JP7372142B2 - Hexagonal boron nitride powder and its manufacturing method, and cosmetics and its manufacturing method - Google Patents
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- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 title claims description 103
- 239000002537 cosmetic Substances 0.000 title claims description 29
- 238000004519 manufacturing process Methods 0.000 title claims description 24
- 239000000843 powder Substances 0.000 claims description 35
- 238000010304 firing Methods 0.000 claims description 26
- 229910052582 BN Inorganic materials 0.000 claims description 25
- 239000002994 raw material Substances 0.000 claims description 18
- 238000005259 measurement Methods 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000012752 auxiliary agent Substances 0.000 claims description 8
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 7
- 229910052796 boron Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- -1 nitrogen-containing compound Chemical class 0.000 claims description 3
- 238000010298 pulverizing process Methods 0.000 claims 1
- 230000002776 aggregation Effects 0.000 description 17
- 239000000047 product Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000005054 agglomeration Methods 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 9
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
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- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 125000000524 functional group Chemical group 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
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-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
- 238000002156 mixing Methods 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 239000007787 solid Substances 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
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052786 argon Inorganic materials 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
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 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
- 239000006082 mold release agent Substances 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- 238000003756 stirring 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
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000002238 attenuated effect 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
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- 238000010908 decantation Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-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
- 239000000706 filtrate Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000314 lubricant Substances 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
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000007670 refining Methods 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
- 238000005070 sampling Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 235000011182 sodium carbonates Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
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- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
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- Cosmetics (AREA)
Description
本開示は、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に関する。 The present disclosure relates to a hexagonal boron nitride powder and a method for producing the same, and a cosmetic and a method for producing the same.
窒化ホウ素は、潤滑性、高熱伝導性、及び絶縁性等を有しており、固体潤滑剤、離型剤、樹脂及びゴムの充填材、化粧料（化粧品ともいう）の原料、並びに耐熱性を有する絶縁性焼結体等、幅広い用途に利用されている。 Boron nitride has lubricity, high thermal conductivity, and insulation properties, and is used as a solid lubricant, mold release agent, resin and rubber filler, raw material for cosmetics (also referred to as cosmetics), and has heat resistance. It is used in a wide range of applications, such as insulating sintered bodies.
化粧料に配合される六方晶窒化ホウ素粉末の機能としては、化粧料への滑り性、伸び性、隠ぺい性の向上、及び、光沢性の付与等が挙げられる。特に、六方晶窒化ホウ素粉末は、同様の機能を有するタルク粉末及びマイカ粉末に比べて滑り性に優れているため、優れた滑り性が求められる化粧料に汎用されている。特許文献１では、滑り性を改善するために、せん断応力と加圧力の比を所定の数値範囲にすることが提案されている。 Functions of the hexagonal boron nitride powder blended into cosmetics include improving slipperiness, spreadability, and concealment properties of cosmetics, and imparting glossiness to the cosmetics. In particular, hexagonal boron nitride powder has superior slip properties compared to talc powder and mica powder, which have similar functions, and is therefore widely used in cosmetics that require excellent slip properties. Patent Document 1 proposes setting the ratio of shear stress to pressing force within a predetermined numerical range in order to improve slipperiness.
六方晶窒化ホウ素粉末は、水分等の要因によって凝集ダマを形成する場合がある。凝集すると流動性が低下し、滑り性及びハンドリング性が損なわれることが懸念される。そこで、本開示では、凝集を抑制することが可能な六方晶窒化ホウ素粉末及びその製造方法を提供する。また、本開示では、上述の六方晶窒化ホウ素粉末を用いることによって凝集を抑制し、伸び性に優れる化粧料及びその製造方法を提供する。 Hexagonal boron nitride powder may form agglomerated lumps due to factors such as moisture. There is concern that agglomeration will reduce fluidity and impair slipperiness and handling. Therefore, the present disclosure provides hexagonal boron nitride powder that can suppress agglomeration and a method for producing the same. Further, the present disclosure provides a cosmetic that suppresses agglomeration and has excellent extensibility by using the above-described hexagonal boron nitride powder, and a method for producing the same.
本開示の一側面に係る六方晶窒化ホウ素粉末は、帯電減衰性測定によって求められる正電荷と負電荷の減衰速度を比較したときに、正電荷の減衰速度の方が、負電荷の減衰速度よりも大きい。六方晶窒化ホウ素粉末は、例えば、粒子同士の摩擦、及び収容容器の内壁との摩擦等の要因によって帯電する場合がある。ここで、正電荷が生じると、大気中に存在する水分子における酸素原子の極性が負であるため、大気中の水分によって正電荷に帯電している六方晶窒化ホウ素粉末が凝集する。しかしながら、上記六方晶窒化ホウ素粉末は、正電荷の減衰速度の方が、負電荷の減衰速度よりも大きいため、正電荷が速やかに減衰する。したがって、大気中の水分による凝集を抑制することができる。 In the hexagonal boron nitride powder according to one aspect of the present disclosure, when the decay rates of positive charges and negative charges determined by charge decay property measurement are compared, the decay rate of positive charges is faster than the decay rate of negative charges. It's also big. The hexagonal boron nitride powder may become electrically charged due to factors such as friction between the particles and friction with the inner wall of the container. Here, when a positive charge is generated, the hexagonal boron nitride powder, which is positively charged by the moisture in the atmosphere, aggregates because the polarity of oxygen atoms in water molecules present in the atmosphere is negative. However, in the hexagonal boron nitride powder, the decay rate of positive charges is greater than the decay rate of negative charges, so the positive charges decay quickly. Therefore, aggregation due to moisture in the atmosphere can be suppressed.
上記六方晶窒化ホウ素粉末の負電荷の減衰速度に対する正電荷の減衰速度の比は１．５以下であってよい。これによって、正電荷と負電荷の減衰速度の差異が小さくなり、電荷の偏りを抑制することができる。したがって、水分子のみならず、他の分子が介在することによる凝集を抑制することができる。 The ratio of the decay rate of positive charges to the decay rate of negative charges in the hexagonal boron nitride powder may be 1.5 or less. This reduces the difference in decay rate between positive charges and negative charges, making it possible to suppress charge bias. Therefore, aggregation caused not only by water molecules but also by other molecules can be suppressed.
上記六方晶窒化ホウ素粉末は、化粧料の原料用であってよい。上記六方晶窒化ホウ素粉末は、凝集が抑制されているため、伸び性に優れる。したがって、化粧料の原料用に好適である。 The hexagonal boron nitride powder may be used as a raw material for cosmetics. The hexagonal boron nitride powder has excellent elongation properties because agglomeration is suppressed. Therefore, it is suitable for use as a raw material for cosmetics.
本開示の一側面に係る六方晶窒化ホウ素粉末の製造方法は、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、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℃の温度で、１０～５０時間加熱して焼成する焼成工程と、焼成工程で得られる焼成物を粉砕、洗浄及び乾燥し、六方晶窒化ホウ素粉末を得る精製工程と、を有し、帯電減衰性測定によって求められる正電荷と負電荷の減衰速度を比較したときに、正電荷の減衰速度の方が負電荷の減衰速度よりも大きい、六方晶窒化ホウ素粉末の製造方法を提供する。 A method for producing hexagonal boron nitride powder according to one aspect of the present disclosure includes raw material powder containing a boron-containing compound powder and a nitrogen-containing compound powder in an atmosphere of an inert gas, ammonia gas, or a mixed gas thereof. A calcination step in which a calcined product containing hexagonal boron nitride is obtained by firing at a temperature of 600 to 1300°C; A firing step of heating and firing in an atmosphere at a temperature of 1900 to 2100° C. for 10 to 50 hours, and a purification step of crushing, washing and drying the fired product obtained in the firing step to obtain hexagonal boron nitride powder. A method for producing a hexagonal boron nitride powder, which has a positive charge decay rate that is larger than a negative charge decay rate when comparing the decay rates of positive charges and negative charges determined by charge decay property measurement. I will provide a.
上記製造方法は、焼成工程よりも低い温度で焼成する仮焼工程を有することによって、粒径が小さく結晶性の低い六方晶窒化ホウ素を形成することができる。焼成工程では、助剤を用いて１９００～２１００℃で焼成することによって、六方晶窒化ホウ素の結晶性を高くしつつ、六方晶窒化ホウ素の粒子の表面における水酸基等の官能基を低減することができる。これによって、帯電し難く、且つ帯電しても、電荷が速やかに減衰する六方晶窒化ホウ素粉末を得ることができる。このような六方晶窒化ホウ素粉末は、静電気による凝集を抑制することができる。また、六方晶窒化ホウ素粉末は、帯電減衰性測定によって求められる正電荷と負電荷の減衰速度を比較したときに、正電荷の減衰速度の方が負電荷の減衰速度よりも大きい。このため、正電荷が速やかに減衰する。したがって、大気中の水分による凝集を抑制することができる。 The above manufacturing method includes a calcination step in which firing is performed at a lower temperature than the calcination step, thereby making it possible to form hexagonal boron nitride with a small particle size and low crystallinity. In the firing process, by firing at 1900 to 2100°C using an auxiliary agent, it is possible to increase the crystallinity of hexagonal boron nitride while reducing functional groups such as hydroxyl groups on the surface of hexagonal boron nitride particles. can. This makes it possible to obtain a hexagonal boron nitride powder that is difficult to be charged and whose charge quickly decays even if it is charged. Such hexagonal boron nitride powder can suppress aggregation due to static electricity. Further, in the hexagonal boron nitride powder, when the decay rates of positive charges and negative charges determined by charge decay property measurement are compared, the decay rate of positive charges is greater than the decay rate of negative charges. For this reason, positive charges are quickly attenuated. Therefore, aggregation due to moisture in the atmosphere can be suppressed.
本開示の一側面に係る化粧料は、上述の六方晶窒化ホウ素粉末を含む。上述の六方晶窒化ホウ素粉末は、大気中の水分等の要因による凝集を抑制することができる。このような六方晶窒化ホウ素粉末を含む化粧料は、優れた伸び性を有する。 A cosmetic according to one aspect of the present disclosure includes the hexagonal boron nitride powder described above. The hexagonal boron nitride powder described above can suppress aggregation caused by factors such as moisture in the atmosphere. Cosmetics containing such hexagonal boron nitride powder have excellent elongation properties.
本開示の一側面に係る化粧料の製造方法は、上述のいずれか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。上述の製造方法で得られる六方晶窒化ホウ素粉末は、大気中の水分等の要因による凝集を抑制することができる。このため、このような六方晶窒化ホウ素粉末を原料として用いて製造された化粧料は、優れた伸び性を有する。 A method for producing a cosmetic according to one aspect of the present disclosure produces a cosmetic using hexagonal boron nitride powder obtained by any of the above-mentioned production methods as a raw material. The hexagonal boron nitride powder obtained by the above manufacturing method can suppress aggregation due to factors such as moisture in the atmosphere. Therefore, cosmetics produced using such hexagonal boron nitride powder as a raw material have excellent elongation properties.
本開示によれば、凝集を抑制することが可能な六方晶窒化ホウ素粉末及びその製造方法を提供することができる。また、本開示によれば、上述の六方晶窒化ホウ素粉末を用いることによって凝集を抑制し、伸び性に優れる化粧料及びその製造方法を提供することができる。 According to the present disclosure, it is possible to provide a hexagonal boron nitride powder that can suppress agglomeration and a method for manufacturing the same. Further, according to the present disclosure, by using the above-described hexagonal boron nitride powder, it is possible to suppress agglomeration and provide a cosmetic with excellent extensibility, and a method for producing the same.
以下、本開示の実施形態を説明する。ただし、以下の実施形態は、本開示を説明するための例示であり、本開示を以下の内容に限定する趣旨ではない。 Embodiments of the present disclosure will be described below. However, the following embodiments are examples for explaining the present disclosure, and are not intended to limit the present disclosure to the following contents.
本実施形態の六方晶窒化ホウ素粉末は、帯電減衰性測定によって求められる正負の電荷の減衰速度を比較したときに、正電荷の減衰速度の方が、負電荷の減衰速度よりも大きい。このような六方晶窒化ホウ素粉末は、負電荷よりも正電荷の方が速やかに減衰する。したがって、水分子の酸素原子と六方晶窒化ホウ素粉末の正電荷との水素結合によって生じる凝集を抑制することができる。負電荷の減衰速度に対する正電荷の減衰速度の比は、１を超え且つ１．５以下であってよい。この比が１に近づくと、正電荷と負電荷の減衰速度の差が小さくなり、粒子表面における静電気を速やかに除去することができる。 In the hexagonal boron nitride powder of this embodiment, when comparing the decay rates of positive and negative charges determined by charge decay property measurement, the decay rate of positive charges is greater than the decay rate of negative charges. In such hexagonal boron nitride powder, positive charges attenuate more quickly than negative charges. Therefore, aggregation caused by hydrogen bonding between oxygen atoms of water molecules and positive charges of hexagonal boron nitride powder can be suppressed. The ratio of the decay rate of positive charges to the decay rate of negative charges may be greater than 1 and less than or equal to 1.5. When this ratio approaches 1, the difference in decay rate between positive charges and negative charges becomes small, and static electricity on the particle surface can be quickly removed.
本開示における帯電減衰性測定は、市販の測定装置を用いて、ＪＩＳ Ｃ６１３４０－２－１：２００６に準拠して測定され、静電気電荷拡散率測定とも称されるものである。測定装置としては、例えば、株式会社ナノシーズ製のＮＳ－Ｄ１００（製品名）が挙げられる。この測定で得られる表面電位減衰曲線を用いて、下記式より減衰速度（α）を算出する。 The charge decay property measurement in the present disclosure is measured using a commercially available measuring device in accordance with JIS C61340-2-1:2006, and is also referred to as electrostatic charge diffusivity measurement. Examples of the measuring device include NS-D100 (product name) manufactured by Nano Seeds Co., Ltd. Using the surface potential decay curve obtained in this measurement, the decay rate (α) is calculated from the following formula.
式中、ｔは減衰時間、Ｖは減衰時間ｔにおける表面電位、Ｖ０は初期表面電位、αは減衰速度をそれぞれ示す。減衰速度αは、六方晶窒化ホウ素粉末を、所定の電位差のコロナ放電において帯電させて求めることができる。減衰時間ｔの最大値を６００秒とし、６００秒になるまでの表面電位Ｖを測定する。初期表面電位Ｖ０の値と、所定の減衰時間ｔの際の表面電位Ｖの値の関係を指数近似することによって、αが得られる。上述の測定は、六方晶窒化ホウ素粉末を正電荷と負電荷のそれぞれに帯電させて行う。このとき、両者の電荷量は同じとして、正電荷と負電荷の減衰速度をそれぞれ求める。正電荷と負電荷の減衰速度の差の絶対値は、０．００５未満であってよく、０．００３未満であってもよい。 In the formula, t is the decay time, V is the surface potential at the decay time t, V 0 is the initial surface potential, and α is the decay rate. The decay rate α can be determined by charging hexagonal boron nitride powder in a corona discharge with a predetermined potential difference. The maximum value of the decay time t is set to 600 seconds, and the surface potential V is measured until the decay time t reaches 600 seconds. α is obtained by exponentially approximating the relationship between the value of the initial surface potential V 0 and the value of the surface potential V at a predetermined decay time t. The above measurements are performed by charging the hexagonal boron nitride powder with a positive charge and a negative charge, respectively. At this time, the attenuation rates of the positive charge and the negative charge are determined respectively, assuming that the amount of charge is the same for both. The absolute value of the difference in decay rate between positive charge and negative charge may be less than 0.005, and may be less than 0.003.
本実施形態に係る六方晶窒化ホウ素粉末は、凝集ダマを形成し難いため、滑り性及びハンドリング性に優れる。このため、種々の用途に好適に用いることができる。例えば、離型剤及び敷き粉等に用いられる。また、この六方晶窒化ホウ素粉末は、凝集が抑制されることによって、媒体（人肌等）に塗布したときに優れた伸び性を有する。このため、例えば化粧料の原料用に好適である。すなわち、本開示は、六方晶窒化ホウ素を化粧料の原料として使用する使用方法も提供することができる。 The hexagonal boron nitride powder according to this embodiment is difficult to form agglomerated lumps, and therefore has excellent slipperiness and handling properties. Therefore, it can be suitably used for various purposes. For example, it is used as a mold release agent and a spreading powder. Further, this hexagonal boron nitride powder has excellent extensibility when applied to a medium (such as human skin) due to suppressed aggregation. Therefore, it is suitable for use as a raw material for cosmetics, for example. That is, the present disclosure can also provide a method of using hexagonal boron nitride as a raw material for cosmetics.
一実施形態に係る化粧料は、上述の六方晶窒化ホウ素粉末を含有する。この六方晶窒化ホウ素粉末は、表面に発生した静電気のうち、負電荷よりも正電荷を速やかに低減することができる。このため、六方晶窒化ホウ素粉末は水分による凝集が抑制され、優れた伸び性を有する。 A cosmetic according to one embodiment contains the above-described hexagonal boron nitride powder. Of the static electricity generated on the surface, this hexagonal boron nitride powder can reduce positive charges more quickly than negative charges. Therefore, the hexagonal boron nitride powder is suppressed from agglomeration due to moisture, and has excellent elongation properties.
化粧料としては、例えば、ファンデーション（パウダーファンデーション、リキッドファンデーション、クリームファンデーション）、フェイスパウダー、ポイントメイク、アイシャドー、アイライナー、マニュキュア、口紅、頬紅、及びマスカラ等が挙げられる。これらのうち、ファンデーション及びアイシャドーには、六方晶窒化ホウ素粉末が特に良く適合する。化粧料における六方晶窒化ホウ素粉末の含有量は、例えば０．１～７０質量％である。化粧料は公知の方法によって製造することができる。化粧料の製造方法は、例えば、六方晶窒化ホウ素粉末と他の原料とを配合して混合する工程を有する。 Examples of cosmetics include foundations (powder foundation, liquid foundation, cream foundation), face powder, point makeup, eye shadow, eyeliner, nail polish, lipstick, blush, mascara, and the like. Among these, hexagonal boron nitride powder is particularly well suited for foundations and eye shadows. The content of hexagonal boron nitride powder in the cosmetic is, for example, 0.1 to 70% by mass. Cosmetics can be manufactured by known methods. A method for producing cosmetics includes, for example, a step of blending and mixing hexagonal boron nitride powder and other raw materials.
一実施形態に係る六方晶窒化ホウ素粉末の製造方法は、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、不活性ガス雰囲気中、アンモニアガス雰囲気中、又はこれらの混合ガス雰囲気中、６００～１３００℃で焼成して、低結晶性の六方晶窒化ホウ素、及び非晶質の六方晶窒化ホウ素からなる群より選ばれる少なくとも一方を含む仮焼物を得る仮焼工程と、仮焼物と助剤とを含む混合粉末を、不活性ガス及び／又はアンモニアガスの雰囲気中、１９００～２１００℃の温度で、１０～５０時間加熱して焼成物を得る焼成工程と、焼成物を粉砕、洗浄、及び乾燥し、乾燥粉末を得る精製工程と、を有する。 A method for producing hexagonal boron nitride powder according to one embodiment includes raw material powder containing powder of a boron-containing compound and powder of a compound containing nitrogen in an inert gas atmosphere, an ammonia gas atmosphere, or a mixture thereof. A calcination step of obtaining a calcined product containing at least one selected from the group consisting of low-crystalline hexagonal boron nitride and amorphous hexagonal boron nitride by firing at 600 to 1300°C in a gas atmosphere; A firing step in which a mixed powder containing a calcined product and an auxiliary agent is heated in an atmosphere of inert gas and/or ammonia gas at a temperature of 1900 to 2100°C for 10 to 50 hours to obtain a fired product; and a purification step of crushing, washing, and drying to obtain a dry powder.
ホウ素を含む化合物としては、ホウ酸、酸化ホウ素及びホウ砂等が挙げられる。窒素を含む化合物としては、ジシアンジアミド、メラミン、及び尿素が挙げられる。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におけるホウ素原子と窒素原子のモル比は、ホウ素原子：窒素原子＝２：８～８：２であってよく、３：７～７：３であってもよい。原料粉末は、上記化合物以外の成分を含んでもよい。例えば、助剤として炭酸リチウム及び炭酸ナトリウムなどの炭酸塩を含んでよい。また、炭素等の還元性物質を含んでよい。 Examples of compounds containing boron include boric acid, boron oxide, and borax. Compounds containing nitrogen include dicyandiamide , melamine, and urea. The molar ratio of boron atoms to nitrogen atoms in the raw material powder containing powder of a boron-containing compound and powder of a compound containing nitrogen may be boron atoms:nitrogen atoms=2:8 to 8:2, and 3:7. The ratio may be 7:3. The raw material powder may contain components other than the above-mentioned compounds. For example, carbonates such as lithium carbonate and sodium carbonate may be included as auxiliaries. Further, it may contain a reducing substance such as carbon.
上述の成分を含有する原料粉末を、例えば電気炉を用いて、窒素ガス、ヘリウムガス、又はアルゴンガス等の不活性雰囲気中、アンモニア雰囲気中、或いはこれらを混合した混合ガス雰囲気中で仮焼する。仮焼温度は、６００～１３００℃であってよく、８００～１２００℃であってよく、９００～１１００℃であってもよい。仮焼時間は、例えば０．５～５時間であってよく、１～４時間であってもよい。 The raw material powder containing the above-mentioned components is calcined in an inert atmosphere such as nitrogen gas, helium gas, or argon gas, an ammonia atmosphere, or a mixed gas atmosphere of these by using, for example, an electric furnace. . The calcination temperature may be 600 to 1300°C, 800 to 1200°C, or 900 to 1100°C. The calcination time may be, for example, 0.5 to 5 hours, or 1 to 4 hours.
仮焼によって得られる仮焼物は、低結晶性の六方晶窒化ホウ素、及び非晶質の六方晶窒化ホウ素からなる群より選ばれる少なくとも一方を含む。仮焼工程は、後述の焼成工程よりも低温で窒化ホウ素の反応を進行させる。このため、粒成長を抑制し、最終的に得られる窒化ホウ素粉末の粒径を小さくすることができる。また、六方晶窒化ホウ素粉末の比表面積を大きくすることができる。 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. In the calcination step, the reaction of boron nitride proceeds at a lower temperature than in the calcination step described below. Therefore, grain growth can be suppressed and the particle size of the ultimately obtained boron nitride powder can be reduced. Further, the specific surface area of the hexagonal boron nitride powder can be increased.
次に、得られた仮焼物と助剤とを配合して混合し、混合粉末を得る。助剤としては、ホウ酸ナトリウム等のホウ酸塩、並びに、炭酸ナトリウム、炭酸カルシウム及び炭酸リチウム等の炭酸塩が挙げられる。六方晶窒化ホウ素を含む仮焼物１００質量部に対する、助剤の配合量は２～２０質量部であってよく、２～８質量部であってもよい。このような混合粉末を、例えば電気炉中、窒素ガス、ヘリウムガス、又はアルゴンガス等の不活性雰囲気中、アンモニア雰囲気中、或いはこれらを含む混合ガス雰囲気中で焼成する。 Next, the obtained calcined product and an auxiliary agent are blended and mixed to obtain a mixed powder. Auxiliary agents include borates such as sodium borate, and carbonates such as sodium carbonate, calcium carbonate, and lithium carbonate. The blending amount of the auxiliary agent may be 2 to 20 parts by mass, or 2 to 8 parts by mass, based on 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.
焼成工程では、助剤の存在下、窒化ホウ素の生成及び結晶化が進行する。これによって、仮焼物に含まれる窒化ホウ素の結晶性を高めることができる。焼成温度は、１９００～２１００℃であり、１９５０～２０５０℃であってもよい。焼成時間は、例えば１０～５０時間であってよく、２０～４０時間であってもよい。このような条件で焼成することによって、粒子の表面に存在する水酸基等の官能基を飛散させ、静電気を帯び難い六方晶窒化ホウ素粉末を得ることができる。 In the firing step, the production and crystallization of boron nitride progress in the presence of an auxiliary agent. Thereby, the crystallinity of boron nitride contained in the calcined product can be improved. The firing temperature is 1900 to 2100°C, and may be 1950 to 2050°C. The firing time may be, for example, 10 to 50 hours, or 20 to 40 hours. By firing under such conditions, functional groups such as hydroxyl groups present on the surface of the particles are scattered, and hexagonal boron nitride powder that is not easily charged with static electricity can be obtained.
焼成温度が低くなり過ぎると、六方晶窒化ホウ素の表面における官能基の量が増加する傾向にある。六方晶窒化ホウ素の官能基の量が増加すると、静電気を帯びやすくなり凝集し易くなる傾向にある。焼成時間が短くなり過ぎたときも同様の傾向にある。一方、焼成温度が高くなり過ぎると、六方晶窒化ホウ素の結晶成長が進み過ぎて、一次粒子が凝集する傾向にある。焼成時間が長くなり過ぎたときも同様の傾向にある。 If the firing temperature becomes too low, the amount of functional groups on the surface of hexagonal boron nitride tends to increase. As the amount of functional groups in hexagonal boron nitride increases, it tends to be more easily charged with static electricity and more likely to aggregate. A similar tendency occurs when the firing time becomes too short. On the other hand, if the firing temperature becomes too high, the crystal growth of hexagonal boron nitride progresses too much, and the primary particles tend to aggregate. A similar tendency occurs when the firing time is too long.
焼成工程で得られた焼成物は、通常の粉砕装置で粉砕してよい。粉砕した粉砕粉の中には、六方晶窒化ホウ素以外に不純物が含まれる場合がある。不純物としては、残存する助剤、及び水溶性ホウ素化合物等が挙げられる。精製工程では、このような不純物を、洗浄によって低減する。洗浄後、固液分離して乾燥し、乾燥粉末を得る。洗浄に用いる洗浄液としては、水、酸性物質を含む水溶液、有機溶媒、有機溶媒と水との混合液等が挙げられる。不純物の二次的な混入を避ける観点から、電気伝導度が１ｍＳ／ｍ以下の水を使用してよい。酸性物質としては、例えば塩酸、硝酸等の無機酸が挙げられる。有機溶媒としては、例えば、メタノール、エタノール、プロパノール、イソプロピルアルコール及びアセトン等の水溶性の有機溶媒が挙げられる。洗浄方法に特に制限はなく、例えば、粉砕粉を洗浄液中に浸漬し撹拌して洗浄してよく、粉砕粉に洗浄液をスプレーして洗浄してもよい。 The fired product obtained in the firing process may be pulverized using a conventional pulverizer. The pulverized powder may contain impurities other than hexagonal boron nitride. Examples of impurities include remaining auxiliary agents and water-soluble boron compounds. In the purification process, such impurities are reduced by washing. After washing, solid-liquid separation is performed and dried to obtain a dry powder. Examples of the cleaning liquid used for cleaning include water, an aqueous solution containing an acidic substance, an organic solvent, and a mixed solution of an organic solvent and water. From the viewpoint of avoiding secondary contamination of impurities, water having an electrical conductivity of 1 mS/m or less may be used. Examples of acidic substances include inorganic acids such as hydrochloric acid and nitric acid. Examples of the organic solvent include water-soluble organic solvents such as methanol, ethanol, propanol, isopropyl alcohol, and acetone. There are no particular restrictions on the cleaning method; for example, the pulverized powder may be immersed in a cleaning liquid and washed by stirring, or the pulverized powder may be cleaned by spraying the cleaning liquid onto the pulverized powder.
洗浄終了後、デカンテーション、吸引ろ過機、加圧ろ過機、回転式ろ過機、沈降分離機又はこれらを組み合わせた装置を用いて洗浄液を固液分離してよい。分離した固形分を通常の乾燥機で乾燥して乾燥粉末を得てもよい。乾燥機は、例えば、棚式乾燥機、流動層乾燥機、噴霧乾燥機、回転型乾燥機、ベルト式乾燥機、及びこれらの組み合わせが挙げられる。乾燥後に、粗大粒子を除去するために、例えば篩による分級を行ってもよい。 After the washing is completed, the washing liquid may be separated into solid and liquid using decantation, a suction filter, a pressure filter, a rotary filter, a sedimentation separator, or a combination thereof. The separated solids may be dried in a conventional dryer to obtain a dry powder. Dryers include, for example, tray dryers, fluidized bed dryers, spray dryers, rotary dryers, belt dryers, and combinations thereof. After drying, classification using a sieve may be performed, for example, in order to remove coarse particles.
このようにして、上述の六方晶窒化ホウ素粉末を得ることができる。上記製造方法で得られる六方晶窒化ホウ素粉末は、帯電減衰性測定によって求められる正負の電荷の減衰速度を比較したときに、正電荷の減衰速度の方が、負電荷の減衰速度よりも大きくてよい。また、負電荷の減衰速度に対する正電荷の減衰速度の比は、１を超え且つ１．５以下であってよい。 In this way, the above-mentioned hexagonal boron nitride powder can be obtained. In the hexagonal boron nitride powder obtained by the above manufacturing method, when comparing the decay rates of positive and negative charges determined by charge decay property measurement, the decay rate of positive charges is greater than the decay rate of negative charges. good. Further, the ratio of the decay rate of positive charges to the decay rate of negative charges may exceed 1 and be 1.5 or less.
上述の六方晶窒化ホウ素粉末の実施形態に係る説明は、六方晶窒化ホウ素粉末の製造方法にも適用することができる。六方晶窒化ホウ素粉末の製造方法は、上述の実施形態に限定されない。例えば、焼成工程の後に、超音波振動を与えるホモジナイザー等を用いて、六方晶窒化ホウ素粉末を解砕する解砕工程を行ってもよい。 The description of the embodiment of the hexagonal boron nitride powder described above can also be applied to the method of manufacturing the hexagonal boron nitride powder. The method for producing hexagonal boron nitride powder is not limited to the embodiments described above. For example, after the firing step, a crushing step of crushing the hexagonal boron nitride powder may be performed using a homogenizer or the like that applies ultrasonic vibration.
以上、本開示の幾つかの実施形態について説明したが、本開示は上記実施形態に何ら限定されるものではない。 Although several embodiments of the present disclosure have been described above, the present disclosure is not limited to the above embodiments.
実施例及び比較例を参照して本開示の内容をより詳細に説明するが、本開示は下記の実施例に限定されるものではない。 The contents of the present disclosure will be explained in more detail with reference to Examples and Comparative Examples, but the present disclosure is not limited to the following Examples.
（実施例１）
［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。
(Example 1)
[Preparation of hexagonal boron nitride powder]
<Calcination process>
100.0 g of boric acid powder (purity of 99.8% by mass or more, manufactured by Kanto Kagaku 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. The mixture was 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. While flowing nitrogen gas into the electric furnace, the temperature was raised from room temperature to 1000°C at a rate of 10°C/min. After holding at 1000°C for 2 hours, heating was stopped and the mixture was allowed to cool naturally. The electric furnace was opened when the temperature became 100°C or less. In this way, a calcined product containing hexagonal boron nitride with low crystallinity was obtained.
＜焼成工程＞
仮焼物１００．０ｇに、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℃で３０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。
<Baking process>
3.0 g of sodium carbonate (purity of 99.5% by mass or more) was added to 100.0 g of the calcined product, and mixed for 10 minutes using an alumina mortar. The mixture was placed in the electric furnace described above. While flowing nitrogen gas into the electric furnace, the temperature was raised from room temperature to 2000°C at a rate of 10°C/min. After holding at 2000°C for 30 hours, heating was stopped and the mixture was allowed to cool naturally. The electric furnace was opened when the temperature became 100°C or lower. The obtained fired product was collected and ground in an alumina mortar for 3 minutes to obtain a coarse powder of hexagonal boron nitride.
＜精製工程＞
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分間攪拌した。攪拌後、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。得られた乾燥粉末を、実施例１の六方晶窒化ホウ素粉末とした。
<Refining process>
In order to remove impurities contained in the hexagonal boron nitride coarse powder, 30 g of the coarse powder was added to 500 g of dilute nitric acid (nitric acid concentration: 5% by mass) and stirred at room temperature for 60 minutes. After stirring, solid-liquid separation was performed by suction filtration, and water (electrical conductivity: 1 mS/m) was replaced and washed until the filtrate became neutral. After washing, it was dried at 120° C. for 3 hours using a drier to obtain a dry powder. The obtained dry powder was used as the hexagonal boron nitride powder of Example 1.
［六方晶窒化ホウ素粉末の評価］
＜外観の評価＞
得られた六方晶窒化ホウ素粉末の外観を観察した。その結果、六方晶窒化ホウ素粉末は、凝集しておらず、流動性に優れることが確認された。
[Evaluation of hexagonal boron nitride powder]
<Appearance evaluation>
The appearance of the obtained hexagonal boron nitride powder was observed. As a result, it was confirmed that the hexagonal boron nitride powder was not agglomerated and had excellent fluidity.
＜帯電減衰性の評価＞
実施例１で作製した六方晶窒化ホウ素粉末の帯電減衰性を、静電気拡散率測定装置（株式会社ナノシーズ製、製品名：ＮＳ－Ｄ１００）を用い、ＪＩＳ Ｃ６１３４０－２－１：２００６に準拠して測定した。測定は、温度２３℃、及び相対湿度５０％に調整された恒湿恒温槽内で行った。正電荷及び負電荷のチャージ時間は１秒間、サンプリング周波数は１Ｈｚ、測定時間は６００秒間とした。センサーから粉体表面までの距離は約１ｍｍとした。５ｃｍ×５ｃｍ×０．４ｃｍ（１０ｃｍ３）のセルに測定試料を入れてサンプルプレートに置き、コロナ放電にて帯電させた。帯電は、正電荷と負電荷のそれぞれで行った。帯電後、測定センサーを駆動し、表面電位の減衰を測定した。得られた表面電位減衰曲線から、正電荷及び負電荷のそれぞれにおける、初期表面電位Ｖ０と６００秒間経過するまでの表面電位（終期表面電位Ｖ１）を求めた。測定間隔は１秒間とした。初期表面電位Ｖ０の値と、所定の減衰時間ｔの際の表面電位Ｖの値の関係を次式に指数近似することによって、減衰速度αを求めた。
<Evaluation of charge attenuation>
The charge decay property of the hexagonal boron nitride powder produced in Example 1 was measured using an electrostatic diffusivity measuring device (manufactured by Nano Seeds Co., Ltd., product name: NS-D100) in accordance with JIS C61340-2-1:2006. It was measured. The measurement was carried out in a constant humidity and temperature chamber adjusted to a temperature of 23° C. and a relative humidity of 50%. The charging time for positive charges and negative charges was 1 second, the sampling frequency was 1 Hz, and the measurement time was 600 seconds. The distance from the sensor to the powder surface was approximately 1 mm. A measurement sample was placed in a 5 cm x 5 cm x 0.4 cm (10 cm 3 ) cell, placed on a sample plate, and charged by corona discharge. Charging was performed with positive charge and negative charge, respectively. After charging, the measurement sensor was driven and the attenuation of the surface potential was measured. From the obtained surface potential decay curves, the initial surface potential V 0 and the surface potential (final surface potential V 1 ) until 600 seconds had elapsed were determined for each of the positive charge and the negative charge. The measurement interval was 1 second. The decay rate α was determined by exponentially approximating the relationship between the value of the initial surface potential V 0 and the value of the surface potential V at a predetermined decay time t using the following equation.
上式中、ｔは減衰時間、Ｖは減衰時間ｔにおける表面電位、Ｖ０は初期表面電位、αは減衰速度をそれぞれ示す。結果を表２に示す。 In the above formula, t is the decay time, V is the surface potential at the decay time t, V 0 is the initial surface potential, and α is the decay rate. The results are shown in Table 2.
＜伸び性の評価＞
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。
<Evaluation of extensibility>
0.2 g of hexagonal boron nitride powder was placed on one end of the artificial skin (length x width = 10 mm x 50 mm). The hexagonal boron nitride powder was stretched in the vertical direction using a spatula so as to spread the hexagonal boron nitride powder onto the surface of the artificial skin. Image analysis was performed using commercially available image analysis software (WinROOF) to determine the ratio of the area of the hexagonal boron nitride powder applied to the total area of the artificial skin. The larger this area ratio is, the better the elongation property is. The evaluation criteria for elongation were as shown in Table 1 according to the area ratio. The elongation evaluation results were as shown in Table 2.
（実施例２）
焼成工程の保持時間を１５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評価を行った。評価結果は表２に示すとおりであった。得られた六方晶窒化ホウ素粉末の外観を観察した。その結果、六方晶窒化ホウ素粉末は、殆ど凝集しておらず、流動性に優れることが確認された。
(Example 2)
Hexagonal boron nitride powder was prepared in the same manner as in Example 1 except that the holding time in the firing step was 15 hours. Then, in the same manner as in Example 1, the hexagonal boron nitride powder was evaluated. The evaluation results were as shown in Table 2. The appearance of the obtained hexagonal boron nitride powder was observed. As a result, it was confirmed that the hexagonal boron nitride powder was hardly agglomerated and had excellent fluidity.
（実施例３）
焼成工程の保持温度を１９００℃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評価を行った。評価結果は表２に示すとおりであった。得られた六方晶窒化ホウ素粉末の外観を観察した。その結果、六方晶窒化ホウ素粉末は、殆ど凝集しておらず、流動性に優れることが確認された。
(Example 3)
Hexagonal boron nitride powder was prepared in the same manner as in Example 1 except that the holding temperature in the firing step was 1900°C. Then, in the same manner as in Example 1, the hexagonal boron nitride powder was evaluated. The evaluation results were as shown in Table 2. The appearance of the obtained hexagonal boron nitride powder was observed. As a result, it was confirmed that the hexagonal boron nitride powder was hardly agglomerated and had excellent fluidity.
（比較例１）
焼成工程における焼成温度を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、評価を行った。結果は表２に示すとおりであった。得られた六方晶窒化ホウ素粉末の外観を観察した。その結果、六方晶窒化ホウ素粉末は、凝集していた。
(Comparative example 1)
Hexagonal boron nitride powder was prepared in the same manner as in Example 1 except that the firing temperature in the firing step was 1700°C. Evaluation was performed in the same manner as in Example 1. The results were as shown in Table 2. The appearance of the obtained hexagonal boron nitride powder was observed. As a result, the hexagonal boron nitride powder was found to be agglomerated.
表２の「減衰速度の比」の欄には、負電荷の減衰速度に対する正電荷の減衰速度の比を示した。実施例１～３の六方晶窒化ホウ素粉末は、正電荷の減衰速度の方が負電荷の減衰速度よりも大きかった。外観を観察すると、比較例１は、凝集ダマを形成しているのに対し、実施例１～３では、凝集ダマが比較例１よりも明らかに少なかった。また、実施例１～３の方が、比較例１よりも、優れた伸び性を有していた。 The "Ratio of Decay Speed" column in Table 2 shows the ratio of the decay speed of positive charges to the decay speed of negative charges. In the hexagonal boron nitride powders of Examples 1 to 3, the rate of decay of positive charges was greater than the rate of decay of negative charges. When observing the appearance, Comparative Example 1 formed aggregated lumps, whereas Examples 1 to 3 had clearly fewer aggregated lumps than Comparative Example 1. Furthermore, Examples 1 to 3 had better elongation properties than Comparative Example 1.
本開示によれば、凝集が抑制された六方晶窒化ホウ素粉末及びその製造方法が提供される。また、上述の六方晶窒化ホウ素粉末を用いることによって凝集が抑制され伸び性に優れる化粧料が提供される。 According to the present disclosure, a hexagonal boron nitride powder with suppressed agglomeration and a method for producing the same are provided. Moreover, by using the above-mentioned hexagonal boron nitride powder, a cosmetic composition with excellent extensibility and suppressed agglomeration can be provided.
Claims (5)
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℃の温度で、１０～５０時間加熱して焼成する焼成工程と、
前記焼成工程で得られる焼成物を粉砕、洗浄及び乾燥し、六方晶窒化ホウ素粉末を得る精製工程と、を有し、
帯電減衰性測定によって求められる正電荷と負電荷の減衰速度を比較したときに、正電荷の減衰速度の方が負電荷の減衰速度よりも大きい、化粧料の原料用の六方晶窒化ホウ素粉末の製造方法。 Raw material powder containing boron-containing compound powder and nitrogen-containing compound powder is fired at 600 to 1300°C in an atmosphere of inert gas, ammonia gas, or a mixed gas of these to produce a powder containing hexagonal boron nitride. a calcination step for obtaining a calcined product;
A firing step of heating and firing the mixed powder containing the calcined material and the auxiliary agent at a temperature of 1900 to 2100° C. for 10 to 50 hours in an atmosphere of inert gas, ammonia gas, or a mixed gas thereof;
A purification step of pulverizing, washing and drying the fired product obtained in the firing step to obtain hexagonal boron nitride powder,
When comparing the decay rate of positive charge and negative charge determined by charge decay property measurement, the decay rate of positive charge is larger than the decay rate of negative charge. Production method.
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