公开(公告)号：US07414159B2

公开(公告)日：2008-08-19

申请号：US10547733

申请日：2004-03-03

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

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

IPC分类号： C07C41/18

CPC分类号： B01D1/225 ,  B01D1/305 ,  C08G2/08 ,  C08G2/24

摘要： 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.

摘要翻译： 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：US20070106096A1

公开(公告)日：2007-05-10

申请号：US10547733

申请日：2004-03-03

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

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

IPC分类号： C07C41/03

CPC分类号： B01D1/225 ,  B01D1/305 ,  C08G2/08 ,  C08G2/24

摘要： 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.

摘要翻译： 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：US20060185513A1

公开(公告)日：2006-08-24

申请号：US10547440

申请日：2004-03-03

申请人： Eckhard Stroefer ,  Neven Lang ,  Ulrich Steinbrenner ,  Hans Hasse ,  Thomas Grutzner

发明人： Eckhard Stroefer ,  Neven Lang ,  Ulrich Steinbrenner ,  Hans Hasse ,  Thomas Grutzner

IPC分类号： B01D19/00

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蒸发温度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：US07345207B2

公开(公告)日：2008-03-18

申请号：US10547732

申请日：2004-03-04

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

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

IPC分类号： G07C45/78 ,  C08G8/04

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

摘要： 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.]

摘要翻译： 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] <？in-line-formula description =“In-line Formulas”end =“tail”？> <？in-line-formula description =“In-line Formulas”end =“lead”？>其中T < （c）= A + Bx（c / 100）+ Cx（c / 100）2 + Dx（c / 100）3 < line-formula description =“In-line Formulas”end =“tail”？> A = + 68.759，B = + 124.77，C = -12.851，D = -10.095，其中c是瞬时CH 2， / 在蒸发期间甲醛水溶液的重量百分比为20〜99重量％。

公开(公告)号：US20100145079A1

公开(公告)日：2010-06-10

申请号：US12532430

申请日：2008-03-27

申请人： Eckhard Stroefer ,  Neven Lang ,  Markus Siegert ,  Hans Hasse

发明人： Eckhard Stroefer ,  Neven Lang ,  Markus Siegert ,  Hans Hasse

IPC分类号： C07D323/06

CPC分类号： C07D323/06

摘要： 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).

摘要翻译： 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

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

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

IPC分类号： C07D305/12 ,  C07C41/03

CPC分类号： C07D323/06 ,  B01D3/146 ,  B01D3/36 ,  Y02P20/127

摘要： 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.

摘要翻译： 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：US20060211841A1

公开(公告)日：2006-09-21

申请号：US10547732

申请日：2004-03-04

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

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

IPC分类号： C08G14/02 ,  C08G8/04

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

摘要： 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.]

摘要翻译： 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：US20100152466A1

公开(公告)日：2010-06-17

申请号：US12063171

申请日：2006-08-04

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

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

摘要翻译： 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

申请人： Eckhard Stroefer ,  Neven Lang ,  Markus Siegert ,  Hans Hasse

发明人： Eckhard Stroefer ,  Neven Lang ,  Markus Siegert ,  Hans Hasse

IPC分类号： C07D323/06

CPC分类号： C07D323/06

摘要： 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.

摘要翻译： 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：US20080194845A1

公开(公告)日：2008-08-14

申请号：US11997619

申请日：2006-07-19

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, 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).

摘要翻译： 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。