公开(公告)号：US08450507B2

公开(公告)日：2013-05-28

申请号：US12304223

申请日：2007-06-11

Applicant: Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Christoph Sigwart

Inventor： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Christoph Sigwart

IPC: C07D323/06

CPC classification number: C07D323/06 ,  Y02P20/125

Abstract: An integrated process for preparing trioxane from formaldehyde.

Abstract translation: 从甲醛制备三恶烷的综合方法。

公开(公告)号：US08350063B2

公开(公告)日：2013-01-08

申请号：US12682294

申请日：2008-09-22

Applicant: Markus Siegert ,  Neven Lang ,  Laszlo Szarvas ,  Christoph Sigwart ,  Franz Niklaus Windlin ,  Eckhard Stroefer

Inventor： Markus Siegert ,  Neven Lang ,  Laszlo Szarvas ,  Christoph Sigwart ,  Franz Niklaus Windlin ,  Eckhard Stroefer

IPC: C07D323/06 ,  C07D45/00 ,  B01D3/10

CPC classification number: C07D323/06

Abstract: A process for separating trioxane from a feed stream I comprising formaldehyde, trioxane and water, in which a) a feed stream I comprising formaldehyde as main component and trioxane and water as secondary components is provided, b) the feed stream I, a recycle stream V and a recycle stream VII comprising formaldehyde as main component and water and trioxane as secondary components are fed into a first distillation stage and distilled at a pressure of from 0.1 to 2.5 bar to give a stream II comprising formaldehyde as main component and water as secondary component and a stream III comprising trioxane as main component and water and formaldehyde as secondary components and a stream X comprising water, trioxane and formaldehyde, c) the stream III is, if appropriate after removal of low boilers from the stream III in a low boiler removal stage, distilled in a second distillation stage at a pressure of from 0.2 to 17.5 bar, with the pressure in the second distillation stage being from 0.1 to 15 bar higher than the pressure in the first distillation stage, to give a stream IV consisting essentially of trioxane and the recycle stream V comprising trioxane as main component and water and formaldehyde as secondary components, c1) the stream IV is purified in at least one further trioxane distillation stage at a pressure at the top of from 0.5 to 2 bar to give purified trioxane as side offtake stream XII in the enrichment section of the column, d) the stream X and, if appropriate, a stream IX comprising water as main component are fed into a third distillation stage and distilled at a pressure of from 1 to 10 bar to give a stream VI consisting essentially of water and a recycle stream VII comprising formaldehyde as main component and water and trioxane as secondary components, is described.

Abstract translation: 提供了从包含甲醛，三恶烷和水的进料流I中分离三恶烷的方法，其中a）以甲醛为主要成分的进料流I和作为次要组分的三恶烷和水，b）进料流I，再循环流 V和包含甲醛作为主要成分的再循环料流VII和作为次要成分的水和三恶烷进料到第一蒸馏阶段并在0.1至2.5巴的压力下蒸馏，得到包含甲醛作为主要成分的流II和作为次要的水 组分和包含三恶烷作为主要组分的流III和作为次要组分的水和甲醛，以及包含水，三恶烷和甲醛的流X，如果在低锅炉中从流III中除去低锅炉之后，则流III 去除阶段，在第二蒸馏阶段在0.2至17.5巴的压力下蒸馏，第二蒸馏阶段的压力为0.1 得到基本上由三恶烷组成的物流IV和包含三恶烷作为主要成分的再循环流V，以及作为次要组分的水和甲醛，c1）流IV至少纯化 在0.5至2巴的顶部的压力下进一步进一步三恶烷蒸馏阶段，以在柱的富集部分中提供作为侧馏出物流XII的纯化的三恶烷，d）流X和如果合适的话，将包含水的流IX 主要组分进料到第三蒸馏阶段并在1至10巴的压力下蒸馏，得到基本上由水组成的料流VI和包含甲醛作为主要成分的再循环料流VII和作为次要成分的水和三恶烷。

公开(公告)号：US20100324311A1

公开(公告)日：2010-12-23

申请号：US12809338

申请日：2008-12-11

Applicant: Markus Siegert ,  Neven Lang ,  Joachim Thiel ,  Eckhard Stroefer ,  Christoph Sigwart

Inventor： Markus Siegert ,  Neven Lang ,  Joachim Thiel ,  Eckhard Stroefer ,  Christoph Sigwart

IPC: C07D323/06

CPC classification number: C07D323/06 ,  Y02P20/127

Abstract: A process for preparing crude trioxane (1) having a concentration in the range from 50 to 75% by weight of trioxane by trimerization of formaldehyde from an aqueous formaldehyde solution (2) in the presence of an acid catalyst (3) and concentration of the trioxane from the reaction mixture from the trimerization by distillation, wherein the trimerization of the formaldehyde and the concentration of the trioxane from the reaction mixture from the trimerization are carried out in a single column (K) which is divided by a horizontal dividing plate (T) into a lower column region (A) and an upper column region (B), with the lower column region (A) and the upper column region (B) being connected by an external vapor line and an external liquid line, and a reactive distillation in which the formaldehyde is trimerized to trioxane and the trioxane in the reaction mixture is concentrated to the solubility limit of formaldehyde is carried out in the lower column region (A) at a pressure in the range from 1 to 5 bar and a distillation in which the trioxane is concentrated to give crude trioxane having a concentration in the range from 50 to 75% by weight is carried out in the upper column region (B) at a pressure in the range from 200 to 900 mbar, is proposed.

Abstract translation: 一种在酸催化剂（3）的存在下，通过甲醛从甲醛水溶液（2）中三聚化而制备浓度在50至75重量％范围内的三恶烷的粗三恶烷（1）的方法， 来自三聚的蒸馏反应混合物中的三恶烷，其中甲醛的三聚和来自三聚反应​​混合物的三恶烷的浓度在单塔（K）中进行，该柱由水平分隔板（T ）下部列区域（A）和上部列区域（B），其中下部列区域（A）和上部列区域（B）通过外部蒸汽管线和外部液体管线连接，并且反应性 将甲醛三聚为三恶烷并将反应混合物中的三恶烷浓缩至甲醛的溶解度极限的蒸馏，在下部塔区（A）中在压力下进行 nge为1至5巴，并且其中三恶烷浓缩以产生浓度为50至75重量％浓度的粗三恶烷的蒸馏在上部塔区（B）中以 建议200至900毫巴。

公开(公告)号：US20100152466A1

公开(公告)日：2010-06-17

申请号：US12063171

申请日：2006-08-04

Applicant: Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese ,  Markus Siegert ,  Hans Hasse ,  Thomas Gruetzner ,  Sergej Blagov

Inventor： Neven Lang ,  Eckhard Stroefer ,  Achim Stammer ,  Thorsten Friese ,  Markus Siegert ,  Hans Hasse ,  Thomas Gruetzner ,  Sergej Blagov

IPC: C07D323/06

CPC classification number: C07D323/06 ,  Y02P20/125

Abstract: The invention relates to an integrated process for preparing trioxane from formaldehyde in which 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 is 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 and a recycle stream D1 comprising trioxane, water and formaldehyde are 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 0.1 to 2.5 bar to obtain the recycle stream D1 comprising trioxane, water and formaldehyde, and a stream D2 consisting substantially of water and formaldehyde.

Abstract translation: 本发明涉及从甲醛制备三恶烷的综合方法，其中将包含水和甲醛的流A1和基本上由水和甲醛组成的再循环流B2进料到三恶烷合成反应器中，其中甲醛被转化成三恶烷，以获得 产物流A2包含三恶烷，水和甲醛; 将料流A2加入到第一蒸馏塔中，并在0.1-2.5巴的压力下进行蒸馏，得到富含三恶烷的料流B1，基本上由水和甲醛组成的料流B2; 将料流B1和包含三恶烷，水和甲醛的再循环流D1进料至第二蒸馏塔，并在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C2和包含三恶烷的料流C1 ，水和甲醛; 将料流C1进料至第三蒸馏塔并在0.1-2.5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D1和基本上由水和甲醛组成的料流D 2。

公开(公告)号：US20100130756A1

公开(公告)日：2010-05-27

申请号：US12593964

申请日：2008-03-27

Applicant: Eckhard Stroefer ,  Neven Lang ,  Markus Siegert ,  Hans Hasse

Inventor： Eckhard Stroefer ,  Neven Lang ,  Markus Siegert ,  Hans Hasse

IPC: C07D323/06

CPC classification number: C07D323/06

Abstract: A process for preparing trioxane from trioxymethylene glycol dimethyl ether (POMDMEn=3) by converting trioxymethylene glycol dimethyl ether in the presence of an acidic catalyst and subsequent distillative workup of the reaction mixture, comprising the steps of: a) feeding trioxymethylene glycol dimethyl ether (POMDMEn=3) or a mixture comprising trioxymethylene glycol dimethyl ether into a reactor and converting it in the presence of an acidic catalyst to a mixture a comprising trioxane, formaldehyde, water, methylene glycol (MG), polyoxymethylene glycols (MGn>1), methanol, hemiformals (HF), methylal (POMDMEn=1) and polyoxymethylene glycol dimethyl ethers (POMDMEn>1); b) distillatively separating the reaction mixture a into a low boiler fraction b1 comprising trioxane, formaldehyde, water, methylene glycol, methanol, hemiformal (HFn=1), methylal and dioxymethylene glycol dimethyl ether (POMDMEn=2), and a high boiler fraction b2 comprising polyoxymethylene glycols (MGn>1), hemiformals (HFn>1) and polyoxymethylene glycol dimethyl ethers (POMDMEn>2); c) distillatively separating the low boiler fraction b1 into a low boiler fraction c1 comprising formaldehyde, water, methylene glycol, methanol, hemiformal (HFn=1), methylal and dioxymethylene glycol dimethyl ether (POMDMEn=2), and a high boiler fraction c2 comprising trioxane.

Abstract translation: 一种通过在酸性催化剂存在下转化三甘醇二甲醚和随后的反应混合物的蒸馏后处理由三甘醇二甲醚（POMDMEn = 3）制备三恶烷的方法，包括以下步骤：a）将三亚甲基二醇二甲醚 POMDMEn = 3）或包含三亚甲基二醇二甲醚的混合物加入到反应器中并在酸性催化剂存在下将其转化为包含三恶烷，甲醛，水，亚甲基二醇（MG），聚氧化亚甲基二醇（MGn1）， 甲醇，半缩甲醛（HF），甲缩醛（POMDMEn = 1）和聚氧化亚甲基二醇二甲醚（POMDMEn> 1）; b）将反应混合物a蒸馏分离成包含三恶烷，甲醛，水，亚甲基二醇，甲醇，半缩甲醛（HFn = 1），甲缩醛和二甲亚甲基二醇二甲醚（POMDMEn = 2）的低沸点馏分b1和高沸点馏分 b2包含聚甲醛二醇（MGn> 1），半缩甲醛（HFn1）和聚甲醛二醇二甲醚（POMDMEn> 2）; c）将低沸点馏分b1蒸馏分离成包含甲醛，水，亚甲基二醇，甲醇，半缩甲醛（HFn = 1），甲缩醛和二羟甲基二醇二甲醚（POMDMEn = 2）的低沸点馏分c1，以及高锅炉馏分c2 包括三恶烷。

公开(公告)号：US20100121081A1

公开(公告)日：2010-05-13

申请号：US12523741

申请日：2008-01-23

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

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

IPC: C07D323/06

CPC classification number: C07D323/06 ,  B01D3/146 ,  B01D3/148

Abstract: 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 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, and a stream X which comprises water, trioxane and formaldehyde, c) 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 the recycle stream V which comprises trioxane as the main component and water and formaldehyde as the secondary components, d) feeding the stream X and if appropriate a stream IX which comprises water as the main component 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.

Abstract translation: 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，并在0.1至2.5巴的压力下蒸馏以获得包含甲醛作为主要的流II 组分和水作为次要组分，以及包含三恶烷作为主要组分的流III和作为次要组分的水和甲醛，以及包含水，三恶烷和甲醛的流X，c）蒸馏流III，任选地在除去 在低锅炉去除阶段来自流III的低锅炉，在0.2至17.5巴的压力的第二蒸馏阶段中，第二蒸馏中的压力 酸化阶段比第一蒸馏阶段的压力高0.1至15巴，以获得基本上由三恶烷组成的料流IV和包含三恶烷作为主要成分的再循环流V，水和甲醛作为次要组分，d ），并且如果合适的话，将包含水作为主要成分的物流IX进料到第三蒸馏阶段并在1至10巴的压力下蒸馏以获得基本上由水和循环流VII组成的物流VI， 以甲醛为主要成分，水和三恶烷为次要成分。

公开(公告)号：US20080194845A1

公开(公告)日：2008-08-14

申请号：US11997619

申请日：2006-07-19

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

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

IPC: C07D323/06

CPC classification number: C07D323/06 ,  Y02P20/125

Abstract: The invention relates to an integrated process for preparing trioxane from formaldehyde, comprising the steps of: a) 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 and allowed to react to obtain a product stream A2 comprising trioxane, water and formaldehyde; b) stream A2 is fed to a first low-pressure distillation column and distilled at a pressure of from 0.1 to 2.5 bar to obtain a stream B1 enriched in trioxane and additionally comprising water and formaldehyde, and the recycle stream B2 consisting substantially of formaldehyde and water; c) stream B1 and a recycle stream D1 comprising trioxane, water and formaldehyde are fed to a second low-pressure distillation column and distilled at a pressure of from 0.1 to 2.5 bar to obtain a stream C1 comprising predominantly trioxane and additionally formaldehyde and water, and a stream C2 consisting substantially of formaldehyde and water; d) stream C1 is fed to a high-pressure distillation column and distilled at a pressure of from 0.2 to 17.5 bar to obtain the recycle stream D1 and a product stream D2 consisting substantially of trioxane, in which a removal of the low boilers present in streams B1 or C1 may be undertaken between steps b) and c) or c) and d).

Abstract translation: 本发明涉及从甲醛制备三恶烷的综合方法，包括以下步骤：a）将包含水和甲醛的流A 1和基本上由水和甲醛组成的循环流B 2加入到三恶烷合成反应器中， 反应以获得包含三恶烷，水和甲醛的产物流A 2; b）将料流A 2加入到第一低压蒸馏塔中并在0.1至2.5巴的压力下蒸馏以获得富含三恶烷并另外包含水和甲醛的料流B 1，并且再循环料流B 2基本上 的甲醛和水; c）料流B 1和包含三恶烷，水和甲醛的再循环料流D 1进料到第二低压蒸馏塔中，并在0.1至2.5巴的压力下蒸馏以获得主要含有三恶烷和另外的甲醛的料流C 1 和水，以及基本上由甲醛和水组成的料流C 2; d）将料流C 1加入高压蒸馏塔中，并在0.2至17.5巴的压力下进行蒸馏，以获得基本上由三恶烷组成的再循环流D 1和产物流D 2，其中将低 在流B 1或C 1中存在的锅炉可以在步骤b）和c）或c）和d）之间进行。

公开(公告)号：US20070272540A1

公开(公告)日：2007-11-29

申请号：US10583698

申请日：2004-12-21

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

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

IPC: B01D3/00 ,  C07D323/06

CPC classification number: C07D323/06

Abstract: 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：US20070142677A1

公开(公告)日：2007-06-21

申请号：US10581986

申请日：2004-12-23

Applicant: Gerhard Olbert ,  Thorsten Johann ,  Markus Weber ,  Neven Lang ,  Eckhard Stroefer ,  Martin Fiene ,  Markus Siegert

Inventor： Gerhard Olbert ,  Thorsten Johann ,  Markus Weber ,  Neven Lang ,  Eckhard Stroefer ,  Martin Fiene ,  Markus Siegert

IPC: C07C45/29

CPC classification number: F28D9/0031 ,  B01J8/0214 ,  B01J8/0285 ,  B01J8/0415 ,  B01J8/0419 ,  B01J8/0496 ,  B01J19/249 ,  B01J2208/0015 ,  B01J2208/00513 ,  B01J2208/025 ,  B01J2219/1923 ,  B01J2219/2453 ,  B01J2219/2455 ,  B01J2219/2458 ,  B01J2219/2459 ,  B01J2219/2462 ,  B01J2219/2481 ,  B01J2219/2485 ,  C07C45/38 ,  F28F2250/104 ,  C07C47/04

Abstract: A process for preparing formaldehyde by gas-phase oxidation of methanol vapor by means of a gas stream comprising molecular oxygen in the presence of a fixed-bed catalyst comprising iron and molybdenum, wherein the process is carried out in a reactor (1) having heat-exchange plates (2) which are arranged in the longitudinal direction of the reactor (1) and have a spacing between them and through which a heat transfer medium flows, inlet and outlet facilities (3, 4) for the heat transfer medium to the heat-exchange plates (2) and also gaps (5) between heat-exchange plates (2) in which the fixed-bed catalyst is present and into which the methanol vapor and the gas stream comprising molecular oxygen are passed, is described.

Abstract translation: 一种通过在包含铁和钼的固定床催化剂存在下，通过包含分子氧的气流将甲醇蒸汽气相氧化制备甲醛的方法，其中该方法在具有热量的反应器（1）中进行 - 交换板（2），其沿反应器（1）的纵向布置并且在它们之间具有间隔，传热介质流过该间隔，用于传热介质的入口和出口设备（3,4） 描述了存在固定床催化剂的热交换板（2）之间的热交换板（2）和间隙（5），其中甲醇蒸气和包含分子氧的气流通过其中。

公开(公告)号：US20100280195A1

公开(公告)日：2010-11-04

申请号：US12747742

申请日：2008-12-11

Applicant: Markus Siegert ,  Tobias Kortekamp ,  Eckhard Stroefer ,  Christoph Sigwart ,  Neven Lang

Inventor： Markus Siegert ,  Tobias Kortekamp ,  Eckhard Stroefer ,  Christoph Sigwart ,  Neven Lang

IPC: C08G65/06 ,  C08F2/00

CPC classification number: C07D323/06 ,  C08G2/10

Abstract: A process for preparing polyoxymethylene homopolymers or copolymers (7) by homopolymerization or copolymerization of trioxane, starting from methanol (1), in which methanol (1) is oxidized in a first reactor in a first production plant (A) to give an aqueous formaldehyde-comprising stream (2) which is fed to a second production plant (B) in which pure trioxane (6) is obtained and removal of low boilers (5) by distillation is carried out and the pure trioxane (6) is fed to a third production plant (C) in which it is homopolymerized or copolymerized to form polyoxymethylene homopolymers or copolymers (7), wherein the low boiler stream (5) from the low boiler removal column (K 2) is recycled to the feed stream into the first reactor in the first production plant (A), is proposed.

Abstract translation: 从甲醇（1）开始，通过三恶烷的均聚或共聚制备聚甲醛均聚物或共聚物（7）的方法，其中甲醇（1）在第一生产设备（A）中的第一反应器中被氧化，得到甲醛水溶液 （2），其被供给到其中获得纯三恶烷（6）并通过蒸馏除去低锅炉（5）的第二生产设备（B），并将纯三恶烷（6）进料至 第三生产厂（C），其中其被均聚或共聚以形成聚甲醛均聚物或共聚物（7），其中来自低锅炉除去塔（K 2）的低沸点物流（5）被再循环到进料流中， 提出了第一个生产厂（A）中的反应堆。