JP5341333B2 - Method for producing powder cosmetics - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a process for producing a powdered cosmetic excellent in a feeling of use, particularly makeup durability. <P>SOLUTION: The process for producing a powdered cosmetic includes a slurry preparation step of mixing a powdered component, an oily component as a binder, and an amino modified silicone as a dispersing agent in a volatile solvent to form a slurry, and a drying step of drying the above slurry to obtain a dried powder and obtains a powdered cosmetic from the dried powder, and a drying apparatus 14 to be used in the drying step renders the slurry fine droplets by mechanical shearing force and blows a dry gas against the fine droplets to perform drying of the slurry. <P>COPYRIGHT: (C)2009,JPO&amp;INPIT

Description

  The present invention relates to a method for producing a powder cosmetic, and more particularly to improvement of the cosmetic durability of the powder cosmetic.

  Powder cosmetics represented by powdery foundations, etc. have been conventionally used with agitation mixers such as Henschel mixer (registered trademark), Nauter mixer (registered trademark), ribbon blender, kneader, etc. Etc., and the mixture was crushed with a pulverizer such as a pulverizer, and then filled in a metal or resin inner dish, or further dry press molded. These conventional methods are in the form of dry mixing in which the powder component and a small amount of oily component as a binder are mixed without adding a solvent, and dry molding in which pressure molding is performed in a dry powder state. It is called the dry process and has been used for a long time.

In recent years, various methods relating to mixing and molding have been developed for powder cosmetics in order to improve characteristics such as a feeling of use. For example, wet mixing is performed in which a powder component and an oil component are added to a volatile solvent to form a slurry, and then filled into a container in a slurry state and the solvent is removed by vacuum suction or the like to form a powder (wet molding) Such a method for producing a powder cosmetic is proposed, which is called a wet manufacturing method.
In addition, various devices used in wet mixing in which a powder component and oil are mixed in a volatile solvent have been widely studied. For example, after obtaining a pulverized solution obtained by pulverizing a polymer powder in a volatile solvent using a medium stirring mill, the pulverized solution and a powder such as pigment are mixed in a wet mixer such as a disper to obtain a slurry. A volatile solvent is removed from the resulting slurry to obtain a dry powder, which is further pulverized by a pulverizer and then dry-molded to obtain a solid powder cosmetic (Patent Document 1) or during wet mixing. A medium stirring mill is used. After the obtained slurry is filled in the container, wet molding is performed by suction pressing, or the solvent is removed from the obtained slurry to obtain a dry powder, and the dry powder is further pulverized by a pulverizer, followed by dry molding. The manufacturing method (patent document 2) etc. of the powder solid cosmetics obtained by performing is proposed.

In addition, with the diversification and sophistication of recent user needs, not only satisfaction such as ease of use on puffs and use feeling when applied to the skin, but also productivity and work environment. After further improvement in the aspect of the above, a method for manufacturing powder cosmetics (W & D manufacturing method) obtained by high-dispersion in a wet system using a bead mill and drying fine particles with a flash dryer has been proposed. (Patent Document 3).
Japanese Patent Laid-Open No. 9-30926 Japanese Patent No. 3608778 JP 2007-55990 A

However, the powder cosmetic obtained by the above production method has a good texture that is smooth and uniform while having a moist feeling like a liquid when applied to the skin. However, even though it could be provided as a powder cosmetic for autumn and winter, it could not be applied to a powder cosmetic for spring and summer.
This invention is made | formed in view of the said subject, The objective is to provide the manufacturing method for manufacturing the powder cosmetics excellent in use feeling, especially makeup lasting.

［Ａは−Ｒ^２ＮＨ_２もしくは−Ｒ^２ＮＨＲ^３ＮＨ_２（ここでＲ^２及びＲ^３は炭素数１〜８のアルキレン基である）であり、Ｒ^１は炭素数１〜３０のアルキル基、シクロアルキル基、アリール基、アラルキル基、およびフッ素置換アルキル基からなる群より互いに独立に選択される基であり、ｍは５０＜ｍ＜４００の整数、及びｎは１＜ｎ＜２０の整数であり、ｓ及びｔは互いに独立に０〜３の整数である。］
In order to achieve the above object, the present inventors paid attention to a component (dispersant) that has a high possibility of adsorbing to the powder, and as a result of intensive studies, the dispersant has high water and oil repellency during the wet high dispersion process. It was found that a powdered cosmetic material having a long-lasting makeup compared with products manufactured by a conventional method can be obtained by adding a dry powder.
That is, in the method for producing a powder cosmetic of the present invention, a powder component, an oily component as a binder, and an amino-modified silicone represented by the following general formula (1) as a dispersant are mixed in a volatile solvent to form a slurry. a slurry preparation step of, and a drying step to obtain a dry powder by drying the slurry, a method of producing a powder cosmetic to obtain a powder cosmetic from said dry powder, drying apparatus used in the drying step, the slurry was fine liquid droplets by a mechanical shearing force, Ri drying apparatus der of drying the slurry by blowing drying gas into the fine droplets, the amino-modified silicone 0.1 to 5.0 A powder cosmetic containing mass% is obtained .

[A is -R ² NH ₂ or -R ² NHR ³ NH ₂ (where R ² and R ³ are alkylene groups having 1 to 8 carbon atoms), and R ¹ is an alkyl group having 1 to 30 carbon atoms. , A cycloalkyl group, an aryl group, an aralkyl group, and a fluorine-substituted alkyl group, each independently selected from the group consisting of m, an integer of 50 <m <400, and n is an integer of 1 <n <20 S and t are integers of 0 to 3 independently of each other. ]

[式（２）において、ｍは５０＜ｍ＜４００の整数、及びｎは１＜ｎ＜２０の整数である。]
In the above production method, the amino-modified silicone is preferably an aminoethylaminopropylmethylsiloxane / dimethylsiloxane copolymer represented by the following general formula (2).

[In Formula (2), m is an integer of 50 <m <400, and n is an integer of 1 <n <20 . ]

In the above manufacturing method, the drying apparatus used in the drying step includes a hollow casing, a shearing means for shearing slurry by a shearing member provided in the casing to form microdroplets, Supplying means for supplying slurry to the shearing member, blowing means for blowing dry gas into the housing, supplying dry gas to the slurry made into fine droplets by the shearing means, and drying the slurry It is preferable that the drying apparatus includes a collecting unit that collects the dry powder generated by doing so.
In the above production method, in the slurry preparation step, a powder component and an oil component are mixed in a volatile solvent using a medium stirring mill, and the powder component is crushed and / or pulverized and / or dispersed. It is preferable to obtain a slurry.

In the above production method, a powder component other than the pearl pigment is obtained as a dry powder by the slurry adjusting step and the drying step, and a powder cosmetic is obtained using a powder obtained by mixing the dry powder and the pearl pigment. Is preferred.
In the above production method, it is preferable to further include a solidification step of filling a container with the dry powder and / or the powder obtained by mixing the dry powder and the pearl pigment, and solidifying by dry molding.

According to the method for producing a powder cosmetic according to the present invention, since the amino-modified silicone as a dispersant is added and mixed in the slurry adjustment step, it is possible to obtain a powder cosmetic with a long makeup.

Hereinafter, preferred embodiments according to the present invention will be described. FIG. 1 is a diagram showing an example of a device configuration used in a manufacturing method according to an embodiment of the present invention. The method for producing a powder cosmetic according to the present embodiment comprises a slurry preparation step in which a powder component, an oily component as a binder, and an amino-modified silicone as a dispersant are mixed in a volatile solvent to form a slurry, and the slurry is dried. And a drying step of obtaining a dry powder.
First, in the slurry adjustment step, the powder component, the oil component and the amino-modified silicone are mixed in a volatile solvent using the medium stirring mill 10 shown in FIG. 1, and the powder component is crushed / ground / dispersed. A slurry is obtained. The obtained slurry is temporarily stored in the storage tank 12 and supplied to the drying device 14 at a predetermined flow rate.

The drying device 14 used in the present embodiment makes the slurry fine droplets by mechanical shearing force, that is, shearing force generated by rotation of shearing members (plate-like members 34a, 34b, 34c) provided in the shearing means 18. The slurry is dried by blowing a dry gas to the fine droplets. The shape of the shearing member is not particularly limited as long as it meets the purpose of the present invention. For example, the shape of the shearing member may be any shape such as a blade shape or a disk shape in addition to the plate shape as described above. .
Thus, in this embodiment, since dry powder is manufactured using the drying apparatus 14 which dries in the state which made the slurry into the fine droplet, the dry powder which hardly agglomerates the powder component at the time of drying is obtained. Can do. Therefore, it is possible to provide a powder cosmetic that is excellent in use feeling when applied to the skin. Moreover, since it is not necessary to crush again after drying, it is excellent in productivity and work environment.

It is also preferable to further include a step of filling the obtained dry powder into a container and solidifying by dry press molding. The obtained solid powder cosmetics are excellent not only in the feeling of use but also in the usability such as how to puff.
Moreover, as shown in FIG. 1, in the slurry preparation process, it is preferable to use a medium stirring mill 10 in order to mix the powdered oil component and the oil component as a binder in a volatile solvent. By using a medium stirring mill, it is possible to obtain a slurry in which the oil component is cleanly coated on the surface of the powder component, and by using the slurry, a powder cosmetic with even more excellent use feeling and usability can be obtained. .

Furthermore, when manufacturing a powder cosmetic containing a pearl pigment, first, a slurry is prepared using powder components other than the pearl pigment in the slurry preparation step, and in the drying step, this slurry is dried to dry without containing the pearl pigment. Obtain a powder. And it is suitable to mix a pearl pigment and the dry powder which does not contain a pearl pigment, and to obtain a powder cosmetic using this mixed powder. By adopting such a production method, a powder cosmetic excellent in pearl feeling can be obtained.
The above is the outline of the method for producing a powder cosmetic according to the present invention, and each step will be described in detail below.

<Slurry preparation process>
Examples of the method for mixing the powder component and the oil component in a volatile solvent to form a slurry include the following methods.
(A) Powder and oil previously dry-mixed / pulverized with a Henschel mixer (registered trademark) or pulverizer, etc. are added to a volatile solvent, and a disper mixer, a homogenizer, a planetary mixer, a twin-screw kneader, etc. By mixing / dispersing method.
(B) A method in which powder and oil are added to a volatile solvent and, if necessary, premixed with a disper mixer or the like, and then pulverized / ground / dispersed with a medium stirring mill.
(C) A partly specific powder component having strong cohesive properties such as polymer elastic powder and fine particle powder is added to a volatile solvent. If necessary, this is premixed with a disper mixer or the like, and then a medium stirring mill is used. A dispersion is obtained by pulverizing / pulverizing / dispersing, adding the dispersion and other powdered oil, and further using a wet mixer or a medium stirring mill.
In addition, it is suitable to use a medium stirring mill in the slurry preparation step (for example, (B) and (C) above). The medium agitation mill is a medium in which a dispersion liquid composed of a powder component (and an oil component) and a solvent is contained in a container filled with a solid dispersion medium (medium) such as beads and the liquid in the container is agitated. The powder component is crushed / pulverized / dispersed by impact force, frictional force, and the like.

2 and 3 are schematic configuration diagrams showing examples of a medium stirring mill preferably used in the present invention. The medium agitating mill that can be suitably used in the present invention is not particularly limited to the following, and any medium stirring mill may be used as long as the object of the present invention can be achieved.
The medium stirring mill 110 in the example shown in FIG. 2 is attached to a substantially cylindrical container 112, a drive shaft 114 inserted into the container 112, a drive motor 116 that rotationally drives the drive shaft 114, and the drive shaft 114. A plurality of stirring disks 118a to 118f. The inside of the container 112 is divided into a dispersion chamber 120 for crushing / pulverizing / dispersing the powder component and an extraction chamber 122 for extracting the treated dispersion liquid. A supply port 124 for supplying the dispersion liquid to be treated is provided on the dispersion chamber 120 side of the container 112, and an extraction port 126 for taking out the treated dispersion liquid is provided on the extraction chamber 122 side. A partition wall 130 having an opening 128 is provided between the dispersion chamber 120 and the extraction chamber 122, and a separation disk 132 attached to the drive shaft 114 is disposed in the vicinity of the partition wall 130. 128 is disposed so as to cover 128. A gap is provided between the partition wall 130 and the separation disk 132, and this gap is used as a separation slit 134 for separating the solid dispersion medium and the dispersion liquid to be treated.

The dispersion liquid containing the powder component and the solvent is sequentially supplied from the supply port 124 to the dispersion chamber 120 in the container 112, and the dispersion liquid in the dispersion chamber 120 sequentially moves toward the extraction chamber 122. At this time, the drive shaft 114 is rotationally driven by the drive motor 116, and the stirring disks 118a to 118f are rotating. The dispersion chamber 120 is filled with a large number of solid dispersion media 136, and the solid dispersion media 136 are stirred together with the dispersion by the rotation of the stirring disks 118a to 118f. The agglomerated powder component in the dispersion is crushed / pulverized / dispersed by impact force or shear stress from the solid dispersion medium 136.
The pulverized / ground / dispersed dispersion liquid passes through the separation slit 134 between the partition wall 130 and the separation disk 132 between the dispersion chamber 120 and the extraction chamber 122 and flows into the extraction chamber 122. , Extracted from the extraction port 126 to the outside. The separation slit 134 is sized so that the solid dispersion medium 136 does not flow out of the dispersion chamber 120 into the extraction chamber 122. Therefore, when the dispersion liquid passes through the separation slit 134, the dispersion liquid (powder component + solvent) and the solid dispersion medium 136 are separated, and only the dispersion liquid enters the extraction chamber.

  FIG. 3 is a schematic configuration diagram of an annular type medium stirring mill. The medium agitating mill 210 shown in FIG. 3 includes a container 212 having a substantially W-shaped cross section that is symmetric with respect to the central axis A, and a substantially inverted U-shaped rotor that is provided in the container 212 and is rotatable about the central axis A. 214 and a drive motor 216 that rotationally drives the rotor 214. An annular space 218 is formed between the inner surface of the container 216 and the outer surface of the rotor 214, and the annular space 218 has a shape having a substantially V-shaped cross section on both sides of the central axis A. Further, the container 212 is formed with a supply port 220 for sending the dispersion liquid (powder component + solvent) to be processed into the annular space 218 and an extraction port 222 for taking out the treated dispersion liquid from the annular space 218. Yes. The annular space 218 is filled with a solid dispersion medium 224, and the annular space 218 is used as a dispersion chamber for crushing / pulverizing / dispersing the powder components in the dispersion.

The dispersion supplied from the supply port 220 is sent to the annular space 218 through the inlet slit 226. The fed dispersion liquid moves in the annular space 218 and is taken out from the extraction port 222 through the outlet slit 228. At this time, by rotating the rotor 214 around the central axis A in the annular space 218, the dispersion liquid and the solid dispersion medium 224 in the annular space 218 are agitated. Then, the agglomerated powder component in the dispersion is crushed / pulverized / dispersed by the impact force or shear stress from the solid dispersion medium 224. Thereafter, the dispersion passes through the exit slit 228 and is taken out from the extraction port 222.
The exit slit 228 has such a size that the solid dispersion medium 224 does not flow out of the annular space 218, and functions as a separation means for separating the dispersion (powder component + solvent) from the solid dispersion medium 224. In addition, the rotor 214 is provided with a return hole 230 for returning the solid dispersion medium 224 to the inlet side so that the solid dispersion medium 224 does not stay near the outlet.

The reason for crushing / pulverizing / dispersing the powder and oil in a volatile solvent using a medium stirring mill is that the mixing / dispersing state of the powder component and the oil component can be increased, and the surface of the powder component can be uniformly distributed This is because the oily component can be coated, so that a powder cosmetic with a good feel to use can be obtained. It is also possible to easily pulverize a highly cohesive powder and disperse it uniformly in a volatile solvent.
Examples of the medium agitating mill include, in addition to those described above, a batch type bead mill such as a basket mill, a horizontal type, a vertical type, an annular type continuous type bead mill, a sand grinder mill, a ball mill, and Micros (registered trademark). And the like can be used without any particular limitation as long as they meet the object of the present invention. That is, when blending powder components in an agglomerated state, there is no particular limitation as long as the powder components can be agglomerated to stir and disperse to a state close to primary particles and the oily component can be uniformly attached to the powder surface Can be used.

  The medium used in the medium agitating mill is preferably beads, and beads made of glass, alumina, zirconia, steel, flint stone and the like can be used, and zirconia is particularly preferable. Further, as the size of the beads, those having a diameter of about 0.5 to 10 mm are usually preferably used, but those having a diameter of about 2 mm to 5 mm are preferably used in the present invention. If the bead diameter is too small, crushing of extender pigments such as mica and talc will proceed excessively, adversely affecting the feel of use, and the hardness after molding will become difficult to remove, caking etc. It becomes easy to cause. On the other hand, if the size of the beads is too large, the aggregation of the powder component cannot be sufficiently solved, and it becomes difficult to uniformly coat the oil component.

The volatile solvent used in the present invention is not particularly limited, but purified water, cyclic silicone, ethanol, light liquid isoparaffin, lower alcohol, ethers, LPG, fluorocarbon, N-methylpyrrolidone, fluoroalcohol, volatile linear chain Silicone, next-generation chlorofluorocarbon, and the like. One or more of these solvents can be mixed and used appropriately according to the characteristics of the powder component to be used and the characteristics of the oil component.
In the slurry preparation step, the amount ratio (mass ratio) of the powder component to the oil component depends on the oil component used and the type of the powder component, but the powder component / oil component = 60/40 to 99.5 / 0. .5 is preferred. In addition, the amount of the volatile solvent used at this time depends on the polarity and specific gravity of the volatile solvent to be used, and thus cannot be specified, but it is important to ensure fluidity that enables processing with a medium stirring mill. It is.

<Drying process>
Next, an example of a drying apparatus used in the drying process of the manufacturing method according to the embodiment of the present invention will be described with reference to FIG. Note that the drying apparatus used in the manufacturing method according to the present embodiment is not limited to that shown in FIG. 1, and may be any apparatus provided with shearing means for mechanically turning the slurry into fine droplets. The drying device 14 shown in FIG. 1 is configured such that a slurry is dried by a hollow casing 16 serving as a place for drying the slurry and a rotating shearing member (plate-shaped members 34a, 34b, 34c) provided in the casing 16. Shearing means 18 for forming fine droplets, supply means 20 for supplying slurry to the shearing members (plate-like members 34a, 34b, 34c) in the casing 16, and dry gas is blown into the casing 16 to shear the means. 18 is provided with a blowing means 22 for supplying a drying gas to the slurry made into fine droplets by 18 and a collecting means 24 for collecting the dry powder generated by drying the slurry.

The casing 16 has a vertical, hollow, and substantially cylindrical shape, and has a discharge port 26 that discharges dry powder and dry gas at the top, and a blower that supplies dry gas from the blowing means 22 into the casing 16 at the bottom. A mouth 28 is provided. Further, the supply port 30 for supplying the slurry into the housing 16 is located between the discharge port 26 located at the top of the housing 16 and the blower port 28 located at the bottom.
The shearing means 18 rotates the rotary shaft 32 provided in the vertical direction from the bottom of the housing 16, shear members (plate-like members 34 a, 34 b, 34 c) provided at right angles to the rotary shaft 32, and the rotary shaft 32. And a drive unit 36. The drive unit 36 is disposed outside the housing 16 and transmits a rotational force to the shearing members (plate-like members 34a, 34b, 34c) via the rotation shaft 32. The shearing member shown in FIG. 1 is configured by three plate-like members 34a, 34b, and 34c provided at right angles to the rotation shaft 32 at intervals in the vertical direction. These shear members are located below the slurry supply port 30 and above the dry gas blowing port 28. By rotating the rotating shaft 32 by the drive unit 36 constituted by a motor or the like, the plate-like members 34a, 34b, 34c rotate in the horizontal direction around the rotating shaft 32 in the housing 16, and this mechanical shearing is performed. The slurry is made into fine droplets by force.

The supply means 20 supplies the slurry sent from the storage tank 12 into the housing 16. The slurry supplied into the housing 16 falls toward the plate-like members 34a, 34b, and 34c, and is made into fine droplets by the rotating plate-like members 34a, 34b, and 34c. Further, the dry gas sent from the blowing means 22 is blown into the housing 16 from the blower port 28. Since the dry gas is supplied toward the tangential direction of the horizontal section of the casing 16 and the plate members 34a, 34b, and 34c are rotating, the dry gas flow blown into the casing 16 swirls. It becomes a flow. When the slurry in the form of fine droplets comes into contact with this dry gas flow, the slurry is further refined and dried to form a dry powder. The dry powder is blown up to the upper part of the housing 16 together with the dry gas flow, and is discharged from the discharge port 26. The dry powder discharged out of the casing 16 from the discharge port 26 is collected by the collecting means 24.
A classifying means 38 is provided at the portion of the discharge port 26 in the housing 16. The classifying means 38 is configured as an orifice provided in the discharge port 26, and prevents large particles, lumps, undried products, etc. from entering the collecting means 24. Note that the configuration of the classification means is not limited to this, and other configurations may be used.

Thus, by giving mechanical shearing force to the slurry by the shear members (plate-like members 34a, 34b, 34c) and drying the slurry in the form of fine droplets, a dry powder with less aggregation can be obtained. it can. The reason why the dry powder has less agglomeration is that fine droplets reduce the amount of powder components present in the droplets, so that aggregation during drying is less likely to occur, and aggregation of powder components that occurs during the drying process It may be solved by a shearing force caused by a shearing member or a swirling flow.
Here, as the shearing member, a member constituted by a plate-like member rotating in the horizontal direction is shown, but in addition to this, a member constituted by a plate-like member rotating in the vertical direction (rotating shaft in the horizontal direction) is also provided. May be. Further, the shape of the shearing member is not limited to the above-described one, and examples thereof include a blade shape (such as a rod member perpendicular to the rotation axis provided with a cutter perpendicularly), a disk shape, and the like. Also, the number of shear members is not particularly limited.

The above-mentioned drying apparatus is of a type called a flash dryer. For example, a spin flash dryer manufactured by APV Nordic Anhyro, a dry meister manufactured by Hosokawa Micron, a vertical stirring dryer manufactured by Tsukishima Kikai Co., Ltd. Is mentioned. The drying apparatus suitably used in the present invention is not limited to this, and any system having a shearing mechanism in the system may be used, and any of a vertical type and a horizontal type may be used.
Further, the temperature of the drying gas used for drying can be changed depending on the boiling point of the volatile solvent used. In addition, since the drying efficiency increases as the temperature of the drying gas increases, it is desirable to set the temperature to a high temperature within a range that does not adversely affect the modification of the dry powder constituents by heat.
In addition, since an inert gas such as nitrogen gas or Ar gas is sealed in the housing 16, the explosion resistance is improved, so that the work environment is improved. In addition, the solvent can be recovered by incorporating a solvent recovery mechanism such as a condenser.

<Solidification process>
In the method for producing a powder cosmetic according to an embodiment of the present invention, it is preferable that the method further includes a solidification step of filling a dry powder into a container and solidifying the powder by dry molding. As the solidification method, a conventionally known dry press molding or the like may be used. The powdered solid cosmetic thus obtained also has good usability (adhesiveness to puff), which is an advantage of dry molding, while maintaining the excellent feeling of use that is an advantage of the wet manufacturing method. In addition, in the case of conventional wet molding including a step of filling a slurry into a container by injection filling, since it is necessary to consider the filling properties of the slurry, there are limitations on the raw materials to be used, but normal dry press molding is performed As long as there is no limitation on the raw materials used, there is an advantage.
Moreover, the blending amount of the dry powder when obtaining the powder cosmetic is preferably 0.5 to 100 parts by weight, more preferably 30 to 100 parts by weight with respect to 100 parts by weight of the cosmetic.

  Furthermore, when creating powder cosmetics to which pearl pigments typified by titanium mica and glass pearls are added, first of all, using the powder component of the portion other than the pearl pigments, the slurry preparation step and the drying step are performed. A dry powder is obtained. This dry powder and the required amount of pearl pigment are mixed in a dry mixer with low shearing force such as a Henschel mixer or Nauter mixer to make a mixed powder, and the mixed powder is filled into a container or further dry-molded to make a powder makeup. Get a fee. The powder cosmetic obtained by this method is not only excellent in use feeling and usability, but also excellent in pearl feeling.

  The pearl pigment used in the present invention is not particularly limited, and those commonly used in conventional cosmetics can be used. Typical examples include mica titanium, iron oxide-coated mica titanium, low-order titanium oxide-coated mica titanium, photochromic titanium mica, talc instead of mica as a substrate, glass, synthetic fluorine phlogopite, silica, oxychloride The thing using bismuth etc. is mentioned. Furthermore, examples of the covering include low-order titanium oxide, iron oxide, alumina, silica, zirconia, zinc oxide, cobalt oxide, and aluminum in addition to titanium oxide. Further, as functional pearl pigments having excellent optical properties, pearl pigment surfaces coated with resin particles (JP-A-11-92688), pearl pigment surfaces coated with aluminum hydroxide particles (JP 2002-2002) 146238), a pearl pigment surface coated with zinc oxide particles (JP 2003-261421), a pearl pigment surface coated with barium sulfate particles (JP 2003-61229), and the like. Functional pearl pigments in which the surface of these pearl pigments is coated with various particles tend to be easily lost when a strong force is applied to the coated particles. However, according to the above method, since the pearl pigment is applied only when it is mixed with the dry powder, it is not necessary to mix with a very strong force, and the particles coated with the pearl pigment may be lost. Is small. Therefore, according to said manufacturing method, it can mix | blend with powder cosmetics, without impairing the function of a functional pearl pigment.

  The production method according to the present invention is suitably applied to powdered or solid powder cosmetics such as foundations, eye shadows, teak colors, body powders, perfume powders, baby powders, pressed powders, deodorant powders, and candy. .

  In the powder cosmetics produced by the production method according to the present invention, other components usually used for external preparations for skin such as cosmetics and pharmaceuticals, for example, amino-modified silicone, powder components, within the range not impairing the effects of the present invention. Liquid fats, solid fats, waxes, hydrocarbons, higher fatty acids, higher alcohols, esters, anionic surfactants, cationic surfactants, amphoteric surfactants, nonionic surfactants, humectants, water-soluble polymers, thickening Agent, film agent, ultraviolet absorber, sequestering agent, lower alcohol, polyhydric alcohol, sugar, amino acid, organic amine, polymer emulsion, pH adjuster, skin nutrient, vitamin, antioxidant, antioxidant aid , Fragrance, water and the like can be appropriately blended as necessary, and can be produced by conventional methods according to the intended dosage form. Specific ingredients that can be blended are listed below, but a powder cosmetic can be prepared by blending the above-mentioned essential blending ingredients and any one or more of the following ingredients.

[式１において、Ａは−Ｒ^２ＮＨ_２もしくは−Ｒ^２ＮＨＲ^３ＮＨ_２（ここでＲ^２及びＲ^３は炭素数１〜８のアルキレン基である）であり、
Ｒ^１は炭素数１〜３０のアルキル基、シクロアルキル基、アリール基、アラルキル基、およびフッ素置換アルキル基からなる群より互いに独立に選択される基であり、
ｍは５０＜ｍ＜４００の整数、及びｎは１＜ｎ＜２０の整数であり、ｓ及びｔは互いに独立に０〜３の整数であり、ただし、１≦ｎ＋ｓ＋ｔである。]
上記Ｒ^１の例としては、メチル基、エチル基、プロピル基、ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、ノニル基、デシル基等のアルキル基、シクロペンチル基、シクロヘキシル基等のシクロアルキル基、トリフロロプロピル基、ヘプタデカフロロン基等のフッ素置換アルキル基で表される有機基などを挙げることができる。好ましくは、メチル基、フェニル基、トリフロロプロピル基である。
また、Ｒ^２及びＲ^３の例としては、メチル基、エチレン基、プロピレン基、ブチレン基、ペンチレン基等を挙げることができ、好ましくは、メチレン基、エチレン基、プロピレン基である。
Examples of amino-modified silicones include those in which an amino group is grafted to the silicone main chain, those having an amino group added to one end of the silicone main chain, those having an amino group added to both ends of the silicone main chain, silicone main chain And those having an amino group added to both ends thereof and further grafted with an amino group, and those having a silicone main chain and an amino group grafted on the silicone main chain. In the present invention, an amino-modified silicone represented by the following formula is used.

[In Formula 1, A is ^-R 2 NH ₂ or ^-R ₂ ^NHR 3 NH 2 (where ^{R 2} and ^{R 3} is an alkylene group having 1 to 8 carbon atoms),
R ¹ is a group independently selected from the group consisting of an alkyl group having 1 to 30 carbon atoms, a cycloalkyl group, an aryl group, an aralkyl group, and a fluorine-substituted alkyl group;
m is an integer of 50 <m <400, and n is an integer of 1 <n <20, and s and t are independently an integer of 0 to 3, provided that 1 ≦ n + s + t. ]
Examples of R ¹ include methyl groups, ethyl groups, propyl groups, butyl groups, pentyl groups, hexyl groups, heptyl groups, octyl groups, nonyl groups, decyl groups and other alkyl groups, cyclopentyl groups, cyclohexyl groups and other cyclo groups. Examples thereof include organic groups represented by fluorine-substituted alkyl groups such as an alkyl group, a trifluoropropyl group, and a heptadecafluorolone group. Preferably, they are a methyl group, a phenyl group, and a trifluoropropyl group.
Examples of R ² and R ³ include a methyl group, an ethylene group, a propylene group, a butylene group, and a pentylene group, and a methylene group, an ethylene group, and a propylene group are preferable.

  Examples of the powder component include talc, kaolin, sericite (sericite), muscovite, phlogopite, synthetic mica, saucite, biotite, fired talc, fired sericite, fired muscovite, fired phlogopite, permiculite, Magnesium carbonate, calcium carbonate, aluminum silicate, barium silicate, calcium silicate, magnesium silicate, strontium silicate, metal tungstate, magnesium, silica, zeolite, barium sulfate, calcined calcium sulfate (baked gypsum), calcium phosphate, Fluorine apatite, hydroxyapatite, ceramic powder, metal soap (eg, zinc myristate, calcium palmitate, aluminum stearate), boron nitride, photochromic titanium oxide (titanium dioxide sintered with iron oxide), reduced zinc white Organic powder (For example, silicone elastomer powder, silicone powder, silicone resin-coated silicone elastomer powder, polyamide resin powder (nylon powder), polyethylene powder, polymethyl methacrylate powder, polystyrene powder, copolymer resin powder of styrene and acrylic acid, benzoguanamine resin Powder, polytetrafluoroethylene powder, cellulose powder, etc.); inorganic white pigments (eg, titanium dioxide, zinc oxide, etc.); inorganic red pigments (eg, iron oxide (Bengara), iron titanate, etc.); inorganic brown Pigments (for example, γ-iron oxide, etc.); inorganic yellow pigments (for example, yellow iron oxide, ocher, etc.); inorganic black pigments (for example, black iron oxide, low-order titanium oxide, etc.); inorganic purple pigments (for example, , Mango violet, cobalt violet, etc.); inorganic green pigments (eg chromium oxide, hydroxide) Chromium, cobalt titanate, etc.); inorganic blue pigments (eg ultramarine, bitumen, etc.); pearl pigments (eg, bismuth oxychloride, fish scale foil, titanium mica, iron oxide-coated mica titanium, low-order titanium oxide-coated mica titanium, Titanium mica having photochromic properties, talc instead of mica as a substrate, glass, synthetic fluorine phlogopite, silica, bismuth oxychloride, etc., in addition to titanium oxide as coating, low-order titanium oxide, colored titanium oxide, Iron oxide, alumina, silica, zirconia, zinc oxide, cobalt oxide, aluminum coated, etc., functional pearl pigment coated with resin particles on the surface of pearl pigment (JP-A-11-92688), pearl pigment surface Aluminum hydroxide particles coated (JP 2002-146238), pearl pigment surface coated with zinc oxide particles JP 2003-261421), pearl pigment surface coated with barium sulfate particles (JP 2003-61229), etc .; metal powder pigments (eg, aluminum powder, copper powder, etc.); zirconium, barium, aluminum lake, etc. Organic pigments (for example, red 201, red 202, red 204, red 205, red 220, red 226, red 228, red 405, orange 203, orange 204, yellow 205, yellow Organic pigments such as No. 401 and Blue No. 404, Red No. 3, Red No. 104, Red No. 106, Red No. 227, Red No. 230, Red No. 401, Red No. 505, Orange No. 205, Yellow No. 4, Yellow No. 5 No., Yellow No. 202, Yellow No. 203, Green No. 3 and Blue No. 1); natural pigments (for example, chlorophyll, β-carotene and the like) and the like.

Examples of liquid oils include avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil, southern castor oil, castor oil, linseed oil , Safflower oil, cottonseed oil, eno oil, soybean oil, peanut oil, tea seed oil, kaya oil, rice bran oil, cinnagiri oil, Japanese kiri oil, jojoba oil, germ oil, triglycerin and the like.
Examples of the solid fat include cacao butter, palm oil, horse fat, hydrogenated palm oil, palm oil, beef tallow, sheep fat, hydrogenated beef tallow, palm kernel oil, pork fat, beef bone fat, owl kernel oil, hydrogenated oil, cattle Leg fats, moles, hydrogenated castor oil and the like.

Examples of waxes include beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, ibota wax, whale wax, montan wax, nuka wax, lanolin, kapok wax, lanolin acetate, liquid lanolin, sugar cane wax, lanolin fatty acid isopropyl, hexyl laurate, and reduced lanolin. , Jojoballow, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate, POE cholesterol ether, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether, and the like.
Examples of the hydrocarbon oil include liquid paraffin, ozokerite, squalane, pristane, paraffin, ceresin, squalene, petrolatum, microcrystalline wax, and the like.
Examples of the higher fatty acid include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, undecylenic acid, toluic acid, isostearic acid, linoleic acid, linolenic acid, eicosapentaenoic acid (EPA), docosahexaenoic acid ( DHA) and the like.

Examples of higher alcohols include linear alcohols (eg, lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol); branched chain alcohols (eg, monostearyl glycerin ether (batyl alcohol) ), 2-decyltetradecinol, lanolin alcohol, cholesterol, phytosterol, hexyl decanol, isostearyl alcohol, octyldodecanol and the like.
Synthetic ester oils include isopropyl myristate, cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, hexyl laurate, myristyl myristate, decyl oleate, hexyl decyl dimethyloctanoate, cetyl lactate, myristyl lactate Lanolin acetate, isocetyl stearate, isocetyl isostearate, cholesteryl 12-hydroxystearate, ethylene glycol di-2-ethylhexanoate, dipentaerythritol fatty acid ester, monoisostearate N-alkyl glycol, neopentyl glycol dicaprate, apple Acid diisostearyl, di-2-heptylundecanoic acid glycerin, tri-2-ethylhexanoic acid trimethylolpropane, triisostearic acid trimethylo Propane, tetra-2-ethylhexanoate pentaerythritol, glycerol tri-2-ethylhexanoate, glycerol trioctanoate, glycerol triisopalmitate, trimethylolpropane triisostearate, cetyl 2-ethylhexanoate, 2-ethylhexyl palmi Tate, glyceryl trimyristate, glyceride tri-2-heptylundecanoate, castor oil fatty acid methyl ester, oleyl oleate, acetoglyceride, 2-heptylundecyl palmitate, diisobutyl adipate, N-lauroyl-L-glutamic acid-2 -Octyldodecyl ester, di-2-heptylundecyl adipate, ethyl laurate, di-2-ethylhexyl sebacate, 2-hexyldecyl myristate, 2-hexyldecyl palmitate, 2-hexyldecyl adipate Le, diisopropyl sebacate, 2-ethylhexyl succinate, and triethyl citrate.

  Anionic surfactants include, for example, fatty acid soaps (eg, sodium laurate, sodium palmitate, etc.); higher alkyl sulfates (eg, sodium lauryl sulfate, potassium lauryl sulfate, etc.); alkyl ether sulfates (eg, POE-lauryl sulfate triethanolamine, POE-sodium lauryl sulfate, etc.); N-acyl sarcosine acids (eg, sodium lauroyl sarcosine, etc.); higher fatty acid amide sulfonates (eg, sodium N-myristoyl-N-methyl taurate, palm Oil fatty acid methyl tauride sodium, lauryl methyl tauride sodium, etc .; phosphate ester salt (POE-oleyl ether sodium phosphate, POE-stearyl ether phosphate, etc.); sulfosuccinate (eg, di-2-ethylhexyl sulfo) Sodium succinate, monolauroyl monoethanolamide sodium polyoxyethylene sulfosuccinate, sodium lauryl polypropylene glycol sulfosuccinate, etc.); alkyl benzene sulfonates (eg, sodium linear dodecyl benzene sulfonate, triethanol amine linear dodecyl benzene sulfonate, linear dodecyl) Higher fatty acid ester sulfates (eg, hydrogenated coconut oil fatty acid sodium glycerol sulfate); N-acyl glutamate (eg, monosodium N-lauroyl glutamate, disodium N-stearoyl glutamate, N-myristoyl) -L-glutamic acid monosodium, etc.); sulfated oil (eg funnel oil); POE-alkyl ether carboxylic acid; POE-alkyl allyl ether Α-olefin sulfonates; higher fatty acid ester sulfonates; secondary alcohol sulfates; higher fatty acid alkylolamide sulfates; lauroyl monoethanolamide sodium succinate; N-palmitoyl aspartate ditriethanolamine ; Sodium caseinate and the like.

  Examples of the cationic surfactant include alkyltrimethylammonium salts (eg, stearyltrimethylammonium chloride, lauryltrimethylammonium chloride, etc.); alkylpyridinium salts (eg, cetylpyridinium chloride, etc.); distearyldimethylammonium dialkyldimethylammonium chloride; Poly (N, N'-dimethyl-3,5-methylenepiperidinium chloride); alkyl quaternary ammonium salt; alkyldimethylbenzylammonium salt; alkylisoquinolinium salt; dialkyl morpholinium salt; POE-alkylamine; Examples include alkylamine salts; polyamine fatty acid derivatives; amyl alcohol fatty acid derivatives; benzalkonium chloride; benzethonium chloride and the like.

  Examples of amphoteric surfactants include imidazoline-based amphoteric surfactants (eg, 2-undecyl-N, N, N- (hydroxyethylcarboxymethyl) -2-imidazoline sodium, 2-cocoyl-2-imidazolinium hydroxide). Side-1-carboxyethyloxy disodium salt, etc.); betaine surfactants (for example, 2-heptadecyl-N-carboxymethyl-N-hydroxyethylimidazolinium betaine, lauryldimethylaminoacetic acid betaine, alkylbetaine, amide betaine) , Sulfobetaine, etc.).

  Examples of the lipophilic nonionic surfactant include sorbitan fatty acid esters (for example, sorbitan monooleate, sorbitan monoisostearate, sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan sesquioleate, Sorbitan trioleate, diglycerol sorbitan penta-2-ethylhexylate, diglycerol sorbitan tetra-2-ethylhexylate); glycerin polyglycerin fatty acids (eg mono cottonseed oil fatty acid glycerin, monoerucic acid glycerin, sesquioleate glycerin, monostearin) Glycerin acid, α, α'-oleic acid pyroglutamate glycerin, monostearic acid glycerin malic acid, etc.); propylene glycol fatty acid esters (eg monostearies) Propylene glycolate, etc.); hardened castor oil derivative; glycerin alkyl ether, etc.

  Examples of hydrophilic nonionic surfactants include POE-sorbitan fatty acid esters (for example, POE-sorbitan monooleate, POE-sorbitan monostearate, POE-sorbitan monooleate, POE-sorbitan tetraoleate). POE sorbite fatty acid esters (eg, POE-sorbite monolaurate, POE-sorbite monooleate, POE-sorbite pentaoleate, POE-sorbite monostearate, etc.); POE-glycerin fatty acid esters (eg, POE- POE-monooleate such as glycerol monostearate, POE-glycerol monoisostearate, POE-glycerol triisostearate); POE-fatty acid esters (eg POE-distearate, POE-monodiolate, ethylene glycol distearate, etc.) POE-alkyl ethers (eg POE- Lauryl ether, POE-oleyl ether, POE-stearyl ether, POE-behenyl ether, POE-2-octyldodecyl ether, POE-cholestanol ether, etc.); Pluronic type (eg, Pluronic, etc.); POE / POP-alkyl ether (For example, POE / POP-cetyl ether, POE / POP-2-decyltetradecyl ether, POE / POP-monobutyl ether, POE / POP-hydrogenated lanolin, POE / POP-glycerin ether, etc.); Tetra POE / Tetra POP-ethylenediamine condensates (eg Tetronic, etc.); POE-castor oil hardened castor oil derivatives (eg POE-castor oil, POE-hardened castor oil, POE-hardened castor oil monoisostearate, POE-hardened castor Oil triisostearate, POE-hardened castor oil monopyroglutamic acid monoisostearic acid diester, POE-hardened castor oil maleic acid, etc.) POE-beeswax lanolin derivatives (eg POE-sorbite beeswax); alkanolamides (eg coconut oil fatty acid diethanolamide, lauric acid monoethanolamide, fatty acid isopropanolamide, etc.); POE-propylene glycol fatty acid ester; POE-alkylamine POE-fatty acid amide; sucrose fatty acid ester; alkyl ethoxydimethylamine oxide; trioleyl phosphate and the like.

  Examples of the humectant include polyethylene glycol, propylene glycol, glycerin, 1,3-butylene glycol, xylitol, sorbitol, maltitol, chondroitin sulfate, hyaluronic acid, mucoitin sulfate, caronic acid, atelocollagen, cholesteryl-12-hydroxystearate Sodium lactate, bile salt, dl-pyrrolidone carboxylate, alkylene oxide derivative, short-chain soluble collagen, diglycerin (EO) PO adduct, Izayoi rose extract, yarrow extract, merirot extract and the like.

  Examples of natural water-soluble polymers include plant-based polymers (for example, gum arabic, gum tragacanth, galactan, guar gum, carob gum, caraya gum, carrageenan, pectin, agar, quince seed (malmello), alge colloid (guckweed extract), starch (Rice, corn, potato, wheat), glycyrrhizic acid); microbial polymers (eg, xanthan gum, dextran, succinoglucan, bullulan, etc.); animal polymers (eg, collagen, casein, albumin, gelatin, etc.), etc. Is mentioned.

  Semi-synthetic water-soluble polymers include, for example, starch polymers (eg, carboxymethyl starch, methylhydroxypropyl starch, etc.); cellulose polymers (methylcellulose, ethylcellulose, methylhydroxypropylcellulose, hydroxyethylcellulose, sodium cellulose sulfate) Hydroxypropylcellulose, carboxymethylcellulose, sodium carboxymethylcellulose, crystalline cellulose, cellulose powder and the like); alginic acid polymers (for example, sodium alginate, propylene glycol alginate, etc.) and the like.

  Synthetic water-soluble polymers include, for example, vinyl polymers (eg, polyvinyl alcohol, polyvinyl methyl ether, polyvinyl pyrrolidone, carboxyvinyl polymer); polyoxyethylene polymers (eg, polyethylene glycol 20,000, 40,000, 60,000). Polyoxyethylene polyoxypropylene copolymer, etc.); acrylic polymers (for example, sodium polyacrylate, polyethyl acrylate, polyacrylamide, etc.); polyethyleneimine; cationic polymers, and the like.

  Examples of the thickener include gum arabic, carrageenan, caraya gum, gum tragacanth, carob gum, quince seed (malmello), casein, dextrin, gelatin, sodium pectate, sodium alginate, methylcellulose, ethylcellulose, CMC, hydroxyethylcellulose, hydroxypropyl Cellulose, PVA, PVM, PVP, sodium polyacrylate, carboxyvinyl polymer, locust bean gum, guar gum, tamarind gum, cellulose dialkyldimethylammonium sulfate, xanthan gum, magnesium aluminum silicate, bentonite, hectorite, silicate A1Mg (vee gum), Examples thereof include laponite and silicic anhydride.

  Examples of UV absorbers include benzoic acid UV absorbers (eg, paraaminobenzoic acid (hereinafter abbreviated as PABA), PABA monoglycerin ester, N, N-dipropoxy PABA ethyl ester, N, N-diethoxy PABA ethyl ester. N, N-dimethyl PABA ethyl ester, N, N-dimethyl PABA butyl ester, N, N-dimethyl PABA ethyl ester, etc.); anthranilic acid-based ultraviolet absorbers (eg, homomenthyl-N-acetylanthranylate, etc.); Salicylic acid ultraviolet absorbers (for example, amyl salicylate, menthyl salicylate, homomenthyl salicylate, octyl salicylate, phenyl salicylate, benzyl salicylate, p-isopropanol phenyl salicylate, etc.); cinnamic acid ultraviolet absorbers (for example, octylmethoxycinnamate, ethyl) -4-Isopropyl cinnamate , Methyl-2,5-diisopropylcinnamate, ethyl-2,4-diisopropylcinnamate, methyl-2,4-diisopropylcinnamate, propyl-p-methoxycinnamate, isopropyl-p-methoxycinnamate, isoamyl-p -Methoxycinnamate, octyl-p-methoxycinnamate (2-ethylhexyl-p-methoxycinnamate), 2-ethoxyethyl-p-methoxycinnamate, cyclohexyl-p-methoxycinnamate, ethyl-α-cyano-β -Phenyl cinnamate, 2-ethylhexyl-α-cyano-β-phenyl cinnamate, glyceryl mono-2-ethylhexanoyl-diparamethoxy cinnamate, etc.); benzophenone UV absorbers (for example, 2,4-dihydroxybenzophenone) 2,2'-dihydroxy-4-methoxybenzophenone, 2,2'-dihydroxy-4,4'-dimethoxybenzo Enone, 2,2 ', 4,4'-Tetrahydroxybenzophenone, 2-hydroxy-4-methoxybenzophenone, 2-hydroxy-4-methoxy-4'-methylbenzophenone, 2-hydroxy-4-methoxybenzophenone-5- Sulfonate, 4-phenylbenzophenone, 2-ethylhexyl-4′-phenyl-benzophenone-2-carboxylate, 2-hydroxy-4-n-octoxybenzophenone, 4-hydroxy-3-carboxybenzophenone, etc.); 3- (4'-methylbenzylidene) -d, l-camphor, 3-benzylidene-d, l-camphor; 2-phenyl-5-methylbenzoxazole; 2,2'-hydroxy-5-methylphenylbenzotriazole; 2 -(2'-hydroxy-5'-t-octylphenyl) benzotriazole; 2- (2'-hydroxy-5'-methylphenylbenzotriazole); dibenzalazine; dianisoylmethane; 4-methoxy-4'-t-butyl Benzoylmethane; 5- (3,3-dimethyl-2-norbornylidene) -3-pentan-2-one, dimorpholinopyridazino; 2-ethylhexyl-2-cyano-3,3-diphenyl acrylate; 2,4- And bis-{[4- (2-ethylhexyloxy) -2-hydroxy] -phenyl} -6- (4-methoxyphenyl)-(1,3,5) -triazine.

  Examples of the sequestering agent include 1-hydroxyethane-1,1-diphosphonic acid, 1-hydroxyethane-1,1-diphosphonic acid tetrasodium salt, disodium edetate, trisodium edetate, and tetrasodium edetate. Sodium citrate, sodium polyphosphate, sodium metaphosphate, gluconic acid, phosphoric acid, citric acid, ascorbic acid, succinic acid, edetic acid, trisodium ethylenediaminehydroxyethyl triacetate and the like.

  Examples of the lower alcohol include ethanol, propanol, isopropanol, isobutyl alcohol, t-butyl alcohol and the like.

  Examples of the polyhydric alcohol include divalent alcohols (for example, ethylene glycol, propylene glycol, trimethylene glycol, 1,2-butylene glycol, 1,3-butylene glycol, tetramethylene glycol, 2,3-butylene glycol, Pentamethylene glycol, 2-butene-1,4-diol, hexylene glycol, octylene glycol, etc.); trivalent alcohol (eg, glycerin, trimethylolpropane, etc.); tetravalent alcohol (eg, 1,2,6) Pentaerythritol such as hexanetriol); pentahydric alcohol (eg, xylitol, etc.); hexavalent alcohol (eg, sorbitol, mannitol, etc.); polyhydric alcohol polymer (eg, diethylene glycol, dipropylene glycol, triethylene glycol, polypropylene Glycol, tetraethylene glycol, diglycerin, polyethylene glycol, triglycerin, tetraglycerin, polyglycerin, etc.); divalent alcohol alkyl ethers (for example, ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene) Glycol monophenyl ether, ethylene glycol monohexyl ether, ethylene glycol mono 2-methylhexyl ether, ethylene glycol isoamyl ether, ethylene glycol benzyl ether, ethylene glycol isopropyl ether, ethylene glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, etc.) ; Dihydric alcohol alkyl ester Tellurium (for example, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol butyl ether, diethylene glycol methyl ethyl ether, triethylene glycol monomethyl ether, triethylene glycol monoethyl ether, propylene glycol monomethyl ether , Propylene glycol monoethyl ether, propylene glycol monobutyl ether, propylene glycol isopropyl ether, dipropylene glycol methyl ether, dipropylene glycol ethyl ether, dipropylene glycol butyl ether, etc.); divalent alcohol Ether esters (eg, ethylene glycol monomethyl ether acetate, ethylene glycol monoethyl ether acetate, ethylene glycol monobutyl ether acetate, ethylene glycol monophenyl ether acetate, ethylene glycol diazinate, ethylene glycol disuccinate, diethylene glycol monoethyl ether acetate, diethylene glycol) Monobutyl ether acetate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, propylene glycol monopropyl ether acetate, propylene glycol monophenyl ether acetate, etc .; glycerin monoalkyl ether (for example, xyl alcohol, ceralkyl alcohol) Sugar alcohol (for example, sorbitol, maltitol, maltotriose, mannitol, sucrose, erythritol, glucose, fructose, amylolytic sugar, maltose, xylitolose, amylolytic sugar reducing alcohol, etc.); Solid; Tetrahydrofurfuryl alcohol; POE-Tetrahydrofurfuryl alcohol; POP-Butyl ether; POP / POE-Butyl ether; Tripolyoxypropylene glycerin ether; POP-glycerin ether; POP-glycerin ether phosphate; POP / POE-pentane erythritol Examples include ether and polyglycerin.

  Monosaccharides include, for example, tricarbon sugars (eg, D-glyceryl aldehyde, dihydroxyacetone, etc.); tetracarbon sugars (eg, D-erythrose, D-erythrulose, D-treose, erythritol, etc.); pentose sugars (eg, , L-arabinose, D-xylose, L-lyxose, D-arabinose, D-ribose, D-ribulose, D-xylulose, L-xylulose, etc .; hexose (eg, D-glucose, D-talose, D) -Bucicose, D-galactose, D-fructose, L-galactose, L-mannose, D-tagatose, etc.); pentose sugar (eg, aldheptose, heproose, etc.); octose sugar (eg, octulose, etc.); For example, 2-deoxy-D-ribose, 6-deoxy-L-galactose, 6-deoxy-L-mannose, etc .; amino sugar (eg, D-glucosamine, D-galactosamine, shea Acid, Aminouron acid, muramic acid); uronic acid (e.g., D- glucuronic acid, D- mannuronic acid, L- guluronic acid, D- galacturonic acid, L- iduronic acid) and the like.

  Examples of the oligosaccharides include sucrose, gnocyanose, umbelliferose, lactose, planteose, isoliquinoses, α, α-trehalose, raffinose, lycnose, umbilicin, stachyose verbus courses and the like.

  Examples of the polysaccharide include cellulose, quince seed, chondroitin sulfate, starch, galactan, dermatan sulfate, glycogen, gum arabic, heparan sulfate, hyaluronic acid, tragacanth gum, keratan sulfate, chondroitin, xanthan gum, mucoitin sulfate, guar gum, dextran, kerato sulfate. , Locust bean gum, succinoglucan, caronic acid and the like.

  Examples of amino acids include neutral amino acids (eg, threonine, cysteine, etc.); basic amino acids (eg, hydroxylysine, etc.) and the like. Examples of amino acid derivatives include acyl sarcosine sodium (lauroyl sarcosine sodium), acyl glutamate, acyl β-alanine sodium, glutathione, and pyrrolidone carboxylic acid.

Examples of the organic amine include monoethanolamine, diethanolamine, triethanolamine, morpholine, triisopropanolamine, 2-amino-2-methyl-1,3-propanediol, and 2-amino-2-methyl-1-propanol. Is mentioned.
Examples of the polymer emulsion include an acrylic resin emulsion, a polyethyl acrylate emulsion, an acrylic resin liquid, a polyacryl alkyl ester emulsion, a polyvinyl acetate resin emulsion, and a natural rubber latex.

Examples of the pH adjuster include buffers such as lactic acid-sodium lactate, citric acid-sodium citrate, and succinic acid-sodium succinate.
Examples of vitamins include vitamins A, B1, B2, B6, C, E and derivatives thereof, pantothenic acid and derivatives thereof, biotin and the like.
Examples of the antioxidant include tocopherols, dibutylhydroxytoluene, butylhydroxyanisole, gallic acid esters and the like.

  Examples of the antioxidant assistant include phosphoric acid, citric acid, ascorbic acid, maleic acid, malonic acid, succinic acid, fumaric acid, kephalin, hexametaphosphate, phytic acid, and ethylenediaminetetraacetic acid.

  Other ingredients that can be blended include, for example, preservatives (ethyl paraben, butyl paraben, etc.); anti-inflammatory agents (eg, glycyrrhizic acid derivatives, glycyrrhetinic acid derivatives, salicylic acid derivatives, hinokitiol, zinc oxide, allantoin, etc.); whitening agents (for example, Extract, placenta extract, saxifrage extract, arbutin, etc.); various extracts (eg, buckwheat, auren, shikon, peonies, assembly, birch, sage, loquat, carrot, aloe, mallow), iris, grape, yokuinin, loofah, lily , Saffron, nematode, ginger, hypericum, onionis, garlic, capsicum, chimney, red snapper, seaweed, etc.), activator (eg, royal jelly, photosensitizer, cholesterol derivative, etc.); blood circulation promoter (eg, nonyl acid wallenylamide, nicotine) Acid Gyl ester, nicotinic acid β-butoxyethyl ester, capsaicin, gingerone, cantalis tincture, ictamol, tannic acid, α-borneol, tocopherol nicotinate, inositol hexanicotinate, cyclandrate, cinnarizine, trazoline, acetylcholine, verapamil, cephalanthin , Γ-oryzanol, etc.); antiseborrheic agents (eg, sulfur, thianthol, etc.); anti-inflammatory agents (eg, tranexamic acid, thiotaurine, hypotaurine, etc.) and the like.

  Furthermore, edetate disodium, edetate trisodium, sodium citrate, sodium polyphosphate, sodium metaphosphate, gluconic acid, malic acid and other metal sequestering agents, caffeine, tannin, verapamil, tranexamic acid and its derivatives, licorice, Various herbal extracts such as Karin and Ichiyakusou, drugs such as tocopherol acetate, glycyrrhizic acid, glycyrrhizic acid and derivatives or salts thereof, whitening agents such as vitamin C, magnesium ascorbate phosphate, glucoside ascorbate, arbutin, kojic acid, Amino acids such as arginine and lysine and derivatives thereof, saccharides such as fructose, mannose, erythritol, trehalose and xylitol can also be appropriately blended.

[式（２）において、ｍは５０＜ｍ＜４００の整数、及びｎは１＜ｎ＜２０の整数である。]
＜スラリー調製工程＞
下記処方表１に示す粉末成分と油性成分とその他の成分を混合し、エチルアルコール中にディスパーミキサーにて混合し、スラリー粘度を２０００ｍＰａ・ｓ程度に調整した後、２ｍｍφのジルコニアビーズを充填した媒体攪拌ミル（サンドグラインダーミル）を用いて、解砕／粉砕／分散を行った。これにより粉末スラリーを得た。
＜粉末化粧料の製造＞
前記粉末スラリーを、攪拌乾燥装置ドライマイスター（ホソカワミクロン社製）を用い、微小液滴の状態で乾燥を行い、乾燥粉末を得た。
得られた乾燥粉末を樹脂製の中皿容器に充填し、公知の方法で乾式プレス成型を行い、固形状の粉末化粧料を得た。

Examples and the like according to the present invention will be described below, but the present invention is not limited thereto. In addition, the quantity in the following prescription is shown by the mass%.
Example 1 : Aminoethylaminopropylmethylsiloxane / dimethylsiloxane copolymer

[In Formula (2), m is an integer of 50 <m <400, and n is an integer of 1 <n <20. ]
<Slurry preparation process>
A medium filled with 2 mmφ zirconia beads after mixing the powder component, oily component and other components shown in the following formulation table 1, mixing in ethyl alcohol with a disper mixer, and adjusting the slurry viscosity to about 2000 mPa · s. Crushing / pulverization / dispersion was performed using a stirring mill (sand grinder mill). This obtained the powder slurry.
<Manufacture of powder cosmetics>
The powder slurry was dried in the form of fine droplets using a stirrer / dryer Dry Meister (manufactured by Hosokawa Micron) to obtain a dry powder.
The obtained dry powder was filled into a resin middle dish container and dry press molded by a known method to obtain a solid powder cosmetic.

Measurement of Contact Angle for Water The method for measuring the water contact angle is not particularly limited, but a contact angle measuring device known to those skilled in the art can be used. Examples of the contact angle measuring device include CA-V150 (manufactured by Kyowa Interface Science Co., Ltd.). In the present invention, for example, a water droplet having a particle size of about 1.5 mm is dropped on the surface coated with the water-insoluble composite coating, and after 1000 milliseconds have elapsed, the contact angle between the coating surface and the water droplet is measured. . The contact angle in the present invention means an angle from the surface of the coating to the inside of the water droplet to the tangent to the outer surface of the water droplet. Usually, the larger the contact angle, the higher the water repellency of the surface of the coating (FIG. 8). ), It is considered that the powder cosmetic is difficult to fall off due to moisture such as sweat, and the makeup lasting is good.

About the powder cosmetics of Example 1 obtained by said manufacturing process and Comparative Examples 1-6, the measurement result of the contact angle with respect to water is shown in FIG.
As can be seen from FIG. 4, it is clear that the powder cosmetic of Example 1 to which aminoethylaminopropylmethylsiloxane / dimethylsiloxane copolymer, which is an amino-modified silicone, is added as a dispersant can obtain the largest contact angle. became.
On the other hand, Comparative Example 1 in which no dispersant was added did not have the same contact angle as that of Example 1 in which amino-modified silicone was added. In addition, Comparative Example 2 in which a polyoxyethylene / methylpolysiloxane copolymer was added as another dispersant, Comparative Example 3 in which a highly polymerized dimethylsiloxane / methyl (aminopropyl) siloxane copolymer was added, and sesquiisostearic acid were added In Comparative Example 4 and Comparative Example 5 to which distearyldimethylammonium chloride was added, the contact angle as large as Example 1 could not be obtained. And the comparative example 6 which added and manufactured the powder component which performed the silicone process without adding amino modification silicone was a little small compared with Example 1, but obtained the height of the comparable contact angle. .

Measurement of Contact Angle for Oil Further , according to the method for measuring the contact angle for water described above, the measurement results of the contact angle for oil of the powder cosmetics of Example 1 and Comparative Examples 1 to 6 are shown in FIG. . It is considered that the larger the contact angle with oil, the higher the oil repellency on the surface of the coating, and the powder cosmetics are less likely to fall off due to oil such as sebum, and the cosmetic durability is considered to be good.
And it turns out that the contact angle with respect to oil becomes large significantly compared with Comparative Examples 1-6 as for the powder cosmetics obtained by prescription of Example 1 so that FIG. 5 may show. In Comparative Example 6 where the contact angle with respect to water was as high as that of Example 1, the height as high as that of Example 1 could not be obtained with respect to the height of the contact angle with respect to oil.
That is, from the above results, it has been clarified that, when amino-modified silicone is added to the powder cosmetic production process, a powder cosmetic having high water repellency and extremely high oil repellency can be provided.

Subsequently, as shown in the following Formulation Table 2, Example 1 in which 1% by mass of amino-modified silicone was added to the total amount of the powder cosmetic, Example 2 in which 0.2% by mass of amino-modified silicone was added, and amino As Example 3 in which 0.5% by mass of the modified silicone was added and Example 4 in which 2% by mass of the amino-modified silicone was added, a powder cosmetic was obtained by changing the ratio of adding the amino-modified silicone.
Using the powder cosmetics of Examples 1 to 4 above, the results of measuring the contact angle with water are shown in FIG. 6, and the results of measuring the contact angle with oil are shown in FIG.

As can be seen from FIG. 6, in Comparative Example 1 in which no dispersant was added, the contact angle to water as high as in Examples 1 to 4 in which the amino-modified silicone was added could not be obtained. And even if it changed the ratio which adds amino-modified silicone, it became clear that there is no big difference regarding the contact angle with respect to water.
On the other hand, as can be seen from FIG. 7, the contact angle with respect to oil is smaller in Example 2 to which 0.2% by mass of amino-modified silicone is added than in other examples to which 0.5% by mass or more is added. However, it became clear that it was larger than Comparative Example 1 in which no dispersant was added and Comparative Example 6 in which the powder component subjected to silicone treatment was added.
Further, Example 1 to which 1.0% by mass of amino-modified silicone was added had the largest contact angle with respect to oil, and Example 4 to which 2.0% by mass was added was the next largest, but 0.2% by mass or more of amino-modified silicone was added. It became clear that it will become large compared with each comparative example if it adds.

  From the above, in order to obtain a powder cosmetic having both water repellency and oil repellency, it is preferable to add 0.1 to 5.0% by mass of amino-modified silicone in the powder cosmetic, especially 0. It is preferable to add 0.5 to 1.5% by mass.

<Slurry preparation process>
A medium filled with 2 mmφ zirconia beads after mixing the powder component, oil component and other components shown in the following Formulation Table 3, mixing in ethyl alcohol with a disper mixer, and adjusting the slurry viscosity to about 2000 mPa · s. Crushing / pulverization / dispersion was performed using a stirring mill (sand grinder mill). This obtained the powder slurry.
<Manufacture of powder cosmetics>
The powder slurry was dried in the form of fine droplets using a stirrer / dryer Dry Meister (manufactured by Hosokawa Micron) to obtain a dry powder.
The obtained dry powder was filled into a resin middle dish container and dry press molded by a known method to obtain a solid powder cosmetic.

<Evaluation of cosmetics>
As described below, sensory characteristics of the powdered solid cosmetic obtained above were evaluated with respect to the feeling of use (smoothness, uniform finish, color appearance, makeup lasting) when applied to the skin.
The following sensory property evaluation items were evaluated using 20 panelists specializing in sensory property evaluation.
Evaluation Criteria ・ Smoothness ◎: Out of 20 people answered that 17 or more are smooth ○: Out of 20 people answered that 12 to 16 or more were smooth △: Out of 20 people, 9 to 11 or more were smooth ×: Answers that 5 to 8 or more of the 20 people are smooth. ××: Answers that 4 or less of the 20 people are smooth. • Uniform finish ◎: 17 of the 20 people The above answers indicate that the finish is uniform. ○: Among 20 people, 12 to 16 or more respond that the finish is uniform. △: Among 20 people, 9 to 11 or more respond that the finish is uniform. ×: Out of 20 people, 5 to 8 or more responded that there was a uniform finish. × ×: Out of 20 people, 4 or less responded that there was a uniform finish. • Color appearance ◎: Out of 20 people, 17 More than one person answered that there is a fit to the skin ○: Among 20 people, 12 to 16 or more answered that there was a fit to the skin △: Among 20 people, 9 to 11 or more responded to the skin There are times Answer ×: Out of 20 people, 5 to 8 or more responded that it fits the skin XX: Out of 20 people, 4 or less answered that it fits the skin ・ Make-up ◎: Out of 20 people , 17 or more responded that they had a moist feeling ○: Among 20 people, 12 to 16 or more responded that they had a moist feeling △: Of 20 people, 9 to 11 or more responded that they had a moist feeling ×: 20 Among the names, 5-8 or more responded that they had a moist feeling. XX: Among 20 people, 4 or less responded that they had a moist feeling.

表４から分かるように、本発明にかかる製造方法で製造した実施例５の粉末化粧料はなめらかさ、均一な仕上がり感、色の出、化粧持ちといった使用感触に優れていた。これは、媒体ミルでスラリーを調製することにより粉体成分の表面に油分及びアミノ変性シリコーンが均一に被覆され、この状態が乾燥粉末とした後も保たれているためであると考えられる。
一方、アミノ変性シリコーンを添加せずに、シリコーン処理を施した粉末成分を添加して製造した比較例７は、なめらかさ、均一な仕上がり感、色の出といった使用感触に優れていたが、化粧持ちといった使用感触が欠如していることが確認された。また、アミノ変性シリコーンを添加せず、シリコーン処理を施していない粉末成分を添加して製造した比較例８の粉末化粧料は、色の出、化粧持ちといった使用感触が欠如していることが確認された。
以上の結果より、アミノ変性シリコーンを添加した本発明の粉末化粧料の製造方法は化粧持ちに優れたものであることが分かる。 The results of the above test are shown in Table 1 below.

As can be seen from Table 4, the powder cosmetic of Example 5 produced by the production method according to the present invention was excellent in use feeling such as smoothness, uniform finish, color appearance, and long-lasting makeup. This is presumably because the oil component and the amino-modified silicone are uniformly coated on the surface of the powder component by preparing the slurry with a medium mill, and this state is maintained even after the dry powder is formed.
On the other hand, Comparative Example 7 produced by adding a silicone-treated powder component without adding an amino-modified silicone was excellent in use feeling such as smoothness, uniform finish, and color appearance. It was confirmed that the feeling of use such as holding was lacking. In addition, it was confirmed that the powder cosmetic of Comparative Example 8 produced by adding a powder component not subjected to silicone treatment without adding amino-modified silicone lacks the feeling of use such as color appearance and long-lasting makeup. It was done.
From the above results, it can be seen that the method for producing a powder cosmetic of the present invention to which an amino-modified silicone is added is excellent in long-lasting makeup.

<Manufacturing process>
The powder component and oil component of Examples 6 and 7 shown in the following Table 5 are mixed, mixed in ethyl alcohol with a disper mixer, and after adjusting the slurry viscosity to about 2000 mPa · s, 3 mmφ zirconia beads are added. Crushing / pulverization / dispersion was performed using a filled medium stirring mill (sand grinder mill). The obtained powder slurry was dried with a dry meister (manufactured by Hosokawa Micron Corporation), and the obtained dry powder and the pearl pigment part were mixed with a Henschel mixer, respectively, to obtain a mixed dry powder.
The obtained mixed dry powder and other components were mixed, filled into a container, and a powdered solid cosmetic was obtained by known dry press molding. The obtained powdered solid cosmetic was very excellent in use feeling and pearl feeling.

The powder component and the oil component of Example 8 shown in the following formulation table 6 were mixed, mixed in ethyl alcohol with a disper mixer, and the slurry viscosity was adjusted to about 2000 mPa · s, and then filled with 2 mmφ zirconia beads. Crushing / pulverization / dispersion was performed using a medium stirring mill (sand grinder mill). The obtained powder slurry was dried with a dry meister (manufactured by Hosokawa Micron Corporation) to obtain a mixed dry powder.
The obtained mixed dry powder and other components were mixed, filled into a container, and a powdered solid cosmetic was obtained by known dry press molding.
The obtained powdered solid cosmetic was very excellent in use feeling.

The schematic block diagram of the apparatus used with the manufacturing method concerning embodiment of this invention Diagram showing an example of a medium agitating mill Diagram showing an example of a medium agitating mill Measurement results of contact angle of powder cosmetics against water Measurement results of contact angle of powder cosmetics to oil Measurement results of contact angle of powder cosmetics against water Measurement results of contact angle of powder cosmetics against water Explanatory drawing regarding contact angle measurement in the present invention

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Medium stirring mill 12 Storage tank 14 Drying device 16 Housing | casing 18 Shearing means 20 Supply means 22 Blowing means 24 Collection means

Claims (6)

A slurry preparation step in which a powder component, an oily component as a binder, and an amino-modified silicone represented by the following general formula (1) as a dispersant are mixed in a volatile solvent to form a slurry, and the slurry is dried and dried and a drying step to obtain a powder, a method of producing a powder cosmetic to obtain a powder cosmetic from said dry powder, drying apparatus used in the drying step is to fine liquid droplets by a mechanical shearing force to the slurry and wherein the fine drying apparatus der of drying the slurry by blowing drying gas into fine droplets is, to obtain a powder cosmetic containing the amino-modified silicone 0.1 to 5.0 wt% A method for producing a powder cosmetic.

[A is -R ² NH ₂ or -R ² NHR ³ NH ₂ (where R ² and R ³ are alkylene groups having 1 to 8 carbon atoms), and R ¹ is an alkyl group having 1 to 30 carbon atoms. , A cycloalkyl group, an aryl group, an aralkyl group, and a fluorine-substituted alkyl group, each independently selected from the group consisting of m, an integer of 50 <m <400, and n is an integer of 1 <n <20 S and t are integers of 0 to 3 independently of each other. ] The manufacturing method according to claim 1,
The method for producing a powder cosmetic, wherein the amino-modified silicone is an aminoethylaminopropylmethylsiloxane / dimethylsiloxane copolymer represented by the following general formula (2).

[In Formula (2), m is an integer of 50 <m <400, and n is an integer of 1 <n <20. ] In the manufacturing method of Claim 1 or 2 ,
The drying device used in the drying step includes a hollow casing, a shearing means for shearing the slurry into a fine droplet by a shearing member provided in the casing, and a slurry to the shearing member in the casing A supply means for supplying air, a blowing means for blowing dry gas into the housing, and supplying and contacting the dry gas with the slurry made into fine droplets by the shearing means, and drying caused by drying the slurry A method for producing a powder cosmetic, comprising: a drying device comprising a collecting means for collecting powder. In the manufacturing method in any one of Claim 1 to 3 ,
In the slurry preparation step, using a medium stirring mill, a powder component and an oil component are mixed in a volatile solvent, and the powder component is crushed and / or pulverized and / or dispersed to obtain a slurry. A method for producing a powder cosmetic, which is characterized. In the manufacturing method in any one of Claim 1 to 4 ,
Powder cosmetics characterized in that powder components other than pearl pigments are made into dry powders by the slurry adjustment step and the drying step, and powder cosmetics are obtained using powders obtained by mixing the dry powders and pearl pigments Manufacturing method. In the manufacturing method in any one of Claim 1 to 5 ,
A method for producing a powder cosmetic, further comprising a solidification step of filling the dry powder and / or powder obtained by mixing the dry powder and a pearl pigment into a container and solidifying the powder by dry molding .

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