WO2022264327A1 - 六方晶窒化ホウ素粉末及びその製造方法、並びに化粧料及びその製造方法 - Google Patents
六方晶窒化ホウ素粉末及びその製造方法、並びに化粧料及びその製造方法 Download PDFInfo
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- WO2022264327A1 WO2022264327A1 PCT/JP2021/022907 JP2021022907W WO2022264327A1 WO 2022264327 A1 WO2022264327 A1 WO 2022264327A1 JP 2021022907 W JP2021022907 W JP 2021022907W WO 2022264327 A1 WO2022264327 A1 WO 2022264327A1
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- boron nitride
- hexagonal boron
- powder
- nitride powder
- cosmetics
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims abstract description 113
- 239000002537 cosmetic Substances 0.000 title claims description 43
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- 238000000034 method Methods 0.000 title description 21
- 229910052582 BN Inorganic materials 0.000 claims abstract description 36
- 239000011163 secondary particle Substances 0.000 claims abstract description 36
- 239000002245 particle Substances 0.000 claims abstract description 34
- 239000011164 primary particle Substances 0.000 claims abstract description 26
- 238000009826 distribution Methods 0.000 claims abstract description 13
- 230000001186 cumulative effect Effects 0.000 claims abstract description 7
- 238000007561 laser diffraction method Methods 0.000 claims abstract description 6
- 238000000790 scattering method Methods 0.000 claims abstract description 6
- 230000004931 aggregating effect Effects 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 41
- 239000002994 raw material Substances 0.000 claims description 30
- 238000000137 annealing Methods 0.000 claims description 28
- 238000010304 firing Methods 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 239000012752 auxiliary agent Substances 0.000 claims description 10
- 230000002776 aggregation Effects 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 238000004220 aggregation Methods 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- -1 nitrogen-containing compound Chemical class 0.000 claims description 2
- 238000005121 nitriding Methods 0.000 claims 1
- 239000000047 product Substances 0.000 description 20
- 230000008569 process Effects 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 8
- 239000011362 coarse particle Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 229910001873 dinitrogen Inorganic materials 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 230000004313 glare Effects 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 2
- 229910052808 lithium carbonate Inorganic materials 0.000 description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010908 decantation Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 235000011182 sodium carbonates Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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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
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/064—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with boron
- C01B21/0648—After-treatment, e.g. grinding, purification
-
- 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
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
-
- 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
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
- A61Q1/10—Preparations containing skin colorants, e.g. pigments for eyes, e.g. eyeliner, mascara
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Definitions
- the present disclosure relates to a hexagonal boron nitride powder and a method for producing the same, as well as a cosmetic and a method for producing the same.
- Boron nitride has lubricating properties, high thermal conductivity, insulating properties, etc., and is used as a raw material for solid lubricants, release agents, resin and rubber fillers, cosmetics (also called cosmetics), and heat resistance. It is used for a wide range of applications such as insulating sintered bodies with
- hexagonal boron nitride powder that is blended in cosmetics include improving the slipperiness, spreadability, and concealability of cosmetics, and imparting gloss.
- hexagonal boron nitride powder has excellent lubricity as compared with talc powder and mica powder, which have similar functions, and is therefore widely used in cosmetics that require excellent lubricity.
- Patent Literature 1 proposes setting the average particle size and the maximum particle size within predetermined numerical ranges in order to improve the lubricity of the hexagonal boron nitride powder.
- the present disclosure provides a hexagonal boron nitride powder and a method for producing the same that enable the production of cosmetics with excellent elongation.
- the present disclosure provides a cosmetic having excellent spreadability by using the hexagonal boron nitride powder described above, and a method for producing the same.
- the hexagonal boron nitride powder according to one aspect of the present disclosure includes secondary particles formed by agglomeration of primary particles of hexagonal boron nitride, and is measured by a laser diffraction/scattering method.
- D50 is 3 to 30 ⁇ m
- D90 /D10 is 4.0 or more.
- the hexagonal boron nitride powder Since the hexagonal boron nitride powder has a D50 of 3 to 30 ⁇ m, it contains primary particles having a size suitable for elongation. As described above, the primary particles have a size suitable for elongation, but the D90/D10 is large, so the volume ratio of the secondary particles formed by agglomeration of the primary particles can be increased. Secondary particles can have larger voids within the particles than primary particles. Therefore, a hexagonal boron nitride powder having a large volume fraction of secondary particles is bulky and has a fluffy appearance. When such a hexagonal boron nitride powder is spread, it is spread while the agglomerated secondary particles are broken. Therefore, it has excellent extensibility. Such a hexagonal boron nitride powder is suitable as a raw material for cosmetics.
- the D90/D50 of the hexagonal boron nitride powder may be 1.7 or more.
- the ratio of the secondary particles can be further increased, and the elongation-improving effect of the secondary particles during spreading can be further increased. Therefore, it is possible to obtain a hexagonal boron nitride powder having even better elongation.
- the D90 of the hexagonal boron nitride powder may be 50 ⁇ m or less. As a result, coarse particles formed by excessive aggregation of primary particles can be reduced, and rough feeling can be reduced when used as a raw material for cosmetics.
- the hexagonal boron nitride powder may be used as a raw material for cosmetics.
- the hexagonal boron nitride powder is excellent in extensibility, and therefore suitable as a raw material for cosmetics.
- a method for producing a hexagonal boron nitride powder is to prepare a raw material powder containing a boron-containing compound powder and a nitrogen-containing compound powder in an atmosphere of an inert gas, an ammonia gas, or a mixed gas thereof.
- the above production method includes a calcining step of firing at a temperature lower than that of the firing step, and a firing step of firing using an auxiliary agent, thereby producing primary particles of hexagonal boron nitride having a small particle size and high crystallinity. can be formed. Further, the refining process reduces the amount of auxiliary agents remaining in the fired product, and grain growth in the subsequent annealing process can be suppressed. By performing the crushing step after the annealing step, it is possible to crush coarse particles into secondary particles having an appropriate size while maintaining secondary particles in which primary particles are agglomerated.
- the hexagonal boron nitride powder obtained in this way can increase the volume ratio of secondary particles in which primary particles are agglomerated. Secondary particles have larger voids in the particles than primary particles. Therefore, a hexagonal boron nitride powder having a large volume fraction of secondary particles is bulky and has a fluffy appearance. When such a hexagonal boron nitride powder is spread, it is spread while the agglomerated secondary particles are broken. Therefore, it has excellent extensibility. Such a hexagonal boron nitride powder is suitable as a raw material for cosmetics.
- the hexagonal boron nitride powder obtained in the crushing step of the above production method has an integrated value from a small particle size in the cumulative distribution of volume-based particle sizes measured by a laser diffraction/scattering method.
- D50 may be 3 to 30 ⁇ m
- D90/D10 may be 4.0 or more, where D10, D50, and D90 are the particle diameters at 90% and 90%, respectively.
- a cosmetic according to one aspect of the present disclosure contains the hexagonal boron nitride powder described above.
- the hexagonal boron nitride powder described above has excellent extensibility when spread. Therefore, a cosmetic containing such a hexagonal boron nitride powder has excellent spreadability.
- a method for producing a cosmetic according to one aspect of the present disclosure produces a cosmetic using the hexagonal boron nitride powder obtained by any of the above-described production methods as a raw material.
- the hexagonal boron nitride powder obtained by the production method described above has excellent elongation when spread. Therefore, a cosmetic produced using such a hexagonal boron nitride powder as a raw material has excellent spreadability.
- the present disclosure it is possible to provide a hexagonal boron nitride powder and a method for producing the same that enable the production of cosmetics with excellent spreadability. Further, according to the present disclosure, it is possible to provide a cosmetic having excellent spreadability by using the hexagonal boron nitride powder described above, and a method for producing the same.
- FIG. 1 is a diagram showing a volume-based cumulative distribution of particle diameters measured by a laser diffraction/scattering method.
- the integrated value from the small particle size is 10 of the total %, 50%, and 90%, D50 is 3 to 30 ⁇ m, and D90/D10 is 4.0 or more, where D10, D50, and D90 are the particle diameters when reaching %, 50%, and 90%, respectively.
- D10, D50, and D90 in the present disclosure are measured with a commercially available laser diffraction particle size distribution analyzer.
- D10, D50 and D90 have a relationship of D10 ⁇ D50 ⁇ D90.
- D50 may be 5 ⁇ m or more, or may be 7 ⁇ m or more, from the viewpoint of further improving slipperiness when used as a raw material for cosmetics.
- D50 may be 25 ⁇ m or less, or may be 20 ⁇ m or less, from the viewpoint of reducing glare in appearance when used as a raw material for cosmetics.
- D90 may be 50 ⁇ m or less, 45 ⁇ m or less, or 40 ⁇ m or less. As a result, coarse particles formed by excessive aggregation of primary particles can be reduced, and rough feeling can be reduced when used as a raw material for cosmetics. D90 may be 18 ⁇ m or more, or may be 19 ⁇ m or more, from the viewpoint of further improving elongation. An example range for D90 may be 18-50 ⁇ m.
- D10 may be 2 ⁇ m or more, and may be 3 ⁇ m or more. This can further improve extensibility. D10 may be 10 ⁇ m or less, and may be 8 ⁇ m or less. This makes it possible to reduce glare in appearance when used as a raw material for cosmetics. An example range for D10 may be 2-10 ⁇ m. D10, D50 and D90 can be adjusted by, for example, the particle size distribution of the raw material powder, the calcining temperature and calcining time, the calcining temperature and calcining time, the annealing temperature and annealing time, and the like.
- D90/D10 may be 4.5 or more, 5.0 or more, or 6.0 or more. By increasing D90/D10 in this way, the ratio and size of secondary particles to primary particles can be sufficiently increased. As a result, the voids contained in the secondary particles are increased, the appearance becomes more fluffy, and the spreadability when spread out can be further improved.
- the upper limit of D90/D10 may be 10 or 8.0 from the viewpoint of manufacturing cost reduction.
- D90/D10 can be adjusted, for example, by changing the firing temperature and firing time in the firing step and the annealing temperature and annealing time in the annealing step.
- An example range for D90/D10 may be 4.0-10.
- D90/D50 may be 1.7 or more, 1.8 or more, or 2.0 or more.
- the ratio of the secondary particles can be further increased, and the elongation-improving effect of the secondary particles during spreading can be further increased. Therefore, it is possible to obtain a hexagonal boron nitride powder having even better elongation.
- the upper limit of D90/D50 may be 6.0 or 4.0.
- D90/D50 can be adjusted, for example, by changing the annealing temperature and annealing time of the annealing step.
- An example range for D90/D50 may be from 1.7 to 6.0.
- D50/D10 may be 4.0 or less, 3.0 or less, or 2.8 or less. As a result, the variation in the particle size of the primary particles can be reduced, and the hiding power can be sufficiently enhanced. From the viewpoint of manufacturing cost reduction, the lower limit of D50/D10 may be 1.5 or more, or may be 2.0 or more. D50/D10 can be adjusted, for example, by changing the firing time of the firing process. An example range for D50/D10 may be from 1.5 to 4.0.
- the bulk density of the hexagonal boron nitride powder may be 0.45 g/cm 3 or less, 0.41 cm 3 or less, or 0.35 cm 3 or less. Having such a low bulk density can result in a hexagonal boron nitride powder having a fluffier appearance.
- the bulk density can be measured in accordance with JIS R1628-1997 "Method for measuring bulk density of fine ceramic powder".
- the primary particles have a size suitable for elongation, but the D90/D10 is large, so the volume ratio of the secondary particles formed by agglomeration of the primary particles is increased. can do. Secondary particles can have larger voids within the particles than primary particles. Therefore, the hexagonal boron nitride powder containing many secondary particles becomes bulky and has a fluffy appearance. When such a hexagonal boron nitride powder is spread, it is spread while the agglomerated secondary particles are broken. Therefore, it has excellent extensibility.
- Such a hexagonal boron nitride powder is suitable as a raw material for cosmetics. That is, the present disclosure can also provide a method of using hexagonal boron nitride as a raw material for cosmetics.
- a cosmetic according to one embodiment contains the hexagonal boron nitride powder described above. Therefore, the cosmetic containing this hexagonal boron nitride powder has excellent spreadability.
- examples of cosmetics include foundation (powder foundation, liquid foundation, cream foundation), face powder, point makeup, eye shadow, eyeliner, nail polish, lipstick, blush, and mascara.
- hexagonal boron nitride powder is particularly well suited for foundation and eyeshadow.
- the content of hexagonal boron nitride powder in cosmetics is, for example, 0.1 to 70% by mass.
- Cosmetics can be manufactured by a known method.
- a method for producing cosmetics includes, for example, a step of blending and mixing hexagonal boron nitride powder and other raw materials.
- a method for producing a hexagonal boron nitride powder is to prepare a raw material powder containing a powder of a compound containing boron and a powder of a compound containing nitrogen in an atmosphere of an inert gas, an ammonia gas, or a mixed gas thereof, A calcination step of obtaining a calcined product containing hexagonal boron nitride by calcining at 600 to 1300 ° C., and a mixed powder containing hexagonal boron nitride and an auxiliary agent is subjected to an inert gas, ammonia gas, or a mixed gas thereof. Firing in an atmosphere at 1900 to 2100 ° C.
- a fired product containing hexagonal boron nitride having higher crystallinity than the hexagonal boron nitride in the mixed powder washing and drying the fired product to dry powder.
- Compounds containing boron include boric acid, boron oxide and borax.
- Nitrogen-containing compounds include cyandiamide, melamine, and urea.
- the raw material powder may contain components other than the above compounds. For example, carbonates such as lithium carbonate and sodium carbonate may be included as calcination aids. It may also contain a reducing substance such as carbon.
- a raw material powder containing the above-described components is calcined in an inert atmosphere such as nitrogen gas, helium gas, or argon gas, in an ammonia atmosphere, or in a mixed gas atmosphere in which these are mixed, using an electric furnace, for example.
- the calcination temperature may be 600-1300°C, 800-1200°C, or 900-1100°C.
- the calcination time may be, for example, 0.5 to 5 hours, or 1 to 4 hours.
- the calcined material obtained by calcining contains at least one selected from the group consisting of low-crystalline hexagonal boron nitride and amorphous hexagonal boron nitride.
- the reaction of boron nitride proceeds at a lower temperature than in the later-described firing process. Therefore, grain growth can be suppressed, and the particle size of the primary particles in the finally obtained boron nitride powder can be reduced.
- auxiliary agent examples include borates such as sodium borate and carbonates such as sodium carbonate, calcium carbonate and lithium carbonate.
- the amount of the auxiliary agent may be 2 to 20 parts by mass, or may be 2 to 8 parts by mass, with respect to 100 parts by mass of the calcined material containing hexagonal boron nitride.
- Such a mixed powder is fired, for example, in an electric furnace, in an inert atmosphere such as nitrogen gas, helium gas, or argon gas, in an ammonia atmosphere, or in a mixed gas atmosphere containing these.
- the firing temperature is 1900-2100°C.
- the firing temperature may be 1950-2050°C.
- the firing time may be, for example, 0.5 to 5 hours, or 1 to 4 hours.
- the firing temperature is too low, it tends to be difficult to generate sufficient secondary particles of hexagonal boron nitride.
- the volume ratio of the secondary particles is small, the lubricity tends to be lowered when used as a raw material for cosmetics. The same tendency is observed when the baking time is too short.
- the firing temperature is too high, crystal growth and aggregation of hexagonal boron nitride proceed excessively, and when used as a raw material for cosmetics, there is a tendency for the glare to become strong.
- the fired product obtained in the firing process may contain impurities other than hexagonal boron nitride.
- Impurities include residual auxiliary agents, water-soluble boron compounds, and the like.
- the cleaning liquid used for cleaning includes water, an aqueous solution containing an acidic substance, an organic solvent, a mixed liquid of an organic solvent and water, and the like. From the viewpoint of avoiding secondary contamination of impurities, water having an electric conductivity of 1 mS/m or less may be used.
- acidic substances include inorganic acids such as hydrochloric acid and nitric acid.
- organic solvents include water-soluble organic solvents such as methanol, ethanol, propanol, isopropyl alcohol and acetone.
- the washing method is not particularly limited, and for example, the baked product may be washed by immersing it in a washing liquid and stirring it, or it may be washed by spraying the washing liquid on the baked product.
- the washing liquid may be solid-liquid separated using a decantation, a suction filter, a pressure filter, a rotary filter, a sedimentation separator, or a combination of these.
- a dry powder may be obtained by drying the separated solid content in a conventional dryer. Dryers include, for example, tray dryers, fluid bed dryers, spray dryers, rotary dryers, belt dryers, and combinations thereof. After drying, classification, for example with a sieve, may be carried out in order to remove coarse particles.
- the dry powder is heated to 1900 to 2100° C. in an inert atmosphere such as nitrogen gas, helium gas, or argon gas, in an ammonia atmosphere, or in a mixed gas atmosphere of these, using an electric furnace, for example. heat up.
- the annealing temperature may be 1950° C. or higher from the viewpoint of sufficiently aggregating the primary particles. Also, the annealing temperature may be 2050° C. or lower from the viewpoint of suppressing grain growth of primary grains.
- the annealing time may be, for example, 0.5 to 5 hours, or 1 to 4 hours, from the viewpoint of sufficiently reducing the oxygen content and suppressing grain growth.
- the heat-treated material obtained in the annealing process is crushed.
- the crushing step is preferably carried out by a method of applying an impact to the extent that the aggregated secondary particles are not destroyed. From this point of view, it is preferable to use a homogenizer that applies ultrasonic vibrations to the heat-treated material dispersed in the solvent in the pulverizing step.
- the solvent those exemplified as the washing solution in the purification step can be used.
- the D90/D10 value of the hexagonal boron nitride powder can be adjusted by the homogenizer crushing time after the annealing process. Specifically, the longer the crushing time, the smaller the value of D90/D10. Also, when the crushing time is shortened, the value of D90/D10 increases. In this way, the value of D90/D10 can be adjusted within a desired range by adjusting the time for pulverization by the homogenizer in the pulverization step after the annealing step or the like.
- the hexagonal boron nitride powder described above can be obtained.
- the description relating to the embodiment of the hexagonal boron nitride powder can be applied to the above manufacturing method.
- Example 1 [Preparation of hexagonal boron nitride powder] ⁇ Temporary firing process> 100.0 g of boric acid powder (purity of 99.8% by mass or more, manufactured by Kanto Chemical Co., Ltd.) and 90.0 g of melamine powder (purity of 99.0% by mass or more, manufactured by Wako Pure Chemical Industries, Ltd.) were added using an alumina mortar. Mixed for 10 minutes to obtain a mixed raw material. The mixed raw material after drying was placed in a container made of hexagonal boron nitride and placed in an electric furnace. The temperature was raised from room temperature to 1000° C. at a rate of 10° C./min while nitrogen gas was circulated in the electric furnace. After holding at 1000° C. for 2 hours, the heating was stopped and the mixture was allowed to cool naturally. The electric furnace was opened when the temperature became 100° C. or lower. Thus, a calcined product containing low-crystalline hexagonal boron nitride was obtained.
- ⁇ Crushing process> 30 g of hexagonal boron nitride coarse powder obtained in the annealing step is put into 300 ml of water, and is subjected to ultrasonic waves for 5 minutes at 500 W and 20 kHz using a homogenizer (manufactured by SONIC & MATERIALS, INC., trade name: VC505). dispersed. Thereafter, 500 g of diluted nitric acid (concentration of nitric acid: 5% by mass) was added to remove impurities contained in the coarse powder, and the mixture was stirred at room temperature for 60 minutes.
- a homogenizer manufactured by SONIC & MATERIALS, INC., trade name: VC505
- FIG. 1 is a graph showing the volume-based cumulative distribution of particle diameters obtained by this measurement.
- D10, D50, and D90 was as shown in Table 2.
- Table 2 also shows the values of D90/D10, D90/D50, and D50/D10.
- Example 2 A hexagonal boron nitride powder was prepared in the same manner as in Example 1, except that the heating temperature in the annealing step was set to 2050°C. Then, in the same manner as in Example 1, each measurement and evaluation of the hexagonal boron nitride powder was performed. The results were as shown in FIG. 1 and Table 2.
- Example 3 A hexagonal boron nitride powder was prepared in the same manner as in Example 1, except that the holding time in the annealing step was 5 hours. Then, in the same manner as in Example 1, each measurement and evaluation of the hexagonal boron nitride powder was performed. The results were as shown in FIG. 1 and Table 2.
- Example 4 A hexagonal boron nitride powder was prepared in the same manner as in Example 1, except that the homogenizer time in the crushing step was changed to 8 minutes. Then, in the same manner as in Example 1, each measurement and evaluation of the hexagonal boron nitride powder was performed. The results were as shown in Table 2.
- Example 1 A hexagonal boron nitride powder was prepared in the same manner as in Example 1, except that the heating temperature in the annealing step was 1700°C. Each measurement and evaluation of the hexagonal boron nitride powder was carried out in the same manner as in Example 1. The results were as shown in FIG. 1 and Table 2.
- Examples 1 to 4 contained secondary particles in which primary particles aggregated. Examples 1 to 4 had a larger D90/D10 value than Comparative Example 1 and had a fluffy appearance. Therefore, Examples 1 to 4 contained more secondary particles than Comparative Example 1, and exhibited excellent elongation. The hexagonal boron nitride powder of Example 1, which was the most agglomerated, had the best elongation.
- a hexagonal boron nitride powder and a method for producing the same are provided that enable the production of cosmetics having excellent spreadability. Further, a cosmetic having excellent spreadability by using the hexagonal boron nitride powder described above and a method for producing the same are provided.
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Abstract
Description
[六方晶窒化ホウ素粉末の調製]
<仮焼工程>
ホウ酸粉末(純度99.8質量%以上、関東化学社製)100.0g、及びメラミン粉末(純度99.0質量%以上、和光純薬社製)90.0gを、アルミナ製乳鉢を用いて10分間混合し混合原料を得た。乾燥後の混合原料を、六方晶窒化ホウ素製の容器に入れ、電気炉内に配置した。電気炉内に窒素ガスを流通させながら、10℃/分の速度で室温から1000℃に昇温した。1000℃で2時間保持した後、加熱を止めて自然冷却した。温度が100℃以下になった時点で電気炉を開放した。このようにして、低結晶性の六方晶窒化ホウ素を含む仮焼物を得た。
仮焼物100.0gに、助剤として炭酸ナトリウム(純度99.5質量%以上)を3.0g添加し、アルミナ製乳鉢を用いて10分間混合した。混合物を、上述の電気炉内に配置した。電気炉内に窒素ガスを流通させながら、10℃/分の速度で室温から2000℃に昇温した。2000℃の焼成温度で4時間保持した後、加熱を止めて自然冷却した。温度が100℃以下になった時点で電気炉を開放した。得られた焼成物を回収し、アルミナ製乳鉢で3分間粉砕して、六方晶窒化ホウ素の粗粉を得た。
六方晶窒化ホウ素の粗粉中に含まれる不純物を除くため、希硝酸500g(硝酸濃度:5質量%)に、粗粉を30g投入し、室温で60分間撹拌した。撹拌後、吸引ろ過によって固液分離し、ろ液が中性になるまで水(電気伝導度1mS/m)を入れ替えて洗浄した。洗浄後、乾燥機を用いて120℃で3時間乾燥して乾燥粉末を得た。
粗粒を除去した乾燥粉末を、上述の電気炉内に配置した。電気炉内に窒素ガスを流通させながら、10℃/分の速度で室温から2000℃に昇温した。2000℃で4時間保持した後、加熱を止めて自然冷却した。温度が100℃以下になった時点で電気炉を開放した。得られた焼成物を回収し、六方晶窒化ホウ素粉末の粗粉を得た。
アニール工程で得られた六方晶窒化ホウ素の粗粉30gを水300mlに投入し、ホモジナイザ(SONIC & MATERIALS,INC.製、商品名:VC505)を用いて、500W、20kHzの条件で5分間超音波分散させた。その後、粗粉中に含まれる不純物を除くため、希硝酸500g(硝酸濃度:5質量%)を加え、室温で60分間撹拌した。撹拌後、吸引ろ過によって固液分離し、ろ液が中性になるまで水(電気伝導度:1mS/m)を入れ替えて洗浄した。洗浄後、乾燥機を用いて120℃で3時間乾燥して乾燥粉末を得た。得られた乾燥粉末から、超音波振動篩(株式会社興和工業所社製、商品名:KFS-1000、目開き250μm)を用いて、粗粒を除去した。これを実施例1の六方晶窒化ホウ素粉末とした。
<粒度分布の測定>
実施例1で調製した六方晶窒化ホウ素粉末の体積基準の粒度分布を、レーザー回折式粒子径分布測定装置(日機装株式会社製、装置名:MT3300EX)を用いて測定した。図1は、この測定によって得られた、体積基準の粒子径の累積分布を示すグラフである。図1に示す累積分布において、小粒径からの積算値が全体の10%、50%及び90%に達したときの粒子径を、それぞれD10,D50,D90としたとき、D10,D50,D90のそれぞれの値は表2に示すとおりであった。表2には、D90/D10、D90/D50、及びD50/D10の値も併せて示した。
人工皮膚(縦×横=10mm×50mm)の一端に、六方晶窒化ホウ素粉末0.2gを載せた。人工皮膚の表面に六方晶窒化ホウ素粉末を塗り付けるように、ヘラを用いて六方晶窒化ホウ素粉末を縦方向に沿って伸ばした。市販の画像解析ソフトウェア(WinROOF)を用いて画像解析を行って、人工皮膚の全面積に対する、六方晶窒化ホウ素粉末の塗布面積の割合を求めた。この面積割合が大きいほど伸び性が優れている。伸び性の評価基準は、面積割合に応じて表1に示すとおりとした。伸び性の評価結果は表2に示すとおりであった。
アニール工程の加熱温度を2050℃にしたこと以外は、実施例1と同様にして六方晶窒化ホウ素粉末を調製した。そして、実施例1と同様にして、六方晶窒化ホウ素粉末の各測定及び評価を行った。結果は図1及び表2に示すとおりであった。
アニール工程の保持時間を5時間にしたこと以外は、実施例1と同様にして六方晶窒化ホウ素粉末を調製した。そして、実施例1と同様にして、六方晶窒化ホウ素粉末の各測定及び評価を行った。結果は図1及び表2に示すとおりであった。
解砕工程におけるホモジナイザの時間を8分間に変更したこと以外は、実施例1と同様にして六方晶窒化ホウ素粉末を調製した。そして、実施例1と同様にして、六方晶窒化ホウ素粉末の各測定及び評価を行った。結果は表2に示すとおりであった。
アニール工程における加熱温度を1700℃としたこと以外は実施例1と同様にして六方晶窒化ホウ素粉末を調製した。実施例1と同様にして六方晶窒化ホウ素粉末の各測定及び評価を行った。結果は図1及び表2に示すとおりであった。
Claims (8)
- 六方晶窒化ホウ素の一次粒子が凝集して形成される二次粒子を含み、
レーザー回折・散乱法によって測定される体積基準の粒子径の累積分布において、小粒径からの積算値が全体の10%、50%及び90%に達したときの粒子径を、それぞれD10、D50及びD90としたときに、D50が3~30μmであり、
D90/D10が4.0以上である、六方晶窒化ホウ素粉末。 - D90/D50が1.7以上である、請求項1に記載の六方晶窒化ホウ素粉末。
- D90が50μm以下である、請求項1又は2に記載の六方晶窒化ホウ素粉末。
- 化粧料の原料用である、請求項1~3のいずれか一項に記載の六方晶窒化ホウ素粉末。
- ホウ素を含む化合物の粉末と窒素を含む化合物の粉末を含有する原料粉末を、不活性ガス、アンモニアガス又はこれらの混合ガスの雰囲気中、600~1300℃で焼成して、六方晶窒化ホウ素を含む仮焼物を得る仮焼工程と、
前記仮焼物と助剤とを含む混合粉末を、不活性ガス、アンモニアガス又はこれらの混合ガスの雰囲気中、1900~2100℃で焼成して、前記仮焼物における六方晶窒化ホウ素よりも高い結晶性を有する六方晶窒化ホウ素を含む焼成物を得る焼成工程と、
前記焼成物を洗浄及び乾燥して乾燥粉末を得る精製工程と、
前記乾燥粉末を、不活性ガス、アンモニアガス又はこれらの混合ガスの雰囲気中、1900~2100℃でアニールして六方晶窒化ホウ素の一次粒子が凝集して形成される二次粒子を含む加熱処理物を得るアニール工程と、
前記加熱処理物を解砕して前記二次粒子を含む六方晶窒化ホウ素粉末を得る解砕工程と、を有する、六方晶窒化ホウ素粉末の製造方法。 - 前記解砕工程で得られる前記六方晶窒化ホウ素粉末は、レーザー回折・散乱法によって測定される体積基準の粒子径の累積分布において、小粒径からの積算値が全体の10%、50%及び90%に達したときの粒子径を、それぞれD10,D50,D90としたときに、D50が3~30μmであり、D90/D10が4.0以上である、請求項5に記載の六方晶窒化ホウ素粉末の製造方法。
- 請求項1~4のいずれか一項の六方晶窒化ホウ素粉末を含む化粧料。
- 請求項5又は6の製造方法で得られる六方晶窒化ホウ素粉末を原料として用いて化粧料を製造する、化粧料の製造方法。
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