JP2006519700A - 流体力学的キャビテーション結晶化装置および方法 - Google Patents
流体力学的キャビテーション結晶化装置および方法 Download PDFInfo
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Abstract
Description
30グラムの工業状グレードNaCl(塩化ナトリウム−供給溶液)を,ビーカー内の蒸留水100mlに溶解させた。200mlのエタノール(逆溶媒(エタノール95%+メタノール5%,Aldric(商標)))を,逆溶媒/供給溶液の容積比=2:1となるように,ビーカーに添加した。
溶液をNaCl(塩化ナトリウム)結晶が現れるまで攪拌した。攪拌後,生成物をフィルターにかけた。結晶粒の大きさ(d90)は150ミクロンであった。
結晶化プロセスを,図4に図示で,上述したキャビテーション装置400で実行し,ここで,装置400は,8,000psi,公称流速800ml/minの動作能力をもつ。使用されたオリフィスは0.010インチ(0.0254cm)の直径,600psi上部圧力のものである。エタノール(逆溶媒)を,高圧で貫通チャネル415に供給し,NaCl(供給溶液)を高圧で,オリフィス450の上流のポート455を経て貫通チャネル415に,逆溶媒/供給溶液比が2:1で導入した。組み合わされた逆溶媒と供給溶液はオリフィス450を通過し,流体力学的キャビテーションにより核の形成がなされる。
結晶粒の大きさ(d90)は30ミクロンであった。
例2の結晶化プロセスが結晶化装置400で繰り返されたが,3,000psiという非常に高い流体力学的圧力の下でなされた。
結晶粒の大きさ(d90)は20ミクロンであった。
例2の結晶化プロセスが結晶化装置400で繰り返されたが,6,500psiという非常に高い流体力学的圧力の下でなされた。
結晶粒の大きさ(d90)は14ミクロンであった。
例2の結晶化プロセスが結晶化装置400で繰り返されたが,1,000psiという非常に高い流体力学的圧力の下でなされた。
結晶粒の大きさ(d90)は10ミクロンであった。
結晶化プロセスを,図5に図示で,上述したキャビテーション装置500で実行し,ここで,使用されたオリフィスは400psi上部圧力の下,0.010インチ(0.0254cm)の直径をもつ。
2000mlのエタノール(逆溶媒)を結晶化装置500で循環させた。250mlのNaClの溶液が入口ポート455を経てオリフィス450の局所制限部に直接向かうように結晶化デバイス500に添加した。添加時間は7分であった。
結晶粒の大きさ(d90)は20ミクロンであった。
Claims (30)
- 結晶化キャビテーションを利用して,化合物を結晶化するための方法であって,
結晶化させるべき化合物を含む溶液の,少なくともひとつの流体流と,逆溶媒の,少なくともひとつの流体流とを混合するプロセスと,
結晶の核を生成し,さらに結晶を直接形成するために,流体力学的キャビテーションを形成すべく,流れの局所制限部に,圧力が上昇した混合流体を通過させる工程と,
を含む方法。 - 結晶化させるべき化合物が無機剤である,請求項1の記載の方法。
- 結晶化させるべき化合物が有機材である,請求項1の記載の方法。
- 混合する工程が,流れの局所制限部の前で生ずる,請求項1に記載の方法。
- 混合する工程が,流れの局所制限部で生ずる,請求項1に記載の方法。
- 流体力学的キャビテーションがキャビテーション発生器により形成される,請求項1に記載の方法。
- 流体力学的キャビテーションを使用して化合物を結晶化する装置であって,
貫通チャネルであって,該貫通チャネルに逆溶媒を入れるための入口を有するところの貫通チャネルと,
結晶化させるべき化合物を含む溶液を貫通チャネルに導入し,逆溶媒と溶液とを混合できるように,貫通チャネル内に位置するポートと,
流体力学的キャビテーションにより結晶の核を生成し,さらに結晶を直接形成するために,流れの局所制限部を形成すべく,貫通チャネル内に位置するキャビテーション発生器と,
を含む装置。 - 貫通チャネルが実質的に円形の断面を有する,請求項7に記載の装置。
- ポートが,流れの局所制限部の上流に位置する,請求項7に記載の装置。
- ポートが,流れの局所制限部内に位置する,請求項7に記載の装置。
- 結晶化させるべき化合物を含む第二の溶液を導入するために,貫通チャネルに位置する第二のポートをさらに含む,請求項7に記載の装置。
- 第二のポートが流れの局所制限部の上流に位置する,請求項11に記載の装置。
- 第二のポートが流れの局所制限部内に位置する,請求項11に記載の装置。
- キャビテーション発生器が貫通チャネル内に位置するバッフルを含み,該バッフルが,流体流と衝突する円錐状表面,および貫通チャネルとともに流れの局所制限部を形成する円筒状表面を有する,請求項7に記載の装置。
- 流れの局所制限部が環状オリフィスである,請求項14に記載の装置。
- キャビテーション発生器が,流れの局所制限部を形成するように中に位置する,少なくともひとつのオリフィスを有するディスクを含む,請求項7に記載の装置。
- キャビテーション発生器が,貫通チャネルの壁から離れた少なくともひとつのバッフルを含み,このことにより,流れの局所制限部が,その壁とバッフルとの間に形成される,請求項6に記載の方法。
- 少なくともひとつの界面活性剤を,混合した流体流に添加する,請求項1に記載の方法。
- 結晶の核の生成および直接の結晶の形成が,流れの局所制限部の下流に位置する流体力学的キャビテーション場で生じる,請求項1に記載の方法。
- 結晶化プロセスで結晶の核を形成する方法であって,
少なくともひとつの供給溶液の流体流および少なくとのひとつの逆溶媒の流体流を水力学的キャビテーション結晶化装置に流し,該装置内で,混合流体流を形成するために,供給溶液および逆溶媒を混合する工程と,
前記装置内で,混合した流体流を流れの局所制限部に通過させ,このことにより流れの局所制限部の下流にキャビテーション泡を形成する工程と,
結晶の核を生成し,結晶を生成するために、キャビテーションを上昇した静的圧力領域で潰す工程と,
を含む方法。 - 少なくともひとつの界面活性剤を流体力学的キャビテーション結晶化装置に添加する工程と,供給溶液,逆溶媒および混合した流体流のひとつ以上と界面活性剤と混合する工程とを含む,請求項20に記載の方法。
- 結晶を分離する工程を含む,請求項20に記載の方法。
- 少なくともひとつの供給溶液または少なくともひとつの逆溶媒が,エタノール,メタノール,エチルアセテート,ハロゲン化溶媒,塩化メチレン,アセトニトリル,酢酸,ヘキサン,エーテルおよび水のひとつ以上を含む,請求項20に記載の方法。
- 少なくともひとつの供給溶液または少なくともひとつの逆溶媒がひとつ以上の界面活性剤を含む,請求項20に記載の方法。
- 流れの局所制限部が,貫通チャネルの壁の少なくとも一部と,該壁の少なくとも一部から離れたバッフルとの間に画定される,請求項20に記載の方法。
- 装置内の流れの局所制限部に,混合した流体流を通過させる工程が,その混合した流体流の速度を,少なくともひとつの供給溶液と少なくともひとつの逆溶媒の物理的特性により決定される最小速度に増加させることを含む,請求項20に記載の方法。
- 化合物から結晶を形成する方法であって,
流体力学的キャビテーションを形成することができる装置内の流れの局所制限部に第一の流体を流す工程と,
流れの局所制限部に第二の流体を導入して第一の流体と第二の流体との混合流体を形成する工程と,
流れの局所制限部の下流に流体力学的キャビテーション場,および混合流体中にキャビテーション泡を生成する工程と,
結晶の核を生成し,結晶を形成するために、キャビテーションを上昇した静的圧力領域で潰す工程と,
を含む方法。 - 第一の流体が少なくともひとつの供給溶液を含み,第二の流体が少なくともひとつの逆溶媒を含む,請求項27に記載の方法。
- 第一の流体が少なくともひとつの逆溶媒を含み,第二の流体が少なくともひとつの供給溶液を含む,請求項27に記載の方法。
- 流れの局所制限部が,貫通チャネルの壁の少なくとも一部,該壁の少なくとも一部から離れたバッフルとの間に画定される,請求項27に記載の方法。
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US60/452,046 | 2003-03-04 | ||
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US7314516B2 (en) | 2004-12-29 | 2008-01-01 | Five Star Technologies, Inc. | Hydrodynamic cavitation crystallization device and process |
US9732068B1 (en) | 2013-03-15 | 2017-08-15 | GenSyn Technologies, Inc. | System for crystalizing chemical compounds and methodologies for utilizing the same |
WO2015087268A2 (en) | 2013-12-12 | 2015-06-18 | Indian Institute Of Technology Madras | Systems and methods for gas hydrate slurry formation |
CN112569628A (zh) * | 2020-12-09 | 2021-03-30 | 湖北富奕达电子科技有限公司 | 一种对内部结晶后颗粒直接输出的磷酸二氢铝的结晶反应釜 |
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GB899667A (en) * | 1960-04-19 | 1962-06-27 | Glaxo Lab Ltd | Crystalline griseofulvin |
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SU1785115A1 (ru) * | 1990-06-04 | 1996-05-10 | Кировский Политехнический Институт | Кавитационный смеситель |
DE69112917T2 (de) * | 1990-06-15 | 1996-05-15 | Merck & Co Inc | Kristallisationsverfahren zur Verbesserung der Kristallstruktur und -grösse. |
ATE161742T1 (de) * | 1992-10-06 | 1998-01-15 | Merck & Co Inc | Kristallisationsvorrichtung mit zwei strahlen |
GB9413202D0 (en) * | 1994-06-30 | 1994-08-24 | Univ Bradford | Method and apparatus for the formation of particles |
WO1997030292A1 (en) | 1996-02-15 | 1997-08-21 | Oleg Vyacheslavovich Kozyuk | Method and device for obtaining a free disperse system in liquid |
AUPO129096A0 (en) | 1996-07-26 | 1996-08-22 | Boc Gases Australia Limited | Oxygen dissolver for pipelines or pipe outlets |
US5937906A (en) | 1997-05-06 | 1999-08-17 | Kozyuk; Oleg V. | Method and apparatus for conducting sonochemical reactions and processes using hydrodynamic cavitation |
US5931771A (en) | 1997-12-24 | 1999-08-03 | Kozyuk; Oleg V. | Method and apparatus for producing ultra-thin emulsions and dispersions |
US6365555B1 (en) | 1999-10-25 | 2002-04-02 | Worcester Polytechnic Institute | Method of preparing metal containing compounds using hydrodynamic cavitation |
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US5969207A (en) * | 1994-02-02 | 1999-10-19 | Kozyuk; Oleg V. | Method for changing the qualitative and quantitative composition of a mixture of liquid hydrocarbons based on the effects of cavitation |
WO2000053282A1 (en) * | 1999-03-10 | 2000-09-14 | Smithkline Beecham P.L.C. | Crystallization process for producing fine crystal products |
JP2002540930A (ja) * | 1999-04-08 | 2002-12-03 | ペント ベルント | 化学的プロセスおよび物理的プロセスを実施するための方法および装置 |
WO2001014036A1 (en) * | 1999-08-19 | 2001-03-01 | Aventis Pharma Limited | Process for producing fine medicinal substances |
WO2001032125A2 (en) * | 1999-11-03 | 2001-05-10 | Glaxo Group Limited | Apparatus and process for preparing crystalline particles |
WO2001062373A1 (de) * | 2000-02-28 | 2001-08-30 | Locher, Manfred, Lorenz | Kavitationsmischer |
WO2002089942A1 (en) * | 2001-05-05 | 2002-11-14 | Accentus Plc | Formation of small crystals |
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EP1603652A2 (en) | 2005-12-14 |
CA2517727A1 (en) | 2004-09-16 |
WO2004078338B1 (en) | 2005-08-11 |
JP5090729B2 (ja) | 2012-12-05 |
WO2004078338A2 (en) | 2004-09-16 |
MXPA05009413A (es) | 2005-11-04 |
EP1603652B1 (en) | 2009-07-01 |
EP1603652A4 (en) | 2006-08-09 |
WO2004078338A3 (en) | 2005-06-02 |
DE602004021781D1 (de) | 2009-08-13 |
EP2165745A1 (en) | 2010-03-24 |
CA2517727C (en) | 2012-09-04 |
ATE435059T1 (de) | 2009-07-15 |
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