全文下载:2012040345
戚春杰a, 李露a*, 刘仕伟a, 于世涛a, 解从霞b
(青岛科技大学 a. 化工学院;b. 化学与分子工程学院, 山东 青岛 266042)
摘要: 以十八胺聚氧乙烯醚类化合物 (AC 1812,AC 1815,AC 1820,AC 1830) 为阳离子,合成了7种长链脂肪胺类酸性离子液体。通过FT-IR 、1H NMR和13C NMR对它们的结构进行了表征,并分别用于催化α-蒎烯一步酯化合成松油醇,其中离子液体十八胺聚氧乙烯醚硫酸盐(\[AC 1815\]+\[HSO4\]-)的催化效果较佳。以该离子液体为例考察影响反应的因素,确定了较佳的反应条件为: n(α-蒎烯) ∶ n(离子液体) ∶ n (氯乙酸) ∶ n(水) =1 ∶ 0.05 ∶ 1 ∶ 5,n(α-蒎烯) = 0.06 mol,反应温度 80 ℃,反应时间 8 h。在此条件下,α-蒎烯转化率为94.0 %,松油醇产率为 59.8 %。该催化剂可重复使用,重复使用 5 次时,α-蒎烯转化率为 91.5 %,松油醇产率仍达 56.8 %。
关键词: α-蒎烯;酸性离子液体;水合;松油醇;催化
中图分类号:TQ 351.4 文献标志码: A
收稿日期:2011-12-28
基金项目: 国家自然科学基金项目(3100275);国家博士后基金项目(20100471496).
作者简介: 戚春杰(1987—),女,硕士研究生.*通信联系人.
Synthesis of Terpinol Catalyzed by Octadecylamine Ethoxylates Ionic Liquid
QI Chun-jiea, LI Lua, LIU Shi-weia, YU Shi-taoa, XIE Cong-xiab
(a. College of Chemical Engineering; b.College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology,Qingdao 266042,China)
Abstract: Seven acidic ionic liquids were synthesized using octadecylamine ethoxylates (AC 1812, AC 1815, AC 1820, AC 1830) as cation and characterized by FT-IR, 1H NMR and 13C NMR. The ionic liquids were used as catalyst in synthesis of terpinol by hydration of α-pinene. It was found that the ionic liquid polyoxyethylene octadecylamine ether sulphate (\[AC 1815\]+\[HSO4\]-) was an excellent catalyst for synthesis of terpinol. Using this ionic liquid as catalyst, the effects of reaction conditions on α-pinene hydration results were investigated. The obtained optimum conditions were n(α-pinene) ∶ n(ionic liquid) ∶ n(chloroactic acid)∶n(water)=1 ∶ 0.05∶ 1 ∶ 5, n(α-pinene)=0.06 mol, reaction temperature 80 ℃ and reaction time 8 h.Under the optimum conditions, the conversion of α-pinene was 94.0 % and the yield of terpinol was 59.8 %. When the catalyst was reused for 5 times,the conversion of α-pinene and the yield of terpinol were still 91.5 % and 56.8 % respectively.
Key words: α-pinene; acidic ionic liquid; hydration; terpinol; catalysis