JP4611989B2 - マイクロチャネルプロセス技術を用いてエマルジョンを作製するプロセス - Google Patents
マイクロチャネルプロセス技術を用いてエマルジョンを作製するプロセス Download PDFInfo
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- JP4611989B2 JP4611989B2 JP2006532956A JP2006532956A JP4611989B2 JP 4611989 B2 JP4611989 B2 JP 4611989B2 JP 2006532956 A JP2006532956 A JP 2006532956A JP 2006532956 A JP2006532956 A JP 2006532956A JP 4611989 B2 JP4611989 B2 JP 4611989B2
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Description
プロセスマイクロチャネルおよび/または液体チャネルに密着して加熱および/または冷却を制御する熱交換チャネルは、複数のプロセスマイクロチャネルの間の一様な温度プロファイルを提供することができる。これによって、混合タンクなどの従来の処理設備を用いて得ることができるよりも速い速度での一様な加熱および冷却が可能になる。多重チャネルマイクロチャネルミキサーにおいて、プロセス流れの長さ方向の少なくともいくつかの軸位置で、プロセスマイクロチャネル間の温度差を約5℃より小さく、一つの実施態様では約2℃より小さく、一つの実施態様では約1℃より小さくすることができる。
本発明のプロセスは、ビチューメンを含有する高速沈降エマルジョンをつくるために用いることができる。これらのエマルジョンは、道路、車道および類似物などのセメントまたはアスファルト表面のための表面装飾として用いることができる。これらのエマルジョンは、約60から約70重量%のビチューメンを含み、処理される表面の上に吹き付けることができる。これらの表面装飾の上にチッピングを広げ、ロールして適切な埋め込みおよび整列を確実にする。これは、防水表面シールおよび改善した表面組織も提供する。
本発明のプロセスは、晶析プロセス、例えば連続晶析プロセス中で用いることができる。このプロセスは、指定されるサイズの粉を単離、精製および/または製造するために用いることができる。そのような結晶の例は、高度に精製した砂糖を含む。エマルジョン晶析では、融解物は、バルク融解物中より低い速度で均一な核形成が起こるように、エマルジョンの液滴中で結晶化することができる。このプロセスは無溶媒で実行することができ、従って低い資本および運転費の利点を提供することができる。
本発明のプロセスは、液晶をつくるために用いることができる。このプロセスで作製される液晶は、分散相が適所に「ロックされる」ので、乳化剤および/または界面活性剤の使用を減らす助けとなり得る。
1.ヘキサン中5分間超音波照射する。多孔性基板がオイルに予備露出されている場合、その都度新しいヘキサンを用いて、ヘキサン超音波処理を繰り返す。
2.室温で一夜または乾燥庫中80℃で10〜20分間空気中で乾燥する。
3.多孔性基板を20%硝酸中20分間超音波照射する。
4.多孔性基板を新しい脱イオン水中5分間超音波照射する。
5.水のpHの読みが5を超えるまで、工程#4を少なくとも3回繰り返す。
6.多孔性基板をアセトンまたはイソプロパノール中で3分間超音波照射する。
7.室温で一夜または乾燥庫中80℃で10〜20分間空気乾燥する。
次に、以下の手順を用いて、多孔性基板を熱処理槽中で熱処理する。すなわち、
1.排気し、窒素で再び満たすことを3回行なう。
2.水素および水の存在下、毎分3.5℃の速度で650℃まで加熱する。
3.窒素を流しながら温度を650℃に30分間維持する。
4.空気中で100時間650℃に温度を維持する。
5.空気中で毎分3.5℃の速度で室温に冷却する。
細孔サイズおよび数に対する熱処理効果をキャラクタリゼーションする方法の一つは、水を用いて透過性試験を実施することである。同じ流量を用いて、熱処理多孔基板および未熱処理多孔基板を通してポンプで水を送液する。図29に示すように、異なる圧力降下曲線が得られる。熱処理基板は、未熱処理基板の圧力降下より高い圧力降下を有する。本実施例では、平均細孔サイズは、0.5から0.44ミクロンに減少し、一方、細孔間距離は0.5から0.6ミクロンに増加する。
重量部
第一の液体(連続水相)
水 82.90
カーボポール(Carbopol)934(ビー・エフ・グッドリッチ(BF Goodrich)/ハリス・アンド・フォード(Harris and Fordが供給する樹脂と特定される製品) 0.20
Na EDTA(ダウケミカル社(Dow Chemical Company)が供給する製品) 0.05
グリセリンUSP(フムコ(Humco)が供給する製品) 4.00
第二の液体(不連続オイル)
ステアリン酸 2.00
セチルアルコール 0.50
モノステアリン酸グリセリン 0.20
モノステアリン酸エチレングリコール 0.30
プロピルパラベン 0.10
メチルパラベン 0.20
ミネラルオイル 7.00
シリコーンフルードDC200(ダウコーニング(Dow Corning)が供給するシリコーンフルードと特定される製品) 1.00
トゥイーン20(ユニケマ・アメリカズ(アイ・シー・アイ)(Uniqema Americas(ICI))が供給する界面活性剤と特定される製品) 0.50
トリエタノールアミン 0.90
以下のプロセス工程が用いられる。すなわち、
1.第二の液体のすべての成分をビーカー中で混合して、75℃に加熱する。トリエタノールアミンは、最後に加える。次に、オイル相貯槽中で第二の液体を75℃に維持する。
2.カーボポール934を水の中に分散させ、75℃に加熱して第一の液体を調製する。次に、第一の液体のための残りの成分を加える。連続相液体ポンプに接続している貯槽中で第一の液体を75℃に維持する。
3.すべての構成部品のためのシステムの加熱動力を75±10℃に調節し、安定化させる。
4.連続相液体ポンプを起動し、2.5リットル/分の流量に設定する。
5.オイルポンプを起動し、2.5ミリリットル/分の流量に設定する。多孔基板中の圧力降下を10〜20psiaに維持する。
6.所望量の第二の液体が第一の液体と混合されるまで第一の液体を循環させる。
7.貯槽を冷水/氷浴中に置くことによって、または貯槽中に造られた冷却コイルのスイッチを入れることによって、製品エマルジョンを38℃より低い温度に冷却する。
Claims (36)
- マイクロチャネルミキサー中でエマルジョンをつくる方法であって、
前記マイクロチャネルミキサーは、複数のプロセスマイクロチャネル(110,110a;410;510,520,530,540)を含み、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)は、開口区域(140,140a;240;415,425,435,445;511,521,531,541)を備える壁(112,112a;512)および隣接する液体チャネル(170,170a;270;420,430,440,450;550,560)を有し、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)および液体チャネル(170,170a;270;420,430,440,450;550,560)は、離間した平行な複数のシートまたはプレートから作製され、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)および液体チャネル(170,170a;270;420,430,440,450;550,560)は、互いに隣接し、横方向に積層した垂直配向面または上下方向に積層した水平配向面の形で配置され、
前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)内に第一の液体を流す工程、および
前記開口区域(140,140a;240;415,425,435,445;511,521,531,541)を通して前記液体チャネル(170,170a;270;420,430,440,450;550,560)から第二の液体を前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)に流入させ、前記第一の液体と接触させて前記エマルジョンを作製し、ここで該第一の液体は、連続相を形成し、該第二の液体は、該連続相中に分散した不連続相を形成する工程
からなることを特徴とする方法。 - 前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)と熱交換器との間で熱が交換される、請求項1に記載の方法。
- 前記第一の液体および前記第二の液体は、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中の混合ゾーン(113,113a;413;515,525,535,545)で互いに接触する、請求項1または2に記載の方法。
- 前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)は、前記混合ゾーン(113,113a;413;515,525,535,545)中に狭くなった断面を有する、請求項1に記載の方法。
- 前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)は、対向する間隔の離れた複数壁を含み、前記間隔の離れた壁のそれぞれは開口区域を有し、前記第二の液体は前記間隔の離れた壁の前記開口区域を通って前記液体チャネル(170,170a;270;420,430,440,450;550,560)から流れる、請求項1に記載の方法。
- 前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)および前記液体チャネル(170,170a;270;420,430,440,450;550,560)は、エマルジョン作製ユニット(100,100A,100B,100C,100D;200;400,400a,400b;500)中にあり、各エマルジョン作製ユニット(100,100A,100B,100C,100D;200;400,400a,400b;500)は、第一のプロセスマイクロチャネル、第二のプロセスマイクロチャネル、および前記第一のプロセスマイクロチャネルと前記第二のプロセスマイクロチャネルとの間に配置される液体チャネルからなり、各プロセスマイクロチャネルは、開口区域を備える壁を有し、前記第一の液体は、前記第一のプロセスマイクロチャネルおよび前記第二のプロセスマイクロチャネルを通って流れ、前記第二の液体は、前記液体チャネルから前記第一のプロセスマイクロチャネル中の前記開口区域を通って前記第一の液体と接触して流れ、前記第二のプロセスマイクロチャネル中の開口区域を通って前記第一の液体と接触して流れる、請求項1に記載の方法。
- 各液体チャネル(170,170a;270;420,430,440,450;550,560)は、別の開口区域を備え、
前記プロセスは、前記別の開口区域を通して第三の液体を通し、前記液体チャネル中の第二の液体と接触させて液体混合物を形成する工程、および
前記開口区域を通して前記液体混合物を前記プロセスマイクロチャネル中に流入させて前記第一の液体と接触させる工程、
をさらに含む請求項1に記載の方法。 - 前記第一の液体および/または第二の液体は、熱交換チャネル(190;570,580)中の熱交換流体と熱を交換し、前記熱交換チャネル(190;570,580)は、離間した平行な複数のシートまたはプレートから作製される、請求項1に記載の方法。
- 前記プロセスマイクロチャネルのそれぞれの中で別々のエマルジョンが作製され、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)の少なくとも二つの中で作製されるエマルジョンは互いに異なる、請求項1から8のいずれかひとつに記載の方法。
- 各プロセスマイクロチャネル(110,110a;410;510,520,530,540)は二つ以上の開口区域(140,140a;240;415,425,435,445;511,521,531,541)を含み、該開口区域(140,140a;240;415,425,435,445;511,521,531,541)のそれぞれを通って別々の第二の液体が流れる、請求項1に記載の方法。
- 各プロセスマイクロチャネル(110,110a;410;510,520,530,540)は、前記開口区域(140,140a;240;415,425,435,445;511,521,531,541)に隣接する混合ゾーン(113,113a;413;515,525,535,545)と、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)への入口から前記混合ゾーン(113,113a;413;515,525,535,545)まで広がる非開口領域(111,111a;117,117a;411;514,524,534,544)とを有する、請求項1に記載の方法。
- 前記マイクロチャネルミキサーは、少なくとも二つの前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)を含む、請求項1に記載の方法。
- 前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)は、少なくとも一つの第一の液体マニホールドに接続され、該第一の液体は、前記少なくとも一つの第一の液体マニホールドを通って前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)へ流れる、請求項1に記載の方法。
- 前記マイクロチャネルミキサーは、前記液体チャネル(170,170a;270;420,430,440,450;550,560)に接続される少なくとも一つの第二の液体マニホールドをさらに含み、前記第二の液体は、前記少なくとも一つの第二の液体マニホールドを通って前記液体チャネル(170,170a;270;420,430,440,450;550,560)へ流れる、請求項13に記載の方法。
- 前記マイクロチャネルミキサーは、前記熱交換チャネル(190;570,580)と該熱交換チャネルに接続される少なくとも一つの熱交換マニホールドとをさらに含み、熱交換流体が該熱交換マニホールド(350;450)を通って前記熱交換チャネル(190;570,580)へ流れる、請求項13に記載の方法。
- 前記マイクロチャネルミキサーは、横に並べられるかまたは上下に積み重ねられる複数のエマルジョン作製ユニット(100,100A,100B,100C,100D;200;400,400a,400b;500)を備え、各エマルジョン作製ユニット(100,100A,100B,100C,100D;200;400,400a,400b;500)は、プロセスマイクロチャネル(110,110a;410;510,520,530,540)および隣接する液体チャネル(170,170a;270;420,430,440,450;550,560)からなり、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)および隣接液体チャネル(170,170a;270;420,430,440,450;550,560)は、共通の壁を有し、該共通の壁には開口区域(140,140a;240;415,425,435,445;511,521,531,541)がある、請求項1に記載の方法。
- 各開口区域(140,140a;240;415,425,435,445;511,521,531,541)は比較的厚いシートまたはプレートの上に載る比較的薄いシートを含み、前記比較的薄いシートは複数の比較的小さな開口を含み、前記比較的厚いシートまたはプレートは複数の比較的大きな開口を含み、前記比較的小さな開口は、前記比較的大きな開口から当該比較的小さな開口を通して液体を流すのに十分なように、前記比較的大きな開口と位置合わせされており;または各開口区域は多孔質材料から作られ、該多孔質材料は金属、非金属、酸化されている、またはアルミナ、ニッケルまたはそれらの組み合わせでコーティングされており;または各開口区域は、多孔質材料から作られ、前記多孔質材料の表面は、前記表面の細孔を液体充填材で埋め、前記充填材を固化させ、前記表面を研削および/または研磨し、前記充填材を取り除くことによって処理される、請求項1に記載の方法。
- 各プロセスマイクロチャネル(110,110a;410;510,520,530,540)は、前記プロセスマイクロチャネルを通る液体の流れに垂直な最大50mmの内部寸法を有する、請求項1に記載の方法。
- 各プロセスマイクロチャネル(110,110a;410;510,520,530,540)は、鋼;モネル;インコネル;アルミニウム;チタン;ニッケル;銅;真鍮;任意の前記金属の合金;重合体;セラミック;ガラス;重合体とガラス繊維とを含むコンポジット;石英;ケイ素;またはそれらの二つ以上の組み合わせからなる材料で作られる、請求項1に記載の方法。
- 各液体チャネル(170,170a;270;420,430,440,450;550,560)は、該液体チャネル(170,170a;270;420,430,440,450;550,560)を通る液体の流れに垂直な0.05mmから100cmの内部寸法を有する、請求項1に記載の方法。
- 前記熱交換器は、電熱素子、抵抗加熱器、非流体冷却素子および/または熱交換チャネル(190;570,580)からなり、該熱交換チャネル(190;570,580)は、該熱交換チャネル(190;570,580)通る熱交換流体の流れに垂直な最大50mmの内部寸法を有する請求項2に記載の方法。
- 前記熱交換器は、熱交換チャネルと該熱交換チャネル(190;570,580)中の熱交換流体からなり、該熱交換流体は、前記熱交換チャネル(190;570,580)中で相変化を受ける、請求項2に記載の方法。
- 前記熱交換器は、熱交換チャネル(190;570,580)からなり、該交換チャネル(190;570,580)で吸熱プロセスが実施される、または前記交換チャネル(190;570,580)で発熱プロセスが実施される、請求項2に記載の方法。
- 前記熱交換器は、熱交換チャネル(190;570,580)および該熱交換チャネル(190;570,580)中の熱交換流体からなり、該熱交換流体は、前記第一液体、前記第二液体、前記第一液体と前記第二液体との混合液体、空気、水蒸気、液体水、一酸化炭素、二酸化炭素、気体窒素、液体窒素、気体炭化水素または液体炭化水素からなる、請求項2に記載の方法。
- 前記不連続相は、最大200ミクロンの範囲の体積基準平均直径と、0.01から10の範囲のスパンを有する液滴からなる、請求項1に記載の方法。
- 前記エマルジョンは、油中水エマルジョン、水中油エマルジョン、水中油中水エマルジョン、または油中水中油エマルジョンである、請求項1に記載の方法。
- 前記エマルジョンは、有機液体、液体炭化水素、天然オイル、合成オイル、植物起源の誘導液体、鉱物起源の誘導液体、通常液体の炭化水素燃料、脂肪族アルコール、脂肪酸エステル、またはそれらの混合物からなる、請求項1に記載の方法。
- 前記エマルジョンは、6個から22個の炭素原子の直鎖脂肪酸と6個から22個の炭素原子の直鎖または分岐脂肪族アルコールとのエステル;6個から13個の炭素原子の分岐カルボン酸と6個から22個の炭素原子の直鎖または分岐脂肪族アルコールとのエステル;18個から38個の炭素原子のアルキルヒドロキシカルボン酸と6個から22個の炭素原子の直鎖または分岐脂肪族アルコールとのエステル;6個から22個の炭素原子の直鎖または分岐脂肪酸と多価アルコールおよび/またはゲルベ(Guerbet)アルコールとのエステル;6個から18個の炭素原子の一つ以上の脂肪酸からつくられるトリグリセリド;6個から18個の炭素原子の一つ以上の脂肪酸からつくられるモノ、ジおよび/またはトリグリセリドの混合物;6個から22個の炭素原子の一つ以上の脂肪族アルコールおよび/またはゲルベアルコールと一つ以上の芳香族カルボン酸とのエステル;2個から12個の炭素原子の一つ以上のジカルボン酸と1個から22個の炭素原子を含む一つ以上の直鎖または分岐アルコール、2個から10個の炭素原子および2個から6個のヒドロキシル基を含む一つ以上のポリオール、または一つ以上のアルコールおよび一つ以上のポリオールの混合物とのエステル;2個から12個の炭素原子の一つ以上のジカルボン酸と1個から22個の炭素原子の一つ以上のアルコールとのエステル;安息香酸と6個から22個の炭素原子の直鎖および/または分岐アルコールとのエステル;6個から22個の炭素原子の一つ以上の分岐第一アルコール、6個から22個の炭素原子の一つ以上の直鎖および/または分岐脂肪族アルコール炭酸エステル;6個から22個の炭素原子の一つ以上の脂肪族アルコールからつくられる一つ以上のゲルベ(Guerbet)炭酸エステル;各アルキル基が1個から12個の炭素原子を含む一つ以上のジアルキルナフタレート;アルキル基あたり6個から22個の炭素原子を含む一つ以上の直鎖または分岐、対称または非対称ジアルキルエーテル;6個から22個の炭素原子のエポキシド化脂肪酸エステルと2個から10個の炭素原子および2個から6個のヒドロキシル基を含むポリオールとの一つ以上の開環生成物からなる、請求項1に記載の方法。
- 前記エマルジョンは、さらに、少なくとも一つの乳化剤;界面活性剤;紫外線保護因子;ワックス;稠度因子;増粘剤;過脂肪剤;安定剤;カチオン性、アニオン性、双性イオン、両性または非イオン性重合体;シリコーン化合物;脂肪;ワックス;レシチン;リン脂質;生体薬剤;酸化防止剤;脱臭剤;発汗抑制剤;フケ防止剤;膨潤剤;駆虫剤;自己なめし剤;チロシン阻害剤;可溶化剤;防腐剤;香油;色素;またはそれら二つ以上の混合物からなる、請求項1に記載の方法。
- 前記エマルジョン中に固体が分散する、請求項1に記載の方法。
- 前記エマルジョンの光学的または熱光学的特性が前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で調節され、または化学反応が前記プロセスマイクロチャネル中で実施され、または生物プロセスが前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で実施され、または液体吸着プロセスが前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で実施され、または液−気吸着プロセスが前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で実施され、または液体分離プロセスが前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で実施され、または固化プロセスが前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で実施され、またはガス化プロセスが前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で実施され、または前記エマルジョン中の帯電粒子が前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中で追跡されることからなる、請求項1に記載の方法。
- 前記エマルジョンは、スキンケア製品、ペイントまたはコーティング組成物、接着剤組成物、グルー組成物、コーキング組成物、シーラント組成物、食品組成物、農業用組成物、医薬品組成物、燃料組成物、潤滑剤組成物、表面装飾組成物、シリコーンエマルジョン、結晶を含む組成物、液晶組成物、ワックスエマルジョン、または二重エマルジョンである、請求項1に記載の方法。
- 前記方法は、分あたり少なくとも1リットルのエマルジョンを製造する、請求項1に記載の方法。
- 前記プロセスマイクロチャネル壁と該プロセスマイクロチャネル(110,110a;410;510,520,530,540)内の前記エマルジョンの流量との間の温度勾配は、前記プロセスマイクロチャネル中の同じ軸方向位置において5℃以下である、請求項2に記載の方法。
- 前記熱交換器は、前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)の長さに沿って複数の温度ゾーンを含む、請求項2に記載の方法。
- 前記プロセスマイクロチャネル(110,110a;410;510,520,530,540)中を流れる前記液体の流速は、秒あたり0.01から100mの範囲である、請求項1に記載の方法。
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US10/440,056 US7485671B2 (en) | 2003-05-16 | 2003-05-16 | Process for forming an emulsion using microchannel process technology |
US54815204P | 2004-02-25 | 2004-02-25 | |
PCT/US2004/014736 WO2004103539A2 (en) | 2003-05-16 | 2004-05-12 | Process for forming an emulsion using microchannel process technology |
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2004
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- 2004-05-12 JP JP2006532956A patent/JP4611989B2/ja not_active Expired - Fee Related
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- 2004-05-12 EP EP04751902A patent/EP1633463B1/en not_active Expired - Lifetime
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EP1633463A2 (en) | 2006-03-15 |
CA2526965A1 (en) | 2004-12-02 |
DE602004009681T2 (de) | 2008-08-14 |
CA2526965C (en) | 2011-10-11 |
JP2007516067A (ja) | 2007-06-21 |
EP1633463B1 (en) | 2007-10-24 |
US7307104B2 (en) | 2007-12-11 |
US20040234566A1 (en) | 2004-11-25 |
DE602004009681D1 (de) | 2007-12-06 |
ATE376451T1 (de) | 2007-11-15 |
WO2004103539A3 (en) | 2005-05-19 |
US20080182910A1 (en) | 2008-07-31 |
WO2004103539A2 (en) | 2004-12-02 |
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