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林产化学与工业

林产化学与工业 ›› 2008, Vol. 28 ›› Issue (04): 34-38.

• 论文 • 上一篇    下一篇

酸性离子液体催化合成乙酸龙脑酯

季开慧1, 刘仕伟2, 解从霞3, 于世涛1, 刘福胜1, 周光强1   

  1. 1. 青岛科技大学化工学院, 山东青岛, 266042;2. 中国林业科学研究院林产化学工业研究所, 国家林业局林产化学工程重点开放性实验室, 江苏南京, 210042;3. 青岛科技大学化学与分子工程学院, 山东青岛, 266042
  • 收稿日期:2007-09-11 修回日期:1900-01-01 出版日期:2008-08-30 发布日期:2008-08-30
  • 通讯作者: 于世涛,教授,博士生导师,主要从事催化、精细化工及林产化工方面的研究;E-mail:yushitaoqust@126.com。

Synthesis of Bornyl Acetate from α-Pinene Catalyzed by Acidic Ionic Liquid

JI Kai-hui1, LIU Shi-wei2, XIE Cong-xia3, YU Shi-tao1, LIU Fu-sheng1, ZHOU Guang-qiang1   

  1. 1. College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China;2. Institute of Chemical Industry of Forest Products, CAF;Key and Open Lab.on Forest Chemical Engineering, SFA, Nanjing 210042, China;3. College of Chemistry and Molecular Engineering, Qingdao University of Science and Technology, Qingdao 266042, China
  • Received:2007-09-11 Revised:1900-01-01 Online:2008-08-30 Published:2008-08-30

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摘要： 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):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9.90%,乙酸龙脑酯选择性4.07%.并对催化体系的重复使用性进行了考察,重复使用次时,α-蒎烯转化率仍达87.4%,乙酸龙脑酯选择性40.6%.

关键词: α-蒎烯, 酸性离子液体, 酯化反应, 催化

Abstract: An acidic ionic liquid, namely (3-sulfonyl)propyltriethylamine hydrosulfate[HSO3-(CH2)3N(C2H5)3HSO4 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)3CH2SO3HSO4-ClCH2COOH 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(α-pinene):n[N(Et)3(CH2)3SO3H]HSO4:n(chloroacetic acid):n(acetic acid) 5:0.6:5:14,reaction temperature 30℃, reaction time 10h. 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%.

Key words: α-pinene, acidic ionic liquid, esterification, catalysis

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