公开(公告)号：US20040167359A1

公开(公告)日：2004-08-26

申请号：US10733278

申请日：2003-12-12

Applicant: DEGUSA AG

Inventor： Stefan Leininger ,  Juergen Herwig ,  Martin Roos ,  Georg Oenbrink

IPC: C07C249/04

CPC classification number: C07C249/04 ,  C07C2601/20 ,  C07C251/44

Abstract: An oxime is synthesized by ammoximation of a carbonyl compound. In stage (i) of the process, a carbonyl compound containing 6 to 20 C atoms is reacted with ammonia and hydrogen peroxide in the presence of a) an organic solvent that is a1) at least partly water-soluble, a2) stable under ammoximation conditions, a3) has a boiling point of higher than 100null C. and/or is capable of forming a two-phase azeotrope with water, and b) a titanium-containing heterogeneous catalyst. After the reaction, the catalyst is separated from the reaction mixture. The oxime is crystallized and separated from the reaction mixture. Water is removed from the remaining mother liquor, provided the mother liquor is a two-phase system in which one of the phases is an aqueous phase. Water or a water-containing two-phase azeotrope is distilled off from the mother liquor, while the distillation bottoms and, optionally, the predominantly organic phase of the azeotrope are recycled to stage (i).

Abstract translation: 通过羰基化合物的肟化合成肟。 在该方法的阶段（i）中，在a）至少部分水溶性的有机溶剂存在下，使含有6-20个碳原子的羰基化合物与氨和过氧化氢反应，a2）在氨肟化下稳定 条件a3）的沸点高于100℃，和/或能够与水形成两相共沸物，和b）含钛的非均相催化剂。 反应后，将催化剂与反应混合物分离。 将肟结晶并与反应混合物分离。 如果母液是其中一相是水相的两相系统，则从剩余的母液中除去水。 从母液中蒸馏掉水或含水的两相共沸物，同时将蒸馏塔底物和任选的共沸物的主要有机相再循环至阶段（i）。