制备了酸功能化离子液体(3-磺酸基)丙基三乙基铵硫酸氢盐[N(Et)3(CH2)3SO3H]HSO4,并用FT-IR、^1H NMR和^13C NMR对其进行了表征。将其与氯乙酸组成的复合催化体系用于催化α-蒎烯一步酯化反应,详细考察了离子液体用量、反应温度、反应时间、反应物配比等因素对酯化反应的影响,得到了较佳的反应条件:n(α-蒎烯):n[N(Et)3(CH2)3SO3H]HSO4:n(氯乙酸):n(乙酸)5:0.6:5:14,反应温度30℃,反应时间10h。在该条件下α-蒎烯转化率为95.90%,乙酸龙脑酯选择性45.07%。并对催化体系的重复使用性进行了考察,重复使用5次时,α-蒎烯转化率仍达87.4%,乙酸龙脑酯选择性40、6%。
An acidic ionic liquid, namely (3-sulfonyl)propyltriethylamine hydrosulfate [ HSO3-(CH2)3N (C2H5)3 ] HSO4 was prepared and characterized by FT-IR, ^1H NMR and ^13C NMR. Esterification of α-pinene catalyzed over the composite catalytic system of [N(Et)3(CH2)3SO3H ] HSO4-ClCH2 COOH was studied. The influences of reaction factors, such as amount of acidic ionic liquid, reaction temperature, reaction time and proportion of reactants were investigated. The optimum conditions for α-pinene esterification were obtained as follows: n (a-pinene) : n [N (Et)3(CH2)3 S03 H ] HSO4 : n ( chloroacetic acid ) : n ( acetic acid ) 5 : 0.6:5: 14, reaction temperature 30 ℃, reaction time 10 h. Under the above conditions, the conversion of α-pinene was 95.90 % and the selectivity of bornyl ester was 45.07 %. The reusability of the composite catalytic system was investigated. Under the optimum conditions, when the composite catalytic system was repeatedly used for 5 times, α-pinene conversion reached 87.4 % and the selectivity of bornyl ester was 40.6 %. α