公开(公告)号：US5606102A

公开(公告)日：1997-02-25

申请号：US508133

申请日：1995-07-27

申请人： Michel Fauconet ,  Christian Lacroix ,  Nathalie Hess ,  Jacqueline Bessalem

发明人： Michel Fauconet ,  Christian Lacroix ,  Nathalie Hess ,  Jacqueline Bessalem

IPC分类号： B01J27/053 ,  C07C67/08 ,  C07C67/48 ,  C07C69/54 ,  C07C69/52

CPC分类号： C07C67/08

摘要： In this esterification, catalysed by H.sub.2 SO.sub.4, the crude reaction mixture comprising ester, butanol, acrylic acid, BuSO.sub.4 H and traces of H.sub.2 SO.sub.4 is obtained; BuSO.sub.4 H is hydrolysed (in R2) to H.sub.2 SO.sub.4 using pure water or water generated during the reaction; after hydrolysis, the medium is separated by settling (in D2) into an organic phase containing ester, butanol and part of the unconverted acid; and an aqueous phase containing H.sub.2 SO.sub.4 and the remainder of the unconverted acid; the organic phase is washed under alkaline conditions in order to neutralize the acrylic acid to alkaline acrylate which is soluble in the aqueous phase and then the neutralized organic phase is washed with water; the acid present in alkaline salt form in the aqueous phase from the 1st basic neutralization is regenerated by addition of the acidic aqueous phase (8) resulting from the separation by settling (in D2) of the hydrolysis stage; the acid (10) thus regenerated in this aqueous phase is extracted (in C5) by a solvent chosen from butanol, butyl acrylate or a mixture of butyl acrylate and butanol; the organic phase (13) obtained at the head of the extraction column (C5), containing mainly acid and butanol or ester, or a mixture of butanol and ester, is recycled to the esterification reactor (R1); the aqueous phase (15) recovered at the foot of the column (C5) is conveyed as feed to a distillation column (C6) for recovering butanol (16) at the head, for the purpose of recycling it upstream and of discarding the spent aqueous liquors, which are virtually free from organic pollution.

摘要翻译： 在该酯化反应中，由H 2 SO 4催化，得到包含酯，丁醇，丙烯酸，BuSO 4 H和痕量H 2 SO 4的粗反应混合物; 使用在反应过程中产生的纯水或水将BuSO 4 H（在R2中）水解成H 2 SO 4; 水解后，通过沉淀（在D2中）将介质分离成含有酯的酯，丁醇和部分未转化的酸; 和含有H 2 SO 4的水相和未转化的酸的其余部分; 有机相在碱性条件下洗涤，以将丙烯酸中和到可溶于水相的碱性丙烯酸酯，然后中和的有机相用水洗涤; 在第一碱性中和的水相中以碱式盐形式存在的酸通过加入通过水解阶段的沉降（在D2中）分离产生的酸性水相（8）而再生; 在该水相中再生的酸（10）通过选自丁醇，丙烯酸丁酯或丙烯酸丁酯和丁醇的混合物的溶剂萃取（在C5中） 在主要含有酸和丁醇或酯的萃取塔（C5）的头部或丁醇和酯的混合物中获得的有机相（13）被再循环到酯化反应器（R1）中; 在柱（C5）的底部回收的水相（15）作为进料输送到用于在头部回收丁醇（16）的蒸馏塔（C6），以将其上游再循环并丢弃废水 几乎没有有机污染的酒。

公开(公告)号：US4745214A

公开(公告)日：1988-05-17

申请号：US876602

申请日：1986-06-20

申请人： Raymond Hess ,  Christian Lacroix

发明人： Raymond Hess ,  Christian Lacroix

IPC分类号： C07C219/08 ,  C07C67/00 ,  C07C69/52 ,  C07C213/00 ,  C07C213/02 ,  C07C231/00 ,  C07C231/12 ,  C07C233/38

CPC分类号： C07C219/08 ,  C07C213/08

摘要： For the preparation of an aqueous solution of unsaturated quaternary ammonium salts of the formula (I):H.sub.2 C.dbd.C--(R.sub.3)C(O)--A--R.sub.4 --N.sup..sym. (R.sub.1)(R.sub.2)(R).X.sup..crclbar.,e.g., methacryloyloxyethyltrimethylammonium chloridethe steps of:(a) reacting a (meth)acrylic monomer, e.g., dimethylaminoethyl methacrylate in a closed reactor, in the presence of a polymerization inhibitor, e.g., 3,5-ditert-butyl-4-hydroxytoluene, with 5 to 20% of the weight quantity of quaternizing agent, e.g., methylchloride, required for the reaction, wherein the latter agent is introduced into the reactor continuously,(b) adding water and the remainder of the quaternizing agent continuously until the required concentration of quaternary ammonium salt in water is obtained,(c) maintaining the temperature at a value of between 30.degree. and 60.degree. C. during the stages (a) and (b), and(d) maintaining a stream of gas containing oxygen in the reaction mixture during the stages (a) and (b) and especially as the end of the reaction approaches, such that the volume ratio of gas at the reactor outlet to the oxygen introduced at the inlet of this same reactor is less than 100/l.

摘要翻译： 制备式（I）的不饱和季铵盐水溶液：H2C = C-（R3）C（O）-A-R4-N（+）（R1）（R2）（R） （ - ），例如甲基丙烯酰氧基乙基三甲基氯化铵，步骤：（a）在封闭反应器中，使（甲基）丙烯酸单体例如甲基丙烯酸二甲基氨基乙酯在聚合抑制剂例如3,5-二叔丁基 - 4-羟基甲苯，其中5至20重量％的季铵化剂，例如反应所需的甲基氯，其中将后一种试剂连续引入反应器，（b）连续加入水和其余季铵化剂 直到获得所需浓度的季铵盐，（c）在阶段（a）和（b）期间将温度保持在30℃至60℃之间，和（d）保持在 在步骤（a）和（b）期间，特别是当反应结束时，反应混合物中含氧的气体接近 ，使得反应器出口处的气体与在该相同反应器的入口处引入的氧气的体积比小于100 / l。

公开(公告)号：US5260480A

公开(公告)日：1993-11-09

申请号：US883930

申请日：1992-05-14

申请人： Christian Lacroix ,  Raymond Hess

发明人： Christian Lacroix ,  Raymond Hess

IPC分类号： C07C219/08 ,  C07C233/38 ,  C07C69/52

CPC分类号： C07C219/08 ,  C07C213/08 ,  C07C233/38

摘要： A process for the preparation of aqueous solutions of unsaturated quaternary ammonium salts corresponding to the following formula:H.sub.2 C=C(R.sub.3)--C(O)--A--R.sub.4 --N.sup.+ (R.sub.1)(R.sub.2)(R)X.sup.-

摘要翻译： PCT No.PCT / FR89 / 00036 Sec。 371 1990年9月7日第 102（e）1990年9月7日PCT PCT 1989年2月2日PCT公布。 出版物WO89 / 07588 日本：1989年8月24日。一种制备对应于下式的不饱和季铵盐水溶液的方法：H2C = C（R3）-C（O）-A-R4-N +（R1）（R2）（ R）X-

公开(公告)号：US5207874A

公开(公告)日：1993-05-04

申请号：US717289

申请日：1991-06-20

申请人： Raymond Hess ,  Christian Lacroix

发明人： Raymond Hess ,  Christian Lacroix

IPC分类号： C07D301/30 ,  B01D3/36 ,  C07D301/32 ,  C07D303/16

CPC分类号： B01D3/36 ,  C07D303/16 ,  Y10S203/13 ,  Y10S203/22

摘要： The purification by distillation of glycidyl (meth)acrylate containing light products containing epichlorohydrin and light impurities, and heavy impurities comprises: in a first stage, a distillation of the glycidyl (meth)acrylate to be purified is conducted in the presence of a first solvent, e.g., water, capable of forming a low boiling point heteroazeotrope with the light impurities and epichlorohydrin, so as to obtain a head fraction which consists essentially of a solvent-light products heteroazeotrope; and, in a second stage, the glycidyl (meth)acrylate thus freed from the light products is subjected to a distillation in the presence of a second solvent, e.g., water, capable of forming a low boiling point azeotrope with glycidyl (meth)acrylate, so as to obtain a head fraction consisting essentially of the second solvent and the required pure glycidyl (meth)acrylate, thus freed from the heavy impurities, the said solvents being present, during these two distillations, throughout the distillation zone, including the boiler.

摘要翻译： 通过蒸馏含有含有表氯醇和轻杂质的轻质产物的缩水甘油酯（轻质杂质）和重杂质的纯化包括：在第一阶段中，待纯化的（甲基）丙烯酸缩水甘油酯的蒸馏在第一溶剂存在下进行 例如水，能够与轻杂质和表氯醇形成低沸点杂合物，以获得基本上由溶剂光产物杂化物组成的头部分; 并且在第二阶段中，使得与轻质产物相脱离的（甲基）丙烯酸缩水甘油酯在与（甲基）丙烯酸缩水甘油酯形成低沸点共沸物的第二溶剂例如水的存在下进行蒸馏 ，从而获得主要由第二溶剂和所需的纯的（甲基）丙烯酸缩水甘油酯组成的头部馏分，因此在这两个蒸馏过程中，所有溶剂都存在于整个蒸馏区域，包括锅炉 。

公开(公告)号：US5659072A

公开(公告)日：1997-08-19

申请号：US491670

申请日：1995-06-19

申请人： Jacqueline Bessalem ,  Michel Fauconet ,  Christian Lacroix ,  Nathalie Hess

发明人： Jacqueline Bessalem ,  Michel Fauconet ,  Christian Lacroix ,  Nathalie Hess

IPC分类号： B01J27/02 ,  C07B61/00 ,  C07C67/08 ,  C07C67/54 ,  C07C67/58 ,  C07C67/62 ,  C07C69/54 ,  C07C67/48

CPC分类号： C07C67/08

摘要： An acrylic acid ester is manufactured by reaction of the said acid and an alcohol chosen from C.sub.5 or above primary and secondary aliphatic monoalcohols, in the presence of an acid as esterification catalyst and of a polymerization inhibitor, the alcohol being capable of forming a heteroazeotrope with water, the water formed by the esterification reaction being entrained by distillation in a column in the form of a heteroazeotropic mixture with the alcohol, which mixture, containing an amount of unreacted acrylic acid, is then subjected, after condensation, to a separation in order to give an upper organic phase which is recycled to the head of the distillation column and a lower aqueous phase which is withdrawn; according to the invention, an extraction (for example in an extraction column EC) of the acrylic acid contained in the condensed heteroazeotropic mixture (M) intended for phase separation with an esterifying-alcohol-rich mixture, and the acrylic acid thus extracted is returned to the head of the distillation column (DC), as a constituent of the recycled organic phase, with an increase in the level of reflux into the distillation column (DC) relative to the natural reflux.

摘要翻译： 在酸作为酯化催化剂和聚合抑制剂的存在下，所述酸和选自C5或以上的伯和仲脂族一元醇的醇反应制备丙烯酸酯，该醇能够形成具有 水中，通过酯化反应形成的水通过与醇的混合物形式的柱蒸馏而夹带，该混合物含有一定量的未反应的丙烯酸，然后在冷凝后按顺序分离 以产生再循环到蒸馏塔头部的上部有机相和取出的下部水相; 根据本发明，返回用于与富含酯化醇的混合物相分离的冷凝杂合混合物（M）中所含的丙烯酸和由此提取的丙烯酸的萃取（例如萃取塔EC） 作为回收有机相的组分，蒸馏塔（DC）的头部相对于天然回流的回流进入蒸馏塔（DC）的水平增加。