公开(公告)号：US07981391B2

公开(公告)日：2011-07-19

申请号：US12541674

申请日：2009-08-14

申请人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Jürgen Glenneberg ,  Wolfgang Wöll

发明人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Jürgen Glenneberg ,  Wolfgang Wöll

IPC分类号： C01B15/023 ,  C01B15/037

CPC分类号： C01B15/013 ,  C01B15/023 ,  C07D301/12

摘要： An aqueous hydrogen peroxide solution containing i) less than 50 wppm alkali metals, alkaline earth metals or combinations thereof in total, irrespective whether the alkali or alkaline earth metals are present in cationic or complex form; ii) less than 50 wppm of amines having a pkB of less than 4.5 or the corresponding protonated compounds in total; and iii) at least 100 wppm anions or compounds that can dissociate to form anions in total, where the wppm are based on the weight of hydrogen peroxide and the concentration of hydrogen peroxide is more than 50% by weight based on the total weight of the hydrogen peroxide solution. A process for preparation of said hydrogen peroxide solution and the use of said solution in a process for epoxidation of olefins is also disclosed.

摘要翻译： 含有i）含有i）总计少于50wppm的碱金属，碱土金属或其组合的过氧化氢水溶液，不论碱金属或碱土金属是以阳离子或复合形式存在; ii）小于50wppm的pkB小于4.5的胺或相应的质子化合物总计; 和iii）至少100wppm的阴离子或化合物，其可以离解以形成阴离子，其中wppm基于过氧化氢的重量，并且过氧化氢的浓度基于总重量的50重量％ 过氧化氢溶液。 还公开了制备所述过氧化氢溶液的方法和在烯烃环氧化方法中使用所述溶液。

公开(公告)号：US20090294727A1

公开(公告)日：2009-12-03

申请号：US12541674

申请日：2009-08-14

申请人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Jürgen Glenneberg ,  Wolfgang Wöll

发明人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Jürgen Glenneberg ,  Wolfgang Wöll

IPC分类号： C01B15/01

CPC分类号： C01B15/013 ,  C01B15/023 ,  C07D301/12

摘要： An aqueous hydrogen peroxide solution containing i) less than 50 wppm alkali metals, alkaline earth metals or combinations thereof in total, irrespective whether the alkali or alkaline earth metals are present in cationic or complex form; ii) less than 50 wppm of amines having a pkB of less than 4.5 or the corresponding protonated compounds in total; and iii) at least 100 wppm anions or compounds that can dissociate to form anions in total, where the wppm are based on the weight of hydrogen peroxide and the concentration of hydrogen peroxide is more than 50% by weight based on the total weight of the hydrogen peroxide solution. A process for preparation of said hydrogen peroxide solution and the use of said solution in a process for epoxidation of olefins is also disclosed.

摘要翻译： 含有i）含有i）总计少于50wppm的碱金属，碱土金属或其组合的过氧化氢水溶液，不论碱金属或碱土金属是以阳离子或复合形式存在; ii）小于50wppm的pkB小于4.5的胺或相应的质子化合物总计; 和iii）至少100wppm的阴离子或化合物，其可以离解以形成阴离子，其中wppm基于过氧化氢的重量，并且过氧化氢的浓度基于总重量的50重量％ 过氧化氢溶液。 还公开了制备所述过氧化氢溶液的方法和在烯烃环氧化方法中使用所述溶液。

公开(公告)号：US07722847B2

公开(公告)日：2010-05-25

申请号：US10669978

申请日：2003-09-24

申请人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Jürgen Glenneberg ,  Wolfgang Wöll

发明人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Jürgen Glenneberg ,  Wolfgang Wöll

IPC分类号： C01B15/023 ,  C01B15/037

CPC分类号： C01B15/013 ,  C01B15/023 ,  C07D301/12

摘要： An aqueous hydrogen peroxide solution containing i) less than 50 wppm alkali metals, alkaline earth metals or combinations thereof in total, irrespective whether the alkali or alkaline earth metals are present in cationic or complex form; ii) less than 50 wppm of amines having a pkB of less than 4.5 or the corresponding protonated compounds in total; and iii) at least 100 wppm anions or compounds that can dissociate to form anions in total, where the wppm are based on the weight of hydrogen peroxide and the concentration of hydrogen peroxide is more than 50% by weight based on the total weight of the hydrogen peroxide solution. A process for preparation of said hydrogen peroxide solution and the use of said solution in a process for epoxidation of olefins is also disclosed.

摘要翻译： 含有i）含有i）总计少于50wppm的碱金属，碱土金属或其组合的过氧化氢水溶液，不论碱金属或碱土金属是以阳离子或复合形式存在; ii）小于50wppm的pkB小于4.5的胺或相应的质子化合物总计; 和iii）至少100wppm的阴离子或化合物，其可以离解以形成阴离子，其中wppm基于过氧化氢的重量，并且过氧化氢的浓度基于总重量的50重量％ 过氧化氢溶液。 还公开了制备所述过氧化氢溶液的方法和在烯烃环氧化方法中使用所述溶液。

公开(公告)号：US07141683B2

公开(公告)日：2006-11-28

申请号：US10428607

申请日：2003-05-02

申请人： Thomas Haas ,  Georg Thiele ,  Gerald Moroff ,  Norbert Ullrich ,  Willi Hofen ,  Guido Stochniol ,  Hubertus Eickhoff ,  Werner Pohl ,  Wolfgang Wöll ,  Claudia Brasse ,  José Berges ,  Percy Kampeis

发明人： Thomas Haas ,  Georg Thiele ,  Gerald Moroff ,  Norbert Ullrich ,  Willi Hofen ,  Guido Stochniol ,  Hubertus Eickhoff ,  Werner Pohl ,  Wolfgang Wöll ,  Claudia Brasse ,  José Berges ,  Percy Kampeis

IPC分类号： C07D301/12

CPC分类号： C07D301/12

摘要： A process for the epoxidation of olefins which includes i) reacting an olefin with hydrogen peroxide in presence of an epoxidation catalyst and an alcoholic solvent; ii) separating product olefin oxide and unreacted olefin from the reaction product of step i); iii) recovering a stream comprising the alcoholic solvent; and iv) subjecting the recovered stream of step iii) to hydrogenation.

摘要翻译： 烯烃环氧化方法，其包括：i）在环氧化催化剂和醇溶剂的存在下使烯烃与过氧化氢反应; ii）从步骤i）的反应产物中分离产物烯烃氧化物和未反应的烯烃; iii）回收包含醇溶剂的料流; 和iv）使回收的步骤iii）的流经受氢化。

公开(公告)号：US07169945B2

公开(公告)日：2007-01-30

申请号：US10724300

申请日：2003-11-26

申请人： Thomas Haas ,  Willi Hofen ,  Wolfgang Wöll ,  Claudia Brasse ,  Guido Stochniol ,  Norbert Ullrich

发明人： Thomas Haas ,  Willi Hofen ,  Wolfgang Wöll ,  Claudia Brasse ,  Guido Stochniol ,  Norbert Ullrich

IPC分类号： C07D301/12

CPC分类号： C07D301/12 ,  Y02P20/584

摘要： A process for the catalytic epoxidation of olefins in the presence of a titanium containing zeolite catalyst and a polar solvent whereby the deactivation of the catalyst upon recycling of the solvent has been considerably reduced. In the process one or more nitrogen containing compounds are introduced at some stage, a solvent stream is recovered, treated to contain less than 50 wppm nitrogen in the form of organic nitrogen compounds and at least a part of it is recycled to the epoxidation step. Also disclosed is a process for the catalytic epoxidation of propene which integrates the treatment and recycle of the solvent into the workup of the reaction mixture.

摘要翻译： 一种在含钛沸石催化剂和极性溶剂的存在下烯烃的催化环氧化方法，从而显着减少了在溶剂再循环时催化剂失活。 在该过程中，在一些阶段引入一种或多种含氮化合物，回收溶剂流，将其处理为含有少于50wppm氮的有机氮化合物形式，并将其至少一部分再循环至环氧化步骤。 还公开了丙烯的催化环氧化方法，其将溶剂的处理和再循环整合到反应混合物的后处理中。

公开(公告)号：US06878836B2

公开(公告)日：2005-04-12

申请号：US10839572

申请日：2004-05-05

申请人： Thomas Haas ,  Claudia Brasse ,  Wolfgang Wöll ,  Willi Hofen ,  Bernd Jaeger ,  Guido Stochniol ,  Norbert Ullrich

发明人： Thomas Haas ,  Claudia Brasse ,  Wolfgang Wöll ,  Willi Hofen ,  Bernd Jaeger ,  Guido Stochniol ,  Norbert Ullrich

IPC分类号： C07D301/12 ,  C07D303/04

CPC分类号： C07D303/04 ,  C07D301/12 ,  Y02P20/584

摘要： A process for the continuous epoxidation of propene with hydrogen peroxide in the presence of a titanium silicalite catalyst and a methanol solvent, wherein the catalyst is periodically regenerated by washing with a methanol solvent at a temperature of at least 100° C. and the epoxidation reaction is carried out for periods of more than 300 h between two regeneration steps.

摘要翻译： 一种在钛硅沸石催化剂和甲醇溶剂存在下用过氧化氢连续环氧化丙烯的方法，其中催化剂通过在至少100℃的温度下用甲醇溶剂洗涤并周期性地再生，并且环氧化反应 在两个再生步骤之间进行超过300小时的时间。

公开(公告)号：US06838572B2

公开(公告)日：2005-01-04

申请号：US10669993

申请日：2003-09-24

申请人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Willi Hofen ,  Wolfgang Wöll ,  Georg Thiele

发明人： Thomas Haas ,  Claudia Brasse ,  Guido Stochniol ,  Willi Hofen ,  Wolfgang Wöll ,  Georg Thiele

IPC分类号： C01B15/013 ,  C01B15/023 ,  C07D301/12

CPC分类号： C01B15/013 ,  C01B15/023 ,  C07D301/12

摘要： A continuous process for the epoxidation of olefins with hydrogen peroxide in the presence of a heterogeneous catalyst promoting the epoxidation reaction, whereby the aqueous reaction mixture contains i) an olefin; ii) hydrogen peroxide; iii) less than 100 wppm of alkali metals, earth alkali metals, both irrespective whether in ionic, complex or covalently bonded form, bases or cations of bases having a pkB of less than 4.5, or combinations thereof; and, iv) at least 100 wppm of bases or cations of bases having a pkB of at least 4.5 or combinations thereof, whereby the wppm are based on the total weight of hydrogen peroxide in the reaction mixture.

摘要翻译： 在促进环氧化反应的多相催化剂的存在下用过氧化氢环氧化烯烃的连续方法，由此含水反应混合物含有i）烯烃; ii）过氧化氢; iii）小于100wppm的碱金属，碱土金属，无论是在离子，复合或共价键合的形式，碱性或pKB小于4.5的碱的阳离子，或其组合; 和iv）至少100wppm的pkB至少为4.5的碱或碱的阳离子或其组合，其中wppm是基于反应混合物中过氧化氢的总重量。

公开(公告)号：US06447744B1

公开(公告)日：2002-09-10

申请号：US09706184

申请日：2000-11-06

申请人： Thomas Haas ,  Jürgen Glenneberg ,  Rudolf Wagner ,  Matthias Creutz ,  Jörg Sauer ,  Rudolf Vanheertum

发明人： Thomas Haas ,  Jürgen Glenneberg ,  Rudolf Wagner ,  Matthias Creutz ,  Jörg Sauer ,  Rudolf Vanheertum

IPC分类号： C01B15023

CPC分类号： B01J35/023 ,  B01J8/0242 ,  B01J10/002 ,  B01J23/44 ,  B01J2208/00106 ,  C01B15/023

摘要： In carrying out the hydrogenation stage of the anthraquinone process for the preparation of hydrogen peroxide in a hydrogenation reactor on a fixed bed catalyst of a particulate catalyst, the service life of the catalyst is increased in that the working solution comprising the reaction carrier and a gas phase comprising hydrogen, are passed through the hydrogenation reactor from the bottom upwards. The empty tube speed of the working solution is 0.05 to 100 m/h, preferably 10 to 50 m/h.

摘要翻译： 在用于在颗粒催化剂的固定床催化剂上的氢化反应器中制备过氧化氢的氢醌化步骤中，催化剂的使用寿命增加，包括反应载体和气体的工作溶液 包含氢的相，从底部向上通过氢化反应器。 工作溶液的空管速度为0.05〜100m / h，优选为10〜50m / h。

公开(公告)号：US07195748B2

公开(公告)日：2007-03-27

申请号：US10476202

申请日：2003-03-04

申请人： Bernd Jaeger ,  Thomas Haas ,  Jürgen Glenneberg ,  Jürgen Grunert

发明人： Bernd Jaeger ,  Thomas Haas ,  Jürgen Glenneberg ,  Jürgen Grunert

IPC分类号： C01B15/023

CPC分类号： C01B15/023 ,  B01J23/96 ,  B01J35/023 ,  Y02P20/584

摘要： The invention relates to a process for the production of hydrogen peroxide by the anthraquinone process, comprising a hydrogenation stage, an oxidation stage and an extraction stage. According to the invention, catalytic hydrogenation of anthraquinone derivatives dissolved in a working solution is carried out in the presence of added molecular oxygen. Per mol hydrogen, 0.1 to 10 mmol oxygen is preferably introduced into the hydrogenation stage with the hydrogenating gas, in mixture with an inert gas and/or dissolved and/or dispersed in the working solution. This increases the residence time of the catalyst.

摘要翻译： 本发明涉及一种通过蒽醌法生产过氧化氢的方法，包括氢化阶段，氧化阶段和萃取阶段。 根据本发明，溶解在工作溶液中的蒽醌衍生物的催化氢化在加入的分子氧的存在下进行。 每摩尔氢气，优选将0.1至10mmol氧气与氢化气体一起引入氢化阶段，与惰性气体混合和/或溶解和/或分散在工作溶液中。 这增加了催化剂的停留时间。

公开(公告)号：US07091384B2

公开(公告)日：2006-08-15

申请号：US10516319

申请日：2003-06-25

申请人： Bernd Jaeger ,  Thomas Haas ,  Guido Stochniol ,  Christian Lettmann ,  Willi Hofen ,  Klaus Stadtmueller ,  Joerg Lotz

发明人： Bernd Jaeger ,  Thomas Haas ,  Guido Stochniol ,  Christian Lettmann ,  Willi Hofen ,  Klaus Stadtmueller ,  Joerg Lotz

IPC分类号： C07C209/72

CPC分类号： C07C209/72 ,  C07C211/36

摘要： The invention relates to a process for increasing the selectivity of the hydrogenation of 4,4′-diaminodiphenylmethane (4,4′-MDA) to diaminodicyclohexylmethane (4,4′-HMDA) by catalytic hydrogenation of a mixture containing 4,4′-MDA as the main component and its mono-N-methyl derivative as a secondary component. According to the invention, the hydrogenation is terminated before a conversion of 4,4′-MDA to 4,4′-HMDA of 99% is achieved. Under these conditions, a substantially smaller proportion of the N-methyl-4,4′-MDA is hydrogenated to N-methyl-4,4-HMDA.

摘要翻译： 本发明涉及通过催化氢化含有4,4'-二氨基二苯基甲烷（4,4'-MDA）的混合物的方法提高4,4'-二氨基二苯基甲烷（4,4'-MDA） MDA为主要成分，其单-N-甲基衍生物为次要成分。 根据本发明，在将4,4'-MDA转化为99％的4,4'-HMDA之前终止氢化。 在这些条件下，将大部分比例的N-甲基-4,4'-MDA氢化成N-甲基-4,4-HMDA。