JP2011219767A - 水性もしくは非水性媒体にポリマー樹脂を押し出しかつ機械的に分散させる連続方法 - Google Patents
水性もしくは非水性媒体にポリマー樹脂を押し出しかつ機械的に分散させる連続方法 Download PDFInfo
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Abstract
【解決手段】機械的分散機にポリマーを含む溶融したもしくは液体分散相の流体を溶融したもしくは液体連続相の流体と合流させ、分散液もしくは乳濁液を形成する工程を含み、ここで(a)前記連続相が前記分散相と実質的に不混和性であり、(b)前記ポリマーが自己分散性であり、又は分散相もしくは連続相のいずれか又は両者が安定化量の界面活性剤を含み、(c)前記ポリマーが機械的分散機と組み合わせた押出機に連続的に押出しされることを特徴とする、安定な分散液もしくは乳濁液を製造する方法。
【選択図】なし
Description
(a)前記連続相が前記分散相と実質的に不混和性であり、
(b)前記ポリマーが自己分散性であり、又は分散相もしくは連続相のいずれか又は両者が安定化量の界面活性剤を含み、
(c)前記ポリマーが機械的分散機と組み合わせた押出機に連続的に押出しされること
を特徴とする。
(a)分散機にR1の流速で連続相液体流体及びR2の流速で分散相液体もしくは溶融流体を連続的に合流させること、及び
(b)この合流させた流体を外部表面活性剤を実質的に存在させないで、相転化することなく分散相比の高い乳濁液を形成するに十分な混合速度で混合すること
の工程を含み、前記分散相液体流体が自己分散性ポリマー又はプレポリマーを含み、R2:R1がこの分散相比の高い乳濁液の中間体積平均粒度が2μm未満であり又は多分散度が2未満であるような比である方法である。
以下の例は本発明を説明するものであり、本発明の範囲を制限するものではない。
連続ハイブリッド分散機において、水中の1タイプエポキシ樹脂(Dow RTC 30240.22)の分散液を製造した。この系は、エポキシ樹脂を70℃にて溶融させ、送り出し、そして分散液を安定させるために必要な界面活性剤と混合するための二軸押出機を含む。上記エポキシ樹脂を25g/minで二軸押出機に供給し、同時に界面活性剤混合物を4.6g/minで押出機のバレルに加えた。界面活性剤は、40/42/10の質量比のDISPONIL TA-430界面活性剤(Henkelの商標)、ATSURF 108界面活性剤(ICI Surfactantsの商標)、及びAEROSOL OT-75(Cytec industriesの商標)の混合物からなる。29.6g/minの速度で押出機から出た後、樹脂/界面活性剤混合物は75℃において5ml/minの速度で流れる水の流体と合流された。この合流された流体をローター分散機(E.T.Oakes, N.Y.)の入口に供給した。34.6g/minの速度で流れる得られた分散液を、40ml/minの速度で流れる第二の水の流体と合流させた。混合した流体を遠心ポンプミキサーに入れ、40パーセント固体レベルまで希釈した。サンプルを集め、その粒度は0.40μmであり、多分散度(粒子の数平均直径に対する体積平均直径の比)は1.17であった。
例1に記載の装置を用い、連続法でエポキシ樹脂ブレンドの分散液を製造した。この樹脂ブレンドは、74.1パーセントの2タイプエポキシ樹脂(DOW DER 692、当量690)、24.4パーセントのエポキシ/フェノール硬化剤(DER 84)、0.8パーセントのベンゾイン(Aldrich Chemical)及び0.7パーセントのRESIFLOW P67流動調節剤(Estron Chemicalの商標)からなる。このブレンドを60g/minの速度で押出機に供給し、26.1g/minのDISPONIL TA-430とATSURF 108界面活性剤の混合物(53/47質量パーセント)と混合した。押出機から出した後、100℃の溶融体を86.1g/minの速度で、95℃でOakes分散機の入口に供給する前に、2.8ml/minの速度で流れるAEROSOL OT-75の流体と合流させた31.4ml/minで流れる水の流体と合流させた。当初の水流体と界面活性剤の流体の合流させた流体の速度は34.2ml/minであった。分散機を出る際に、遠心ミキサーの上流で追加水を加え、この分散液を48パーセント固体まで希釈した。得られた分散液は0.87μmの体積粒度及び2.6の多分散度を有していた。
上記例2に記載の装置を用い、連続法でエポキシ樹脂ブレンドの分散液を製造した。この樹脂ブレンドは、51.3パーセントの2タイプエポキシ樹脂(DOW DER 6224、当量707)と48.7パーセントのポリエステル樹脂(DSM, Uralac P-5598、当量739)の混合物からなる。このブレンドを50g/minの速度で押出機に供給し、7.7g/minのDISPONIL OT-41とATSURF 108界面活性剤の混合物(53/47質量パーセント)と混合した。120℃の溶融体を押出機から出し、11.5g/minの速度で流れる界面活性剤と水を含む流体(10ml/minの速度で流れる水の流体と1.5ml/minの速度で流れるAEROSOL OT-75界面活性剤の流体を合流させることにより形成)と合流させた。この合流させた流体を120℃においてOakes分散機の入口に供給した。分散機を出る際に、遠心ミキサーの上流で追加水を加え、この分散液を44パーセント固体まで希釈した。得られた分散液は5.8μmの体積粒度及び1.8の多分散度を有していた。
一軸押出機を遠心ポンプベース分散機と組み合わせた連続ハイブリッド分散機を用いてVoranolポリエーテルポリオール中のPrimacorEAAの分散液を製造した。ポリマー溶融体を約130℃の温度において10.7g/minの速度で押出機から出し、35g/minの速度で流れる熱い液体ポリエーテルポリオールの流体と合流させる。この合流させた流体を遠心ポンプに送り、ポリマーをポリオールに分散させた。ミキサーから出る際に、生成物を集め、Coulter LS-230粒度分析機を用いて粒度を分析した。全体の体積平均粒度は4.2μmであり、多分散度は6.4であった。
上記例2に記載の装置を用い、連続法でエポキシ樹脂ブレンドの分散液を製造した。この樹脂ブレンドは、51.3パーセントの2タイプエポキシ樹脂(DOW DER 6224、当量707)と48.7パーセントのポリエステル樹脂(DSM, Uralac P-5598、当量739)の混合物からなる。このブレンドを50g/minの速度で押出機に供給し、別の入口からATSURF 108界面活性剤(2.5g/min)を押出機に加えた。この樹脂及びATSURF 108界面活性剤を80〜105℃の温度において分散機に供給した。同時に、ドデシルベンゼンスルホン酸のナトリウム塩を0.5g/minの速度で分散機の上流の水相に加えた。水/アニオン界面活性剤相を25g/minの速度で分散機に供給し、52.5g/minの速度で流れる押出物と合流させた。得られた固体含量の高い分散液流体(77.5g/minの速度で流れる)を希釈ミキサー中で20g/minの速度で流れる水似より希釈し、固体含量が54%である分散液を形成した。得られた分散液は1.3μmの体積粒度及び1.5の多分散度を有していた。
Claims (17)
- 安定な分散液もしくは乳濁液の連続製造方法であって、機械的分散機にポリマーを含む溶融したもしくは液体分散相の流体を溶融したもしくは液体連続相の流体と合流させ、分散液もしくは乳濁液を形成する工程を含み、ここで
(a)前記連続相が前記分散相と実質的に不混和性であり、
(b)前記ポリマーが自己分散性であり、又は分散相もしくは連続相のいずれか又は両者が安定化量の界面活性剤を含み、
(c)前記ポリマーが機械的分散機と組み合わせた押出機に連続的に押出しされること
を特徴とする方法。 - 前記連続相が水又はポリエーテルポリオールである、請求項1記載の方法。
- 前記ポリマーが
(a)他の添加剤をこのポリマーと混合する配合押出法、又は
(b)溶融押出法
によって連続的に押出される、請求項1記載の方法。 - 前記分散相がエポキシ樹脂、ポリエステル、ポリウレタン樹脂、ポリオレフィン、もしくはエチレン−アクリル酸コポリマー、またはこれらの混合物もしくはハイブリッドを含む、請求項3記載の方法。
- 前記分散相がエポキシ樹脂及び硬化剤を含み、前記連続相が水を含む、請求項4記載の方法。
- 前記分散相がポリエチレンを含み、前記連続相がポリエーテルポリオールを含み、このポリエチレン及びポリエーテルポリオールが、無水マレイン酸もしくは無水マレイン酸の半エステルがグラフトしたポリオレフィンとモノアミンポリオールとを反応させることにより製造された安定化量の界面活性剤により安定化されている、請求項4記載の方法。
- 分散相流体と連続相流体を混合する前に、触媒と硬化剤を溶融したポリマー分散相の流体に加える、請求項4記載の方法。
- 前記連続相が水を含み、前記ポリマーがイオン電荷を有するか又は連続相中の酸もしくは塩基の存在によってイオン性にされる基を含む、請求項3記載の方法。
- 前記ポリマーがイオン電荷を有する、請求項8記載の方法。
- 前記ポリマーがカルボン酸基を含み、前記連続相が水及び十分な部分のこの酸基を中和してこのポリマーを電着性にするに十分な塩基を含む、請求項8記載の方法。
- 前記ポリマーがアミン基を含み、前記連続相が水及び十分な部分のこのアミン基を中和してこのポリマーを電着性にするに十分な酸を含む、請求項8記載の方法。
- 前記ポリマーがカルボキシレート基又は4級アンモニウム塩基もしくはアミン塩基によりイオン電荷が与えられている、請求項8記載の方法。
- 導電性表面に安定な水性分散液もしくは乳濁液の一部を付着させる工程をさらに含む、請求項8記載の方法。
- 相転化することのない分散相比の高い乳濁液を製造する方法であって、
(a)分散機にR1の流速で連続相液体流体及びR2の流速で分散相液体もしくは溶融流体を連続的に合流させること、及び
(b)この合流させた流体を外部表面活性剤を実質的に存在させないで、相転化することなく分散相比の高い乳濁液を形成するに十分な混合速度で混合すること
の工程を含み、前記分散相液体流体が自己分散性ポリマー又はプレポリマーを含み、R2:R1がこの分散相比の高い乳濁液の中間体積平均粒度が2μm未満であり又は多分散度が2未満であるような比である方法。 - 前記分散相液体流体がエチレン−アクリル酸コポリマーまたはその中和した塩を含み、前記連続相液体流体がポリエーテルポリオールを含む、請求項14記載の方法。
- 前記分散相液体流体がエポキシ樹脂、ポリエステル、ポリウレタン、又はこれらの組み合わせもしくはハイブリッドを含み、この樹脂がイオン性もしくは非イオン性親水性基の化学的混入によって自己分散性となっている、請求項14記載の方法。
- 前記分散相液体流体が、イオン性又は親水性基の化学的混入によって自己分散性となっているジイソシアネート末端ポリウレタンプレポリマーを含む、請求項14記載の方法。
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US (1) | US6512024B1 (ja) |
EP (1) | EP1189977B2 (ja) |
JP (2) | JP2003500506A (ja) |
KR (1) | KR100750281B1 (ja) |
AR (2) | AR024037A1 (ja) |
AT (1) | ATE291603T1 (ja) |
AU (2) | AU5032900A (ja) |
BR (1) | BR0011596A (ja) |
CA (2) | CA2373551C (ja) |
DE (1) | DE60018931T3 (ja) |
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Also Published As
Publication number | Publication date |
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DE60018931T3 (de) | 2013-02-28 |
WO2000071609A1 (en) | 2000-11-30 |
DE60018931D1 (de) | 2005-04-28 |
CA2373551A1 (en) | 2000-11-30 |
EP1189977A1 (en) | 2002-03-27 |
MXPA01011847A (es) | 2002-05-06 |
AU5032900A (en) | 2000-12-12 |
CA2645399A1 (en) | 2000-11-30 |
EP1189977B2 (en) | 2012-10-10 |
TWI225872B (en) | 2005-01-01 |
KR20020022668A (ko) | 2002-03-27 |
CA2645399C (en) | 2010-11-02 |
DE60018931T2 (de) | 2005-07-28 |
AU5033000A (en) | 2000-12-12 |
BR0011596A (pt) | 2002-03-05 |
JP5643161B2 (ja) | 2014-12-17 |
EP1189977B1 (en) | 2005-03-23 |
US6512024B1 (en) | 2003-01-28 |
WO2000071608A1 (en) | 2000-11-30 |
ATE291603T1 (de) | 2005-04-15 |
JP2003500506A (ja) | 2003-01-07 |
KR100750281B1 (ko) | 2007-08-20 |
CA2373551C (en) | 2009-10-06 |
AR024037A1 (es) | 2002-09-04 |
AR024038A1 (es) | 2002-09-04 |
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