公开(公告)号：US07329330B2

公开(公告)日：2008-02-12

申请号：US10451738

申请日：2002-01-08

申请人： Martin Gall ,  Gerd Kaibel ,  Thomas Krug ,  Harald Rust ,  Frank Stein

发明人： Martin Gall ,  Gerd Kaibel ,  Thomas Krug ,  Harald Rust ,  Frank Stein

IPC分类号： B01D3/14 ,  B01D3/42 ,  C07C29/80

CPC分类号： C07D315/00 ,  B01D3/14 ,  B01D3/141 ,  C07C29/80 ,  Y10S203/20 ,  C07C31/26 ,  C07C31/20

摘要： A process for working up by distillation the crude products obtained in the process according to DE-A 196 07 954 and containing 1,6-hexanediol (HDO), 1,5-pentanediol (PDO) or caprolactone (CLO) in order to obtain the corresponding pure products, the working-up by distillation being carried out in each case in a dividing wall column (TK) in which a dividing wall (T) is arranged in the longitudinal direction of the column with formation of an upper common column region (1), a lower common column region (6), a feed section (2, 4) having a rectification section (2) and stripping section (4), and a take-off section (3, 5) having a stripping section (3) and rectification section (5), with feeding of the respective crude product HDO, PLO or CLO in the middle region of the feed section (2, 4) and removal of the high boiler fraction (C) from the bottom of the column, of the low boiler fraction (A) via the top of the column and of the medium boiler fraction (B) from the middle region of the take-off section (3, 5), or in thermally coupled columns.

摘要翻译： 通过蒸馏处理根据DE-A 196 07954的方法获得的含有1,6-己二醇（HDO），1,5-戊二醇（PDO）或己内酯（CLO）的粗产物的方法，以获得 相应的纯产品，在各种情况下在分隔壁塔（TK）中进行蒸馏处理，其中分隔壁（T）沿塔的纵向方向排列，形成上共同区域 （1），较低的公共列区域（6），具有整流部分（2）和汽提部分（4）的进料部分（2,4）和具有汽提部分的取出部分（3,5） （3）和整流部分（5），在进料部分（2,4）的中间区域供给相应的粗产物HDO，PLO或CLO，并将高沸点馏分（C）从底部 通过塔顶和中间锅炉馏分（B）从中间排出低沸点馏分（A） 起飞段（3,5）的区域，或热耦合柱。

公开(公告)号：US06727395B1

公开(公告)日：2004-04-27

申请号：US10018338

申请日：2001-12-19

申请人： Frank Stein ,  Thomas Krug ,  Thomas Nöbel ,  Harald Rust

发明人： Frank Stein ,  Thomas Krug ,  Thomas Nöbel ,  Harald Rust

IPC分类号： C07C2700

CPC分类号： C07C29/149 ,  C07C31/20

摘要： A process for preparing 1,6-hexanediol from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol after water extraction of the reaction mixture followed by extraction with aqueous sodium hydroxide solution, by esterification of the acids and hydrogenation comprises a) liberating the carboxylic acids from the alkaline extract by addition of a mineral acid, b) fractionating the organic phase comprising carboxylic acids to give a distillate comprising the low molecular weight monocarboxylic acids and a residue comprising adipic acid and 6-hydroxycaproic acid, c) reacting the monocarboxylic an dicarboxylic acids present in the aqueous dicarboxylic acid mixture with a low molecular weight alcohol to give the corresponding carboxylic esters, d) freeing the esterification mixture obtained of excess alcohol and low boilers in a first distillation step, e) fractionating the bottom product in a second distillation step to give an ester fraction essentially free of 1,4-cyclohexanediols and a fraction comprising at least the major part of the 1,4-cyclohexanediols, f) catalytically hydrogenating the ester fraction which is essentially free of 1,4-cyclohexanediols and g) isolating 1,6-hexanediol from the hydrogenation product in a manner known per se in a final distillation step.

摘要翻译： 从包含己二酸，6-羟基己酸和少量1,4-环己二醇的羧酸混合物制备1,6-己二醇的方法，其在水提取后在环己烷氧化成环己酮/环己醇时作为副产物获得 的反应混合物，然后用氢氧化钠水溶液萃取，通过酸的酯化和氢化反应，包括a）通过加入无机酸从碱性提取物中释放出羧酸，b）将包含羧酸的有机相分馏得到馏出物 包括低分子量单羧酸和包含己二酸和6-羟基己酸的残基，c）使一元羧酸与二羧酸混合物中存在的二羧酸与低分子量醇反应，得到相应的羧酸酯，d）释放 在第一馏出物中获得过量酒精和低锅炉的酯化混合物 e步骤，e）在第二蒸馏步骤中分馏底部产物，得到基本上不含1,4-环己烷二醇的酯馏分和至少包含大部分1,4-环己烷二醇的馏分，f）催化氢化酯 基本上不含1,4-环己烷二醇的馏分，和g）在最终蒸馏步骤中以本身已知的方式从氢化产物中分离出1,6-己二醇。

公开(公告)号：US06288286B1

公开(公告)日：2001-09-11

申请号：US09700366

申请日：2000-11-15

申请人： Frank Stein ,  Thomas Krug ,  Martin Gall ,  Gabriele Iffland

发明人： Frank Stein ,  Thomas Krug ,  Martin Gall ,  Gabriele Iffland

IPC分类号： C07C2700

CPC分类号： C07C29/149 ,  C07C2601/14 ,  C07C31/20 ,  C07C35/08

摘要： A process for preparing 1,6-hexanediol from a carboxylic acid mixture obtained as by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol with oxygen or oxygen-comprising gases and by aqueous extraction of the reaction mixture and comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols by esterification of the acids and hydrogenation, by a) reacting the mono- and dicarboxylic acids in the aqueous dicarboxylic acid mixture with a low molecular weight alcohol to form the corresponding carboxylic esters, b) conducting a first distillation to remove excess alcohol and low boilers from the esterification mixture obtained, c) conducting a second distillation to separate the bottom product into an ester fraction which is essentially free from 1,4-cyclohexanediols and a fraction which includes at least the larger proportion of the 1,4-cyclohexanediols, d) subjecting the ester fraction essentially free from 1,4-cyclohexanediols to a catalytic hydrogenation, and e) subjecting the hydrogenation effluent to a distillation to recover 1,6-hexanediol in a conventional manner, comprises using an aqueous dicarboxylic acid mixture comprising more than 20 ppm of cobalt and more than 40 ppm of phosphorus in the form of phosphate and passing this aqueous dicarboxylic acid mixture through a cation exchanger and after the esterification of step (a) through an anion exchanger.

摘要翻译： 从环己烷氧化成环己酮/环己醇与氧气或含氧气体的副产物得到的羧酸混合物中制备1,6-己二醇的方法，并通过水提取反应混合物，并包含己二酸，6- 羟基己酸和少量的1,4-环己烷二醇通过酸的酯化和氢化，a）使二羧酸二羧酸混合物与低分子量醇反应形成相应的羧酸酯，b）导电 从所得到的酯化混合物中除去多余的醇和低沸点物的第一次蒸馏，c）进行第二次蒸馏以将底部产物分离成基本上不含1,4-环己烷二醇的酯馏分和至少包括较大的 1,4-环己烷二醇的比例，d）将基本上不含1,4-环己烷二醇的酯馏分进行催化水解 国家和地区）使氢化流出物以常规方式进行蒸馏以回收1,6-己二醇，包括使用包含大于20ppm钴的多余二羧酸混合物和大于40ppm磷酸盐形式的磷， 使该含水二羧酸混合物通过阳离子交换剂，并且在步骤（a）通过阴离子交换剂酯化之后。

公开(公告)号：US06831182B2

公开(公告)日：2004-12-14

申请号：US10433424

申请日：2003-06-04

申请人： Holger Borchert ,  Stephan Schlitter ,  Rolf-Hartmuth Fischer ,  Markus Rösch ,  Frank Stein ,  Ralf-Thomas Rahn ,  Alexander Weck ,  Gerd Kaibel

发明人： Holger Borchert ,  Stephan Schlitter ,  Rolf-Hartmuth Fischer ,  Markus Rösch ,  Frank Stein ,  Ralf-Thomas Rahn ,  Alexander Weck ,  Gerd Kaibel

IPC分类号： C07D30708

CPC分类号： C07D307/08

摘要： The present invention relates to a process for the gas-phase hydrogenation of C4-dicarboxylic acids and/or their derivatives over a catalyst based on copper oxide to give substituted or unsubstituted &ggr;-butyrolactone and/or tetrahydrofuran, which comprises, which a first reaction zone in which the C4-dicarboxylic acid and/or its derivatives is/are reacted to give a mixture comprising a substituted or unsubstituted &ggr;-butyrolactone as main product and a subsequent second reaction zone in which the substituted or unsubstituted &ggr;-butyrolactone present in the mixture from the first hydrogenation step is reacted at a temperature lower than the temperature in the first hydrogenation step to give substituted or unsubstituted tetrahydrofuran.

公开(公告)号：US5981769A

公开(公告)日：1999-11-09

申请号：US125974

申请日：1998-08-28

申请人： Karl Gerhard Baur ,  Rolf Fischer ,  Rolf Pinkos ,  Frank Stein ,  Boris Breitscheidel ,  Harald Rust

发明人： Karl Gerhard Baur ,  Rolf Fischer ,  Rolf Pinkos ,  Frank Stein ,  Boris Breitscheidel ,  Harald Rust

IPC分类号： C07D313/04 ,  C07C27/12 ,  C07C29/149 ,  C07C29/80 ,  C07C29/88 ,  C07C31/20 ,  C07C31/27 ,  C07C51/31 ,  C07D315/00 ,  C07D313/00

CPC分类号： C07D315/00 ,  C07C29/149 ,  C07C29/80 ,  C07C29/88 ,  C07C51/313 ,  C07C2101/14

摘要： 1,6-hexanediol and .epsilon.-caprolactone are prepared from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as a by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol using oxygen or oxygen-containing gases by water extraction of the reaction mixture, by esterifying and hydrogenating a substream to give hexanediol and cyclizing 6-hydroxycaproic esters to give caprolactone.

摘要翻译： PCT No.PCT / EP97 / 00990 371日期1998年8月28日 102（e）1998年8月28日PCT PCT 1997年2月28日PCT公布。 公开号WO97 / 31883 日期1991年9月4日，1991年6月 - 己二醇和ε-己内酯由包含己二酸，6-羟基己酸和少量1,4-环己二醇的羧酸混合物制备，其作为副产物在氧化 使用氧或含氧气体通过水提取反应混合物，通过酯化和氢化子流，得到己二醇并环化6-羟基己酸酯，得到己内酯，得到环己烷至环己酮/环己醇。

公开(公告)号：US6008418A

公开(公告)日：1999-12-28

申请号：US125976

申请日：1998-08-28

申请人： Karl Gerhard Baur ,  Rolf Fischer ,  Rolf Pinkos ,  Frank Stein ,  Harald Rust ,  Boris Breitscheidel

发明人： Karl Gerhard Baur ,  Rolf Fischer ,  Rolf Pinkos ,  Frank Stein ,  Harald Rust ,  Boris Breitscheidel

IPC分类号： B01J23/80 ,  B01J23/889 ,  C07B61/00 ,  C07C29/149 ,  C07C31/20

CPC分类号： C07C29/149

摘要： 1,6-Hexanediol is prepared from a carboxylic acid mixture comprising adipic acid, 6-hydroxycaproic acid and small amounts of 1,4-cyclohexanediols which is obtained as a by-product in the oxidation of cyclohexane to cyclohexanone/cyclohexanol by water extraction of the reaction mixture, by esterification of the acids and hydrogenation whereina) the monocarboxylic and dicarboxylic acids present in the aqueous dicarboxylic acid mixture are reacted with a low molecular weight alcohol to give the corresponding carboxylic esters,b) the resulting esterification mixture is freed of excess alcohol and low boilers in a first distillation stage,c) the bottoms are fractionated in a second distillation stage to give an ester fraction essentially free of 1,4-cyclohexanediols and a fraction comprising at least the major part of the 1,4-cyclohexanediols,d) the ester fraction essentially free of 1,4-cyclohexanediols is catalytically hydrogenated ande) in a pure distillation stage, 1,6-hexanediol is isolated from the hydrogenation product in a manner known per se.

摘要翻译： PCT No.PCT / EP97 / 00980 Sec。 371日期1998年8月28日 102（e）1998年8月28日PCT PCT 1997年2月28日PCT公布。 公开号WO97 / 31882 日期1991年9月4日6,6-己二醇由包含己二酸，6-羟基己酸和少量1,4-环己二醇的羧酸混合物制备，其作为副产物在环己烷氧化成环己酮/ 环己醇通过水提取反应混合物，通过酸的酯化和氢化，其中存在于二羧酸水溶液混合物中的单羧酸和二羧酸与低分子量醇反应得到相应的羧酸酯，b）得到的 酯化混合物在第一蒸馏阶段中不含过量的醇和低沸点，c）在第二蒸馏阶段对塔底物进行分馏，得到基本上不含1,4-环己烷二醇的酯馏分和至少包含至少大部分 1,4-环己烷二醇，d）基本上不含1,4-环己烷二醇的酯馏分是催化氢化的，e）在纯蒸馏阶段， 以本身已知的方式从加氢产物中分离出1,6-己二醇。

公开(公告)号：US06359108B1

公开(公告)日：2002-03-19

申请号：US09423459

申请日：1999-11-09

申请人： Karsten Eller ,  Frank Stein ,  Christoph Sigwart ,  Rainer Becker ,  Klaus-Dieter Plitzko ,  Rolf Fischer ,  Ulrich Müller

发明人： Karsten Eller ,  Frank Stein ,  Christoph Sigwart ,  Rainer Becker ,  Klaus-Dieter Plitzko ,  Rolf Fischer ,  Ulrich Müller

IPC分类号： C08G5968

CPC分类号： B01J29/049 ,  C08G65/2657

摘要： A process for polymerizing cyclic ethers over a heterogeneous catalyst comprises using a heterogeneous catalyst comprising one or more pillared interlayered clays (PILCs).

摘要翻译： 在非均相催化剂上聚合环醚的方法包括使用包含一个或多个柱状中间层粘土（PILC）的多相催化剂。

公开(公告)号：US06211401B1

公开(公告)日：2001-04-03

申请号：US09308320

申请日：1999-05-19

申请人： Karsten Eller ,  Christoph Sigwart ,  Rainer Becker ,  Klaus-Dieter Plitzko ,  Rolf Fischer ,  Frank Stein ,  Ulrich Müller ,  Michael Hesse

发明人： Karsten Eller ,  Christoph Sigwart ,  Rainer Becker ,  Klaus-Dieter Plitzko ,  Rolf Fischer ,  Frank Stein ,  Ulrich Müller ,  Michael Hesse

IPC分类号： C07C6724

CPC分类号： C08G65/2693 ,  B01J23/24 ,  C08G65/20

摘要： Polytetrahydrofuran, tetrahydrofuran copolymers, diesters or monoesters of these polymers are prepared by polymerizing tetrahydrofuran in the presence of at least one telogen and/or comonomer on a heterogeneous carrier catalyst which contains on an oxidic carrier material as active mass a catalytically active amount of at least one oxygenous molybdenum and/or tungsten compound and, when the precursor compounds of the active mass have been applied to the carrier material precursor, has been calcined at temperatures of between 500° C. and 1000° C. The catalyst used contains a promotor which comprises at least one element or a compound of an element of the 2nd, 3rd including the lanthanides, 5th, 6th, 7th, 8th or 14th group of the periodic system of elements.

摘要翻译： 这些聚合物的四氢呋喃共聚物，二酯或单酯通过在至少一种前体和/或共聚单体存在下在非均相载体催化剂的存在下聚合四氢呋喃来制备，所述非均相载体催化剂在氧化载体材料上作为活性物质至少具有催化活性量 一种氧钼和/或钨化合物，并且当将活性物质的前体化合物已经施加到载体材料前体时，已经在500℃和1000℃之间的温度下煅烧。所使用的催化剂包含一种促进剂， 包括至少一种元素或元素的化合物，其包括元素周期性系统的镧系元素，第5，第6，第7，第8或第14组的第2,3族元素。

公开(公告)号：US20100209708A1

公开(公告)日：2010-08-19

申请号：US12676488

申请日：2008-09-09

申请人： Markus Braun ,  Rainer Dyllick-Brenzinger ,  Matthias Maase ,  Frank Stein ,  Megan Turner ,  Eric Uerdingen

发明人： Markus Braun ,  Rainer Dyllick-Brenzinger ,  Matthias Maase ,  Frank Stein ,  Megan Turner ,  Eric Uerdingen

IPC分类号： B32B5/00 ,  C08B1/00

CPC分类号： C08J3/24 ,  C08H8/00 ,  C08J2301/02 ,  C08J2397/02 ,  Y10T428/2982

摘要： Crosslinked cellulose beads or lignocellulose beads (referred to as beads for short), wherein at least 50% by weight of the beads have a particle diameter greater than 800 μm (21° C., 1 bar, determined by sieve analysis).

摘要翻译： 交联的纤维素珠或木质纤维素珠（简称为珠），其中至少50重量％的珠具有大于800μm的粒径（21℃，1巴，通过筛分分析确定）。

公开(公告)号：US20060004890A1

公开(公告)日：2006-01-05

申请号：US10865215

申请日：2004-06-10

申请人： Bruce Semple ,  Frank Stein

发明人： Bruce Semple ,  Frank Stein

IPC分类号： G06F17/30

CPC分类号： G06F16/10 ,  G06F16/38

摘要： Methods and systems are disclosed for providing incremental backup and restore operations for a file system having a large number of files. A file system accessing a mass storage device is augmented by including an enhanced directory services component (EDSC) that has an associated EDSC database that contains file system information regarding contents of the file system including file attributes. Accordingly, high-performance backup and restore operations can be performed by directly or indirectly querying the EDSC database to obtain fill attributes rather than traversing the file system's native file attribute data structures. This enables the file system to provide more consistent response to applications requesting file status independent of the number of files stored in the file system.

摘要翻译： 公开了用于为具有大量文件的文件系统提供增量备份和恢复操作的方法和系统。 通过包括具有相关联的EDSC数据库的增强目录服务组件（EDSC）来增加访问大容量存储设备的文件系统，所述EDSC数据库包含关于包括文件属性的文件系统的内容的文件系统信息。 因此，可以通过直接或间接查询EDSC数据库来获得填充属性而不是遍历文件系统的本机文件属性数据结构来执行高性能备份和恢复操作。 这使得文件系统能够对请求文件状态的应用提供更一致的响应，而与文件系统中存储的文件数量无关。