微通道反应器内硝酸氧化合成对硝基苯甲酸  

Synthesis of p-Nitrobenzoic Acid by Nitric Acid Oxidation in Microchannel Reactor

作　　者：冯志强 宋红刚 王金 汪敦佳 魏先红 FENG Zhiqiang;SONG Honggang;WANG Jin;WANG Dunjia;WEI Xianhong(College of Chemistry and Chemical Engineering,Hubei Normal University,Huangshi 435002,China;Huangshi Hanwei Technology Co.,Ltd.,Huangshi 435002,China)

机构地区：[1]湖北师范大学化学化工学院,湖北黄石435002 [2]黄石汉微科技有限公司,湖北黄石435002

出　　处：《化工技术与开发》2023年第3期26-29,共4页Technology & Development of Chemical Industry

摘　　要：在微通道反应器内,以冰醋酸和水为溶剂,用氧气和稀硝酸氧化对硝基甲苯,合成了对硝基苯甲酸。通过条件实验得到了较优的反应条件:氧化反应温度205℃、压力4.0MPa、对硝基甲苯浓度为10%、硝酸浓度为29.2%、泵入的反应液流量为10m L·min^(-1)、氧气流量为0.5L·min^(-1)。在此优化条件下进行母液循环套用实验,最终对硝基苯甲酸成品的总收率为72.6%,液相色谱纯度在99.0%以上。实验结果表明,该工艺操作简便、安全可控、绿色环保,特别适用于连续化生产工艺。In the microchannel reactor, p-nitrobenzoic acid was synthesized by oxidation of p-nitrotoluene with dilute nitric acid and oxygen in glacial acetic acid and water. The optimum reaction conditions were obtained through the condition experiment: the oxidation reaction temperature was 205℃, the pressure was 4.0MPa, the concentration of p-nitrotoluene was 10%, the concentration of nitric acid was 29.2%. Meanwhile the flow rate of the reaction liquid was 10 mL/min and the flow rate of oxygen was 0.5L/min. Under the optimum reaction conditions, the test of the mother solution recycle was performed and the total yield of p-nitrobenzoic acid was 72.6% and the purity of liquid chromatography was over 99.0%. The result showed that the process was easy to operate, safe and controllable, green and environmentally friendly, especially suitable for continuous production process.

关 键 词：对硝基苯甲酸 对硝基甲苯 硝酸氧化 微通道反应器 

分 类 号：O625.511[理学—有机化学]