反应-共沸精馏合成N-甲酰吗啉

报道了一种将反应精馏和共沸精馏耦合制备N-甲酰吗啉的新工艺,分别确定了工艺的最佳操作条件和理论塔板数。当吗啉和甲酸的进料摩尔比为1.02,以RA-01作为共沸精馏溶剂,溶剂比为8,反应段、精馏段和提馏段理论塔板数分别为5、18和6时,反应精馏实验得到的N-甲酰吗啉平均收率为99.45%。采用闪蒸法提纯N-甲酰吗啉,产物纯度99.96%,总收率99.15%。工艺实验与模拟计算的一致性较好。

SYNTHESIS OF N-FORMYLMORPHOLINE BY REACTIVE-AZEOTROPIC DISTILLATION

A new coupled process consisting of reactive distillation and azeotropic distillation was used for the synthesis of N-formylmorpholine(NFM).The optimal conditions were found by experiments and simulation.When the mole ratio of morpholine to formic acid was 1.02,residence time in reaction section was 3.0 h,volume ratio of circulating solvent to charging rate of formic acid per-hour was 8, the NTP of the reaction,rectification and stripping sections were 5,18 and 6,respectively,with the average yield of NFM being 99.45%.The crude NFM was treated by flash evaporation,and the puri- ty of the product was above 99.96% after treatment.The overall yield of the product was 99.15%. The simulation result of this process is close to the experiment data.