合成并表征了3种Brφnsted酸性离子液体硫酸三乙基铵盐[Et3NH][HSO4]、磷酸三乙基铵盐[Et3NH][H2PO4]和N-甲基咪唑硫酸盐[HMIM][HSO4],考察了这3种离子液体在催化芳樟醇和乙酸酐酯化反应中的催化活性。结果表明,离子液体[HMIM][HSO4]的催化性能最高,当[HMIM][HSO4]的用量为反应物总质量的10%,n(芳樟醇)∶n(乙酸酐)=1∶2,反应温度90℃,反应时间2h乙酸芳樟酯的产率可达91.4%,选择性为100%。反应结束后,减压脱去过量的酸酐和反应生成的乙酸,离子液体与酯化产物成两相,便于分离与再生。离子液体[HMIM][HSO4]重复使用6次后,乙酸芳樟酯的产率仍可达86.2%。
Three Brφnsted acidic ionic liquids including triethylammonium sulfate([Et3NH][HSO4]),triethylammonium dihydrogen phosphate([Et3NH][H2PO4]) and N-methyl imidazole sulfate([HMIM][HSO4]) were synthesized and characterized.The catalytic activities of the acidic ionic liquids for the synthesis of linalyl acetate were also investigated.The results showed that has the best catalytic activity among them.The yield of linalyl acetate was 91.4% and the selectivity was 100% under the following optimal conditions: amount of 10% on the total mass of reactants,molar ratio of linalyl alcohol to acetic anhydride of 1∶2,temperature of 90 ℃,and reaction time of 2 h.After the reaction,the excessive acetic anhydride and the generation of acetic acid were removed by distillation under reduced pressure,the ionic liquid and esters were then separated to two phases in nature.The above process completed both separation and regeneration of the ionic liquid,and the regenerated ionic liquid was directly used to another new synthesis.When the ionic liquid of was reused 6 times,the yield of linalyl acetate could still reach 86.2%.