催化精馏合成乙酸乙酯的工业试验  

Industrial experimental study of ethyl acetate synthesis via catalytic distillation

作　　者：李柏春[1] 徐敬瑞[1] 李晓红[2] 张昌伟[2] 田淑娜[1] 

机构地区：[1]河北工业大学化工学院,天津300130 [2]天津市普莱特科技发展有限公司,天津300384

出　　处：《化学工程》2011年第7期22-26,共5页Chemical Engineering(China)

基　　金：河北省自然基金资助项目(B2007000021)

摘　　要：以固体酸为催化剂,在中试催化精馏塔中进行了乙酸与乙醇反应制备乙酸乙酯的工业试验,试验塔的精馏段塔径为600 mm,内装陶瓷规整填料,反应精馏段塔径为1 000 mm,内装7层立体催化精馏塔板。采用连续操作,考察了不同的回流比、釜酸质量分数、进料流量对反应和分离过程的影响,同时测定了塔板上气液相质量分数的分布。通过试验得到了适宜的操作条件:当回流比(质量比)为3.5—4.5,釜酸质量分数为60%—80%,进料流量为150—600 L/h时,酯化塔顶中乙酸乙酯质量分数为84%—92%,乙酸质量分数低于0.003%,该催化精馏工艺可长期连续稳定操作,年产乙酸乙酯4 000 t。在此基础上采用Aspen Plus过程模拟软件对该工艺过程进行模拟计算,模拟结果与试验结果吻合较好。The industrial process of synthesizing ethyl acetate by catalytic distillation was studied with solid acid as catalyst,acetic and ethanol as starting materials in a pilot catalytic distillation column.The rectifying section of catalytic distillation column with diameter of 600 mm was packed with ceramic structured packing.The reactive distillation section with a diameter of 1 000 mm was installed with seven solid reactive spray trays.The influence of different reflux ratio,mass fraction of acetic acid at bottom,feed flow rate on reaction and separation processes was tested under continuous operation.At the same time the mass fraction of gas and liquid on the tray was measured.The feasible operation conditions were obtained,such as reflux ratio（mass ratio） 3.5-4.5,the mass fraction 60%-80% of acetic acid at bottom,the feed flow rate 150-600 L/h.Under such conditions the mass fraction of ethyl acetate at the top is 84%-92%,and the mass fraction of acetate acid is under 0.003%.This catalytic distillation process can be continuously operated steadily with an ethyl acetate production capacity of 4 000 t/a.The Aspen Plus was used to simulate the synthesis process of ethyl acetate.The results are in good agreement with experimental ones.

关 键 词：乙酸乙酯 催化精馏 固体酸催化剂 工业试验 

分 类 号：TQ225.241[化学工程—有机化工]