石油炼制与化工 ›› 2024, Vol. 55 ›› Issue (1): 218-225.

• 特约研究报告 • 上一篇    下一篇

以吗啉与环氧乙烷为原料的无催化剂连续快速合成吗啉乙醇工艺研究

吴东鑫,王洪鹏,梁作飞,张利雄   

  1. 南京工业大学化工学院,材料化学工程全国重点实验室
  • 收稿日期:2023-09-18 修回日期:2023-10-14 出版日期:2024-01-12 发布日期:2024-01-15
  • 通讯作者: 张利雄 E-mail:lxzhangnjut@gmail.com

DEVELOPMENT OF RAPID CONTINUOUS CATALYST-FREE SYNTHESIS PROCESS OF MORPHOLINE ETHANOL USING MORPHOLINE AND ETHYLENE OXIDE AS RAW MATERIALS


  • Received:2023-09-18 Revised:2023-10-14 Online:2024-01-12 Published:2024-01-15
  • Contact: Lixiong LiZhang E-mail:lxzhangnjut@gmail.com

摘要: 针对以吗啉和环氧乙烷为原料合成吗啉乙醇的反应路线收率不高、反应时间长、安全性不好和需使用催化剂的问题,在以SIMM-V2微混合器和不锈钢管组成的微通道反应器中,进行了连续快速制备吗啉乙醇的工艺研究,考察了反应温度、停留时间、体系压力、物料配比和流量等因素对产物收率的影响。结果表明:利用该反应器,在无催化剂条件下和更短的反应时间内可获得与釜式反应器相当的收率;产物收率随着反应温度、停留时间、环氧乙烷配比的增加均呈现先升高再降低趋势,且相互之间会有影响;存在一个较宽泛的反应条件操作窗口,即在给定某一个条件时,可以通过调节其他条件获得相同的产物收率。在典型的反应条件下,如温度为150 ℃、吗啉与环氧乙烷摩尔比为1:1.08、停留时间为3 min、总流量为1 mL/min、体系压力为2.5 MPa时,吗啉转化率可达99.55%,吗啉乙醇的选择性为97.1%,远高于釜式反应的结果。

关键词: 吗啉乙醇, 吗啉, 环氧乙烷, 微通道反应器, 强放热反应

Abstract: In order to solve the problems of the synthesis of morpholine ethanol from morpholine and ethylene oxide, such as low yield, long reaction time, poor safety and the use of catalysts, in a microchannel reactor consisting of SIMM-V2 micro-mixer and a stainless steel tube, the continuous and rapid preparation of morpholine ethanol was studied, and the effects of reaction temperature, residence time, system pressure, molar ratio of raw materials and flow rate were investigated. The results showed that the yield of the reactor was almost equal comparable to that of the kettle reactor under the condition of no catalyst and shorter reaction time. With the increase of reaction temperature, residence time, and molar ratio, the yield of the product increased first and then decreased, there was a wide window of reaction conditions, that was, given a certain condition, the other conditions could be adjusted to obtain the same yield. Under typical reaction conditions, such as a temperature of 150 ℃, a morpholine to ethylene oxide molar ratio of 1:1.08, a residence time of 3 min, a total flow rate of 1 mL/min, and a system pressure of 2.5 MPa, the conversion of morpholine could reach 99.55%, and the selectivity of morpholine ethanol was 97.1%, which was much higher than that of the batch reaction.

Key words: morpholine ethanol, morpholine, ethylene oxide, microchannel reactor, strong exothermic reaction