水溶液法合成2,3,4-三羟基苯甲酸的响应面优化

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

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。

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 and1H NMR spectra.