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生物质化学工程 ›› 2014, Vol. 48 ›› Issue (3): 36-39.doi: 10.3969/j.issn.1673-5854.2014.03.007

• 研究报告 • 上一篇    下一篇

水溶液法合成2,3,4-三羟基苯甲酸的响应面优化

姜萍1, 胡海渴1, 杜青林2   

  1. 1. 南京林业大学 化学工程学院, 江苏 南京 210037;
    2. 舒城县林业局, 安徽 六安 231300
  • 收稿日期:2014-01-21 出版日期:2014-05-30 发布日期:2014-05-29
  • 作者简介:姜 萍(1969- ),女,黑龙江宜春人,副教授,硕士生导师,主要从事天然产物化学与应用研究;E-mail:cq_cheng@hotmail.com。
  • 基金资助:
    广西林产化学与工程协同创新中心基金项目(2013A03);江苏高校优势学科建设工程资助项目(无编号)

Optimization of Synthesis of 2,3,4-Trihydroxybenzoic Acid with Water by Response Surface Method

JIANG Ping1, HU Hai-ke1, DU Qing-lin2   

  1. 1. College of Chemical Engineering Nanjing Forestry University, Nanjing 210037, China;
    2. Shucheng Forestry, Liuan 231300, China
  • Received:2014-01-21 Online:2014-05-30 Published:2014-05-29

摘要: 以焦性没食子酸为原料与碳酸氢钠反应合成2,3,4-三羟基苯甲酸。在单因素试验的基础上,利用Design-Expert软件响应面优化,并建立反应产品得率的二次多项回归模型,得出2,3,4-三羟基苯甲酸的最佳合成条件。为了实验操作简便,取焦性没食子酸与碳酸氢钠的质量之比1:3,反应温度为90 ℃,反应时间为4.5 h,在此条件下2,3,4-三羟基苯甲酸的得率为37.57%。产品经过显微熔点测定、 FT-IR分析和1H HMR分析,证实为目标产物。

关键词: 焦性没食子酸, 2, 3, 4-三羟基苯甲酸, 响应面, 合成

Abstract: 2,3,4-trihydroxy benzoic was prepared using pyrogallic acid and sodium bicarbonate. On the basis of single factor test,Design-Expert software was used for response surface optimization. A quadratic polynomial regression model and the optimum conditions were obtained. To keep the test simple, the optimum synthesis conditions were as follows: m(pyrogallic acid)/m(sodium bicarbonate)1:3, reaction temperature 90 ℃, reaction time 4.5 h. Under optimal conditions, the yield of 2,3,4-trihydroxybenzoic acid was 37.57%. The final product was confirmed with melting point, FT-IR and 1H NMR spectra.

Key words: pyrogallic acid, 2,3,4-trihydroxybenzoic acid, response surface method, synthesis

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