JP5940556B2 - エマルジョンの製造方法 - Google Patents
エマルジョンの製造方法 Download PDFInfo
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- JP5940556B2 JP5940556B2 JP2013546646A JP2013546646A JP5940556B2 JP 5940556 B2 JP5940556 B2 JP 5940556B2 JP 2013546646 A JP2013546646 A JP 2013546646A JP 2013546646 A JP2013546646 A JP 2013546646A JP 5940556 B2 JP5940556 B2 JP 5940556B2
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Description
a) 水と水中油型乳化剤を混合して、水相を形成するステップと、
b) 親油性化合物を液体の形態にして、親油性相を形成するステップと、
c) ステップa)の水相とステップb)の親油性相を変形抑制ダイナミックミキサータイプまたはキャビティトランスファーミキサータイプの分布および分散混合装置で混合して、水を連続相とするエマルジョンを作製するステップと
を含み、ミキサーは、伸長流を液体組成物中で誘導するのに適しており、狭い間隔で並んだ相対的に移動可能な、少なくとも1つが中に一連の空洞を有する対向表面を含み、各表面上の空洞を、使用時に液体の流れの断面積が装置を通して少なくとも3倍連続的に増減するように配置される製造方法を提供する。
スパン=[90%積算径における粒子径]-[10%積算径における粒子径]/[50%積算径における粒子径]。
国際公開第96/20270号と同様に、CTMは、対向表面を含み、表面の少なくとも1つ、好ましくは両面が、その中に形成された一連の空洞を有し、表面が相互に相対的に移動し、液体材料が表面間を通り、各表面の空洞を連続的に通過する経路に沿って流れるミキサーと定義される。空洞は、液体が表面間を流れるときせん断が液体に加えられるように当該表面上に配置されている。空洞は、材料がミキサーを通過するとき、流れ有効断面積(effective cross sectional flow area)の変化が比較的小さくなるように、それぞれの表面に配置されている。このようなミキサーにおいては、主に分布混合が得られる。一般に、流れの断面積は、装置を通して3倍未満しか変わらない。表面間の材料の流れに対して概ね垂直方向における表面の相対的運動によって、せん断が加えられる。
・ステーター空洞が、「ローター環」すなわちローター空洞の連続する環を分離する周方向に延びる環によって対向している位置におけるステーター空洞を通したA-A;
・ステーター空洞がローター空洞によって対向している位置におけるステーター空洞とローター空洞との間のB-B;
・ローター空洞が「ステーター環」すなわちステーター空洞の連続する環を分離する周方向に延びる環によって対向している位置におけるローター空洞を通したC-C;
・ローター空洞がステーター空洞によって対向している位置におけるローター空洞とステーター空洞との間のD-D。
国際公開第96/20270号と同様に、CDDMは、対向表面を含み、表面の少なくとも1つ、好ましくは両面が、その中に形成された一連の空洞を有し、表面が相互に相対的に移動し、液体材料が表面間を通り、各表面の空洞を連続的に通過する経路に沿って流れ、伸長変形および/またはせん断変形、好ましくは伸長変形とせん断変形の両方を受けるミキサーとして説明されることによってCTMと区別される。空洞は、表面間の材料の流れと概ね垂直な方向で、表面の相対的な移動によってせん断が加えられるように当該表面上に配置されている。せん断に加えて、著しい伸長流ならびに効率的な分布および分散混合は、対向表面と、装置を通して液体の流れの断面積が少なくとも5倍連続的に増減するように配置された、対向表面内の空洞とを有する装置を設けることによって確実になり得る。
・ステーター空洞が、「ローター環」、すなわちローター空洞の連続する環を分離する周方向に延びる環によって対向している位置におけるステーター空洞を通したA-A;
・「ローター環」がステーター環によって対向している位置において形成される環を通したステーター空洞とローター空洞との間のB-B;
・ローター空洞が「ステーター環」、すなわちステーター空洞の連続する環を分離する周方向に延びる環によって対向している位置におけるローター空洞を通したC-C;
・ローター空洞がステーター空洞によって対向している位置におけるローター空洞とステーター空洞との間のD-D。
本発明は、水を連続相とするエマルジョンの製造方法であって、エマルジョンの分散相が親油性化合物を含み、分散相のザウタ平均粒径が1マイクロメートル未満であり、分散相の濃度がエマルジョンの少なくとも20質量%であり、
a) 水と水中油型乳化剤を混合して、水相を形成するステップと、
b) 親油性化合物を液体の形態にして、親油性相を形成するステップと、
c) ステップa)の水相とステップb)の親油性相を変形抑制ダイナミックミキサータイプまたはキャビティトランスファーミキサータイプの分布および分散混合装置で混合して、水を連続相とするエマルジョンを作製するステップと
を含み、ミキサーは、伸長流を液体組成物中で誘導するのに適しており、狭い間隔で並んだ相対的に移動可能な、少なくとも1つが中に一連の空洞を有する対向表面を含み、各表面上の空洞は、使用時に液体の流れの断面積が装置を通して少なくとも3倍連続的に増減するように配置される製造方法を提供する。
ステップc)において、水を連続相とするエマルジョンが、変形抑制ダイナミックミキサータイプまたはキャビティトランスファーミキサータイプの分布および分散混合装置で、ステップa)の水相とステップb)の親油性相とを混合することによって調製され、ここでミキサーは、伸長流を液体組成物中で誘導するのに適しており、狭い間隔で並んだ相対的に移動可能な、少なくとも1つが中に一連の空洞を有する対向表面を含み、各表面上の空洞は、使用時に液体の流れの断面積が装置を通して少なくとも3倍連続的に増減するように配置される。
第1の表面1は、少なくとも3つの空洞3を含み、空洞の少なくとも1つは、表面1に対して深さ9を有し、
第2の表面2は、少なくとも3つの空洞4を含み、空洞の少なくとも1つは、表面2に対して深さ10を有し、
装置を通過する間に利用可能な液体の流れの断面積が少なくとも3回連続的に増減し、
表面1は、2つの空洞の間で長さ5を有し、
表面2は、2つの空洞の間で長さ6を有し、
表面1、2は、対応する長さ5、6が重なって長さ8を有するスリットを作り、または重ならず、長さ81を作るように位置され、
空洞は、装置を通過する間に利用可能な液体の流れの断面積が少なくとも3倍空洞内で連続的に増大し、少なくとも3分の1にスリット内で減少するように配置され、
2つの表面1、2の間の距離7は、2マイクロメートル〜300マイクロメートルの間であり、
長さ8と2つの表面1、2の間の距離7との比が0〜250の範囲であり、
または長さ81と2つの表面1、2の間の距離7との比が0〜30の範囲である。
本発明は、本発明による方法によって得られる、水を連続相とするエマルジョンも提供する。このようなエマルジョンは、親油性化合物を含む分散相を含み、分散相のザウタ平均粒径は、1マイクロメートル未満であり、分散相の濃度は、エマルジョンの少なくとも20質量%である。
図2および図10に概略的に表したCDDM装置で実験を実施した。この装置は、円筒形ドラムおよび同軸スリーブを備える(対向表面1、2は、円筒形である)。対向表面1、2は、それぞれドラムの外表面およびスリーブの内表面によって規定される。CDDMは、以下のパラメータによって記述することができる:
- スリットの高さ7は、10マイクロメートルであり、
- スリットの長さ8は、120マイクロメートルであり、
- 装置の全長は、10センチメートルであり(長さは、流体が混合されるゾーンを意味する)、
- 軸方向(流れの方向)にCDDMの長さにわたって、流れは、高さ7を有する6つのスリットを経験し、この流れは、6回収縮し、
- 空洞3、4の深さは、最大で2ミリメートルであり、
- ステーターの内径は、25ミリメートルであり、
- 装置の回転速度は、1分間当たり最大25,000回転であり、これは、1分間当たり最大で18,000回転で、これらの実験において稼働した。
粒径およびその分布は、計測器のMastersizer 2000およびZetasizer Nano series ZS(Malvern Instruments、UK)を用いて、静的および動的光散乱(それぞれSLSおよびDLS)を使用して求めた。作製した分散液を、脱イオン水を使用して最初に希釈した(約100倍)。SLS技法を使用して、DLS技法によって行った測定と比較し、DLS検出範囲を越えるより大きい粒子の存在も確認した。ザウタ平均粒径(d3,2)、d4,3、およびスパンは、SLSを使用して求めた。
低温電界放出走査電子顕微鏡を使用した。分散液1滴を内径1mmの黄銅リベット上にマウントし、窒素スラッシュの中に入れた。Gatan Alto 2500クライオプランジャー(cryoplunger)、低温プレパレーションチャンバーに移した後、試料を-98℃で砕き、15秒間エッチングし、-110℃に冷却し、2nmのPt/Pdで被覆した。検査は、5KVで稼働される、-150℃のGatanコールドステージを備えたJEOL 6301F走査型電子顕微鏡を使用して実施した。
CDDM装置を使用した、高度に濃縮されたステロール装填コロイド分散液の調製
Myritol(登録商標)318(中鎖トリグリセリド(MCT)油、Cognis、Monheim am Rhein、ドイツ製)、および結晶性フィトステロールブレンド(84%のβ-シトステロール、7%のフィトスタノール、9%の他のステロールを含有、Cognis、Monheim am Rhein、ドイツ製)を分散相材料として使用した。Tween(登録商標)20として商業的に公知の非イオン性乳化剤ポリオキシエチレン(20)モノラウリン酸ソルビタンは、Sigma Aldrich(UK)から購入した。ホスホリポン80は、Phospholipid GmbH(Cologne、ドイツ)によって供給された。
CDDM装置を、20〜80mL/sの範囲内の流量、および0〜18,000rpmのローター速度で稼働させた。圧力低下は、40〜80barの程度であった。MCT油中に分散したフィトステロールの液滴サイズ分布を静的光散乱によって求め(図3および表1を参照)、これは、すべての回転速度の動的プロセスが、静的プロセスより狭い液滴サイズ分布、したがってより低い多分散性をもたらしたことを示した。15,000rpmで分かるように、より速い速度は、液滴が単分散である液滴サイズ分布に対してより大きいインパクトをもたらし得る。より速い速度で、乳化剤分子は、界面に急速に到達することができ、これは直ちに吸着される。
高濃度のフィトステロールを微細な油滴中に順調に組み込むことができた。この種類の配合物では、活性分子は、過飽和の油溶液中にあり、この場合、各1個の液滴の体積は、処理の間にさらに低減される。表面積が増大すると、1滴当たりの結晶核の数が減少し、したがって、結晶核が互いに到達する機会が減り、結晶化はほとんど起こり得ない。
高圧ホモジナイザーを使用した、ステロール装填コロイド分散液の調製
実施例1と同じ原料を使用し、さらに固体グリセリルトリドデカノエート(glyceryl tridodecanoate)(トリラウリン、Fluka製、46.5℃の融点)をSigma Aldrich(UK)から得た。水中油型(O/W)コロイド分散液を、高圧ホモジナイザー、Microfluidizer M-110S(Microfluidics Internationational Corporation、MA-Newton、USA)を使用して調製した。これは、以下の主要なコンポーネント、すなわち、空気圧モーター、増圧器ポンプ、および相互作用チャンバーからなる。これは、約200〜1,600barの圧力範囲、および約250〜600mL/分(約4〜10mL/s)の流量範囲内で動作することができる。分散相と連続相の比は、10〜90(w/w)であった。連続相中で、乳化剤Tween20の百分率を1%〜4%に変化させ、水の百分率を86%〜89%に変化させた。分散相(10%)は、MCT油またはトリラウリン中の多様なレベルのフィトステロールを用いて調製した。フィトステロールは、全コロイド分散液に基づいて1wt%〜4wt%の範囲であった。これは、10wt%〜40wt%の分散相に等価である。
CDDM装置を使用した、高度に濃縮されたシリコーンワックス装填コロイド分散液の調製
分散相としてシリコーンワックス(ステアリルジメチコンであるSilCare 41M65、Clariant、UK製;融点32℃)を含有するエマルジョンを、CDDMを使用して作製した。ポリマーのPET-POET(国際公開第2010/105922号(A1)に記載されているように社内で調製したポリエチレンテレフタレート-コ-ポリオキシエチレンテレフタレート)を乳化剤として使用した。さらに、ポリオキシエチレン(20)モノラウリン酸ソルビタン乳化剤(Tween(登録商標)20、Sigma Aldrich、UK製)を標準的な対照乳化剤として使用した。
水(27wt%)中のシリコーンワックス(60wt%)コロイド分散液を作製し、Tween20(13wt%)によって安定化させた。CDDM装置に対するd3,2、d4,3、スパン、および圧力低下の結果を以下の表に示す。
水(31wt%)中のシリコーンワックス(60wt%)コロイド分散液を作製し、PET-POET(9wt%)によって安定化させた。CDDM装置に対するd3,2、d4,3、スパン、および圧力低下の結果を以下の表に示す。
高圧ホモジナイザーを使用した、シリコーンワックスコロイド分散液の調製
実施例3と同じ原料を使用した。連続相として脱イオン水および最大1%の乳化剤、ならびに分散相として5%のシリコーンワックスを用いてエマルジョンを調製した。シリコーンワックスは、約80℃〜90℃で融解させた。連続相も80℃〜90℃に加熱して、分散相の温度に合わせた。1つの試料は、香料をさらに含有した。次いで、分散相を連続相に添加し、ローター-ステーターシステム(Ultra Turrax T25 basic(IKA-WERKE GmbH & Co. KG、Staufen、ドイツ)を使用して、13,500rpmで5〜20分間均質化することによって粗いエマルジョンを形成した。粗いエマルジョンの均質化は、温度がワックスの融点より上で維持されることを保証するために水浴に接続された、二重に密封したビーカー内で実施した。粗いエマルジョンを均質化した後、高圧ホモジナイザーのMicrofluidizer M-110S(Microfluidics Internationational Corporation、MA-Newton、USA)を使用して、1,200barで約2サイクルにわたって、これを直ちにさらに均質化した。試料を滅菌容器内に収集し、試料が室温(20℃)に到達するまで冷却するためにベンチ上に放置した。流量は、1秒当たり約4〜6mLであった。
2 表面
3 空洞
4 空洞
5 長さ
6 長さ
7 距離
8 長さ
9 深さ
10 深さ
11 長さ
81 長さ
Claims (13)
- 水を連続相とするエマルジョンの製造方法であって、
前記エマルジョンの分散相が親油性化合物を含み、前記分散相のザウタ平均粒径が1マイクロメートル未満であり、前記分散相の濃度が前記エマルジョンの少なくとも20質量%であり、
(a) 水と水中油型乳化剤を混合して水相を形成するステップと、
(b) 前記親油性化合物を液体の形態にして、親油性相を形成するステップと、
(c) ステップa)の前記水相とステップb)の前記親油性相を変形抑制ダイナミックミキサータイプまたはキャビティトランスファーミキサータイプの分布および分散混合装置で混合して、水を連続相とするエマルジョンを作製するステップと
を含み、前記ミキサーが、伸長流を液体組成物中で誘導し、狭い間隔で並んだ相対的に移動可能な、少なくとも1つが中に一連の空洞を有する対向表面を含み、各表面上の前記空洞が、使用時に前記液体の流れの断面積が前記装置を通して少なくとも3倍連続的に増減するように配置される製造方法。 - ステップa)において、混合物の温度が最大で110℃である、請求項1に記載の方法。
- ステップb)において、前記親油性化合物が、温度を上昇させて前記化合物を融解させることによって液体の形態にされる、請求項1または2に記載の方法。
- 前記親油性化合物が、レシチン、脂肪酸、モノグリセリド、ジグリセリド、トリグリセリド、フィトステロール、フィトスタノール、フィトステリル-脂肪酸エステル、フィトスタニル-脂肪酸エステル、ワックス、脂肪アルコール、カロテノイド、油溶性着色剤、油溶性ビタミン、油溶性香料、油溶性フレグランス、油溶性薬物、鉱油もしくは誘導体、ペトロラタムもしくは誘導体、またはシリコーン油もしくは誘導体、あるいはこれらの化合物の組合せを含む、請求項1から3のいずれか一項に記載の方法。
- 前記親油性化合物が、フィトステロール、カロテノイド、およびこれらの化合物の誘導体の群から選択される、請求項1から4のいずれか一項に記載の方法。
- ステップb)において、前記親油性化合物が非水性相と混合される、請求項1から5のいずれか一項に記載の方法。
- 前記非水性相中の前記親油性化合物の濃度が、少なくとも5質量%である、請求項6に記載の方法。
- 後続のステップにおいて、ステップc)の前記混合物が冷却される、請求項1から7のいずれか一項に記載の方法。
- 前記分散相の前記ザウタ平均粒径が500ナノメートル未満である、請求項1から8のいずれか一項に記載の方法。
- 前記分散相の前記濃度が、前記エマルジョンの少なくとも40質量%である、請求項1から9のいずれか一項に記載の方法。
- ステップc)において、前記変形抑制ダイナミックミキサーまたはキャビティトランスファーミキサーが、距離(7)によって間隔が置かれた2つの対向表面(1、2)を含み、
第1の表面(1)は、少なくとも3つの空洞(3)を含み、前記空洞の少なくとも1つは、前記表面(1)に対して深さ(9)を有し、
第2の表面(2)は、少なくとも3つの空洞(4)を含み、前記空洞の少なくとも1つは、表面(2)に対して深さ(10)を有し、
前記装置を通過する間に利用可能な前記液体の流れの断面積が少なくとも3回連続的に増減し、
前記表面(1)は、2つの空洞の間で長さ(5)を有し、
前記表面(2)は、2つの空洞の間で長さ(6)を有し、
前記表面(1、2)は、対応する前記長さ(5、6)が重なって長さ(8)を有するスリットを作り、または重ならず、長さ(81)を作るように位置され、
前記空洞は、前記装置を通過する間に利用可能な前記液体の流れの前記断面積が少なくとも3倍前記空洞内で連続的に増大し、少なくとも3分の1に前記スリット内で減少するように配置され、
前記2つの表面(1、2)の間の前記距離(7)は、2マイクロメートル〜300マイクロメートルの間であり、
前記長さ(8)と前記2つの表面(1、2)の間の前記距離(7)との比が0〜250の範囲であり、
または前記長さ(81)と前記2つの表面(1、2)の間の前記距離(7)との比が0〜30の範囲である、
請求項1から10のいずれか一項に記載の方法。 - 前記ミキサーが200bar未満の圧力で動作する、請求項1から11のいずれか一項に記載の方法。
- 前記表面の一方が、1分間当たり1,000〜25,000回転の間の周波数で他方の表面に対して回転する、請求項1から12のいずれか一項に記載の方法。
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DE102006053497A1 (de) | 2006-11-14 | 2008-05-15 | Clariant International Limited | Verfahren zur kontinuierlichen Herstellung von Dispersionen in einem Wirbelkammerreaktor |
WO2008125380A1 (en) | 2007-04-11 | 2008-10-23 | Unilever N.V. | Edible fat continuous spreads |
GB0901954D0 (en) * | 2009-02-09 | 2009-03-11 | Unilever Plc | Improvments relating to mixing apparatus |
GB0901956D0 (en) | 2009-02-09 | 2009-03-11 | Unilever Plc | Improvements relating to mixing apparatus |
GB0901955D0 (en) | 2009-02-09 | 2009-03-11 | Unilever Plc | Improvments relating to mixing apparatus |
GB0904700D0 (en) | 2009-03-19 | 2009-04-29 | Unilever Plc | Improvements relating to benefit agent delivery |
DE102010029651A1 (de) | 2010-06-02 | 2011-12-08 | Carl Zeiss Smt Gmbh | Verfahren zum Betrieb einer Projektionsbelichtungsanlage für die Mikrolithographie mit Korrektur von durch rigorose Effekte der Maske induzierten Abbildungsfehlern |
WO2012065824A1 (en) * | 2010-11-15 | 2012-05-24 | Unilever Nv | Mixing apparatus and method for mixing fluids |
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CA2821061A1 (en) | 2012-07-05 |
US20140113852A1 (en) | 2014-04-24 |
CN103459008A (zh) | 2013-12-18 |
BR112013016302A2 (pt) | 2018-06-26 |
US9352289B2 (en) | 2016-05-31 |
EP2658638B1 (en) | 2014-09-03 |
WO2012089474A1 (en) | 2012-07-05 |
ES2524120T3 (es) | 2014-12-04 |
EA201300772A1 (ru) | 2014-11-28 |
BR112013016302B1 (pt) | 2020-10-27 |
JP2014507261A (ja) | 2014-03-27 |
EP2658638A1 (en) | 2013-11-06 |
EA024947B1 (ru) | 2016-11-30 |
CN103459008B (zh) | 2015-08-19 |
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