A new energetic dipotassium 3,3΄-dinitro-5,5΄-bis-1,2,4-triazole-1,1΄-diolate [K2(DNOBT)] was synthesized, and structurally characterized by elemental analysis, IR spectra, 13C NMR and single-crystal X-ray diffraction. K2(DNOBT)•2H2O crystallizes in monoclinic system, space group P21/n with a = 6.0446(10), b = 15.999(3), c = 6.4169(11) Å, β = 99.421(2)°, V = 612.21(18) Å3, Z = 4, Dc = 2.009 gcm-3, F(000) = 372, μ = 0.838 mm-1, S = 1.012, the final R = 0.0248 and wR (I > 2(I)) = 0.0604. Thermal decomposition of the title compound was studied by using DSC and TG-DTG, and there is primarily one exothermic decomposition process at 371.5 ℃.
Financially supported by the National Natural Science Foundation of China (No. 21373157)
通讯作者:
wbz600@163.com.
E-mail: wbz600@163.com
引用本文:
罗义芬;毕福强;翟连杰;王锡杰;廉鹏;王伯周. Synthesis, Crystal Structure and Thermal Decomposition of a New Energetic Dipotassium 3,3΄-Dinitro-5,5΄-bis-1,2,4-triazole-1,1΄-diolate[J]. 结构化学, 2017, 36(2): 211-216.
LUO Yi-Fen;BI Fu-Qiang;ZHAI Lian-Jie;WANG Xi-Jie;LIAN Peng;WANG Bo-Zhou. 一种新型含能化合物1,1΄-二羟基-3,3΄-二硝基-5,5΄-联-1,2,4-三唑二钾盐的合成、晶体结构与热性能研究. CHINESE JOURNAL OF STRUCTURAL CHEMISTRY, 2017, 36(2): 211-216.
REFERENCES
(1)Dippold, A. A.; Klapötke, T. M. Synthesis and characterization of 3,3΄-bis(dinitromethyl)-5,5΄-azo-1H-1,2,4-triazole. Z. Anorg. Allg. Chem. 2011, 637, 14531457.
(2) Zhang, Y. Q.; Parrishb, D. A.; Shreeve, J. M. Derivatives of 5-nitro-1,2,3-2H-triazole–high performance energetic materials. J. Mater. Chem. A 2013, 1, 585593.
(3) Dippold, A. A.; Klapötke, T. M.; Martin, F. A. Synthesis and characterization of bis(triaminoguanidinium) 5,5΄-dinitrimino-3,3΄-azo-1H- 1,2,4-triazolate – a novel insensitive energetic material. Z. Anorg. Allg. Chem. 2011, 637, 11811193.
(4) Dippold, A. A.; Feller, M.; Klapötke T. M. 5,5΄-Dinitrimino-3,3΄-methylene-1H-1,2,4-bistriazole – a metal free primary explosive combining excellent thermal stability and high performance. Cent. Eur. J. Energ. Mater. 2011, 8, 261278.
(5) Dippold, A. A.; Klapötke, T. M.; Winter, N. Insensitive nitrogen-rich energetic compounds based on the 5,5΄-dinitro-3,3΄-bi-1,2,4-triazol-2-ide anion. Eur. J. Inorg. Chem. 2012, 34743484.
(6) Dippold, A. A.; Klapötke T. M. A study of dinitro-bis-1,2,4-triazole-1,1΄-diol and derivatives: design of high-performance insensitive energetic materials by the introduction of N‑oxides . J. Am. Chem. Soc. 2013, 135, 99319938.
(7) Li, Z. M.; Zhang, J. G.; Yang, W.; Sun, M.; Zhang, T. L. Synthesis and structural characterization of a new 1D polymeric energetic complex [Hg(DAT)Cl2]n. Chin. J. Struct. Chem. 2013, 32, 653658.
(8) Gao, H. X.; Joo, Y. H.; Parrish, D. A.; Vo, T.; Shreeve, J. M. 1-Amino-1-hydrazino-2,2-dinitroethene and corresponding salts: synthesis, characterization, and thermolysis studies. Chem. Eur. J. 2011, 17, 46134618.
(9) Song, J. H.; Zhou, Z. M.; Cao, D.; Huang, H. F.; Liang, X.; Wang, K.; Zhang, J. 2-(Dinitromethylene)-1-nitro-1,3-diazacyclopentane-based energetic salts. Z. Anorg. Allg. Chem. 2012, 638, 811820.
(10) Klapötke, T. M.; Laub, H. A.; Stierstorfer, J. Synthesis and characterization of a new class of energetic compounds–ammonium nitriminotetrazolates. Propellants Explos., Pyrotech. 2008, 33, 421430.
(11) Brand, H.; Mayer, P.; Polborn, K.; Schulz, A.; Weigand, J. J. Blue alkali dinitrosomethanides: synthesis, structure, and bonding. J. Am. Chem. Soc. 2005, 127, 13601361.
(12) Yang, L.; Wu, B. D.; Zhang, T. L.; Liu, Z. H.; Zhang, J. G. Preparation, crystal structure, thermal decomposition, and explosive properties of [Cd(en)(N3)2]n. Propellants Explos., Pyrotech. 2010, 35, 521528.
(13) Song, J. H.; Zhou, Z. M.; Huang, H. F.; Cao, D.; Liang, L. X. Synthesis and characteristics of bis(2,2-dinitroethyl-N-nitro) ethylenediamine-based energetic salts. Z. Anorg. Allg. Chem. 2012, 638, 957–964.
(14) Xu, C.; Bi, F. Q.; Zhang, M.; Liu, Q.; Ding, K. W.; Ge, Z. X. Synthesis, structural characterization and properties of bis(1,5-diamino-1H-tetrazolium) 3,3΄-bis(nitramino)-4,4΄-azofurazan. Chin. J. Struct. Chem. 2015, 34, 13411346.
(15) Xu, K. Z.; Zuo, X. G.; Zhang, H.; Yan, B.; Huang, J.; Ma, H. X.; Wang, B. Z.; Zhao, F. Q. Synthesis and thermal behavior of a new high-energy organic potassium salt. J. Therm. Anal. Calorim. 2012, 110, 585–591.
(16) Chen, H. Y.; Zhang, T. L.; Zhang, J. G.; Yang, L.; Qiao, X. J. Synthesis, characterization and properties of tri-substitute potassium salt of trinitrophloroglucinol. Chin. J. Chem. 2007, 25, 5965.
(17) Zhai, L. J.; Wang, B. Z.; Fan, X. Z.; Li, X. Z. Synthesis, crystal structure and thermal decomposition of a new energetic potassium salt bis(dinitromethyl)ether. Chin. J. Struct. Chem. 2014, 33, 13531359.
(18) Luo, Y. F.; Wang, Z. J.; Bi, F. Q.; Wang, B. Z.; Zhou, C.; Ge, Z. X. Synthesis and properties of insensitive energetic material MAD-X1. Chin. J. Expl. Propell. 2015, 38, 1317.
(19) Sheldrick, G. M. SHELXS-97. Program for Crystal Structure Solution. University of Göttingen, Germany 1997.
(20) Sheldrick, G. M. SHELXL-97. Program for Crystal Structure Refinement. University of Göttingen, Germany 1997.