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林产化学与工业

林产化学与工业 ›› 2013, Vol. 33 ›› Issue (5): 88-92.doi: 10.3969/j.issn.0253-2417.2013.05.017

• 1研究报告 • 上一篇    下一篇

微波辐照法固体碱合成假性紫罗兰酮

赵扬1, 陆强1, 罗金岳1,2   

  1. 1. 南京林业大学 化学工程学院, 江苏 南京 210037;2. 江苏省生物质 绿色燃料与化学品重点实验室, 江苏 南京 210037
  • 收稿日期:2012-09-10 修回日期:1900-01-01 出版日期:2013-10-30 发布日期:2013-10-30
  • 通讯作者: 罗金岳,男,教授,硕士生导师,主要研究方向为林产化学加工;E-mail:luojinyue@njfu.com.cn。

Synthesis of Pseudoionone Catalyzed by Solid Base under Microwave Irradiation

ZHAO Yang1, LU Qiang1, LUO Jin-yue1,2   

  1. 1. College of Chemical Engineering, Nanjing Forestry University, Nanjing 210037, China;2. Jiangsu Key Lab of Biomass-based Green Fuels and Chemicals, Nanjing 210037, China
  • Received:2012-09-10 Revised:1900-01-01 Online:2013-10-30 Published:2013-10-30

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摘要： 以柠檬醛和丙酮为原料,在微波辐照下,合成假性紫罗兰酮。采用红外光谱(FT-IR)、气相色谱(GC-MS)和核磁共振(1H NMR)等手段对产物进行了表征,确定了产物结构。探讨了催化剂种类、催化剂用量、反应温度、反应时间、微波功率以及反应物物质的量对假性紫罗兰酮得率的影响,得到适宜的工艺条件为：柠檬醛 0.1 mol,以NaOH/KOH(物质的量1:1)为催化剂,n(柠檬醛):n(丙酮):n(催化剂)1:8:0.1,微波功率 400 W,反应时间 2 h,反应温度 50℃。在上述条件下,产物得率为 93.4%。微波辐照法较传统方法大大缩短了反应时间。

关键词: 微波辐照法, 假紫罗兰酮, 固体碱

Abstract: Pseudoionone was synthesized by citral and acetone under microwave. The structure of pseudoionone was identified by IR, GC-MS and 1H NMR. Effects of different types of catalysts, catalysts' dosage, reaction temperature, reaction time, microwave power and molar ratio of raw materials on the yield of product were discussed. The optimum reaction conditions were：NaOH/KOH (1:1) mixture as catalyst, n(citral):n(acetone):n(catalyst) 1:8:0.1,microwave power 400 W, reaction time 2 h and reaction temperature 50℃. Under these conditions, the yield of product reached 93.4%. The reaction time is much shorter under microwave irradiation than that under traditional method.

Key words: microwave irradiation, pseudoionone, solid base

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