Powder containing titanium oxide particles as main component, method for producing the same, and cosmetic composition containing the same
By producing titanium dioxide particles with controlled nano-content and specific morphological characteristics, the issues of environmental impact, regulation compliance, and aesthetic concerns in cosmetics are addressed, achieving effective UV protection and improved cosmetic properties.
Patent Information
- Application Number
- JP2024037158
- Authority / Receiving Office
- JP · JP
- Patent Type
- Applications
- Current Assignee / Owner
- Filing Date
- 2024-03-11
- Publication Date
- 2025-09-25
AI Technical Summary
Cosmetics containing high amounts of UV scattering agents like titanium dioxide face issues such as environmental concerns, percutaneous absorption, and aesthetic problems like a rough skin feel and white cast, while nano-order substances are subject to regulations and consumer avoidance, limiting design freedom.
Controlled production of titanium dioxide particles with a specific aspect ratio, minor axis length, and standard deviation to minimize nano-order content, using a method involving hydrochloric acid concentration, addition time, and temperature to produce titanium(IV) oxide particles with a morphology of rod-shaped particles aggregated into fibers.
The resulting powder provides effective UV protection, complies with nano-order substance regulations, and offers a natural finish and improved spreadability in cosmetics, enhancing design freedom.
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Figure 2025138207000001_ABST
Abstract
Description
[Technical Field]
[0001] The present invention relates to a powder containing titanium(IV) oxide particles as a main component and a method for producing the same, and also to a cosmetic composition containing the powder. [Background technology]
[0002] Conventionally, sun care cosmetics contain active ingredients such as ultraviolet absorbers that convert ultraviolet rays into other energy sources and ultraviolet scattering agents that reflect or scatter ultraviolet rays. Titanium oxide is used as an ultraviolet scattering agent.
[0003] One of the development goals for suncare cosmetics has been to obtain cosmetics with strong UV protection. While UV protection can be enhanced by incorporating a large amount of UV absorbers or UV scattering agents, cosmetics containing large amounts of UV absorbers tend to be avoided due to concerns about environmental impact and percutaneous absorption, and the amount of UV absorber that can be incorporated may be restricted in some countries or regions where the cosmetics are sold. On the other hand, incorporating large amounts of UV scattering agents, such as fine particle titanium dioxide or zinc oxide, in cosmetics can cause various problems, such as a rough feeling on the skin, reduced design freedom, and an unnatural finish due to an excessively strong white color, known as a white cast.
[0004] One form of titanium oxide with excellent UV protection properties is particles with an average diameter of about 10 to 80 nm (Non-Patent Document 1), or particles with one side of that size. In JP 2010-173863 A (Patent Document 1), the present applicant proposed cocoon-shaped rutile-type titanium oxide in which the major axis faces of rod-shaped particles are oriented and aggregated in the minor axis direction to form spherical or ellipsoidal shapes, the oriented and aggregated particles having an apparent average major axis length of 80 to 300 nm, an apparent average minor axis length of 30 to 150 nm, and an apparent average axial ratio of the oriented and aggregated particles (apparent average major axis length / apparent average minor axis length) of 1.1 to 4, and also proposed a cosmetic composition containing these aggregated particles. [Prior art documents] [Patent documents]
[0005] [Patent Document 1] Japanese Patent Application Laid-Open No. 2010-173863 [Non-patent literature]
[0006] [Non-Patent Document 1] Manabu Kiyono, Titanium Oxide Research Group, "Titanium Oxide - Properties and Application Technology - 2nd Edition", Gihodo Publishing, January 2017, pp. 267-271 Summary of the Invention [Problem to be solved by the invention]
[0007] In recent years, growing health consciousness in Europe has led to some opposition to the addition of nano-order substances to cosmetics. Despite the publication of experimental results by Christopher SJ Campbell et al. showing that nano-order particles are not absorbed by healthy skin when applied to the skin (Christopher SJ Campbell et al., Journal of Controlled Release, Volume 162, Issue 1, 20 August 2012, pages 201-207), consumer concerns remain, and European regulatory authorities have already imposed restrictions on the amount and processing method of nano-order substances. Some titanium dioxide powders used as UV scattering agents to date are nano-order or contain high amounts of nano-order particles. These powders are subject to nano-order substance regulations, making them difficult to freely incorporate. Furthermore, nano-order substances are sometimes avoided simply because they are nano-order substances. It would be desirable to develop UV scattering agents that can be sold as non-nanomaterials by strictly controlling the nano-order particle content in titanium dioxide powder. Cosmetics using such ultraviolet scattering agents also have the advantage of allowing greater freedom in design.
[0008] An object of the present invention is to provide a powder containing titanium oxide particles as a main component with a controlled content of nanoparticles, and a cosmetic composition containing this powder. [Means for solving the problem]
[0009] In order to solve the above problems, the present inventors have studied in more detail the conditions for producing the cocoon-shaped rutile-type titanium dioxide of Patent Document 1, and as a result, have found that by controlling the hydrochloric acid concentration, the hydrochloric acid addition time, and the liquid temperature, it is possible to produce titanium dioxide having an aspect ratio of 1.50 or more and 2.00 or less, and a minor axis length D 50 The value is 105 nm or more and less than 150 nm, and the average minor axis length b ave (nm) and standard deviation σ of minor axis length b (nm) is (b ave -100) / σ b It has been found that a powder containing titanium(IV) oxide particles as a main component can be obtained, satisfying a ratio of 1.3 or more. It has also been found that by using this powder in a cosmetic composition, it is possible to realize a cosmetic composition with a controlled nanoparticle content. The present invention includes, but is not limited to, the following.
[0010] [Aspect 1] The aspect ratio is 1.50 or more and 2.00 or less, and the minor axis length D 50 The value is 105 nm or more and less than 150 nm, and the average minor axis length b ave (nm) and standard deviation σ of minor axis length b (nm) is of the following formula: (b ave -100) / σ b ≧1.3 A powder whose main component is titanium(IV) oxide particles that meets the above requirements. [Aspect 2] Average minor axis length of particles b ave (nm) and standard deviation σ of minor axis length b (nm) further has the following formula: (150-b ave ) / σ b ≧1.3 2. The powder of claim 1, wherein [Aspect 3] 3. The powder according to claim 1 or 2, wherein the particles have a morphology of rod-shaped particles aggregated into fibers. [Aspect 4] 4. The particle of embodiment 3, wherein a projection of the particle is approximately ellipsoidal. [Aspect 5] 5. The powder of any one of aspects 1 to 4, wherein the crystalline layer of the titanium(IV) oxide particles is in the rutile form. [Aspect 6] adding an aliphatic hydroxy acid compound to an acid-soluble titanium compound; Then, hydrochloric acid is added for X (h) to make the hydrochloric acid concentration Y (g / L); Dissolving acid-soluble titanium compounds at Z (℃) after adding hydrochloric acid wherein X, Y, and Z are of the following formulas (1) and (2): (1) 2.60≦Y / Z≦3.45 (2) Y 1 / 2 ×Z / X≦475 A method for producing a powder according to any one of aspects 1 to 5, wherein [Aspect 7] The method of claim 6, wherein X is 2.0 or greater. [Aspect 8] Aspect 8. The method of any one of aspects 6 to 7, wherein the acid-soluble titanium compound is sodium titanate. [Aspect 9] A cosmetic composition comprising the powder according to any one of aspects 1 to 5. [Effects of the Invention]
[0011] The powder of the present invention, which is primarily composed of titanium(IV) oxide particles, has a controlled nanoparticle content, and when incorporated into cosmetics, particularly suncare cosmetics, it can provide cosmetics that comply with regulations on nano-order substances.
[0012] While the names and definitions of nano-order substances vary by country and organization, the European standard (Commission Recommendation of 10.6.2022) defines powders containing 50% or more particles (called nanoparticles) whose smallest side length is less than 100 nm as nanomaterials and subject to regulation. Therefore, by controlling the proportion of nanoparticles constituting the powder to less than 50%, it is possible to obtain powders for cosmetics that comply with regulations. Regarding regulations in countries and regions outside of Europe, it is believed that it is possible to determine whether the powder of the present invention complies with regulations by referring to the data described in this specification below. [Brief explanation of the drawings]
[0013] [Figure 1] 1 is a transmission electron microscope photograph showing titanium (IV) oxide particles obtained in Example 2. [Figure 2] 1 is a transmission electron microscope photograph showing titanium (IV) oxide particles obtained in Example 3. [Figure 3] 1 is a transmission electron microscope photograph showing particles of titanium (IV) oxide obtained in Comparative Example 1. [Figure 4] 1 is a transmission electron microscope photograph showing particles of titanium (IV) oxide obtained in Comparative Example 3. DETAILED DESCRIPTION OF THE INVENTION
[0014] The powder of the present invention is composed primarily of titanium(IV) oxide particles. Specifically, "composed primarily of titanium(IV) oxide particles" means that the titanium(IV) oxide particles are contained in the particles constituting the powder at a ratio of 600 g / kg or more, preferably 700 g / kg or more, and more preferably 850 g / kg or more.
[0015] The titanium(IV) oxide particles constituting the powder of the present invention have an aspect ratio of 1.50 or more and 2.00 or less. An aspect ratio of 1.50 or more provides excellent UV protection, while an aspect ratio of 2.00 or less is less likely to produce a whitish appearance. The lower limit is preferably 1.55 or more, more preferably 1.60 or more, and the upper limit is preferably 1.90 or less, more preferably 1.87 or less, and even more preferably 1.85 or less.
[0016] The titanium (IV) oxide particles constituting the powder of the present invention have a median minor axis length (D 50 The value is called the D value.) is 105 nm or more and less than 150 nm. 50 If the value is 105 nm or more, the standard that the proportion of nanoparticles is less than 50% by number can be more reliably achieved. 50 If the value is 150 nm or less, the UV protection is high and white cast is less likely to occur. 50 The lower limit of the value is more preferably 108 nm or more, even more preferably 110 nm or more, and even more preferably 115 nm or more, and the upper limit is more preferably 140 nm or less, even more preferably 138 nm or less, and even more preferably 135 nm or less. 50 The value was calculated by observing approximately 300 particles using a transmission electron microscope, and the value (median) of the minor axis length of 50% of the total number of particles was used as the D value. 50 The median value based on the number of major axis lengths is D 50 The value divided by this is the aspect ratio.
[0017] The major axis length of the titanium(IV) oxide particles constituting the powder of the present invention is not particularly limited, but the median major axis length is preferably 150 nm or more and 300 nm or less. The lower limit is more preferably 180 nm or more, and the upper limit is more preferably 270 nm or less.
[0018] The titanium (IV) oxide particles constituting the powder of the present invention have a number-based arithmetic mean value b ave (nm) and standard deviation σ of minor axis length b (nm) satisfies the following formula: (b ave -100) / σ b ≧1.3 Standard deviation is an index that shows the dispersion of data. In a normal distribution, there are 683 / 1000 elements between the value obtained by subtracting the standard deviation from the mean and the value obtained by adding the standard deviation to the mean. The number of elements that are less than the value obtained by subtracting the standard deviation from the mean is (1000-683) / 2, which means that there are less than 159 / 1000 elements. In other words, b ave and σ b (b ave -100) / σ b If the value satisfies ≧ 1.0, it can be said that there are less than 159 particles (nanoparticles) with a minor axis length of 100 nm or less. Similarly, there are 800 particles / 1000 between the value obtained by subtracting 1.3 times the standard deviation from the average value and the value obtained by adding 1.3 times the standard deviation to the average value, so b ave and σ b (b ave -100) / σ b If the condition ≧1.3 is satisfied, the content of nanoparticles is less than 100 / 1000.
[0019] (b ave -100) / σ b is more preferably 1.6 or more, even more preferably 2.0 or more, even more preferably 2.6 or more, even more preferably 3.0 or more, and very preferably 4.0 or more. There are 900 / 1000 particles between the mean value plus or minus 1.6 times the standard deviation, 954 / 1000 particles between the mean value plus or minus 2.0 times the standard deviation, 990 / 1000 particles between the mean value plus or minus 2.6 times the standard deviation, 997 / 1000 particles between the mean value plus or minus 3.0 times the standard deviation, and at least 999 / 1000 particles between the mean value plus or minus 4.0 times the standard deviation. Therefore, (b ave -100) / σ b When the ratio is 1.6 or more, the nanoparticle content is less than 50 nanoparticles / 1000 nanoparticles; when the ratio is 2.0 or more, the nanoparticle content is 23 nanoparticles / 1000 nanoparticles or less; when the ratio is 2.6 or more, the nanoparticle content is 5 nanoparticles / 1000 nanoparticles; when the ratio is 3.0 or more, the nanoparticle content is 2 nanoparticles / 1000 nanoparticles or less; when the ratio is 4.0 or more, the nanoparticle content is 1 nanoparticle / 1000 nanoparticles or less. ave and σ bis calculated from the value of the minor axis length of each particle determined by observation with the above-mentioned transmission electron microscope.
[0020] The titanium (IV) oxide particles constituting the powder of the present invention have an average minor axis length b ave (nm) and standard deviation σ of minor axis length b It is preferable that (nm) also satisfies the following formula: (150-b ave ) / σ b ≧1.3 b ave and σ b If the above formula is satisfied, the proportion of particles with a minor axis length exceeding 150 nm will be less than 100 / 1000 of all particles. (150-b ave ) / σ b is more preferably 1.6 or more, even more preferably 2.0 or more, even more preferably 2.6 or more, even more preferably 3.0 or more, and very preferably 4.0 or more.
[0021] The standard deviation of the minor axis length is σ b The standard deviation of the minor axis length is preferably 30 nm or less, more preferably 20 nm or less, even more preferably 15 nm or less, and even more preferably 12 nm or less. If the standard deviation of the minor axis length is within the above range, the particle size will be uniform, and the powder will tend to have a good feel when added to cosmetics.
[0022] In order to reduce the content of nanoparticles, the titanium(IV) oxide particles constituting the powder of the present invention preferably have a ratio of particles having a minor axis length of less than 100 nm of 80 g / kg or less, more preferably 60 g / kg or less, even more preferably 35 g / kg or less, and even more preferably 20 g / kg or less. Since the titanium(IV) oxide particles constituting the powder of the present invention are considered to have no variation in density among the individual particles, the volume ratio can be considered to be the same as the mass ratio.
[0023] The titanium (IV) oxide particles constituting the powder of the present invention preferably have a narrow particle size distribution. Specifically, the average minor axis length b aveIt is preferable that the ratio of particles having a minor axis length within the range of ±12 nm is 700 g / kg or more of all particles. ave The proportion of particles with minor axis lengths within ±10 nm is 700 g / kg or more of all particles.
[0024] Another index is the minor axis length b of the particle with the largest minor axis length among the observed particles. MAX the minor axis length D 50 Value divided by value b MAX / D 50 is preferably 1.80 or less, and more preferably 1.50 or less. When the titanium(IV) oxide particles constituting the powder of the present invention satisfy the above indexes, the particle size distribution is sufficiently narrow, and the ultraviolet protection properties tend to be good when added to cosmetics.
[0025] The titanium(IV) oxide particles constituting the powder of the present invention preferably have a fibrous form consisting of minute rod-shaped particles. Here, "agglomeration of minute particles" refers to a state in which minute particles are aggregated and connected to one another. Furthermore, "agglomeration in a fibrous form" refers to a state in which the rod-shaped particles are aligned in the long axis direction and are aggregated so that the short axis length of the particle excluding the ends is approximately constant. It is preferable that there are no constrictions or protrusions. When the long axes of the rod-shaped particles are aligned randomly or orthogonally oriented in the majority during aggregation, or when the aggregated particles are perfectly circular, the rod-shaped particles are not considered to be aggregated in a fibrous form. Note that the aggregation of the minute rod-shaped particles that form the titanium(IV) oxide particles is not usually broken down during processes such as mixing, stirring, and surface treatments typically performed in this field, or during use in applications such as cosmetic materials. Therefore, in the present invention, the term "particles" generally refers to titanium(IV) oxide particles (including those in the form of aggregated rod-shaped particles), and when referring to the minor axis length or major axis length of a particle, unless otherwise specified, it refers to the minor axis length or major axis length of the titanium(IV) oxide particles (or the aggregated particles in the case of aggregated rod-shaped particles).
[0026] When titanium(IV) oxide particles are in the form of rod-shaped particles aggregated into fibers, they exhibit enhanced UV protection and facilitate the realization of a more natural finish when incorporated into cosmetics. The reasons for this are unclear, but are thought to be as follows: The UV protection of titanium(IV) oxide particles in the form of rod-shaped particles aggregated into fibers is enhanced compared to solid titanium(IV) oxide particles of the same particle diameter, because each individual rod-shaped particle has the ability to scatter UV light. Furthermore, titanium(IV) oxide particles in the form of rod-shaped particles aggregated into fibers leave numerous spaces within the particles, which scatters incident light, imparting a slightly blurred, soft impression to the scattered visible light, thereby facilitating the realization of a natural color. Furthermore, powders containing titanium(IV) oxide particles in the form of rod-shaped particles aggregated into fibers are thought to have better spreadability than powders containing solid titanium(IV) oxide particles of the same particle diameter, due to the smaller contact points between individual particles within the powder.
[0027] The rod-shaped particles constituting the titanium (IV) oxide particles preferably have a number-based median major axis length of 20 nm to 350 nm, and a number-based median minor axis length of 3 nm to 12 nm. The lower limit of the median major axis length of the rod-shaped particles is preferably 30 nm or more, and the upper limit is preferably 300 nm or less, and the lower limit of the minor axis is preferably 8 nm or more, and the upper limit is 11 nm or less. The number-based median major axis length and minor axis length of the rod-shaped particles are calculated by observing approximately 300 rod-shaped particles using a transmission electron microscope.
[0028] The titanium(IV) oxide particles constituting the powder of the present invention preferably have a roughly ellipsoidal shape without corners in their projection. A roughly ellipsoidal shape refers to a shape close to an ellipse with protrusions and irregularities on the surface. A roughly ellipsoidal projection of the particles is preferred because it tends to make the cosmetic feel smooth when added to the cosmetic. The projection of the particles is observed using a transmission electron microscope. The number density of the protrusions and irregularities on the surface is not particularly limited. It is expected that the titanium(IV) oxide particles constituting the powder of the present invention will have a shape close to an ellipsoid when observed using a scanning electron microscope.
[0029] The titanium(IV) oxide particles constituting the powder of the present invention are preferably rutile titanium(IV) oxide. Rutile titanium(IV) oxide has a weaker blue color and is less active than anatase titanium(IV) oxide, and is capable of absorbing longer wavelength ultraviolet light than anatase titanium(IV) oxide. Compared to titanium(IV) oxides of crystalline phases other than rutile and anatase, it is superior in terms of manufacturability and stability. The crystalline phase of titanium(IV) oxide can be determined by confirming the main peak of each crystalline phase (e.g., the diffraction intensity of the (110) plane of rutile titanium(IV) oxide) using an X-ray diffractometer.
[0030] The crystallite diameter of the titanium(IV) oxide particles constituting the powder of the present invention is preferably 20 nm or less. If the crystallite diameter is 20 nm or less, the finish tends to be natural when added to cosmetics. The lower limit is not particularly limited, but is 5 nm or more. The upper limit is preferably 15 nm or less, more preferably 12 nm or less, and the lower limit is preferably 7 nm or more, more preferably 8 nm or more.
[0031] The titanium (IV) oxide particles constituting the powder of the present invention have a specific surface area of 140 m 2 / g or more 225m 2 / g or less. 2 If it is more than 225m / g, the UV protection is likely to be good. 2 If the ratio is 1 / g or less, a good feel is likely to be obtained. 2 / g or more, more preferably 160m 2 / g or more, and the upper limit is preferably 215m 2 / g or less, more preferably 200m 2 / g or less.
[0032] The entire or at least a portion of the surface of the particles constituting the powder of the present invention may be coated with a layer of an inorganic and / or organic material. The inorganic material may include one or more of aluminum, silicon, zinc, titanium, zirconium, iron, cerium, and tin, preferably in the form of an oxide, hydroxide, or oxyhydroxide thereof. The organic material is preferably one or more of silicone-based compounds such as dimethylpolysiloxane and methylhydrogenpolysiloxane; silane-, aluminum-, titanium-, and zirconium-based coupling agents; fluorine compounds such as perfluoroalkyl phosphate compounds; and fatty acids such as lauric acid and stearic acid. Other materials that may be used include hydrocarbons, lecithin, amino acids, polyethylene, wax, and the like.
[0033] (Manufacturing method) The titanium(IV) oxide particles constituting the powder of the present invention can be obtained by a method comprising gradually adding hydrochloric acid to a slurry containing an acid-soluble titanium compound and an aliphatic hydroxy acid compound, and heating the mixture to dissolve the acid-soluble titanium compound (dissolution step).
[0034] The acid-soluble titanium compound may be any titanium compound soluble in hydrochloric acid, such as titanium hydroxide or sodium titanate. Sodium titanate is particularly preferred as such an acid-soluble titanium compound. The concentration of the acid-soluble titanium compound used is preferably 40 g / L or more and 100 g / L or less in terms of TiO2 after the addition of hydrochloric acid, as described below. The preferred slurry medium is water.
[0035] Examples of aliphatic hydroxy acid compounds include lactic acid, glycolic acid, citric acid, tartaric acid, isocitric acid, and salts thereof, with citric acid being particularly preferred due to its availability and low cost. These compounds may be used alone or in combination of two or more. The amount added is not limited, but is preferably 10 g / kg or more and 50 g / kg or less relative to TiO2.
[0036] Next, hydrochloric acid is gradually added to the slurry containing the acid-soluble titanium compound and the aliphatic hydroxy acid compound. After the addition of hydrochloric acid, the mixture is heated to dissolve the acid-soluble titanium compound. In the dissolution step, X (h) represents the time for adding hydrochloric acid, Y (g / L) represents the concentration of hydrochloric acid in the system during dissolution, and Z (°C) represents the liquid temperature during the dissolution step. X, Y, and Z satisfy the following formula: (1) 2.60≦Y / Z≦3.45 (2) Y 1 / 2 ×Z / X≦475 The reason for this is not clear, but the general trend is that the minor axis length of titanium (IV) oxide particles increases as Y / Z increases, and the particle size distribution of the minor axis length increases as Y / Z increases. 1 / 2 × The smaller the Z / X ratio, the smaller the D of the minor axis. 50 The value tends to be between 105 nm and 150 nm, and Y 1 / 2 If ×Z / X is 475 or less, the particle size distribution of the minor axis length becomes narrow (b ave -100) / σ b ≧1.3 is easily satisfied. The lower limit of Y / Z is more preferably 2.80 or more. 1 / 2 The upper limit of ×Z / X is more preferably 350 or less. 1 / 2 The lower limit of ×Z / X is not particularly limited.
[0037] The hydrochloric acid addition time X is preferably 2.0 hours or more. If the hydrochloric acid addition time is 2.0 hours or more, particles with a narrow particle size distribution of minor axis lengths can be obtained, and the resulting powder has small fluctuations in properties. It is more preferably 4.0 hours or more. The upper limit of the hydrochloric acid addition time is not particularly limited, but as a guideline, it is 50.0 hours or less from the viewpoint of efficiency in industrial production. The hydrochloric acid concentration Y is not particularly limited, but is 100 g / L or more and 170 g / L or less, with the upper limit more preferably 165 g / L or less, and even more preferably 160 g / L or less, and the lower limit more preferably 140 g / L or more. The liquid temperature Z in the dissolution step is preferably 35°C or more and 65°C or less, with the upper limit more preferably 60°C or less, and even more preferably 55°C or less, and the lower limit more preferably 40°C or more.
[0038] The time for which the solution is kept at temperature Z (° C.) is not particularly limited, but is preferably 10 hours or more. The upper limit is not particularly limited, but is preferably 60 hours or less from the viewpoint of production efficiency. After dissolution, the sample is preferably cooled, filtered, washed, and recovered by maintaining the solution at a constant temperature to precipitate titanium(IV) oxide. While the conditions for precipitation are not limited, it is preferable to maintain the solution at 60°C or higher and 100°C or lower for 1 hour or longer. The temperature is more preferably 70°C or higher and 100°C or lower. While there are no particular limitations on the upper limit of the retention time, 25 hours or shorter is preferable. There are no particular limitations on the methods for cooling, filtering, and washing. It is preferable to perform the process using procedures commonly used in this field.
[0039] The titanium(IV) oxide particles obtained above may have at least a portion of their surface coated with an inorganic and / or organic layer. The coating method is not particularly limited, and commonly used methods can be used. By coating at least a portion of the particle surface with an inorganic layer, for example, it is possible to improve dispersion stability and durability in a dispersion medium. Usable inorganic substances include, for example, one or more of metals such as aluminum, silicon, zinc, titanium, zirconium, iron, cerium, and tin. Oxides, hydroxides, or oxyhydroxides of these metals are preferred. There are no limitations on the type of metal salt.
[0040] Depending on the intended use of the cosmetic, the particles can be treated to be water- and / or oil-repellent by coating at least a portion of the particle surface with a layer of an organic substance. Examples of organic substances include silicone compounds such as dimethylpolysiloxane and methylhydrogenpolysiloxane, silane-, aluminum-, titanium-, and zirconium-based coupling agents, fluorine compounds such as perfluoroalkyl phosphate compounds, hydrocarbons, lecithin, amino acids, polyethylene, wax, and fatty acids such as lauric acid and stearic acid.
[0041] The titanium(IV) oxide particles obtained above may be calcined. Calcination makes it possible to adjust the hiding power. The surface of the calcined particles may be further coated with an inorganic and / or organic layer.
[0042] (Application) The use of the powder of the present invention is not particularly limited, but it is particularly suitable for use in cosmetics. By adding the powder of the present invention, it is possible to impart UV protection properties to a cosmetic composition. Furthermore, when added to cosmetics, the powder of the present invention is less likely to cause a white cast, has good spreadability, and is smooth to the touch.
[0043] The powder of the present invention has a controlled content of nanoparticles, and by using the powder of the present invention, a cosmetic composition that does not fall under the current European nanomaterial regulations can be obtained. When the powder of the present invention is used in cosmetics, the powder may be mixed with other cosmetic raw materials according to known methods. It is preferable that the powder be previously coated on its surface. When mixing with other cosmetic raw materials, the powder may be mixed with the other raw materials as is, or the powder may be dispersed in a dispersion medium to prepare a dispersion, and then this dispersion may be mixed with the other raw materials. In the present invention, the term "cosmetic composition containing powder" includes not only cosmetics containing the powder of the present invention as is (in powder form), but also cosmetics in which the powder is dispersed in a dispersion medium to prepare a dispersion and then incorporated into the cosmetic.
[0044] The content of the powder of the present invention in a cosmetic composition can be set as desired depending on the required properties of the various cosmetic compositions, but is preferably 1 g / kg or more and 500 g / kg or less. A powder content of 1 g / kg or more in a cosmetic composition can impart UV protection properties to the cosmetic, while a powder content of 500 g / kg or less can achieve a non-powdery feel. The lower limit is more preferably 5 g / kg, even more preferably 10 g / kg or more, and the upper limit is preferably 450 g / kg or less. The powder of the present invention may be a mixture of two or more powders that differ in one or more of the major axis length, minor axis length, and aspect ratio, or titanium oxides of different particle sizes and / or shapes may be further blended into a cosmetic composition containing the powder of the present invention depending on the purpose.
[0045] When preparing a cosmetic composition containing the titanium(IV) oxide powder of the present invention, various components used in ordinary cosmetics, such as inorganic pigments and organic pigments, can be used in combination as needed. Examples of inorganic pigments that can be used in combination include titanium oxide, zinc oxide, red iron oxide, yellow iron oxide, black iron oxide, brown iron oxide, ultramarine, Prussian blue, cerium oxide, talc, muscovite, synthetic mica, phlogopite, biotite, synthetic fluorphlogopite, titanium mica, micaceous iron oxide, sericite, zeolite, kaolin, bentonite, clay, silicic acid, silicic acid anhydride, magnesium silicate, 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 complexes thereof. Examples of organic pigments that can be used in combination include silicone powder, silicone elastic powder, polyurethane powder, cellulose powder, nylon powder, urethane powder, silk powder, polymethyl methacrylate (PMMA) powder, starch, polyethylene powder, polystyrene powder, carbon black, tar dyes, natural dyes, metal soaps such as zinc stearate, and complexes thereof.
[0046] In addition to the above-mentioned components, cosmetic compositions containing the powder of the present invention may contain other components depending on the purpose, within quantitative and qualitative ranges that do not impair the effects of the present invention. For example, oily components, pigments, pH adjusters, moisturizers, thickeners, surfactants, dispersants, stabilizers, colorants, preservatives, antioxidants, sequestering agents, astringents, anti-inflammatory agents, ultraviolet absorbers, fragrances, etc. may be appropriately blended within ranges that do not impair the effects of the present invention.
[0047] Cosmetic compositions containing the powder of the present invention can be produced by known methods. The cosmetic formulation may be in any form, such as powder, powder solid, cream, emulsion, lotion, oily liquid, oily solid, or paste. For example, the cosmetic may be in the form of makeup cosmetics, skin care cosmetics, or hair care cosmetics, such as makeup base, foundation, concealer, face powder, control color, sunscreen cosmetics, lipstick, lip balm, eye shadow, eyeliner, mascara, blush color, nail polish, body powder, perfume powder, or baby powder.
[0048] In addition to cosmetics, the powder of the present invention can be used in various fields where titanium dioxide is generally used, including, but not limited to, resin compositions, paints, inks, toner additives, photocatalysts, electrical and electronic materials, heat insulating materials, radio wave blocking materials, and ultraviolet blocking materials.
[0049] For example, the powder of the present invention has a characteristic that gaps tend to form between particles due to its particle shape, and it is believed that when added to a resin, it has the effect of preventing the formation of so-called clumps. This characteristic is also believed to be applicable in the fields of ink, paint, and electrical and electronic materials. That is, a cosmetic composition, resin composition, paint, ink, or electrical and electronic material containing the powder of the present invention is one aspect of the present invention. From another perspective, the use of the powder of the present invention in a cosmetic composition, resin composition, paint, ink, or electrical and electronic material is also one aspect of the present invention. For example, the use of the powder of the present invention to produce a cosmetic composition, resin composition, paint, ink, or electrical and electronic material can also be said to be one aspect of the present invention.
[0050] Before describing the examples, the test methods used in the present invention will be described. [Evaluation items and evaluation methods] [Average long axis length and average short axis length of titanium oxide particles b ave , minor axis length D 50 value, aspect ratio, b MAX / D 50 ] Measurements were made using a JEOL JEM-1400plus transmission electron microscope. The observation magnification was 30,000x (10,000x observation magnification of the transmission electron microscope x 3x print). The length of the longest part of each particle was taken as the major axis length, and the length of the longest part perpendicular to the major axis was taken as the minor axis length. The major and minor axis lengths of approximately 300 particles were evaluated using the image analysis software ImageJ. From the major and minor axis lengths of approximately 300 particles, the median of the number of major axis lengths and the median of the number of minor axis lengths (D 50 value), the arithmetic mean value b of the number of minor axis lengths ave Calculate the median of the major axis length, D 50 The value obtained by dividing the particle size by the particle size was taken as the aspect ratio of the powder. MAX Let b MAX / D 50 was calculated.
[0051] Standard Deviation From the observation data of the above approximately 300 particles, the standard deviation of the minor axis length σ b Calculate (b ave -100) / σ b was calculated.
[0052] [Percentage of particles with a minor axis length of less than 100 nm, minor axis length is b ave The proportion of particles within ±12 nm, the minor axis length is b ave Percentage of particles within ±10 nm The observation data for the approximately 300 particles described above was separated into particles with a minor axis length of less than 100 nm and other particles. Because the projected shapes of all the particles observed were roughly elliptical, the volume of each particle was approximated as being proportional to the value obtained by multiplying the major axis length by the square of the minor axis length. The volume fraction was calculated by dividing the sum of the values obtained by multiplying the major axis length by the square of the minor axis length for all particles with a minor axis length of less than 100 nm by the sum of the values obtained by multiplying the major axis length by the square of the minor axis length for all particles. Furthermore, because it is believed that there is no variation in the density of the individual particles, the resulting volume fraction was used as the mass fraction.
[0053] Minor axis length is b ave Within ±12 nm and b aveFor particles within ±10 nm, the minor axis length is b ave Within ±12 nm or b ave The same calculation was performed separately for particles within ±10 nm and other particles.
[0054] [Crystalline phase, crystallite size] Using a Rigaku RINT-TTRIII X-ray diffractometer, the target was copper (Cu), the tube voltage was 50 kV, the tube current was 300 mA, the divergence slit was set to automatic mode, the vertical divergence slit was 10 mm, the scattering slit was 1 / 2°, the receiving slit was 0.3 mm, and the scanning speed was 0.2° / min. The 2θ range was scanned from 20° to 35°, and the diffraction intensities of the peaks corresponding to the (110) plane of rutile titanium dioxide (IV) and the (101) plane of anatase titanium dioxide (IV) were measured.
[0055] In addition, the diffraction intensity of the peak corresponding to the (110) plane of rutile titanium dioxide (IV) was measured in the 2θ range of 26.5° to 28.5°, and the crystallite size was calculated using the Scherrer equation.
[0056] [Specific surface area] Using a Micromeritics Gemini VII 2390, 0.2 g of a sample was degassed using a Micromeritics VacuPrep 061 at 150°C for 30 minutes, then cooled for 15 minutes, and then measured by the BET single-point method. [Example]
[0057] The present invention will be described in more detail below with reference to examples, which are provided for illustrative purposes only and are not intended to limit the scope of the invention. In the stirring operations described in the examples and comparative examples, the rotation speed is appropriately adjusted to ensure that the entire liquid is mixed uniformly and that droplets do not scatter, taking into consideration properties related to the behavior of the liquid during stirring, such as the liquid volume, viscosity, and shape of the container. Furthermore, in cases where the same effect can be obtained by using any company's commonly available commercially available product, such as sodium hydroxide or hydrochloric acid, the names of the manufacturer and distributor are omitted.
[0058] [Example 1] Commercially available sodium titanate was mixed with water, and the concentration was adjusted so that the TiO2 concentration would be 80 g / L after the addition of hydrochloric acid, which will be described later. Citric acid was added so that the amount was 30 g / kg relative to TiO2, and then 400 g / L of hydrochloric acid was gradually added over 5.3 hours until the hydrochloric acid concentration reached 155 g / L. After the addition of hydrochloric acid was completed, the slurry was heated while stirring using a HEIDON (registered trademark) 600G (hereinafter referred to as "stirrer") manufactured by Shinto Scientific Co., Ltd., and the liquid temperature was kept at 50°C for 20 hours with stirring. Y / Z was 3.10, Y 1 / 2 ×Z / X was 117. Thereafter, the liquid temperature was raised and maintained at 80°C for 8 hours to precipitate solids, which were then cooled to room temperature, filtered, and washed to obtain a white powder A.
[0059] Powder A is composed of particles that are composed of minute rod-shaped particles aggregated in a fibrous form and have a roughly elliptical projection. The particles have a median major axis length of 218 nm and a median minor axis length of D 50 is 123 nm, aspect ratio is 1.78, average minor axis length b ave is 121 nm, (b ave -100) / σ b is 2.0, (150-b ave ) / σ b The crystal phase was confirmed by X-ray diffraction analysis, and the main peak was derived from rutile-type titanium dioxide (IV), and no peak was derived from anatase-type titanium dioxide. The crystallite diameter was 9 nm, and the specific surface area was 190 m 2 / kg, particles with a minor axis length of less than 100 nm (nanoparticles) are 5g / kg of the total particles constituting the powder, b MAX / D 50 is 1.26, and the minor axis length is b ave Particles within ±12 nm are 796 g / kg of the total particle weight, and the minor axis length is b ave The particles within ±10 nm accounted for 748 g / kg of the total particles.
[0060] [Example 2] White powder B was obtained in the same manner as in Example 1, except that hydrochloric acid was added over 2.2 hours and the liquid temperature during the dissolution process was adjusted to 55°C. Figure 1 shows a transmission electron microscope photograph of powder B. Powder B was composed of particles that were approximately ellipsoidal in projection, with minute rod-shaped particles agglomerated into fibers. The properties of the particles and powder are shown in Table 2.
[0061] [Example 3] White powder C was obtained in the same manner as in Example 1, except that hydrochloric acid was added over 6.0 hours. Figure 2 shows a transmission electron microscope photograph of powder C. Powder C was composed of particles with a roughly elliptical projection, in which minute rod-shaped particles were aggregated in a fibrous form. The properties of the particles and powder are shown in Table 2.
[0062] [Example 4] White powder D was obtained in the same manner as in Example 1, except that hydrochloric acid was added over 5.0 hours. Powder D consisted of particles with a roughly elliptical projection, consisting of minute rod-shaped particles aggregated in a fibrous form. The properties of the particles and powder are shown in Table 2.
[0063] [Example 5] White powder E was obtained in the same manner as in Example 4, except that the liquid temperature during the dissolution step was adjusted to 45°C. Powder E was composed of particles that were approximately elliptical in projection, consisting of tiny rod-shaped particles aggregated in a fibrous form. The properties of the particles and powder are shown in Table 2.
[0064] [Example 6] White powder F was obtained in the same manner as in Example 1, except that the TiO concentration after the addition of hydrochloric acid was adjusted to 60 g / L, the amount of citric acid added was 25 g / kg relative to TiO, hydrochloric acid was added over 10.0 hours until the hydrochloric acid concentration reached 160 g / L, the holding time for the dissolution step was 30 hours, and the precipitation was held at 80°C for 10 hours. Powder F was composed of particles with a roughly elliptical projection, consisting of tiny rod-shaped particles aggregated in a fibrous form. The particle and powder properties are shown in Table 2.
[0065] [Example 7] White powder G was obtained using the same procedure as in Example 6, except that hydrochloric acid was added over 30.0 hours until the hydrochloric acid concentration reached 145 g / L, the liquid temperature during the dissolution process was 42°C, the holding time during the dissolution process was 40 hours, and the holding time during precipitation was 20 hours. Powder G was composed of particles with a roughly elliptical projection, consisting of tiny rod-shaped particles aggregated in a fibrous form. The particle and powder properties are shown in Table 2.
[0066] [Example 8] White powder H was obtained using the same procedure as in Example 7, except that the TiO2 concentration after the addition of hydrochloric acid was adjusted to 40 g / L, hydrochloric acid was added over 40.0 hours until the hydrochloric acid concentration reached 142 g / L, and the liquid temperature during the dissolution process was 44°C. Powder H was composed of particles with a roughly elliptical projection, consisting of tiny rod-shaped particles aggregated in a fibrous form. The particle and powder properties are shown in Table 2.
[0067] [Example 9] White powder I was obtained in the same manner as in Example 1, except that hydrochloric acid was added over 2.0 hours until the hydrochloric acid concentration reached 158 g / L and the liquid temperature during the dissolution process was 60°C. Powder I was composed of particles that were approximately ellipsoidal in projection, consisting of tiny rod-shaped particles aggregated in a fibrous form. The properties of the particles and powder are shown in Table 2.
[0068] [Comparative Example 1] White powder O was obtained in the same manner as in Example 1, except that hydrochloric acid was added over 1.5 hours and the liquid temperature during the dissolution process was adjusted to 60°C. Figure 3 shows a transmission electron microscope photograph of powder O. Powder O was composed of particles that were approximately ellipsoidal in projection, with minute rod-shaped particles agglomerating into fibers. The properties of the particles and powder are shown in Table 2.
[0069] Comparative Example 2 White powder P was obtained in the same manner as in Comparative Example 1, except that the hydrochloric acid concentration was 150 g / L. Powder P was composed of particles that were approximately elliptical in projection, with minute rod-shaped particles agglomerated into fibers. The properties of the particles and powder are shown in Table 2.
[0070] Comparative Example 3 White powder Q was obtained in the same manner as in Comparative Example 2, except that hydrochloric acid was gradually added over 1.3 hours until the hydrochloric acid concentration reached 175 g / L and the liquid temperature during the dissolution process was adjusted to 50°C. Figure 4 shows a transmission electron microscope photograph of powder Q. Powder Q was composed of particles that were approximately ellipsoidal in projection, with minute rod-shaped particles agglomerated into fibers. The properties of the particles and powder are shown in Table 2.
[0071] Table 1 shows the production conditions for the powders of the Examples and Comparative Examples, and Table 2 shows the properties of the particles and powders obtained in the Examples and Comparative Examples.
[0072] [Table 1]
[0073] [Table 2]
[0074] As is clear from Table 2, the powders A to I obtained in Examples 1 to 9 had a (b ave -100) / σ b , (150-b ave ) / σ b Both are 1.3 or more. The powders of Examples 1 to 9 have a small content of nanoparticles and are not considered nanomaterials under the current European standards. On the other hand, the majority of the particles constituting the powders of Powders O and P obtained in Comparative Examples are nanoparticles, and are considered nanomaterials under the European standards. Powder Q has a D 50 Because the value is large, it cannot be said that the film has sufficient properties in terms of UV protection and prevention of white cast.
[0075] (Cosmetic composition) The cosmetic composition containing the powder of the present invention will be described below. Powder C obtained in the example was surface-treated with commercially available stearic acid (stearic acid-treated powder C), and a W / O type liquid foundation was prepared using the powder.
[0076] [Formulation example 1: W / O type liquid foundation] (Ingredients) Mixing ratio (g / kg) 1. Cross-linked polyether-modified silicone (Note 1) 40 2. Cross-linked dimethylpolysiloxane (Note 2) 60 3. Branched polyether-modified silicone (Note 3) 20 4. Decamethylcyclopentasiloxane 210 5. Dimethylpolysiloxane (6mm 2 / s(25℃)) 70 6. Stearic acid treated powder C 150 7. Silicone-treated talc (Note 4) 40 8. Silicone-treated coloring agent (Note 4) 15 9. 1,3-Butylene glycol 50 10. Sodium citrate 4 11. Sodium Chloride 5 12. Preservatives (appropriate amount) 13.Purified water remainder (Note 1) Shin-Etsu Chemical Co., Ltd.: KSG-210 (Note 2) Shin-Etsu Chemical Co., Ltd.: KSG-15 (Note 3) Shin-Etsu Chemical Co., Ltd.: KF-6028 (Note 4) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-9909 (Manufacturing method) A: Ingredients 6 to 8 were mixed uniformly. B: Components 1 to 5 were mixed uniformly and A was dispersed uniformly. C: Ingredients 9 to 13 were mixed uniformly. D: C was gradually added to B while stirring and emulsified to obtain a W / O type liquid foundation.
[0077] [Evaluation items and evaluation methods for cosmetics] The obtained cosmetics were subjected to a UV protection test and a sensory test. (UV protection test) The prepared W / O type liquid foundation was applied to the Transpore tape at 2 mg / cm 2After application, UV protection was measured using a Labsphere UV-1000S SPF analyzer. SPF (Sun Protection Factor) is used as the standard for UV protection. Although it depends on the usage conditions, an SPF value of 24 or higher can be considered to provide sufficient UV protection in everyday use.
[0078] (sensory test) The prepared W / O type liquid foundation was used by 10 panelists, who performed a sensory evaluation on a 5-point scale for spreadability, smoothness, roughness, transparency, coverage, white cast, and makeup durability, and the average score was used to determine the results. (Evaluation criteria: spreadability, smoothness, roughness, transparency, coverage, and makeup staying power) Very good: 5 points Good: 4 points Normal: 3 points Slightly poor: 2 points Defective: 1 point (Evaluation criteria for white cast) No whitish impression even when viewed from a distance of 30 cm: 5 points There is a momentary sense of discomfort when viewed from a distance of 30 cm: 4 points At a distance of 30cm, it appears whitish, but at a distance of 1m, it does not appear whitish: 3 points When viewed from a distance of 1m, it gives a whitish impression: 2 points It looks like it has been painted white: 1 point.
[0079] The results of the UV protection test and the sensory test are shown in Table 3. The sensory test results can be considered to pass if the average score is 3.0 points or more.
[0080] [Table 3]
[0081] The results of the UV protection test and the sensory test showed that the foundation containing the powder obtained in the examples of the present invention had good UV protection properties, a good feel such as spreadability and smoothness, and a good finish such as the resistance to white cast and good coverage. As mentioned above, the powder of the present invention has a controlled nanoparticle content, and also showed good UV protection properties and good results in the sensory test.
[0082] A powder foundation was prepared using the powder obtained in the example. [Formulation example 2: Powder foundation] (Ingredients) Mixing ratio (g / kg) 1. Caprylylsilane-treated mica (Note 1) 400 2. Powder C 50 3. Silicone-treated talc (Note 2) residue 4. Silicone-treated pigment-grade titanium dioxide (Note 2) 50 5. Silicone-treated titanium dioxide microparticles (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. Preservatives (appropriate amount) 14.Fragrance (appropriate amount) 15. Crosslinked dimethylpolysiloxane (Note 5) 40 16. Glyceryl Trioctanoate 20 17. Squalane 10 (Note 1) Surface treated with Shin-Etsu Chemical Co., Ltd.'s AES-3083 (Note 2) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-9909 (Note 3) Shin-Etsu Chemical Co., Ltd.: KSP-300 (Note 4) Shin-Etsu Chemical Co., Ltd.: KMP-590 (Note 5) Shin-Etsu Chemical Co., Ltd.: KSG-16 (Manufacturing method) A: Ingredients 1 to 13 were mixed and ground uniformly. B: Ingredients 15 to 17 were mixed uniformly and added to A and mixed uniformly. C: Component 14 was added to B, and the mixture was press-molded into a mold to obtain a powder foundation. The obtained powder foundation spread smoothly and lightly, had excellent makeup durability, and gave a natural impression.
[0083] The powder obtained in the example was used to prepare a pressed powder. [Formulation example 3: Pressed powder] (Ingredients) Mixing ratio (g / kg) 1. Talc residue 2.PMMA (7μm) (Note 1) 100 3. Sericite 300 4. Scaly silica (Note 2) 30 5. Powder E 60 6. Preservatives (appropriate amount) 7. Appropriate amount of coloring material 8. Ethylhexyl methoxycinnamate 30 9. Squalane 20 10. Preservatives (appropriate amount) 11. Antioxidant (appropriate amount) 12.Fragrance (appropriate amount) (Note 1) Matsumoto Yushi Pharmaceutical Co., Ltd.: Matsumoto Microsphere M-100 (Note 2) AGC Si-Tech Co., Ltd.: Sun Lovely (registered trademark) C (Manufacturing method) A: Ingredients 1 to 7 were mixed and ground. B: A was transferred to a LAB.MIXER LM-110T manufactured by HANIL Electric. Co., Ltd. (hereinafter referred to as "Henschel mixer"), and ingredients 8 to 12 were added and mixed uniformly. C: B was pulverized using a sample mill TASM-1 manufactured by Tokyo Atomizer Mfg. Co., Ltd. (hereinafter referred to as "atomizer"), and this was press-molded into an aluminum dish to obtain a pressed powder. The obtained pressed powder had excellent spreadability and smoothness when applied, and furthermore, gave a natural impression even after application.
[0084] A 2-way cake foundation was produced using the powder obtained in the example. [Formulation example 4: 2-way cake foundation] (Ingredients) Mixing ratio (g / kg) 1. Silicone-treated talc (Note 1) residue 2. Powder D 100 3. Silicone-treated mica (Note 1) 200 4. Silicone-treated sericite (Note 1) 360 5. Nylon powder 100 6. Silicone-treated yellow iron oxide (Note 1) 10 7. Silicone-treated red iron oxide (Note 1) 5 8. Silicone-treated black iron oxide (Note 1) 1 9. Dimethylpolysiloxane 1000cs 60 10. Isotridecyl isononanoate 30 11. Squalane 30 12. Preservatives 2 13. Antioxidant 1 (Note 1) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-99P (Manufacturing method) A: Ingredients 9 to 13 were heated and dissolved. B: Components 1 to 8 were mixed in a Henschel mixer, and then A was mixed therewith. C: B was pulverized using an atomizer and pressed into an aluminum dish to obtain a 2-way cake foundation. The obtained 2-way cake foundation spreads smoothly and smoothly upon application, and even after application, it has adequate coverage and does not leave a white cast, giving a natural impression.
[0085] An oil-based cake foundation was prepared using the powder obtained in the example. [Formulation example 5: Oily cake foundation] (Ingredients) Mixing ratio (g / kg) 1. Silicone-treated talc (Note 1) 53 2. Powder A 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. Ceresin 15 10. Decamethylcyclopentasiloxane 140 11. Isononyl isononanoate residue 12. Polyglyceryl Diisostearate 20 13. Dextrin Palmitate 10 14. Ethylhexyl methoxycinnamate 30 15. Preservatives (appropriate amount) 16. Antioxidant (appropriate amount) (Note 1) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-96A (Manufacturing method) A: Components 1 to 6 were mixed in a Henschel mixer and pulverized uniformly. B: Ingredients 7 to 16 were heated and dissolved, and A was added and stirred uniformly. C: After degassing, B was poured into a tray and gradually cooled to room temperature to obtain an oil-based cake foundation. The oil-based cake foundation obtained spreads smoothly and smoothly upon application, and furthermore, due to its adequate covering power, it does not leave a white cast even after application, giving a natural impression.
[0086] A stick foundation was prepared using the powder obtained in the example. [Formulation example 6: Stick foundation] (Ingredients) Mixing ratio (g / kg) 1. Dimethylpolysiloxane 180 2. Decamethylcyclopentasiloxane 300 3. Ethylhexyl methoxycinnamate 50 4. Diisostearyl Malate 40 5. Candelilla Wax 60 6. Hydrogenated Jojoba Esters 40 7. Cetyl Dimethicone Copolyol 20 8. Sorbitan Sesquiisostearate 5 9. Antioxidant (appropriate amount) 10. Preservatives (appropriate amount) 11.Fragrance (appropriate amount) 12. Silicone-treated coloring agent (Note 1) 5 13. Powder B 85 14. Silicone-treated talc (Note 1) 60 15. Silicone-treated mica (Note 1) 20 16. Polymethyl methacrylate 20 17.Purified water remainder 18. Sodium citrate 3 19. 1,3-Butylene Glycol 30 20. Glycerin 20 21. Preservatives (appropriate amount) (Note 1) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-99P (Manufacturing method) A: Ingredients 12 to 16 were mixed in a Henschel mixer. B: Components 1 to 11 were weighed into a container that could hold the entire amount, and dissolved by heating. C: Ingredients 17 to 21 were weighed into a separate container and dissolved by heating. D: A was added to B and dispersed uniformly, and C was added and emulsified. E: After degassing, D was poured into a mold and gradually cooled to room temperature to obtain a stick foundation. The obtained stick foundation spreads smoothly and smoothly upon application, and furthermore, due to its adequate covering power, it does not leave a white cast even after application, giving a natural impression.
[0087] A W / O emulsion foundation was prepared using the powder obtained in the example. [Formulation example 7: W / O emulsion foundation] (Ingredients) Mixing ratio (g / kg) 1. POE modified silicone (HLB=4.5) 8 2. Polyglyceryl Polyricinoleate 5 3. Neopentyl glycol dicaprate 30 4. Squalane 10 5. Pentaerythrityl tetraoctanoate 20 6. Inulin stearate (Note 1) 10 7. Ethylhexyl methoxycinnamate 40 8. Cyclomethicone 154 9. Preservatives (appropriate amount) 10. Antioxidant (appropriate amount) 11.Fragrance (appropriate amount) 12. Powder D 80 13. Silicone-treated talc (Note 2) 57 14. Silicone-treated coloring agent (Note 2) 10 15.Purified water remainder 16. 1,3-Butylene Glycol 60 17. Glycerin 10 18. Sodium Chloride 10 19. Preservatives (appropriate amount) (Note 1) Chiba Flour Mills: Leopard (registered trademark) ISK (Note 2) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-99P (Manufacturing method) A: Ingredients 12 to 14 were mixed in a Henschel mixer. B: Components 1 to 11 were added to A and dispersed uniformly using a stirrer. C: In a separate container, ingredients 15 to 19 were heated and dissolved. D: C was added to B and emulsified, and then cooled to room temperature to obtain a W / O emulsion foundation. The obtained W / O emulsion foundation spreads smoothly and smoothly upon application, and even after application, it has adequate coverage and does not leave a white cast, giving a natural impression.
[0088] An O / W emulsion foundation was prepared using the powder obtained in the example. [Formulation example 8: O / W emulsion foundation] (Ingredients) Mixing ratio (g / kg) 1. Stearic acid 4 2. Isostearic acid 3 Cetyl 3,2-ethylhexanoate 40 4. Liquid Paraffin 110 5. POE(10) Stearyl Ether 20 6. Cetyl Alcohol 3 7. Preservatives 2 8. Talc 150 9. Colorant 40 10. Powder B 30 11. Triethanolamine 4 12. Propylene Glycol 50 13.Purified water 541 14. Antioxidant 3 (Manufacturing method) A: Components 1 to 7 were heated and dissolved at 85°C. B: Ingredients 8 to 10 were mixed and ground. C: Ingredients 11 to 14 were heated to 85°C and melted and mixed. D: B was added to A and dispersed uniformly, C was gradually added to this and emulsified, and the mixture was stirred and cooled to room temperature. The mixture was then poured into a suitable container to obtain an O / W emulsion foundation. The obtained O / W emulsion foundation spreads smoothly and smoothly upon application, and even after application, it has adequate coverage and does not leave a white cast, giving a natural impression.
[0089] A moisturizing O / W type cream was prepared using the powder obtained in the example. [Formulation Example 9: Moisturizing O / W type cream] (Ingredients) Mixing ratio (g / kg) 1. Crosslinked dimethylpolysiloxane (Note 1) 80 2. Crosslinked dimethylpolysiloxane (Note 2) 280 3. Decamethylcyclopentasiloxane 100 4. Powder A 50 5. Branched polyglycerin-modified silicone (Note 3) 3 6. Branched polyglycerin-modified silicone (Note 4) 6 7. (Acrylamide / sodium acryloyldimethyltaurate) copolymer (Note 5) 6 8. Ammonium acrylate dimethyl taurate / VP copolymer (5% aqueous solution) (Note 6) 120 9. Polyethylene Glycol 400 10 10. Sodium lactate 50 11. 1,3-Butylene Glycol 50 12.Purified water 245 (Note 1) Shin-Etsu Chemical Co., Ltd.: KSG-15 (Note 2) Shin-Etsu Chemical Co., Ltd.: KSG-16 (Note 3) Shin-Etsu Chemical Co., Ltd.: KF-6104 (Note 4) Shin-Etsu Chemical Co., Ltd.: KF-6100 (Note 5) Seppic: Simulgel 600 (Note 6) Clariant: Aristoflex (registered trademark) AVC (Manufacturing method) A: Components 3 to 5 were mixed and dispersed uniformly. B: Components 1, 2 and A were mixed together and mixed uniformly. C: Ingredients 6 to 12 were mixed uniformly. D: B was gradually added to C while stirring and emulsified to obtain a moisturizing O / W type cream. The obtained moisturizing O / W type cream spread easily, had no squeaky feeling, and was also highly stable.
[0090] An O / W type cream was prepared using the powder obtained in the example. [Formulation example 10: O / W type cream] (Ingredients) Mixing ratio (g / kg) 1. Crosslinked dimethylpolysiloxane (Note 1) 50 2. Powder C 10 3. Glyceryl Triisostearate 80 4. Cetyl alcohol 5 5. Stearic acid 10 6. Glyceryl Monostearate 5 7. Sorbitan Sesquioleate 5 8. Polyoxyethylene sorbitan monooleate 10 9. Triethanolamine 5 10. Carbomer (1% aqueous solution) 200 11. Locust bean gum (2% aqueous solution) 50 12. 1,3-Butylene Glycol 70 13. Preservatives (appropriate amount) 14.Fragrance (appropriate amount) 15.Purified water 490 (Note 1) Shin-Etsu Chemical Co., Ltd.: KSG-15 (Manufacturing method) A: Ingredients 1 to 8 were heated and mixed until homogenous. B: Ingredients 9 to 13 and 15 were mixed and heated. C: While stirring, B was gradually added to A and emulsified. After cooling, ingredient 14 was added to obtain an O / W cream. The obtained O / W type cream spread easily and had excellent stability.
[0091] A W / O type cream was prepared using the powder obtained in the example. [Formulation example 11: W / O type cream] (Ingredients) Mixing ratio (g / kg) 1. Cross-linked alkyl polyether modified silicone (Note 1) 30 2. Cross-linked alkyl-modified dimethylpolysiloxane (Note 2) 40 3. Alkyl-modified branched polyether-modified silicone (Note 3) 10 4. Meadowhoo Oil 35 5. Macadamia nut oil 50 6. Jojoba Oil 100 7. Hybrid silicone composite powder (Note 4) 30 8. Powder D 20 9. 1,3-Butylene glycol 80 10. Glycine 30 11. Sodium citrate 2 12. Sodium Chloride 5 13. Preservatives (appropriate amount) 14.Fragrance (appropriate amount) 15.Purified water remainder (Note 1) Shin-Etsu Chemical Co., Ltd.: KSG-340 (Note 2) Shin-Etsu Chemical Co., Ltd.: KSG-44 (Note 3) Shin-Etsu Chemical Co., Ltd.: KF-6038 (Note 4) Shin-Etsu Chemical Co., Ltd.: KSP-100 (Manufacturing method) A: Ingredients 1 to 8 were mixed uniformly. B: Ingredients 9 to 13 and ingredient 15 were mixed uniformly. C: While stirring, B was gradually added to A and emulsified, and ingredient 14 was added to obtain a W / O type cream. The obtained W / O type cream spread easily without any squeaky feeling, had good makeup lasting power, and was also excellent in stability.
[0092] A body lotion was prepared using the powder obtained in the example. [Formulation example 12: Body lotion] (Ingredients) Mixing ratio (g / kg) 1. Ethanol 170 2.1,3-Butylene Glycol 30 3. Branched polyglycerin-modified silicone (Note 1) 5 4. Glyceryl Trioctanoate 10 5. Powder E 20 6. Hybrid silicone composite powder (Note 2) 100 7. Ammonium dimethyl acrylate taurate / VP copolymer 4 8. Xanthan gum (2% aqueous solution) 60 9. Sodium Chloride 1 10.Purified water 600 (Note 1) Shin-Etsu Chemical Co., Ltd.: KF-6100 (Note 2) Shin-Etsu Chemical Co., Ltd.: KSP-100 (Manufacturing method) A: Ingredients 1 to 6 were mixed uniformly. B: Ingredients 7 to 10 were mixed uniformly. C: A was gradually added to B while stirring, and mixed to obtain a body lotion. The obtained body lotion spread easily and had excellent stability.
[0093] A sun-cut cream was prepared using the powder obtained in the example. [Formulation Example 13: Sun Cut Cream] (Ingredients) Mixing ratio (g / kg) 1. Cross-linked polyether-modified silicone (Note 1) 20 2. Crosslinked dimethylpolysiloxane (Note 2) 30 3. Branched polyether-modified silicone (Note 3) 15 4. Glyceryl Trioctanoate 35 5. Decamethylcyclopentasiloxane 68 6. Dimethyl distearyl ammonium hectorite 12 7. Titanium oxide dispersion (Note 4) 200 8. Zinc oxide dispersion (Note 5) 150 9. Powder E 20 10. Branched polyglycerin-modified silicone (Note 6) 5 11. 1,3-Butylene Glycol 50 12. Sodium citrate 2 13. Sodium Chloride 5 14.Purified water 388 (Note 1) Shin-Etsu Chemical Co., Ltd.: KSG-210 (Note 2) Shin-Etsu Chemical Co., Ltd.: KSG-15 (Note 3) Shin-Etsu Chemical Co., Ltd.: KF-6028P (Note 4) Shin-Etsu Chemical Co., Ltd.: SPD-T6 (Note 5) Shin-Etsu Chemical Co., Ltd.: SPD-Z6 (Note 6) Shin-Etsu Chemical Co., Ltd.: KF-6104 (Manufacturing method) A: Component 10 was dissolved in a portion of component 5, and component 9 was dispersed uniformly. B: Components 1 to 4, the remainder of component 5, components 6 to 8, and component A were mixed uniformly. C: Ingredients 11 to 14 were mixed. D: C was added to B and emulsified to obtain sun-cut cream. The resulting sun-cut cream could be applied evenly, spread easily, and had excellent stability.
[0094] A pressed cheek color was prepared using the powder obtained in the example. [Formulation example 14: Pressed cheek color] (Ingredients) Mixing ratio (g / kg) 1. Acrylic silicone resin treated mica (Note 1) 120 2. Silicone-treated talc (Note 2) 721 3. Red No. 202 3 4. Yellow Iron Oxide 25 5. Black iron oxide 3 6. Silicone-treated pigment-grade titanium dioxide (Note 2) 5 7. Powder C 3 8. Phenyl-modified hybrid silicone composite powder (Note 3) 20 9. Dimethylpolysiloxane (6mm 2 / sec(25℃)) 50 10. Vaseline 20 11. Polyethylene wax 30 (Note 1) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KP-574 (Note 2) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-9909 (Note 3) Shin-Etsu Chemical Co., Ltd.: KSP-300 (Manufacturing method) A: Components 1 to 8 were dispersed evenly. B: Ingredients 9 to 11 were mixed together under heating. C: B was added to A and mixed uniformly, and the mixture was press-molded into a metal plate to obtain a pressed cheek color. The pressed cheek color obtained spread easily, was free from any squeaking, and had excellent stability.
[0095] The powder obtained in the example was used to prepare a loose powder. [Formulation example 15: Loose powder] (Ingredients) Mixing ratio (g / kg) 1. Talc residue 2. Powder B10 3. Amihope (registered trademark) LL 30 4.PMMA (10μm) (Note 1) 80 5. Preservatives (appropriate amount) 6. Appropriate amount of coloring material 7. Squalane 10 8. Antioxidants (appropriate amount) 9.Fragrance (appropriate amount) (Note 1) Matsumoto Yushi Pharmaceutical Co., Ltd.: Matsumoto Microsphere S-100 (Manufacturing method) A: Ingredients 1 to 7 were mixed and ground. B: A was transferred to a Henschel mixer, and ingredients 8 and 9 were added and mixed until homogeneous. C: B was pulverized using an atomizer and packed to obtain loose powder. The obtained loose powder spreads smoothly and smoothly upon application, and furthermore, due to its adequate covering power, it does not produce a whitish cast even after application, giving a natural impression.
[0096] A lipstick was prepared using the powder obtained in the example. [Formulation example 16: Lipstick] (Ingredients) Mixing ratio (g / kg) 1. Ceresin 120 2. Carnauba wax 10 Glyceryl 3.2-ethylhexanoate 140 4. Mineral oil 150 5. Hydrogenated Polyisobutene 200 6. Methylphenylpolysiloxane 200 7. Octyldodecyl Resinoleate 50 8. Red No. 202 10 9. Powder D 40 10. Titanium Mica 30 11. Antioxidant (appropriate amount) 12. Preservatives (appropriate amount) (Manufacturing method) A: Ingredients 1 to 12 were heated and mixed together and stirred until homogenous. B: After degassing A, it was poured into a mold and rapidly cooled to obtain a lipstick. The lipstick obtained had a moderate spreadability and a natural color.
[0097] Lip colors were prepared using the powders obtained in the examples. [Formulation example 17: Lip color] (Ingredients) Mixing ratio (g / kg) 1. Dextrin palmitate 80 Glyceryl 2,2-ethylhexanoate 140 3. Methylphenylpolysiloxane residue 4. Octyldodecyl Resinoleate 150 5. Hydrogenated Polyisobutene 200 6. Mineral oil 300 7. Red No. 202 1 8. Titanium Mica 10 9, Powder C 5 10. Preservatives (appropriate amount) 11. Antioxidant (appropriate amount) (Manufacturing method) A: Ingredients 1 to 11 were heated and mixed together and stirred until homogenous. B: After degassing A, the mixture was poured into a suitable container and gradually cooled to room temperature to obtain a lip color. The lip color obtained had excellent gloss and moderate thickness, and also had a natural color.
[0098] Lip gloss was prepared using the powder obtained in the example. [Formulation example 18: Lip gloss] (Ingredients) Mixing ratio (g / kg) 1. Palmitic acid dextrin 100 2. Diisostearyl Malate 450 3. Liquid paraffin (500cs) 436 4. Preservatives 1 5. Antioxidant 1 6. Mica Titanium 1 7. Aluminum powder 1 8. Powder E 10 (Manufacturing method) A: Components 1 to 5 were heated to 85°C and dissolved uniformly. B: Add ingredients 6 to 8 to A and disperse evenly. C: B was filled into a container at a high temperature and then rapidly cooled to room temperature to obtain a lip gloss. The lip gloss obtained was stable over time and had a natural color.
[0099] An eyeliner was prepared using the powder obtained in the example. [Formulation Example 19: Eyeliner] (Ingredients) Mixing ratio (g / kg) 1. Black iron oxide 70 2. Powder A 50 3. Vinyl acetate resin emulsion 455 4. Concentrated Glycerin 60 5. POE(20) Sorbitan Laurate 18 6. Carboxymethylcellulose (10% aqueous solution) 180 7.Purified water remainder 8. Preservatives 1 9.Fragrance 2 (Manufacturing method) A: Components 5 and 6 were added to component 7, and components 1 to 3 were added to this, followed by treatment in a Mitsui Electric Co., Ltd. colloid mill CM-1. B: Components 4, 8, and 9 were mixed, and A was added at 70°C and dispersed uniformly. The mixture was then cooled and filled to obtain an eyeliner. The resulting eyeliner had excellent makeup durability and color tone.
[0100] Mascara was prepared using the powder obtained in the example. [Formulation Example 20: Mascara] (Ingredients) Mixing ratio (g / kg) 1.Wed 260 2. Polyvinylpyrrolidone 20 3. Butylene Glycol 20 4. 1% cationized cellulose aqueous solution 100 5. Bentonite 5 6. Triethanolamine 17 7. Talc 27 8. Powder E 10 9. Yellow Iron Oxide 9 10. Bengala 9 11. Black Iron Oxide 48 12. Carnauba Wax 55 13. Beeswax 90 14. Stearic Acid 20 15. Self-emulsifying glyceryl stearate 20 16. Propylene Glycol Stearate 20 17. Hydrogenated polyisobutene 20 18. Cyclomethicone 40 19. Preservatives (appropriate amount) 20. Antioxidant (appropriate amount) 21. Resin emulsion 200 (Manufacturing method) A: Ingredients 7 to 11 were mixed in a Henschel mixer. B: Components A was added to components 1 to 6 and dispersed uniformly using a stirrer. C: In a separate container, ingredients 12 to 20 were heated and dissolved. D: C was added to B and emulsified, then cooled to 40°C, component 21 was added, and cooled to room temperature to obtain a mascara. The resulting mascara had a moderate gloss, adhered well to the eyebrows, lasted well, and had excellent color tone.
[0101] A cream eye shadow was prepared using the powder obtained in the example. [Formula Example 21: Cream eyeshadow] (Ingredients) Mixing ratio (g / kg) 1. Acrylic silicone resin melt product (Note 1) 100 2. Stearyl-modified acrylic silicone resin (Note 2) 20 3. Branched polyether-modified silicone (Note 3) 15 4. Decamethylcyclopentasiloxane 203 5. Isotridecyl isononanoate 30 6. Dimethyl distearyl ammonium hectorite 12 7. Acrylic silicone resin treated pigment (Note 4) 100 8. Powder D 100 9. Spherical nylon 30 10. Talc 40 11. Ethanol 50 12.Purified water 300 (Note 1) Shin-Etsu Chemical Co., Ltd.: KP-545 (Note 2) Shin-Etsu Chemical Co., Ltd.: KP-561P (Note 3) Shin-Etsu Chemical Co., Ltd.: KF-6028P (Note 4) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KP-574 (Manufacturing method) A: Components 1 to 6 were mixed, and then components 7 to 10 were added and mixed until uniformly dispersed. B: Ingredients 11 and 12 were mixed. C: B was added to A and emulsified to obtain a cream eyeshadow. The resulting cream eye shadow spread easily, was not rough, and had excellent stability.
[0102] An eye shadow was prepared using the powder obtained in the example. [Formulation example 22: Eye shadow] (Ingredients) Mixing ratio (g / kg) 1. Silicone-treated talc (Note 1) 365 2. Powder B 90 3. Boron nitride 90 4. Titanium Mica 347 5. Dimethicone 1000cs 50 6. Red No. 202 5 7. Neopentyl glycol dioctanoate 10 8. Squalane 40 9. Preservatives (appropriate amount) 10. Antioxidant (appropriate amount) (Note 1) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KF-99P (Manufacturing method) A: Ingredients 1 to 5 were mixed and ground. B: A was transferred to a Henschel mixer, and ingredients 6 to 10, which had been mixed separately, were added and mixed until homogenous. C: B was pulverized using an atomizer and pressed into an aluminum dish to obtain eyeshadow. The resulting eye shadow was excellent in makeup durability, color tone, and usability.
[0103] Nail enamel was prepared using the powder obtained in the example. [Formulation Example 23: Nail Enamel] (Ingredients) Mixing ratio (g / kg) 1. Nitrocellulose (1 / 2 sec) 100 2. Modified alkyd resin 100 3. Acetyltributyl citrate 50 4. Butyl acetate 149 5. Ethyl acetate 195 6. Ethanol 50 7. Toluene 340 8. Ultramarine 5 9. Powder D 1 10. Organically modified montmorillonite 10 (Manufacturing method) A: Ingredients 8 and 9 were dissolved in a portion of ingredients 2 and 3, and the mixture was thoroughly mixed. B: Components 1, 4 to 7, and 10 were added to the remainder of components 2 and 3 in A, mixed, and filled into a container to obtain nail enamel. The nail enamel obtained had excellent stability over time and excellent color tone.
[0104] The powder obtained in the example was used to prepare a solid polyhydric alcohol-in-oil emulsified blush. [Formulation Example 24: Solid oil-based polyhydric alcohol emulsified cheek blush] (Ingredients) Mixing ratio (g / kg) 1. Cross-linked polyglycerin-modified silicone (Note 1) 30 2. Cross-linked dimethylpolysiloxane (Note 2) 50 3. Decamethylcyclopentasiloxane 180 4. Dimethylpolysiloxane (6mm 2 / sec(25℃)) 216 5. Cetyl isooctanoate 50 6. Behenyl-modified acrylic silicone resin (Note 2) 30 7. Paraffin wax (melting point 80℃) 90 8. Dimethyl distearyl ammonium hectorite 2 9. Powder A 100 10. Acrylic silicone treated purple No. 401 (Note 3) 50 11. Acrylic silicone treated black iron oxide (Note 3) 2 12. Acrylic silicone treated mica (Note 3) 50 13. Preservatives (appropriate amount) 14.Fragrance (appropriate amount) 15. 1,3-Butylene Glycol 145 (Note 1) Shin-Etsu Chemical Co., Ltd.: KSG-710 (Note 2) Shin-Etsu Chemical Co., Ltd.: KSG-15 (Note 3) Surface treated with Shin-Etsu Chemical Co., Ltd.'s KP-562P (Manufacturing method) A: Components 1 to 8 were heated to 80°C and mixed uniformly. B: Ingredients 9 to 12 were mixed uniformly, added to A, and dispersed uniformly. C: Ingredients 13 and 15 were mixed and heated to 80°C. D: C was added to B and emulsified, then ingredient 14 was added and the mixture was poured into a metal dish and cooled to obtain a solid polyhydric alcohol-in-oil emulsified blush. The obtained solid polyhydric alcohol-in-oil emulsified cheek rouge spread easily and lasted well.
[0105] A blush was prepared using the powder obtained in the example. [Prescription Example 25: Cheek rouge] (Ingredients) Mixing ratio (g / kg) 1. Talc Residue 2. Sericite 609 3. Fine particle titanium dioxide 30 4. Powder C 20 5. Coloring agent (appropriate amount) 6. Ethylhexyl methoxycinnamate 30 7. Octyl Palmitate 50 8. Preservatives (appropriate amount) 9. Antioxidants (appropriate amount) (Manufacturing method) A: Components 6 to 9 were heated and dissolved. B: Components 1 to 5 were mixed in a Henschel mixer, and then A was mixed therewith. C: B was crushed using an atomizer and molded into a medium dish to obtain cheek rouge. The resulting cheek rouge spread smoothly and had a natural color when applied.
[0106] A cream lipstick was prepared using the powder obtained in the example. [Formulation example 26: Cream lipstick] (Ingredients) Mixing ratio (g / kg) 1. Palmitic acid / ethylhexanoic acid dextrin (Note 1) 90 2. Dipolyglyceryl triisostearate 100 3. Glyceryl Trioctanoate 80 4. Alkyl-modified cross-linked dimethylpolysiloxane (Note 2) 80 5. Alkyl-modified branched polyglycerin-modified silicone (Note 3) 20 6. Decamethylcyclopentasiloxane 395 7. 1,3-Butylene Glycol 50 8.Purified water remainder 9. Red No. 201 Appropriate amount 10. Red No. 226 Appropriate amount 11. Yellow No. 4 Appropriate amount 12. Powder B appropriate amount 13. Mica (appropriate amount) 14.Fragrance (appropriate amount) (Note 1) Chiba Flour Mills: Leopard (registered trademark) TT (Note 2) Shin-Etsu Chemical Co., Ltd.: KSG-43 (Note 3) Shin-Etsu Chemical Co., Ltd.: KF-6105 (Manufacturing method) A: Components 9 to 12 were mixed with a portion of component 2, and the mixture was dispersed using an Imex three-roll mill BR-100VIII. B: Components 1, the remainder of 2, and 3 to 6 were heated and mixed uniformly. C: A was added to B and mixed uniformly. D: Ingredients 7 and 8 were mixed and heated, then added to C and emulsified. E: Components 13 and 14 were added to D to obtain a cream lipstick. The resulting creamy lipstick spread easily and smoothly on the lips, was moist and did not dry out, did not cast a white cast or smudge, and had good makeup wear.
[0107] A facial cleanser was prepared using the powder obtained in the example. [Prescription Example 27: Facial Cleanser] (Ingredients) Mixing ratio (g / kg) 1. Lauric Acid 30 2. Myristic acid 90 3. Palmitic acid 80 4. Stearic Acid 100 5. Glycerin 150 6. 1,3-Butylene Glycol 70 7. Glyceryl Stearate 15 8. Preservatives 2 9. Chelating Agent 1 10.Water Residual 11. Potassium hydroxide 60 12. Cocamidopropyl Betaine 33 13. Potassium Cocoyl Glycinate 30 14. Glycosyltrehalose 45 15.Powder C 15 (Manufacturing method) A: Components 1 to 9 were mixed and heated to dissolve. B: Components 10 and 11 were weighed into a separate container and added to A, followed by saponification. C: Components 12 to 15 were added to B, mixed uniformly with stirring, and then cooled to room temperature. The mixture was then filled into a suitable container to obtain a facial cleanser. The resulting facial cleanser had a uniform white appearance and maintained sufficient cleansing properties.
Claims
1. The aspect ratio is 1.50 or more and 2.00 or less, and the minor axis length D of the particle is 50 The value is 105 nm or more and less than 150 nm, and the average minor axis length b ave (nm) and the standard deviation of the minor axis length σ b (nm) is of the following formula: (b) ave -100) / s b ≧1.3 A powder containing titanium (IV) oxide particles as its main component, which satisfies the above requirements.
2. Average minor axis length of particles b ave (nm) and the standard deviation of the minor axis length σ b (nm) further has the following formula: (150-A) ave ) / s b ≧1.3 The powder according to claim 1 , which satisfies the above.
3. 3. The powder according to claim 1, wherein the particles have a morphology in which rod-like particles are aggregated in a fibrous form.
4. 4. The particle of claim 3, wherein the projection of the particle is approximately ellipsoidal.
5. 3. The powder according to claim 1, wherein the crystalline layer of the titanium(IV) oxide particles is of the rutile type.
6. adding an aliphatic hydroxy acid compound to an acid-soluble titanium compound; Then, hydrochloric acid is added for X (h) to make the hydrochloric acid concentration Y (g / L); Dissolving the acid-soluble titanium compound at Z (°C) after adding hydrochloric acid X, Y, and Z are represented by the following formulas (1) and (2): (1) 2.60≦Y / Z≦3.45 (2)Y 1/2 ×Z / X≦475 The method for producing powder according to claim 1 or 2, which satisfies the above.
7. The method according to claim 6, wherein X is 2.0 or more.
8. 7. The method according to claim 6, wherein the acid-soluble titanium compound is sodium titanate.
9. A cosmetic composition containing the powder according to claim 1 or 2.
Citation Information
Patent Citations
Straw-bundled rutile-type titanium dioxide, cosmetics using the same and external additive for toner using the same
JP2010173863A