4,4'-二硝基二苯醚的合成工艺研究

Synthesis of 4,4'-dintitrodiphenyl ether

用对硝基氯苯一步缩合法合成4,4’-二硝基二苯醚(DNDPE),研究了反应温度、原料配比(包括对硝基氯苯与碳酸钠、亚硝酸钠的摩尔比)、反应时间、溶剂量对DNDPE收率的影响,并用HPLC对目的产物进行分析。结果表明:DNDPE的较佳合成工艺条件为反应温度150℃,n(碳酸钠)∶n(对硝基氯苯)=0.7,n(亚硝酸钠)∶n(对硝基氯苯)=0.8,反应时间7h,n(DMF)∶n(对硝基氯苯)=5,溶剂回收循环利用可行。在该条件下,DNDPE收率可达77.3%。

The synthesis of 4,4＇-dinitrodiphenyl ether（DNDPE） from direct condensation of p-chloronitrobenzene （p-CNB） was introduced. DNDPE yield was taken as an index, reaction temperature, molar ratios of p-CNB-sodium car- bonate and p-CNB-sodium nitrite, reaction time and solvent amount were studied. The target product was analyzed by HPLC. The results showed that the optimal process conditions of DNDPE were obtained as follows：the reaction tempera- ture was 150℃, n（NazCOa） ： n（p-CNB）=0. 7, n（NaNO2） ： n（p-CNB）=0. 8, the reaction time was 7 h; n（DMF） ： n（p- CNB） =5, recycling solvents was feasible. Under above optimal conditions, the yield of DNDPE was about 77.3%.