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Synthesis and Characterization of Guanidine Dinitramide Crystal

구아니딘 디나이트라아마이드 결정의 합성 및 특성 분석

  • Kim, Wooram (Department of Applied Environmental Science, Kyun Hee University) ;
  • Kwon, Younja (Department of Applied Environmental Science, Kyun Hee University) ;
  • Jo, Youngmin (Department of Applied Environmental Science, Kyun Hee University) ;
  • Park, Youngchul (Agency for Defense Development 4th R&D Institute 1 Department)
  • 김우람 (경희대학교 환경응용과학과) ;
  • 권윤자 (경희대학교 환경응용과학과) ;
  • 조영민 (경희대학교 환경응용과학과) ;
  • 박영철 (국방과학연구소 4 기술연구본부)
  • Received : 2015.10.16
  • Accepted : 2015.11.16
  • Published : 2015.12.10

Abstract

An environmentally favorable solid oxidizer, guanidine dinitramide ($H_2C(NH_2)NH_2N(NO_2)_2$), with high purity and synthesis yield was prepared using guanidine carbonate ($NH_2C(=NH)NH_2{\cdot}1/2H_2CO_3$). Two different crystalline forms (${\alpha}$-form and ${\beta}$-form) were obtained depending on the solvent used and synthesis process. Despite of the same chemical composition, Raman-IR and TGA-DSC revealed that different structures existed between them. In particular, the thermal analysis showed the exothermic temperature of ${\alpha}$-form at $155.7^{\circ}C$ while $191.6^{\circ}C$ for ${\beta}$-form. The caloric value of ${\alpha}$-form was 536.4 J/g which was 2.5 times larger than that of ${\beta}$-form, 1310 J/g. In addition, ${\alpha}$-form was steeply decomposed with one-step variation, but ${\beta}$-form followed a two-step thermal decomposition pattern.

Keywords

Guanidine;nitramide;solid propellant;green oxidizer;crystal structure

References

  1. O. A. Luk'yanov, V. P. Gorelik, and V. A. Tartakovsky, Dinitramide and its salts, Russ. Chem. Bull., 44, 108-112 (1995). https://doi.org/10.1007/BF00696969
  2. A. S. Gohardani, J. Stanojev, A. Demairee, K. Anflo, M. Persson, N. Wingborg, and C. Nilsson, Green space propulsion: Opportunities and prospects, Prog. Aerosp. Sci., 71, 128-149 (2014). https://doi.org/10.1016/j.paerosci.2014.08.001
  3. B. Slettenhaar, J. F. Zevenbergen, H. J. Pasman, A. G. M. Maree, and J. L. P. A. Moerel, Study on catalytic ignition of HNF based non toxic monopropellants, 39th AIAA Joint Propulsion Conference, July 20-23, Huntsville USA (2003).
  4. L. Courthéoux, S. Rossignol, C. Kappenstein, and N. Pillet, Improvement of catalyst for the decomposition of HAN-based monopropellant - comparison between aerogel and xerogel, 39th AIAA Joint Propulsion Conference, July 20-23, Huntsville USA (2003).
  5. S. ROSTLUND, C. VORDE, C. SJOQVIST, and S. CALSSON, Pyrotechnic thermal fuse, EP Patent 1885668 B1 (2006).
  6. N. Latypov and A. Langlet, The method of producing Dinitramide salts, WO Patent 1999046202 A1 (1999).
  7. X. K. Yang, K. Z. Xu, F. Q. Zhao, X. Yang, H. Wang, J. R. Ji, and Y. Y. Wang, Thermal Behavior, Specific Heat Capacity and Adiabatic Time-to-explosion of GDN, Chem. Res. Chinese Universites, 25(1), 76-80 (2009).
  8. W. R. Kim, Y. J. Kwon, Y. M. Jo, and S. T. Jung, Synthesis of Organic salt Oxidizer, Guanidine Dinitramide, J. Korea Oil Chem. Soc., 31(3), 345-351 (2014). https://doi.org/10.12925/jkocs.2014.31.3.345
  9. A. Langlet, H. Ostmark, and N. Wingborg, Method of preparing dinitramidic acid and salts thereof, US Patent 5976483 (1999).
  10. R. Adihiyaman and S. K. Basu, Crystal Modification of dipyridamole using different solvents and crystallization conditions, Int. J. Pharm., 321, 27-34 (2006). https://doi.org/10.1016/j.ijpharm.2006.04.021
  11. Y. Kawashima, T. Niwa, H. Takeuchi, T. Hino, Y. Itoh, and S. Furuyama, Characterization of Polymorphs of Tranilast Anhydrate and Tranilast Monohydrate When Crystallized by two solvent change spherical crystallization techniques, J. Pharm. Sci., 80(5), 472-478 (1991). https://doi.org/10.1002/jps.2600800515
  12. G. H. Nazeri, R. Mastour, M. Fayaznia, and P. Keyghobadi, Synthesis of Ammonium Dinitramide by Nitration of Potassium and Ammonium Sulfate. The Effect of Sulfamate Conterion on ADN Purity, Iran. J. Chem. Chem. Eng., 27(1), 85-89 (2008).