肟交换法制备乙醛肟工艺的研究  

Study on Preparation of Acetaldoxime by Oxime Exchange

作　　者：刘梓良 韩宇莹 王双 王传兴[1] Liu Ziliang;Han Yuying;Wang Shuang;Wang Chuanxing(Chemical Engineering Institute,Qingdao University of Science and Technology,Qingdao Shandong 266000,China)

机构地区：[1]青岛科技大学化工学院,山东青岛266000

出　　处：《石油化工高等学校学报》2021年第6期7-15,共9页Journal of Petrochemical Universities

基　　金：山东省腐蚀科学重点实验室开放课题(KLCS201911)。

摘　　要：肟交换法是一种制备乙醛肟的新兴工艺,但反应过程存在乙醛肟易被空气氧化等问题,且反应液中存在多组共沸物,分离提纯得到高纯度的乙醛肟较为困难。以丁酮肟为原料,通过向反应器内充入0.2 MPa的氮气,有效避免了乙醛肟氧化与原料乙醛、丁酮肟的挥发,乙醛肟反应选择性达96.12%。开发了产物的提纯工艺,通过AspenPlus模拟,初步确定减压精馏分离反应液的基本流程,考察了压力、塔板数、回流比、进料位置等操作参数对分离过程的影响。在此基础上,依据模拟确定的操作参数进行实验,确定最优分离提纯工艺,得到纯度为95.33%的乙醛肟产品,收率可达94.31%。本研究可为肟交换法制备乙醛肟的工业化提供一定的指导。Oxime exchange is a novel process preparing acetaldehyde oxime,but some disadvantages in the reaction process also exist,such as easily oxidized acetaldoxime by air,many azeotropes in the reaction solution,and hardly separated and purified acetaldoxime.The oxidation of acetaldehyde oxime and volatilization of acetaldehyde and butanone oxime were avoided using 0.2 MPa nitrogen as protective gas during the reaction process.The selectivity of acetaldehyde oxime is 96.12%.Moreover,an effective purification process of the product was developed.Firstly,the basic process of separation of reaction liquid by vacuum distillation was simulated by Aspen plus.The influences of pressure,plate number,reflux ratio and feed position on the separation process were investigated.According to the operating parameters of simulation,the optimum separation and purification process in actual reaction were determined.In this condition,the purity of the resulting acetaldoxime is 95.33%with the yield of 94.31%.This work could provide guidance for the industrialization of acetaldehyde oxime by oxime exchange method.

关 键 词：乙醛肟 肟交换法 氮气 AspenPlus模拟 减压精馏 

分 类 号：TQ224.1[化学工程—有机化工]