4-二甲胺基吡啶催化合成乙酰水杨酸的研究

化工论文编号:HG059  论文字数:10414,页数:23

目  录
中文摘要 I
英文摘要 II
目  录 III
1 绪论 1
1.1 乙酰水杨酸的简介 1
1.2 乙酰水杨酸的催化合成 2
1.3 合成方法的改进 4
1.4 乙酰水杨酸的应用 4
2 实验部分 6
2.1 实验原理 6
2.2 实验药品及仪器 7
3 结果与讨论 10
3.1 最佳反应条件的选择 10
3.2 正交试验设计 13
3.3 产品分析 15
3.4 结论 15
4．总结与展望 16
致  谢 17
参考文献 18

摘要：本文研究了水杨酸和乙酸酐在4-二甲胺基吡啶的催化作用下合成乙酰水杨酸的最优化条件。分别探索了单因素下各水平的反应温度，反应时间，催化剂用量以及酸酐摩尔比对产率的影响。在此基础上采用四因素三水平来设计正交试验，通过正交试验得出其最优化反应条件为：反应温度为70℃，反应时间为60min，催化剂用量为水杨酸的18%，酸酐摩尔比为1:3。在此条件下的合成反应所得产率最大，为83.12%。产物经三氯化铁检验不显紫色，说明产品不含酚羟基。用4-二甲胺基吡啶为催化剂，催化活性高,反应安全,后处理简单,是一类较好的环境友好催化剂,值得工业化借鉴。

关键词：乙酰水杨酸；4-二甲胺基吡啶；催化；合成

4-Dimethylamino Pyridine Catalyzed Synthesis of Acetyl Salicylic Acid
Abstract: In this paper, the research of optimum conditions in synthesizing the acetylsalicylic acid was done with salicylic acid & acetic anhydride as basic materials  and  4-dimethylamino pyridine as catalyst. With single factor changing, The effect of reaction temperature、reaction time、catalyst dosage plus materials’ molar ratio on yield  was respectively explored at various levels. On that basis, the orthogonal test of four factors at three different levels was used to get the optimum conditions of reaction temperature 70 ℃、reaction time 60min、the ratio of salicylic acid to catalyst 18% as well as anhydride molar ratio 1:3. Upon these conditions, the yield reaches the maximization of 83.12%.Besides,when treated with FeCl3, the product didn’t present purple,which showed it contain no the phenolic hydroxyl. Furthermore, using  environment-friendly 4-dimethyl- amino pyridine as catalyst can improve the catalytic activity、reaction safety plus post-treatment and should be industrialized.
Key words: Acetylsalicylic acid; 4-dimethylamino pyridine; Catalyst; Synthesis