公开(公告)号：US06281386B1

公开(公告)日：2001-08-28

申请号：US09308756

申请日：1999-05-25

申请人： Michel Fauconet ,  Marc Esch ,  Denis Laurent

发明人： Michel Fauconet ,  Marc Esch ,  Denis Laurent

IPC分类号： C07C5142

CPC分类号： C07C51/48 ,  C07C57/04

摘要： The method consists in extracting acrylic acid by countercurrent filtration washing of reaction gases by at least a hydrophobic absorbing heavy solvent, then recuperating the purified acrylic acid from the solution obtained at the end of this extracting step. As hydrophobic absorbing heavy solvent at least a hydrophobic aromatic compound is used having: a boiling point under atmospheric pressure between 260° C. and 380° C.; a crystallisation temperature less than 35° C. and a viscosity less than 10 mPa·s in a range of temperature between 30-80° C.

摘要翻译： 该方法包括通过至少一种疏水性吸收重溶剂对反应气体进行逆流过滤洗涤，然后从该提取步骤结束时获得的溶液中回收纯化的丙烯酸来萃取丙烯酸。 作为疏水性吸收重溶剂，使用至少一种疏水性芳香族化合物，其具有260℃至380℃之间的大气压下的沸点。 结晶温度低于35℃，粘度在30-80℃之间的温度范围内低于10mPa.s。

公开(公告)号：US5705688A

公开(公告)日：1998-01-06

申请号：US682188

申请日：1996-07-17

申请人： Michel Fauconet ,  Marc Esch ,  Yves Samuel ,  Denis Laurent

发明人： Michel Fauconet ,  Marc Esch ,  Yves Samuel ,  Denis Laurent

IPC分类号： C07C57/05 ,  C07B61/00 ,  C07C51/42 ,  C07C51/48 ,  C07C57/07

CPC分类号： C07C51/48 ,  Y02P20/582

摘要： Acrylic acid obtained by catalytic oxidation of propylene, extracted by countercurrent washing of the reaction gases which at least one hydrophobic heavy solvent in an extraction column (C1) is purified. To this end, a distillation of the stream (5) obtained at the bottom of the column (C1) is conducted in a column (C3) so as to obtain a very pure acrylic acid stream (6) at the top of the column (C3), allowing acrylic acid to pass at the bottom (7); the bottom stream (7) is conveyed as feed into the lower part of a distillation column (C4) from which a stream (9) rich in maleic anhydride and impurities of boiling temperatures situated between that of acrylic acid and that of the heavy solvent is drawn off sideways on a tray situated between the feed and the top of the column; a stream (8) rich in acrylic acid, which is returned as feed to the column (C3) is distilled at the top of the column (C4); and a stream (1) containing heavy solvent and heavy impurities, which is recycled to the top of the column (C1), is recovered at the bottom of the column (C4).

摘要翻译： 通过丙烯的催化氧化获得的丙烯酸，通过逆流洗涤提取塔（C1）中的至少一种疏水性重质溶剂的反应气体进行提纯。 为此，在柱（C1）的底部获得的料流（5）的蒸馏在柱（C3）中进行，以便在塔顶获得非常纯的丙烯酸流（6）（ C3），允许丙烯酸在底部通过（7）; 底部料流（7）作为进料输送到蒸馏塔（C4）的下部，富含马来酸酐的料流（9）和沸点温度位于丙烯酸与重溶剂之间的杂质是 在位于进料塔和塔顶之间的托盘上侧向拉出; 在柱（C4）的顶部蒸馏富含丙烯酸的物流（8），其作为进料（C3）的进料返回。 并且在柱（C4）的底部回收含有重溶剂和重杂质的流（1），其被再循环到塔（C1）的顶部。

公开(公告)号：US06352619B1

公开(公告)日：2002-03-05

申请号：US09254874

申请日：1999-04-14

申请人： Michel Fauconet ,  Francis Augustin ,  Marc Esch

发明人： Michel Fauconet ,  Francis Augustin ,  Marc Esch

IPC分类号： B01D334

CPC分类号： C07C51/487 ,  C07C51/44 ,  C07C51/50 ,  Y10S203/22 ,  C07C57/04

摘要： Process for purifying acrylic acid in order to remove the polymer-type impurities in those places in the distillation columns in which they have a tendency to accumulate, and more particularly a process directed towards removing the polymeric impurities which are formed during a step for removing the aldehyde impurities from acrylic acid, according to which step the medium containing the acrylic acid to be purified is distilled by adding to this medium at least one amino compound of hydrazine type and by flushing away, at the foot of the distillation column, the heavy compounds formed by the said hydrazine-type amino compound(s) with the impurities. According to the invention, the acrylic acid to be purified is also distilled in the presence of at least one compound from the class of nonionic surface agents and of at least one polymerization inhibitor. Polysaccharide ethers and acetates, in particular ethers derived from cellulose or starch, may be mentioned as nonionic surface agents.

摘要翻译： 用于净化丙烯酸的方法，以便去除它们具有积聚趋势的蒸馏塔中的那些位置的聚合物型杂质，更具体地，涉及去除在除去所述聚合物杂质的步骤期间形成的聚合物杂质的方法 根据该步骤，将含有待纯化的丙烯酸的培养基通过向该培养基中加入至少一种肼型氨基化合物并在蒸馏塔的底部冲洗掉重质化合物 由所述肼型氨基化合物与杂质形成。根据本发明，待纯化的丙烯酸还在至少一种来自非离子表面活性剂的化合物和至少一种 聚合抑制剂。 多糖醚和乙酸酯，特别是衍生自纤维素或淀粉的醚，可以被称为非离子表面活性剂。

公开(公告)号：US5510514A

公开(公告)日：1996-04-23

申请号：US187282

申请日：1994-01-27

申请人： Michel Fauconet ,  Norbert Richard ,  Marc Esch ,  Nadine Colin

发明人： Michel Fauconet ,  Norbert Richard ,  Marc Esch ,  Nadine Colin

IPC分类号： C07B61/00 ,  C07C67/08 ,  C07C67/58 ,  C07C69/54 ,  C07C67/48

CPC分类号： C07C67/08

摘要： An alkyl (meth)acrylate is prepared by a direct esterification (in 1) of (meth)acrylic acid by the corresponding alcohol, catalysed by H.sub.2 SO.sub.4. To the crude reaction mixture (C.sub.1) comprising the desired ester, alcohol, (meth)acrylic acid, alkyl hydrogen sulphate and traces of H.sub.2 SO.sub.4, there is added (in 3) a base to neutralize the acidic species, the resulting salts passing into the aqueous phase (A.sub.1), which is separated from the organic phase (O.sub.1) containing the desired ester. The light products (L.sub.1) containing the alcohol are recovered (in 4) from the aqueous phase, and the waste waters (W.sub.2) are expelled. A hydrolysis is carried out (in 8) of the alkyl hydrogen sulphate present in the aqueous phase (A.sub.1) obtained after the separation which is carried out after neutralization (in 3), to form the alcohol and H.sub.2 SO.sub.4 in this phase, the acidic species resulting from the hydrolysis are neutralized by introduction of a base .into the medium, and the resulting aqueous phase (A.sub.3) is directed to the step for recovery of the alcohol. Pollution of the waters (W.sub.2), attributable to the alkyl hydrogen sulphate, is thus avoided.

摘要翻译： （甲基）丙烯酸烷基酯由（甲基）丙烯酸通过相应的醇直接酯化（在1）中，由H 2 SO 4催化。 向包含所需酯，醇，（甲基）丙烯酸，烷基硫酸氢盐和痕量H 2 SO 4的粗反应混合物（C1）中加入（3）碱以中和酸性物质，所得盐进入 水相（A1），其与含有所需酯的有机相（O1）分离。 从水相中回收含有醇的轻质产物（L1）（4），废水（W2）被排出。 在分离后得到的水相（A1）中存在的烷基硫酸氢盐（在3中）进行水解（在8中），在该相中形成醇和H 2 SO 4，酸性物质 通过在介质中引入碱来中和水解产生的水相，并且将所得水相（A3）引导至用于回收醇的步骤。 因此避免了归因于烷基硫酸氢盐的水（W2）的污染。

公开(公告)号：US5883261A

公开(公告)日：1999-03-16

申请号：US931284

申请日：1997-09-16

申请人： Marc Esch ,  Alain Riondel

发明人： Marc Esch ,  Alain Riondel

IPC分类号： C07D233/34 ,  B01J31/02 ,  C07B61/00 ,  C07D233/30 ,  C07D233/32 ,  C07D239/10 ,  C07D243/04 ,  C07D233/14

CPC分类号： C07D233/32

摘要： Process for the manufacture of a compound of formula (I) by reaction of at least one (meth)acrylate of formula (II) with a heterocyclic alcohol of formula (III) in the presence of sodium methoxide as catalyst, characterized in that the sodium methoxide is gradually introduced, as a solution, throughout the synthesis: ##STR1## R.sup.1 =hydrogen or methyl; A and B each independently represent a straight or branched hydrocarbon chain having from 2 to 5 carbon atoms; R.sup.2 =C.sub.1 -C.sub.4 alkyl group.

摘要翻译： 通过至少一种式（II）的（甲基）丙烯酸酯与式（III）的杂环醇在甲醇钠作为催化剂的存在下反应制备式（I）化合物的方法，其特征在于钠 在整个合成过程中逐渐引入甲醇钠作为溶液。图像（I）图像（II）各自独立地表示具有2至5个碳原子的直链或支链烃链; R2 = C1-C4烷基。

公开(公告)号：US06743938B1

公开(公告)日：2004-06-01

申请号：US10049463

申请日：2002-08-02

申请人： Jean-Francois Croizy ,  Marc Esch ,  Gilbert Esquirol

发明人： Jean-Francois Croizy ,  Marc Esch ,  Gilbert Esquirol

IPC分类号： C07C25308

CPC分类号： C07C253/00 ,  C07C255/12

摘要： This process for the production of the methyl ethyl ketone cyanohydrin of formula (I) is characterized by the fact that hydrocyanic acid and methyl ethyl ketone are reacted in the presence of diethylamine as a catalyst.

摘要翻译： 用于制备式（I）的甲基乙基酮氰醇的该方法的特征在于氢化氰酸和甲基乙基酮在二乙胺作为催化剂存在下反应。

公开(公告)号：US06521782B1

公开(公告)日：2003-02-18

申请号：US09889727

申请日：2001-09-27

申请人： Alain Riondel ,  Gilles Herbst ,  Marc Esch ,  Eric Delaunay ,  Peter Meyer

发明人： Alain Riondel ,  Gilles Herbst ,  Marc Esch ,  Eric Delaunay ,  Peter Meyer

IPC分类号： C07C6952

CPC分类号： C07C213/08 ,  C07C219/08

摘要： The present invention relates to a process for the manufacture of aqueous solutions of unsaturated quaternary ammonium salts. The salts can correspond to the following formula (I): in which R represents a methyl or benzyl radical, by reaction, in the presence of water, of N,N-dimethyl-amninoethyl acrylate (DAMEA) with a quaternizing agent of formula (II): R—Cl  (II) in which R is as defined above. Generally, the reaction is carried out in a closed reactor, which includes all the DAMEA and has been pressurized by air or depleted air to 0.5 to 3 bar, by continuously introducing, at a temperature of 35 to 65° C., the quatenlizing agent (II) and the water, until a concentration of salt (I) in the water is obtained. The water starts to be introduced beginning when 0-20% of the amount by weight of the quaternizing agent (II) necessary for the reaction has been added and it being possible for the pressure at the end of the reaction to reach 9 bar. Next, the reactor can be depressurized while keeping the oxygen content constant by simultaneous introduction of air and, after returning to atmospheric pressure, the residual quaternizing agent may be removed.

摘要翻译： 本发明涉及一种制备不饱和季铵盐水溶液的方法。 盐可以对应于下式（I）：其中R表示甲基或苄基，通过在水存在下，将N，N-二甲基 - 氨基甲基乙基丙烯酸酯（DAMEA）与式（I）的季铵化剂反应 II）：其中R如上所定义。 通常，反应在封闭的反应器中进行，该反应器包括所有的DAMEA，并通过空气或贫化空气将其加压至0.5-3巴，通过在35至65℃的温度下连续引入季戊酸化剂 （II）和水，直到获得水中的盐（I）浓度。 当加入反应所需的季铵化剂（II）的重量的0-20％时，开始引入水，反应结束时的压力可能达到9巴。 接下来，可以通过同时引入空气同时保持氧含量恒定来减压反应器，并且在返回到大气压之后，可以除去残留的季铵化剂。

公开(公告)号：US5498723A

公开(公告)日：1996-03-12

申请号：US329964

申请日：1994-10-27

申请人： Alain Riondel ,  Gilles Herbst ,  Marc Esch

发明人： Alain Riondel ,  Gilles Herbst ,  Marc Esch

IPC分类号： C07D243/04 ,  B01J31/02 ,  C07B61/00 ,  C07D233/04 ,  C07D233/32 ,  C07D239/06 ,  C07D239/10 ,  C07D245/02 ,  C07D233/70

CPC分类号： C07D233/32

摘要： A compound (I) is prepared by reacting at least one (meth)acrylate (II) with a heterocyclic alcohol (III), in the presence of at least one catalyst chosen from magnesium alkoxides Mg(OR).sub.2. ##STR1## R=C.sub.1 -C.sub.4 alkyl. R.sup.1 =H, CH.sub.3 ; A, B=straight or branched C.sub.2 -C.sub.5 hydrocarbon chain; R.sup.2 =C.sub.1 -C.sub.4 alkyl.

摘要翻译： 在至少一种选自烷醇镁（OR）2的催化剂的存在下，使至少一种（甲基）丙烯酸酯（II）与杂环醇（III）反应制备化合物（I）。 （Ⅰ）图像（II）图像（III）R = C1-C4烷基。 R1 = H，CH3; A，B =直链或支链C 2 -C 5烃链; R2 = C1-C4烷基。

公开(公告)号：US06673884B2

公开(公告)日：2004-01-06

申请号：US09959622

申请日：2002-08-28

申请人： Alain Riondel ,  Denis Tembou N'Zudie ,  Marc Esch ,  Vladimir Chaplinski ,  Didier Vanhoye

发明人： Alain Riondel ,  Denis Tembou N'Zudie ,  Marc Esch ,  Vladimir Chaplinski ,  Didier Vanhoye

IPC分类号： C08F12600

CPC分类号： C07C213/08 ,  C07C219/08

摘要： To prepare compound (I), a quaternising agent R3—X⊖ is introduced into a solution, in an organic solvent or a mixture of organic solvents, of a compound of formula (III), at a temperature of 35 to 80° C., and the reaction is then allowed to continue at said temperature until compound (III) has disappeared completely or substantially completely, after which water is added and then an aqueous solution of compound (I) is separated and the water removed as necessary. R1=H or —CH3; R2=one of —CH3, —C2H5, —C3H7 and —C4H9; the two R3 are the same or different and each represents one of —CH3, —C2H5, —C3H7, —C4H9 and —CH2C6H5; and the two X⊖ are the same or different and each represents Cl⊖ or Br⊖.

摘要翻译： 为了制备化合物（I），在35℃的温度下将季铵化物R 3 -X'引入式（III）化合物的有机溶剂或有机溶剂的混合物的溶液中 至80℃，然后使所述反应在所述温度下继续，直到化合物（III）完全或基本上完全消失，然后加入水，然后分离出化合物（I）的水溶液，并除去水 R 1 = H或-CH 3; R 2 = -CH 3，-C 2 H 5，-C 3 H 7和-C 4 H 9之一; 两个R 3相同或不同，各自表示-CH 3，-C 2 H 5，-C 3 H 7，-C 4 H 9和-CH 2 C 6 H 5中的一个; 两个X <⊖>相同或不同，分别表示Cl <⊖>或Br <⊖>。

公开(公告)号：US07151190B1

公开(公告)日：2006-12-19

申请号：US09889699

申请日：2000-01-20

申请人： Alain Riondel ,  Gilles Herbst ,  Marc Esch

发明人： Alain Riondel ,  Gilles Herbst ,  Marc Esch

IPC分类号： C07C69/533

CPC分类号： C07C213/08 ,  C07C219/08

摘要： The invention concerns a method for making aqueous solutions of unsaturated quaternary ammonium salts of formula (I) by reacting, in the presence of water, N,N-dimethylaminoethyl acrylate with a quaternizing agent of formula (II): R—Cl, said method is characterized in that it consists in: (a) in a closed reactor containing 5 60 wt. % of N,N-dimethylaminoethyl acrylate required for the reaction and which has been pressurized with air or depleted air at 0.5 to 3 bars, carrying out the reaction by continuously introducing, at a temperature ranging between 35 to 65° C., the quaternizing agent (II), and water, and finally the remaining N,N-dimethylaminoethyl acrylate, until the desired concentration of salt (I) in the water is reached, the water being introduced only when 0–20 wt. % of the amount required for the quaternizing agent (II) reaction has been added; the introduction of the remaining N,N-dimethylaminoethyl acrylate starting only when 20–80 wt. % required for the quaternizing agent (II) reaction has been added; and the pressure at the end of the reaction capable of reaching 9 bars; then (b) in depressurizing while maintaining the oxygen content constant by simultaneous introduction of air and, after returning to atmospheric pressure, eliminating the residual quaternizing agent. In formule (I) and (II). R=methyl or benzyl.

摘要翻译： 本发明涉及一种制备式（I）的不饱和季铵盐的水溶液的方法，该方法是在水，N，N-二甲基氨基乙基丙烯酸酯与式（II）的季铵化剂：R-Cl的存在下反应，所述方法 其特征在于它包括：（a）在含有60重量％ 反应中所需的N，N-二甲基氨基乙基丙烯酸酯的百分比，并且已经用空气或贫的空气在0.5至3巴加压，通过在35至65℃的温度范围内连续引入季铵化 （II）和水，最后是剩余的N，N-二甲基氨基乙基丙烯酸酯，直到达到所需浓度的盐（I），仅在0-20wt。 添加季铵化剂（II）反应所需量的％; 引入剩余的N，N-二甲基氨基乙基丙烯酸酯仅在20-80wt。 加入季铵化剂（II）反应所需的％; 反应结束时的压力可以达到9巴; 然后（b）在同时引入空气的同时保持氧含量恒定的同时减压，并且在返回到大气压力之后，消除残留的季铵化剂。 在式（I）和（II）中。 R =甲基或苄基。