响应面法优化微波辐射合成对硝基苯甲酸乙酯

Response surface optimization of synthesis of p-nitro-ethylbenzoate under microwave irradiation

采用微波辐射方法,对硝基苯甲酸与乙醇作原料,三氯化铝作催化剂合成对硝基苯甲酸乙酯。研究了醇酸比、微波辐射功率、微波辐射时间、催化剂用量对产物收率的影响。在单因素实验基础上,固定微波辐射功率400W,利用响应面法优化对硝基苯甲酸乙酯合成工艺。得到最佳工艺条件:醇酸比为5.2:1、微波辐射时间为9.8min、催化剂用量为对硝基苯甲酸质量的17.4%,收率达92.08%。产品结构经红外表征。

The p-nitro-ethylbenzoate was prepared by microwave irradiation method with p-nitrobenzoic acid andethanol as raw materials and aluminum chlorid as catalyst. The yield of p-nitro-ethylbenzoate were influenced by themole ratio of ethanol and p-nitrobenzoic acid, microwave irradiation power, microwave irradiation time and the amountof catalyst（the mass ratio of aluminum chlorid and p-nitrobenzoic acid）. On the basis of single factor experiments, themicrowave irradiation power was fixed at 400 W, the synthesis process of p-nitro-ethylbenzoate was optimized by responsesurface methodology. The optimized process conditions were as follows： the mole ratio of ethanol and p-nitrobenzoic acidwas 5.2, the microwave irradiation time was 9.8min and the mass ratio of aluminum chlorid and p-nitrobenzoic acid was17.4%. The yield of p-nitro-ethylbenzoate can reach 92.08%. Product structure was characterized by IR.