JP7436595B2 - 複合粉体及びその製造方法 - Google Patents
複合粉体及びその製造方法 Download PDFInfo
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- JP7436595B2 JP7436595B2 JP2022154425A JP2022154425A JP7436595B2 JP 7436595 B2 JP7436595 B2 JP 7436595B2 JP 2022154425 A JP2022154425 A JP 2022154425A JP 2022154425 A JP2022154425 A JP 2022154425A JP 7436595 B2 JP7436595 B2 JP 7436595B2
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- metal oxide
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- phase
- composite powder
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Landscapes
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Description
疎水化金属酸化物エアロゲル粉体を、水親和性の機能成分を含有する水溶性有機溶媒に分散させた後、乾燥することを特徴とする複合粉体の製造方法が提供される。
(1)水性の金属酸化物ゾルを調整する工程
(2)該水性の金属酸化物ゾルをW相とする、O/W/O型エマルションもしくはW/O型エマルションを形成する工程
(3)前記金属酸化物ゾルをゲル化させることにより、前記エマルションをゲル化体がO相に分散した分散液へと変換する工程
(4)O相とW相の2層に分離させる工程
(5)W相を回収して前記ゲル化体がW相に分散した分散液を得る工程
(6)該分散液にシリル化剤を添加する工程
(7)シリル化されたゲル化体を回収する工程
を順に行って、得られた疎水化金属酸化物エアロゲル粉体を、常温で液状を呈する水親和性の機能性成分を含有する水溶性有機溶媒に分散させることにより、細孔中に上記機能性成分を融液の状態で担持せしめ、乾燥することを特徴とする複合粉体の製造方法が提供される。
(1)水性の金属酸化物ゾルを調整する工程
(2)該水性の金属酸化物ゾルをW相とする、O/W/O型エマルションもしくはW/O型エマルションを形成する工程
(3)前記金属酸化物ゾルをゲル化させることにより、前記エマルションをゲル化体がO相に分散した分散液へと変換する工程
(4)O相とW相の2層に分離させる工程
(5)W相を回収して前記ゲル化体がW相に分散した分散液を得る工程
(6)該分散液にシリル化剤を添加する工程
を順に行って、得られたシリル化されたゲル化体に常温で液状を呈する水親和性の機能性成分を含有する水溶性有機溶媒を混合することにより、疎水化金属酸化物エアロゲル粉体の細孔に上記機能性成分を融液の状態で担持させた後、乾燥することを特徴とする複合粉体の製造方法が提供される。
本発明の複合粉体において、疎水化金属酸化物エアロゲル粉体を構成する金属元素は特に限定されることなく、常温・常圧、大気中で安定な酸化物を構成する金属元素であればよい。このような金属酸化物を具体的に例示すると、シリカ(二酸化ケイ素)、アルミナ、チタニア、ジルコニア、マグネシア(MgO)、酸化鉄、酸化銅、酸化亜鉛、酸化錫、酸化タングステン、酸化バナジウム等の単独酸化物、及びこれらのうちの2種以上の金属元素を含む複合酸化物(例えばシリカ-アルミナ、シリカ-チタニア、シリカ-チタニア-ジルコニア等。)が挙げられる。また複合酸化物の場合、単独酸化物が水分に対して比較的敏感なアルカリ金属やアルカリ土類金属(周期律第4周期(Ca)以降)を構成金属元素として含むことも可能である。
上記式(1)において、Sは当該粒子が画像中に占める面積(投影面積)を表す。Lは画像中における当該粒子の外周部の長さ(周囲長)を表す。
本発明の複合粉体において、疎水化金属酸化物エアロゲル粉体の細孔に、常温で液状を呈する水親和性の機能性成分を融液の状態で担持させることが最大の特徴である。即ち、従来の疎水化金属酸化物エアロゲル粉体の使用態様は、高い吸油性を有する粉としての特性を利用したものが殆どであったが、本発明の複合粉体は、前記特定の疎水化金属酸化物エアロゲル粉体の細孔に、機能性成分の融液を担持しておくことにより、油分との接触によりこれを吸収し、担持により内在している上記融液を放出するという従来に無い機能を発揮する。
本発明の複合粉体の製造方法は特に制限されないが、以下の方法により疎水化金属酸化物エアロゲル粉体を製造し、その後、或いは、その製造過程において水親和性の機能性成分の融液を、疎水化金属酸化物エアロゲル粉体の細孔に担持する方法が挙げられる。
本発明に使用する疎水化金属酸化物エアロゲル粉体の製造方法は特に制限されないが、例えば、前記球状の疎水化金属酸化物エアロゲル粉体は、以下に述べる方法により好ましく製造することができる。
本発明の疎水化金属酸化物エアロゲル粉体を構成する粒子を高強度にするという観点から、解乳後に0.5~24時間程度、熟成(エージング(aging))を行うことによってゲル化反応(脱水縮合反応)をさらに進行させることも好ましい。当該熟成は室温~80℃程度で保持することによって行うことができる。
実施例及び比較例で製造した疎水化金属酸化物エアロゲル粉体及び複合粉体に対して、以下の項目について試験を行った。
2000個以上の疎水化金属酸化物エアロゲル粉体粒子についてSEM(日立ハイテクノロジーズ製S-5500、加速電圧3.0kV、二次電子検出)を用いて倍率1000倍で観察したSEM像を画像解析し、上述の定義に従って平均円形度を算出した。
40mlのエタノールに対して当該疎水化金属酸化物エアロゲル粉体を0.3g添加し、シャープマニュファクチュアリング株式会社製の超音波洗浄機UT-105Sを用いて、出力100wで5分間分散させた。尚、上記分散は、外径35mmΦ、容量50mlのラボランスクリュー管瓶を使用し、適正量の水を入れた洗浄槽内に設置して行った。
BET比表面積、及びBJH細孔容積の測定は、上述の定義に従って日本ベル株式会社製BELSORP-maxにより行った。吸油量の測定は、JIS K5101-13-1に規定されている「精製あまに油法」により行った。
複合粉体の機能を確認するために、実施例、比較例において得られた複合粉体を用いて、以下の試験を行った。複合粉体1gにエタノール10g添加し、撹拌子を用いて1000rpmで30分間混合し、複合粉体に坦持したグリセリンをエタノールに抽出した。0.45μmのフィルターで濾別し、エタノール中のグリセリン濃度をガスクロマトグラフィーにより測定することで複合粉体のグリセリン濃度を算出し、この値を接触試験の初期値とした。次に、複合粉体1gにオレイン酸6gを添加し十分に混合した。さらに精製水6gを加えて、複合粉体から放出されたグリセリンを精製水に抽出した。水層を0.45μmのフィルターで濾別後、水層中のグリセリン濃度をガスクロマトグラフィーにより測定し、初期値との比により放出率rを算出した。
実施例、比較例において得られた複合粉体を75メッシュのふるいを通した後、容器に担持した。次に、試験者10名により、得られた複合粉体を実際に顔に塗布してもらい、塗布時の「滑らかさ」、「ソフトフォーカス効果」、「ひんやり感」、塗布後の「テカリの無さ」「しっとり感」について評価した。
以下の方法により、疎水化金属酸化物エアロゲル粉体を製造した。
イソプロピルアルコールを40g、イオン交換水を60g加えて攪拌羽で攪拌し、同時に2%水酸化ナトリウムを2.5g加えて、2.5時間W相を熟成させた。その後、静置することによりO相を上層、W相を下層とする2層に分離した。
実施例1のシリル化処理におけるシリル化剤の使用量を4gとしてシリル化処理後、48%水酸化ナトリウムを18.5g、イオン交換水18.5g加え、攪拌羽で攪拌しながら30分間中和処理を行った。その後、硫酸塩等を除去するためにイオン交換水100mLで3回洗浄後し、濾別した。得られた湿潤ケーク50gに、IPA400g、グリセリン2.5gを加えた後、ロータリーエバポレーターを用いて温度70℃、真空度100hpa以下としてIPAおよび水を除去し、疎水化金属酸化物エアロゲル粉体が19質量%、グリセリン80質量%、水1質量%の複合粉体を得た。
また、その複合粉体をヘプタンに抽出後、ヘプタンを乾燥させることで得られた疎水化金属酸化物エアロゲル粉体の物性を及び複合粉体の物性を表1に示す。
実施例1の方法で得られたM値が47の疎水化金属酸化物エアロゲル粉体10gにイソプロピルアルコール100g、グリセリン2gを加えた後、ロータリーエバポレーターを用いて温度70℃、真空度50hpa以下としてIPAおよび水を除去し、疎水化金属酸化物エアロゲル粉体が83質量%、グリセリン16質量%、水1質量%の複合粉体を得た。
実施例1の方法で得られたM値が47の疎水化金属酸化物エアロゲル粉体5gにイソプロピルアルコール50g、グリセリン5g、表3記載の処方により調製したパウダーファンデーション40gを加えた。その後、ロータリーエバポレーターを用いて温度70℃、真空度50hpa以下としてIPAを除去し、疎水化金属酸化物エアロゲル粉体が10質量%、グリセリン78質量%、その他の粉体11質量%、水1質量%のパウダーファンデーションを得た。
実施例1の方法で得られたM値が47の疎水化金属酸化物エアロゲル粉体5gに、イソプロピルアルコール50gを加えた後、予めトラネキサム酸(trans-4-アミノメチル-1-シクロヘキサンカルボン酸)が20質量%となるようにグリセリンを用いて調製しておいた融液40gを加え、ロータリーエバポレーターを用いて、温度70℃、真空度70hpa以下としてIPAを除去し、疎水化金属酸化物エアロゲル粉体が50質量%、グリセリン41質量%、トラネキサム酸9質量%となる複合粉体を得た。
M値が62の疎水化金属酸化物エアロゲル粉体の物性及び複合粉体の物性を表2に示す。この疎水化金属酸化物エアロゲル粉体は細孔内に水親和性の機能性成分の融液を担持することができなかった。
M値が15の疎水化金属酸化物エアロゲル粉体の物性及びこれを使用して、実施例1と同様の方法により得られた複合粉体の物性を表2に示す。得られた複合粉体の皮脂との接触試験を実施した結果、放出率r=5%となり、水親和性の機能性成分の放出は極めて少なかった。
M値が0の疎水化金属酸化物エアロゲル粉体の物性及びこれを使用して、実施例1と同様の方法により得られた複合粉体の物性を表2に示す。得られた複合粉体の皮脂との接触試験を実施した結果、放出率r=0%となり、皮脂との接触による水親和性の機能性成分は放出されなかった。
Claims (3)
- 疎水化金属酸化物エアロゲル粉体の細孔内に常温で液状を呈する水親和性の機能性成分を融液の状態で担持させた複合粉体の製造方法であって、
疎水化金属酸化物エアロゲル粉体を、水親和性の機能成分を含有する水溶性有機溶媒に分散させた後、乾燥することを特徴とする複合粉体の製造方法。 - 疎水化金属酸化物エアロゲル粉体の細孔内に常温で液状を呈する水親和性の機能性成分を融液の状態で担持させた複合粉体の製造方法であって、
(1)水性の金属酸化物ゾルを調整する工程
(2)該水性の金属酸化物ゾルをW相とする、O/W/O型エマルションもしくはW/O型エマルションを形成する工程
(3)前記金属酸化物ゾルをゲル化させることにより、前記エマルションをゲル化体がO相に分散した分散液へと変換する工程
(4)O相とW相の2層に分離させる工程
(5)W相を回収して前記ゲル化体がW相に分散した分散液を得る工程
(6)該分散液にシリル化剤を添加する工程
(7)シリル化されたゲル化体を回収する工程
を順に行って、得られた疎水化金属酸化物エアロゲル粉体を、常温で液状を呈する水親和性の機能性成分を含有する水溶性有機溶媒に分散させることにより、細孔中に上記機能性成分を融液の状態で担持せしめ、乾燥することを特徴とする複合粉体の製造方法。 - 疎水化金属酸化物エアロゲル粉体の細孔内に常温で液状を呈する水親和性の機能性成分を融液の状態で担持させた複合粉体の製造方法であって、
(1)水性の金属酸化物ゾルを調整する工程
(2)該水性の金属酸化物ゾルをW相とする、O/W/O型エマルションもしくはW/O型エマルションを形成する工程
(3)前記金属酸化物ゾルをゲル化させることにより、前記エマルションをゲル化体がO相に分散した分散液へと変換する工程
(4)O相とW相の2層に分離させる工程
(5)W相を回収して前記ゲル化体がW相に分散した分散液を得る工程
(6)該分散液にシリル化剤を添加する工程
を順に行って、得られたシリル化されたゲル化体に常温で液状を呈する水親和性の機能性成分を含有する水溶性有機溶媒を混合することにより、疎水化金属酸化物エアロゲル粉体の細孔に上記機能性成分を融液の状態で担持させた後、乾燥することを特徴とする複合粉体の製造方法。
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