- 上一篇：新型异官能团交联剂的设计合成及其在基因载体中的应用
- 下一篇：胱氨酸二甲酯间卟啉钴（II）合成研究
摘要1,2-二硝基胍（DNG）是一种新型的高性能、中敏感度炸药，作为合成1,2-二硝基胍铵（ADNQ）和1,7-二氨基-1,7-二硝氨基-2,4,6-三硝基-2,4,6-三氮杂庚烷（APX）的原料，具有很高的研究价值。本文以硝基胍（NQ）为原料，采用100%硝酸-20%发烟硫酸、发烟硝酸-五氧化二磷两种硝化体系，经硝化反应合成1,2-二硝基胍（DNG）。研究了不同因素对产物产率的影响规律，分别得到两种体系的最佳工艺条件：①n（HNO3）：n（NQ）=7.5：1，V（H2SO4）：V（HNO3）=4：3，反应时间为8 h，反应温度为10 ℃，产率达41.93%；②m（NQ）=2.6g时，m（P2O5）=7.5g，V（HNO3）=10ml，反应时间为3h，反应温度为10℃，产率达38.93%。通过IR，1H NMR、13C NMR、MS等手段对1,2-二硝基胍（DNG）的结构进行表征，并采用热重分析仪（TG）和差示扫描量热仪（DSC）对1,2-二硝基胍（DNG）的热分解性能进行了测试。TG和DSC测试结果表明：DNG具有良好的热稳定性，最大峰温为182.83 ℃。62951
毕业论文关键词 1,2-二硝基胍（DNG）；硝基胍（NQ）；硝化反应；热分解性能
毕业设计说明书（论文）外文摘要
Title Synthesis and Properties of 1,2-Dinitroguanidine
Abstract 1,2-Dinitroguanidine(DNG) is a novel explosive with high performance and moderate sensitivity, as a raw material for synthetic ammonium-dinitroguanidine (ADNQ) and 1,7-diamino-1,7-dinitrimino-2,4,6-trinitro-2,4,6-triazaheptane (APX), has a very high research value. In this paper, we used nitroguanidine (NQ) as a raw material to compose 1,2 - dinitroguanidine (DNG) in two kinds of nitrification system, nitric acid and its mixtures with 20% oleum or phosphorus pentoxide. The affecting factors on the two systems of DNG were investigated. The results show that the optimized conditions of the nitration reaction are: ①the molar ratio of HNO3 to NQ 7.5:1, the volume ratio of H2SO4 to HNO3 4:3, the reaction time 8h, temperature 10℃, The yield of DNG can reach up to 41.93%. ②when the mass of NQ was 2.6g, the mass of P2O5 was 7.5g, the volume of fuming nitric acid was 10ml, the reaction time 3h, temperature 10℃, the yield of DNG can reach up to 38.93%. The structure of DNG were identified by IR spectra, 1H NMR, 13C NMR and mass spectra. And the thermal decomposition behavior of DNG was also studied using thermogravimetry (TG) and differential scanning calorimetry (DSC) methods. The TG and DSC results show that DNG had a good thermal stability, the maximum temperature peak was 182.83 ℃.
Keywords 1,2-Dinitroguanidine(DNG); nitroguanidine(NQ); nitration; thermal decomposition behavior
1 绪论 1
1.1 研究背景 1
1.2 1,2-二硝基胍(DNQ) 2
1.3 硝化体系 5
1.4 热分析 6
1.5 本文研究的目的和意义 7
1.6 本文研究的内容 8
2 合成方案设计 9
3 实验部分 10
3.1 实验仪器及药品 10
3.2 100%硝酸-发烟硫酸体系反应过程及表征 10
3.3 结果与讨论 10
3.3.1 硝酸与硝基胍摩尔比对反应产率的影响 10
3.3.2 探究发烟硫酸与硝酸体积比对产率的影响 11
3.3.3 探究反应时间对产率的影响