公开(公告)号：AU2004308627A1

公开(公告)日：2005-07-14

申请号：AU2004308627

申请日：2004-12-21

Applicant: BASF AG

Inventor： OTT MICHAEL ,  GRUTZNER THOMAS ,  FRIESE THORSTEN ,  LANG NEVEN ,  HASSE HANS ,  SIEGERT MARKUS ,  STAMMER ACHIM ,  BLAGOV SERGEJ ,  STROEFER ECKHARD

IPC: C07D323/06 ,  B01D3/14 ,  B01D3/36

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.

公开(公告)号：AU2006259100B2

公开(公告)日：2011-04-07

申请号：AU2006259100

申请日：2006-06-12

Applicant: BASF AG

Inventor： BLAGOV SERGEJ ,  HASSE HANS ,  STROFER ECKHARD

IPC: C08G2/08 ,  C07C41/56

Abstract: Processes for preparing tri- and tetraoxymethylene glycol dimethyl ether (POMDMEn=3,4) include feeding a reaction mixture of an aqueous formaldehyde solution and methanol into a reactive evaporator and separating into a first low boiler fraction and a first high boiler fraction, recycling the first high boiler fraction into the reactor, feeding the first low boiler fraction into a first distillation column and separating into a second low boiler fraction and a second high boiler fraction, recycling the second high boiler fraction into the reactive evaporator, feeding the second low boiler fraction into a second distillation column and separating into a third low boiler fraction and a third high boiler fraction, feeding the third high boiler fraction into a phase separation apparatus and separating into an aqueous phase and an organic phase, and feeding the organic phase into a third distillation column and separating into a low and high boiler fractions.

公开(公告)号：AU2006310719B2

公开(公告)日：2011-03-31

申请号：AU2006310719

申请日：2006-06-12

Applicant: BASF AG

Inventor： BLAGOV SERGEJ ,  HASSE HANS ,  STROEFER ECKHARD

IPC: C08G65/00

Abstract: Preparing tri-/tetra oxymethylene glycol dimethylether (I) comprises e.g. distilling an aqueous formaldehyde solution and methanol in a reactor to form a reaction mixture containing polyoxy methylene glycol dimethylether (III); distilling the reaction mixture to form a high-boiling fraction (A2) containing e.g. (III); distilling (A2) to form e.g. a low-boiling fraction (A3) having e.g. (I); distilling (A3) to form a high-boiling fraction (A5) having e.g. (I); and distilling (A5) to form an organic phase containing (I). Preparing tri-/tetra oxymethylene glycol dimethylether through the conversion of formaldehyde with methanol and successive distillation of a reaction mixture, comprises: feeding an aqueous formaldehyde solution and methanol in a reactor to form the reaction mixture containing formaldehyde, water, methylene glycol, polyoxymethylene glycol, methanol, hemiformal, methylal and polyoxymethylene glycol dimethylether (III); feeding the reaction mixture into a first distillation column (5) and separating a low-boiling fraction (A1) containing formaldehyde, water, methylene glycol, methanol, methylal and polyoxy methylene glycoldimethylether and a high-boiling fraction (A2) containing formaldehyde, water, methanol, polyoxymethylene glycol, hemiformal and (III); feeding (A2) into a second distillation column (8) and separating a low-boiling fraction (A3) containing formaldehyde, water, methylene glycol, polyoxymethylene glycol, methanol, hemiformal, di-chloroethylene and (I) and a high-boiling containing polyoxymethylene glycol, high-boiling hemiformal and high-boiling polyoxymethylene glycol dimethylether; feeding (A3) and optionally feed-back stream containing formaldehyde, water, methylene glycol and polyoxymethylene glycol into a third distillation column (13) and separating a high volatile fraction (A4) containing formaldehyde, water, methanol, polyoxymethylene glycol, hemiformal and dioxymethylene glycol dimethylether and a high-boiling fraction (A5) containing formaldehyde, water, methylene glycol, polyoxymethylene glycol and (I); feeding (A5) in to a phase separator and separating an aqueous phase containing formaldehyde, water, methylene glycol and polyoxymethyleneglycol and an organic phase containing (I); feeding the organic phase into a fourth distillation column (18) and separating a low-boiling fraction (A6) containing formaldehyde, water, methylene glycol and polyoxymethylene glycol and a high-boiling fraction containing (I); and optionally feeding the aqueous phase in a fifth distillation column (24) and separating a low-boiling fraction (A7) containing formaldehyde, water, methylene glycol and polyoxymethylene glycol and a high-boiling fraction containing water.

公开(公告)号：NZ564178A

公开(公告)日：2009-11-27

申请号：NZ56417806

申请日：2006-06-12

Applicant: BASF AG

Inventor： STROEFER ECKHARD ,  HASSE HANS ,  BLAGOV SERGEJ

IPC: C07C41/56 ,  C08G2/08

Abstract: A process for preparing tri- and tetraoxymethylene glycol dimethyl ether (POMDMEn=3,4) by reacting formaldehyde with methanol and subsequently working up the reaction mixture by distillation is disclosed, wherein the process comprises the steps of: a) feeding aqueous formaldehyde solution and methanol into a reactor and reacting to give a mixture a comprising formaldehyde, water, methylene glycol (MG), polyoxymethylene glycols (MGn>1), methanol, hemiformals (HF), methylal (POMDMEn=1) and polyoxymethylene glycol dimethyl ethers (POMDMEn>1); b) feeding the reaction mixture a into a reactive evaporator and separating into a low boiler fraction b1 comprising formaldehyde, water, methanol, methylene glycol, polyoxymethylene glycols, hemiformals, methylal and polyoxymethylene glycol dimethyl ethers (POMDMEn>1), and a high boiler fraction b2 comprising polyoxymethylene glycols, hemiformals (HFn>1) and polyoxymethylene glycol dimethyl ethers (POMDMEn>3), and recycling the high boiler fraction b2 into the reactor (step a)); c) feeding the low boiler fraction b1 into a first distillation column and separating into a low boiler fraction c1 comprising formaldehyde, water, methylene glycol, methanol, hemiformals, methylal, di-, tri- and tetraoxymethylene glycol dimethyl ether (POMDMEn=2,3,4), and a high boiler fraction c2 comprising polyoxymethylene glycols, high-boiling hemiformals (HFn>1) and high-boiling polyoxymethylene glycol dimethyl ethers (POMDMEn>4), and recycling the high boiler fraction c2 into the reactive evaporator (step b)); d) feeding the low boiler fraction c1 into a second distillation column and separating into a low boiler fraction d1 comprising formaldehyde, water, methanol, polyoxymethylene glycols, hemiformals, methylal and dioxymethylene glycol dimethyl ether methylene glycol, polyoxymethylene glycols, tri- and tetraoxymethylene glycol dimethyl ether (POMDMEn=3,4); e) feeding the high boiler fraction d2 into a phase separation apparatus and separating into an aqueous phase e1 substantially consisting of formaldehyde, water, methylene glycol and polyoxymethylene glycols, and an organic phase e2 comprising tri- and tetraoxymethylene glycol dimethyl ether (POMDMEn=3,4); f) feeding the organic phase e2 into a third distillation column and separating into a low boiler fraction f1 substantially consisting of formaldehyde, water, methylene glycol and polyoxymethylene glycols, and a high boiler fraction f2 substantially consisting of tri- and tetraoxymethylene glycol dimethyl ether (POMDMEn=3,4); and g) optionally feeding the aqueous phase e1 into a fourth distillation column and separating into a low boiler fraction g1 substantially consisting of formaldehyde, water, methylene glycol and polyoxymethylene glycols, and a high boiler fraction substantially consisting of water.

公开(公告)号：NZ563490A

公开(公告)日：2009-11-27

申请号：NZ56349006

申请日：2006-06-12

Applicant: BASF AG

Inventor： STROFER ECKHARD ,  SCHELLING HEINER ,  HASSE HANS ,  BLAGOV SERGEJ

IPC: C07C41/50 ,  C07C43/30

Abstract: A process for preparing polyoxymethylene dialkyl ethers of formula: H2m+1CmO(CH2O)nCmH2m+1 where n is 2 to 10, m independently is 1 or 2 is disclosed, in which a dialkyl ether selected from dimethyl ether, methyl ethyl ether or diethyl ether and trioxane are fed into a reactor and reacted in the presence of an acid catalyst, whereby the amount of water introduced into the reaction mixture with the dialkyl ether, trioxane and/or the catalyst is less than 1 % by weight based on the reaction mixture.

公开(公告)号：MX2008001005A

公开(公告)日：2008-03-25

申请号：MX2008001005

申请日：2006-08-04

Applicant: BASF AG

Inventor： STROEFER ECKHARD ,  HASSE HANS ,  LANG NEVEN ,  STAMMER ACHIM ,  FRIESE THORSTEN ,  SIEGERT MARKUS ,  GRUTZNER THOMAS ,  BLAGOV SERGEJ

IPC: C07D323/06

Abstract: La invencion se relaciona con un proceso integrado para prepara trioxano de formaldehido en el que una corriente A1 que comprende agua y formaldehido y una corriente B2 de reciclado que consiste substancialmente de agua y formaldehido se alimentan a un reactor de sintesis de trioxano en el que el formaldehido se convierte en trioxano para obtener una corriente A2 de producto que comprende trioxano, agua y formaldehido; la corriente A2 se alimenta a una primera columna de destilacion y se destila a una presion en la escala de 0.1 a 2.5 bar para obtener una corriente B1 enriquecida en trioxano, y la corriente B2 que consiste substancialmente de agua y formaldehido; la corriente B1 y la corriente D1 de reciclado que comprende trioxano, agua y formaldehido se alimentan a una segunda columna de destilacion y se destilan a una presion en la escala de 0.2 a 17.5 bar para obtener una corriente C2 de producto que consiste substancialmente detrioxano, y una corriente C1 que comprende trioxano, agua y formaldehido; la corriente C1 se alimenta a una tercera columna de destilacion y se destila a una presion en la escala de 0.1 a 2.5 bar para obtener la corriente D1 de reciclado que comprende trioxano, agua y formaldehido, y una corriente D2 que consiste substancialmente de agua y formaldehido. (Figura 1).

公开(公告)号：MX2008001002A

公开(公告)日：2008-03-25

申请号：MX2008001002

申请日：2006-08-01

Applicant: BASF AG

Inventor： STROFER ECKHARD ,  HASSE HANS ,  LANG NEVEN ,  STAMMER ACHIM ,  FRIESE THORSTEN ,  SIEGERT MARKUS ,  GRUTZNER THOMAS ,  BLAGOV SERGEJ

IPC: C07D323/06

Abstract: La invencion se relaciona con un proceso integrado para preparar trioxano a partir de formaldehido en el que, en un primer paso, una corriente A1 que comprende agua y formaldehido y una corriente B2 de reciclado que consiste substancialmente de agua y formaldehido se alimentan a un reactor de sintesis de trioxano en el que el formaldehido se convierte en trioxano para obtener una corriente A2 de producto que comprende trioxano, agua y formaldehido. La corriente A2 y la corriente D1 de reciclado que comprende trioxano, agua y formaldehido se alimentan a una primera columna de destilacion y se destilan a una presion en la escala de 0.1 a 2.5 bar para obtener una corriente B1 enriquecida en trioxano, y la corriente B2 que consiste substancialmente de agua y formaldehido. La corriente B1 se alimenta a una segunda columna de destilacion y se destila a una presion en la escala de 0.2 a 17.-5 bar para obtener una corriente C2 de producto que consiste substancialmente de trioxano, y una corriente C1 que comprende trioxano, agua y formaldehido. La corriente C1 se alimenta a una tercer acolumna de destilacion y se destila a una presion en la escala de 1 a 10 bar para obtener la corriente D1 de reciclado que comprende trioxano, agua y formaldehido, y una corriente D2 que consiste substancialmente de agua.

公开(公告)号：MX2007014949A

公开(公告)日：2008-02-15

申请号：MX2007014949

申请日：2006-06-12

Applicant: BASF AG

Inventor： STROEFER ECKHARD ,  HASSE HANS ,  BLAGOV SERGEJ

IPC: C08G65/00

Abstract: Un proceso para preparar eter dimetilico de tri- y tetraoximetilenglicol (POMDMEn=3,4) haciendo reaccionar formaldehido con metanol y subsecuentemente trabajar la mezcla de reaccion mediante destilacion, que comprende los pasos de: a) alimentar solucion de formaldehido acuosa y metanol hacia un reactor y hacer reaccionar para proporcionar una mezcla que comprende formaldehido, agua, metilenglicol (MG), polioximetilenglicoles (MGn>1), metanol, hemiformales (HF), metilal (POMDMEn=1) y esteres dimetilicos de polioximetilenglicol (POMDMEn>1); b) alimentar la mezcla de reaccion a una primera columna de destilacion y separar en una fraccion b1 de ebullidor bajo y una fraccion b2 de ebullidor alto que comprende formaldehido, agua, metanol, polioximetilenglicoles, hemiformales y esteres dimetilicos de polioximetilenglicol (POMDMEn>1); c) alimentar la fraccion b2 de ebullidor alto en una segunda columna de destilacion y separar hacia una fraccion c1 de ebullidor bajo que comprende formaldehido, agua, metilenglicol, polioximetilenglicoles, metanol, hemiformales, y eter dimetailico de di-, t6ri-y tetraoximetilenglicol (POMDMEn=2,3,4), y una fraccion c2 de ebullidor alto; d) alimentar la fraccion c1 de ebullidor bajo a un tercera columna de destilacion y separar en una fraccion d1 de ebullidor bajo y una fraccion d2 de ebullidor alto que consiste substancialmente de formaldehido, agua, metilenglicol, polioximetilenglicoles, eter dimetilico de tri- y tetraoximetilenglicol (POMDMEn=3,4); e) alimentar la fraccion d2 de ebullidor alto a un aparato de separacion de fase y separar en una fase e1 acuosa que consiste substancialmente de formaldehido, agua, metilenglicol y polioximetilenglicoles, y una fase e2 organica que comprende eter dimetilico de tri- y tetraoximetlenglicol (POMDMEn=3,4); f) alimentar la fase e2 organica en una cuarta columna de destilacion y separar en una fraccion f1 de ebullidor bajo que consiste substancialmente de formaldehido, agua, metilenglicol y polioximetilenglicoles, y una fraccion f2 de ebullidor alto que consiste substancialmente de eter dimetilico de tri- y tetraoximetilenglicol (POMDMEn=3,4).

公开(公告)号：NO20076301L

公开(公告)日：2008-01-14

申请号：NO20076301

申请日：2007-12-07

Applicant: BASF AG

Inventor： STROFER ECKHARD ,  HASSE HANS ,  BLAGOV SERGEJ

IPC: C08G2/08 ,  C07C41/56

Abstract: Processes for preparing tri- and tetraoxymethylene glycol dimethyl ether (POMDMEn=3,4) include feeding a reaction mixture of an aqueous formaldehyde solution and methanol into a reactive evaporator and separating into a first low boiler fraction and a first high boiler fraction, recycling the first high boiler fraction into the reactor, feeding the first low boiler fraction into a first distillation column and separating into a second low boiler fraction and a second high boiler fraction, recycling the second high boiler fraction into the reactive evaporator, feeding the second low boiler fraction into a second distillation column and separating into a third low boiler fraction and a third high boiler fraction, feeding the third high boiler fraction into a phase separation apparatus and separating into an aqueous phase and an organic phase, and feeding the organic phase into a third distillation column and separating into a low and high boiler fractions.

公开(公告)号：NO20076065L

公开(公告)日：2008-01-14

申请号：NO20076065

申请日：2007-11-26

Applicant: BASF AG

Inventor： HASSE HANS ,  STROEFER ECKHARD ,  BLAGOV SERGEJ

IPC: C08G65/00 ,  C07C41/56 ,  C08G2/08

Abstract: Preparing tri-/tetra oxymethylene glycol dimethylether (I) comprises e.g. distilling an aqueous formaldehyde solution and methanol in a reactor to form a reaction mixture containing polyoxy methylene glycol dimethylether (III); distilling the reaction mixture to form a high-boiling fraction (A2) containing e.g. (III); distilling (A2) to form e.g. a low-boiling fraction (A3) having e.g. (I); distilling (A3) to form a high-boiling fraction (A5) having e.g. (I); and distilling (A5) to form an organic phase containing (I). Preparing tri-/tetra oxymethylene glycol dimethylether through the conversion of formaldehyde with methanol and successive distillation of a reaction mixture, comprises: feeding an aqueous formaldehyde solution and methanol in a reactor to form the reaction mixture containing formaldehyde, water, methylene glycol, polyoxymethylene glycol, methanol, hemiformal, methylal and polyoxymethylene glycol dimethylether (III); feeding the reaction mixture into a first distillation column (5) and separating a low-boiling fraction (A1) containing formaldehyde, water, methylene glycol, methanol, methylal and polyoxy methylene glycoldimethylether and a high-boiling fraction (A2) containing formaldehyde, water, methanol, polyoxymethylene glycol, hemiformal and (III); feeding (A2) into a second distillation column (8) and separating a low-boiling fraction (A3) containing formaldehyde, water, methylene glycol, polyoxymethylene glycol, methanol, hemiformal, di-chloroethylene and (I) and a high-boiling containing polyoxymethylene glycol, high-boiling hemiformal and high-boiling polyoxymethylene glycol dimethylether; feeding (A3) and optionally feed-back stream containing formaldehyde, water, methylene glycol and polyoxymethylene glycol into a third distillation column (13) and separating a high volatile fraction (A4) containing formaldehyde, water, methanol, polyoxymethylene glycol, hemiformal and dioxymethylene glycol dimethylether and a high-boiling fraction (A5) containing formaldehyde, water, methylene glycol, polyoxymethylene glycol and (I); feeding (A5) in to a phase separator and separating an aqueous phase containing formaldehyde, water, methylene glycol and polyoxymethyleneglycol and an organic phase containing (I); feeding the organic phase into a fourth distillation column (18) and separating a low-boiling fraction (A6) containing formaldehyde, water, methylene glycol and polyoxymethylene glycol and a high-boiling fraction containing (I); and optionally feeding the aqueous phase in a fifth distillation column (24) and separating a low-boiling fraction (A7) containing formaldehyde, water, methylene glycol and polyoxymethylene glycol and a high-boiling fraction containing water.