JP2010513690A - 分散体の製造方法 - Google Patents
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Abstract
Description
A−B (I)
式I中のA基は、ナノ粒子の表面と結合することができる基又は部分である。ナノ粒子が溶媒中で処理される状況下で、B基はナノ粒子を処理するために使用されるいかなる溶媒についても相溶性を有する基である。ナノ粒子が溶媒中で処理されない状況下では、B基は、ナノ粒子の不可逆的な凝集を阻止することができる基又は部分である。A及びB構成成分は、結合基が、所望の表面適合性をも付与できる場合には、同一であることが可能である。この相溶性を有する基はマイクロ粒子と反応性であってよいが、一般的には非反応性である。結合組成物は、1つを超える構成成分から構成されても、又は1つを超える工程で作製されてよく、例えば、A組成物は、ナノ粒子の表面と反応するA’部分から構成され、その後、Bと反応し得るA”部分が後に続いてよい。付加順序は重要ではなく、すなわち、A’A”B構成成分の反応は、ナノ粒子との結合前に全体として又は部分的に行うことができる。コーティングにおけるナノ粒子の更なる説明は、M.リンゼンビューラー(Linsenbuhler, M.)ら(「パウダー・テクノロジー(Powder Technology)」158巻、2003年、3〜20頁)に見出すことができる。
表面改質ナノ粒子は、米国特許第6,586,483号(コルブ(Kolb)ら)に記載される手順により調製された。ナルコ(NALCO)2326コロイダルシリカ(ナノ粒子)は、ナルコ・ケミカル社(Nalco Chemical Co.)(イリノイ州ナパーヴィル(Naperville))から入手された。シリカナノ粒子は、ワッカー・シリコーンズ社(Wacker Silicones Corp.)(ミシガン州エイドリアン(Adrian))から入手可能なイソオクチルトリメトキシシランで表面改質され、イソオクチルシラン表面改質シリカナノ粒子として採取された。
セラミック微小球は、米国特許公開第2006/0122049−A1号(H.マーシャル(Marshall)ら)に記載されるように調製され、1重量%の表面改質ナノ粒子(上記のもの)と混合されて、微小球内でのナノ粒子の向上した分散を示した(試料Qとして参照される)。対照試料は、ナノ粒子を有さないセラミック微小球を含有した。使用された微小球は、凝集体を含有した。対照試料及び試料Qは別個の容器の中で混合されて、元々存在していた凝集微小球の減少に留意された。試料Qでは、可視的な凝集体は観察されず、25%ミキサー速度設定で約1分間の混合後に、自由流動性ブレンドが観察された。50%ミキサー速度設定で約2分間の混合後に、対照試料は元々の凝集体の50%超を保有し、断続的な流動を有した。試料Qは、表面改質ナノ粒子を有さない対照試料と対比して、表面改質ナノ粒子の分散体とのセラミック微小球の向上した流動性及び混合を示した。
バンシルW20(微小球)と組み合わせられた表面改質ナノ粒子の分散体1重量パーセント(重量%)及び0.1重量%が調製された。
比較例Aは、エポン(Epon)2004、ジシアンジアミドAB 04、エピ−キュア(Epi-Cure)P103、SMC 1108、緑色顔料C.I.74260、レシフロウ(Resiflow)PL−200、及びバンシル(Vansil)W20(微小球)などの構成成分から、表1(下記)に指示されるようなグラムで構成された。この組成物は、混合及び押出成形プロセスを使用して作製された。この組成物は、まず高剪断ミキサー(サーモプリズム(Thermo Prism)型番B21R 9054 STR/2041)の中で約4000回転毎分(rpm)で20分間にわたってプレミックスされた。プレミックス後に、試料は、30.5cm(12インチ)共回転二軸押出成形機(B&Pプロセシングシステムズ(B&P Processing Systems)、型番MP−2019、15:1の17〜90°のニーディングブロック及び2〜60°のフォワードニーディングブロック)を供給速度設定点1.5で使用して溶融混合された。押出成形機からの組成物の出口温度、押出成形機スクリュー速度、及び混合後の組成物の材料処理量が、表1(下記)に列記される。この実施例は、ナノ粒子及び微小球の分散体を有さなかった。
表1に列記される実施例1〜4は分散体を含む組成物を記載する。これらの分散体の微小球及びナノ粒子は、樹脂及び他の構成成分とのプレミックスに先立って、上記のように調製された。この項に記載される組成物の構成成分は、まず高剪断ミキサー(サーモプリズム(Thermo Prism)型番B21R 9054 STR/2041)の中で約4000rpm(回転毎分)で20秒間にわたってプレミックスされた。次に、この組成物は、30.5cm(12インチ)共回転二軸押出成形機(B&Pプロセシングシステムズ(B&P Processing Systems)、型番MP−2019、15:1の17〜90°のニーディングブロック及び2〜60°のフォワードニーディングブロック)を供給速度設定点1.5で使用して溶融混合され、材料処理量が記録された。押出成形機からの組成物の出口温度、押出成形機スクリュー速度、及び混合後の組成物の材料処理量が、表1(下記)に列記される。
Claims (17)
- 分散体の製造方法であって、該方法が、
マイクロ粒子、ナノ粒子及び流体ポリマー構成成分を混合して分散体を形成する工程を含み、そこでは、前記ナノ粒子が、ナノ粒子を有さない比較可能な分散体と対比して、材料処理量を増加するために十分な分量で存在する、方法。 - 前記ナノ粒子が、ナノ粒子を有さない比較可能な分散体と対比して、混合時間を削減するために十分な分量で存在する、請求項1に記載の方法。
- 前記マイクロ粒子が、充填剤、増量剤、セラミックビーズ、セラミックバブル、セラミック微小球、顔料、及びこれらの組み合わせからなる群から選択される、請求項1に記載の方法。
- 前記マイクロ粒子が、0.5マイクロメートルを超える中央粒径を有する、請求項1に記載の方法。
- 前記ナノ粒子が、シリカ、チタニア、アルミナ、酸化ニッケル、ジルコニア、バナジア、セリア、酸化鉄、酸化アンチモン、酸化スズ、酸化亜鉛、リン酸カルシウム、カルシウムヒドロキシアパタイト、及びこれらの組み合わせからなる群から選択される、請求項1に記載の方法。
- 前記流体ポリマー構成成分が、ポリマー樹脂、オリゴマー樹脂、モノマー及びこれらの組み合わせからなる群から選択される、請求項1に記載の方法。
- 前記流体ポリマー構成成分が、熱可塑性又は熱硬化性樹脂である、請求項1に記載の方法。
- 前記ナノ粒子が、表面改質されている、請求項1に記載の方法。
- 前記ナノ粒子が、イソオクチル官能基化シリカナノ粒子である、請求項1に記載の方法。
- 前記ナノ粒子が、前記マイクロ粒子内に分散されている、請求項1に記載の方法。
- 前記材料処理量が、少なくとも5パーセント増加されている、請求項1に記載の方法。
- 前記混合時間が、少なくとも5パーセント削減されている、請求項2に記載の方法。
- 前記ナノ粒子の前記マイクロ粒子に対する重量比が、少なくとも1:100,000である、請求項1に記載の方法。
- 前記ナノ粒子が、前記分散体の総重量に基づいて、少なくとも0.00075重量パーセントの濃度で存在する、請求項1に記載の方法。
- マイクロ粒子、ナノ粒子、及び流体ポリマー構成成分を含む分散体であって、前記ナノ粒子が、ナノ粒子を有さない比較可能な分散体と対比して、材料処理量を増加するために十分な分量で存在する、分散体。
- 前記マイクロ粒子が、顔料を含む、請求項15に記載の分散体。
- 硬化性構成成分を更に含む、請求項15に記載の分散体を含む組成物。
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Application Number | Priority Date | Filing Date | Title |
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US11/615,552 US20080153963A1 (en) | 2006-12-22 | 2006-12-22 | Method for making a dispersion |
US11/615,552 | 2006-12-22 | ||
PCT/US2007/086720 WO2008079631A1 (en) | 2006-12-22 | 2007-12-07 | Method for making a dispersion |
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JP2010513690A true JP2010513690A (ja) | 2010-04-30 |
JP2010513690A5 JP2010513690A5 (ja) | 2011-02-03 |
JP5231445B2 JP5231445B2 (ja) | 2013-07-10 |
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JP2009543048A Active JP5231445B2 (ja) | 2006-12-22 | 2007-12-07 | 分散体の製造方法 |
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US (1) | US20080153963A1 (ja) |
EP (1) | EP2121811B1 (ja) |
JP (1) | JP5231445B2 (ja) |
CN (1) | CN101563400B (ja) |
WO (1) | WO2008079631A1 (ja) |
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WO2008079631A1 (en) | 2008-07-03 |
EP2121811B1 (en) | 2014-06-18 |
EP2121811A1 (en) | 2009-11-25 |
JP5231445B2 (ja) | 2013-07-10 |
CN101563400B (zh) | 2014-03-19 |
US20080153963A1 (en) | 2008-06-26 |
EP2121811A4 (en) | 2011-08-03 |
CN101563400A (zh) | 2009-10-21 |
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