摘要FOX-7的化学名称是1,1-二氨基-2,2-二硝基乙烯，简称DADE。是一种新型的高能低感化合物。自1998年FOX-7首次合成以来，因其性能优良，在含能材料领域受到广泛关注。目前FOX-7在生产过程中的产率只有38%，因此FOX-7的合成工艺优化仍然是一项非常重要的研究工作。当前有三种关于FOX-7主流合成方法的报道，但是这些方法都存在硝化过程中酸的消耗量大，对温度的控制要求严格，反应过程中放热剧烈等缺点。
本论文采用改进的合成方法，以2-甲基-4,6-二羟基嘧啶为原料，用硝硫混酸对其硝化，再进行水解得到FOX-7。通过单因素实验研究反应温度，反应时间和原料与发烟硝酸的摩尔比对FOX-7产率的影响。通过正交试验的结果确定较佳的合成工艺条件。结果显示，反应温度为20℃，反应时间为60min，2-甲基-4,6-二羟基嘧啶与发烟硝酸的摩尔比为1:4。5，发烟硝酸与浓硫酸的体积比为1:3，产物最高得率达到78。2%。通过熔点、核磁、TLC、红外等对所合成的化合物进行结构表征。结果证实制备所得产物与目标产物一致。并结合文献推测了由2-甲基-4,6-二羟基嘧啶为原料合成FOX-7的反应机理。78025
毕业论文关键词：高能钝感炸药； 2-甲基-4,6-二羟基嘧啶；FOX-7；硝化
毕业设计论文外文摘要
The study of synthesis of high energetic and low sensitive compound
Abstract The chemical name of FOX-7 is 1,1-Diamino-2,2-dinitroethylene, referred DADE。 It’s a new energetic material。 Since 1998, it has been paid widespread attention in the field of energetic materials because of its excellent performance。 The production rate of FOX-7 is only 38% in the production process, so the process optimization is still a very important research。 Currently, there are three kinds of main synthetic methods about the FOX-7, but these methods have some shortcoming, such as too much acid in the process of nitrification, strict control of the temperature, violent exothermic during the reaction。
In this paper, the improved synthetic method is adopted : the 4,6-Dihydeoxy-2-methy pyrimidine is nitrified by the nitric-sulfuric acid, after hydrolysis of the compound synthesized to afford FOX-7。 Influence of factors of reaction temperature, reaction time, molar ratio of the raw material and fuming nitric acid was researched by single element experiment。 The optimum conditions of synthesis was determined by orthogonal experiment。 It turns out that molar ratio of 4,6-Dihydeoxy-2-methy pyrimidine and fuming nitric is 1:4。5,volume of fuming nitric and concentrated sulfuric is 1:3, temperature is 20℃ and maintained for 60 min。 The maximum yield is 78。2%。
The products are characterized by Melting Point Test, TLC, NMR and IR。 It turns out that the preparation of the products is in accordance with objective product。 According to the literature, the reaction mechanism is speculated that Process for synthesizing FOX-7 from 2- methyl-4,6-dihydroxy pyrimidine。
Keywords: Insensitive high explosive; 4,6-Dihydeoxy-2-methy pyrimidine; FOX-7; Nitration
目 次
1 绪论 1
1。1 高能低感炸药的研究意义 1
1。2 高能低感炸药研究进展 1
1。4 本文研究内容 6
2 实验原理与分离技术 7
2。1 硝化反应 7
2。2 硝化试剂 7
2。3 重结晶 高能低感化合物的合成研究:http://www.youerw.com/huaxue/lunwen_89790.html