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1.发明授权Process for the production of alkyl (meth)acrylates by direct esterification 失效通过直接酯化生产（甲基）丙烯酸烷基酯的方法
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
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。
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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。
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3.发明授权公开(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
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。
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4.发明授权Process for the purification of acrylic acid obtained by catalytic oxidation of propylene 失效通过丙烯的催化氧化得到的丙烯酸的纯化方法
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
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。
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5.发明授权
公开(公告)号：US5734075A
公开(公告)日：1998-03-31
申请号：US570773
申请日：1995-12-12
IPC分类号： C07C27/00 , C07C27/28 , C07C29/80 , C07C31/02 , C07C51/44 , C07C51/487 , C07C57/04 , C07C57/055 , C07C57/07 , C07C67/08 , C07C67/327 , C07C67/54 , C07C67/60 , C07C69/54 , C07C67/48 , C07C51/42
CPC分类号： C07C51/487 , C07C51/44 , C07C67/327 , C07C67/60
摘要： To recover these noble products consisting of acrylic acid monomer, acrylic ester monomers and alcohols, a thermal cracking is performed in the absence of catalyst on a mixture of heavy distillation residues originating, on the one hand, from the manufacture of acrylic acid and, on the other hand, from the manufacture of the esters, the light fraction originating from the dissociation reactions is continuously vaporized during the cracking operation and this light fraction is distilled in order to recover, after condensation, the required products. The process according to the invention may consist in conducting the cracking of the mixture of heavy residues, optionally preheated, in a reactor (R1); feeding a distillation column (C1) with the light cracking products; recovering the required mixture of light noble products at the head of column (C1); recycling the flow recovered at the foot of column (C1) into the reactor (R1); recovering the heavy residue from the reactor (R1) and sending it to a removal treatment, if appropriate after having diluted it with a part of the flow recovered at the foot of column (C1), the remainder of the said flow being recycled into the reactor (R1). Figure to be published: FIG. 1
摘要翻译： 为了回收由丙烯酸单体，丙烯酸酯单体和醇组成的这些贵重产物，在不存在催化剂的情况下，在重馏分残余物的混合物上进行热裂解，一方面源于丙烯酸的制备， 另一方面，从酯的制造出发，解离反应中的轻馏分在裂解操作期间被连续蒸发，并将该轻馏分蒸馏以在冷凝后回收所需产物。 根据本发明的方法可以包括在反应器（R1）中进行任选预热的重残余物混合物的裂化; 向轻馏分产物中加入蒸馏塔（C1）; 在色谱柱（C1）的头部回收所需的淡色产物混合物; 将在柱（C1）的脚处回收的流回收到反应器（R1）中; 从反应器（R1）中回收重质残余物，并将其送入去除处理（如果适用），将其用塔（C1）底部回收的一部分流体稀释后，将其余的所述流回收到 反应器（R1）。 图将被公布：
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公开(公告)号：US20120190890A1
公开(公告)日：2012-07-26
申请号：US13386096
申请日：2010-06-29
申请人： Michel Fauconet
发明人： Michel Fauconet
IPC分类号： C07C51/16
摘要： An aim of the present invention is to produce, from glycerol, a bioresourced acrylic acid, that is to say an acrylic acid essentially based on a carbon source of natural origin, corresponding to a degree of purity corresponding to the requirements of the users.The process according to the invention comprises a final stage of purification of the acrylic acid by fractional crystallization applied to one of the acrylic acid fractions resulting from the purification line employed after having extracted the acrylic acid, obtained from glycerol, by countercurrentwise absorption with a heavy hydrophobic solvent.
摘要翻译： 本发明的目的是从甘油生产生物相关的丙烯酸，也就是说基本上是以天然来源的碳源为基础的丙烯酸，对应于与使用者的要求相对应的纯度。 根据本发明的方法包括通过分级结晶施加到由从甘油获得的丙烯酸中提取的纯化线之后产生的纯化线之一的丙烯酸馏分的纯化纯化的最后阶段，通过逆向吸收与重质 疏水性溶剂。
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公开(公告)号：US20120178965A1
公开(公告)日：2012-07-12
申请号：US13386186
申请日：2010-06-29
申请人： Michel Fauconet
发明人： Michel Fauconet
摘要： An aim of the present invention is to produce, from glycerol, a bioresourced acrylic acid, that is to say an acrylic acid essentially based on a carbon source of natural origin, meeting all the quality criteria of monomers customarily used as starting material in processes for polymerization of acrylic acid and of its esters, via an economical process. The process according to the invention comprises a final stage of extraction of acrylic acid by fractional crystallization applied to one of the effluents resulting from the acrylic acid purification chain, the location of this final stage possibly depending on the initial feedstock treated, the nature and the source of the glycerol used in the process, purity specifications to be achieved for the final acrylic acid, or finally economic criteria.
摘要翻译： 本发明的目的是从甘油生产生物来源的丙烯酸，也就是说基本上以天然来源的碳源为基础的丙烯酸，满足通常用作起始原料的单体的所有质量标准 通过经济的方法聚合丙烯酸及其酯。 根据本发明的方法包括通过分级结晶萃取丙烯酸的最后阶段，其应用于由丙烯酸纯化链产生的流出物之一，该最终阶段的位置可能取决于所处理的初始原料，性质和 在该过程中使用的甘油的来源，对于最终的丙烯酸要达到的纯度规格，或者最后的经济标准。
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8.发明授权
公开(公告)号：US5659072A
公开(公告)日：1997-08-19
申请号：US491670
申请日：1995-06-19
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。
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公开(公告)号：US07029556B1
公开(公告)日：2006-04-18
申请号：US10130989
申请日：2000-11-15
摘要： The invention concerns a method of purifying a (meth) acrylic monomer selected among (meth) acrylic acids and their esters, by distillation in the presence of at least a polymerisation inhibitor requiring input of oxygen and/or an inhibitor having better efficacy in the presence of oxygen for stabilizing the liquid phase. The invention is characterized in that the distillation is performed in the presence of a NO2 gas, with an oxygen/organic vapor (p/p) ratio ranging between 0.02 and 3%, and with a NO2 condensed organic vapor (p/p) ratio ranging between 0.01 and 50 ppm.
摘要翻译： 本发明涉及一种纯化选自（甲基）丙烯酸及其酯的（甲基）丙烯酸单体的方法，该方法是在需要输入氧的至少一种聚合抑制剂和/或在存在下具有更好功效的抑制剂的存在下蒸馏 的氧气用于稳定液相。 本发明的特征在于，在NO 2气体存在下进行蒸馏，其中氧/有机蒸气（p / p）比在0.02和3％之间， 浓度有机蒸气（p / p）的比例范围为0.01至50ppm。
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公开(公告)号：US5606102A
公开(公告)日：1997-02-25
申请号：US508133
申请日：1995-07-27
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。
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