WO2014156805A1 - Magnetic powder for cosmetic agent - Google Patents
Magnetic powder for cosmetic agent Download PDFInfo
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- WO2014156805A1 WO2014156805A1 PCT/JP2014/057248 JP2014057248W WO2014156805A1 WO 2014156805 A1 WO2014156805 A1 WO 2014156805A1 JP 2014057248 W JP2014057248 W JP 2014057248W WO 2014156805 A1 WO2014156805 A1 WO 2014156805A1
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- magnetic powder
- cosmetics
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0216—Solid or semisolid forms
- A61K8/022—Powders; Compacted Powders
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/12—Face or body powders for grooming, adorning or absorbing
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/14—Preparations for removing make-up
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/47—Magnetic materials; Paramagnetic compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
Definitions
- the present invention relates to a magnetic powder for a cosmetic used in a cosmetic applied to the skin.
- a cosmetic agent that becomes a film after application can be easily separated from the skin by grasping and peeling off a part thereof.
- a method of removing from the skin what remains in the paste state even after application a method of wiping with cotton or the like, or washing off with warm water or the like is common.
- Patent Document 1 proposes a method in which a cosmetic agent mixed with iron powder and a remover provided with a magnet in the main body are used in combination.
- a cosmetic agent mixed with iron powder and a remover provided with a magnet in the main body are used in combination.
- the used beauty agent applied to the skin can be easily removed by magnetic force, and dirt and waste on the skin can be removed. Can be removed together with iron powder in cosmetics.
- Patent Documents 2 to 3 disclose examples of beauty agents that can be adsorbed and removed from the skin by magnetic force. These cosmetics are made by mixing iron powder or iron oxide with a cream-like base material containing nutritional components and the like. After the cosmetics are adsorbed and removed, the nutritional components remain on the skin surface. I am trying. Thereby, it is going to exhibit two effects, the effect
- the above-described problems caused by the oxidation of the iron powder can be solved to some extent.
- the reddish brown hematite (Fe 2 O 3 ) contained in the iron oxide makes the beauty agent mixed with magnetic powder reddish, so it is difficult to achieve a color tone that is preferable as a beauty agent. It was.
- the present invention has been made in view of such a background, and an object of the present invention is to provide an optimal magnetic powder for a cosmetic agent that can be adsorbed and removed from the cosmetic agent applied to the skin.
- One aspect of the present invention is a magnetic powder for cosmetics configured to be adsorbed and removed from a cosmetic applied to the skin,
- the magnetite content is 80% by mass or more, and the balance consists of wustite, hematite and inevitable impurities,
- the volume average particle size obtained from the particle size distribution obtained by the laser diffraction scattering method is 50 to 75 ⁇ m
- a magnetic powder for a cosmetic agent wherein the content of particles having a particle size of less than 37 ⁇ m is 15% by mass or less and the content of particles having a particle size of 105 ⁇ m or more is 5% by mass or less. is there.
- the magnetic powder for cosmetics is made of iron oxide. Therefore, after mixing with a beauty agent, it is hard to receive further oxidation, and the beauty agent which mixed the said magnetic powder for beauty agents becomes easy to suppress the dispersion
- the magnetic powder for cosmetics controls both the ratio of chemical components contained therein and the particle size distribution within the specific range.
- both the ease of adsorption of the magnetic powder for cosmetics from the skin and the good touch when touching the skin are achieved. It can be optimized at the same time, and the phenomenon of redness of the cosmetic can be suppressed.
- the magnetite content ratio is set to the specified value or more, and the volume average particle size of the magnetic powder for cosmetics is controlled to 50 ⁇ m or more, and the content of the small-sized particles is further set to the specified amount or less.
- the magnetic force acting on the entire magnetic powder for beauty agent can be increased.
- the user can efficiently adsorb and remove the magnetic powder for cosmetics from the skin.
- the said magnetic powder for cosmetics is hard to remain on the skin surface, it is not necessary to separately wash the face for removing the magnetic powder for cosmetics, and the convenience for the user can be improved.
- the magnetic powder for cosmetics is Roughness at the time of contact with the skin can be reduced.
- the beauty agent using the magnetic powder for beauty agent exhibits a smooth touch.
- the magnetic powder for cosmetics has optimum characteristics for inclusion in cosmetics that are adsorbed and removed from the skin.
- the magnetic powder for beauty agent is used by being mixed with a fluid beauty agent such as paste or liquid.
- the beauty agent contains various beauty components, and is configured to have a beauty effect such as replenishing nutrients to the skin or raising the dirt component of the skin.
- the cosmetic agent may be configured so that at least a part thereof remains on the skin surface when the magnetic powder for cosmetic agent is adsorbed and removed from the skin by a magnetic force according to the beauty effect to be obtained.
- the magnetic powder for beauty agent may be configured so that almost all is removed from the skin surface.
- magnetite Fe 3 O 4
- hematite Fe 2 O 3
- magnetite is a ferromagnetic material having ferrimagnetism
- hematite and wustite are antiferromagnetic materials. Therefore, by increasing the content of magnetite, a large magnetic force can be applied to the entire magnetic powder for beauty agent, and the adsorption removal of the beauty agent can be performed more efficiently.
- hematite exhibits a reddish brown color, it is possible to suppress the phenomenon that the cosmetic agent is reddish by reducing the content thereof. As described above, not only the control of chemical components but also the fine control of the particle size distribution allows these effects to be exhibited more reliably.
- the volume average particle diameter can be calculated as the cumulative 50% particle diameter (median diameter) obtained by the volume distribution mode and display under the sieve in the particle diameter distribution obtained by the laser diffraction scattering method.
- the content of particles having a particle size of less than 37 ⁇ m is measured, for example, as the amount of particles that can pass through a standard sieve having a nominal size of 37 ⁇ m (400 mesh). Can do.
- the content of particles having a particle size of 105 ⁇ m or more is measured, for example, as the amount of particles that cannot pass through a standard sieve having a nominal size of 105 ⁇ m (145 mesh). be able to.
- the volume average particle size is less than 50 ⁇ m
- the particle size distribution tends to have a large content of particles having an excessively small particle size.
- the magnetic force acting on individual particles becomes weaker as the particle size is smaller. Therefore, when many particles having an excessively small particle size are contained, the magnetic force acting on the entire beauty powder magnetic powder tends to be weakened, and the beauty powder magnetic powder may be difficult to be adsorbed and removed from the skin.
- the volume average particle size exceeds 75 ⁇ m
- the particle size distribution has a large content of particles having an excessively large particle size. Therefore, in this case, there is a possibility that the feeling of use is deteriorated, for example, the feel of the beauty agent mixed with the magnetic powder for beauty agent becomes worse.
- the volume average particle diameter of the magnetic powder for cosmetics is controlled within the above specific range, and further, by controlling both the content of the small particle and the content of the large particle, an appropriate size can be obtained. An optimal particle size distribution with an increased content of particles can be realized. Then, by finely controlling the particle size distribution as described above, by controlling the chemical component, the magnetic powder for cosmetics exhibits optimum characteristics for inclusion in the cosmetic.
- the magnetic powder for cosmetics preferably has a hematite content of 5% by mass or less.
- the ratio of the diamagnetic substance in the magnetic powder for cosmetics is reduced, it becomes easier to increase the magnetic force acting on the entire magnetic powder for cosmetics, and the adsorption and removal of the magnetic powder for cosmetics is more efficient. Can be done automatically.
- the content of red-brown hematite is reduced, it is possible to more reliably suppress the phenomenon that the cosmetic agent is reddish.
- the transmittance at a wavelength of 474 nm of the supernatant obtained by dispersing the magnetic powder for cosmetics in methanol is 90% or more.
- the transmittance of the supernatant liquid is mainly composed of hematite, and is used as a value indicating the content of particles having a particle size that is extremely small enough to disperse in methanol.
- the transmittance is 90% or more, it is possible to sufficiently reduce the content of the above-described particles having a very small particle diameter. Such particles having a very small particle size are not preferable because they are reduced in the adsorption and removal efficiency of the magnetic powder for cosmetics and cause the cosmetics to be reddish. In addition, the smaller the particle size, the easier it is to deteriorate the performance of the cosmetic magnetic powder. Therefore, by controlling the transmittance of the supernatant liquid as an index and controlling the value within the above specific range, it is possible to further improve the adsorption removal efficiency of the magnetic powder for cosmetics, and the phenomenon that the cosmetics become reddish. It can suppress more reliably.
- the content of wustite is preferably 15% by mass or less.
- the ratio of the diamagnetic substance in the magnetic powder for beauty agent is reduced, the magnetic force acting on the entire magnetic powder for beauty agent can be made stronger. As a result, it is possible to more efficiently adsorb and remove the magnetic powder for cosmetics.
- wustite has a lower degree of oxidation than magnetite and the like, reducing the wustite content makes the magnetic powder for cosmetics less susceptible to further oxidation. As a result, the performance of the magnetic powder for beauty agents can be stabilized for a longer period of time.
- the magnetic powder for beauty agents has a saturation magnetization of 80 Am 2 / kg or more.
- the magnetization of the magnetic powder for beauty agent can be sufficiently increased, and the magnetic force acting on the magnetic powder for beauty agent can be further increased.
- the magnetic powder for cosmetics can perform adsorption removal from the skin more efficiently.
- the cosmetic magnetic powder preferably has an apparent density of 1.95 to 2.65 g / cm 3 .
- the apparent density of the magnetic powder for beauty agents is a value used as an index of the average shape of the particles constituting the magnetic powder for beauty agents.
- the magnetic powder for cosmetics having a high apparent density tends to have a larger mass of individual particles than the magnetic powder for cosmetics having a low apparent density. Therefore, the magnetic force which acts on the whole magnetic powder for beauty agents tends to become large. As this cause, for example, when the apparent density is increased, the volume of the cavity existing inside the particle is decreased.
- the apparent density of the magnetic powder for beauty agents exceeds 2.65 g / cm 3 , the content of excessively large particles may increase. Therefore, there is a possibility that it is difficult to disperse uniformly in a state of being mixed with a cosmetic agent. In some cases, the magnetic powder for cosmetic agent may be precipitated during storage.
- the apparent density is less than 1.95 g / cm 3
- the uneven shape of the particles may become excessively large.
- the viscosity of the beauty agent may be increased, and in some cases, it may be difficult to apply to the skin.
- the apparent density is less than 1.95 g / cm 3
- the particles are likely to be fused excessively, and the unevenness of the particles may be excessively increased by the fusion as described above. Further, along with this, when the fused particles are crushed, the unevenness of the particles generated by the pulverization may become excessively large. Therefore, in this case, the ease of spreading when applying the cosmetic agent to the skin may be deteriorated, or the touch when applying the beauty agent may be deteriorated.
- the beauty powder magnetic powder preferably has a specific surface area of 200 to 450 cm 2 / g as measured using an air permeation method.
- the specific surface area of the magnetic powder for beauty agent is an index of the fine structure such as pores formed on the surface of the particles, and the larger the specific surface area value, the more pores and the like are formed.
- the specific surface area of the magnetic powder for beauty agents is less than 200 cm 2 / g, there is a possibility that fine structures such as pores are not sufficiently formed. Therefore, it is difficult for the cosmetic agent to be held on the surface of the particles, and it may be difficult to disperse in the cosmetic agent.
- the specific surface area of the magnetic powder for cosmetic agent exceeds 450 cm 2 / g, the fine structure may be excessively formed, and the cosmetic component may enter the fine structure. Therefore, the amount of cosmetic ingredients that can act directly on the skin is reduced, and the cosmetic effect may be reduced.
- the magnetic powder for beauty agent may be configured such that the magnetic powder for beauty agent can exhibit another function by a technique such as binding a cosmetic ingredient to the surface or applying a coating.
- functions to be applied to the magnetic powder for beauty agents include improving the dispersibility of the magnetic powder for beauty agents using a surfactant, etc., and using the magnetic powder for beauty agents using a resin component that adsorbs sebum For example, it is possible to absorb and remove sebum from the skin.
- the magnetic powder for cosmetics when the surface of the magnetic powder for cosmetics is modified with a surface modifier such as a coating agent, it is preferable that the magnetic powder for cosmetics contains a large number of particles with an appropriately large uneven shape. . Particles having a reasonably large uneven shape have a larger surface area than when the uneven shape is small, so that it is easy to retain the surface modifier. Therefore, the magnetic powder for cosmetics containing a large amount of such particles can more easily obtain the effect of surface modification by the surface modifier. On the other hand, when a large amount of particles such as a substantially spherical shape having a small concavo-convex shape are contained, the surface modifier is difficult to adhere to the individual particles, which may make it difficult to obtain the effect of surface modification.
- the apparent density is preferably 1.95 to 2.65 g / cm 3
- the specific surface area as measured by the air permeation method is 200 to 200 450cm is preferably 2 / g. If either one of the values of the apparent density and the specific surface area is in the above specific range, it is easy to obtain the surface modification effect, and if both satisfy the above specific range, the surface modification effect can be further obtained. It becomes easy.
- the magnetic powder for cosmetics contains inevitable impurities derived from raw materials and manufacturing processes in addition to magnetite, hematite, and wustite.
- Inevitable impurities include, for example, lead and arsenic, but their content is usually regulated to lead: 40 ppm or less and arsenic: 10 ppm or less.
- a method for producing the magnetic powder for cosmetics will be described.
- a method for producing the magnetic powder for beauty agent a conventionally known method can be employed.
- a method for performing classification treatment is mentioned.
- magnetite collected from natural ores including magnetite, iron oxide manufactured industrially, and the like can be used as a raw material for the magnetic powder for beauty agents.
- magnetite may be used as the raw material obtained by reducing the industrially produced hematite (Fe 2 O 3).
- hematite the purity and chemical components of the obtained magnetite can be easily adjusted.
- the quality of the magnetic powder for beauty agents can be more easily stabilized.
- hematite is reduced to magnetite by heating in a state where it coexists with a carbon component.
- This reaction theoretically follows the following reaction formula. 6Fe 2 O 3 + C ⁇ 4Fe 3 O 4 + CO 2 Therefore, in order to completely reduce hematite to magnetite, at least 1.25 parts by mass of carbon is required for 100 parts by mass of hematite. Under actual production conditions, hematite may not be completely reduced by blending according to the above reaction formula, so it is preferable to blend more than 1.25 parts by mass of carbon.
- the method of preparing the granulated product from the pulverized and mixed raw materials may be a dry method or a wet method.
- the wet method for example, the raw material and water are mixed and pulverized with a ball mill or the like, and then a dispersant, a binder or the like is added as necessary to adjust the viscosity to obtain a slurry-like mixture. Thereafter, the mixture can be granulated using a spray dryer.
- the granulated product is usually fired by heating at a temperature of 1100 to 1400 ° C. for 1 to 24 hours.
- a known furnace such as a rotary electric furnace, a batch electric furnace, a tunnel electric furnace, or the like can be used.
- the atmosphere during firing can be appropriately selected in consideration of the target degree of oxidation and magnetic characteristics.
- a known method such as air classification, mesh filtration, or sedimentation can be used.
- dry recovery it is also possible to recover with a cyclone or the like. It is also possible to combine a plurality of these classification methods. By performing the classification process using these methods, the particle size distribution of the magnetic powder for beauty agents can be adjusted to a desired distribution.
- magnetic separation may be performed as necessary. By performing magnetic separation, particles having a low magnetic susceptibility can be removed.
- the magnetic powder for cosmetics of this example is formed from magnetite exhibiting ferromagnetism. Further, as shown in Table 1, the magnetic powder for cosmetics of this example has a volume average particle size determined from the particle size distribution obtained by the laser diffraction scattering method of 50 to 75 ⁇ m and a particle size of less than 37 ⁇ m. The content of a certain particle (small particle) is 15% by mass or less, and the content of a particle (large particle) having a particle size of 105 ⁇ m or more is 5% by mass or less.
- the magnetic powder for beauty agent is used by being mixed with a paste-like beauty agent 1 applied to the skin as shown in FIG.
- the cosmetic agent 1 of this example is configured such that after the magnetic powder for cosmetic agent is adsorbed and removed from the skin by the magnetic force generated from the magnetic force generating surface 20 of the remover 2, the cosmetic components remain on the skin surface.
- various cosmetic magnetic powders (samples No. 1 to No. 15) shown in Table 1 were prepared by the following manufacturing method.
- the spherical granulated product whose particle size was adjusted was heated at 1320 ° C. for 3 hours to reduce the raw material hematite, and a fired product containing magnetite as a main component was obtained.
- the granulated product was heated in a nitrogen atmosphere using a tunnel electric furnace.
- a classification treatment was performed by using a combination of a gyro shifter and an air classifier to adjust the particle size distribution. Thereafter, magnetic separation was carried out to select particles having a high magnetic susceptibility, and a magnetic powder for cosmetics (sample No. 1) containing magnetite as a main component was obtained.
- Sample No. 1 In the production method of No. 1, sample No. 1 was changed by appropriately changing the amount of carbon black to be added, heating conditions, and classification conditions. 2 to No. 13 was obtained.
- the spherical granulated product whose particle size was adjusted was heated at 1310 ° C. for 3 hours to react hematite and trimanganese tetroxide to obtain a fired product mainly composed of Mn ferrite.
- the granulated product was heated in a nitrogen atmosphere using a tunnel electric furnace.
- a classification treatment was performed by using a combination of a gyro shifter and an air classifier to adjust the particle size distribution. Thereafter, magnetic separation was carried out to select particles having a high magnetic susceptibility, and a magnetic powder for cosmetics (sample No. 15) mainly composed of Mn ferrite was obtained.
- ⁇ Volume average particle diameter> After adding 0.2% sodium hexametaphosphate aqueous solution to the sample, ultrasonic treatment is performed for 1 minute using an ultrasonic homogenizer (UH-3C, manufactured by Ultrasonic Industry Co., Ltd.) to obtain a magnetic powder dispersion for cosmetics. Prepared. This dispersion was introduced into a Microtrac particle size analyzer (manufactured by Nikkiso Co., Ltd., Model 9320-X100) and measured under conditions of a refractive index of 1.81, a temperature of 25 ⁇ 5 ° C., and a humidity of 55 ⁇ 15%, and laser diffraction. The particle size distribution by the scattering method was obtained. From the obtained particle size distribution, the 50% cumulative particle size in the volume distribution mode and under the sieve display was calculated, and this was defined as the volume average particle size (median diameter).
- UH-3C Ultrasonic Industry Co., Ltd.
- ⁇ Apparent density> In accordance with the apparent density test method for metal powder specified in JIS Z 2504, measurement was performed by the following method.
- a device comprising a funnel, a cup, a funnel support, a support bar and a support base having an orifice with a pore diameter of 2.5 + 0.2 / 0 mm was used.
- a horizontal spatula formed of a nonmagnetic material was moved horizontally along the opening surface of the cup, and the sample raised on the cup was scraped off. Thereafter, the side of the cup was lightly tapped to stabilize the sample, and the sample adhering to the side of the cup was wiped off, and then the weight of the sample in the cup was weighed using a balance having a weight of 200 g and a sensitivity of 50 mg.
- the value obtained by multiplying the obtained weight value by 0.04 and rounding this value to the second decimal place using the rounding method defined in JIS Z 8401 is the apparent density (g / cm 3 ). did.
- Saturation magnetization, residual magnetization and coercive force were read from this hysteresis loop. Saturation magnetization, residual magnetization, and coercive force were measured by filling a cell having an inner diameter of 7 mm ⁇ ⁇ 0.02 mm and a height of 10 mm ⁇ 0.1 mm with a sample of about 1 g, 4 ⁇ I coil: 30 turns, applied magnetic field: 3000 oersted. Performed under conditions.
- ⁇ in the equation (1) is the porosity of the sample packed layer obtained by the following equation (2).
- ⁇ Magnetite composition ratio> For cosmetic agent magnetic powder mainly composed of magnetite, magnetite by X-ray diffraction method (Fe 3 O 4), the composition ratio of hematite (Fe 2 O 3) and wustite (FeO) was calculated by the following method.
- X'PertPRO MPD manufactured by Panalical Co., Ltd. was used as a measuring apparatus. Measurement was performed by continuous scanning at 0.2 ° / sec using a Co tube (CoK ⁇ ray) as an X-ray source and a concentrated optical system and a high-speed detector “X′Celarator” as an optical system. Analysis of the measurement results is performed in the same way as ordinary powder crystal structure analysis using the analysis software “X'PertHighScore”. After identifying the crystal structure, the obtained crystal structure is refined and converted to weight. The abundance ratio was calculated. In calculating the abundance ratio, the abundance ratios of magnetite, hematite, and wustite were calculated using Fe and O as essential elements.
- the X-ray source used for X-ray diffraction measurement can be measured without problems even with a Cu tube, but in the case of a sample containing a large amount of Fe, the background becomes larger than the peak to be measured, so the Co tube Is preferred. Further, the optical system may obtain the same result even when the parallel method is used. However, since the X-ray intensity is low and the measurement takes time, the measurement with the concentrated optical system is preferable. Further, the speed of the continuous scan is not particularly limited, but in order to obtain a sufficient S / N ratio when analyzing the crystal structure, the peak intensity of the (311) plane which is the main peak of magnetite is set to 50000 cps or more. The measurement was performed by setting the sample in the sample cell so that the particles were not oriented in a specific preferred direction.
- Table 1 shows various properties of the magnetic powder for cosmetics evaluated by the above methods.
- -Magnetic powder for beauty agents 60.0% by mass ⁇ Glycerin 20.0% by mass ⁇ Methylparaben 0.38% by mass ⁇ Decamethylcyclopentasiloxane 1.3% by mass ⁇ Trioctylglyceryl 3.8% by mass ⁇ Cetyl 2-ethylhexanoate 3.8% by mass ⁇ Bentonite 0.19% by mass ⁇ Polyoxyethylene / methylpolysiloxane copolymer 2.25% by mass ⁇ Polyglyceryl monolaurate 0.25% by mass -Sodium polyacrylate 0.01% by mass ⁇ Sodium hydroxide 0.03% by mass ⁇ Sodium ascorbate 0.13 mass% ⁇ Perfume 0.13 mass% ⁇ Water balance
- a beauty agent mixed with magnetic powder for beauty agent was applied to a flat plate placed on a horizontal surface.
- the height from the flat plate to the test head when the magnetic powder for cosmetics was adsorbed on the test head was measured from the top of the cosmetic applied with the test head containing the neodymium magnet. It is shown in the column of “Adsorption distance”.
- the value described in Table 2 indicates that the larger the magnetic powder for cosmetic agent is, the easier it is to remove by adsorption.
- the neodymium magnet built in the test head was a cylinder with a diameter of about 25 mm and a height of about 8 mm, and the surface magnetic flux density of the magnet alone was 266 mT. Further, a 2 mm-thick yoke material having a disk shape was disposed on the end face facing upward of the neodymium magnet.
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Abstract
Description
マグネタイトの含有量が80質量%以上であり、残部がウスタイト、ヘマタイト及び不可避不純物からなり、
レーザー回折散乱法により得られる粒径分布から求めた体積平均粒径が50~75μmであり、
粒径が37μm未満である粒子の含有量が15質量%以下であり、かつ、粒径が105μm以上である粒子の含有量が5質量%以下であることを特徴とする美容剤用磁性粉にある。 One aspect of the present invention is a magnetic powder for cosmetics configured to be adsorbed and removed from a cosmetic applied to the skin,
The magnetite content is 80% by mass or more, and the balance consists of wustite, hematite and inevitable impurities,
The volume average particle size obtained from the particle size distribution obtained by the laser diffraction scattering method is 50 to 75 μm,
A magnetic powder for a cosmetic agent, wherein the content of particles having a particle size of less than 37 μm is 15% by mass or less and the content of particles having a particle size of 105 μm or more is 5% by mass or less. is there.
6Fe2O3 + C → 4Fe3O4 + CO2
従って、ヘマタイトを完全にマグネタイトに還元するためには、100質量部のヘマタイトに対して少なくとも1.25質量部の炭素が必要となる。実際の製造条件においては、上記の反応式に従った配合ではヘマタイトが完全には還元されない場合があるため、炭素を1.25質量部よりも多く配合することが好ましい。 For example, hematite is reduced to magnetite by heating in a state where it coexists with a carbon component. This reaction theoretically follows the following reaction formula.
6Fe 2 O 3 + C → 4Fe 3 O 4 + CO 2
Therefore, in order to completely reduce hematite to magnetite, at least 1.25 parts by mass of carbon is required for 100 parts by mass of hematite. Under actual production conditions, hematite may not be completely reduced by blending according to the above reaction formula, so it is preferable to blend more than 1.25 parts by mass of carbon.
ヘマタイト(Fe2O3)を粉砕した粉末に対し、固形分が55質量%となるように水を加えてスラリーを調製した。次いで、得られたスラリーの固形分に対して1質量%のポリビニルアルコールと、0.9質量%のカーボンブラックと、0.5質量%のポリカルボン酸塩とをスラリーに加えた後、この混合物に水を加えて固形分が55質量%のスラリーを調製した。次いで、アトライターを用いて得られたスラリーを1時間攪拌した。その後、スプレードライヤーを用いてスラリーを球状に造粒し、ジャイロシフターを用いて得られた造粒物の粒度調整を行った。 <Method for producing magnetic powder for beauty agent mainly composed of magnetite>
Water was added to the powder obtained by pulverizing hematite (Fe 2 O 3 ) so that the solid content was 55% by mass to prepare a slurry. Next, after adding 1% by weight of polyvinyl alcohol, 0.9% by weight of carbon black, and 0.5% by weight of polycarboxylate salt to the solid content of the obtained slurry, this mixture was added. Water was added to the slurry to prepare a slurry having a solid content of 55% by mass. Subsequently, the slurry obtained using an attritor was stirred for 1 hour. Thereafter, the slurry was granulated into a spherical shape using a spray dryer, and the particle size of the granulated product obtained using a gyro shifter was adjusted.
ヘマタイト及び四酸化三マンガンをMnO:20mol%、Fe2O3:80mol%となるように秤量し、湿式のメディアミルで1時間粉砕してスラリーを得た。得られたスラリーをスプレードライヤーにて乾燥し、球状の造粒物を得た。次いで、ジャイロシフターを用いて得られた造粒物の粒度調整を行った後、950℃で2時間加熱することにより仮焼成を行った。 <Method for Producing Magnetic Powder for Beauty Agent with Mn Ferrite as Main Component>
Hematite and trimanganese tetroxide were weighed so as to be MnO: 20 mol% and Fe 2 O 3 : 80 mol%, and pulverized with a wet media mill for 1 hour to obtain a slurry. The obtained slurry was dried with a spray dryer to obtain a spherical granulated product. Subsequently, after adjusting the particle size of the granulated product obtained using a gyro shifter, it was calcined by heating at 950 ° C. for 2 hours.
試料に0.2%ヘキサメタリン酸ナトリウム水溶液を加えた後、ウルトラソニックホモジナイザー(超音波工業社製、UH-3C)を用いて1分間の超音波処理を行って美容剤用磁性粉の分散液を調製した。この分散液をマイクロトラック粒度分析計(日機装株式会社製、Model9320-X100)に導入し、屈折率1.81、温度25±5℃、湿度55±15%の条件下で測定を行い、レーザー回折散乱法による粒径分布を得た。得られた粒径分布から、体積分布モード、ふるい下表示での累積50%粒子径を算出し、これを体積平均粒径(メジアン径)とした。 <Volume average particle diameter>
After adding 0.2% sodium hexametaphosphate aqueous solution to the sample, ultrasonic treatment is performed for 1 minute using an ultrasonic homogenizer (UH-3C, manufactured by Ultrasonic Industry Co., Ltd.) to obtain a magnetic powder dispersion for cosmetics. Prepared. This dispersion was introduced into a Microtrac particle size analyzer (manufactured by Nikkiso Co., Ltd., Model 9320-X100) and measured under conditions of a refractive index of 1.81, a temperature of 25 ± 5 ° C., and a humidity of 55 ± 15%, and laser diffraction. The particle size distribution by the scattering method was obtained. From the obtained particle size distribution, the 50% cumulative particle size in the volume distribution mode and under the sieve display was calculated, and this was defined as the volume average particle size (median diameter).
JIS Z 8801に規定される標準ふるいを用いて、JIS H 2601に準じた方法により試料の分級を行った。これにより、呼び寸法37μm(400メッシュ)の標準ふるいを通過した粒子(小径粒子)の含有量及び呼び寸法105μm(145メッシュ)の標準ふるいを通過しなかった粒子(大径粒子)の含有量を測定した。 <Content of small particle and content of large particle>
Using a standard sieve defined in JIS Z 8801, the samples were classified by a method according to JIS H 2601. Thereby, the content of particles (small particle) that passed through a standard sieve having a nominal size of 37 μm (400 mesh) and the content of particles (large particle) that did not pass through the standard sieve having a nominal size of 105 μm (145 mesh) were obtained. It was measured.
JIS Z 2504に規定される金属粉の見掛密度試験方法に準じて、以下の方法により測定を行った。見掛密度の測定装置は、孔径2.5+0.2/0mmのオリフィスを有する漏斗、コップ、漏斗支持器、支持棒及び支持台からなるものを用いた。まず、少なくとも150gの試料を漏斗に注ぎ、漏斗から流れ出す試料を漏斗の下方に設置したコップに直接流し入れた。コップが試料で満たされた後、試料がコップからあふれ出した時点で直ちに試料の流入を止めた。 <Apparent density>
In accordance with the apparent density test method for metal powder specified in JIS Z 2504, measurement was performed by the following method. As an apparent density measuring device, a device comprising a funnel, a cup, a funnel support, a support bar and a support base having an orifice with a pore diameter of 2.5 + 0.2 / 0 mm was used. First, at least 150 g of sample was poured into the funnel and the sample flowing out of the funnel was poured directly into a cup placed under the funnel. After the cup was filled with the sample, the sample flow was stopped immediately when the sample overflowed from the cup.
積分型B-Hトレーサー((株)理研電子製、BHU-60型)を使用して以下の手順で測定した。まず、電磁石間に磁場測定用Hコイル及び磁化測定用4πIコイルを入れ、試料を4πIコイル内に入れる。次いで、電磁石の電流を変化させ磁場Hを変化させたHコイル及び4πIコイルの出力をそれぞれ積分し、X軸にH出力をとり、Y軸に4πIコイルの出力をとったヒステリシスループを記録紙に描く。このヒステリシスループから飽和磁化、残留磁化及び保磁力を読み取った。飽和磁化、残留磁化及び保磁力の測定は、内径7mmφ±0.02mm、高さ10mm±0.1mmのセルに約1gの試料を充填し、4πIコイル:巻数30回、印加磁場:3000エルステッドの条件で行った。 <Saturation magnetization, residual magnetization and coercivity>
Measurement was carried out by the following procedure using an integral type BH tracer (manufactured by Riken Denshi Co., Ltd., BHU-60 type). First, an H coil for magnetic field measurement and a 4πI coil for magnetization measurement are placed between electromagnets, and a sample is placed in the 4πI coil. Next, the output of the H coil and the 4πI coil whose magnetic field H is changed by changing the current of the electromagnet is integrated, the H output is taken on the X axis, and the hysteresis loop taking the output of the 4πI coil on the Y axis is applied to the recording paper. Draw. Saturation magnetization, residual magnetization and coercive force were read from this hysteresis loop. Saturation magnetization, residual magnetization, and coercive force were measured by filling a cell having an inner diameter of 7 mmφ ± 0.02 mm and a height of 10 mm ± 0.1 mm with a sample of about 1 g, 4πI coil: 30 turns, applied magnetic field: 3000 oersted. Performed under conditions.
15gの試料を秤量し、これを50mlのサンプル瓶に入れた。このサンプル瓶に20mlのメタノールを加えて蓋をした後、回転式撹拌機を用いて150rpmで20分間撹拌を行った。撹拌が完了した後、サンプル瓶の底に磁石を当接させて試料を吸着させ、この状態でサンプル瓶を手で3回振り混ぜた。その後、サンプル瓶の上澄み液を3ml採取し、可視分光光度計(オガワ精機社製、Model6100)を用いて波長474nmにおける上澄み液の透過率を測定した。なお、透過率の測定におけるブランクサンプルとしては、メタノールを用いた。 <Supernatant transmittance>
A 15 g sample was weighed and placed in a 50 ml sample bottle. After adding 20 ml of methanol to the sample bottle and capping, the sample bottle was stirred at 150 rpm for 20 minutes using a rotary stirrer. After the stirring was completed, a sample was adsorbed by bringing a magnet into contact with the bottom of the sample bottle, and in this state, the sample bottle was shaken three times by hand. Thereafter, 3 ml of the supernatant of the sample bottle was collected, and the transmittance of the supernatant at a wavelength of 474 nm was measured using a visible spectrophotometer (Ogawa Seiki, Model 6100). In addition, methanol was used as a blank sample in the transmittance measurement.
試料をプラスチック製試料筒に充填した後、粉体比表面積測定装置(島津製作所製、SS-100型)を用いて空気透過法による比表面積を測定した。より具体的な試料の充填方法及び測定手順は、以下の通りである。 <Specific surface area>
After filling the sample into a plastic sample tube, the specific surface area was measured by an air permeation method using a powder specific surface area measuring device (SS-100 model, manufactured by Shimadzu Corporation). A more specific sample filling method and measurement procedure are as follows.
プラスチック製試料筒にふるい板を入れ、更にその上にろ紙を1枚敷いた状態で試料筒をパウダーテスター(ホソカワミクロン社製)のタップ架台に設置した。次いで、試料を試料筒の1/3程度まで注ぎ入れ、パウダーテスターを作動させて試料筒を60秒間タップした。タップ後、試料筒の2/3程度まで試料を注ぎ足し、再度パウダーテスターを作動させて試料筒を60秒間タップした。その後、試料筒を満たすまで試料を注ぎ足し、パウダーテスターを作動させて試料筒を60秒間タップした。3回目のタップが完了した後、試料筒に付着した余分な試料を刷毛やワイパー等を用いて除去し、試料の充填を完了した。 (1) Filling of sample A sieve plate was placed in a plastic sample tube, and a filter paper was further laid on the sieve plate, and the sample tube was placed on a tap stand of a powder tester (manufactured by Hosokawa Micron). Next, the sample was poured into about 1/3 of the sample tube, the powder tester was activated, and the sample tube was tapped for 60 seconds. After tapping, the sample was poured to about 2/3 of the sample tube, the powder tester was operated again, and the sample tube was tapped for 60 seconds. Thereafter, the sample was added until the sample tube was filled, the powder tester was operated, and the sample tube was tapped for 60 seconds. After the third tap was completed, the excess sample adhering to the sample tube was removed using a brush, a wiper or the like, and the sample filling was completed.
試料筒の下部にワセリンを塗布し、この部分を測定管に接続した後、測定管に純水を注入した。次いで、測定装置の下部流出口のコックを開いて純水を測定管から流出させ、測定管内の水位が20cc分だけ低下するまでの時間tを測定した。これにより得られた、20ccの空気が試料充填層を透過するまでに要する時間t(sec)と、試料管内に充填した試料の重量W(g)とをKozeny-Carmanの式(下記式(1)参照)に代入し、試料の比表面積Swを求めた。 (2) Measurement of specific surface area Vaseline was applied to the lower part of the sample tube, and after connecting this part to the measurement tube, pure water was injected into the measurement tube. Next, the cock at the lower outlet of the measuring device was opened to allow pure water to flow out of the measuring tube, and the time t until the water level in the measuring tube decreased by 20 cc was measured. The time t (sec) required for 20 cc of air thus obtained to permeate the sample packed bed and the weight W (g) of the sample filled in the sample tube are expressed by the Kozeny-Carman equation (the following equation (1) The specific surface area Sw of the sample was determined.
試料の比表面積:Sw(cm2/g)
試料の密度:ρ(g/cm3)
空気の粘性係数:η(g/cm・sec)
試料充填層の厚さ:L(cm)
試料充填層を透過した空気の体積:Q(cc)
試料充填層の両端間の圧力差:ΔP(g/cm2)
試料充填層の断面積:A(cm2) The meanings of the other symbols in the above formulas (1) and (2) are as follows.
Specific surface area of sample: Sw (cm 2 / g)
Sample density: ρ (g / cm 3 )
Air viscosity coefficient: η (g / cm · sec)
Sample packed layer thickness: L (cm)
Volume of air that has passed through the sample packed bed: Q (cc)
Pressure difference between both ends of sample packed bed: ΔP (g / cm 2 )
Cross-sectional area of sample packed layer: A (cm 2 )
マグネタイトを主成分とする美容剤用磁性粉について、X線回折法によるマグネタイト(Fe3O4)、ヘマタイト(Fe2O3)及びウスタイト(FeO)の組成比を以下の方法で算出した。 <Magnetite composition ratio>
For cosmetic agent magnetic powder mainly composed of magnetite, magnetite by X-ray diffraction method (Fe 3 O 4), the composition ratio of
・美容剤用磁性粉 60.0質量%
・グリセリン 20.0質量%
・メチルパラベン 0.38質量%
・デカメチルシクロペンタシロキサン 1.3質量%
・トリオクチルグリセリル 3.8質量%
・2-エチルヘキサン酸セチル 3.8質量%
・ベントナイト 0.19質量%
・ポリオキシエチレン・メチルポリシロキサン共重合体 2.25質量%
・モノラウリン酸ポリグリセリル 0.25質量%
・ポリアクリル酸ナトリウム 0.01質量%
・水酸化ナトリウム 0.03質量%
・アスコルビン酸リン酸ナトリウム 0.13質量%
・香料 0.13質量%
・水 残部 In addition, the cosmetics which have the following compositions were used for the said characteristic evaluation.
-Magnetic powder for beauty agents 60.0% by mass
・ Glycerin 20.0% by mass
・ Methylparaben 0.38% by mass
・ Decamethylcyclopentasiloxane 1.3% by mass
・ Trioctylglyceryl 3.8% by mass
・ Cetyl 2-ethylhexanoate 3.8% by mass
・ Bentonite 0.19% by mass
・ Polyoxyethylene / methylpolysiloxane copolymer 2.25% by mass
・ Polyglyceryl monolaurate 0.25% by mass
-Sodium polyacrylate 0.01% by mass
・ Sodium hydroxide 0.03% by mass
・ Sodium ascorbate 0.13 mass%
・ Perfume 0.13 mass%
・ Water balance
水平面に載置した平板状に美容剤用磁性粉を混合した美容剤を塗布した。ネオジム磁石を内蔵した試験ヘッドを塗布した美容剤の上方から近づけ、美容剤用磁性粉が試験ヘッドに吸着された時点における平板から試験ヘッドまでの高さを測定し、その値を表2中の「吸着距離」の欄に示した。表2に記載した値は、大きいほど美容剤用磁性粉が吸着除去されやすいことを示す。なお、試験ヘッドに内蔵したネオジム磁石は、直径約25mm、高さ約8mmの円筒状であり、磁石単体での表面磁束密度は266mTであった。また、ネオジム磁石の上方を向いた端面に円板状を呈する厚さ2mmのヨーク材を配して用いた。 <Adsorption removal>
A beauty agent mixed with magnetic powder for beauty agent was applied to a flat plate placed on a horizontal surface. The height from the flat plate to the test head when the magnetic powder for cosmetics was adsorbed on the test head was measured from the top of the cosmetic applied with the test head containing the neodymium magnet. It is shown in the column of “Adsorption distance”. The value described in Table 2 indicates that the larger the magnetic powder for cosmetic agent is, the easier it is to remove by adsorption. The neodymium magnet built in the test head was a cylinder with a diameter of about 25 mm and a height of about 8 mm, and the surface magnetic flux density of the magnet alone was 266 mT. Further, a 2 mm-thick yoke material having a disk shape was disposed on the end face facing upward of the neodymium magnet.
美容剤を手の甲に塗布したときの肌触りを評価し、表2に示した。なお、表2に示す各記号の意味は、以下の通りである。
A:ざらつき感は全く感じられない
B:ざらつき感はほとんど感じられない
C:ざらつき感を感じるが、塗り広げることはできる
D:ざらつき感を感じ、塗り広げることができない <Feel>
The feel when the cosmetic agent was applied to the back of the hand was evaluated and is shown in Table 2. In addition, the meaning of each symbol shown in Table 2 is as follows.
A: Feeling of roughness is not felt at all B: Feeling of roughness is hardly felt C: Feeling of roughness is felt but can be spread D: Feeling of roughness is felt
測色色差計(日本電色工業株式会社製、型式「ZE 2000」)を用いて美容剤用磁性粉のL値(明度)、a値(緑~赤の色度)、b値(青~黄の色度)を測定し、各々の値を表2に示した。なお、測定には、5gの美容剤用磁性粉を用いた。 <Color tone>
Using a colorimetric color difference meter (manufactured by Nippon Denshoku Industries Co., Ltd., model “ZE 2000”), the L value (lightness), a value (green to red chromaticity), b value (blue to Yellow chromaticity) was measured and the respective values are shown in Table 2. For the measurement, 5 g of magnetic powder for cosmetics was used.
Claims (7)
- 肌に塗布された美容剤から磁力により吸着除去可能に構成された美容剤用磁性粉であって、
マグネタイトの含有量が80質量%以上であり、残部がウスタイト、ヘマタイト及び不可避不純物からなり、
レーザー回折散乱法により得られる粒径分布から求めた体積平均粒径が50~75μmであり、
粒径が37μm未満である粒子の含有量が15質量%以下であり、かつ、粒径が105μm以上である粒子の含有量が5質量%以下であることを特徴とする美容剤用磁性粉。 It is a magnetic powder for cosmetics that can be adsorbed and removed by magnetic force from the cosmetics applied to the skin,
The magnetite content is 80% by mass or more, and the balance consists of wustite, hematite and inevitable impurities,
The volume average particle size obtained from the particle size distribution obtained by the laser diffraction scattering method is 50 to 75 μm,
A magnetic powder for cosmetics, wherein the content of particles having a particle size of less than 37 μm is 15% by mass or less, and the content of particles having a particle size of 105 μm or more is 5% by mass or less. - 請求項1に記載の美容剤用磁性粉において、ヘマタイトの含有量が5質量%以下であることを特徴とする美容剤用磁性粉。 The magnetic powder for cosmetics according to claim 1, wherein the hematite content is 5% by mass or less.
- 請求項1または2に記載の美容剤用磁性粉において、該美容剤用磁性粉をメタノールに分散させて得られる上澄み液の、波長474nmにおける透過率が90%以上であることを特徴とする美容剤用磁性粉。 The cosmetic magnetic powder according to claim 1 or 2, wherein the transmittance at a wavelength of 474 nm of a supernatant obtained by dispersing the cosmetic magnetic powder in methanol is 90% or more. Magnetic powder for agent.
- 請求項1~3のいずれか1項に記載の美容剤用磁性粉において、ウスタイトの含有量が15質量%以下であることを特徴とする美容剤用磁性粉。 The magnetic powder for cosmetics according to any one of claims 1 to 3, wherein the content of wustite is 15% by mass or less.
- 請求項1~4のいずれか1項に記載の美容剤用磁性粉において、飽和磁化が80Am2/kg以上であることを特徴とする美容剤用磁性粉。 The magnetic powder for cosmetics according to any one of claims 1 to 4, wherein the saturation magnetization is 80 Am 2 / kg or more.
- 請求項1~5のいずれか1項に記載の美容剤用磁性粉において、見掛密度が1.95~2.65g/cm3であることを特徴とする美容剤用磁性粉。 6. The cosmetic magnetic powder according to claim 1, wherein the apparent density is 1.95 to 2.65 g / cm 3 .
- 請求項1~6のいずれか1項に記載の美容剤用磁性粉において、空気透過法を用いて測定したときの表面積が200~450cm2/gであることを特徴とする美容剤用磁性粉。 The magnetic powder for cosmetics according to any one of claims 1 to 6, wherein the magnetic powder for cosmetics has a surface area of 200 to 450 cm 2 / g as measured using an air permeation method. .
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- 2014-03-18 JP JP2015508337A patent/JP6363063B2/en active Active
- 2014-03-18 CN CN201480014147.4A patent/CN105188640A/en active Pending
- 2014-03-18 WO PCT/JP2014/057248 patent/WO2014156805A1/en active Application Filing
- 2014-03-27 TW TW103111487A patent/TWI627969B/en not_active IP Right Cessation
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPWO2014156804A1 (en) * | 2013-03-29 | 2017-02-16 | 株式会社 Mtg | Magnetic powder for beauty agents |
JP2016540735A (en) * | 2013-10-22 | 2016-12-28 | ユニリーバー・ナームローゼ・ベンノートシヤープ | Composition |
WO2015079942A1 (en) * | 2013-11-29 | 2015-06-04 | 株式会社 Mtg | Water-based skin care agent |
JP2015127327A (en) * | 2013-11-29 | 2015-07-09 | 株式会社 Mtg | Aqueous skin care preparation |
JPWO2015079942A1 (en) * | 2013-11-29 | 2017-03-16 | 株式会社 Mtg | Water-based skin care agent |
US10932997B2 (en) | 2013-11-29 | 2021-03-02 | Mtg Co., Ltd. | Aqueous skin care agent |
JP2015120649A (en) * | 2013-12-20 | 2015-07-02 | 株式会社 Mtg | Skin care agent |
Also Published As
Publication number | Publication date |
---|---|
JP6363063B2 (en) | 2018-07-25 |
CN105188640A (en) | 2015-12-23 |
TW201517926A (en) | 2015-05-16 |
TWI627969B (en) | 2018-07-01 |
JPWO2014156805A1 (en) | 2017-02-16 |
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