ResearchonS202一／Zr02solidsuperacidinsynthesisofn—amylacetateundermicrowaveradiation  

Research on S2O^2 8-/ZrO2 solid superacid in synthesis of n-amyl acetate under microwave radiation

作　　者：陶利燕[1] 候鑫[1] 王刚[1] 徐骏[1] 董成[1] 聂沃[1] 曹汉迪[1] 张立庆[1] 

机构地区：[1]浙江科技学院生物与化学工程学院,杭州310023

出　　处：《浙江科技学院学报》2013年第5期329-334,共6页Journal of Zhejiang University of Science and Technology

基　　金：浙江省自然科学基金资助项目（Y404082）;浙江省大学生科技创新活动计划（新苗人才计划）（2011R415025）

摘　　要：采用沉淀一浸渍法制得S2O62 8-／ZrO2固体超强酸，在微波辐射下催化合成乙酸正戊酯。通过单因素实验和正交实验优化了合成的反应条件；采用Hammett指示剂法、BET法、红外光谱、电子透镜技术和x_射线衍射对其进行了表征。实验结果表明，采用最佳制备条件下得到的催化剂在微波辐射下催化合成乙酸正戊酯的最优合成条件为：醇酸摩尔比1．9：1，反应温度135℃，反应时间25min，催化剂用量1．2g，功率500W，收率为97．8％。该工艺具有绿色、安全、操作简单和收率高等优点。The synthesis of n-amyl acetate catalyzed by solid superacid catalyst S2O^2 8-/ZrOz, which was prepared by method of precipitation and impregnation. The single factor experiment and orthogonal experiment was used to optimize the reaction conditions of synthesis. The catalyst were characterized by using Hammett, BET, IR, TEM and XRD. The optimal condition for synthesis of n-amyl acetate by using the best catalyst under microwave radiation are n-pentanol/acetic acid 1.9 ： 1, reaction temperature 135 ℃, reaction time 25 min, amount of catalyst 1.2 g, radiation power 550 W, yield 97.8%. This approach is green, safe, high yield and easy to operate for production of n-amyl acetate.

关 键 词：固体超强酸 乙酸正戊酯 催化酯化 微波合成 正交设计 表征 

分 类 号：O643.32[理学—物理化学] TQ225.241[理学—化学]