Powder for cosmetic composition comprising calcium titanium composite oxide

Abstract

To provide a material which is to be blended into a cosmetic composition having UV-B blocking ability, while having high transparency without taking on a blue tinge.SOLUTION: The present invention provides a powder which is to be blended into a cosmetic composition and is composed of a calcium titanium composite oxide, having an average particle diameter of 25 nm to 110 nm. It is preferable that the powder is blended into a cosmetic composition in such an amount that the content of calcium titanium composite oxide in the cosmetic composition is 300 g / kg or less.SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to a calcium titanium composite oxide used for the purpose of being incorporated into a cosmetic composition.

Background Art

[0002] In makeup, sunburn is a serious problem. Sunburn refers to symptoms such as pigmentation and inflammation that occur in the skin of humans exposed to ultraviolet rays, which significantly impairs the appearance. Especially in summer when the amount of ultraviolet rays is high, it is no exaggeration to say that the effectiveness of sunburn prevention holds the key to the impression. According to the Japan Cosmetic Industry Association, among the lights generally called ultraviolet rays, the light with a wavelength of 280 nm to 320 nm, which causes red inflammation on the skin and is the cause of freckles and liver spots, significantly impairing the appearance, is called UV-B.

[0003] In order to protect the skin from UV-B, conventionally, ultraviolet ray protectants composed of titanium oxide and zinc oxide have been used. In Japanese Patent Laid-Open No. 62-228006 (Patent Document 1), a cosmetic having an ultraviolet ray protection effect is obtained by using zinc oxide having an average particle size of 70 to 300 μm in combination with fine particle titanium oxide having an average particle size of 30 to 70 μm. However, zinc oxide and titanium oxide are white and have a large hiding power, and may give an unnatural impression such that the applied part, especially the face, appears white and floating. This phenomenon is called the "whitening phenomenon" and is a major problem for users. Although Patent Document 1 also mentions the adverse effects of an increase in hiding power, it cannot be said that this problem has been sufficiently considered. As an effective means for preventing the whitening phenomenon, it is possible to reduce the particle size of the ultraviolet ray protectant to improve transparency. In Example 2 of Japanese Patent Laid-Open No. 2001-262119 (Patent Document 2), a compound in which Al is dissolved in ZnO having an average secondary particle size of 0.66 μm is obtained, and it is described that this compound is excellent in both transparency and ultraviolet ray absorbability.

[0004] On the one hand, when using a cosmetic containing an ultraviolet light protector with a small particle size, even though no blue pigment is formulated, the cosmetic composition may faintly exhibit a blue color tone. Although there has been discussion about this phenomenon, it is presumed to occur because of a phenomenon called Rayleigh scattering, in which powders preferentially scatter light with a short wavelength in natural light. Rayleigh scattering is explained, for example, in Non-Patent Document 1. When the area where the cosmetic composition is applied faintly exhibits a blue color tone, it gives an impression that the user's health condition is not excellent compared to the surroundings, significantly impairing the original purpose of using the cosmetic. In Japanese Patent Laid-Open No. 8-48614 (Patent Document 3), by formulating 0.1 to 20 parts by weight of yellow titanium oxide in a makeup cosmetic containing 0.5 to 20 parts by weight of rod-shaped powder, the blue color tone caused by the rod-shaped powder is canceled out. However, this method requires the formulation of rod-shaped powder and yellow titanium oxide, and as the types of powders to be added increase, the phenomenon that the color of the cosmetic composition becomes uneven due to poor dispersion of the powders is likely to occur.

[0005] In addition, regarding titanium(IV) oxide containing rutile-type titanium oxide, it is considered that the possibility of health hazards cannot be denied, and regarding zinc oxide, it is considered that it has a great impact on aquatic organisms. Centered around Europe, there is a growing movement to reduce the usage amount or use alternative materials. Japanese Patent Publication No. 2018-514509 (Patent Document 4) describes a UV protection composition containing barium titanate, and it is suggested from FIG. 1A that barium titanate can be an alternative to titanium dioxide TiO2 as an ultraviolet absorber.

[0006] Patent Document 4 states that a sunscreen composition is generally preferably transparent, and although it is described that the colored compositions obtained in some embodiments are substantially transparent, it is also described that they may be faintly colored. The specific color of the composition is not mentioned, and no method for eliminating the blue color tone is mentioned at all. In addition, since barium titanate is designated as a poison in Japan, it is not suitable for formulation in a cosmetic composition.

Prior Art Documents

Patent Document

[0007]

Patent Document 1

Patent Document 2

Patent Document 3

Patent Document 4

Non-Patent Document

[0008]

Non-Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0009] There is a need for a material that can replace titanium oxide and zinc oxide with a substance other than barium titanate and does not exhibit a blue color tone.

[0010] An object of the present invention is to provide a material that has the ability to block UV - B, has high transparency when incorporated into a cosmetic composition, is less likely to cause a whitening phenomenon, and does not exhibit a blue color tone.

Means for Solving the Problems

[0011] As a result of intensive studies on the above - mentioned materials, the inventors have found that a powder composed of a calcium - titanium composite oxide with an average particle diameter of 25 nm or more and 110 nm or less has the ability to block UV - B, and when this is incorporated into a cosmetic composition, no whitening phenomenon occurs and it does not exhibit a blue color tone.

[0012] The present invention includes, but is not limited to, the following. [1] A powder for use in a cosmetic composition, which is composed of calcium titanate composite oxide particles having an average particle diameter of 25 nm or more and 110 nm or less. [2] The powder according to [1], wherein the roundness of the particles is 0.80 or more. [3] The powder according to [1] or [2], which has a coating layer of an inorganic substance and / or an organic substance on at least a part of the surface of the particles. [4] A dispersion containing the powder according to any one of [1] to [3] and a dispersion medium. [5] A cosmetic composition containing the powder according to any one of [1] to [3] or the dispersion according to [4]. [6] A cosmetic composition containing the powder according to any one of [1] to [3] or the dispersion according to [4] in an amount such that the amount of calcium titanate composite oxide is 300 g / kg or less.

Advantages of the Invention

[0013] The cosmetic composition containing the powder obtained in the present invention is excellent in the ability to block UV-B, and thus can be suitably used as a cosmetic composition for blocking UV-B.

[0014] Further, the cosmetic composition containing the powder obtained in the present invention has high transparency, so that when applied to the skin, no whitening phenomenon occurs, and a natural impression can be given to the user.

[0015] Furthermore, the cosmetic composition containing the powder obtained in the present invention does not exhibit a blue color tone. The blue color tone generally refers to blue or a color tone close thereto in the commonly used name of JIS. Although there are large individual differences depending on the physical characteristics of the user and the senses of the observer, generally, if there are parts on the user's face that exhibit these color tones, it will give an impression that the health condition is not excellent, significantly impairing the purpose of use as a cosmetic. Since the cosmetic composition of the present invention does not exhibit a blue color tone, it can give a healthy impression to the user.

Embodiments for Carrying Out the Invention

[0016] The "powder made of calcium titanium composite oxide" obtained in the present invention means that most of the particles constituting the powder are calcium titanium composite oxide particles, or that the proportion of calcium titanium composite oxide in the composition of each particle is large. It is most preferable that all particles of the powder of the present invention are made of pure calcium titanium composite oxide that does not contain any impurities, but in addition to calcium titanium composite oxide, the powder may contain unreacted materials during the synthesis reaction of calcium titanium composite oxide, unavoidable impurities derived from raw materials, and inorganic and / or organic substances derived from the coating layer. Specifically, if 600 g / kg or more, preferably 650 g / kg or more, and more preferably 700 g / kg or more of the entire powder is made of calcium titanium composite oxide, it can be considered as a powder made of calcium titanium composite oxide that realizes the effects of the present invention.

[0017] The powder to be blended in the cosmetic composition of the present invention has an average particle size of 110 nm or less, more preferably 100 nm or less, even more preferably 95 nm or less, and even more preferably 93 nm or less. If the average particle size is 110 nm or less, the white cast phenomenon does not occur and the powder does not exhibit a blue color. In addition, the average particle size is 25 nm or more, more preferably 30 nm or more, and even more preferably 35 nm or more. If the average particle size is 25 nm or more, the probability of occurrence of aggregation that becomes a problem when blended in a cosmetic composition and used is sufficiently small. The average particle size is evaluated by the method described below. In addition, when the average particle size is referred to in the present invention, it refers to a value rounded off to one decimal place.

[0018] The powder of the present invention has the effect of preventing the occurrence of a white cast phenomenon and preventing a blue color when blended in a cosmetic composition. Although the mechanism by which such an effect is obtained has not been clarified, the present inventors speculate that the small average particle size of the particles constituting the powder of the present invention and the moderate refractive index of the calcium titanium composite oxide create an optical synergistic effect, which suppresses both the white cast phenomenon and the blue color when the powder is used in a cosmetic composition.

[0019] The powder incorporated into the cosmetic composition of the present invention is not particularly limited with respect to the particle size distribution of the constituent particles. However, in the present invention, it is preferable that the particle size distribution of the individual particles constituting the powder is narrow, and it is most preferable that the histogram plotting the number of particles against the particle size has a single peak. As a rough guide, it is preferable that the standard deviation of the particle sizes of about 300 particles measured by the method described later is less than 15.0 nm.

[0020] The powder incorporated into the cosmetic composition of the present invention preferably has a roundness of 0.80 or more for the particles constituting the powder. More preferably, it is 0.81 or more. If the roundness is 0.80 or more, a smooth feel can be achieved. There is no particular upper limit for the roundness of the particles. Theoretically, the maximum is 1.00. The roundness is evaluated by the method described later.

[0021] The powder incorporated into the cosmetic composition of the present invention is not particularly limited with respect to the variation in roundness and shape. However, it is desirable that the proportion of particles having the same roundness and / or the same shape is large. Specifically, it is preferable that the standard deviation of the roundness of about 200 particles measured by the method described later is less than 0.07.

[0022] In order to impart hydrophobicity, optical properties, etc. to the powder incorporated into the cosmetic composition of the present invention, it is desirable that a coating layer is present on at least a part of the surface of the particles constituting the powder. The coating layer may be a coating layer made of an organic substance or a coating layer made of an inorganic substance. Two or more coating layers may be present, or both an organic layer and an inorganic layer may be present. Details of the coating layer will be described later.

[0023] The powder obtained in the present invention usually does not contain titanium oxide or has a low content thereof. The cosmetic composition using the powder obtained in the present invention can be used as a cosmetic that does not contain titanium oxide or has a low content of titanium oxide. Specifically, the titanium oxide content of the powder is preferably 200 g / kg or less, more preferably 100 g / kg or less. As a method for evaluating the content, it can be obtained by comparing the peak intensity derived from titanium oxide and the peak intensity derived from calcium titanium composite oxide obtained by X-ray diffraction measurement with a calibration curve. The calibration curve is prepared by measuring and plotting at least three points of a mixture of calcium titanium composite oxide and titanium oxide with a known mixing ratio.

[0024] The powder to be incorporated into the cosmetic composition of the present invention is preferably dispersed in a dispersion medium and used as a dispersion. The dispersion can be used in cosmetic compositions such as sunscreen agents and sunscreens.

[0025] The powder obtained in the present invention is preferably incorporated into a cosmetic composition. The dosage form of the cosmetic composition is not particularly limited, but typically, it is preferably incorporated into skin cosmetics including sunscreen agents.

[0026] When incorporating the powder or dispersion obtained in the present invention into a cosmetic composition, these amounts are preferably incorporated in such an amount that the amount of calcium titanium composite oxide in the cosmetic composition is 300 g / kg or less, preferably 270 g / kg or less. If the above amount is 300 g / kg or less, the cosmetic composition will have a smooth feel and can maintain higher transparency. The lower limit of the amount is not particularly limited. Generally, if the above amount is 45 g / kg or more, a sufficient ultraviolet ray protection effect can be imparted to the cosmetic without separately adding an ultraviolet ray protection agent. More preferably, it is 50 g / kg or more. When used in combination with other ultraviolet ray protection agents, or when incorporated into a cosmetic composition that does not require an ultraviolet ray protection effect, the amount may be smaller. The lower limit of the amount is merely a guide and is 10 g / kg, more preferably 20 g / kg.

[0027] (Manufacturing method) The manufacturing method of the powder to be blended in the cosmetic composition of the present invention is not particularly limited. Typically, it can be obtained by mixing a titanium source typified by metatitanic acid and a calcium source typified by calcium hydroxide, heating them, and removing excess calcium.

[0028] When manufacturing the powder composed of calcium titanate composite oxide particles to be blended in the cosmetic composition of the present invention, one or more sugars selected from monosaccharides such as glucose and fructose and disaccharides such as maltose may be added to the raw materials. When adding the sugars as described above, the total addition amount thereof is preferably 0.500 mol or less relative to titanium. If the addition amount of the sugar is 0.500 mol or less, the sugar and titanium oxide are less likely to remain. Generally, when the addition amount of the sugar is large, the particles tend to be small. However, when blended in the cosmetic composition, it is preferable that the particles are not too small. From this point as well, the concentration of the sugar to be added is preferably 0.500 mol or less in total relative to titanium. The lower limit is not particularly limited, but it is preferably 0.030 mol or more relative to titanium, and more preferably 0.031 mol or more. In addition, when calcium does not dissolve in water, the addition of sugar is unnecessary.

[0029] The powder to be blended in the cosmetic composition of the present invention can be manufactured by reacting it under high temperature and high pressure using an autoclave.

[0030] Also, the powder to be blended in the cosmetic composition of the present invention can also be manufactured by mixing a titanium source and a calcium source and firing them at a high temperature.

[0031] The powder incorporated into the cosmetic composition of the present invention may be synthesized using methods other than the above. For example, referring to the method described in JP-A-2020-075846, in which a metal compound and an alcohol are added to a titanium peroxo complex dispersion and heat-treated, the powder incorporated into the cosmetic composition of the present invention may be produced. Further, referring to the method described in JP-A-2008-303131, in which calcium ions, titanium ions, and other ions are subjected to a hydrothermal reaction in water in a supercritical or subcritical state, the powder incorporated into the cosmetic composition of the present invention may be produced.

[0032] (Surface coating treatment) For the powder incorporated into the cosmetic composition of the present invention, for example, in order to impart dispersion stability and optical properties in a dispersion medium, at least a part of the surface of the particles constituting the powder may be provided with a coating layer of an inorganic substance such as a hydrous oxide or oxide of a metal such as aluminum, silicon, zinc, titanium, zirconium, iron, cerium, and tin. Metal salts other than the above may be used as the inorganic coating. Further, in order to perform surface modification typified by hydrophobic treatment on at least a part of the surface of the particles, a coating layer of an organic substance may be provided. Examples of the organic coating include silicone compounds such as dimethylpolysiloxane, hydrogen dimethicone, and polysiloxane, coupling agents such as silane-based, aluminum-based, titanium-based, and zirconium-based coupling agents, fluorine compounds such as perfluoroalkyl phosphate compounds, hydrocarbons, lecithin, amino acids, polyethylene, wax, and metal soaps. These treatments may be combined in a plurality, and there is no particular limitation on the order of the treatments at that time. The method of surface treatment is not particularly limited, and a commonly used method may be used. For example, after mixing the material of the coating layer and the powder, the coating layer can be formed using a method such as heat treatment.

[0033] (Dispersion) The powder to be incorporated into the cosmetic composition of the present invention is preferably used in the form of a dispersion dispersed in a dispersion medium. The type of the dispersion medium is not particularly limited, and it may be an aqueous dispersion medium or an oil-based dispersion medium. Specific examples include, as the aqueous dispersion medium, water, ethanol, isobutyl alcohol, propanediol, phenoxyethanol, polyvinyl alcohol, etc., and as the oil-based dispersion medium, aroma oil, olive oil, glycerin, squalane, candelilla wax, 1,3-butylene glycol, pentylene glycol, toluene, petrolatum, castor oil, lanolin, beeswax, isododecane, paraffin, silicone, etc. The method of dispersion is not particularly limited. Specifically, depending on the amount and viscosity of the dispersion medium, devices such as a homogenizer, a homomixer, and a bead mill can be used. Depending on the type and amount of the dispersion medium, it is desirable to perform a surface coating treatment before dispersion.

[0034] (Cosmetic composition) The powder obtained in the present invention can be incorporated into a cosmetic composition and used. In particular, it is preferably incorporated into a skin cosmetic and used as a sunscreen by taking advantage of its ability to block UV-B. In addition, it can be used in a wide range of applications such as foundation, skin care products, makeup bases, and sun oils.

[0035] The cosmetic composition containing the powder obtained in the present invention is excellent in the ability to block UV-B, and thus can be suitably used as a cosmetic composition that blocks UV-B. The smaller the integrated transmittance value in the UV-B region, the greater the ability to block UV-B. In particular, if the integrated transmittance value in the UV-B region is less than 800%·nm, it can be determined that the ability to block UV-B is sufficiently large. In the present invention, the range of 280 nm or more and 320 nm or less is defined as the UV-B region.

[0036] In addition, the cosmetic composition containing the powder obtained in the present invention has high transparency, so that when applied to the skin, no whitening phenomenon occurs, and a natural impression can be given to the user. The higher the integrated transmittance value of light in the region recognizable by humans (hereinafter referred to as the "visible region") is, the higher the transparency is. In particular, if the integrated transmittance value in the visible region is greater than 35000%·nm, it can be determined that the transparency is sufficiently high. In the present invention, the visible region is defined as 380 nm or more and 800 nm or less.

[0037] Furthermore, the cosmetic composition containing the powder obtained in the present invention does not exhibit a blue hue. The greater the integrated transmittance value of light in the region showing purple and blue (hereinafter referred to as the "blue region") is, the smaller the scattered light intensity with a bluish tint becomes, and as a result, it becomes less likely to exhibit a blue hue. In particular, if the integrated transmittance value in the blue region is greater than 9000%·nm, it can be determined that it does not exhibit a blue hue. Furthermore, it is more preferable if the value obtained by dividing the integrated transmittance value in the blue region by the integrated transmittance value in the visible region is greater than 0.250. In the present invention, the blue region is defined as 380 nm or more and 500 nm or less.

[0038] The blue hue generally refers to blue in the JIS common name or a color similar thereto. Although the differences due to the physical characteristics of the user and the feelings of the observer are large, generally, if there are parts on the user's face that exhibit these hues, it gives an impression that the health condition is not excellent, significantly impairing the purpose of use as a cosmetic. Since the cosmetic composition of the present invention does not exhibit a blue hue, it can give a healthy impression to the user.

[0039] The cosmetic composition using the powder obtained in the present invention can have its color adjusted by adding other powders (pigments) within a quantitative and qualitative range that does not impair the effects of the present invention. Inorganic pigments that can usually be used in combination include titanium oxide, zinc oxide, red iron oxide, yellow iron oxide, black iron oxide, ultramarine, dark blue, cerium oxide, talc, muscovite, synthetic mica, phlogopite, biotite, synthetic fluorophlogopite, mica titanium, iron oxide in mica form, sericite, zeolite, kaolin, bentonite, clay, silicic acid, anhydrous silicic acid, magnesium silicate, magnesium aluminum silicate, calcium silicate, barium sulfate, magnesium sulfate, calcium sulfate, calcium carbonate, magnesium carbonate, boron nitride, bismuth oxychloride, alumina, zirconium oxide, magnesium oxide, chromium oxide, calamine, hydroxyapatite, and composites thereof. Organic pigments that can also be used in combination include silicone powder, silicone elastic powder, polyurethane powder, cellulose powder, nylon powder, urethane powder, silk powder, PMMA powder, starch, polyethylene powder, polystyrene powder, carbon black, tar pigment, natural pigment, metal soaps such as zinc stearate, and composites thereof.

[0040] In the cosmetic composition using the powder obtained in the present invention, in order to impart the ability to block UV-A or UV-C, or to further enhance the ability to block UV-B, a UV protectant may be separately added within a quantitative and qualitative range that does not impair the effects of the present invention. The added UV protectant may be an organic UV protectant or an inorganic UV protectant. Note that the cosmetic composition using the powder obtained in the present invention has the ability to block UV-B, which is required for general sunscreen agents and sunburn preventives, even without separately adding a UV protectant. Therefore, the cosmetic composition of the present invention may not contain a UV protectant other than the powder of the present invention.

[0041] The cosmetic composition using the powder obtained in the present invention can contain other components other than the above components within a quantitative and qualitative range that does not impair the effects of the present invention according to the purpose. For example, oily components, pigments, pH adjusters, moisturizers, thickeners, surfactants, dispersants, stabilizers, colorants, preservatives, antioxidants, sequestering agents, astringents, anti-inflammatory agents, fragrances, etc. can also be appropriately blended within the range of achieving the object of the present invention. In particular, blending a plate-like compound typified by mica results in good slipperiness, which is desirable.

[0042] Examples of the dosage forms of cosmetics containing the powder obtained in the present invention are given below.

[0043] The cosmetic composition using the powder obtained in the present invention can be used as a liquid cosmetic. The dosage form may be in any state such as an aqueous dispersion, an oily dispersion, or lotion-like, and can be, for example, a sunscreen, sun oil, makeup base, skin care cosmetic, hair care cosmetic, etc.

[0044] The cosmetic composition using the powder obtained in the present invention can also be used after being made into a liquid cosmetic and sprayed. The shape of the cosmetic when sprayed may be in any state such as foamy or misty. For example, it can be a spray-type sunscreen, makeup base, skin care cosmetic, hair care cosmetic, etc.

[0045] The cosmetic composition using the powder obtained in the present invention can also be used as a gel-like cosmetic. The dosage form may be in any state such as cream-like, emulsion-like, oily liquid-like, paste-like, etc., and can be, for example, a sunscreen, makeup base, makeup cosmetics such as lip cream, hair care cosmetics, etc. It can also be used in cosmetic compositions for washing the body, such as shampoo, conditioner, body shampoo, facial wash foam, peel-off pack, toothpaste, etc.

[0046] The cosmetic composition using the powder obtained in the present invention can also be used as a solid cosmetic. The dosage form may be in any state such as powdery, powder-solid, paste-like, oily-solid, etc. For example, it can be used as makeup cosmetics such as sunscreen agents, makeup bases, foundations, loose powders, concealers, face powders, body powders, perfume powders, baby powders, etc., skin care cosmetics, hair care cosmetics, etc.

[0047] Regardless of the dosage form used, the series of characteristics of the powder obtained in the present invention, which blocks UV-B, has high transparency, and does not exhibit a bluish color, are useful in many dosage forms of cosmetics.

[0048] The cosmetic composition containing the powder obtained in the present invention can be suitably used regardless of the gender of the user. In addition, since calcium titanium composite oxide, which is the main component of the powder obtained in the present invention, has not been reported to cause health hazards, it can be suitably used regardless of the age of the user.

[0049] The cosmetic composition using the powder obtained in the present invention can also be suitably used for animals other than humans. A typical use is sunscreen for pet dogs. In such applications, since there are cases where animals lick and ingest it, the fact that the powder is composed of calcium titanium composite oxide, which has not been reported to cause health hazards, is also useful when formulating for animals other than humans.

[0050] Taking advantage of its ability to block UV-B and high transparency, the powder obtained in the present invention can also be used for applications other than cosmetics. Typical applications include adding it to recently popular plastic visors to help with UV protection, and using it in house paints to mitigate the deterioration of the outer wall caused by ultraviolet rays. In recent years, due to the increasing health awareness, the number of users avoiding products containing titanium oxide in various fields has been increasing, but products using the powder obtained in the present invention can meet the needs of such users.

[0051] Before describing the embodiments, the test methods used in the present invention will be described.

[0052] [Particle size, average particle size] It was measured using a transmission electron microscope JEM-1400plus manufactured by JEOL Ltd. The observation magnification was 50,000 times (observation magnification of the transmission electron microscope 10,000 times × printing 5 times). The diameters of about 300 particles in the observation field of view were evaluated using image analysis software ImageJ and taken as the particle size. The average value of the particle sizes of about 300 particles was taken as the average particle size in the present invention.

[0053] [Circularity] The circularity was evaluated by the circularity when the particles were projected two-dimensionally and was obtained by (circumference of a circle equal to the particle area) / (particle circumference). The average value of the circularities of about 200 particles constituting the powder was taken as the circularity in the present invention.

[0054] [Specific surface area] The specific surface area was measured by the BET single-point method using Gemini VII 2390 manufactured by MICROMERITICS INSTRUMENT CO.

[0055] [Transmittance integral value] First, a dispersion containing the powder of the present invention was prepared by the following procedure. 40.0 g of the powder (not surface-coated) and 4.8 g of methylhydrogenpolysiloxane KF-9901 manufactured by Shin-Etsu Chemical Co., Ltd. were added to an automatic mortar ALG-200WD manufactured by Nippon Tokushu Toryo Co., Ltd., mixed at a pestle rotation speed of 100 rpm for 60 minutes, and heat-treated at 110°C for 3 hours to obtain a surface-treated powder.

[0056] To the Easy Nano RMB type manufactured by Aimax Co., Ltd., 20.0 g of surface-treated powder, 5.0 g of polyglyceryl-3 polydimethylsiloxyethyl dimethicone (KF-6106 manufactured by Shin-Etsu Chemical Co., Ltd.), 25.0 g of decamethylcyclopentasiloxane (KF-995 manufactured by Shin-Etsu Chemical Co., Ltd.), and 200.0 g of φ0.5 mm beads (zirconia ball YTZ (registered trademark)-0.5 manufactured by Nikkato Corporation) were added, dispersed at a disk peripheral speed of 12 m / s for 120 minutes, the beads were filtered off, and a dispersion was obtained.

[0057] Based on the obtained dispersion, a sample for spectroscopic evaluation was prepared. 3.75 g of the dispersion and 5.25 g of decamethylcyclopentasiloxane (KF-995 manufactured by Shin-Etsu Chemical Co., Ltd.) were stirred at 5000 rpm for 2 minutes using a Lab Revolution (registered trademark) manufactured by Primix Corporation equipped with a 25 mm dispersing sawtooth-type turbine. Then, while slowly adding 6.00 g of pure water, it was stirred at 5000 rpm for 5 minutes to prepare a W / O emulsion type sunscreen as a simple cosmetic. The obtained sunscreen was applied to a 60 mm × 60 mm × 3 mm quartz plate using a No. 3 bar coater and dried by exposing it to warm air of 1200 W using a household hair dryer, and this was used as a sample for spectroscopic evaluation.

[0058] The obtained sample for spectroscopic evaluation was measured for transmittance from a wavelength of 250 nm to 800 nm using a spectrophotometer V-670 manufactured by JASCO Corporation, with a data acquisition interval of 2 nm, a UV / Vis band width of 2.0 nm, a scanning speed of 1000 nm / min, a light source of D2 / WI, and a double-beam method. From the measurement results, the transmittance in the region from 380 nm to 800 nm was integrated, and the obtained integrated value was defined as the transmittance integrated value in the visible region. It can be judged that the higher the transmittance integrated value in the visible region, the higher the transparency. Similarly, the transmittance integrated values were obtained for the regions from 380 nm to 500 nm and from 280 nm to 320 nm, and were defined as the transmittance integrated value in the blue region and the transmittance integrated value in the UV-B region, respectively. In addition, by using the cosmetic composition as the above sunscreen, various transmittance integrated values of the cosmetic composition itself can also be obtained.

Example

[0059] Hereinafter, the present invention will be specifically described by way of examples. However, the following examples are merely illustrative and do not limit the scope of the invention in any way.

[0060] In addition, in the stirring operations described in the examples and comparative examples, considering the properties related to the behavior of the liquid during stirring, such as the liquid volume, liquid viscosity, and container shape, the rotation speed is appropriately adjusted so that the entire liquid is uniformly mixed and droplets do not splash around. Also, when the same effect can be obtained using products from any company as long as they are common commercially available products such as sodium hydroxide, the company names of the manufacturers and sellers are omitted.

[0061] [Example 1] After subjecting metatitanic acid obtained by the sulfuric acid method to iron removal and bleaching treatment, an aqueous sodium hydroxide solution was added to adjust the pH to 9.0, desulfurization treatment was performed, and then it was neutralized to pH 5.8 with hydrochloric acid, followed by filtration and washing with water to obtain a washed cake of metatitanic acid with an SO3 content of 9.3 g / kg. Water was added to the washed cake to form a slurry with a Ti concentration of 2.13 mol / L, and then hydrochloric acid was added to adjust the pH to 1.4 for peptization treatment. 0.764 mol of metatitanic acid, which is the peptized product, was taken and put into a reaction vessel as TiO2. Calcium hydroxide was added thereto so that the Ca / Ti molar ratio was 1.15, and further 30.05 g of glucose was added. Then, 0.90 mol of sodium hydroxide was added, and water was added to make the total volume 0.6 L, and the mixed solution was stirred for 30 minutes.

[0062] While further stirring and mixing the above mixed solution, it was heated to 150 °C using an autoclave, held with stirring for 10.0 hours, then cooled to 50 °C, hydrochloric acid was added until the pH reached 5.5, and stirring was continued for another 1 hour. The obtained precipitate was washed by decantation, separated by filtration, and dried in the air at 120 °C for 10 hours to obtain a powder composed of calcium titanate composite oxide particles. The average particle diameter of the particles constituting the obtained powder was 31 nm, the circularity was 0.820, and the specific surface area was 116.4 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and the integrated transmittance value was evaluated. As a result, the integrated transmittance value in the visible region was 35913%·nm, the integrated transmittance value in the blue region was 9448%·nm, and the integrated transmittance value in the UV-B region was 622%·nm.

[0063] [Example 2] The amount of metatitanic acid collected was changed to 0.675 mol as TiO2, the amount of glucose added was changed to 8.02 g, the sodium hydroxide added after glucose addition was changed to 1.08 mol, and the holding time at 150 °C was changed to 6.0 hours. Except for these changes, a powder composed of calcium titanium composite oxide particles was obtained in the same manner as in Example 1. The average particle diameter of the particles constituting the obtained powder was 62 nm, the circularity was 0.824, and the specific surface area was 74.2 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and the integrated transmittance value was evaluated. As a result, the integrated transmittance value in the visible region was 35682%·nm, the integrated transmittance value in the blue region was 9422%·nm, and the integrated transmittance value in the UV-B region was 601%·nm.

[0064] [Example 3] The amount of metatitanic acid collected was changed to 0.675 mol as TiO2, the amount of glucose added was changed to 4.01 g, and the sodium hydroxide added after glucose addition was changed to 1.08 mol. Except for these changes, a powder composed of calcium titanium composite oxide particles was obtained in the same manner as in Example 1. The average particle diameter of the particles constituting the obtained powder was 93 nm, the circularity was 0.814, and the specific surface area was 60.3 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and the integrated transmittance value was evaluated. As a result, the integrated transmittance value in the visible region was 35340%·nm, the integrated transmittance value in the blue region was 9113%·nm, and the integrated transmittance value in the UV-B region was 251%·nm.

[0065] [Example 4] Metatitanic acid was calcined in air at 500 °C for 40 minutes. 0.021 mol of the obtained calcined product of metatitanic acid was taken as TiO2, and 6.32 g of calcium carbonate and the calcined product of metatitanic acid were pulverized and mixed for 4 hours using an Ishikawa-type stirring and crushing machine AG-A type manufactured by Ishikawa Factory Co., Ltd. The pulverized and mixed raw materials were calcined at 850 °C for 40 minutes.

[0066] The calcined product was washed in a solution obtained by adding hydrochloric acid to pure water, and further washed with pure water, and then dried in air at 120 °C to obtain a powder composed of calcium titanate composite oxide particles. The average particle diameter of the particles constituting the obtained powder was 37 nm, the circularity was 0.870, and the specific surface area was 42.9 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and when the transmittance integral value was evaluated, the transmittance integral value in the visible region was 36220%·nm, the transmittance integral value in the blue region was 9579%·nm, and the transmittance integral value in the UV-B region was 374%·nm.

[0067] [Comparative Example 1] A powder composed of calcium titanate composite oxide particles was obtained in the same manner as in Example 1, except that the amount of metatitanic acid taken as TiO2 was changed to 0.675 mol, the amount of glucose added was changed to 3.51 g, and the sodium hydroxide added after adding glucose was changed to 1.08 mol. The average particle diameter of the particles constituting the obtained powder was 131 nm, the circularity was 0.837, and the specific surface area was 44.0 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and when the transmittance integral value was evaluated, the transmittance integral value in the visible region was 33006%·nm, the transmittance integral value in the blue region was 7942%·nm, and the transmittance integral value in the UV-B region was 217%·nm.

[0068] [Comparative Example 2] The amount of metatitanic acid taken was changed to 0.675 mol as TiO2, the amount of glucose added was changed to 2.76 g, and the sodium hydroxide added after glucose addition was changed to 1.08 mol. A powder composed of calcium titanate composite oxide particles was obtained in the same manner as in Example 1, except that the heating operation was carried out in the atmosphere at 95 °C for a holding time of 18.0 hours. The average particle diameter of the particles constituting the obtained powder was 212 nm, the circularity was 0.826, and the specific surface area was 34.9 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and when the transmittance integral value was evaluated, the transmittance integral value in the visible region was 32618%·nm, the transmittance integral value in the blue region was 7671%·nm, and the transmittance integral value in the UV-B region was 293%·nm.

[0069] [Comparative Example 3] The amount of metatitanic acid taken was changed to 0.675 mol as TiO2, glucose was not added, and the sodium hydroxide added in the subsequent step was changed to 1.08 mol. A powder composed of calcium titanate composite oxide particles was obtained in the same manner as in Example 1, except that the heating operation was carried out in the atmosphere at 95 °C for a holding time of 18.0 hours. The average particle diameter of the particles constituting the obtained powder was 311 nm, the circularity was 0.697, and the specific surface area was 16.8 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and when the transmittance integral value was evaluated, the transmittance integral value in the visible region was 24013%·nm, the transmittance integral value in the blue region was 4205%·nm, and the transmittance integral value in the UV-B region was 493%·nm.

[0070] [Comparative Example 4] A powder of ultrafine titanium oxide ST-450EC for cosmetics manufactured by Titanium Industry Co., Ltd. was used. The particle diameter of this powder was 38 nm, the circularity was 0.470, and the specific surface area was 51.3 m 2 / g. Using this, a sample for spectroscopic evaluation was prepared, and when the transmittance integral value was evaluated, the transmittance integral value in the visible region was 35191%·nm, the transmittance integral value in the blue region was 8723%·nm, and the transmittance integral value in the UV-B region was 3%·nm.

[0071] [Reference Example 1] A commercially available water-in-oil (W / O) type sunscreen agent was applied to a quartz plate and dried to obtain a sample for spectroscopic evaluation. When the integrated transmittance value was evaluated, the integrated transmittance value in the visible region was 32396%·nm, the integrated transmittance value in the blue region was 8243%·nm, and the integrated transmittance value in the UV-B region was 953%·nm.

[0072] [Table 1]

[0073] [Table 2]

[0074] Table 1 shows the production conditions of the examples and comparative examples.

[0075] Table 2 shows the powder characteristics and integrated transmittance values of the examples, comparative examples, and reference examples.

[0076] From Table 2, it can be seen that for a cosmetic composition containing calcium titanate composite oxide particles with an average particle diameter of 25 nm or more and 110 nm or less, the integrated transmittance value in the UV-B region is less than 800%·nm, the integrated transmittance value in the visible region is greater than 35000%·nm, the integrated transmittance value in the blue region is greater than 9000%·nm, and the value obtained by dividing the integrated transmittance value in the blue region by the integrated transmittance value in the visible region is greater than 0.250. Comparative Examples 1 to 3 with a particle diameter greater than 110 nm and Comparative Example 4 using titanium oxide instead of calcium titanate composite oxide do not satisfy the above conditions.

[0077] From the above evaluation results, it is considered that the powder of the present invention has the ability to block UV-B, and when incorporated into a cosmetic composition, it has high transparency and does not exhibit a blue color.

[0078] A sensory test was conducted on the transparency and blue color of the powder of the present invention when incorporated into a cosmetic composition.

[0079] (Sensory Evaluation of Cosmetic Composition) Using the powders of the examples and comparative examples, a W / O type sunscreen was prepared by the method described in the column of [transmittance integral value] above.

[0080] (White floating phenomenon) The obtained sunscreen and the sunscreen of Reference Example 1 were applied to the faces of 10 panelists, and the white floating phenomenon was scored according to the following criteria. The higher the score, the less the occurrence of the white floating phenomenon. (Evaluation criteria) 3 points: Even when viewed from a distance of 30 cm, there is no sense of incongruity compared to the uncoated area. 2 points: There is a sense of incongruity when viewed from a distance of 30 cm, but there is no sense of incongruity when viewed from a position 1 m away. 1 point: There is a sense of incongruity even when viewed from a position more than 1 m away.

[0081] (Bluish color) The obtained sunscreen and the sunscreen of Reference Example 1 were applied to the faces of 10 panelists, and the bluish color was scored according to the following criteria. The higher the score, the less the bluish color. (Evaluation criteria) 3 points: Even when viewed from a distance of 30 cm, there is no bluish color. 2 points: When viewed from a distance of 30 cm, a bluish-white impression is received, but it is not particularly noticeable when viewed from a position 1 m away. 1 point: Even when viewed from a position more than 1 m away, there is a bluish-white impression. (Judgment criteria for comprehensive evaluation) A: The sum of the scores for the white floating phenomenon and the scores for the bluish color is 6 points B: The sum of the scores for the white floating phenomenon and the scores for the bluish color is 4 points or more and less than 6 points C: The sum of the scores for the white floating phenomenon and the scores for the bluish color is less than 4 points

[0082]

Table 3

[0083] From the results of the sensory evaluation, it can be seen that a sunscreen agent using a powder composed of calcium titanate composite oxide particles with an average particle diameter of 25 nm or more and 110 nm or less is less likely to cause white blooming and does not exhibit a blue tint. Further, when compared with the existing titanium dioxide-based sunscreen agent of Comparative Example 4, it was not inferior in terms of the difficulty of occurrence of white blooming, and furthermore, it was less likely to exhibit a blue tint. Furthermore, when compared with the commercially available product of Reference Example 1, both the difficulty of occurrence of white blooming and the difficulty of exhibiting a blue tint were improved.

[0084] From the above evaluation results, it can be said that the powder composed of calcium titanate composite oxide to be blended in the cosmetic composition of the present invention is less likely to cause white blooming and does not exhibit a blue tint when blended in the cosmetic composition, as per the evaluation results of the transmittance integral value.

[0085] Skin cosmetics are a main aspect of the present invention. Formulation examples are shown below.

[0086] [Formulation Example 1] (Manufacture of powder foundation) The following Components 1 to 13 were mixed and uniformly pulverized (Step A), then Components 15 to 17 were uniformly mixed and added to the mixed pulverized product obtained in Step A to make it uniform (Step B). Further, Component 14 was added and press-molded in a mold to obtain a powder foundation (Step C).

[0087] When the obtained powder foundation was applied to the skin, no white blooming occurred and no blue tint was exhibited. Also, when the applied area was checked at a later date, sunburn was very slight. (Components) Blending ratio (g / kg) 1. Caprylyl silane-treated mica (Note 1) 400 2. Caprylyl silane-treated red iron oxide (Note 1) 50 3. Silicone-treated talc (Note 2) balance 4. Silicone-treated powder described in Example 2 (Note 2) 50 5. Silicone-treated fine particle titanium dioxide (Note 2) 50 6. Silicone-treated barium sulfate (Note 2) 100 7. Silicone-treated red iron oxide (Note 2) 4 8. Silicone-treated yellow iron oxide (Note 2) 20 9. Silicone-treated amber (Note 2) 4 10. Silicone-treated black iron oxide (Note 2) 1 11. Phenyl-modified hybrid silicone composite powder (Note 3) 20 12. Spherical polymethylsilsesquioxane powder (Note 4) 5 13. Preservative Appropriate amount 14. Fragrance Appropriate amount 15. Crosslinked dimethylpolysiloxane (Note 5) 40 16. Glyceryl trioctanoate 20 17. Squalane 10 (Note 1) The surface has been treated with AES-3083 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 2) The surface has been treated with KF-9909 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 3) KSP-300 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 4) KMP-590 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 5) KSG-16 manufactured by Shin-Etsu Chemical Co., Ltd.

[0088] [Formulation Example 2] (Manufacture of pressed powder) After mixing and pulverizing the following Components 1 to 7 (Step A), transfer this mixed and pulverized material to a mixer, add Components 8 to 12, and stir and mix uniformly (Step B). Pulverize with a sample mill and press-mold this into an aluminum dish to obtain a pressed powder (Step C).

[0089] When the obtained pressed powder was applied to the skin, no whitening phenomenon occurred, nor did it show a blue tint. Also, when the applied area was checked at a later date, sunburn was very slight. (Components) Mixing ratio (g / kg) 1. Talc Remainder 2. PMMA (Note 1) 100 3. Sericite 300 4. Scaly silica (Note 2) 30 5. Powder described in Example 1 60 6. Preservative Appropriate amount 7. Colorant Appropriate amount 8. Octyl methoxysilicate 30 9. Squalane 20 10. Preservative Appropriate amount 11. Antioxidant Appropriate amount 12. Fragrance Appropriate amount (Note 1) Matsumoto Microsphere M-100, 7 μm product manufactured by Matsumoto Yushi Seiyaku Co., Ltd. (Note 2) Sun Lovely (registered trademark) C manufactured by AGC Si-Tech Co., Ltd.

[0090] [Formulation Example 3] (Manufacture of loose powder) After mixing and pulverizing the following Components 1 to 7 (Step A), this mixed pulverized product was transferred to a mixer, and Components 8 to 10 were added and stirred and mixed to be uniform (Step B). Further, the mixture obtained in Step B was pulverized with a sample mill, and this was filled to obtain loose powder (Step C).

[0091] When the obtained loose powder was applied to the skin, no whitening phenomenon occurred, nor did it show a blue color tone. Also, when the applied area was checked at a later date, the sunburn was very slight. (Components) Mixing ratio (g / kg) 1. Talc Remainder 2. Powder described in Example 4 50 3. Amihope LL 30 4. PMMA (Note 1) 80 5. Preservative Appropriate amount 6. Colorant Appropriate amount 7. Squalane 10 8. Preservative Appropriate amount 9. Antioxidant Appropriate amount 10. Fragrance Appropriate amount (Note 1) Matsumoto Microsphere S-100, 10 μm product manufactured by Matsumoto Yushi Seiyaku Co., Ltd.

[0092] [Formulation Example 4] (Manufacture of Oil-based Foundation) Mix the following Components 1 to 6 in a mixer and grind them uniformly (Process A). Then, heat Components 7 to 16 to 85 °C to dissolve them, add the mixed and ground product obtained in Process A, and stir uniformly (Process B). After defoaming, pour the solid content into a tray and gradually cool it to room temperature to obtain an oil-based foundation (Process C).

[0093] When the obtained oil-based foundation was applied to the skin, no whitening phenomenon occurred, and it did not show a bluish color. Also, when the applied area was checked at a later date, the sunburn was very slight. (Components) Mixing Ratio (g / kg) 1. Silicone-treated Talc (Note 1) 53 2. Powder Described in Example 3 of Silicone Treatment (Note 1) 150 3. Silicone-treated Sericite (Note 1) 282 4. Silicone-treated Red Iron Oxide (Note 1) 5 5. Silicone-treated Yellow Iron Oxide (Note 1) 18 6. Silicone-treated Black Iron Oxide (Note 1) 2 7. Candelilla Wax 10 8. Carnauba Wax 10 9. Ceresine 15 10. Decamethylcyclopentasiloxane 140 11. Isononyl Isononanoate Remainder 12. Polyglyceryl Diisostearate 20 13. Dextrin Palmitate 10 14. Octyl Methoxysilicate 30 15. Preservative Appropriate Amount 16. Antioxidant Appropriate Amount (Note 1) The surface is treated with KF-96A-50cs manufactured by Shin-Etsu Chemical Co., Ltd.

[0094] [Formulation Example 5] (Manufacture of Stick Foundation) Components 12 to 16 were mixed in a mixer (Step A). Further, Components 1 to 11 were weighed into a container that could hold the entire amount, heated to 85°C, and dissolved (Step B). Additionally, Components 17 to 21 were weighed into another container and dissolved (Step C). Subsequently, the mixture obtained in Step A was added to the heat-dissolved product obtained in Step B, dispersed with a stirrer until visually uniform, and then the heat-dissolved product obtained in Step C was added to form an emulsion (Step D). After defoaming, the solid content was poured into a mold and slowly cooled to room temperature to obtain a stick foundation (Step E).

[0095] When the obtained stick foundation was applied to the skin, no whitening phenomenon occurred, nor did it exhibit a blue tint. Also, when the applied area was checked at a later date, sunburn was very slight. (Component) Mixing ratio (g / kg) 1. Dimethylpolysiloxane 180 2. Decamethylcyclopentasiloxane 300 3. Octyl methoxysilicate 50 4. Diisostearyl malate 40 5. Candelilla wax 60 6. Hydrogenated jojoba ester 40 7. Cetyl dimethicone copolyol 20 8. Sorbitan sesquisoisostearate 5 9. Antioxidant Appropriate amount 10. Preservative Appropriate amount 11. Fragrance Appropriate amount 12. Silicone-treated colorant (Note 1) 5 13. Powder described in Example 1 of silicone treatment (Note 1) 85 14. Silicone-treated talc (Note 1) 60 15. Silicone-treated mica (Note 1) 20 16. Methyl polymethacrylate 20 17. Purified water Remainder 18. Sodium citrate 3 19. 1,3-Butylene glycol 30 20. Glycerin 20 21. Preservative Appropriate amount (Note 1) The surface has been treated with KF-99P manufactured by Shin-Etsu Chemical Co., Ltd.

[0096] [Formulation Example 6] (Manufacture of W / O Emulsion Foundation) After stirring and mixing Components 12 to 14 in a mixer (Step A), Components 1 to 11 were added and dispersed using a stirrer until visually uniform (Step B). On the other hand, Components 15 to 19 were heated and dissolved in another container (Step C). Then, the heated and dissolved product obtained in Step C was added to the dispersion obtained in Step B, emulsified, and then cooled to room temperature to obtain a W / O emulsion foundation (Step D).

[0097] When the obtained W / O emulsion foundation was applied to the skin, no whitening phenomenon occurred, nor did it show a blue tint. Also, when the applied area was checked at a later date, sunburn was very slight. (Components) Blending Ratio (g / kg) 1. POE-modified silicone (Note 1) 8 2. Polyglyceryl polyricinoleate 5 3. Neopentyl glycol dicaprate 30 4. Squalane 10 5. Pentaerythrityl tetraoctanoate 20 6. Inulin stearate (Note 2) 10 7. Octyl methoxycinnamate 40 8. Decamethylcyclopentasiloxane 154 9. Preservative Appropriate amount 10. Antioxidant Appropriate amount 11. Fragrance Appropriate amount 12. Powder described in Silicone Treatment Example 4 (Note 3) 80 13. Silicone-treated talc (Note 3) 57 14. Silicone-treated colorant (Note 3) 10 15. Purified water Remainder 16. 1,3-Butylene glycol 60 17. Glycerin 10 18. Sodium chloride 10 19. Appropriate amount of preservative (Note 1) Product with HLB value of 4.5 (Note 2) Leopal (registered trademark) ISK manufactured by Chiba Flour Milling Co., Ltd. (Note 3) Surface-treated with KF-9901 manufactured by Shin-Etsu Chemical Co., Ltd.

[0098] [Formulation Example 7] (Manufacture of O / W emulsion type foundation) Components 1 to 7 below were heated and dissolved at 85°C (Step A). Also, components 8 to 10 were mixed and pulverized (Step B). Further, components 11 to 15 were heated to 85°C, dissolved and mixed (Step C). Then, the pulverized mixture obtained in Step B was added to the heated and dissolved product obtained in Step A, and dispersed using a stirrer until visually uniform. The dissolved mixture obtained in Step C was gradually added thereto for emulsification, and the mixture was stirred and cooled to room temperature. Next, it was filled into an appropriate container to obtain an O / W emulsion type foundation (Step D).

[0099] When the obtained O / W emulsion type foundation was applied to the skin, no whitening phenomenon occurred, nor did it show a bluish tint. Also, when the applied area was checked at a later date, sunburn was very slight. (Components) Mixing ratio (g / kg) 1. Stearic acid 4 2. Isostearic acid 3 3. Cetyl 2-ethylhexanoate 40 4. Liquid paraffin 110 5. Polyoxyethylene (10) stearyl ether 20 6. Cetyl alcohol 3 7. Preservative 2 8. Talc 150 9. Colorant 40 10. Powder described in Example 2 50 11. Triethanolamine 4 12. Propylene glycol 50 13. Purified water 521 14. Preservative 2 15. Antioxidant 1

[0100] [Formulation Example 8] (Manufacture of W / O Liquid Foundation) After uniformly mixing Components 8 to 12 (Step A), a part of Component 4 and Component 13 were mixed and added to the mixture obtained in Step A, and dispersed using a stirrer until visually uniform. (Step B). Also, Components 1 to 3, the remainder of Component 4, and Components 5 to 7 were mixed and dispersed using a stirrer until visually uniform (Step C). Further, Components 14 to 18 and Component 20 were mixed and dispersed using a stirrer until visually uniform (Step D). While stirring the dispersion obtained in Step C, the mixture obtained in Step D was gradually added and emulsified, and further the dispersion obtained in Step B and Component 19 were added to obtain a W / O liquid foundation. (Step E).

[0101] When the obtained W / O liquid foundation was applied to the skin, no whitening phenomenon occurred, nor did it exhibit a blue tint. Also, when the applied area was checked at a later date, the sunburn was very slight. (Components) Blending Ratio (g / kg) 1. Crosslinked polyether-modified silicone (Note 1) 30 2. Crosslinked dimethylpolysiloxane (Note 2) 50 3. Branched polyether-modified silicone (Note 3) 20 4. Decamethylcyclopentasiloxane 211 5. Cetyl isooctanoate 50 6. Dimethylpolysiloxane (Note 4) 65 7. Dimethyldistearylammonium hectorite 12 8. Powder described in Silicone Treatment Example 3 (Note 5) 50 9. Silicone-treated pigment-grade titanium oxide (Note 5) 50 10. Silicone-treated red iron oxide (Note 5) 4 11. Silicone-treated yellow iron oxide (Note 5) 10 12. Silicone-treated black iron oxide (Note 5) 1 13. Acrylic silicone resin dissolved product (Note 6) 20 14. 1,3-Butylene glycol 50 15. Xanthan gum (Note 7) 50 16. Sodium citrate 2 17. Sodium chloride 5 18. Preservative Appropriate amount 19. Flavor Appropriate amount 20. Purified water The remainder (Note 1) KSG-210 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 2) KSG-15 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 3) KF-6028P manufactured by Shin-Etsu Chemical Co., Ltd. (Note 4) 6 mm 2 / second (25 °C) product (Note 5) The surface has been treated with KF-9909 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 6) KP-575 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 7) 20 g / kg aqueous solution

[0102] [Formulation Example 9] (Manufacture of 2WAY cake foundation) Mix Components 1 to 7 with a Henschel mixer (Step A). After mixing Components 8 to 11, which have been heated and dissolved, thereto (Step B), pulverize with an atomizer and press-mold in an aluminum dish to obtain the target 2WAY foundation (Step C).

[0103] When the obtained 2WAY foundation was applied to the skin, no whitening phenomenon occurred and no blue color was exhibited. Also, when the applied area was checked at a later date, sunburn was very slight. (Components) Blending ratio (g / kg) 1. Dimethicone-treated talc The remainder 2. Powder described in Dimethicone-treated Example 1 100 3. Dimethicone-treated mica 200 4. Dimethicone-treated sericite 360 5. Nylon powder 100 6. Dimethicone-treated red iron oxide 29 7. Dimethicone 1000 cs 60 8. Isotridecyl isononanoate 30 9. Squalane 30 10. Tocopherol 1 11. 1,3-Butylene Glycol 10

[0104] [Formulation Example 10] (Manufacture of Oil Cake Foundation) Components 1 to 5 were mixed in a Henschel mixer and uniformly pulverized (Step A). Components 6 to 12 were heated and dissolved, the powder part was added, and it was uniformly stirred (Step B). After defoaming, the bulk was poured into a tray and gradually cooled to room temperature to obtain the target oil cake foundation (Step C).

[0105] When the obtained oil cake foundation was applied to the skin, no whitening phenomenon occurred, nor did it show a bluish color. Also, when the applied area was checked at a later date, the sunburn was very slight. (Components) Blending Ratio (g / kg) 1. Dimethicone-Treated Talc Remainder 2. Pigment Described in Example 4 of Dimethicone Treatment 130 3. Dimethicone-Treated Sericite 280 4. Dimethicone-Treated Red Iron Oxide 27 5. Dimethicone-Treated Black Iron Oxide 1 6. Candelilla Wax 10 7. Carnauba Wax 10 8. Ceresin 15 9. Cyclopentasiloxane 140 10. Isononyl Isononanoate 250 11. Polyglyceryl Diisostearate 20 12. Ethylhexyl Methoxycinnamate 30 [Formulation Example 11] (Manufacture of Sun Cut Cream) Component 7 was added to a part of Component 5 below to make it uniform, and Components 8 and 9 were added and dispersed using a bead mill (Step A). Further, Components 1 to 4, the remainder of Component 5, and Component 6 were uniformly mixed (Step B). Furthermore, Components 10 to 12 and Component 14 were dispersed using a stirrer until visually uniform (Step C). Subsequently, the dispersion obtained in Step C was added to the mixture obtained in Step B and emulsified, and the dispersion obtained in Step A and Component 13 were added to obtain a sun cut cream (Step D).

[0106] When the obtained sun cut cream was applied to the skin, no whitening phenomenon occurred, nor did it exhibit a blue tint. And when the applied area was checked at a later date, the sunburn was very slight. (Component) Blending ratio (g / kg) 1. Crosslinked polyether-modified silicone (Note 1) 30 2. Crosslinked dimethylpolysiloxane (Note 2) 20 3. Alkyl-modified branched polyether-modified silicone (Note 3) 10 4. Neopentyl glycol dioctanoate 50 5. Decamethylcyclopentasiloxane 175 6. Octyl methoxysilicate 60 7. Acrylic silicone resin dissolved product (Note 4) 100 8. Caprylyl silane-treated fine particle zinc oxide (Note 5) 200 9. Powder described in Example 1 with caprylyl silane treatment (Note 5) 30 10. 1,3-Butylene glycol 20 11. Sodium citrate 2 12. Sodium chloride 5 13. Perfume Appropriate amount 14. Purified water Remainder (Note 1) KSG-240 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 2) KSG-15 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 3) KF-6038 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 4) KP-575 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 5) The surface has been treated with AES-3083 manufactured by Shin-Etsu Chemical Co., Ltd.

[0107] [Formulation Example 12] (Manufacture of W / O Emulsion Sunscreen Agent) After uniformly mixing Components 1 to 5, Component 6 was uniformly dispersed (Step A). Next, Components 7 to 11 were uniformly mixed (Step B). While stirring, the mixture obtained in Step B was added to the dispersion obtained in Step A and emulsified to obtain a W / O emulsion sunscreen agent (Step C).

[0108] When the obtained W / O emulsion sunscreen agent was applied to the skin, no whitening phenomenon occurred, nor did it show a blue tint. And when the applied area was checked at a later date, the sunburn was very slight. (Components) Mixing Ratio (g / kg) 1. Crosslinked Polyether-Modified Silicone (Note 1) 20 2. Crosslinked Dimethylpolysiloxane (Note 2) 30 3. Decamethylcyclopentasiloxane 135 4. Dimethylpolysiloxane (6 mm 2 / sec (25 °C)) 70 5. Powder Described in Silicone Treatment Example 3 (Note 3) 250 6. Silicone-Treated Talc 40 7. 1,3-Butylene Glycol 50 8. Sodium Citrate 4 9. Sodium Chloride 5 10. Preservative Appropriate Amount 11. Purified Water Remainder (Note 1) KSG-210 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 2) KSG-15 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 3) The surface has been treated with KF-9909 manufactured by Shin-Etsu Chemical Co., Ltd.

[0109] [Formulation Example 13] (Manufacture of O / W Emulsion Sunscreen Agent) Components 1 to 9 were uniformly mixed (Step A). Subsequently, components 10 to 15 were uniformly mixed (Step B). While stirring, the mixture obtained in Step B was added to the mixture obtained in Step A and emulsified to obtain an O / W emulsion sunscreen (Step C).

[0110] When the obtained O / W emulsion sunscreen was applied to the skin, no whitening phenomenon occurred, nor did it exhibit a blue tint. And when the applied area was checked at a later date, the sunburn was very slight. (Component) Mixing ratio (g / kg) 1. Lauryl betaine 1 2. Isostearic acid 2 3. Diethylhexyl succinate 145 4. Cyclomethicone 20 5. Dimethicone 20 6. 2-Ethylhexyl 2-ethylhexanoate 20 7. Behenyl alcohol 1 8. Batyl alcohol 1 9. Polyoxybutylene polyoxypropylene glycol 20 10. Ethanol 80 11. Triethanolamine 3 12. EDTA-3Na 1 13. Phenoxyethanol 3 14. Powder described in Example 1 80 15. Purified water The remainder

[0111] [Formulation Example 14] (Manufacture of W / O cream sunscreen) Components 1 to 7 were uniformly mixed (Step A). Subsequently, components 8 to 13 and component 15 were uniformly mixed (Step B). While stirring, the mixture obtained in Step B was added to the mixture obtained in Step A and emulsified, and component 14 was added to obtain a W / O cream sunscreen (Step C).

[0112] The obtained W / O cream sunscreen did not show a whitening phenomenon or a blue tint when applied to the skin. It was also confirmed that it had no cracking feeling, had a slight spreading property, excellent adhesiveness and good retention, and was very excellent in usability and stability. In addition, when the applied area was checked at a later date, sunburn was very slight. (Ingredient) Blending ratio (g / kg) 1. Crosslinked alkyl-polyether modified silicone (Note 1) 30 2. Crosslinked alkyl modified dimethylpolysiloxane (Note 2) 40 3. Alkyl modified branched polyether modified silicone (Note 3) 10 4. Meadowfoam oil 35 5. Macadamia nut oil 50 6. Jojoba oil 100 7. Hybrid silicone composite powder (Note 4) 30 8. Powder described in Example 4 50 9. 1,3-Butylene glycol 80 10. Glycine 30 11. Sodium citrate 2 12. Sodium chloride 5 13. Preservative Appropriate amount 14. Fragrance Appropriate amount 15. Purified water Remainder (Note 1) KSG-340 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 2) KSG-44 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 3) KF-6038 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 4) KSP-100 manufactured by Shin-Etsu Chemical Co., Ltd.

[0113] [Formulation Example 15] (Manufacture of O / W cream sunscreen) Ingredients 1 to 7 were heated and mixed to make them uniform (Step A). Next, Ingredients 8 to 13 and Ingredient 15 were uniformly mixed (Step B). While stirring, the mixture obtained in Step A was added to the mixture obtained in Step B for emulsification, and Ingredient 14 was added to obtain an O / W cream sunscreen (Step C).

[0114] When the obtained O / W cream sunscreen was applied to the skin, no whitening phenomenon occurred, nor did it show a blue tint. It was non-greasy and oily, smooth, had a slight spreadability, excellent adhesion, good fit, good makeup retention, little change with temperature and over time, and was confirmed to be very excellent in usability and stability. In addition, when the applied area was checked later, sunburn was very slight. (Ingredients) Blending ratio (g / kg) 1. Crosslinked dimethylpolysiloxane (Note 1) 50 2. Glyceryl triisostearate 80 3. Cetyl alcohol 5 4. Stearic acid 10 5. Glyceryl monostearate 5 6. Sorbitan sesquioleate 5 7. Powder treated with coupling agent described in Example 4 of Preparation Example (Note 2) 50 8. Polyoxyethylene sorbitan monooleate 10 9. Triethanolamine 5 10. Carbomer (10 g / kg aqueous solution) 200 11. Locust bean gum (20 g / kg aqueous solution) 50 12. 1,3-Butylene glycol 70 13. Preservative Appropriate amount 14. Fragrance Appropriate amount 15. Purified water Remainder (Note 1) KSG-15 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 2) The surface has been treated with OFS-6341 manufactured by Dow Chemical Japan Co., Ltd.

[0115] [Formulation Example 16] (Manufacture of O / W gel sunscreen) Components 1 to 4 were uniformly mixed (Step A). Then, after uniformly mixing Components 6 and 7, Component 5 was added and uniformly mixed (Step B). While stirring, the mixture obtained in Step A was added to the mixture obtained in Step B and emulsified to obtain an O / W gel sunscreen (Step C).

[0116] When the obtained O / W gel sunscreen was applied to the skin, no whitening phenomenon occurred, nor did it show a blue tint. Moreover, it was non-greasy and smooth, had a slight spreading property, excellent adhesion, good fit, and was confirmed to be very excellent in usability and stability. In addition, when the applied area was checked at a later date, the sunburn was very slight. (Ingredients) Blending ratio (g / kg) 1. Polyhydroxystearic acid 3 2. Ethylhexyl methoxycinnamate 47 3. Liquid paraffin 295 4. Powder described in Example 1 50 5. Sodium acrylate / sodium acryloyldimethyltaurate copolymer / isohexadecane / polysorbate 80 (Note 1) 5 6. 1,3-Butylene glycol 60 7. Purified water Remainder (Note 1) SIMULGEL EG QD manufactured by Seppic S.A.

[0117] [Formulation Example 17] (Manufacture of stick-type sunscreen) Components 1 to 4 were heated to 85°C to 90°C and uniformly mixed (Step A). Components 5 and 6 were dissolved in Component 7 to make it uniform (Step B). Components 8 to 10 were uniformly mixed (Step C). While stirring, the mixture obtained in Step B was added to the mixture obtained in Step A and uniformly mixed, then cooled to 70°C to 80°C, and further, the mixture obtained in Step C was added and uniformly mixed. Then, Components 11 to 15 were added, filled into an appropriate container, and cooled to obtain a stick-type sunscreen (Step C).

[0118] When the obtained stick-type sunscreen was applied to the skin, no whitening phenomenon occurred, nor did it show a blue tint. Moreover, it had no creaking feeling, excellent adhesion, and good fit. In addition, when the applied area was checked at a later date, the sunburn was very slight. (Ingredients) Mixing ratio (g / kg) 1. Paraffin wax 280 2. Cetyl alcohol 5 3. White wax 30 4. Carnauba wax 10 5. Methylparaben 1 6. Propylparaben 1 7. Isopropyl myristate 10 8. Oxybenzone 35 9. Octinoxate 75 10. Avobenzone 30 11. Fragrance 10 12. White petrolatum 433 13. Lanolin 10 14. Isopyl lanolate 20 15. Powder described in Example 2 50

[0119] [Formulation Example 18] (Manufacture of spray-type sunscreen) Components 1 to 7 were mixed and dissolved at 80 °C to make them uniform (Step A). Components 8 to 10 and Component 13 were mixed and dissolved at 80 °C to make them uniform (Step B). The mixture obtained in Step B was added to the mixture obtained in Step A and emulsified. After cooling to 30 °C, Components 11 and 12 were stirred and mixed. The resulting emulsion for spray was filled into a pump-type spray container to obtain a spray-type sunscreen (Step C).

[0120] When the obtained spray-type sunscreen was applied to the skin, no whitening phenomenon occurred, nor did it show a blue tint. And it was possible to make a nice spray, with little oiliness and a refreshing feeling. In addition, when the applied area was checked at a later date, sunburn was very slight. (Ingredients) Mixing ratio (g / kg) 1. Ethylhexyl methoxycinnamate (Note 1) 65 2. t-Butyl methoxydibenzoylmethane (Note 2) 6 3. Decamethylcyclopentasiloxane (Note 3) 50 4. Powder described in Example 1 of silicone treatment (Note 4) 70 5. Caprylyl methicone (Note 5) 10 6. Sorbitan stearate (Note 6) 10 7. Polysorbate 60 2 8. PEG-11 methyl ether dimethicone 7 9. Acrylic acid / alkyl methacrylate copolymer (Note 7) 1 10. 1,3-Butylene glycol 30 11. Ethanol 100 12. Potassium hydroxide appropriate amount 13. Purified water remainder (Note 1) NOMUCOAT (registered trademark) TAB manufactured by Nisshin Oillio Group, Ltd. (Note 2) Parsol (registered trademark) 1789 manufactured by DSM Nutritional Products Japan Ltd. (Note 3) KF-995 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 4) Surface-treated with KF-9909 manufactured by Shin-Etsu Chemical Co., Ltd. (Note 5) SS-3408 manufactured by Dow Corning Toray Co., Ltd. (Note 6) EMALEX (registered trademark) SPE-100S manufactured by Nippon Emulsion Co., Ltd. (Note 7) PEMULEN (registered trademark) TR-1 manufactured by Lubrizol Japan Ltd.

[0121] [Formulation Example 19] (Manufacture of tanning oil) To Component 1, Components 2 to 7 were sequentially added while stirring at room temperature, and stirred until uniform to obtain tanning oil.

[0122] When the obtained tanning oil was applied to the skin, no whitening phenomenon occurred, and it did not show a blue tint. Also, there was no roughness. When the applied area was intentionally exposed to sunlight and confirmed later, it had a uniform wheat-colored skin. (Components) Blending ratio (g / kg) 1. Ethylhexyl methoxycinnamate 100 2. Isopropyl myristate 100 3. Palm oil 50 4. Natural Vitamin E 1 5. Powder described in Example 1 of silicone treatment (Note 1) 70 6. Perfume Appropriate amount 7. Liquid paraffin The remainder (Note 1) The surface has been treated with KF-9909 manufactured by Shin-Etsu Chemical Co., Ltd.

[0123] The powder of the present invention can be used in addition to skin cosmetic compositions.

[0124] [Formulation Example 20] (Manufacture of body shampoo) Components 1 to 3 were heated to 70°C to 80°C and dissolved (Step A). Next, component 4 was gradually added and saponification was carried out (Step B). When the saponification was completed, the remaining components 5 to 9 were added and stirred until uniform (Step C). It was cooled to 40°C, and components 10 to 12 that had been mixed and pulverized were added thereto, and it was cooled to room temperature while stirring and mixing to obtain the target body shampoo (Step D).

[0125] The obtained body shampoo foamed well and had a smooth texture. (Components) Blending ratio (g / kg) 1. Lauric acid 115 2. Myristic acid 77 3. Palmitic acid 48 4. Potassium hydroxide (purity 480 g / kg) 122 5. Lauryl hydroxysulfobetaine 100 6. Cocamidomonoethanolamide 10 7. Ethylene glycol distearate 20 8. Purified water The remainder 9. EDTA-4Na 1 10. Powder described in Example 4 20 11. Colorant 6 12. Talc 10

[0126] [Formulation Example 21] (Manufacture of facial wash foam) Components 1 to 3 were heated from 70°C to 80°C and dissolved (Step A). Subsequently, Component 4 was gradually added and saponification was carried out (Step B). When the saponification was completed, the remaining Components 5 to 13 were added and stirred until uniform (Step C). It was cooled to 40°C, and Components 14 to 16, which had been mixed and pulverized, were added thereto, and it was cooled to room temperature while stirring and mixing to obtain the target facial wash foam (Step D).

[0127] The obtained facial wash foam foamed well and had a smooth texture. (Component) Mixing ratio (g / kg) 1. Stearic acid 170 2. Myristic acid 70 3. Lauric acid 30 4. Potassium hydroxide (purity 480 g / kg) 120 5. Glyceryl diisostearate PEG-60 30 6. Glyceryl stearate 20 7. Sorbitol 80 8. PEG1500 100 9. Cocamidopropyl betaine 50 10. Glycerin 180 11. EDTA-4Na 1 12. Purified water Remainder 13. Pentylene glycol 15 14. Powder described in Example 1 20 15. Colorant 3 16. Talc 10

[0128] [Formulation Example 22] [Manufacture of Facial Wash Powder] Components 1 to 13 were uniformly mixed with a Henschel mixer to obtain the target facial wash powder.

[0129] The obtained facial wash powder foamed well and had a smooth texture. (Component) Mixing ratio (g / kg) 1. Iron(III) oxide 3 2. Powder described in Example 4 20 3. Talc 200 4. Lauric acid 50 5. Mannitol remainder 6. Potassium myristate 300 7. Glucose 100 8. Potassium myristoyl glutamate 20 9. Sodium cocoamido methyl taurate 30 10. Betaine 10 11. Tanakukurei (registered trademark) 50 12. Guar hydroxypropyltrimonium chloride 5 13. Pentylene glycol 10

[0130] [Formulation Example 23] (Manufacture of film composition) A film composition containing the calcium titanate composite oxide of the present invention was prepared. A part of Component 3 was added to Component 1 and dispersed with a bead mill (Step A). Component 2 and the remainder of Component 3 were mixed and heated, and stirred at 95 °C for 10 minutes (Step B). The dispersion obtained in Step A was added, stirred for 5 minutes, then heating was terminated, and it was poured into a mold (Step C) and dried to obtain a film composition (Step D).

[0131] The obtained film composition had no whiteness or blue tint and was transparent. By industrially applying this formulation example, it is considered possible to obtain a transparent film-like structure having the ability to block UV-B. (Components) Mixing ratio (g / kg) 1. Powder described in Example 1 100 2. Polyvinyl alcohol (Note 1) 100 3. Purified water 800 (Note 1) Polyvinyl alcohol 500 manufactured by Kishida Chemical Co., Ltd.

[0132] [Formulation Example 24] (Manufacture of paint) A paint containing the powder of the present invention was prepared. Components 1 to 4 were mixed with a mixer for 30 to 120 minutes (Step A), and then dispersed with a bead mill to obtain a paint (Step B).

[0133] When the obtained paint was applied on a transparent glass substrate and exposed to light, it was transparent without any whiteness or blue tint. By industrially applying this formulation example, it is considered that a paint having the ability to block UV-B can be obtained. (Component) Mixing ratio (g / kg) 1. Acrylic resin 300 2. Methylhydrogenpolysiloxane surface-treated powder described in Example 4 300 3. Toluene 200 4. Isophorone 200

Claims

1. Powder for use in a cosmetic composition, comprising calcium titanate composite oxide particles having an average particle diameter of 25 nm or more and 110 nm or less.

2. The powder according to Claim 1, wherein the roundness of the particles is 0.80 or more.

3. The powder according to Claim 1 or 2, having a coating layer of an inorganic substance and / or an organic substance on at least a part of the surface of the particles.

4. A dispersion containing the powder according to any one of Claims 1 to 3 and a dispersion medium.

5. A cosmetic composition containing the powder according to any one of Claims 1 to 3 or the dispersion according to Claim 4.

6. A cosmetic composition containing the powder according to any one of Claims 1 to 3 or the dispersion according to Claim 4 in an amount such that the amount of the calcium titanate composite oxide is 300 g / kg or less.

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