公开(公告)号：US20100145079A1

公开(公告)日：2010-06-10

申请号：US12532430

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 formaldehyde, water, methylene glycol, methanol, hemiformal (HFn=1), methylal and dioxymethylene glycol dimethyl ether (POMDMEn=2), and a high boiler fraction b2 comprising trioxane, polyoxymethylene glycols (MGn>1), hemiformals (HFn>1) and polyoxymethylene glycol dimethyl ethers (POMDMEn>2); c) distillatively separating the high boiler fraction b2 into a low boiler fraction c1 comprising trioxane, and a high boiler fraction c2 comprising polyoxymethylene glycols (MGn>1), hemiformals (HFn>1) and polyoxymethylene glycol dimethyl ethers (POMDMEn>2).

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，以及高沸点馏分b2， 三氧杂环己烷，聚甲醛（MGn> 1），半缩甲醛（HFn1）和聚甲醛二醇二甲醚（POMDMEn> 2）; c）将高沸点馏分b2蒸馏成包含三恶烷的低沸点馏分c1和包含聚甲醛二醇（MGn> 1），半缩甲醛（HFn1）和聚甲醛二醇二甲醚（POMDMEn2）的高沸点馏分c2。

公开(公告)号：US20070155972A1

公开(公告)日：2007-07-05

申请号：US10583696

申请日：2004-12-21

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

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

IPC: C07D305/12 ,  C07C41/03

CPC classification number: C07D323/06 ,  B01D3/146 ,  B01D3/36 ,  Y02P20/127

Abstract: A process for removing trioxane from a mixture I of formaldehyde, trioxane and water, by a) distilling the mixture I in a first distillation stage at a pressure of from 0.1 to 2 bar to obtain a stream II which comprises formaldehyde and a stream III which comprises predominantly trioxane and additionally water and formaldehyde, b) mixing the stream III with a recycle stream VII which comprises predominantly trioxane and additionally water and formaldehyde to obtain a stream IIIa which comprises predominantly trioxane and additionally water and formaldehyde, c) distilling the stream IIIa, if appropriate after removing low boilers from the stream III or IIIa in a further distillation stage, in a second distillation stage at a pressure of from 0.2 to 10 bar, the pressure in the second distillation stage being at least 0.1 bar higher than the pressure in the first distillation stage, to obtain a stream IV of trioxane and a stream V which comprises predominantly trioxane and additionally water and formaldehyde, d) distilling the stream V in a third distillation stage at a pressure of from 0.1 to 4 bar to obtain a stream VI which comprises predominantly water and additionally formaldehyde, and the recycle stream VII which comprises predominantly trioxane and additionally water and formaldehyde, e) if appropriate, distilling the stream VI in a fourth distillation stage to obtain a stream VIII which comprises predominantly water, and a stream IX which comprises predominantly formaldehyde.

Abstract translation: 一种从甲醛，三恶烷和水的混合物I中除去三恶烷的方法，通过以下步骤a）在0.1至2巴的压力下在第一蒸馏阶段中蒸馏混合物I以获得包含甲醛和流III的流II 主要包含三恶烷，另外还含有水和甲醛，b）将流III与主要包含三恶烷，另外含有水和甲醛的再循环流VII混合，得到主要含有三恶烷，另外含有水和甲醛的流IIIa，c）蒸馏流IIIa 如果适当，则在进一步蒸馏阶段从流III或IIIa除去低锅炉后，在0.2至10巴的压力的第二蒸馏阶段中，第二蒸馏阶段中的压力比压力高至少0.1巴 在第一蒸馏阶段，获得三恶烷的流IV和主要包含三恶烷并另外包含的流V 和d）在0.1至4巴的压力下在第三蒸馏阶段中蒸馏物流V以获得主要包含水和另外甲醛的物流VI，以及主要包含三恶烷和另外的水的再循环流VII，以及 甲醛，e）如果合适，在第四蒸馏阶段中蒸馏物流VI以获得主要包含水的物流VIII和主要包含甲醛的物流IX。

公开(公告)号：US20070106096A1

公开(公告)日：2007-05-10

申请号：US10547733

申请日：2004-03-03

Applicant: Eckhard Stroefer ,  Neven Lang ,  Ute Lichtfers ,  Ulrich Steinbrenner ,  Hans Hasse

Inventor： Eckhard Stroefer ,  Neven Lang ,  Ute Lichtfers ,  Ulrich Steinbrenner ,  Hans Hasse

IPC: C07C41/03

CPC classification number: B01D1/225 ,  B01D1/305 ,  C08G2/08 ,  C08G2/24

Abstract: A liquid mixture comprising at least one readily volatile and at least one sparingly volatile component is separated in a film evaporator by a process in which (i) a continuous stream of a liquid starting material mixture is provided, (ii) a liquid film is produced from the continuous stream and is brought into contact with a heat exchange surface of the Mm evaporator, (ii) the liquid film is partly evaporated, a gas stream enriched with the at least one readily volatile component and a liquid stream enriched with the at least one sparingly volatile component being obtained, wherein (iv) the heat exchange surface is coated with a catalytically active material which (v) catalyzes, in the liquid film, a chemical reaction in which at least one readily volatile component is formed.

Abstract translation: 包含至少一种容易挥发的和至少一种微量挥发性组分的液体混合物在膜蒸发器中通过以下方法分离，其中（i）提供液体原料混合物的连续流，（ii）产生液膜 从所述连续流中并与所述膜蒸发器的热交换表面接触，（ii）所述液膜部分蒸发，富含所述至少一种易挥发组分的气流和至少富含至少 获得一种微量挥发性组分，其中（iv）热交换表面涂覆有催化活性材料，该催化活性材料（v）在液膜中催化形成至少一种容易挥发的组分的化学反应。

公开(公告)号：US20060211841A1

公开(公告)日：2006-09-21

申请号：US10547732

申请日：2004-03-04

Applicant: Eckhard Stroefer ,  Neven Lang ,  Hans Hasse ,  Thomas Grützner ,  Michael Ott

Inventor： Eckhard Stroefer ,  Neven Lang ,  Hans Hasse ,  Thomas Grützner ,  Michael Ott

IPC: C08G14/02 ,  C08G8/04

CPC classification number: C07C45/002 ,  C07C45/82 ,  C07C47/04

Abstract: Process for preparing high-concentration formaldehyde solutions having a CH2O content of ≧50% by weight from an aqueous formaldehyde solution having a lower CH2O content by evaporation of part of this solution (partial evaporation), in which the aqueous formaldehyde solution is heated to an evaporation temperature T at which the gas phase becomes enriched in water relative to the liquid phase and the gas phase formed is taken off continuously or discontinuously, wherein the evaporation temperature T obeys the relationship: T[° C.]

Abstract translation: 通过蒸发具有较低CH 2 O 2含量的甲醛水溶液制备CH 2 O 2含量> 50重量％的高浓度甲醛溶液的方法 该部分溶液（部分蒸发），其中甲醛水溶液被加热到气相相对于液相富集水的蒸发温度T，形成的气相连续或不连续地取出，其中 蒸发温度T遵循以下关系：<？in-line-formula description =“In-line Formulas”end =“lead”？> T [°C。] <°C] （c）= A + Bx（c / 100）+ Cx（c / 100） ） ^{2 + Dx（c / 100）3和A = + 68.759，B = + 124.77，C = -12.851，D = -10.095，其中c是瞬时 蒸发期间甲醛水溶液的CH 2 O 2 O含量为重量百分比，为20〜99％ ht。}

公开(公告)号：US08530678B2

公开(公告)日：2013-09-10

申请号：US11665840

申请日：2005-10-20

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

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

IPC: C07D323/06

CPC classification number: C07D323/06

Abstract: 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.

Abstract translation: 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

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

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

IPC: C07D323/06

CPC classification number: C07D323/06 ,  Y02P20/125

Abstract: 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.

Abstract translation: 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

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

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

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

CPC classification number: C08G2/10 ,  C07D317/12 ,  C07D323/06 ,  C08G2/20 ,  Y02P20/127 ,  Y02P20/582

Abstract: 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.

Abstract translation: 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

Applicant: Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer

Inventor： Markus Siegert ,  Neven Lang ,  Eckhard Stroefer ,  Achim Stammer

IPC: C07D317/12

CPC classification number: C07D317/12 ,  Y02P20/127

Abstract: 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.

Abstract translation: 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。

公开(公告)号：US20080234459A1

公开(公告)日：2008-09-25

申请号：US12064893

申请日：2006-08-25

Applicant: Neven Lang ,  Knut Zollner ,  Achim Stammer ,  Elmar Stockelmann

Inventor： Neven Lang ,  Knut Zollner ,  Achim Stammer ,  Elmar Stockelmann

IPC: C08G65/08

CPC classification number: C08G2/10 ,  C07D323/06 ,  C08G2/28 ,  Y02P20/582

Abstract: A process for preparing polyoxymethylene homopolymers or copolymers by homopolymerization or copolymerization of trioxane or additionally of suitable comonomers, in which trioxane which still comprises residual monomers is firstly prepared in a monomer plant and is degassed in one or more stages to give one or more vapor streams (13, 14) which are, if appropriate, fed to a condenser (K) in which the condensable fractions of these vapor streams are condensed to give a condensate (15) which is recycled to the polymerization reactor (P) and one or more gaseous, formaldehyde-comprising streams (16) and also a partially degassed polyoxymethylene homopolymer or copolymer (17) which is fed to an extruder (E) or kneader and is mixed with customary additives and processing aids in this to give a polymer melt (19) and extraction of a formaldehyde-comprising extruder or kneader offgas (18) from the extruder (E) or kneader, wherein the formaldehyde-comprising secondary streams (14, 16, 18) from the polymer plant are recycled directly without addition of auxiliaries to the monomer plant, is proposed

Abstract translation: 通过三恶烷或另外合适的共聚单体的均聚或共聚制备聚甲醛均聚物或共聚物的方法，其中仍然包含残余单体的三恶烷首先在单体植物中制备，并在一个或多个阶段中脱气以产生一种或多种蒸气流 （13,14），如果合适的话，它们被供给到冷凝器（K），在该冷凝器（K）中这些蒸汽流的可冷凝馏分被冷凝，得到一个冷凝物（15），其被循环到聚合反应器（P）和一个或多个 气态的含甲醛的物流（16），以及部分脱气的聚甲醛均聚物或共聚物（17），其被输送到挤出机（E）或捏合机中，并与常规添加剂和加工助剂混合，得到聚合物熔体（19 ）和从挤出机（E）或捏合机中提取含甲醛的挤出机或捏合机废气（18），其中含甲醛的二次流（14,16 ，18）从聚合物植物中直接回收而不添加助剂到单体植物

公开(公告)号：US07414159B2

公开(公告)日：2008-08-19

申请号：US10547733

申请日：2004-03-03

Applicant: Eckhard Stroefer ,  Neven Lang ,  Ute Lichtfers ,  Ulrich Steinbrenner ,  Hans Hasse

Inventor： Eckhard Stroefer ,  Neven Lang ,  Ute Lichtfers ,  Ulrich Steinbrenner ,  Hans Hasse

IPC: C07C41/18

CPC classification number: B01D1/225 ,  B01D1/305 ,  C08G2/08 ,  C08G2/24

Abstract: A liquid mixture comprising at least one readily volatile and at least one sparingly volatile component is separated in a film evaporator by a process in which (i) a continuous stream of a liquid starting material mixture is provided, (ii) a liquid film is produced from the continuous stream and is brought into contact with a heat exchange surface of the Mm evaporator, (ii) the liquid film is partly evaporated, a gas stream enriched with the at least one readily volatile component and a liquid stream enriched with the at least one sparingly volatile component being obtained, wherein (iv) the heat exchange surface is coated with a catalytically active material which (v) catalyzes, in the liquid film, a chemical reaction in which at least one readily volatile component is formed.

Abstract translation: 包含至少一种容易挥发的和至少一种微量挥发性组分的液体混合物在膜蒸发器中通过以下方法分离，其中（i）提供液体原料混合物的连续流，（ii）产生液膜 从所述连续流中并与所述膜蒸发器的热交换表面接触，（ii）所述液膜部分蒸发，富含所述至少一种易挥发组分的气流和至少富含至少 获得一种微量挥发性组分，其中（iv）热交换表面涂覆有催化活性材料，该催化活性材料（v）在液膜中催化形成至少一种容易挥发的组分的化学反应。