【摘要】 以尿素为起始原料,经硝硫混酸硝化和水解得到硝酰胺,硝酰胺和三聚甲醛缩合反应得到亚甲基二硝胺(MDNA)。用核磁共振、红外光谱、元素分析和高效液相色谱对产物进行了表征。用DSC研究了MDNA的热分解性能。结果表明,硝酰胺制备MDNA的较佳工艺条件为:硝酰胺与三聚甲醛摩尔比为3∶1,加料温度-13~-10℃,反应温度-8~-5℃,反应时间30min,硫酸质量分数90%,MDNA收率为74.0%。用DSC测得MDNA的热分解温度为122.5℃。更多还原

【Abstract】 Nitramide was obtained by nitration with H2SO4/HNO3 mixed acid and hydrolysis,using urea as starting material,and methylenedinitramine(MDNA)was synthesized by condensation reaction of nitramide with 1,3,5-trioxane.The MDNA was characterized by 1 H NMR,IR,elemental analysis and HPLC.Thermal decomposition performance of MDNA was studied by DSC.Results show that the optimal reaction conditions for preparing MDNA via nitramide are stated as follows:molar ratio of nitramide and 1,3,5-trioxane 3∶1,feeding temperature from-13to-10℃,reaction temperature from-8to-5℃,reaction time 30min and concentration of sulfuric acid 90%.The total yield of MDNA is 74.0%.Thermal decomposition temperature of MDNA obtained by DSC is 122.5℃.更多还原