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酸性离子液体催化合成乙酸龙脑酯

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

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【作者】 季开慧刘仕伟解从霞于世涛刘福胜周光强

【Author】 JI Kai-hui1,LIU Shi-wei2,XIE Cong-xia3,YU Shi-tao1,LIU Fu-sheng1,ZHOU Guang-qiang1(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)

【机构】 青岛科技大学化工学院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青岛科技大学化学与分子工程学院

【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)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%。

【Abstract】 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-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 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 %.

【关键词】 α-蒎烯酸性离子液体酯化反应催化
【Key words】 α-pineneacidic ionic liquidesterificationcatalysis
【基金】 国家自然科学基金(30571463);山东省自然科学基金(Y2005B07)
  • 【文献出处】 林产化学与工业 ,Chemistry and Industry of Forest Products , 编辑部邮箱 ,2008年04期
  • 【分类号】TQ655
  • 【被引频次】6
  • 【下载频次】445
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