【作者】 刘达波；

【导师】 邱祖民；

【作者基本信息】 南昌大学 ， 工业催化， 2008， 硕士

【摘要】 本文使用硅锂钠石基中孔材料做载体,制备出固体超强酸,并用于乙酰水杨酸的合成做探针反应,考察了固体超强酸做催化剂时的用量、酸酐摩尔比及反应温度对乙酰水杨酸合成的影响,得出合成乙酰水杨酸的较佳制备工艺条件:酸酐摩尔比为1:2,催化剂用量为水杨酸质量的1.5%,在75℃反应15 min。浸渍法制备了SO₄^2-/Silinaite固体超强酸催化剂,最佳工艺条件为:硫酸浸渍浓度0.25 mol/L,浸渍2 h,焙烧温度450℃,焙烧时间3 h,得到的乙酰水杨酸的产率达83.4%,此时,催化剂可重复使用2次,并证明了先加乙醇水溶液处理废酸更经济。最后论文用乙酰水杨酸做配体,通过与人体所必需的微量元素——锰配位合成水杨酸锰,对阿司匹林锰的合成进行了初探。以乙酰水杨酸和碳酸氢钠反应,再在70℃水浴中与硫酸锰反应,加沉淀剂叔丁醇,放置结晶,将得到的产物用扩散法结晶得到水杨酸锰晶体,分析了使用乙醇和苯组合的混合溶剂做结晶更佳,指出了未得到乙酰水杨酸锰的原因。通过单晶衍射、FT-IR、质谱进行了表征,并对水杨酸锰的热重、紫外可见光谱、荧光光谱以及磁力性能进行了考察,发现该配合物在生物医药、荧光性能以及磁性性能方面具有广泛的应用价值。更多还原

【Abstract】 Solid super acid was prepared by silinaite-based mesoporous catalysts in the synthesis of acetylsalicylic acid was investigated. The effects of catalyst amount, molar ratio of salicylic acid to acetic anhydride, and reaction temperature on the synthesis of acetylsalicylic acid were studied. Experimental results demonstrated that the optimum reaction conditions were as follows: the molar ratio of salicylic acid to acetic anhydride wasl:2, the amount of catalyst 1.5% vs salicylic acid, while the reaction was carried out at 75℃for 15 min. Solid superacid catalyst SO₄^2-/Silinaite was prepared by immersion. The optimum preparation conditions for the catalyst were 0.25 mol/L of H₂SO₄, immersion time 2h, and 3 h calcinations at 450℃, the yield of acetylsalicylic acid was 83.4%, the solid superacid can be used repeatedly 2 times. It is the lower producing cost that the treatment waste acid by ethanol water solution was first used than other.Manganese salicylic acid was synthesized by acetylsalicylic acid ligand with manganese which is trace elements necessary for the human, primary study on preparation of manganese acetylsalicylate. The synthesis of complex was carried out by reaction of NaHCO₃ with acetylsalicylic acid （equimolar amounts） in water, and mixed with MnSO₄ （the mole rate of MnSO₄: acetylsalicylic acid=1:2） under stirring at 70℃for 30min, tert-butyl alcohol was as precipitant, collected insoluble material from the solution by filtration, then crystallization growth was by solvent diffusion method in ethanol benzene, analyzed the mixed solvents was better, but unfortunately we did not get manganese acetylsalicylate, the reason was directed. Single crystal diffraction, FT-IR, mass spectrum of complex was characterization, TG, UV-Vis, fluorescence spectrum magnetic properties were inspected. Biological pharmaceutical functions, fluorescence and magnetic property of complex can be widely developed and utilized.更多还原