公开(公告)号：EP2032553A1

公开(公告)日：2009-03-11

申请号：EP07730041.6

申请日：2007-06-11

Applicant: BASF SE

Inventor： SIEGERT, Markus ,  LANG, Neven ,  STRÖFER, Eckhard ,  SIGWART, Christoph

IPC: C07D323/06

CPC classification number: C07D323/06 ,  Y02P20/125

Abstract: Integrated method for the preparation of trioxane from formaldehyde, comprising the steps: a) introduction of a feeding flow A1 containing formaldehyde and water and a return flow B3 consisting essentially of formaldehyde and trioxane into a formaldehyde concentration unit, wherein said flows are separated into a formaldehyde-rich flow A2 and a flow A3 consisting essentially of water; b) introduction of a product flow C1, containing trioxane, water, and formaldehyde, a return flow E1 containing trioxane, water, and formaldehyde, and possibly flow A2 into a first low-pressure distillation column, wherein said flows are distilled at a pressure of from 0.1 to 1.5 atmospheres, with a trioxane-enriched flow B1 containing predominantly trioxane, and also water and formaldehyde, a slough removal flow B2 consisting essentially of formaldehyde and water, and the return flow B3 containing predominantly water, and also formaldehyde and trioxane removed as a side removal flow; c) introduction of a slough removal flow B2 and possibly the flow A2 into a trioxane synthesis reactor, wherein said flows are allowed to react, and wherein the flow C1 containing trioxane, water, and formaldehyde is obtained; d) introduction of a flow B1 into a mid-pressure distillation column, wherein said flow is distilled at a pressure of from 1.0 to 3.0 atmospheres, wherein a low boiler stream D1 containing methanol, methylal, and methylformate,and a stream D2 containing predominantly trioxane and also formaldehyde and water are obtained; e) introduction of a stream D2 into a high-pressure distillation column, wherein said stream is distilled at a pressure of from 2.5 to 10.0 atmospheres, wherein the return flow E1 contains trioxane, water, and formaldehyde, and a product flow E2 consisting essentially of trioxane is obtained; wherein flow A2 can be introduced into either the low-pressure distillation column or into the trioxane-35 synthesis reactor, or into both.

Abstract translation: 包括以下步骤：a）将含有甲醛和水的进料流A1和主要由甲醛和三烷组成的回流B3引入甲醛浓缩单元，其中将所述流分离成甲醛 富甲醛流A2和基本上由水组成的流A3; b）将含有三烷，水和甲醛的产物流C1引入含有三烷，水和甲醛的回流E1，并且可能将流A2引入第一低压蒸馏塔中，其中将所述流在压力 用主要含三烷以及水和甲醛的富含三烷的物流B1，主要由甲醛和水组成的撇去物流B2和主要含有水的返回物流B3以及甲醛和三烷 作为侧面去除流去除; c）将脱泥流去除流B2和可能的流A2引入三烷合成反应器中，其中使所述流反应，并且其中获得含有三烷，水和甲醛的流C1; d）将流B1引入中压蒸馏塔中，其中所述流在1.0至3.0大气压的压力下蒸馏，其中含有甲醇，甲缩醛和甲酸甲酯的低沸物流D1和主要含有 三恶烷以及甲醛和水; e）将物流D2引入到高压蒸馏塔中，其中所述物流在2.5至10.0大气压的压力下蒸馏，其中回流E1包含三烷，水和甲醛，产物流E2基本上由 的三恶烷; 其中可将流A2引入低压蒸馏塔或三恶烷-35合成反应器中，或引入两者中。