公开(公告)号：US4344897A

公开(公告)日：1982-08-17

申请号：US102817

申请日：1979-12-13

申请人： Ralf Goedecke ,  Willi Hofen ,  Hermann Seifert ,  Gerd Siekmann

发明人： Ralf Goedecke ,  Willi Hofen ,  Hermann Seifert ,  Gerd Siekmann

IPC分类号： C07C67/00 ,  C07C407/00 ,  C07C409/24 ,  C07C409/26 ,  C07C179/00 ,  B01D3/36

CPC分类号： C07C407/003 ,  C07C407/00

摘要： In a process for the continuous preparation of pure organic solutions of percarboxylic acids having 2 to 5 carbon atoms, by(a) contacting aqueous hydrogen peroxide with a carboxylic acid containing 2 to 5 carbon atoms in the presence of an acid catalyst at a feed molar ratio of H.sub.2 O.sub.2 to carboxylic acid of 0.5:1 to 30:1,(b) isolating an extract essentially containing the percarboxylic acid and possibly the corresponding carboxylic acid not converted in stage (a), by extracting the reaction mixture obtained according to stage (a) with an organic solvent,(c) treating the extract with water or an aqueous solution in an extraction unit provided with one to ten theoretical separation stages and(d) dehydrating the solution of the percarboxylic acid and organic solvent obtained according to (c), by azeotropic distillation,the improvement wherein the organic phase of the top product of the azeotropic distillation, obtained during the dehydration according to (d), is entirely or partially recycled to stage (c) and/or entirely or partially recycled to stage (b).

摘要翻译： 在连续制备具有2至5个碳原子的过羧酸的纯有机溶液的方法中，通过（a）在酸催化剂存在下，在进料摩尔浓度下使过氧化氢水与含2-5个碳原子的羧酸接触 H 2 O 2与羧酸的比例为0.5:1至30:1，（b）通过提取根据阶段（a）获得的反应混合物，分离基本上含有过羧酸的萃取物和可能的（a）阶段未转化的相应羧酸， （c）用有机溶剂处理提取物，（c）在提供有1到10个理论分离阶段的提取单元中用水或水溶液处理提取物，和（d）使根据（c）获得的过羧酸和有机溶剂的溶液脱水 ），通过共沸蒸馏，其中根据（d）在脱水期间获得的共沸蒸馏的顶部产物的有机相完全或部分地回收 循环到阶段（c）和/或完全或部分地循环到阶段（b）。

公开(公告)号：US4089892A

公开(公告)日：1978-05-16

申请号：US678829

申请日：1976-04-28

申请人： Willi Hofen ,  Gerd Schreyer ,  Rolf Wirthwein ,  Helmut Waldmann ,  Gerd Siekmann

发明人： Willi Hofen ,  Gerd Schreyer ,  Rolf Wirthwein ,  Helmut Waldmann ,  Gerd Siekmann

IPC分类号： C07C67/00 ,  C07C407/00 ,  C07C409/24 ,  C07C179/10 ,  B01D3/00

CPC分类号： C07C407/00 ,  C07C407/003

摘要： Process for continuous production of substantially anhydrous solutions of percarboxylic acid in solvent. Aqueous hydrogen peroxide is first reacted with the corresponding carboxylic acid in the presence of acid catalyst to form percarboxylic acid and water (1). The percarboxylic acid is extracted with solvent (5), to provide a solvent phase containing the percarboxylic acid (11) and an aqueous raffinate (7). The solvent phase is subjected to distillation (12) to provide the anhydrous solution (13). In this distillation (12) the hydrogen peroxide remaining in the solvent phase produced in the extraction (5), is distilled off together with water and some solvent, and the hydrogen peroxide is recovered as an aqueous phase and recycled (14). The aqueous raffinate, which contains hydrogen peroxide, is distilled to remove water (8) and the resulting concentrate is recycled (2) for use in the reaction (1).

摘要翻译： 连续生产基本上无水的过羧酸溶剂在溶剂中的方法。 首先在酸催化剂存在下，将过氧化氢水溶液与相应的羧酸反应生成过羧酸和水（1）。 用溶剂（5）萃取过羧酸，提供含有过羧酸（11）和含水萃余液（7）的溶剂相。 对溶剂相进行蒸馏（12）以提供无水溶液（13）。 在该蒸馏（12）中，在萃取（5）中产生的溶剂相中剩余的过氧化氢与水和一些溶剂一起蒸馏出去，并将过氧化氢作为水相回收并回收（14）。 含有过氧化氢的含水萃余液被蒸馏以除去水（8），并将所得浓缩物再循环（2）用于反应（1）。

公开(公告)号：US4088676A

公开(公告)日：1978-05-09

申请号：US678825

申请日：1976-04-28

申请人： Willi Hofen ,  Gunter Prescher ,  Gerd Siekmann ,  Gunter Wolf

发明人： Willi Hofen ,  Gunter Prescher ,  Gerd Siekmann ,  Gunter Wolf

IPC分类号： B01D3/00 ,  C07C67/00 ,  C07C407/00 ,  C07C409/24 ,  C07C409/26 ,  C07C179/10

CPC分类号： C07C409/24 ,  C07C407/00 ,  C07C407/003 ,  Y10S203/06

摘要： A process for the continuous preparation of organic solutions of percarboxylic acids by reaction of an aqueous solution of hydrogen peroxide with the corresponding carboxylic acid in the presence of an acid, water-soluble catalyst which boils above 160.degree. C., extraction of the percarboxylic acid from the resulting reaction mixture using an organic solvent which is immiscible with water, reconcentration of the raffinate, which essentially contains hydrogen peroxide and the acid catalyst, by distilling off water in a distillation column and recycle of the raffinate, concentrated in this way, into the reaction with the carboxylic acid. The raffinate is divided into two partial streams in a ratio of 1 to 25:1. The raffinate is fed to a distillation column which is operated under reduced pressure and which has at least two take-off weirs as tray inserts, the first take-off weir being at least two theoretical plates above the sump phase, the second take-off weir being arranged at least two theoretical plates above the first take-off weir and the section of column between the second take-off weir and the top of the column having at least two theoretical plates. The larger partial stream of the raffinate is passed into the column below the first take-off weir and the smaller partial stream is passed into the column below the second take-off weir. Water is removed at the top of the distillation column. A first side stream, which essentially contains the hydrogen peroxide from the small partial stream of the raffinate from the extraction, is withdrawn from the second take-off weir and is a 2 to 40% strength by weight aqueous solution of hydrogen peroxide, which is optionally fed, together with the larger partial stream of the raffinate from the extraction, into the column below the first take-off weir. A second side stream is withdrawn from the first take-off weir and is an aqueous solution of the acid catalyst which optionally can be further worked up and re-used. The re-concentrated aqueous solution of hydrogen peroxide and acid catalyst, withdrawn as a sump product from the distillation, is recycled into the reaction with carboxylic acid. A third side stream can be taken from a third take-off weir which is arranged not more than 2 theoretical plates below the first take-off weir.The following applications are related to the process hereof for production of propylene oxide as being directed to aspects of the process, some of which are disclosed herein.______________________________________ German Serial U.S. Atty's Docket U.S. Serial No. No. No. ______________________________________ P 25 19 288.5 Bayer 2883 678,819 P 25 19 300.4 Bayer 2884 678,820 P 25 19 299.8 Bayer 2885 678,821 P 25 19 298.7-42 Bayer 2886 678,822 P 25 19 297.6 Bayer 2887 678,823 P 25 19 295.4 Bayer 2888 678,824 P 25 19 292.1-42 Bayer 2890 678,826 P 25 19 291.0-42 Bayer 2891 678,827 P 25 19 289.6 Bayer 2892 678,828 P 25 19 297.4 Bayer 2893 678,829 ______________________________________ All of the German applications were filed Apr. 30, 1975. Those applications are incorporated herein by reference.

公开(公告)号：US5886230A

公开(公告)日：1999-03-23

申请号：US885044

申请日：1997-06-30

申请人： Willi Hofen ,  Wolfgang Boeck ,  Stephan Rautenberg ,  Joerg Sauer ,  Dietrich Arntz ,  Ralf Goedecke ,  Wolfgang Taugner ,  Raymund Sonnenschein

发明人： Willi Hofen ,  Wolfgang Boeck ,  Stephan Rautenberg ,  Joerg Sauer ,  Dietrich Arntz ,  Ralf Goedecke ,  Wolfgang Taugner ,  Raymund Sonnenschein

IPC分类号： B01J21/04 ,  B01J23/30 ,  C07B61/00 ,  C07C319/08 ,  C07C321/04 ,  C07C319/00

CPC分类号： C07C319/08

摘要： A process for continuous production of methyl mercaptan by catalytic reaction of methanol and hydrogen sulfide. Significant improvements in the pretreatment of the feed gas mixture and in utilization of the heat of reaction and the heat content of the product gas mixture. The energy required to vaporize the methanol is derived partly from utilization of the heat of compression of the hydrogen sulfide gas and from the heat content of the product gas leaving the reactor. The heat of reaction is utilized to heat the feed gas mixture to the reaction temperature, with the help of an external gas heater.

摘要翻译： 通过甲醇和硫化氢的催化反应连续生产甲硫醇的方法。 进料气体混合物的预处理以及反应热和产物气体混合物的热含量的显着改进。 蒸发甲醇所需的能量部分来自利用硫化氢气体的压缩热和离开反应器的产物气体的热含量。 借助于外部气体加热器，利用反应热将原料气体混合物加热至反应温度。

公开(公告)号：US5866721A

公开(公告)日：1999-02-02

申请号：US885043

申请日：1997-06-30

申请人： Willi Hofen ,  Wolfgang Boeck ,  Stephan Rautenberg ,  Joerg Sauer ,  Dietrich Arntz ,  Ralf Goedecke ,  Wolfgang Taugner ,  Raymund Sonnenschein

发明人： Willi Hofen ,  Wolfgang Boeck ,  Stephan Rautenberg ,  Joerg Sauer ,  Dietrich Arntz ,  Ralf Goedecke ,  Wolfgang Taugner ,  Raymund Sonnenschein

IPC分类号： C07C319/02 ,  C07C319/28 ,  C07C321/04 ,  C07C319/06

CPC分类号： C07C319/28 ,  Y02P20/582

摘要： A process for separating the product gas mixture from the catalytic synthesis of methyl mercaptan. Because of improved separation of the product gas mixture into its components, less hydrogen sulfide and methyl mercaptan are lost in discharging the inert gases than in the known process. The inert gases can be burned without after-treatment of the exhaust gas. Likewise, the process water that is discharged is less contaminated with polysulfides.

摘要翻译： 从甲硫醇的催化合成中分离产物气体混合物的方法。 由于改进了产物气体混合物与其组分的分离，在排放惰性气体方面比在已知方法中更少的硫化氢和甲基硫醇就会减少。 惰性气体可以在没有废气的后处理的情况下燃烧。 同样，排出的工艺水较少被多硫化物污染。

公开(公告)号：US4341709A

公开(公告)日：1982-07-27

申请号：US150260

申请日：1980-05-15

申请人： Willi Hofen ,  Herbert Klenk ,  Gerd Schreyer ,  Otto Weiberg ,  Helmut Waldmann ,  Hermann Seifert ,  Karl-Hermann Reissinger ,  Wolfgang Swodenk

发明人： Willi Hofen ,  Herbert Klenk ,  Gerd Schreyer ,  Otto Weiberg ,  Helmut Waldmann ,  Hermann Seifert ,  Karl-Hermann Reissinger ,  Wolfgang Swodenk

IPC分类号： C07D313/04 ,  C07D315/00 ,  C07D313/02

CPC分类号： C07D315/00

摘要： A process for the preparation of .epsilon.-caprolactone comprising:(a) reacting cyclohexanone with a solution of perpropionic acid in an organic solvent at a molar ratio of cyclohexanone;perpropionic acid of about 1.1-5:1 at a temperature of about 10.degree. to 80.degree. C. to form a reaction mixture consisting essentially of .epsilon.-caprolactone, propionic acid and organic solvent,(b) distilling the reaction mixture from (a) in a first distillation unit to obtain a distillate comprising the organic solvent and a distillation residue,(c) introducing the distillation residue from (b) at a point into a second distillation unit to obtain a distillate comprising propionic acid and unreacted cyclohexanone, removing from the second distillation unit, separately from one another and at a point below the point of introduction into the second distillation unit, .epsilon.-caprolactone and any high-boiling constituents, and,(d) distilling in a third distillation unit the distillate from (c) to obtain a distillate consisting essentially of propionic acid and a distillation residue comprising a mixture of propionic acid and cyclohexanone.

摘要翻译： 一种制备ε-己内酯的方法，包括：（a）使环己酮与过丙酸在有机溶剂中的溶液以环己酮的摩尔比约1.1-5:1的约0.1〜5:1的摩尔比在约10℃〜 形成基本上由ε-己内酯，丙酸和有机溶剂组成的反应混合物，（b）在第一蒸馏单元中将反应混合物从（a）中蒸馏，得到包含有机溶剂和蒸馏残余物的馏出物 （c）在一点将来自（b）的蒸馏残余物引入第二蒸馏单元以获得包含丙酸和未反应的环己酮的馏出物，从第二蒸馏单元彼此分离并在低于 引入第二蒸馏装置，ε-己内酯和任何高沸点组分，和（d）在第三蒸馏装置中蒸馏出馏出物（c）得到 基本上由丙酸组成的馏出物和包含丙酸和环己酮的混合物的蒸馏残渣。

公开(公告)号：US4369096A

公开(公告)日：1983-01-18

申请号：US179316

申请日：1980-08-18

申请人： Hermann Seifert ,  Helmut Waldmann ,  Rolf Wirthwein ,  Willi Hofen

发明人： Hermann Seifert ,  Helmut Waldmann ,  Rolf Wirthwein ,  Willi Hofen

IPC分类号： C07D301/32 ,  C07D303/04 ,  B01D3/34

CPC分类号： C07D301/32 ,  C07D303/04

摘要： A process has been developed for the purification of expoxides containing carbonyl compounds as impurities wherein the carbonyl compound content is up to 2% by weight of epoxide. Purification is effected by treatment with compounds containing at least one NH.sub.2 group.

摘要翻译： 已经开发了用于纯化含有作为杂质的羰基化合物的含氧化合物的方法，其中羰基化合物含量高达2重量％的环氧化物。 通过用含有至少一个NH 2基团的化合物处理来进行纯化。

公开(公告)号：US20060135826A1

公开(公告)日：2006-06-22

申请号：US11312237

申请日：2005-12-19

申请人： Willi Hofen ,  Thomas Haas ,  Barbel Kolbe

发明人： Willi Hofen ,  Thomas Haas ,  Barbel Kolbe

IPC分类号： C07C29/74

CPC分类号： B01D1/26 ,  B01D3/146 ,  B01D3/148 ,  C07C29/80 ,  Y02P70/34 ,  C07C31/04

摘要： A process for recovering methanol from mixtures containing methanol and water, comprising multistage evaporation with heat integration, wherein the pressure is reduced from each stage to the next, and a downstream series of distillation stages with heat integration, wherein the pressure is increased from each stage to the next. The process reduces the amount of energy required for methanol recovery.

摘要翻译： 一种从含有甲醇和水的混合物中回收甲醇的方法，包括具有热积分的多级蒸发，其中压力从每个阶段下降到下一个阶段，以及下游一系列具有热积分的蒸馏阶段，其中压力从每个阶段增加 到下一个。 该方法减少甲醇回收所需的能量。

公开(公告)号：US06646141B2

公开(公告)日：2003-11-11

申请号：US10203184

申请日：2002-10-04

申请人： Willi Hofen ,  Georg Thiele ,  Alexander Möller

发明人： Willi Hofen ,  Georg Thiele ,  Alexander Möller

IPC分类号： C07D30112

CPC分类号： C07D301/12 ,  C07D301/32

摘要： The present invention relates to a process for the working up of a product stream from the epoxidation of olefins that contains olefin, olefin oxide, water-miscible organic solvent and water, by separating this product stream into an overhead product containing olefin, olefin oxide and organic solvent, and into a bottom product containing organic solvent and water, wherein the separation takes place in a pre-evaporator with at most 5 theoretical separation stages, and 20 to 60% of the total amount of organic solvent introduced with the product stream is removed with the overhead product and the residue remains in the bottom product, as well as a process for the epoxidation of olefins that includes this working up stage.

摘要翻译： 本发明涉及一种通过将该产物流分离成含有烯烃，烯烃氧化物的塔顶产物和来自含有烯烃，烯烃氧化物，水混溶性有机溶剂和水的烯烃的环氧化来处理产物流的方法， 有机溶剂，并进入含有有机溶剂和水的底部产物，其中分离在预蒸发器中进行至多5个理论分离阶段，并且与产物流引入的有机溶剂的总量的20至60％ 用塔顶产物除去残余物残留在底部产物中，以及包括该加工阶段的烯烃环氧化方法。

公开(公告)号：US06610865B2

公开(公告)日：2003-08-26

申请号：US10222343

申请日：2001-08-15

申请人： Willi Hofen ,  Georg Thiele

发明人： Willi Hofen ,  Georg Thiele

IPC分类号： C07D30112

CPC分类号： C07D301/12

摘要： A process for the catalytic epoxidation of olefins with hydrogen peroxide in a continuous flow reaction system, wherein the reaction mixture includes at least one liquid phase which is passed through a fixed catalyst bed positioned between parallel heat exchange plates and the reaction heat is at least partially removed during the course of the reaction by passing a cooling medium through the heat exchange plates.