硒催化CO/H_(2)O体系下高压还原制备M酸的研究

Study on Selenium-catalyzed Preparation of M Acid in CO/H_(2)O System at High Pressure

以硒为催化剂,在高压水相条件下通入一氧化碳,由3,5-二硝基-2,4,6-三甲基苯磺酸制备M酸。确定最优反应条件:3,5-二硝基-2,4,6-三甲基苯磺酸1.45 g(5 mmol);无水碳酸钠0.106 g(1 mmol);Se 0.0316 g(0.4 mmol);PCO 4 MPa;溶剂用量10 mL;反应温度160℃;反应时间3 h。M酸最高纯度可达98.60%。通过正交实验L_(9)(3^(4))可得部分动力学因素对反应的影响强弱顺序为:温度>水量>压强>硒量。

M acid was prepared from 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid by introducing carbon monoxide with selenium as catalyst under high pressure aqueous phase.The optimal reaction conditions was obtained as follows: 3,5-dinitro-2,4,6-trimethylbenzenesulfonic acid 1.45 g(5 mmol);anhydrous sodium carbonate 0.106 g(1 mmol);Se 0.0316 g(0.4 mmol);PCO 4 MPa;amount of solvent 10 mL;reaction temperature 160 ℃;reaction time 3 h.The highest purity of M acid measured was 98.60%.Through orthogonal test L9(34),it can be obtained that the effect of some kinetic factors on the reaction is: temperature>water amount>pressure>selenium amount.