TWI751992B - Emulsion type cosmetic composition comprising inorganic uv blocking agent and method for preparing same - Google Patents

Abstract

Disclosed is an emulsion type cosmetic composition including an inorganic UV blocking agent and amphiphilic anisotropic powder, wherein the inorganic UV blocking agent is inorganic powder, the amphiphilic anisotropic powder includes a first hydrophilic polymer spheroid and a second hydrophobic polymer spheroid, the first polymer spheroid and the second polymer spheroid are bound to each other with a structure in which one polymer spheroid at least partially penetrates into the other polymer spheroid, the first polymer spheroid has a core-shell structure, and the shell has a functional group.

Description

Emulsified cosmetic composition including inorganic UV blocking agent and preparation method thereof

The invention relates to an emulsified cosmetic composition containing an inorganic UV blocking agent and a preparation method thereof.

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.

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.

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.

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.

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.

technical problem

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.

Another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition with excellent skin safety.

Yet another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition, which can improve the white turbidity.

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.

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.

Yet another technical problem to be solved by the present invention is to provide an emulsified cosmetic composition with excellent water resistance and durability.

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

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

In one aspect, the present invention provides an emulsified cosmetic composition comprising an inorganic UV blocking agent stably dispersed therein.

In another aspect, the present invention provides an emulsified cosmetic composition with excellent skin safety.

In yet another aspect, the present invention provides an emulsified cosmetic composition that improves white cloudiness.

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.

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.

In yet another aspect, the present invention provides an emulsified cosmetic composition having excellent water resistance and durability.

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.

best practice

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.

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.

As used herein, "(meth)acryloyl" means acryl and/or methacryloyl.

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.

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.

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.

In one aspect, an emulsified cosmetic composition is provided comprising an inorganic UV blocker and an amphiphilic anisotropic powder.

According to an embodiment, the inorganic UV blocking agent may be an inorganic powder capable of providing UV blocking effect.

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.

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.

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).

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.

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.

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.

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.

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.

According to another embodiment, the vinyl polymer may comprise a vinyl aromatic polymer, in particular polystyrene.

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.

According to yet another embodiment, the functional group may be a siloxane.

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.

According to yet another embodiment, the shell of the polymer sphere may further have a hydrophilic functional group introduced.

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.

According to yet another embodiment, the shell of the first polymer sphere may further have a sugar-containing functional group introduced.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

According to another embodiment, the vinyl monomer may be a vinyl aromatic monomer. The vinyl aromatic monomer can be substituted or unsubstituted styrene.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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).

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.

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.

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.

According to yet another specific embodiment, the reaction modifier may be ammonium hydroxide.

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.

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).

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.

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.

According to yet another specific embodiment, the reaction modifier may be ammonium hydroxide.

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.

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.

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.

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.

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 .

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.

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.

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.

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.

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.

The composition of an embodiment of the present invention contains macroemulsified particles to provide a soft and silky feel in use.

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.

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.

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.

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.

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

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.

MeOH: 甲醇(共溶劑) KPS: 過硫酸鉀(Potassium persulfate )(起始劑) SVBS: 乙烯基苯磺酸鈉(Sodium vinyl benzene sulfonate )(穩定劑) PS: 聚苯乙烯 (聚合物珠粒) CS: 經披覆之具核-殼結構之第一聚合物球形體 DB: 兩親性異向性粉末 [ Preparation Examples 1-4] Preparation Examples 1-4 were obtained according to the compositions of Table 1 below. The preparation method will be described below. The ingredients used to prepare Examples 1-4 are as follows. [Table 1]

MeOH: methanol (co-solvent) KPS: Potassium persulfate (starter) SVBS: Sodium vinyl benzene sulfonate (stabilizer) PS: polystyrene (polymer beads) CS: Coated first polymer spheres with core-shell structure DB: Amphiphilic anisotropic powder

TMSPA: Trimethoxysilyl propylacrylate (functional group)

AIBN: Azobisisobutyronitrile (polymerization initiator)

Preparation Example 1. Preparation of Polystyrene (PS) First Polymer Spheroids

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.

Preparation Example 2. Preparation of Coated First Polymer Spheroids with Core-Shell (CS) Structure

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.

Preparation Example 3. Preparation of Amphiphilic Anisotropic Powder (DB)

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.

Preparation Example 4. Preparation of Hydrophilized Amphiphilic Anisotropic Powder

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.

[ 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 .

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.

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

[Table 2]

[ Test Example 1] Evaluation of physical properties The viscosity of each of the compositions of Examples 1 and 2 and Comparative Example 1 was measured at 30°C using a viscosity agent (LVDV-II+PRO, BROOKFIELD, USA). In addition, the average particle diameter of the emulsified particles in each composition was confirmed by electron microscopic images. The results are then shown in Table 3 below, along with the feel of application to the skin. The electron microscopic image is shown in FIG. 2 . [table 3]

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.

[ Test Example 2] Evaluation of feeling in use Thirty women in their twenties to forties were given a panel to use the cosmetic compositions obtained in Comparative Example 1 and Example 1. The panels were then asked to rate the oily texture, watery feel, spread and cooling effect upon application to the skin, and freshness and matte feel after application, based on a 10 scale (Scale 1: Very Low to Grade 10: extremely high). The average results are shown in Table 4 below. [Table 4]

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.

[ 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.

The sun protection factor (SPF) by selecting system 12 comprises six men and six women subjects of determining, and a sun simulator (81293 (Xenon UV Lamp 1 kW , unfiltered) light at 20-100 mj / cm ² The right and left backs of each subject except the spine were irradiated with UV light at a controlled dose controlled by using an IL1733 radiometer and a SED 240 probe. The determination was then determined 24 hours after UV irradiation redness minimum dose (MED). to determine the blocking effect of UV sample, Example 1 and Comparative Example 1 each in a thickness of ² μL / cm 2 is uniformly applied to the back of the subject and left for 15 minutes drying The UV irradiation was performed when the UV irradiation window was attached and fixed to the sample application site of Example 1 and Comparative Example 1, and the parts outside the irradiation window were shielded from UV rays with leather and towel. Then, the UV irradiation was performed After 24 hours, the minimum redness dose was confirmed and the sun protection factor (SPF) was calculated according to the following Mathematical formula 1. The results are shown in Table 5 below. [Mathematical formula 1] Sun protection factor (SPF) = minimum redness dose at the application site ( MED)/Minimum Redness Dose at non-application site (MED) [Table 5]

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.

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.

Claims (19)

An emulsified cosmetic composition comprising an inorganic UV blocking agent and an amphiphilic anisotropic powder, wherein the inorganic UV blocking agent is an inorganic powder, and the amphiphilic anisotropic powder comprises a first hydrophilic polymer A spherical body and a second hydrophobic polymer sphere, the first polymer sphere and the second polymer sphere are bonded to each other in a structure, wherein the second polymer sphere of which the structure is a part is partially Infiltrating the first polymer sphere to form a core of the first polymer sphere, and the first polymer sphere has a core-shell structure, and the shell has a functional group, the functional group is Siloxane; wherein the amphiphilic anisotropic powder does not contain a cross-linking agent; wherein the composition has a viscosity of 10000-60000cps. The composition of claim 1, wherein the inorganic powder is present in an amount of 0.1-60 wt% based on the total weight of the composition. The composition of claim 1, wherein the inorganic powder comprises at least one selected from the group consisting of titanium dioxide (TiO ₂ ), zinc oxide (ZnO), iron oxide (Fe ₂ O ₃ ), zirconia (ZrO ₂ ), _{silicon dioxide (SiO 2} ), manganese oxide (MnO), aluminum oxide (Al ₂ O ₃ ), cerium oxide (CeO ₃ ), mica, silica, talc and kaolin. The composition of claim 1, wherein the inorganic powder has an average particle size of 5-2000 nm. The composition of claim 1, comprising the amphiphilic anisotropic powder in an amount of 0.1-20 wt % based on the total weight of the composition. The composition according to claim 1, which is a water-in-oil composition. The composition of claim 6, wherein the inorganic powder is dispersed in an oil phase. The composition according to claim 6, wherein the inorganic powder is surface hydrophobized. The composition of claim 1, further comprising an organic UV blocking agent. The composition of claim 9, wherein the organic UV blocking agent is at least one selected from the group consisting of triazine, triazinone, cinnamate, salicylate, octenonitrile , benzophenone, phenyl benzimidazole sulfonic acid, dicamphor sulfonic acid, butyl methoxy dibenzyl methane and cresole trozole trisiloxane. The composition of claim 1, wherein the cores of the second polymer spheres and the first polymer spheres comprise vinyl polymers, and the shells of the first polymer spheres comprise a vinyl monomer Copolymer with a functional group-containing monomer. The composition of claim 11, wherein the vinyl polymer is a vinyl aromatic polymer. The composition of claim 11, wherein the vinyl monomer is a vinyl aromatic monomer. The composition according to claim 11, wherein the functional group-containing monomer is a (meth)acrylate containing siloxane. The composition of claim 1, wherein the amphiphilic anisotropic powder has a symmetrical shape, an asymmetric snowman shape, or an asymmetric inverted snowman shape based on the binding portion, wherein the first polymer spherical body and the second polymer spheres are bonded to each other. The composition of claim 1, wherein the amphiphilic anisotropic powder has a particle size of 100-2500 nm. The composition of claim 1, wherein the amphiphilic anisotropic powder forms macroemulsion particles having an average particle size of 2-200 μm. The composition of claim 1, wherein the shell of the first polymer sphere includes an additionally introduced hydrophilic functional group. The composition of claim 18, wherein the hydrophilic functional group is at least one selected from the group consisting of: carboxylic acid group, phosphonium group, phosphonic acid group, amine group, alkoxy group, ester group, acetate group, polyethylene glycol group and hydroxyl group.

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