Cu-Ni-Co/Al_2O_3气固相催化合成N-甲基吗啉

Synthesis of N-Methylmorpholine over the Catalyst Cu-Ni-Co/Al_2O_3 in the Gas Phase

制备了一系列以Al2O3为载体,含不同活性金属组分的负载型催化剂,其制备过程简单且成本低。以此类催化剂在固定床内由吗啉和甲醇为原料进行气固相接触氨氧化反应制备N-甲基吗啉。考察了不同金属活性组份、反应温度、原料配比、体积空速等因素对反应的影响。经系统的正交优化实验确定了最佳条件,结果表明:当以Cu-Ni-Co/Al2O3型催化剂,醇胺摩尔比为2.2:1,反应体系氢压为0.6MPa,反应温度为190℃,空速为0.18h-1时,N-甲基吗啉的总收率可以达到90%,产品经提纯后纯度可达99%。此外,通过对反应前和失活后的催化剂进行TEM考察发现所制备的催化剂活性组分分散性良好。

A series of catalysts comprising different metal components with Al2O3 as supporter were prepared by impregnation method in this article. N-methylmorpholine was synthesized from morpholine and methanol with the prepared catalysts in the vapor phase through a fixed-bed reactor. The influencing factors,such as different active metal components,reaction temperature,molar ratio of the raw materials and space velocity,were investigated by systematic orthogonal experiments. The results show that when the process is taken on the catalyst of Cu-Ni-Co/Al2O3 with the molar ratio of the raw material （methanol/morpholine） of 2.2：1 and the space velocity of 0.18 h？1 at 190℃ and 0.6 MPa,the yield of N-methylmorpholine could reach 90% with the purity of 99% after purification. The active component dispersal status of the catalysts before reaction and after deactivation was characterized by TEM,and good active component dispersities of the prepared catalysts could be observed.