连续管式反应合成N,N-二甲基苯胺及其精制模拟研究

Study on Preparation of N,N-Dimethylaniline by Continuous Tube Reaction and Simulation of Refining

摘要: 本文制备了盐酸和草酸改性的M-Hβ分子筛催化剂，以苯胺和甲醇为原料，M-Hβ分子筛为催化剂进行连续管式反应合成N,N-二甲基苯胺。以苯胺的转化率和N,N-二甲基苯胺的选择性为目标，考察了原料配比、反应温度及空速等因素对合成N,N-二甲基苯胺的影响，然后通过正交试验进一步优化管式反应的条件，确定最佳工艺。采用ASPEN PLUS模拟软件对产物进行连续侧线精馏、萃取精馏及溶剂回收过程的模拟研究，为进一步分离研究提供基础数据。在管式反应最佳工艺条件下，苯胺的转化率达到99%以上，N,N-二甲基苯胺的选择性大于95%；在精制过程的最佳工艺条件下，N,N-二甲基苯胺的质量分数达到99.96%，收率达到99.86%。

Abstract: The M-Hβ molecular sieve catalyst was prepared, N,N-dimethylaniline was prepared by conti-nuous tubular reaction using aniline and methanol as raw materials and M-Hβ molecular sieve as catalyst. Taking the conversion of aniline and the selectivity of N,N-dimethylaniline rate as the examining goal, the effects of mole ratio of raw materials, reaction temperature and liquid hourly space velocity (LHSV) on the reaction were studied, and then the conditions of the tube reaction are further optimized by the orthogonal experiment to determine the optimum synthesis conditions. The ASPEN PLUS simulation software was used to simulate continuous side distillation and extractive distillation, which provided the basic data for further separation research. Under the optimal conditions, the conversion of aniline was more than 99%, and the selectivity of N,N-dimethylaniline was more than 95%, the purity of N,N-dimethylaniline reached 99.96% and the yield reached 99.86%.