。舉例而言,該無機粉末可經以矽酮(silicone)化合物、脂肪酸、胺基酸或脂肪酸鹽(諸如硬脂酸鋁)處理,但不限於此。According to yet another specific embodiment, the inorganic powder is present in the oil phase of the emulsified composition, and the inorganic powder with surface hydrophobization treatment can be used. This surface hydrophobization treatment can be performed using methods conventional in the cosmetic field. For example, the inorganic powder may be treated with silicone compounds, fatty acids, amino acids or fatty acid salts such as, but not limited to, aluminum stearate.
該無機粉末可具有5 nm-2000 nm之平均粒徑。舉例而言,該平均粒徑可為10 nm-1000 nm。可在上述範圍內提供優異之UV阻斷效果及優異之製劑穩定性且防止白色渾濁現象。The inorganic powder may have an average particle size of 5 nm to 2000 nm. For example, the average particle size may be 10 nm to 1000 nm. It is possible to provide excellent UV blocking effect and excellent formulation stability and prevent white cloudiness within the above range.
根據還另一具體實施例,該兩親性異向性粉末包含一第一親水性 聚合物球形體及一第二疏水性聚合物球形體,其中該第一聚合物球形體及該第二聚合物球形體係以一結構彼此結合,其中一聚合物球形體至少部分地貫穿入其他聚合物球形體,該第一聚合物球形體具有一核-殼結構且該殼具有一官能基團。According to yet another embodiment, the amphiphilic anisotropic powder comprises a first hydrophilic polymer sphere and a second hydrophobic polymer sphere, wherein the first polymer sphere and the second polymer sphere The biosphere systems are combined with each other in a structure in which a polymer sphere at least partially penetrates into other polymer spheres, the first polymer sphere has a core-shell structure and the shell has a functional group.
本文所用之球形體意指由聚合物形成之一單體(single body)。舉例而言,其可能具有一球形、球面(globoidal)或橢圓形及毫米級或奈米級長軸,其係以本體部(section of the body)最大長度為基礎。Spheroid as used herein means a single body formed from a polymer. For example, it may have a spherical, globoidal or elliptical shape and a millimeter or nanoscale major axis based on the maximum length of the section of the body.
根據一具體實施例,該第二聚合物球形體及該第一聚合物球形體之核可能包含乙烯基聚合物,且該第一聚合物球形體之殼可能包含一乙烯基單體之共聚合物,其具一含官能基團之單體。According to an embodiment, the cores of the second polymer spheres and the first polymer spheres may comprise vinyl polymers, and the shells of the first polymer spheres may comprise a copolymer of vinyl monomers A substance having a functional group-containing monomer.
根據另一具體實施例,該乙烯基聚合物可能包含一乙烯基芳香族聚合物,特別為聚苯乙烯。According to another embodiment, the vinyl polymer may comprise a vinyl aromatic polymer, in particular polystyrene.
根據還另一具體實施例,該乙烯基單體可能包含一乙烯基芳香族單體。 舉例而言,該乙烯基單體可為經取代或未經取代之苯乙烯。According to yet another embodiment, the vinyl monomer may comprise a vinyl aromatic monomer. For example, the vinyl monomer can be substituted or unsubstituted styrene.
根據還另一具體實施例,該官能基團可為矽氧烷(siloxane)。According to yet another embodiment, the functional group may be a siloxane.
根據還另一具體實施例,該含官能基團單體可為一含矽氧烷(甲基)丙烯酸酯,特別為至少一選自於由以下所組成之群組:3-(三甲氧基矽基) 丙烯酸丙酯(3-(trimethoxysilyl)propyl acrylate),3-(三甲氧基矽基)甲基丙烯酸丙酯(3-(trimethoxysilyl)propyl methacrylate),乙烯基三乙氧基矽烷(vinyltriethoxysilane)及乙烯基三甲氧基矽烷(vinyltrimethoxysilane),或其組合。According to yet another specific embodiment, the functional group-containing monomer may be a siloxane-containing (meth)acrylate, especially at least one selected from the group consisting of: 3-(trimethoxy) Silyl) propyl acrylate (3-(trimethoxysilyl)propyl acrylate), 3-(trimethoxysilyl)propyl methacrylate (3-(trimethoxysilyl)propyl methacrylate), vinyltriethoxysilane and vinyltrimethoxysilane, or a combination thereof.
根據還另一具體實施例, 該聚合物球形體之殼可能進一步具有被引入之一親水性官能基團。According to yet another embodiment, the shell of the polymer sphere may further have a hydrophilic functional group introduced.
根據還另一具體實施例,該親水性官能基團可為一負價或正價官能基團或聚乙二醇(polyethylene glycol ,PEG)為主之官能基團且可能包含至少一選自於由以下所組成之群組:羧酸(carboxylate)基團、碸(sulfone)基團、磷酸(phosphate)基團、胺基(amino)基團、烷氧基(alkoxy)基團、酯(ester)基團、乙酸(acetate)基團、聚乙二醇(polyethylene)基團及羥基(hydroxyl)基團。According to yet another specific embodiment, the hydrophilic functional group may be a negative-valent or positive-valent functional group or a polyethylene glycol (PEG)-based functional group and may include at least one selected from the group consisting of The group consisting of: carboxylate group, sulfone group, phosphate group, amino group, alkoxy group, ester ) group, acetate group, polyethylene glycol group and hydroxyl group.
根據還另一具體實施例, 該第一聚合物球形體之殼可能進一步具有被引入之一含醣官能基團。According to yet another embodiment, the shell of the first polymer sphere may further have a sugar-containing functional group introduced.
根據還另一具體實施例,該含醣官能基團可衍生自至少一 選自於由以下所組成之群組:N-{N-(3-三乙氧基矽基丙基)氨基乙基}葡糖醯胺(N-{N-(3-triethoxysilylpropyl) aminoethyl}gluconamide),N-(3-三乙氧基矽基丙基)葡糖醯胺(N-(3-triethoxysilylpropyl) gluconamide)及N-{N-(3-三乙氧基矽基丙基)氨基乙基}-寡-質酸醯胺(N-{N-(3-triethoxysilylpropyl)aminoethyl}-oligo- hyaluronamide)。According to yet another embodiment, the sugar-containing functional group may be derived from at least one selected from the group consisting of: N-{N-(3-triethoxysilylpropyl)aminoethyl } Glucosamide (N-{N-(3-triethoxysilylpropyl) aminoethyl}gluconamide), N-(3-triethoxysilylpropyl) gluconamide and N-{N-(3-triethoxysilylpropyl)aminoethyl}-oligo-hyaluronamide.
根據還另一具體實施例,該兩親性異向性粉末可能具有對稱形狀、不對稱雪人形狀或不對稱倒雪人形狀,其係以該第一聚合物球形體及該第二聚合物球形體彼此結合之結合處為基礎。該雪人形狀係指彼此結合及具有不同大小之該第一聚合物球形體及該第二聚合物球形體。According to yet another embodiment, the amphiphilic anisotropic powder may have a symmetrical shape, an asymmetric snowman shape or an asymmetric inverted snowman shape, which is formed by the first polymer sphere and the second polymer sphere based on the combination of each other. The snowman shape refers to the first polymer sphere and the second polymer sphere combined with each other and having different sizes.
根據還另一具體實施例,該兩親性異向性粉末可能具有100-2500 nm之顆粒大小。在一變體中,該兩親性異向性粉末可能具有100-1500 nm、100-500 nm或200-300 nm之顆粒大小。特別地,該兩親性粉末可能具有以下之顆粒大小:100 nm或其以上,200 nm或其以上,300 nm或其以上,400 nm或其以上,500 nm或其以上,600 nm或其以上,700 nm或其以上,800 nm或其以上,900 nm或其以上,1000 nm或其以上,1100 nm或其以上,1200 nm或其以上,1300 nm或其以上,1400 nm或其以上,或1500 nm或其以上;及2500 nm或其以下,2400 nm或其以下,2300 nm或其以下,2200 nm或其以下,2100 nm或其以下,2000 nm或其以下,1900 nm或其以下,1800 nm或其以下,1700 nm或其以下,1600 nm或其以下,1500 nm或其以下,1400 nm或其以下,1300 nm或其以下,1200 nm或其以下,1100 nm或其以下,1000 nm或其以下,900 nm或其以下,800 nm或其以下,700 nm或其以下,600 nm或其以下,500 nm或其以下,400 nm或其以下,300 nm或其以下,或200 nm或其以下。According to yet another embodiment, the amphiphilic anisotropic powder may have a particle size of 100-2500 nm. In a variant, the amphiphilic anisotropic powder may have a particle size of 100-1500 nm, 100-500 nm or 200-300 nm. In particular, the amphiphilic powder may have the following particle sizes: 100 nm or more, 200 nm or more, 300 nm or more, 400 nm or more, 500 nm or more, 600 nm or more , 700 nm or more, 800 nm or more, 900 nm or more, 1000 nm or more, 1100 nm or more, 1200 nm or more, 1300 nm or more, 1400 nm or more, or 1500 nm or above; and 2500 nm or below, 2400 nm or below, 2300 nm or below, 2200 nm or below, 2100 nm or below, 2000 nm or below, 1900 nm or below, 1800 nm or less, 1700 nm or less, 1600 nm or less, 1500 nm or less, 1400 nm or less, 1300 nm or less, 1200 nm or less, 1100 nm or less, 1000 nm or less below, 900 nm or below, 800 nm or below, 700 nm or below, 600 nm or below, 500 nm or below, 400 nm or below, 300 nm or below, or 200 nm or below the following.
根據還另一具體實施例,該兩親性異向性粉末可能形成巨乳化顆粒,其具有2-200 μm之大小。在一變體中,該兩親性異向性粉末可能形成巨乳化顆粒,其具有5-200 μm、10-100 μm、10-50 μm或25 μm之大小。特別地,該兩親性異向性粉末可能形成具有以下大小之乳化顆粒:2 μm或其以上、5 μm或其以上、10 μm或其以上、15 μm或其以上、20 μm或其以上、25 μm或其以上、30 μm或其以上、40 μm或其以上、50 μm或其以上、80 μm或其以上、100 μm或其以上、130 μm或其以上、150 μm或其以上、或180 μm或其以上;及200 μm或其以下、180 μm或其以下、150 μm或其以下、130 μm或其以下、100 μm或其以下、80 μm或其以下、50 μm或其以下、40 μm或其以下、30 μm或其以下、25 μm或其以下、20 μm或其以下、15 μm或其以下、10 μm或其以下、或5 μm或其以下。According to yet another embodiment, the amphiphilic anisotropic powder may form macroemulsified particles, which have a size of 2-200 μm. In a variant, the amphiphilic anisotropic powder may form macroemulsion particles having a size of 5-200 μm, 10-100 μm, 10-50 μm or 25 μm. In particular, the amphiphilic anisotropic powder may form emulsified particles having the following sizes: 2 μm or more, 5 μm or more, 10 μm or more, 15 μm or more, 20 μm or more, 25 μm or more, 30 μm or more, 40 μm or more, 50 μm or more, 80 μm or more, 100 μm or more, 130 μm or more, 150 μm or more, or 180 μm or more; and 200 μm or less, 180 μm or less, 150 μm or less, 130 μm or less, 100 μm or less, 80 μm or less, 50 μm or less, 40 μm or less, 30 μm or less, 25 μm or less, 20 μm or less, 15 μm or less, 10 μm or less, or 5 μm or less.
由於該兩親性異向性粉末之疏水性部分及親水性部分具有對界面之不同定向性,可能會形成巨乳化顆粒,及實現優異使用感之製劑。習知分子層級之表面活性劑難以形成粒徑數十微米之穩定巨乳化顆粒。而且,在習知表面活性劑之情況下,其形成大約數奈米厚度之界面膜。相反地,在本文揭露之兩親性異向性粉末情況下,該界面膜厚度增加為大約數百奈米且憑藉粉末顆粒之強結合作用形成穩定界面膜。因而可顯著改善乳化物之穩定性。Since the hydrophobic part and the hydrophilic part of the amphiphilic anisotropic powder have different orientations to the interface, it is possible to form large emulsified particles, and to realize a formulation with excellent feeling in use. It is difficult for conventional molecular-level surfactants to form stable macro-emulsion particles with a particle size of several tens of microns. Furthermore, in the case of conventional surfactants, they form an interfacial film with a thickness of about several nanometers. In contrast, in the case of the amphiphilic anisotropic powders disclosed herein, the interfacial film thickness is increased to about several hundreds of nanometers and a stable interfacial film is formed by virtue of the strong binding of powder particles. Thus, the stability of the emulsion can be significantly improved.
當一習知分子級表面活性劑形成之界面膜形成一動態(dynamic)乳化相,該兩親性異向性粉末形成之乳化顆粒界面膜之厚度會增加至數百奈米且憑藉粉末顆粒間之強結合性形成一穩定界面膜。因此,可能保持一穩定之乳化狀態,同時不受該無機粉末之影響。When the interfacial film formed by a conventional molecular-level surfactant forms a dynamic emulsion phase, the thickness of the interfacial film formed by the amphiphilic anisotropic powder will increase to several hundreds of nanometers. The strong bond forms a stable interface film. Therefore, it is possible to maintain a stable emulsified state without being affected by the inorganic powder.
根據還另一具體實施例,該兩親性異向性粉末以該組成物之總重為基礎可依以下量存在:0.1 wt%或其以上,0.2 wt%或其以上,0.3 wt%或其以上,0.4 wt%或其以上,0.5 wt%或其以上,0.6 wt%或其以上,0.7 wt%或其以上,0.8 wt%或其以上,0.9 wt%或其以上,或1.0 wt%或其以上;及20 wt%或其以下,19 wt%或其以下,18 wt%或其以下,17 wt%或其以下,16 wt%或其以下,15 wt%或其以下,14 wt%或其以下,13 wt%或其以下,12 wt%或其以下,11 wt%或其以下,10 wt%或其以下,9 wt%或其以下,8 wt%或其以下,7 wt%或其以下,6 wt%或其以下,5 wt%或其以下,4 wt%或其以下,或3 wt%或其以下。舉例而言,該兩親性異向性粉末以該組成物之總重為基礎可依以下量存在:0.1-20 wt%,特別為0.5-10 wt%,更特別為1-5 wt%,甚至更特別為1-3 wt%。可在上述範圍內形成穩定之乳化顆粒且形成具有適當大小之乳化顆粒。According to yet another embodiment, the amphiphilic anisotropic powder may be present in the following amounts based on the total weight of the composition: 0.1 wt% or more, 0.2 wt% or more, 0.3 wt% or more Above, 0.4 wt% or more, 0.5 wt% or more, 0.6 wt% or more, 0.7 wt% or more, 0.8 wt% or more, 0.9 wt% or more, or 1.0 wt% or more and above; and 20 wt% or less, 19 wt% or less, 18 wt% or less, 17 wt% or less, 16 wt% or less, 15 wt% or less, 14 wt% or less Below, 13 wt% or less, 12 wt% or less, 11 wt% or less, 10 wt% or less, 9 wt% or less, 8 wt% or less, 7 wt% or less , 6 wt% or less, 5 wt% or less, 4 wt% or less, or 3 wt% or less. For example, the amphiphilic anisotropic powder may be present in the following amounts, based on the total weight of the composition: 0.1-20 wt%, particularly 0.5-10 wt%, more particularly 1-5 wt%, Even more specifically 1-3 wt%. Stable emulsified particles can be formed within the above range and emulsified particles having an appropriate size can be formed.
該組成物可具有以下黏度:2000 cps或其以上、2100 cps或其以上、2200 cps或其以上、2300 cps或其以上、2400 cps或其以上、2500 cps或其以上、2600 cps或其以上、2700 cps或其以上、2800 cps或其以上、2900 cps或其以上、3000 cps或其以上、3100 cps或其以上、3200 cps或其以上、3300 cps或其以上、3400 cps或其以上、3500 cps或其以上、3600 cps或其以上、3700 cps或其以上、3800 cps或其以上、3900 cps或其以上、4000 cps或其以上、4100 cps或其以上、4200 cps或其以上、4300 cps或其以上、4400 cps或其以上、4500 cps或其以上、4600 cps或其以上、4700 cps或其以上、4800 cps或其以上、4900 cps或其以上、5000 cps或其以上、5100 cps或其以上、5200 cps或其以上、5300 cps或其以上、5400 cps或其以上、5500 cps或其以上、5600 cps或其以上、5700 cps或其以上、5800 cps或其以上、5900 cps或其以上、6000 cps或其以上、6100 cps或其以上、6200 cps或其以上、6300 cps或其以上、6400 cps或其以上、6500 cps或其以上、7000 cps或其以上、7500 cps或其以上、8000 cps或其以上、8500 cps或其以上、9000 cps或其以上、9500 cps或其以上、10000 cps或其以上、11000 cps或其以上、12000 cps或其以上、13000 cps或其以上、14000 cps或其以上、15000 cps或其以上、16000 cps或其以上、17000 cps或其以上、18000 cps或其以上、19000 cps或其以上、或20000 cps或其以上;及60000 cps或其以下、59000 cps或其以下、58000 cps或其以下、57000 cps或其以下、56000 cps或其以下、55000 cps或其以下、54000 cps或其以下、53000 cps或其以下、52000 cps或其以下、51000 cps或其以下、50000 cps或其以下、49000 cps或其以下、48000 cps或其以下、47000 cps或其以下、46000 cps或其以下、45000 cps或其以下、44000 cps或其以下、43000 cps或其以下、42000 cps或其以下、41000 cps或其以下、40000 cps或其以下、39000 cps或其以下、38000 cps或其以下、37000 cps或其以下、36000 cps或其以下、35000 cps或其以下、34000 cps或其以下、33000 cps或其以下、32000 cps或其以下、31000 cps或其以下、或30000 cps或其以下。舉例而言,該黏度可為6000-60000 cps、10000-50000 cps、15000-40000 cps或20000-30000 cps。該組成物可形成具穩固乳化界面之巨乳化顆粒。而且,該無機粉末係被分散在油相中且該不會形成乳化顆粒之單一兩親性異向性粉末也存在用以在即使未存在有其他增稠劑也能提供如此高黏度之製劑。無機粉末可均勻分散而不會沉澱或聚結。此外,該製劑可具有優異之乳化穩定性。The composition may have the following viscosities: 2000 cps or more, 2100 cps or more, 2200 cps or more, 2300 cps or more, 2400 cps or more, 2500 cps or more, 2600 cps or more, 2700 cps or more, 2800 cps or more, 2900 cps or more, 3000 cps or more, 3100 cps or more, 3200 cps or more, 3300 cps or more, 3400 cps or more, 3500 cps or more, 3600 cps or more, 3700 cps or more, 3800 cps or more, 3900 cps or more, 4000 cps or more, 4100 cps or more, 4200 cps or more, 4300 cps or more Above, 4400 cps or above, 4500 cps or above, 4600 cps or above, 4700 cps or above, 4800 cps or above, 4900 cps or above, 5000 cps or above, 5100 cps or above, 5200 cps or more, 5300 cps or more, 5400 cps or more, 5500 cps or more, 5600 cps or more, 5700 cps or more, 5800 cps or more, 5900 cps or more, 6000 cps or above, 6100 cps or above, 6200 cps or above, 6300 cps or above, 6400 cps or above, 6500 cps or above, 7000 cps or above, 7500 cps or above, 8000 cps or above Above, 8500 cps or above, 9000 cps or above, 9500 cps or above, 10000 cps or above, 11000 cps or above, 12000 cps or above, 13000 cps or above, 14000 cps or above, 15,000 cps or more, 16,000 cps or more, 17,000 cps or more, 18,000 cps or more, 19,000 cps or more, or 20,000 cps or more; and 60,000 cps or less, 59,000 cps or less, 58000 cps or less, 57000 cps or less, 56000 cps or less, 55000 cps or less, 54000 cps or less, 53000 cps or less, 52000 cps or less, 51000 cps or less, 50000 cps or below, 49 000 cps or less, 48000 cps or less, 47000 cps or less, 46000 cps or less, 45000 cps or less, 44000 cps or less, 43000 cps or less, 42000 cps or less, 41000 cps or less, 40,000 cps or less, 39,000 cps or less, 38,000 cps or less, 37,000 cps or less, 36,000 cps or less, 35,000 cps or less, 34,000 cps or less, 33,000 cps or less Below, 32000 cps or below, 31000 cps or below, or 30000 cps or below. For example, the viscosity can be 6000-60000 cps, 10000-50000 cps, 15000-40000 cps or 20000-30000 cps. The composition can form large emulsified particles with a stable emulsification interface. Furthermore, the inorganic powder is dispersed in the oil phase and the single amphiphilic anisotropic powder which does not form emulsified particles is also present to provide such high viscosity formulations even in the absence of other thickeners. Inorganic powders are uniformly dispersed without settling or agglomeration. In addition, the formulation may have excellent emulsion stability.
本發明具體實施例之化妝品組成物可能藉由包含以下之方法獲得:製備該兩親性異向性粉末,及使用該兩親性異向性粉末乳化一油相部分及一水相部分。The cosmetic composition of an embodiment of the present invention may be obtained by a method comprising: preparing the amphiphilic anisotropic powder, and using the amphiphilic anisotropic powder to emulsify an oil phase part and an aqueous phase part.
根據一具體實施例,該兩親性異向性粉末可能藉由包含以下之方法獲得:聚合一第一單體以獲得一第一聚合物球形體之核;披覆該第一聚合物球形體之核以獲得具有核-殼結構之一第一聚合物球形體;及使該具核-殼結構之第一聚合物球形體與一第一單體反應以獲得兩親性異向性粉末,其中一第二聚合物球形體係被形成。According to an embodiment, the amphiphilic anisotropic powder may be obtained by a method comprising: polymerizing a first monomer to obtain a core of a first polymer sphere; coating the first polymer sphere to obtain a first polymer sphere having a core-shell structure; and reacting the first polymer sphere having a core-shell structure with a first monomer to obtain an amphiphilic anisotropic powder, One of the second polymeric spherical systems is formed.
圖1係一示意圖,其說明本發明具體實施例之兩親性異向性粉末之形成。可能形成一第二聚合物球形體,其係藉由使該第一聚合物球形體之核貫穿該第一聚合物球形體之殼並藉由使用上述方法朝向外部生長。FIG. 1 is a schematic diagram illustrating the formation of an amphiphilic anisotropic powder according to an embodiment of the present invention. It is possible to form a second polymer sphere by having the core of the first polymer sphere penetrate the shell of the first polymer sphere and grow toward the outside by using the method described above.
根據另一具體實施例,該用於製備兩親性異向性粉末之方法可能包含:(1) 攪拌一第一單體及一聚合反應起始劑以形成一第一聚合物球形體之核;(2) 攪拌該形成之一第一聚合物球形體之核及一第一單體、一聚合反應起始劑及一含官能基團單體以形成具有經披覆之核-殼結構之一第一聚合物球形體;及(3) 攪拌該形成之具核-殼結構之第一聚合物球形體及一第二單體及一聚合反應起始劑以獲得異向性粉末,其中一第二聚合物球形體係被形成。According to another embodiment, the method for preparing an amphiphilic anisotropic powder may include: (1) stirring a first monomer and a polymerization initiator to form a core of a first polymer sphere (2) stirring the core forming a first polymer sphere and a first monomer, a polymerization initiator and a functional group-containing monomer to form a core-shell structure having a coated a first polymer sphere; and (3) stirring the formed first polymer sphere with a core-shell structure and a second monomer and a polymerization initiator to obtain anisotropic powder, wherein a A second polymeric spherical system is formed.
在步驟(1)、(2)及(3)中,該攪拌可為旋轉攪拌。由於需要均勻地機械混合以及化學修飾以產生均勻顆粒,因此較佳為旋轉攪拌。該旋轉攪拌可以在圓柱形反應器中進行,但不限於此。In steps (1), (2) and (3), the stirring may be rotary stirring. Rotary agitation is preferred due to the need for uniform mechanical mixing and chemical modification to produce uniform particles. The rotary stirring may be performed in a cylindrical reactor, but is not limited thereto.
於此,該反應器內部之設計顯著地影響粉末形成。該圓柱形反應器之擋板之大小及位置以及與葉輪之距離對於產生顆粒之均勻性具有顯著影響。較佳地,內葉片及葉輪葉片間之間隔係被最小化以使得其對流及強度均勻,將粉狀反應混合物引入至低於葉片長度之程度並使葉輪保持在高轉速。旋轉速度可為200rpm或其以上,且反應器直徑與高度之比可以為1-3:1-5。特別地,該反應器可能有直徑10-30 cm及高度10-50 cm。該反應器可能有與反應容量成比例之尺寸變量。而且,該圓柱形反應器可能由陶瓷、玻璃等製成。該攪拌較佳係在50-90℃溫度下進行。Here, the design of the reactor interior significantly affects powder formation. The size and position of the baffles of the cylindrical reactor and the distance from the impeller have a significant effect on the uniformity of the particles produced. Preferably, the spacing between the inner vanes and the impeller vanes is minimized to make their convection and intensity uniform, to introduce the powdery reaction mixture below the length of the vanes and to maintain the impeller at high rotational speeds. The rotational speed may be 200 rpm or more, and the ratio of reactor diameter to height may be 1-3:1-5. In particular, the reactor may have a diameter of 10-30 cm and a height of 10-50 cm. The reactor may have dimensional variables proportional to the reaction capacity. Also, the cylindrical reactor may be made of ceramic, glass or the like. The stirring is preferably carried out at a temperature of 50-90°C.
在圓柱形旋轉反應器中之簡單混合可產生均勻顆粒,需要低耗能且提供最大化之反應效率,並因此適於批量生產。習知滾轉(tumbling)方法(包含反應器本身之旋轉)導致該反應器整體於高速度以一定角度及旋轉傾斜,因此需要高耗能並限制該反應器之尺寸。由於反應器大小之此種限制,產量被限制在約數十毫克至數克之小量。因此,習知之滾轉方法並不適用於批量生產。Simple mixing in a cylindrical rotary reactor produces uniform particles, requires low energy consumption and provides maximized reaction efficiency, and is therefore suitable for batch production. The conventional tumbling method (including the rotation of the reactor itself) causes the entire reactor to be tilted at a certain angle and rotation at high speed, thus requiring high energy consumption and limiting the size of the reactor. Due to this limitation in reactor size, yields are limited to small quantities on the order of tens of milligrams to several grams. Therefore, the conventional rolling method is not suitable for mass production.
根據一具體實施例,該第一單體及該第二單體可能相同或不同,且特別地可能為一乙烯基單體。而且,該於步驟(2)加入之第一單體可能與步驟(1)使用之該第一單體相同且該於各步驟中使用之起始劑可能相同或不同。According to an embodiment, the first monomer and the second monomer may be the same or different, and may in particular be a vinyl monomer. Also, the first monomer added in step (2) may be the same as the first monomer used in step (1) and the starter used in each step may be the same or different.
根據另一具體實施例,該乙烯基單體可為一乙烯基芳香族單體。該乙烯基芳香族單體可為經取代或未經取代之苯乙烯。According to another embodiment, the vinyl monomer may be a vinyl aromatic monomer. The vinyl aromatic monomer can be substituted or unsubstituted styrene.
根據還另一具體實施例,該聚合反應起始劑可為自由基聚合反應起始劑。 特別地,該聚合反應起始劑可為一以過氧化物為主或以偶氮為主之起始劑或其組合。而且,可能使用過硫酸銨、過硫酸鈉或過硫酸鉀。According to yet another specific embodiment, the polymerization initiator may be a free radical polymerization initiator. In particular, the polymerization initiator may be a peroxide-based or azo-based initiator or a combination thereof. Furthermore, it is possible to use ammonium persulfate, sodium persulfate or potassium persulfate.
根據還另一具體實施例, 在步驟(1)中,該第一單體及該聚合反應起始劑可以100-1000:1重量比混合。在一變體中,該第一單體及該聚合反應起始劑可以100-750:1、100-500:1或100-250:1重量比混合。According to yet another specific embodiment, in step (1), the first monomer and the polymerization initiator may be mixed in a weight ratio of 100-1000:1. In a variant, the first monomer and the polymerization initiator may be mixed in a weight ratio of 100-750:1, 100-500:1 or 100-250:1.
在一變體中,在步驟(1)中,一穩定劑係與該第一單體及該聚合反應起始劑一起加入,其係以100-1000:1:0.001-5重量比之方式混合該第一單體、該聚合反應起始劑及該穩定劑。該粉末之大小及形狀係藉由控制步驟(1)之該第一聚合物球形體之大小來確認,且該第一聚合物球形體之大小可藉由該第一單體、該聚合反應起始劑及該穩定劑之比例來控制。而且,可能提高異向性粉末之均勻性,其係藉由使該第一單體、該聚合反應起始劑及該穩定劑在上述比例內混合。In a variant, in step (1), a stabilizer is added together with the first monomer and the polymerization initiator, which are mixed in a weight ratio of 100-1000:1:0.001-5 The first monomer, the polymerization initiator and the stabilizer. The size and shape of the powder are confirmed by controlling the size of the first polymer spheres in step (1), and the size of the first polymer spheres can be caused by the first monomer, the polymerization reaction The ratio of the starting agent and the stabilizer is controlled. Also, it is possible to improve the uniformity of the anisotropic powder by mixing the first monomer, the polymerization initiator and the stabilizer within the above-mentioned ratio.
根據一具體實施例,該穩定劑可為離子性乙烯基單體,且可能使用特別為 4-乙烯基苯磺酸鈉(sodium 4-vinylbenzene sulfonate)。該穩定劑防止該顆粒膨脹,且賦予粉末表面正或負價,藉此防止該顆粒靜電聚結(結合)。According to one embodiment, the stabilizer can be an ionic vinyl monomer, and it is possible to use, in particular, sodium 4-vinylbenzene sulfonate. The stabilizer prevents the particles from swelling and imparts positive or negative valence to the powder surface, thereby preventing electrostatic coalescence (bonding) of the particles.
當該兩親性異向性粉末具有200-250 nm大小,其可能由含有以下比例之該第一單體、該聚合反應起始劑及該穩定劑之該第一聚合物球形體獲得:110-130:1:1-5,特別為115-125:1:2-4。When the amphiphilic anisotropic powder has a size of 200-250 nm, it may be obtained from the first polymer spheres containing the first monomer, the polymerization initiator and the stabilizer in the following proportions: 110 -130:1:1-5, especially 115-125:1:2-4.
而且,當該兩親性異向性粉末具有400-450 nm之大小,其可能由含有以下比例之該第一單體、該聚合反應起始劑及該穩定劑之該第一聚合物球形體獲得:225-240:1:1-3,特別為230-235:1:1-3。Also, when the amphiphilic anisotropic powder has a size of 400-450 nm, it may be composed of the first polymer spheres containing the first monomer, the polymerization initiator and the stabilizer in the following proportions Obtained: 225-240:1:1-3, specifically 230-235:1:1-3.
此外,當該兩親性異向性粉末具有1100-2500 nm之大小,其可能由藉以下比例之該第一單體、該聚合反應起始劑及該穩定劑反應製得之該第一聚合物球形體獲得:110-130:1:0,特別為115-125:1:0。In addition, when the amphiphilic anisotropic powder has a size of 1100-2500 nm, it may be obtained by the first polymerization prepared by reacting the first monomer, the polymerization initiator and the stabilizer in the following proportions Sphere body gain: 110-130:1:0, specifically 115-125:1:0.
而且,具不對稱雪人形狀之兩親性異向性粉末可能由藉以下比例之該第一單體、該聚合反應起始劑及該穩定劑反應製得之該第一聚合物球形體獲得:100-140:1:8-12,特別為110-130:1:9-11。Furthermore, the amphiphilic anisotropic powder with an asymmetric snowman shape may be obtained from the first polymer spheres prepared by reacting the first monomer, the polymerization initiator and the stabilizer in the following proportions: 100-140:1:8-12, especially 110-130:1:9-11.
此外,具不對稱倒雪人形狀之兩親性異向性粉末可能由藉以下比例之該第一單體、該聚合反應起始劑及該穩定劑反應製得之該第一聚合物球形體獲得:100-140:1:1-5,特別為110-130:1:2-4。In addition, an amphiphilic anisotropic powder with an asymmetric inverted snowman shape may be obtained from the first polymer spheres prepared by reacting the first monomer, the polymerization initiator and the stabilizer in the following proportions : 100-140:1:1-5, especially 110-130:1:2-4.
根據還另一具體實施例,步驟(2)之該含官能基團之單體可能為含矽氧烷之(甲基)丙烯酸酯,諸如3-(三甲氧基矽基)丙烯酸丙酯(3-(trimethoxysilyl)propyl acrylate)、3-(三甲氧基矽基)甲基丙烯酸丙酯(3-(trimethoxysilyl)propyl methacrylate)、乙烯基三乙氧矽烷(vinyl triethoxysilane)、乙烯基三甲氧矽烷(vinyl trimethoxysilane)或其組合。According to yet another specific embodiment, the functional group-containing monomer of step (2) may be a siloxane-containing (meth)acrylate, such as 3-(trimethoxysilyl)propyl acrylate (3 -(trimethoxysilyl)propyl acrylate), 3-(trimethoxysilyl)propyl methacrylate, vinyl triethoxysilane, vinyl trimethoxysilane trimethoxysilane) or a combination thereof.
根據還另一具體實施例,在步驟(2)中,該第一單體、該聚合反應起始劑及該含官能基團化合物可以80-98:0.2-1.0:1-20重量比混合。在一變體中,該第一單體、該聚合反應起始劑及該含官能基團化合物可以160-200:1:6-40重量比混合。可能根據該反應比例控制披覆程度,然後披覆程度決定兩親性異向性粉末之形狀。當該第一單體、該聚合反應起始劑及該含官能基團化合物係在上述比例內使用,該披覆後度以起始厚度為基礎增加約10-30%,特別為約20%。於此情況下,粉末之形成順利進行,沒有諸如因披覆過厚導致無法形成粉末或因披覆過薄導致粉末多向形成之問題。而且,在上述重量比內可能提高異向性粉末均勻性。According to yet another specific embodiment, in step (2), the first monomer, the polymerization initiator and the functional group-containing compound may be mixed in a weight ratio of 80-98:0.2-1.0:1-20. In a variant, the first monomer, the polymerization initiator and the functional group-containing compound may be mixed in a weight ratio of 160-200:1:6-40. It is possible to control the degree of coating according to the reaction ratio, which then determines the shape of the amphiphilic anisotropic powder. When the first monomer, the polymerization initiator and the functional group-containing compound are used within the above ratios, the coating thickness is increased by about 10-30%, especially about 20%, based on the initial thickness . In this case, the powder formation proceeds smoothly, and there are no problems such as failure to form powder due to too thick coating or multidirectional formation of powder due to too thin coating. Also, it is possible to improve the uniformity of the anisotropic powder within the above weight ratio.
在步驟(3)中,該第一聚合物球形體之核貫穿該殼,由具核-殼結構之該第一聚合物球形體之一方向突出其殼。然後,該突出部分可由該第二單體之聚合物生長以形成異向性粉末之形狀。In step (3), the core of the first polymer sphere penetrates the shell, and the shell protrudes from one direction of the first polymer sphere with the core-shell structure. The protruding portion can then be grown from the polymer of the second monomer to form the shape of the anisotropic powder.
根據還另一具體實施例,在步驟(3)中,該第二單體及該聚合反應起始劑可於150-250:1重量比混合。在一變體,該第二單體及該聚合反應起始劑可於以下重量比混合:160-250:1、170-250:1、180-250:1、190-250:1、200-250:1、210-250:1、220-250: 1、230-250:1或240-250:1。According to yet another specific embodiment, in step (3), the second monomer and the polymerization initiator may be mixed in a weight ratio of 150-250:1. In a variant, the second monomer and the polymerization initiator may be mixed in the following weight ratios: 160-250:1, 170-250:1, 180-250:1, 190-250:1, 200- 250:1, 210-250:1, 220-250:1, 230-250:1 or 240-250:1.
在一變體中,在步驟(3)中,一穩定劑可與該第二單體及該聚合反應起始劑一起加入,其係以該第二單體、該聚合反應起始劑及該穩定劑為150-250:1:0.001-5重量比之方式混合。該穩定劑之特別例係與上述相同。上述重量比可能提高異向性粉末均勻性。In a variant, in step (3), a stabilizer can be added together with the second monomer and the polymerization initiator, which is based on the second monomer, the polymerization initiator and the The stabilizer is mixed in a weight ratio of 150-250:1:0.001-5. Specific examples of the stabilizer are the same as described above. The above weight ratio may improve anisotropic powder uniformity.
根據還另一具體實施例,在步驟(3)中,該第二單體以100重量份具核-殼結構之該第一聚合物球形體為基礎可於40-300重量份之量混合。特別地,當該第二單體以該第一聚合物球形體100重量份為基礎之含量為40-100重量份,獲得不對稱雪人形粉末。當該第二單體之含量為100-150重量份或110-150重量份,獲得對稱之粉末。而且,當該第二單體之含量為150-300重量份或160-300重量份,獲得不對稱倒雪人形粉末。上述重量比可能提高異向性粉末均勻性。According to yet another specific embodiment, in step (3), the second monomer can be mixed in an amount of 40-300 parts by weight based on 100 parts by weight of the first polymer sphere having a core-shell structure. Particularly, when the content of the second monomer is 40-100 parts by weight based on 100 parts by weight of the first polymer spherical body, an asymmetric snowman-shaped powder is obtained. When the content of the second monomer is 100-150 parts by weight or 110-150 parts by weight, a symmetrical powder is obtained. Also, when the content of the second monomer is 150-300 parts by weight or 160-300 parts by weight, an asymmetric inverted snowman-shaped powder is obtained. The above weight ratio may improve anisotropic powder uniformity.
根據還另一具體實施例,該用於製備兩親性異向性粉末之方法可能進一步包括在步驟(3)後之步驟(4)引入親水性官能基團至該異向性粉末。According to yet another specific embodiment, the method for preparing an amphiphilic anisotropic powder may further include introducing a hydrophilic functional group to the anisotropic powder in step (4) after step (3).
根據還另一具體實施例,步驟(4)之該親水性官能基團可能使用矽烷偶聯劑及反應改質劑引入,但不限於此。According to yet another specific embodiment, the hydrophilic functional group in step (4) may be introduced by using a silane coupling agent and a reaction modifier, but is not limited thereto.
根據還另一具體實施例,該矽烷偶聯劑可為至少一 選自於由以下所組成之群組:N-[(3-(三甲氧基矽基)丙基) 乙二胺(N-[(3-(trimethoxysilyl)propyl)ethylenediamine],N-[3-(三甲氧基矽基)丙基]乙烯二銨氯化物(N-[3-(trimethoxysilyl)propyl]ethylene diammonium chloride),(N-丁二醯基-3-胺基丙基)三甲氧基矽烷((N-succinyl-3-aminopropyl)trimethoxysilane),1-[3-(三甲氧基矽基)丙基]脲(1-[3-(trimethoxysilyl)propyl]urea)及3-[(三甲氧基矽基)丙基氧基]-1,2-丙二醇(3-[(trimethoxysilyl)propyloxy]-1,2-propanediol)。特別地,該矽烷偶聯劑可為N-[(3-(三甲氧基矽基)丙基)乙二胺。According to yet another embodiment, the silane coupling agent may be at least one selected from the group consisting of: N-[(3-(trimethoxysilyl)propyl)ethylenediamine (N- [(3-(trimethoxysilyl)propyl)ethylenediamine], N-[3-(trimethoxysilyl)propyl]ethylene diammonium chloride, (N-[3-(trimethoxysilyl)propyl]ethylene diammonium chloride -Butanediyl-3-aminopropyl)trimethoxysilane ((N-succinyl-3-aminopropyl)trimethoxysilane), 1-[3-(trimethoxysilyl)propyl]urea (1-[ 3-(trimethoxysilyl)propyl]urea) and 3-[(trimethoxysilyl)propyloxy]-1,2-propanediol (3-[(trimethoxysilyl)propyloxy]-1,2-propanediol). In particular , the silane coupling agent can be N-[(3-(trimethoxysilyl)propyl)ethylenediamine.
根據還另一具體實施例,該矽烷偶聯劑以100重量份步驟(3)獲得之異向性粉末為基礎可於以下量混合:35-65重量份,特別為40-60重量份。可在上述範圍內充分進行親水化。According to yet another specific embodiment, the silane coupling agent can be mixed in the following amount based on 100 parts by weight of the anisotropic powder obtained in step (3): 35-65 parts by weight, especially 40-60 parts by weight. Hydrophilization can be sufficiently performed within the above range.
根據還另一具體實施例,該反應改質劑可為氫氧化銨。According to yet another specific embodiment, the reaction modifier may be ammonium hydroxide.
根據還另一具體實施例,該反應改質劑以100重量份步驟(3)獲得之異向性粉末為基礎可於以下量混合:85-115重量份,特別為90-110重量份。可在上述範圍內充分進行親水化。According to yet another specific embodiment, the reaction modifier can be mixed in the following amount based on 100 parts by weight of the anisotropic powder obtained in step (3): 85-115 parts by weight, especially 90-110 parts by weight. Hydrophilization can be sufficiently performed within the above range.
根據還另一具體實施例,用於製備兩親性異向性粉末之方法可進一步包含在步驟(3)後之步驟(4)引入一含醣官能基團至該異向性粉末。According to yet another specific embodiment, the method for preparing an amphiphilic anisotropic powder may further include introducing a sugar-containing functional group to the anisotropic powder in step (4) after step (3).
在步驟(4)中,該含醣官能基團可使用一含醣矽烷偶聯劑及一反應改質劑引入,但不限於此。In step (4), the sugar-containing functional group can be introduced using a sugar-containing silane coupling agent and a reaction modifier, but is not limited thereto.
根據還另一具體實施例,該含醣矽烷偶聯劑可為至少一 選自於由以下所組成之群組:N-{N-(3-三乙氧基矽基丙基) 氨基乙基}葡糖醯胺(N-{N-(3-triethoxysilylpropyl) aminoethyl}gluconamide),N-(3-三乙氧基矽基丙基)葡糖醯胺(N-(3-triethoxysilylpropyl) gluconamide)及N-{N-(3-三乙氧基矽基丙基)氨基乙基}-寡-質酸醯胺(N-{N-(3-triethoxysilylpropyl)aminoethyl}-oligo-hyaluronamide)。According to yet another embodiment, the sugar-containing silane coupling agent may be at least one selected from the group consisting of: N-{N-(3-triethoxysilylpropyl)aminoethyl } Glucosamide (N-{N-(3-triethoxysilylpropyl) aminoethyl}gluconamide), N-(3-triethoxysilylpropyl) gluconamide and N-{N-(3-triethoxysilylpropyl)aminoethyl}-oligo-hyaluronamide.
根據還另一具體實施例,該反應改質劑 可為氫氧化銨。According to yet another specific embodiment, the reaction modifier may be ammonium hydroxide.
根據還另一具體實施例,該反應改質劑以100重量份步驟(3)獲得之異向性粉末為基礎可於以下量混合:85-115重量份,特別為90-110重量份。可在上述範圍內充分引入該含醣官能基團。According to yet another specific embodiment, the reaction modifier can be mixed in the following amount based on 100 parts by weight of the anisotropic powder obtained in step (3): 85-115 parts by weight, especially 90-110 parts by weight. The sugar-containing functional group can be sufficiently introduced within the above range.
本文所述用於製備兩親性異向性粉末之方法沒有使用交聯劑,因此不會造成集聚作用及提供高產量及均勻性。而且,本文所述方法使用簡單攪拌製程,相較於滾轉製程更適合批量生產。特別地,本文所述方法之優勢在於可於數十克及數十公斤之大規模生產300 nm大小或更小之奈米大小顆粒。The methods described herein for preparing amphiphilic anisotropic powders do not use cross-linking agents, thus do not cause agglomeration and provide high yield and uniformity. Moreover, the method described herein uses a simple stirring process, which is more suitable for mass production than a tumbling process. In particular, an advantage of the methods described herein is that nano-sized particles of 300 nm size or smaller can be produced on a large scale in tens of grams and tens of kilograms.
根據還另一具體實施例,該組成物可進一步包含一有機UV阻斷劑。該有機UV阻斷劑可包含於美容領域慣用之UV阻斷劑。特別地,該UV阻斷劑可為至少一選自於由三嗪(triazine)、三嗪酮(triazone)、肉桂酸酯(cinnamate)、水楊酸酯(salicylate)、辛烯腈(octocrylene)、二苯甲酮(benzophenone)、苯基苯並咪唑磺酸(phenylbenzimidazole sulfonic acid)、二樟腦磺酸(dicamphor sulfonic acid)、丁基甲氧基二苯甲醯甲烷(butylmethoxydibenzoyl methane)( 亞佛苯酮(avobenzone))及甲酚曲唑三矽氧烷(drometrizole trisiloxane)所組成之群組,但不限於此。According to yet another specific embodiment, the composition may further comprise an organic UV blocking agent. The organic UV blocking agent may include a conventional UV blocking agent in the cosmetic field. In particular, the UV blocking agent may be at least one selected from the group consisting of triazine, triazone, cinnamate, salicylate, and octocrylene. , benzophenone, phenylbenzimidazole sulfonic acid, dicamphor sulfonic acid, butylmethoxydibenzoyl methane ( avobenzone) and drometrizole trisiloxane, but not limited thereto.
該有機UV阻斷劑以該組成物總重為基礎可以0.1-10 wt%之量使用。可在上述範圍內改善UV阻斷效果而無皮膚刺激。The organic UV blocking agent may be used in an amount of 0.1-10 wt% based on the total weight of the composition. The UV blocking effect can be improved within the above range without skin irritation.
根據還另一具體實施例,該乳化物組成物可為水包油(oil-in- water)或油包水(water-in-oil)型乳化物組成物,特別為油包水型組成物。According to yet another specific embodiment, the emulsion composition may be an oil-in-water or water-in-oil type emulsion composition, especially a water-in-oil type composition .
當該組成物係油包水型組成物,該無機粉末存在於作為外相之油相中,因而可穩定分散不會有上述之無機顆粒沉澱或聚結。When the composition is a water-in-oil type composition, the inorganic powder exists in the oil phase as the external phase, so that it can be stably dispersed without precipitation or agglomeration of the above-mentioned inorganic particles.
該油包水型乳化物組成物有作為外相之油相,因而顯示優異之防水性及持久性。根據本組成物,該作為內相之巨顆粒在施用時被擠出至皮膚以藉由摻水現象提供清爽感。因而可避免當外相為油相時可能發生之黏膩感或不適使用感。The water-in-oil emulsion composition has an oil phase as an external phase, and thus exhibits excellent water repellency and durability. According to the present composition, the macroparticles as the internal phase are extruded to the skin upon application to provide a refreshing feeling by the phenomenon of water incorporation. Thus, the sticky or uncomfortable feeling that may occur when the external phase is an oil phase can be avoided.
本發明之一具體實施例之組成物在無增稠劑之情況下達到高黏度且不需分散劑而使無機粉末穩定分散。因而可防止由於添加增稠劑、分散劑或過量表面活性劑而發生之皮膚刺激。The composition of an embodiment of the present invention achieves high viscosity without thickener and does not require dispersant to stably disperse the inorganic powder. Skin irritation due to the addition of thickeners, dispersants or excess surfactants is thus prevented.
本發明之具體實施例之組成物即使含有無機粉末仍顯示出優異之乳化物穩定性,因而可提供乳化物組成物之柔軟使用感同時有摻水效果所致之清爽感及含水(watery)感。特別地,該組成物即使存在有高含量無機粉末仍顯示出上述效果而不影響其穩定性。The composition of the specific embodiment of the present invention exhibits excellent emulsion stability even if it contains inorganic powder, so that it can provide the emulsion composition with a soft use feeling and a refreshing feeling and watery feeling due to the water-incorporating effect. . In particular, the composition exhibits the above-mentioned effects without affecting its stability even in the presence of a high content of inorganic powder.
本發明具體實施例之組成物顯示出在廣溫度範圍內隨時間經過之乳化物穩定性,諸如自-15°C至60°C、特別為-10°C至55°C之溫度範圍。The compositions of embodiments of the present invention exhibit emulsion stability over time over a wide temperature range, such as from -15°C to 60°C, particularly -10°C to 55°C.
本發明具體實施例之組成物包含巨乳化顆粒以提供柔軟及絲滑之使用感。The composition of an embodiment of the present invention contains macroemulsified particles to provide a soft and silky feel in use.
本發明具體實施例之組成物不僅提供清透(clear)感及清涼(cooling)感且能實現優異之含水感及保濕效果,在習知皮膚製劑之情況下則可能有不足之含水感及保濕效果。The composition of the specific embodiment of the present invention not only provides a clear and cooling feeling but also can achieve excellent water feeling and moisturizing effect, which may have insufficient water feeling and moisturizing effect in the case of conventional skin preparations Effect.
本發明具體實施例之組成物提供一霧面及粉狀完成感,其係憑藉存在未形成乳化顆粒之單獨兩親性異向性粉末。The compositions of embodiments of the present invention provide a matte and powdery finish by virtue of the presence of a single amphiphilic anisotropic powder that does not form emulsified particles.
本發明具體實施例之組成物可被配製成各種製劑,包含化妝水(lotion)、乳化物或霜劑(cream)。舉例而言,該組成物可被配製成能提供清透感及含水感之之男士鬚後水(aftershave cosmetics),但不限於此。The compositions of embodiments of the present invention may be formulated into various formulations, including lotions, emulsions or creams. For example, but not limited to, the composition may be formulated to provide men's aftershave cosmetics that provide a clear and hydrated feel.
本發明具體實施例之組成物可將美容或皮膚學上可接受之介質或基質併入來配製。如此之製劑包含任何適用於局部施用之製劑,且可以懸浮液、微乳化物、微膠囊、微顆粒或離子(脂質體)及非離子型囊泡分散劑之形式提供,或霜劑、薄層(skin)、化妝水(lotion)、粉末、軟膏、噴霧或遮瑕棒(conceal stick)之形式提供。而且,該組成物可以泡沫體或氣膠組成物之形式使用,其進一步包含加壓推進劑。如此組成物可由該領域技術人士之已知方法獲得。Compositions of embodiments of the present invention may be formulated incorporating a cosmetically or dermatologically acceptable vehicle or base. Such formulations include any formulation suitable for topical administration and may be provided in the form of suspensions, microemulsions, microcapsules, microparticles or ionic (liposomes) and nonionic vesicle dispersions, or as creams, thin layers (skin), lotion (lotion), powder, ointment, spray or concealer stick (conceal stick) form. Furthermore, the composition may be used in the form of a foam or aerosol composition further comprising a pressurized propellant. Such compositions can be obtained by methods known to those skilled in the art.
本發明具體實施例之組成物可包含習知用於美容或皮膚領域中之補充成份,諸如粉末、脂質、有機溶劑、增溶劑、濃縮劑、膠凝劑、軟化劑、抗氧化劑、懸浮劑、穩定劑、發泡劑、芳香劑、表面活性劑、水、離子或非離子乳化劑、填料、金屬離子螯合劑、螯合劑、防腐劑、維生素、保護劑、潤濕劑、精油(essential oil)、染料、顏料、親水性或親油性活化劑、脂質囊泡或習知用於美容之任何其他成份。此補充成份係以美容或皮膚領域通常使用量引入。本發明具體實施例之組成物可進一步包含皮膚吸收促進劑以提高改善膚況之效果。 發明實施模式Compositions of embodiments of the present invention may contain supplementary ingredients conventionally used in the cosmetic or dermatological fields, such as powders, lipids, organic solvents, solubilizers, concentrates, gelling agents, emollients, antioxidants, suspending agents, Stabilizers, foaming agents, fragrances, surfactants, water, ionic or nonionic emulsifiers, fillers, metal ion sequestrants, chelating agents, preservatives, vitamins, protective agents, wetting agents, essential oils , dyes, pigments, hydrophilic or lipophilic activators, lipid vesicles or any other ingredient conventionally used for cosmetic purposes. This supplement is introduced in amounts commonly used in the cosmetic or dermatological field. The composition of an embodiment of the present invention may further comprise a skin absorption enhancer to enhance the effect of improving skin condition. Invention Implementation Mode
現在將對實施例進行敘述以詳細說明本發明。本領域技術人員將理解以下實施例僅用於說明目的,並非意圖限制本發明之範圍。Examples will now be described to illustrate the invention in detail. Those skilled in the art will understand that the following examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
[ 製備實施例 1-4]
根據下表1之組成物獲得製備實施例 1-4。下文將說明該製備方法。 用於製備實施例1-4之成份係如下所示。 [表 1]
TMSPA:三甲氧基矽基丙烯酸丙酯(Trimethoxysilyl propylacrylate)(官能基團) TMSPA: Trimethoxysilyl propylacrylate (functional group)
AIBN:偶氮二異丁腈(Azobisisobutyronitrile)(聚合反應起始劑) AIBN: Azobisisobutyronitrile (polymerization initiator)
製備實施例1. 製備聚苯乙烯(PS)第一聚合物球形體Preparation Example 1. Preparation of Polystyrene (PS) First Polymer Spheroids
首先,50g苯乙烯單體、1.0g之4-乙烯基苯磺酸鈉穩定劑及0.5g偶氮二異丁腈(AIBN)聚合反應起始劑係在水相中經混合並在75℃下反應8小時。該反應係藉由在直徑11cm高度17cm及由玻璃製成之圓柱形反應器中以200rpm速度攪拌該反應混合物來進行。 First, 50 g of styrene monomer, 1.0 g of sodium 4-vinylbenzenesulfonate stabilizer and 0.5 g of azobisisobutyronitrile (AIBN) polymerization initiator were mixed in the aqueous phase and heated at 75°C The reaction was carried out for 8 hours. The reaction was carried out by stirring the reaction mixture at a speed of 200 rpm in a cylindrical reactor 11 cm in diameter and 17 cm in height and made of glass.
製備實施例2. 製備經披覆之具核-殼(CS)結構之第一聚合物球形體Preparation Example 2. Preparation of Coated First Polymer Spheroids with Core-Shell (CS) Structure
首先,由上述獲得之300g聚苯乙烯(PS)第一聚合物球形顆粒與50g苯乙烯單體混合,使6g之3-(三甲氧基矽基)丙烯酸丙酯(TMSPA)及0.2g偶氮二異丁腈(AIBN)聚合反應起始劑及該反應混合物於75℃反應8小時。該反應藉由在一圓柱形反應器中攪拌反應混合物來進行。 First, 300 g of polystyrene (PS) first polymer spherical particles obtained above were mixed with 50 g of styrene monomer to make 6 g of 3-(trimethoxysilyl) propyl acrylate (TMSPA) and 0.2 g of azo Diisobutyronitrile (AIBN) polymerization initiator and the reaction mixture were reacted at 75°C for 8 hours. The reaction is carried out by stirring the reaction mixture in a cylindrical reactor.
製備實施例3. 製備兩親性異向性粉末(DB)Preparation Example 3. Preparation of Amphiphilic Anisotropic Powder (DB)
首先,將上述得到之聚苯乙烯-核殼(PS-CS)分散物之240g水性分散物與40g苯乙烯單體、0.35g之4-乙烯基苯磺酸鈉穩定劑及0.2g偶氮二異丁腈(AIBN)聚合反應起始劑混合,該反應混合物係被加熱至75℃以進行反應8小時。該反應藉由在一圓柱形反應器中攪拌該反應混合物來進行。於此方式中獲得兩親性異向性粉末。 First, 240 g of the aqueous dispersion of the polystyrene-core-shell (PS-CS) dispersion obtained above was mixed with 40 g of styrene monomer, 0.35 g of sodium 4-vinylbenzenesulfonate stabilizer and 0.2 g of azodicarbonate. Isobutyronitrile (AIBN) polymerization initiators were mixed, and the reaction mixture was heated to 75°C for 8 hours. The reaction is carried out by stirring the reaction mixture in a cylindrical reactor. In this way amphiphilic anisotropic powders are obtained.
製備實施例4. 製備親水化兩親性異向性粉末Preparation Example 4. Preparation of Hydrophilized Amphiphilic Anisotropic Powder
首先,如上述獲得之該異向性粉末之600 g 水性分散物係與30 g之N-[3-(三甲氧基矽基)丙基]乙二胺)矽烷偶聯劑及60 g氫氧化銨之反應改質劑混合,且使該反應混合物於25°C反應24小時以引入親水性官能基團。該反應藉由在一圓柱形反應器中攪拌該反應混合物進行以獲得親水性兩親性異向性粉末。First, 600 g of the aqueous dispersion of the anisotropic powder obtained as above was mixed with 30 g of N-[3-(trimethoxysilyl)propyl]ethylenediamine)silane coupling agent and 60 g of hydroxide A reaction modifier of ammonium was mixed, and the reaction mixture was reacted at 25° C. for 24 hours to introduce hydrophilic functional groups. The reaction was carried out by stirring the reaction mixture in a cylindrical reactor to obtain a hydrophilic amphiphilic anisotropic powder.
[ 實施例及比較實施例 ] 製備乳化型組成物 實施例1及2與比較實施例1之油包水型乳化物組成物係根據下表2之組成物製備。實施例1及2係藉由使用根據製備實施例3製得之該兩親性異向性粉末獲得之乳化物組成物,且比較實施例1係使用習知表面活性劑之一乳化物組成物。 [ Examples and Comparative Examples ] Preparation of emulsified compositions The water-in-oil emulsion compositions of Examples 1 and 2 and Comparative Example 1 were prepared according to the compositions of Table 2 below. Examples 1 and 2 are emulsion compositions obtained by using the amphiphilic anisotropic powder prepared according to Preparation Example 3, and Comparative Example 1 is an emulsion composition using one of the conventional surfactants .
特別地,根據表2之組成物,該油相係被加熱溶解(30°C)。然後,該油相被移至水相並進行初步乳化。之後,引入增稠劑並進行二次乳化,然後進行冷卻及除氣。In particular, according to the composition of Table 2, the oil phase was dissolved by heating (30°C). Then, the oil phase is moved to the water phase and subjected to preliminary emulsification. After that, a thickener is introduced and secondary emulsification is performed, followed by cooling and degassing.
該用於以下實施例及比較實施例之成分係如下所示。 (a) 矽油: 環戊矽氧烷(Cyclopentasiloxane)及環己矽氧烷(cyclohexasiloxane)(PMX-0345 SILOXANE BLEND, Dow Corning) 苯基三甲聚矽氧烷(Phenyl trimethicone)(KF56, Shin Etsu) (b) 油: C12-C15醇苯甲酸酯(Finsolv TN-O, innospec) (c) 無機UV阻斷劑: 二氧化鈦及氧化鋁及硬脂酸(UV Titan M160, Kemira, 17-20 nm) 二氧化鈦及氫氧化鋁及硬脂酸(MT-014Z, Tayca, minor 30-60 nm/major 80-160 nm) (d) 表面活性劑:月桂基PEG-9聚二甲基甲矽烷氧基乙基聚二甲基矽氧烷(Lauryl PEG-9 polydimethylsiloxyethyldimethicone) (KF-6038, Shin Etsu) (e) 兩親性異向性粉末:製備實施例3之兩親性異向性粉末 (f) 金屬離子螯合劑:二鈉EDTA (E.D.T.A.-2NA, Neord Co., Ltd.) (g) 保濕劑:1,3-丁二醇(Daicel) (h) 溶劑:乙醇The ingredients used in the following examples and comparative examples are shown below. (a) Silicone oils: Cyclopentasiloxane and cyclohexasiloxane (PMX-0345 SILOXANE BLEND, Dow Corning) Phenyl trimethicone (KF56, Shin Etsu) ( b) Oil: C12-C15 Alcohol Benzoate (Finsolv TN-O, innospec) (c) Inorganic UV Blockers: Titanium Dioxide and Alumina and Stearic Acid (UV Titan M160, Kemira, 17-20 nm) Titanium Dioxide and aluminum hydroxide and stearic acid (MT-014Z, Tayca, minor 30-60 nm/major 80-160 nm) (d) Surfactant: lauryl PEG-9 polydimethylsiloxyethyl poly Dimethylsiloxane (Lauryl PEG-9 polydimethylsiloxyethyldimethicone) (KF-6038, Shin Etsu) (e) Amphiphilic anisotropic powder: Amphiphilic anisotropic powder of Preparation Example 3 (f) Metal ion chelate Mixture: Disodium EDTA (EDTA-2NA, Neord Co., Ltd.) (g) Humectant: 1,3-Butanediol (Daicel) (h) Solvent: Ethanol
[表2]
[ 測試實施例 1] 評價物理性質
使用黏度劑(LVDV-II+PRO, BROOKFIELD, USA)於30°C測定實施例1及2與比較實施例1之各組成物之黏度。此外,經電子顯微影像確認各組成物中之乳化顆粒平均粒徑。然後將結果與施用於皮膚之使用感一起示於下表3中。該電子顯微影像係示於圖2中。 [表3]
由圖2及表3之結果可見,實施例1及2各自形成高黏度穩定之乳化物且具有大乳化顆粒平均粒徑,藉此提供顯著之乳化顆粒相反轉效果。相反地,比較實施例1具有小乳化顆粒及低黏度。由於如此低之黏度,比較實施例1有無機粉末沉澱之高度可能性且可能因無機粉末容易聚結而造成白色渾濁現象。As can be seen from the results in FIG. 2 and Table 3, each of Examples 1 and 2 formed a highly viscosity-stable emulsion and had a large average particle size of the emulsified particles, thereby providing a significant phase inversion effect of the emulsified particles. In contrast, Comparative Example 1 had small emulsified particles and low viscosity. Due to such a low viscosity, Comparative Example 1 has a high possibility of inorganic powder precipitation and may cause white turbidity due to the easy agglomeration of the inorganic powder.
[ 測試實施例 2] 評價使用感
令三十位二十多歲至四十多歲之女性品評小組使用由比較實施例1及實施例1獲得之化妝品組成物。然後,令該等品評小組評價施用於皮膚時之油質感、含水感、延展性及清涼效果及在施用後之清爽及霧面感,其係基於10等級(等級1: 極低至等級10: 極高)。平均值之結果係示於下表4中。 [表4]
由上述結果可見使用粉末乳化作用之油包水型UV阻斷劑改善使用傳統使用之無機UV阻斷劑之油包水型UV阻斷化妝品組成物之問題,其包含黏膩及油質使用感及乾燥之使用感。而且,實施例1避免使用表面活性劑及分散劑以降低施用時之明顯油質感。由於巨乳化顆粒之摻水效果,實施例1即使高黏度亦改善施用時之輕薄及含水延展性。此外,由於該兩親性異向性粉末,實施例1顯示施用後不會因表面活性劑引起殘留感,且提供清爽及霧面之使用感。相反地,使用傳統表面活性劑之比較實施例1顯示高度油質感及不佳之含水感且具有較低之清涼效果及霧面感,因而提供較差之使用感。From the above results, it can be seen that the use of the water-in-oil UV blocking agent with powder emulsification improves the problems of the water-in-oil UV blocking cosmetic composition using the conventionally used inorganic UV blocking agent, which includes stickiness and oily feeling in use. and dry feel. Furthermore, Example 1 avoids the use of surfactants and dispersants to reduce the overt oily feel upon application. Due to the water-incorporating effect of the giant emulsified particles, even the high viscosity of Example 1 improves the lightness and water ductility during application. In addition, due to the amphiphilic anisotropic powder, Example 1 shows no residual feeling due to surfactant after application, and provides a refreshing and matte feeling in use. In contrast, Comparative Example 1 using the conventional surfactant showed a high oily feel and a poor watery feel and had a lower cooling effect and a matte feel, thus providing a poor feeling in use.
[ 測試實施例 3] 評價 UV 阻斷效果 評估實施例1及比較實施例1各組成物之UV阻斷效果。 [ Test Example 3] Evaluation of UV blocking effect The UV blocking effect of each of the compositions of Example 1 and Comparative Example 1 was evaluated.
該防曬係數(SPF)係藉由選擇包含6男6女之12位受試者來確定,並用陽光模擬儀(81293 (Xenon UV Lamp 1 kW,未經過濾)燈在20-100 mj/cm2
受控劑量下將紫外線照射到除了脊柱以外之每個受試者之右及左背部,該劑量係藉由使用IL1733輻射計及SED 240探頭來控制。然後,在UV照射24小時後確定該確定最小發紅劑量(MED)。 為了確定樣品之UV阻斷效果,實施例1及比較實施例1各以2 μL/cm2
之厚度被均勻地施用至該受試者之背部並停留15分鐘乾燥。該UV照射係UV照射窗被連接及固定在該實施例1及比較實施例1之樣品施用部位時進行,而照射窗以外之部位係使用皮革及毛巾遮擋住UV射線。然後在該UV照射24小時後,根據以下數學式1確認該最小發紅劑量及計算防曬係數(SPF)。結果示於下表5。 [數學式1] 防曬係數(SPF) = 施用產物部位之最小發紅劑量(MED)/非施用部位之最小發紅劑量(MED) [表5]
可見實施例1顯示相較於使用慣用表面活性劑之比較實施例1明顯較高之劑量穩定性及使用感,同時提供與比較實施例1相等之UV阻斷效果。It can be seen that Example 1 shows significantly higher dose stability and feel in use than Comparative Example 1 using conventional surfactants, while providing the same UV blocking effect as Comparative Example 1.
圖1係一示意圖,其說明本發明具體實施例之兩親性異向性粉末之形成。 圖2顯示實施例1及2之組成物之乳化顆粒於30°C觀察到之電子顯微影像。FIG. 1 is a schematic diagram illustrating the formation of an amphiphilic anisotropic powder according to an embodiment of the present invention. Figure 2 shows the electron microscopic images of the emulsified particles of the compositions of Examples 1 and 2 observed at 30°C.
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