RDX酮制备工艺的改进研究

以乌洛托品、脲为原料,以硝酸 五氧化二磷作为硝化剂制备了RDX酮。考察了五氧化二磷的用量、加料方式、反应温度及反应时间等因素对产品得率的影响。结果表明:硝酸与五氧化二磷的质量比为10∶1,加料方式为先加脲素,后加五氧化二磷,5～8℃反应20min,20℃保温20min,产品RDX酮的得率在95%以上。通过元素分析、红外光谱和核磁共振氢谱对产品结构进行了表征。本工艺条件温和,易于控制,产品得率高,反应过程基本无污染,具有重大的工业应用价值。

Study on innovation of technique for preparing RDX ketone

The RDX ketone is synthesized from urotropine and urea,using nitric acide and phosphorus pentoxide as nitrating agent.The effect of the dosage of phosphorus pentoxide,the way of feeding,reaction temperature and reaction time on yield have been investigated.The results showed that the optimum conditions for synthesing RDX ketone were:mass ratio of nitric acide to phosphorus pentoxide was 10∶1,feeding urea before phosphorus pentoxide,reacted 20 min at 5～8 ℃ and thermal insulating 20 min at 20 ℃,the yield of RDX ketone was more than 95%.The product structure are characterized by elemental analysis ,IR and HNMR.This method is that the condition is moedrate,the operation is controlled easily,yield is higher and less pollution during reaction.It will be of important value for industrical application.