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目的:探讨双氧水催化合成对硝基苯甲酸乙酯的可行性,并考察了反应物的摩尔比、催化剂用量、反应温度及反应时间对产物收率的影响。方法:分别采用单因素设计实验与正交设计实验,分析比较这两种方法的最佳反应条件。采用数字熔点仪测定样品的熔点;用GC112A型气相色谱仪测定了产物的纯度;用傅里叶变换红外光谱仪测定产物的结构。结果:双氧水可以作为合成对硝基苯甲酸乙酯的催化剂。综合分析可知:当无水乙醇和对硝基苯甲酸的摩尔比为4:1,催化剂含量为10%,反应温度为80℃,反应时间为2.5-3h时酯化产率可达到最高值。结论:双氧水催化对硝基苯甲酸、无水乙醇合成对硝基苯甲酸乙酯的效率较高,产品纯度高,环境污染小,不失为一种新的合成方法。
OBJECTIVE: To investigate the catalytic effect of hydrogen peroxide on the synthesis of ethyl p-nitrobenzoate. The effects of the mole ratio of the reactants, the amount of catalyst, the reaction temperature and the reaction time on the yield of the product were investigated. Methods: The single factor design experiments and orthogonal design experiments were used to analyze and compare the best reaction conditions of the two methods. The melting point of the sample was measured by digital melting point instrument. The purity of the product was determined by GC112A gas chromatograph. The structure of the product was determined by Fourier transform infrared spectroscopy. Results: Hydrogen peroxide can be used as a catalyst for the synthesis of ethyl p-nitrobenzoate. Comprehensive analysis shows that when the molar ratio of anhydrous ethanol and p-nitrobenzoic acid is 4: 1, the catalyst content is 10%, the reaction temperature is 80 ℃, the reaction time is 2.5-3h esterification yield can reach the highest value. CONCLUSION: Hydrogen peroxide can catalyze the synthesis of p-nitrobenzoate by p-nitrobenzoic acid and anhydrous ethanol with high efficiency, high product purity and low environmental pollution, which is a new synthesis method.