乙酰水杨酸合成实验常见问题分析及优化

Analysis and Optimization of Common Problems in Acetylsalicylic Acid Synthesis Experiment

  • 摘要: 乙酰水杨酸的合成实验是本科教学开设的经典合成实验之一,为解决在教学中使用经典催化剂浓硫酸存在的诸多问题,该文从供试的14种催化剂中筛选出适合本科教学实验的催化剂无水碳酸钠,通过实验优化得到反应物配比最佳为n (水杨酸)∶n (乙酸酐) = 1∶1.8,反应温度为80 ℃,反应时间为30 min;通过调整乙酸酐的水解操作步骤缩短了结晶时间,并对两种催化剂副产物分析发现无水碳酸钠为催化剂时副产物比浓硫酸的更少。

     

    Abstract: The synthesis experiment of acetylsalicylic acid is one of the classic experiments offered in undergraduate teaching. To address the numerous problems associated with the use of concentrated sulfuric acid as a classic catalyst in teaching, this paper screens anhydrous sodium carbonate as a suitable catalyst for undergraduate teaching experiments from 14 tested catalysts. Through experimental optimization, the optimal reactant ratio is determined as n (salicylic acid)∶n (acetic anhydride) = 1∶1.8, with a reaction temperature of 80 ℃ and a reaction time of 30 min. The crystallization time is shortened by adjusting the hydrolysis operation steps of acetic anhydride. The analysis of by-products from the two catalysts reveals that anhydrous sodium carbonate produces fewer by-products than concentrated sulfuric acid.

     

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