公开(公告)号：US20070272540A1

公开(公告)日：2007-11-29

申请号：US10583698

申请日：2004-12-21

申请人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese ,  Hans Hasse

发明人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese ,  Hans Hasse

IPC分类号： B01D3/00 ,  C07D323/06

CPC分类号： C07D323/06

摘要： A process for removing trioxane from a use stream I of formaldehyde, trioxane and water, by a) providing a use stream I which comprises formaldehyde as the main component and trioxane and water as the secondary components, b) mixing the use stream I with a recycle stream VII which comprises trioxane as the main component and formaldehyde and water as the secondary components to obtain a feed stream Ia which comprises formaldehyde as the main component and trioxane and water as the secondary components, c) distilling the use stream Ia in a first distillation stage at a pressure of from 0.1 to 2.5 bar to obtain a stream II which comprises formaldehyde as the main component and water as the secondary component, and a stream III which comprises trioxane as the main component and water and formaldehyde as the secondary components, d) distilling the stream III, optionally after removing low boilers from the stream III in a low boiler removal stage, in a second distillation stage at a pressure of from 0.2 to 17.5 bar, the pressure in the second distillation stage being from 0.1 to 15 bar higher than the pressure in the first distillation stage, to obtain a stream IV which consists substantially of trioxane and a stream V which comprises trioxane as the main component and water and formaldehyde as the secondary components, e) optionally mixing the stream V with a stream IX which comprises water as the main component to obtain a stream Va having a higher water content than the stream V, the stream Va comprising trioxane as the main component and water and formaldehyde as the secondary components, f) distilling the stream V or Va in a third distillation stage at a pressure of from 1 to 10 bar to obtain a stream VI which consists substantially of water and the recycle stream VII which comprises trioxane as the main component and water and formaldehyde as the secondary components

公开(公告)号：US20080281109A1

公开(公告)日：2008-11-13

申请号：US12063155

申请日：2006-08-01

申请人： Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese ,  Markus Siegert ,  Hans Hasse ,  Thomas Grutzner ,  Sergej Blagov

发明人： Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese ,  Markus Siegert ,  Hans Hasse ,  Thomas Grutzner ,  Sergej Blagov

IPC分类号： C07D323/06

CPC分类号： C07D323/06 ,  Y02P20/125

摘要： The invention relates to an integrated process for preparing trioxane from formaldehyde in which, in a first step, a stream A1 comprising water and formaldehyde and a recycle stream B2 consisting substantially of water and formaldehyde are fed to a trioxane synthesis reactor in which the formaldehyde is converted to trioxane to obtain a product stream A2 comprising trioxane, water and formaldehyde. Stream A2 and a recycle stream D1 comprising trioxane, water and formaldehyde are fed to a first distillation column and distilled at a pressure in the range from 0.1 to 2.5 bar to obtain a stream B1 enriched in trioxane, and the stream B2 consisting substantially of water and formaldehyde. Stream B1 is fed to a second distillation column and distilled at a pressure in the range from 0.2 to 17.5 bar to obtain a product stream C2 consisting substantially of trioxane, and a stream C1 comprising trioxane, water and formaldehyde. Stream C1 is fed to a third distillation column and distilled at a pressure in the range from 1 to 10 bar to obtain the recycle stream D1 comprising trioxane, water and formaldehyde, and a stream D2 consisting substantially of water.

摘要翻译： 本发明涉及从甲醛制备三恶烷的综合方法，其中在第一步中，将包含水和甲醛的料流A 1和基本上由水和甲醛组成的再循环料流B 2加入到三恶烷合成反应器中，其中 将甲醛转化成三恶烷，得到包含三恶烷，水和甲醛的产物流A 2。 将流A 2和包含三恶烷，水和甲醛的再循环流D 1加入到第一蒸馏塔中，并在0.1-2.5巴的压力下蒸馏，得到富含三恶烷的料流B 1，并且料流B 2 基本上由水和甲醛组成。 将料流B 1加入到第二蒸馏塔中，在0.2至17.5巴的压力下蒸馏，得到基本上由三恶烷组成的产物流C 2和包含三恶烷，水和甲醛的料流C 1。 将料流C 1加入到第三蒸馏塔中并在1至10巴的压力下进行蒸馏以获得包含三恶烷，水和甲醛的再循环流D 1和基本上由水组成的料流D 2。

公开(公告)号：US07390932B2

公开(公告)日：2008-06-24

申请号：US10547440

申请日：2004-03-03

申请人： Eckard Stroefer ,  Neven Lang ,  Ulrich Steinbrenner ,  Hans Hasse ,  Michael Ott ,  Thomas Grützner

发明人： Eckard Stroefer ,  Neven Lang ,  Ulrich Steinbrenner ,  Hans Hasse ,  Michael Ott ,  Thomas Grützner

IPC分类号： C07C45/78

CPC分类号： C07C45/002 ,  C07C45/82 ,  C07C47/04

摘要： Process for preparing high-concentration gaseous formaldehyde having a molar CH2O:H2O ratio of ≧0.6 from an aqueous formaldehyde solution by evaporation of at least part of the solution, in which the aqueous formaldehyde solution is heated to a vaporization temperature T and the gas phase formed is taken off, wherein the evaporation temperature T obeys the relationship: T[° C.]≧T′min[° C.] where T′min(c)=A+B×(c/100)+C×(c/100)2+D×(c/100)3 and A=+68.759, B=+124.77, C=−12.851, D=−10.095, where c is the instantaneous CH2O content of the aqueous formaldehyde solution during the evaporation in percent by weight and is from 20 to 99% by weight.

摘要翻译： 从甲醛水溶液中制备具有摩尔CH 2 H 2 O:H 2 O 2比值> 0.6的高浓度气态甲醛的方法，通过蒸发至少部分 溶液，其中将甲醛水溶液加热至汽化温度T，取出形成的气相，其中蒸发温度T遵循以下关系：<？in-line-formula description =“In-line formula”end = “lead”？> T [°C]> = T'分钟<°C。<？in-line-formula description =“In-line Formulas”end =“tail”？> 其中T'分钟（c）= A + Bx（c / 100）+ Cx（c / 100）2 + Dx（c / 100） / SUP>和A = + 68.759，B = + 124.77，C = -12.851，D = -10.095，其中c是蒸发期间甲醛水溶液的瞬时CH 2 O 2含量百分比 为20〜99重量％。

公开(公告)号：US08372993B2

公开(公告)日：2013-02-12

申请号：US12523741

申请日：2008-01-23

申请人： Neven Lang ,  Joachim Thiel ,  Eckhard Stroefer ,  Julia Kirschbaum ,  Markus Siegert

发明人： Neven Lang ,  Joachim Thiel ,  Eckhard Stroefer ,  Julia Kirschbaum ,  Markus Siegert

IPC分类号： C07D309/00

CPC分类号： C07D323/06 ,  B01D3/146 ,  B01D3/148

摘要： A process for removing trioxane from a use stream I of formaldehyde, trioxane and water, by a) providing a use stream I which comprises formaldehyde as the main component and trioxane and water as the secondary components, b) feeding the use stream I, a recycle stream V and a recycle stream VII which comprises formaldehyde as the main component and water and trioxane as the secondary components into a first distillation stage and distilling to obtain a stream II a steam III and formaldehyde as the and a steam X c) distilling the stream III, in a second distillation stage the pressure in the second distillation stage being from 0.1 to 15 bar higher than the pressure in the first distillation stage, to obtain a stream IV and the recycle stream V as the secondary components, d) feeding the stream X and if appropriate a stream IX into a third distillation stage and distilling at a pressure of from 1 to 10 bar to obtain a stream VI which consists substantially of water and a recycle stream VII which comprises formaldehyde as the main component and water and trioxane as the secondary components.

摘要翻译： a）从甲醛，三恶烷和水的使用流I中除去三恶烷的方法，通过a）提供包含甲醛作为主要成分的使用流I和作为次要组分的三恶烷和水，b）将使用流I， 循环流V和以甲醛为主要成分的再循环流VII和作为次要组分的水和三恶烷作为第二蒸馏步骤，并蒸馏以获得流II，蒸汽III和甲醛以及蒸汽X c）蒸馏 流III，在第二蒸馏阶段中，第二蒸馏阶段中的压力比第一蒸馏阶段中的压力高0.1至15巴，以获得流IV和再循环流V作为次要组分，d）将 流X并且如果合适的话，将流IX转化成第三蒸馏级并在1至10巴的压力下蒸馏以获得基本上由水和循环流 VII，其中甲醛为主要成分，水和三恶烷为次要成分。

公开(公告)号：US20070293688A1

公开(公告)日：2007-12-20

申请号：US11660530

申请日：2005-08-18

申请人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese

发明人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese

IPC分类号： C07D323/06

CPC分类号： B01D3/146 ,  B01D3/141 ,  C07D323/06

摘要： The present invention relates to a process for distillatively removing pure trioxane from a feedstream (I) comprising trioxane in a proportion of at least 50% by weight, based on the total weight of the feedstream (I), and additionally formaldehyde and water, which comprises feeding the feedstream I and a further aqueous stream (II) which does not contain any components extraneous to the feedstream to a dividing wall column (TWK1) having a dividing wall TW which is arranged substantially perpendicularly and divides the column interior into a feed region (A1), a withdrawal reaction (B1), an upper combined column region (C1) and a lower combined column region (D1), and drawing off from the first dividing wall column (TWK1) a bottom stream (III) comprising pure trioxane and a sidestream (IV) at the withdrawal region (B1), comprising pure water.

摘要翻译： 本发明涉及一种从基于原料流（I）的总重量至少50重量％的比例的另外的甲醛和水的含有三恶烷的原料流（I）蒸馏除去纯三恶烷的方法，以及另外的甲醛和水 包括将进料流I和不含任何与进料流无关的任何组分的另外的水流（II）进料到具有基本上垂直布置的分隔壁TW的分隔壁塔（TWK 1），并将塔内部分成进料 区域（A 1），取出反应（B 1），上部组合塔区域（C 1）和下部混合塔区域（D 1），从第一分隔壁塔（TWK 1） （III），其包含纯三恶烷和在取出区（B1））的侧流（IV），其包含纯水。

公开(公告)号：US20070135660A1

公开(公告)日：2007-06-14

申请号：US10588662

申请日：2005-02-10

申请人： Bernd Rumpf ,  Eckhard Stroefer ,  Ortmund Lang ,  Neven Lang

发明人： Bernd Rumpf ,  Eckhard Stroefer ,  Ortmund Lang ,  Neven Lang

IPC分类号： C07C45/00

CPC分类号： C07C45/82 ,  C07C47/04

摘要： A process for preparing a high-concentration formaldehyde solution by removing water from a lower-concentration formaldehyde solution having a formaldehyde content of from 5 to 50% by weight, in which the lower-concentration formaldehyde solution is fed to a preheater and heated in the preheater, depressurized via a pressure maintenance device and concentrated in a helical tube evaporator to give a vapor stream and the high-concentration formaldehyde solution as bottom stream, wherein the heated lower-concentration formaldehyde hyde solution is depressurized in the pressure maintenance device to give a two-phase mixture which is fed into the helical tube evaporator, is proposed.

摘要翻译： 通过从甲醛含量为5〜50重量％的低浓度甲醛溶液中除去水而制备高浓度甲醛溶液的方法，其中将低浓度甲醛溶液加入到预热器中并在 预热器，通过压力维持装置减压，并浓缩在螺旋管蒸发器中，得到蒸气流，高浓度甲醛溶液作为底部流，其中加压的低浓度甲醛海藻溶液在压力维持装置中减压，得到 提出了进入螺旋管蒸发器的两相混合物。

公开(公告)号：US08530678B2

公开(公告)日：2013-09-10

申请号：US11665840

申请日：2005-10-20

申请人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese

发明人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese

IPC分类号： C07D323/06

CPC分类号： C07D323/06

摘要： Processes are disclosed comprising: (a) reacting an aqueous formaldehyde solution in a reactor in the presence of a suitable catalyst to obtain a reaction product mixture comprising trioxane, formaldehyde and water; (b) distilling the reaction product mixture to form a top stream comprising crude trioxane; and (c) treating the top stream in one or more additional stages to form pure trioxane; wherein an aqueous sidestream is drawn off during the distilling of the reaction mixture.

摘要翻译： 公开的方法包括：（a）在合适的催化剂存在下使甲醛水溶液在反应器中反应，得到包含三恶烷，甲醛和水的反应产物混合物; （b）蒸馏反应产物混合物以形成包含粗三恶烷的顶流; 和（c）在一个或多个附加阶段处理顶部流以形成纯三恶烷; 其中在蒸馏反应混合物期间抽出水分流。

公开(公告)号：US20090187033A1

公开(公告)日：2009-07-23

申请号：US12304223

申请日：2007-06-11

申请人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Christophe Sigwart

发明人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Christophe Sigwart

IPC分类号： C07D323/06

CPC分类号： C07D323/06 ,  Y02P20/125

摘要： An integrated process for preparing trioxane from formaldehyde, comprising the steps of: a) feeding a feed stream A1 comprising formaldehyde and water and a recycle stream B3 comprising predominantly water and additionally formaldehyde and trioxane to a formaldehyde concentration unit and separating it into a formaldehyde-rich stream A2 and a stream A3 consisting essentially of water; b) feeding a product stream C1 comprising trioxane, water and formaldehyde, a recycle stream E1 comprising trioxane, water and formaldehyde, and, if appropriate, the stream A2 to a first low-pressure distillation column and distilling at a pressure of from 0.1 to 1.5 bar, and withdrawing a trioxane-enriched stream B comprising predominantly trioxane and additionally water and formaldehyde, a bottom draw stream B2 consisting essentially of formaldehyde and water, and the recycle stream B3 comprising predominantly water and additionally formaldehyde and trioxane as a side draw stream; c) feeding the bottom draw stream B2 and, if appropriate, the stream A2 to a trioxane synthesis reactor and allowing them to react to obtain the stream C1 comprising trioxane, water and formaldehyde; d) feeding the stream B1 to a medium-pressure distillation column and distilling at a pressure of from 1.0 to 3.0 bar to obtain a low boiler stream D1 comprising methanol, methylal and methyl formate, and a stream D2 comprising predominantly trioxane and additionally formaldehyde and water; e) feeding the stream D2 to a high-pressure distillation column and distilling at a pressure of from 2.5 to 10.0 bar to obtain the recycle stream E1 comprising trioxane, water and formaldehyde, and a product stream E2 consisting essentially of trioxane; the stream A2 being fed either to the low-pressure distillation column or to the trioxane synthesis reactor or to both.

摘要翻译： 一种用于从甲醛制备三恶烷的综合方法，包括以下步骤：a）将包含甲醛和水的进料流A1和主要包含水，再加甲醛和三恶烷的再循环流B3进料至甲醛浓缩装置，并将其分离成甲醛 - 富流A2和基本上由水组成的流A3; b）将包含三恶烷，水和甲醛的产物流C1，包含三恶烷，水和甲醛的循环流E1，以及如果合适的话，将流A2加入到第一低压蒸馏塔中，并在0.1至0.1的压力下蒸馏 包括主要为三恶烷，另外为水和甲醛的三恶烷富集流B，主要由甲醛和水组成的底部牵引流B2，主要包含水和另外的甲醛和三恶烷作为侧馏分流的再循环流B3 ; c）将底部牵引流B2和（如果合适的话）将料流A2加入到三恶烷合成反应器中并使其反应以获得包含三恶烷，水和甲醛的料流C1; d）将料流B1加入到中压蒸馏塔中并在1.0-3.0巴的压力下蒸馏，得到包含甲醇，甲缩醛和甲酸甲酯的低沸点物流D1，以及主要包含三恶烷和另外甲醛的物流D2，以及 水; e）将料流D2加入到高压蒸馏塔中并在2.5至10.0巴的压力下蒸馏以获得包含三恶烷，水和甲醛的再循环流E1和基本上由三恶烷组成的产物流E2; 流A2被供给至低压蒸馏塔或三恶烷合成反应器或两者。

公开(公告)号：US20080283384A1

公开(公告)日：2008-11-20

申请号：US12091976

申请日：2006-10-27

申请人： Neven Lang ,  Ralf Boehling ,  Achim Stammer ,  Jan Oldenburg ,  Markus Siegert ,  Eckhard Stroefer

发明人： Neven Lang ,  Ralf Boehling ,  Achim Stammer ,  Jan Oldenburg ,  Markus Siegert ,  Eckhard Stroefer

IPC分类号： C08G2/10 ,  B01D3/34 ,  C07D317/12 ,  C07D323/06

CPC分类号： C08G2/10 ,  C07D317/12 ,  C07D323/06 ,  C08G2/20 ,  Y02P20/127 ,  Y02P20/582

摘要： The invention relates to a process for preparing trioxane and at least one comonomer for preparing (co)polymers based on trioxane, in which, in a first step, formaldehyde the at least one comonomer reactant are reacted in aqueous solution to give trioxane and comonomer, to obtain a reaction mixture A1 comprising trioxane, comonomer, formaldehyde and water, with or without comonomer reactant. In a second step, the reaction mixture A1 is distilled in a first distillation stage at a first pressure to obtain a stream B1 enriched in trioxane and comonomer and a stream B2 comprising essentially water and formaldehyde, with or without comonomer reactant. In a third step, stream B1 is distilled in a second distillation stage at a pressure which is above the pressure of the first distillation stage to obtain a stream C1 comprising trioxane, comonomer and water and a product stream C2 consisting essentially of comonomer and trioxane.

摘要翻译： 本发明涉及一种制备三恶烷和至少一种共聚单体的方法，该共聚单体用于制备基于三恶烷的（共）聚合物，其中在第一步中，甲醛将至少一种共聚单体反应物在水溶液中反应得到三恶烷和共聚单体， 得到含有或不含共聚单体反应物的三恶烷，共聚单体，甲醛和水的反应混合物A 1。 在第二步中，将反应混合物A 1在第一压力下在第一蒸馏阶段进行蒸馏，以获得富含三恶烷和共聚单体的物流B 1和基本上含有水和甲醛的物流B 2，具有或不含共聚单体反应物。 在第三步骤中，在第二蒸馏阶段，在高于第一蒸馏阶段的压力的压力下蒸馏出料流B 1，以获得包含三恶烷，共聚单体和水的料流C 1和基本上由共聚单体组成的产物流C 2 和三恶烷。

公开(公告)号：US20080255376A1

公开(公告)日：2008-10-16

申请号：US12066093

申请日：2006-09-06

申请人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer

发明人： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer

IPC分类号： C07D317/12

CPC分类号： C07D317/12 ,  Y02P20/127

摘要： Processes comprising: providing a reactive distillation column having an upper region, a middle region and a lower region; feeding ethylene glycol and an aqueous formaldehyde solution into the reactive distillation column in the middle region of the reactive distillation column; reacting the ethylene glycol and the aqueous formaldehyde solution in the reactive distillation column in the presence of a catalyst to form dioxolane; removing a product stream comprising dioxolane in an amount of at least 75% by weight from the upper region of the reactive distillation column; and removing a bottom stream comprising one or more components having boiling points higher than dioxolane from the lower region of the reactive distillation column.

摘要翻译： 方法包括：提供具有上部区域，中间区域和下部区域的反应性蒸馏塔; 将乙二醇和甲醛水溶液进料到反应蒸馏塔的中间区域的反应蒸馏塔中; 在反应蒸馏塔中在催化剂存在下使乙二醇和甲醛水溶液反应形成二氧戊环; 从反应蒸馏塔的上部区域除去包含至少75重量％的二氧戊环的产物流; 并从反应蒸馏塔的下部区域除去包含沸点高于二氧戊环的一种或多种组分的底部物流。