【摘要】 采用化学计量学中的均匀试验设计方法对4,6-二硝基-1,2,3-三氯苯的合成工艺进行了研究.研究结果表明,影响4,6-二硝基-1,2,3-三氯苯收率的因素由大到小依次为反应时间、温度、硝酸与三氯苯的摩尔配比、硫酸与三氯苯的摩尔配比.优化的合成条件为反应时间3.92 h,温度为62.98℃,硝酸与三氯苯的摩尔比为2.31∶1,硫酸与三氯苯的摩尔比为11∶1,4,6-二硝基-1,2,3-三氯苯的最大收率为97.95%.对反应产物进行了高效液相色谱、红外光谱和元素分析.更多还原

【Abstract】 The synthesis technology of 4,6-dinitro-1,2,3trichloro-benzene was studied.Homogeneous design,which is one of the chemometric methods,was used to optimize the synthetic conditions.The results show that the reaction time is the most significant factor that can affect the yield of 4,6-dinitro-1,2,3-trichloro-benzene and then the sequence of the residual factors is as follows,the reaction temperature,the molar ratio of nitric acid to 1,2,3-trichloro-benzene,and the molar ratio of sulphuric acid to 1,2,3-trichloro-benzene.The optimized synthetic conditions are proved to be that the reaction time is 3.92 h,the reaction temperature is 62.98 ℃,the molar ratio of nitric acid to 1,2,3-trichloro-benzene is 2.31∶1 and the molar ratio of sulphuric acid to 1,2,3-trichloro-benzene is 11∶1 and the highest yield can reach to 97.95%.Furthermore the product were analyzed by HPLC,IR and elementary analysis.更多还原