在乙酸乙酯合成的实验教学中,通常使用阿贝折射仪分析产物纯度,误差较大.在本研究中,采用气相色谱内标校正因子法和面积归一化法来测定乙酸乙酯的含量,我们发现内标校正因子法测量的结果准确度高,且操作简单.合成条件为:乙醇、乙酸摩尔比为 1.5∶1,浓硫酸的添加量为2 mL.通过正交实验设计优化乙酸乙酯纯化过程,得到最佳纯化条件:20 mL饱和氯化钠溶液、40 mL 100%饱和氯化钙溶液(每次20 mL)、1.8 g无水硫酸镁.在此条件下提纯,我们将实验教学中普遍合成产率55%提高到80.70%,且纯度高达 96.69%,实现了乙酸乙酯合成产率和纯度的双向提升.
Improving the Yield and Purity of Ethyl Acetate Synthesis by Orthogonal Design
In the experimental teaching of ethyl acetate synthesis,Abbe refractometer was usually used to analyze the purity of the product,and the error was large.In this study,the content of ethyl acetate was determined by gas chromatography internal standard correction factor method and area normalization method.We found that the internal standard correction factor method had high accuracy and simple operation.The synthesis conditions were as follows:the molar ratio of ethanol to acetic acid was 1.5∶1,and the amount of concentrated sulfuric acid was 2 mL.The purification process of ethyl acetate was optimized by orthogonal experimental design,and the best purification conditions were obtained:20 mL saturated sodium chloride solution,40 mL 100%saturated calcium chloride solution(20 mL each time)and 1.8 g anhydrous magnesium sulfate.Under these conditions,we improved the general synthesis yield from 55%to 80.70%,and the purity was as high as 96.69%,which realized the two-way improvement of the synthesis yield and purity of ethyl acetate.
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