公开(公告)号：US5380929A

公开(公告)日：1995-01-10

申请号：US236669

申请日：1994-05-02

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Erhard Jagers ,  Georg Kohl

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Erhard Jagers ,  Georg Kohl

IPC: B01J31/20 ,  C07B61/00 ,  C07C51/12 ,  C07C51/56 ,  C07C53/08 ,  C07C53/12

CPC classification number: C07C51/12 ,  C07C51/56

Abstract: To prepare acetic acid and acetic anhydride, methanol and methyl acetate are reacted under anhydrous conditions with carbon monoxide in the presence of a catalyst system containing carbonyl complexes of group VIII noble metals, methyl iodide, an alkali metal acetate or iodide, or quaternary organophosphonium or organoammonium acetate or iodide, The hot carbonylation mixture is decompressed, the evaporated components are fed to a first distillation zone, and the catalyst solution which remains is fed back to the reaction zone. In the first distillation zone, the volatile carbonylation products are subjected to fractional distillation; the low-boiling methyl iodide and methyl acetate pass back into the reaction zone, and the bottom product produced is a mixture of acetic acid and acetic anhydride, which is split into the pure components in a second distillation zone and a third distillation zone.

Abstract translation: 为了制备乙酸和乙酸酐，在无水条件下，甲醇和乙酸甲酯在含有VIII族贵金属，甲基碘，碱金属乙酸酯或碘化物的羰基络合物或季有机鏻的催化剂体系存在下与一氧化碳反应，或 乙酸有机铵或碘化物。将热羰基化混合物减压，将蒸发的组分进料至第一蒸馏区，将剩余的催化剂溶液反馈回反应区。 在第一蒸馏区中，将挥发性羰基化产物进行分馏; 低沸点甲基碘和乙酸甲酯回到反应区，产生的底部产物是乙酸和乙酸酐的混合物，其在第二蒸馏区和第三蒸馏区被分成纯组分。

公开(公告)号：US4717454A

公开(公告)日：1988-01-05

申请号：US774384

申请日：1985-09-10

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Peter Horstermann ,  Georg Kohl

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Peter Horstermann ,  Georg Kohl

IPC: C07C69/34 ,  B01J31/00 ,  C07C45/00 ,  C07C45/82 ,  C07C45/85 ,  C07C49/08 ,  C07C51/00 ,  C07C51/573 ,  C07C53/12 ,  C07C67/00 ,  B01D5/00

CPC classification number: C07C51/573 ,  C07C45/82 ,  C07C45/85 ,  C07C67/36 ,  C07C67/37 ,  C07C67/60 ,  Y10S203/06

Abstract: A process for removing by product acetone from reaction mixtures obtained by reacting methyl acetate and/or dimethylether with carbon monoxide at elevated temperatures to obtain acetic anhydride in the presence of a catalyst system consisting essentially of carbonyl complexes of noble metals belonging to group VIII of the Periodic System of the elements, acetic acid, an organophosphorus or organonitrogen compound, and methyl iodide whereby the acetone obtained as a by-product during the reaction is subjected to condensation at temperatures of 50.degree. to 250.degree. C., under pressures of 0.01 to 150 bars and at a molar ratio as above defined for the catalyst system constituent of 1:(25-500):(10-100):(15-150) so as to obtain predominantly higher-boiling secondary products to be distillatively separated in a successive distillation zone together with volatile constituents of the catalyst system.

Abstract translation: 通过产物丙酮从反应混合物中除去反应混合物的方法，该反应混合物通过在高温下使乙酸甲酯和/或二甲醚与一氧化碳反应而获得，以在催化剂体系存在下获得乙酸酐，所述催化剂体系主要由以下组分的贵金属的羰基络合物组成： 元素的定期系统，乙酸，有机磷或有机氮化合物和甲基碘，由此在反应过程中作为副产物获得的丙酮在温度为50至250℃，压力为0.01至 150巴，摩尔比如上述对于催化剂体系成分1：（25-500）：（10-100）：（15-150）所定义的摩尔比，从而获得主要是较高沸点的次要产物，以蒸馏分离 连续的蒸馏区和催化剂体系的挥发性成分。

公开(公告)号：US4560518A

公开(公告)日：1985-12-24

申请号：US554593

申请日：1983-11-23

Applicant: Klaus Gehrmann ,  Alexander Ohorodnik ,  Johannes Rosenthal

Inventor： Klaus Gehrmann ,  Alexander Ohorodnik ,  Johannes Rosenthal

IPC: C07F9/32

CPC classification number: C07F9/3211

Abstract: The disclosure relates to a process for the continuous production of 2-carboxyethyl-alkyl-phosphinic acid dialkylesters by reacting an alkanephosphonous acid monoalkylester with an acrylic acid ester in the presence of a metal alcoholate. To this end, the disclosure provides:(a) for a quantity by volume (corresponding to the reactor volume) of 2-carboxyethyl-alkyl-phosphinic acid dialkylester which is to be produced, to be introduced into a reactor adapted to circulate reaction mixture therein, closed in itself and provided with cooling means and an overflow, and circulated in the reactor;(b) for the alkanephosphonous acid monoalkylester, acrylic acid alkylester and an alcoholic solution of the metal alcoholate to be continuously introduced into the reactor while cooling the material circulated therein, and for the whole to be reacted at a temperature of about 0.degree. to 80.degree. C.; and(c) for a mixture containing final product to be continuously removed through the overflow of the reactor and for 2-carboxyethyl-alkyl-phosphinic acid dialkylester to be distillatively separated from the mixture.

Abstract translation: 本公开涉及通过在金属醇化物的存在下使烷基膦酸单烷基酯与丙烯酸酯反应连续制备2-羧乙基 - 烷基 - 次膦酸二烷基酯的方法。 为此，本公开内容提供：（a）待生产的2-羧乙基 - 烷基 - 次膦酸二烷基酯的体积（相当于反应器体积）的量，引入适于使反应混合物循环的反应器 其中本身封闭并设置有冷却装置和溢流器，并在反应器中循环; （b）将烷基亚磺酸单烷基酯，丙烯酸烷基酯和金属醇化物的醇溶液连续引入反应器中同时冷却其中循环的材料，并且整体在约0℃至80℃的温度下反应 DEG; 和（c）含有通过反应器溢流连续除去的最终产物和从该混合物蒸馏出的2-羧基乙基 - 烷基 - 次膦酸二烷基酯的混合物。

公开(公告)号：US4549937A

公开(公告)日：1985-10-29

申请号：US442107

申请日：1982-11-16

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Peter Horstermann ,  Hans-Klaus Kubbeler ,  Georg Kohl

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Peter Horstermann ,  Hans-Klaus Kubbeler ,  Georg Kohl

IPC: C07C69/34 ,  B01J31/00 ,  C07C51/00 ,  C07C51/573 ,  C07C53/12 ,  C07C67/00 ,  C07C67/54 ,  C07C69/16 ,  B01D3/06 ,  C07C51/56

CPC classification number: C07C51/573 ,  C07C67/54

Abstract: The disclosure relates to a process for separating the catalyst system from reaction mixtures which are obtained by reacting methyl acetate and/or dimethylether with carbon monoxide and optionally hydrogen at elevated temperatures to acetic anhydride and optionally ethylidene diacetate in the presence of a catalyst system consisting of carbonyl complexes of noble metals belonging to group VIII of the Periodic System, acetic acid, an organophosphorus or organonitrogen compound, methyl iodide and optionally compounds of carbonyl-yielding common metals, and which issue from the reaction zone under a pressure of 25 to 150 bars at a temperature of 100.degree. to 250.degree. C. More particularly, the reaction mixture coming from the reaction zone is introduced into a separator heated to 60.degree. to 140.degree. C. and released to a pressure of 0.5 to 3.5 bars with spontaneous evaporation of the bulk of volatile constituents; the stream of liquid matter coming from the separator is delivered to a distilling zone and the bulk of still volatile constituents is distilled off therein under a pressure of 0.05 to 1 bar at a base temperature of 70.degree. to 170.degree. C.; and catalyst solution retained as base product is recycled to the reaction zone.

Abstract translation: 本公开涉及一种从反应混合物中分离催化剂体系的方法，其通过使乙酸甲酯和/或二甲醚与一氧化碳和任选的氢气在高温下反应而获得，所述方法是在催化剂体系存在下在高温下在乙酸酐和任选的亚乙基二乙酸酯 属于周期系第VIII族的贵金属的羰基络合物，乙酸，有机磷或有机氮化合物，甲基碘和任选的产生羰基的常见金属的化合物，并且在25至150巴的压力下从反应区发出 更优选地，将来自反应区的反应混合物引入加热至60℃至140℃的隔膜中，并释放至0.5至3.5巴的压力，并自发蒸发 大部分挥发性成分; 来自分离器的液体物流被输送到蒸馏区，并且在基本温度为70至170℃的压力下，在0.05至1巴的压力下蒸馏出大部分挥发性挥发性成分。 将作为基础产物保留的催化剂溶液再循环至反应区。

公开(公告)号：US4444624A

公开(公告)日：1984-04-24

申请号：US412225

申请日：1982-08-27

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Winfried Lork ,  Peter Prinz

IPC: C07C45/00 ,  C07C45/49 ,  C07C45/78 ,  C07C45/82 ,  C07C45/83 ,  C07C49/08 ,  C07C67/00 ,  B01D3/40

CPC classification number: C07C45/82 ,  C07C45/49 ,  C07C45/83

Abstract: The disclosure relates to a process for separating acetone from reaction mixtures originating from the reaction of methyl acetate and/or dimethylether with carbon monoxide and optionally hydrogen in the presence of a catalyst system consisting of carbonyl complexes of noble metals of group VIII of the Periodic System of the elements, acetic acid, an organophosphorus or organonitrogen compound, methyl iodide and optionally carbonyl-yielding compounds of common metals. To this end, the disclosure provides for the reaction mixture containing acetic anhydride, acetic acid, ethylidene diacetate, methyl iodide, acetone and methyl acetate which is distilled off from the catalyst solution, or just its low boiler fraction consisting of methyl acetate, methyl iodide and acetone to be subjected wholly or partially to an extractive distillation with acetic acid and for pure methyl iodide to be distilled off; for an acetone/methyl acetate mixture to be distilled off from the acetic acid extract; for this mixture to be separated in known fashion and for the acetic acid extractant to be recycled into the extraction stage, if desired after separation of the final reaction products comprised of acetic anhydride; ethylidene diacetate and acetic acid.

Abstract translation: 本公开内容涉及在由周期性系统VIII族的贵金属的羰基络合物组成的催化剂体系的存在下，从丙酸甲酯和/或二甲醚与一氧化碳和任选的氢气反应的反应混合物中分离丙酮的方法 的元素，乙酸，有机磷或有机氮化合物，甲基碘和任选的产生羰基的常见金属化合物。 为此，本公开内容提供了从催化剂溶液中蒸馏掉的乙酸酐，乙酸，亚乙基二乙酸酯，甲基碘，丙酮和乙酸甲酯的反应混合物，或仅仅是其由乙酸甲酯，甲基碘 和丙酮完全或部分地进行与乙酸的萃取蒸馏，并将纯甲基碘蒸馏出; 对于从乙酸提取物中蒸出的丙酮/乙酸甲酯混合物; 为了将该混合物以已知方式分离，并且乙酸萃取剂再循环到萃取阶段，如果需要，在分离由乙酸酐组成的最终反应产物之后; 亚乙基二乙酸酯和乙酸。

公开(公告)号：US4430273A

公开(公告)日：1984-02-07

申请号：US366344

申请日：1982-04-07

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Hans-Klaus Kubbeler ,  Klaus Schmitt

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Hans-Klaus Kubbeler ,  Klaus Schmitt

IPC: C07C53/12 ,  B01J31/00 ,  C07B61/00 ,  C07C51/00 ,  C07C51/54 ,  C07C51/56 ,  C07C67/00 ,  C07C51/12

CPC classification number: C07C51/54 ,  C07C51/56

Abstract: The invention provides a process for making acetic anhydride, wherein methyl acetate and/or dimethylether is (are) reacted with carbon monoxide under substantially anhydrous conditions, at temperatures of 350 to 575 K and under pressures of 1 to 300 bars in the presence of a catalyst system comprised of noble metals belonging to group VIII of the periodic system of the elements, or their compounds and iodine and/or its compounds. More specifically, an aliphatic carboxylic acid with 1 to 8 carbon atoms and at least one heterocyclic aromatic compound, in which at least one hetero atom is a quaternary nitrogen atom are used as promoters.

Abstract translation: 本发明提供一种制备乙酸酐的方法，其中乙酸甲酯和/或二甲醚在基本上无水条件下，在一氧化碳条件下，在350-575K的温度和1-300巴的压力下，在 催化剂体系由属于元素周期系的第VIII族的贵金属或其化合物和碘和/或其化合物组成。 更具体地，使用具有1至8个碳原子的脂族羧酸和至少一个杂环芳族化合物，其中至少一个杂原子是季氮原子作为启动子。

公开(公告)号：US4012439A

公开(公告)日：1977-03-15

申请号：US622263

申请日：1975-10-14

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Herbert Joest ,  Peter Zerres

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Herbert Joest ,  Peter Zerres

IPC: B01J31/00 ,  C07B61/00 ,  C07C67/08 ,  C07C69/54

CPC classification number: C07C67/08 ,  C07C67/54

Abstract: N-Butylacrylate is produced by reacting acrylic acid with n-butanol in liquid phase in contact with an acid cation exchanger as a catalyst.To this end, the acrylic acid and butanol are reacted in a molar ratio from 1:1 to 1:2.5, at 80.degree. to 130.degree. C, under a pressure from 3 to 15 atmospheres gauge, and for 20 - 90 minutes.

Abstract translation: 丙烯酸正丁酯通过使丙烯酸与正丁醇在液相中与作为催化剂的酸性阳离子交换剂接触而制备。

公开(公告)号：US3978146A

公开(公告)日：1976-08-31

申请号：US548420

申请日：1975-02-10

Applicant: Alexander Ohorodnik ,  Udo Dettmeier ,  Klaus Gehrmann ,  Heinz-Josef Berns

Inventor： Alexander Ohorodnik ,  Udo Dettmeier ,  Klaus Gehrmann ,  Heinz-Josef Berns

IPC: C07C17/25 ,  C07C17/38 ,  C07C21/21

CPC classification number: C07C17/25 ,  C07C17/383 ,  C07C21/21

Abstract: Production of 2-chlorobutadiene-(1,3) by the dehydrochlorination of 3,4-dichlorobutene-(1) in an aqueous solution of an alkali metal or alkaline earth metal hydroxide in the presence of an alcohol having between 2 and 4 carbon atoms at elevated temperature, and distilling off resulting 2-chlorobutadiene-(1,3). To this end, a reaction zone is continuously supplied with 3,4-dichlorobutene-(1), an alcohol and the aqueous hydroxide solution and the whole is heated to boiling therein while passing a stream of inert gas therethrough; resulting 2-chlorobutadiene-(1,3) is distilled off from the reaction zone and fractionated until pure; a reaction mixture which commences to separate into two layers comprising an upper layer and a lower layer is retained in the reaction zone; aqueous alcohol in excess is continuously removed from said upper layer through an overflow and the alcohol is recovered; the lower layer consisting of an aqueous/alkaline solution of unreacted hydroxide, chloride salt and minor amounts of alcohol is continuously removed through the bottom of the reaction zone; the lower layer is distilled so as to concentrate it; precipitated chloride salt is isolated, and concentrated liquor is recovered.

公开(公告)号：US3954854A

公开(公告)日：1976-05-04

申请号：US549176

申请日：1975-02-12

Applicant: Klaus Gehrmann ,  Heinz Erpenbach ,  Georg Kohl ,  Hans Klaus Kuebbeler

Inventor： Klaus Gehrmann ,  Heinz Erpenbach ,  Georg Kohl ,  Hans Klaus Kuebbeler

IPC: B01J23/00 ,  B01J27/00 ,  B01J31/00 ,  C07B61/00 ,  C07C51/00 ,  C07C51/487 ,  C07C57/065 ,  C07C57/07 ,  C07C57/075 ,  C07C67/00

CPC classification number: C07C51/487

Abstract: Monomeric acrylic acid is recovered from residues originating from processed crude acrylic acid and containing .beta.-acryloyloxypropionic acid, .beta.-acetoxypropionic acid, hydracrylic acid, dihydracrylic acid and polymeric hydracrylic acid. To this end, the residues are heated to temperatures within the range 130.degree. and 250.degree.C under pressures within the range 0.01 and 1 atmosphere absolute in contact with catalysts selected from alkali metal or alkaline earth metal carboxylates, phosphates or borates, or from alkali metal or alkaline earth metal compounds producing carboxylates together with the carboxylic acids being contained in the residues.

Abstract translation: 来自加工粗丙烯酸和含有β-丙烯酰氧基丙酸，β-乙酰氧基丙酸，氢丙烯酸，二丙烯酸和聚合丙烯酸的残余物中回收单体丙烯酸。 为此，将残余物加热到130℃和250℃范围内的温度，在0.01和1个绝对大气压范围内的压力下，与选自碱金属或碱土金属羧酸盐，磷酸盐或硼酸盐或碱的催化剂接触 与残留物中含有的羧酸一起产生羧酸盐的金属或碱土金属化合物。

公开(公告)号：US4892971A

公开(公告)日：1990-01-09

申请号：US257715

申请日：1988-10-14

Applicant: Heinz Erpenbach ,  Klaus Gehrmann ,  Peter Horstermann

Inventor： Heinz Erpenbach ,  Klaus Gehrmann ,  Peter Horstermann

IPC: C07C231/00 ,  B01J23/44 ,  C07B61/00 ,  C07C67/00 ,  C07C231/12 ,  C07C231/14 ,  C07C233/47 ,  C07C237/00

CPC classification number: C07C237/00

Abstract: In the process for the preparation of N-acetylphenylalanine by opening the ring of 2-methyl-4-benzylidene-1,3-oxazolin-5-one with water to give 2-acetaminocinnamic acid and subsequently catalytically hydrogenating the latter, both reaction stages are carried out in a mixture of an aliphatic C.sub.3 -ketone to C.sub.10 -ketone or a water-miscible ether and water as the solvent, and the hydrogenation of the 2-acetaminocinnamic acid is carried out at temperatures of 10.degree. to 50.degree. C. and pressures of 1 to 15 bar in the presence of a supported palladium catalyst.

Abstract translation: 在通过用水打开2-甲基-4-亚苄基-1,3-恶唑啉-5-酮的环以制备N-乙酰基苯丙氨酸的方法中，得到2-乙酰氨基肉桂酸，随后催化氢化后者，两个反应阶段 在脂肪族C 3-酮与C 10 - 酮或水混溶性醚和水作为溶剂的混合物中进行，2-乙酰氨基肉豆蔻酸的氢化在10〜50℃的温度下进行。 和在负载的钯催化剂存在下，压力为1至15巴。