JP5069224B2 - カルボカチオンの関与による発熱反応の段階的実施法 - Google Patents
カルボカチオンの関与による発熱反応の段階的実施法 Download PDFInfo
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- JP5069224B2 JP5069224B2 JP2008512710A JP2008512710A JP5069224B2 JP 5069224 B2 JP5069224 B2 JP 5069224B2 JP 2008512710 A JP2008512710 A JP 2008512710A JP 2008512710 A JP2008512710 A JP 2008512710A JP 5069224 B2 JP5069224 B2 JP 5069224B2
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/30—Micromixers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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- B01J2219/00027—Process aspects
- B01J2219/0004—Processes in series
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00822—Metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00851—Additional features
- B01J2219/00867—Microreactors placed in series, on the same or on different supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00851—Additional features
- B01J2219/00871—Modular assembly
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00889—Mixing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/0095—Control aspects
- B01J2219/00984—Residence time
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00993—Design aspects
- B01J2219/00997—Strategical arrangements of multiple microreactor systems
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
- F28D21/00—Heat-exchange apparatus not covered by any of the groups F28D1/00 - F28D20/00
- F28D2021/0019—Other heat exchangers for particular applications; Heat exchange systems not otherwise provided for
- F28D2021/0052—Other heat exchangers for particular applications; Heat exchange systems not otherwise provided for for mixers
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F2260/00—Heat exchangers or heat exchange elements having special size, e.g. microstructures
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Description
[第1の滞留時間ユニットのための渦巻き式熱交換器の使用]
アクリロニトリル(AN)対ジアセトンアルコール(DiAOH)対H2SO4の化学量論的モル比が1.0:1.0:2.4である反応溶液の滞留時間は、マイクロリアクター(ハステロイ(Hastelloy)製の混合モジュールと熱交換器モジュールとから構成される)において90℃で12秒、渦巻き式熱交換器において90℃で100秒、連続攪拌槽において50℃で2時間である。
実施例1と同様に行った。表1は、用いられる出発物質、滞留時間、温度および収率を示している。
反応は、AN対DiaOH対H2SO4=1.0:1.0:2.2の化学量論比を用いて73.5%の最終収率、ならびに、マイクロリアクターにおいて90℃で12秒、第1の連続攪拌槽において65℃で960秒、第2の連続攪拌槽において55℃で10800秒の滞留時間分布をもたらした。
実施例7と同様に行った。表2は、用いられる出発物質、滞留時間、温度および収率を示している。
Claims (5)
- カルボカチオンの関与による反応を行うための改良された方法であって、
前記反応は、ジアセトンアクリルアミドを得るための、硫酸の存在下での、アクリロニトリルと、ジアセトンアルコール、アセトン、または酸化メシチルとのリッター反応であり、
反応の初期の最も強い発熱段階を、マイクロリアクター中で、60〜120℃の反応温度および1〜30秒の滞留時間で行うことと、
その後のより弱い発熱の複数の段階を、第1の滞留時間ユニット中及び当該第1の滞留時間ユニットに続く第2の滞留時間ユニット中で行うことと、を含み、
前記第1の滞留時間ユニットにおける滞留時間が1〜30分であり、前記第1の滞留時間ユニットにおける反応温度が、前記マイクロリアクター中と同じか、またはそれより5〜30℃だけ低く、
前記第2の滞留時間ユニットにおける滞留時間が1〜10時間であり、
前記マイクロリアクターにおける反応温度、前記第1の滞留時間ユニットにおける反応温度、及び前記第2の滞留時間ユニットにおける反応温度の中で、前記第2の滞留時間ユニットにおける反応温度は、最も低く、
前記第2の滞留時間ユニットにおける反応温度は30〜70℃である、
方法。 - 前記初期の段階には、T字型ミキサー、マイクロジェットリアクター、副流噴射ミキサー(substream injection mixer)、Y字型またはV字型ミキサー、インターデジタル型ミキサー、矩形ミキサー、スロット型ミキサー、三角形多層ミキサー(triangular multilamination mixer)、キャタピラー型ミキサー、サイクロン型ミキサー、またはこれらの組合せの群からの混合モジュールと、マイクロ直交流熱交換器、直交流混合を伴う直交流熱交換器、または積層型向流熱交換器の群からの1つないし複数のマイクロ熱交換器を有する熱交換モジュールとを有するマイクロリアクターが用いられる、請求項1に記載の方法。
- 前記マイクロリアクターの後に、毛細管、熱交換器、任意に熱安定性ループ型リアクター、攪拌槽、または攪拌槽翼列から構成される第1の滞留時間ユニットが存在する、請求項1または2に記載の方法。
- 攪拌槽または攪拌槽翼列が、第2の滞留時間ユニットとして用いられる、請求項1〜3のいずれか一項に記載の方法。
- 前記リッター反応後に加水分解が行われる、請求項1〜4のいずれか一項に記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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AT0087305A AT501927B1 (de) | 2005-05-23 | 2005-05-23 | Verbessertes verfahren zur durchführung von ritterreaktionen, elektrophilen additionen an alkenen oder friedel-crafts-alkylierungen |
ATA873/2005 | 2005-05-23 | ||
PCT/EP2006/003859 WO2006125502A1 (de) | 2005-05-23 | 2006-04-26 | Schrittweise durchführung von exothermen reaktionen unter beteiligung von carbokationen |
Publications (2)
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JP2008542212A JP2008542212A (ja) | 2008-11-27 |
JP5069224B2 true JP5069224B2 (ja) | 2012-11-07 |
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Application Number | Title | Priority Date | Filing Date |
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JP2008512710A Active JP5069224B2 (ja) | 2005-05-23 | 2006-04-26 | カルボカチオンの関与による発熱反応の段階的実施法 |
Country Status (9)
Country | Link |
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US (1) | US9327263B2 (ja) |
EP (1) | EP1890801B1 (ja) |
JP (1) | JP5069224B2 (ja) |
CN (1) | CN101180118B (ja) |
AT (2) | AT501927B1 (ja) |
EA (1) | EA012312B1 (ja) |
ES (1) | ES2366711T3 (ja) |
HK (1) | HK1119617A1 (ja) |
WO (1) | WO2006125502A1 (ja) |
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EP1956023A1 (en) * | 2007-02-06 | 2008-08-13 | Lonza Ag | Method for lithium exchange reactions |
CN104529689B (zh) * | 2015-01-26 | 2016-08-17 | 深圳市一正科技有限公司 | 9,9,10,10-四苯基-9,10-去氧蒽醌的制备方法 |
CN106117083A (zh) * | 2016-06-23 | 2016-11-16 | 南京工业大学 | 在微结构反应器中制备2‑氰乙基‑5‑降冰片烯‑2‑醛的方法 |
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US3151157A (en) * | 1964-09-29 | Process for the preparation of | ||
US5811580A (en) * | 1996-12-04 | 1998-09-22 | The Lubrizol Corporation | Process for the preparation of N-hydrocarbyl-substituted amides via the ritter reaction using solid clay catalysts |
DE19741645A1 (de) * | 1997-09-22 | 1999-03-25 | Bayer Ag | Verfahren und Vorrichtung zur Oxidation organischer Verbindungen in flüssiger Phase unter Verwendung peroxidischer Oxidationsmittel |
JP4086982B2 (ja) * | 1998-12-01 | 2008-05-14 | 株式会社興人 | N−(1,1−ジメチル−3−オキソブチル)アクリルアミドの製造法 |
DE19935691A1 (de) * | 1999-07-29 | 2001-02-01 | Merck Patent Gmbh | Friedel-Crafts-Acylierung im statischen Mikromischer |
DE19946367A1 (de) * | 1999-09-28 | 2001-03-29 | Merck Patent Gmbh | Verfahren zur Bromierung organischer Verbindungen |
US6537506B1 (en) * | 2000-02-03 | 2003-03-25 | Cellular Process Chemistry, Inc. | Miniaturized reaction apparatus |
DE10020632A1 (de) * | 2000-04-27 | 2001-10-31 | Merck Patent Gmbh | Verfahren zur Expodierung von Olefinen |
DE10031380A1 (de) * | 2000-06-28 | 2002-01-10 | Merck Patent Gmbh | Verfahren zur Übertragung von Alkyliden-Gruppen auf organischen Verbindungen |
DE10031381A1 (de) * | 2000-06-28 | 2002-01-10 | Merck Patent Gmbh | Verfahren zur Kupplung von organischen Verbindungen |
US7098360B2 (en) * | 2002-07-16 | 2006-08-29 | Kreido Laboratories | Processes employing multiple successive chemical reaction process steps and apparatus therefore |
DE10321472B4 (de) | 2003-05-13 | 2005-05-12 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Fluidik-Modul, Verfahren zu seiner Herstellung und Verfahren zum Betreiben eines Fluidik-Moduls |
DE10333174A1 (de) * | 2003-07-22 | 2005-02-17 | Cpc Cellular Process Chemistry Systems Gmbh | Verfahren zur Durchführung einer In-Situ-Quench Reaktion |
DE102004007706A1 (de) * | 2004-02-16 | 2005-08-25 | Dynamit Nobel Gmbh Explosivstoff- Und Systemtechnik | Verfahren zur Herstellung von flüssigen Nitratestern |
JP4308087B2 (ja) | 2004-06-03 | 2009-08-05 | 本田技研工業株式会社 | 船外機の操舵角・チルトトリム角調整装置 |
JP4018084B2 (ja) | 2004-07-12 | 2007-12-05 | キュノ株式会社 | セル型フィルタカートリッジ及びその製造方法 |
DE102004038555B3 (de) * | 2004-08-06 | 2005-08-04 | Plinke Gmbh | Modularer Mikroreaktor zur Nitrierung mit Mischsäure |
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- 2006-04-26 AT AT06753420T patent/ATE511917T1/de active
- 2006-04-26 ES ES06753420T patent/ES2366711T3/es active Active
- 2006-04-26 EA EA200702591A patent/EA012312B1/ru not_active IP Right Cessation
- 2006-04-26 JP JP2008512710A patent/JP5069224B2/ja active Active
- 2006-04-26 EP EP06753420A patent/EP1890801B1/de active Active
- 2006-04-26 US US11/920,847 patent/US9327263B2/en active Active
- 2006-04-26 WO PCT/EP2006/003859 patent/WO2006125502A1/de active Application Filing
- 2006-04-26 CN CN2006800179956A patent/CN101180118B/zh active Active
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Also Published As
Publication number | Publication date |
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HK1119617A1 (en) | 2009-03-13 |
EA012312B1 (ru) | 2009-08-28 |
AT501927B1 (de) | 2007-06-15 |
EP1890801A1 (de) | 2008-02-27 |
EA200702591A1 (ru) | 2008-04-28 |
US9327263B2 (en) | 2016-05-03 |
JP2008542212A (ja) | 2008-11-27 |
CN101180118B (zh) | 2011-04-06 |
ATE511917T1 (de) | 2011-06-15 |
WO2006125502A1 (de) | 2006-11-30 |
EP1890801B1 (de) | 2011-06-08 |
CN101180118A (zh) | 2008-05-14 |
ES2366711T3 (es) | 2011-10-24 |
US20080306300A1 (en) | 2008-12-11 |
AT501927A1 (de) | 2006-12-15 |
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