JP4520698B2 - 少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 - Google Patents
少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 Download PDFInfo
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- JP4520698B2 JP4520698B2 JP2002587393A JP2002587393A JP4520698B2 JP 4520698 B2 JP4520698 B2 JP 4520698B2 JP 2002587393 A JP2002587393 A JP 2002587393A JP 2002587393 A JP2002587393 A JP 2002587393A JP 4520698 B2 JP4520698 B2 JP 4520698B2
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
Description
DE−A19909923号の実施例2と同様に、2段階のプロペンの不均一系触媒による気相酸化の冷却された生成物ガス混合物の分別凝縮によって以下の内容の340kg/hの粗製アクリル酸(粗製溶融物)を製造した:
アクリル酸 97.3質量%、
酢酸 0.8質量%、
プロピオン酸 500質量ppm、
フルフラール 700質量ppm、
無水マレイン酸 40質量ppm、
ベンズアルデヒド 200質量ppm、
水 1.3質量%、
フェノチアジン 150質量ppm
(重合禁止剤)。
Claims (3)
- アクリル酸、メタクリル酸及びN−ビニルピロリドンからなる群から選択される少なくとも1種のモノマーの粗製溶融物の結晶化による精製にあたり、精製されるべき粗製溶融物に懸濁結晶化を行い、該懸濁結晶化の間に生じかつ残留溶融物中に懸濁されたモノマー結晶を第1の機械的分離作業の使用によって残留溶融物から分離し、かつ更なる結晶化工程の少なくとも1つにおいて第1の機械的分離作業後に残留する残留溶融物及び/又は分離された、場合により洗浄されたモノマー結晶をそれらの溶融後に結晶化により更に精製する方法において、第1の機械的分離作業で分離された残留溶融物及び/又は第1の機械的分離作業で分離された、場合により洗浄されて再び溶融されたモノマー結晶に、前記少なくとも1つの更なる結晶化工程へのその経路で、第1の機械的分離作業後に少なくとも1つの濾過を行い、その際、フィルタ材料の細孔サイズが50〜1000μmであることを特徴とする方法。
- 結晶化による残留溶融物の更なる精製を懸濁結晶化によって実施する、請求項1記載の方法。
- 結晶化による残留溶融物の更なる精製を流下液膜結晶化によって実施する、請求項1記載の方法。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10122788A DE10122788A1 (de) | 2001-05-10 | 2001-05-10 | Verfahren der kristallisativen Reinigung einer Roh-Schmelze wenigstens eines Monomeren |
PCT/EP2002/004783 WO2002090310A1 (de) | 2001-05-10 | 2002-05-02 | Verfahren der kristallisativen reinigung einer roh-schmelze wenigstens eines monomeren |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2010056941A Division JP2010132711A (ja) | 2001-05-10 | 2010-03-15 | 少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 |
Publications (3)
Publication Number | Publication Date |
---|---|
JP2004528371A JP2004528371A (ja) | 2004-09-16 |
JP2004528371A5 JP2004528371A5 (ja) | 2010-05-20 |
JP4520698B2 true JP4520698B2 (ja) | 2010-08-11 |
Family
ID=7684328
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
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JP2002587393A Expired - Lifetime JP4520698B2 (ja) | 2001-05-10 | 2002-05-02 | 少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 |
JP2010056941A Withdrawn JP2010132711A (ja) | 2001-05-10 | 2010-03-15 | 少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2010056941A Withdrawn JP2010132711A (ja) | 2001-05-10 | 2010-03-15 | 少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 |
Country Status (6)
Country | Link |
---|---|
US (1) | US7319166B2 (ja) |
EP (1) | EP1387824B1 (ja) |
JP (2) | JP4520698B2 (ja) |
CN (1) | CN1234661C (ja) |
DE (2) | DE10122788A1 (ja) |
WO (1) | WO2002090310A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010132711A (ja) * | 2001-05-10 | 2010-06-17 | Basf Se | 少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 |
Families Citing this family (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8194770B2 (en) | 2002-08-27 | 2012-06-05 | Qualcomm Incorporated | Coded MIMO systems with selective channel inversion applied per eigenmode |
US8170513B2 (en) | 2002-10-25 | 2012-05-01 | Qualcomm Incorporated | Data detection and demodulation for wireless communication systems |
US8134976B2 (en) | 2002-10-25 | 2012-03-13 | Qualcomm Incorporated | Channel calibration for a time division duplexed communication system |
US8320301B2 (en) | 2002-10-25 | 2012-11-27 | Qualcomm Incorporated | MIMO WLAN system |
US8218609B2 (en) | 2002-10-25 | 2012-07-10 | Qualcomm Incorporated | Closed-loop rate control for a multi-channel communication system |
US20040081131A1 (en) | 2002-10-25 | 2004-04-29 | Walton Jay Rod | OFDM communication system with multiple OFDM symbol sizes |
US7002900B2 (en) | 2002-10-25 | 2006-02-21 | Qualcomm Incorporated | Transmit diversity processing for a multi-antenna communication system |
US8169944B2 (en) | 2002-10-25 | 2012-05-01 | Qualcomm Incorporated | Random access for wireless multiple-access communication systems |
US8570988B2 (en) | 2002-10-25 | 2013-10-29 | Qualcomm Incorporated | Channel calibration for a time division duplexed communication system |
US8208364B2 (en) | 2002-10-25 | 2012-06-26 | Qualcomm Incorporated | MIMO system with multiple spatial multiplexing modes |
US7324429B2 (en) | 2002-10-25 | 2008-01-29 | Qualcomm, Incorporated | Multi-mode terminal in a wireless MIMO system |
US7986742B2 (en) | 2002-10-25 | 2011-07-26 | Qualcomm Incorporated | Pilots for MIMO communication system |
US9473269B2 (en) | 2003-12-01 | 2016-10-18 | Qualcomm Incorporated | Method and apparatus for providing an efficient control channel structure in a wireless communication system |
DE102004058071A1 (de) * | 2004-12-01 | 2006-06-08 | Basf Ag | Verfahren zur Reinigung von polaren Vinylverbindungen |
US7705181B2 (en) | 2005-03-01 | 2010-04-27 | Basf Akiengesellschaft | Process for removing methacrylic acid from liquid phase comprising acrylic acid as a main constituent and target product, and methacrylic acid as a secondary component |
US7601866B2 (en) | 2005-03-01 | 2009-10-13 | Basf Aktiengesellschaft | Process for removing methacrolein from liquid phase comprising acrylic acid as a main constituent and target product, and methacrolein as a secondary component |
WO2006109869A1 (en) * | 2005-04-11 | 2006-10-19 | Nippon Shokubai Co., Ltd. | Production method of n-vinyl-2-pyrrolidone |
US7466749B2 (en) | 2005-05-12 | 2008-12-16 | Qualcomm Incorporated | Rate selection with margin sharing |
US8358714B2 (en) | 2005-06-16 | 2013-01-22 | Qualcomm Incorporated | Coding and modulation for multiple data streams in a communication system |
DE602007005288D1 (de) | 2006-01-20 | 2010-04-29 | Nippon Catalytic Chem Ind | Verfahren zur Reinigung von Acrylsäure |
JP2007191449A (ja) | 2006-01-20 | 2007-08-02 | Nippon Shokubai Co Ltd | アクリル酸の製造方法 |
JP5274005B2 (ja) * | 2007-12-25 | 2013-08-28 | 三菱レイヨン株式会社 | 易重合性化合物の晶析方法、および晶析装置 |
JP5112898B2 (ja) * | 2008-02-07 | 2013-01-09 | 三菱レイヨン株式会社 | (メタ)アクリル酸の晶析方法およびその晶析システム |
DE102008040799A1 (de) | 2008-07-28 | 2008-12-11 | Basf Se | Verfahren zur Auftrennung von in einem Produktgasgemisch einer partiellen heterogen katalysierten Gasphasenoxidation einer C3-Vorläuferverbindung der Acrylsäure als Hauptbestandteil enthaltener Acrylsäure und als Nebenprodukt enthaltenem Glyoxal |
MY153094A (en) | 2008-07-28 | 2014-12-31 | Basf Se | Process for separating acrylic acid present as a main constituent and glyoxal present as a by-product in a product gas mixture of a partial heterogeneously catalyzed gas phase oxidation of a c3 precursor compound of acrylic acid |
DE102008041573A1 (de) | 2008-08-26 | 2010-03-04 | Basf Se | Verfahren zur Auftrennung von in einem Produktgasgemisch einer partiellen heterogen katalysierten Gasphasenoxidation einer C3-Vorläuferverbindung der Acrylsäure als Hauptbestandteil enhaltener Acrylsäure und als Nebenprodukt enthaltenem Glyoxal |
WO2010134434A1 (ja) * | 2009-05-19 | 2010-11-25 | 株式会社日本触媒 | (メタ)アクリル酸の製造方法 |
DE102011076931A1 (de) | 2011-06-03 | 2012-12-06 | Basf Se | Wässrige Lösung, enthaltend Acrylsäure und deren konjugierte Base |
PL2928574T3 (pl) * | 2013-01-14 | 2022-02-14 | Sulzer Management Ag | Sposób wieloetapowej krystalizacji i aparat do oczyszczania związku |
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DE2606364B2 (de) | 1976-02-18 | 1981-07-30 | Basf Ag, 6700 Ludwigshafen | Verfahren zur Stofftrennung aus einem flüssigen Gemisch durch fraktionierte Kristallisation |
US4656651A (en) | 1985-09-09 | 1987-04-07 | Itt Corporation | System for providing remote services |
CH667816A5 (de) * | 1985-10-09 | 1988-11-15 | Sulzer Ag | Kristallisationsvorrichtung und deren verwendung. |
US5329021A (en) * | 1993-02-04 | 1994-07-12 | Isp Investments Inc. | Process for the production of pure vinyl pyrrolidone |
TW305830B (ja) | 1993-03-26 | 1997-05-21 | Sulzer Chemtech Ag | |
US5523480A (en) * | 1994-03-28 | 1996-06-04 | Rohm And Haas Company | Process for purifying unsaturated carboxylic acids using distillation and melt crystallization |
DE19501326A1 (de) * | 1995-01-18 | 1996-07-25 | Basf Ag | Verfahren der rektifikativen Abtrennung von (Meth)acrylsäure aus einem (Meth)acrylsäure als Hauptbestandteil und niedere Aldehyde als Nebenbestandteile enthaltenden Gemisch in einer aus Abtriebsteil und Verstärkerteil bestehenden Rektifiaktionskolonne |
DE19627679A1 (de) * | 1996-07-10 | 1998-01-15 | Basf Ag | Verfahren zur Reinigung von Roh-Acrylsäure durch Kristallisation |
DE19740252A1 (de) * | 1997-09-12 | 1999-03-18 | Basf Ag | Verfahren zur Herstellung von Acrylsäure und Methacrylsäure |
DE19904820A1 (de) | 1999-02-05 | 2000-08-10 | Stockhausen Chem Fab Gmbh | Verfahren und Vorrichtung zur Reinigung von Stoffen mittels Kristallisation |
JP2000290220A (ja) * | 1999-04-09 | 2000-10-17 | Mitsubishi Chemicals Corp | アクリル酸の精製方法 |
DE19926082A1 (de) | 1999-06-08 | 2000-12-14 | Basf Ag | Verfahren zur Reinigung und Herstellung von Acrylsäure oder Methacrylsäure |
DE19938841A1 (de) * | 1999-08-17 | 2001-02-22 | Basf Ag | Inhibitorkomposition zur Stabilisierung von radikalisch polymerisierbaren Substanzen |
DE10003498A1 (de) | 2000-01-27 | 2001-08-02 | Basf Ag | Reinigungsverfahren für (Meth)acrylsäure |
DE10003497A1 (de) | 2000-01-27 | 2001-04-12 | Basf Ag | Reinigungsverfahren für (Meth)acrylsäure |
DE10039025A1 (de) | 2000-08-10 | 2002-02-21 | Basf Ag | Verfahren zur Reinigung einer Rohacrylsäureschmelze |
DE10026407A1 (de) | 2000-05-29 | 2001-12-06 | Basf Ag | Verfahren der diskontinuierlichen kristallisativen Reinigung von Roh-Acrylsäure |
DE10122788A1 (de) * | 2001-05-10 | 2002-06-06 | Basf Ag | Verfahren der kristallisativen Reinigung einer Roh-Schmelze wenigstens eines Monomeren |
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2001
- 2001-05-10 DE DE10122788A patent/DE10122788A1/de not_active Withdrawn
-
2002
- 2002-05-02 CN CN02809592.8A patent/CN1234661C/zh not_active Expired - Lifetime
- 2002-05-02 EP EP02735324A patent/EP1387824B1/de not_active Expired - Lifetime
- 2002-05-02 JP JP2002587393A patent/JP4520698B2/ja not_active Expired - Lifetime
- 2002-05-02 US US10/476,187 patent/US7319166B2/en active Active
- 2002-05-02 WO PCT/EP2002/004783 patent/WO2002090310A1/de active IP Right Grant
- 2002-05-02 DE DE50210277T patent/DE50210277D1/de not_active Expired - Lifetime
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2010
- 2010-03-15 JP JP2010056941A patent/JP2010132711A/ja not_active Withdrawn
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2010132711A (ja) * | 2001-05-10 | 2010-06-17 | Basf Se | 少なくとも1種のモノマーの粗製溶融物の結晶化による精製のための方法 |
Also Published As
Publication number | Publication date |
---|---|
CN1234661C (zh) | 2006-01-04 |
EP1387824A1 (de) | 2004-02-11 |
US20040133015A1 (en) | 2004-07-08 |
DE10122788A1 (de) | 2002-06-06 |
EP1387824B1 (de) | 2007-06-06 |
JP2010132711A (ja) | 2010-06-17 |
WO2002090310A1 (de) | 2002-11-14 |
DE50210277D1 (de) | 2007-07-19 |
JP2004528371A (ja) | 2004-09-16 |
CN1518530A (zh) | 2004-08-04 |
US7319166B2 (en) | 2008-01-15 |
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