JP2010132711A - 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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- JP2010132711A JP2010132711A JP2010056941A JP2010056941A JP2010132711A JP 2010132711 A JP2010132711 A JP 2010132711A JP 2010056941 A JP2010056941 A JP 2010056941A JP 2010056941 A JP2010056941 A JP 2010056941A JP 2010132711 A JP2010132711 A JP 2010132711A
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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
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- 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
Abstract
【解決手段】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更に精製する方法において、残留溶融物及び/又は再び溶融されたモノマー結晶に、更なる結晶化工程の少なくとも1つへのその経路で、少なくとも1つの更なる機械的な固/液−分離作業を行う。
【選択図】図1
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 (4)
- 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更に精製する方法において、残留溶融物及び/又は再び溶融されたモノマー結晶に、少なくとも1つの更なる結晶化工程へのその経路で、少なくとも1つの更なる機械的な固/液−分離作業を行う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。
- 少なくとも1種のモノマーが、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、請求項1から3までのいずれか1項記載の方法。
Applications Claiming Priority (1)
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 |
Related Parent Applications (1)
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JP2002587393A Division 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 |
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JP2010132711A true JP2010132711A (ja) | 2010-06-17 |
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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 |
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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 |
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US (1) | US7319166B2 (ja) |
EP (1) | EP1387824B1 (ja) |
JP (2) | JP4520698B2 (ja) |
CN (1) | CN1234661C (ja) |
DE (2) | DE10122788A1 (ja) |
WO (1) | WO2002090310A1 (ja) |
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DE10122788A1 (de) * | 2001-05-10 | 2002-06-06 | Basf Ag | Verfahren der kristallisativen Reinigung einer Roh-Schmelze wenigstens eines Monomeren |
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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WO1999014181A1 (de) * | 1997-09-12 | 1999-03-25 | Basf Aktiengesellschaft | Verfahren zur herstellung von acrylsäure und methacrylsäure |
JP2000290220A (ja) * | 1999-04-09 | 2000-10-17 | Mitsubishi Chemicals Corp | アクリル酸の精製方法 |
JP2000514069A (ja) * | 1996-07-10 | 2000-10-24 | ビーエーエスエフ アクチェンゲゼルシャフト | 結晶化による粗製アクリル酸の精製法 |
JP4520698B2 (ja) * | 2001-05-10 | 2010-08-11 | ビーエーエスエフ ソシエタス・ヨーロピア | 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 |
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2001
- 2001-05-10 DE DE10122788A patent/DE10122788A1/de not_active Withdrawn
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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
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH0748311A (ja) * | 1993-03-26 | 1995-02-21 | Sulzer Chemtech Ag | アクリル酸の精製方法と装置、およびその方法により精製されたアクリル酸 |
JPH07278045A (ja) * | 1994-03-28 | 1995-10-24 | Rohm & Haas Co | メタクリル酸の改良された精製方法 |
JP2000514069A (ja) * | 1996-07-10 | 2000-10-24 | ビーエーエスエフ アクチェンゲゼルシャフト | 結晶化による粗製アクリル酸の精製法 |
WO1999014181A1 (de) * | 1997-09-12 | 1999-03-25 | Basf Aktiengesellschaft | Verfahren zur herstellung von acrylsäure und methacrylsäure |
JP2000290220A (ja) * | 1999-04-09 | 2000-10-17 | Mitsubishi Chemicals Corp | アクリル酸の精製方法 |
JP4520698B2 (ja) * | 2001-05-10 | 2010-08-11 | ビーエーエスエフ ソシエタス・ヨーロピア | 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 |
WO2002090310A1 (de) | 2002-11-14 |
JP4520698B2 (ja) | 2010-08-11 |
DE50210277D1 (de) | 2007-07-19 |
JP2004528371A (ja) | 2004-09-16 |
CN1518530A (zh) | 2004-08-04 |
US7319166B2 (en) | 2008-01-15 |
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