制备了7种酸功能化离子液体,分别将其与氯乙酸组成复合催化体系用于催化α-蒎烯一步合成乙酸松油酯,筛选出一种催化效果较佳的离子液体[HS03-pmim]H2PO4,并用FT-IR、^1HNMR和^13CNMR对其进行了表征。考察影响反应的主要因素,确定了较佳的反应条件:n(α-蒎烯):n([HSO3-pmim]H2P04):n(氯乙酸):n(乙酸)=5:0.9:5:14,反应温度40℃,反应时间10h。在此条件下,α-蒎烯转化率为85.6%,乙酸松油酯质量分数为36.0%。该催化体系可重复使用,重复使用5次时,α-蒎烯转化率为83.5%,乙酸松油酯质量分数仍达33.7%。
Seven acidic functional ionic liquids were prepared and used as catalysts in α- pinene esterification. A suitable ionic liquid [HSO3-pmim] H2 PO4 was obtained and characterized by FT-IR, ^1H NMR and ^13C NMR. The influences of factors on a-pinene esterification results were investigated and the obtained optimum conditions were n(α-pinene) : n([HSO3-pmim]H2PO4) : n(chloroactic acid) : n(acetic'acid)=5 : 0. 9 : 5 : 14,reaction temperature 40℃ and reaction time 10 h. Under above conditions, the con- version of α-pinene was 85.6% and the selectivity of terpinyl acetate was 36.0%. When the composite catalytic system was reused for 5 times, a-pinene conversion and selectivity of terpinyl acetate were still 83.5% and 33.7% respectively.