摘要
以醋酸、甲醇为原料,以质子酸离子液体为催化剂和萃取剂,采用反应萃取精馏法制备了醋酸甲酯。考察了质子酸离子液体和配料比、回流比及反应时间对反应萃取精馏的影响。实验结果表明,质子酸离子液体是制备醋酸甲酯的良好催化剂和萃取剂,能消除醋酸甲酯与水或甲醇的共沸点,提高醋酸甲酯的纯度和收率;在3种质子酸离子液体[Hmim]CF3COO,[Hmim]BF4,[Hmim]HSO4中,[Hmim]HSO4(Hmim为N-甲基咪唑)的催化活性最高。反应萃取精馏的最佳工艺条件是:m(HOAc)∶m(CH3OH)∶m([Hmim]HSO4)=100∶50∶1,回流比2.5,反应时间30min。在此条件下,醋酸甲酯的纯度可达99.84%,收率可达98.65%。采用闪蒸的方法可回收醋酸、甲醇及质子酸离子液体,质子酸离子液体可重复使用8次。
Preparation of methyl acetate by reactive and extractive distillation from acetic acid and methanol with Brrnsted acidic ionic liquid as catalyst and extractant was studied. Effects of different Brrnsted acidic ionic liquids on purity and yield of methyl acetate were investigated, and effects of reactant ratio, reflux ratio and reaction time on reactive and extractive distillation were observed. By using [ Hmim] HSO4 （Hmim is N-methylimidazole）, the azeotropic point of methyl acetate-water and the azeotropic point of methyl acetate-methanol disappeared in extractive distillation, and purity and yield to methyl acetate increased. Purity and yield of methyl acetate were 99. 84% and 98.65% respectively when reactant ratio m（HOAc） ： m（CH3OH） ： m（ [Hmim] HSO4） 100 ： 50 ： 1, reflux ratio 2.5 and reaction time 30 min. By flash distillation residue, Brrnsted acidic ionic liquid can be separated from acetic acid and methanol. The acidic ionic liquid [Hmim] HSO4 can be reused for 8 times.
出处
《石油化工》
CAS
CSCD
北大核心
2009年第6期603-607,共5页
Petrochemical Technology
关键词
质子酸离子液体
反应萃取精馏
醋酸
甲醇
醋酸甲酯
酯化反应
Brrnsted acidic ionic liquids
reactive and extractive distillation
acetic acid
methanol
methyl acetate
esterification
作者简介
田敉（1964-），女，重庆市人，大学，讲师，电话15923009563，电邮wkpwkp469@sina．com。
