Research on the SynthesisCharacterization and Pulse Ultrasnic-assisted Extraction of a Low Melting Point Energetic Compound

doi:10.3969/j.issn.1000-1093.2017.02.012

Abstract

Abstract: 1-Methyl-3,5-dinitro-1,2,4-triazole (DNMT) is synthesized from dicyandiamide and methyl hydrazine via a two step procedure (condensation and oxidation). After purification, the melting point is 93~95 ℃. The structure of the target DNMT is characterized by ¹H, ¹³C NMR, FT-IR, MS and elemental analysis. The thermal stability is studied by TG-DTA. The result shows that the thermal decomposition temperature is 281.5 ℃. The reaction mechanism of DNMT in synthesis is primarily discussed. The post- treatment technology is improved, and the method of ultrasonic-assisted liquid-liquid extraction (ULLE) is used to extract the target product with thermal ethyl acetate as extractant. The influence of extraction parameters, such as volume, temperature of extraction solvent, extraction time, etc., on extraction efficiency are investigated. The result shows that ULLE method is conducive to efficiently obtain highly pure product (≥98.68%, HPLC), and the overall yield is raised to 52.8%. Key

Key words: ordnancescienceandtechnology, energeticcompound, lowmeltingpoint, synthesis, ultrasonic-assistedliquid-liquidextraction

CLC Number:

TQ564.3

LUO Jin， LIU Yu-cun， LIU Yan， WANG Jian-hua， CHAI Tao， YUAN Jun-ming， YU Yan-wu，CHANG Shuang-jun. Research on the SynthesisCharacterization and Pulse Ultrasnic-assisted Extraction of a Low Melting Point Energetic Compound[J]. Acta Armamentarii, 2017, 38(2): 292-297.

References

［1］杜志明，张英豪，韩志跃，等. 三唑类富氮杂环化合物的研究进展［J］.北京理工大学学报, 2016, 36(6):551-557.
DU Zhi-ming, ZHANG Ying-hao, HAN Zhi-yue, et al. Research progress on triazole nitogen-rich compounds ［J］. Transactions of Beijing Institute of Technology, 2016, 36(6):551-557. (in Chinese)
[2］贾思媛，张海昊，王伯周，等. 1-甲基-3,5-二氨基-1,2,4-三唑(DAMT)合成方法改进[J].应用化工, 2015, 44(5):896-898.
JIA Si-yuan, ZHANG Hai-hao, WANG Bo-zhou, et al. Improvement of the synthetic process of 1-methyl-3, 5- diamino-1,2,4-triazole (DAMT) [J]. Applied Chemical Industry, 2015, 44(5):896-898.(in Chinese)
[3］ Hiskey M A, Chavez D E, Naud D N. Progress in high-nitrogen chemistry in explosives, propellants and pyrotechnics [C］∥Proceeding of 27th International Pyrotechnics Seminar. Colorado, US：PIPS, 2000.
[4］王亲会. 熔铸混合炸药用载体炸药评述[J].火炸药学报, 2011, 34(5): 25-28.
WANG Qin-hui.Overview of carrier explosive for melt-cast com- posite explosive[J].Chinese Journal of Explosives ＆ Propellants, 2011, 34(5): 25-28. (in Chinese)
[5］ David W P. Synthesis of DNMT: a new energetic, melt-pour ingredient[C]∥2010 Insensitive Munitions and Energetic Materials Technology Symposium. Holston, US:BAE, 2010.
［6］田均均，张庆华，李金山. 含能分子合成最新进展［J］.含能材料, 2016, 24(1): 1-9.
TIAN Jun-jun, ZHANG Qing-hua, LI Jin-shan. Recent advances in energetic molecule synthesis［J］. Chinese Journal of Energetic Materials, 2016, 24(1): 1-9. (in Chinese)

[7］于玲，胡章记，董丽丽. 滤膜吸附结合超声辅助分散液液微萃取/高效液相色谱法测定空气中溴氰菊酯残留[J].分析测试学报,2015,34(12):1354-1359.
YU Ling, HU Zhang-ji, DONG Li-li.Determination of deltamethrin in air by membrane adsorption combined with ultrasound-assisted dispersive liquid-liquid microextraction and high performance liquid chromatography[J]. Journal of Instrumental Analysis, 2015,34(12):1354-1359. (in Chinese)
[8］ Dickman M H, Pope M T. Peroxo and superoxo complexes of chromium, molybdenum, and tungsten[J]. Cheminform, 1994, 94(3):569-584.

第38卷
第2期2017 年2月兵工学报ACTA
ARMAMENTARIIVol.38No.2Feb.2017

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