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Synthesis, Crystal Structure and Performances of BNTF
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1.School of Materials and Engineering, Southwest University of Science and Technology, Mianyang 621010, China;2.Institute of Chemical Materials, CAEP, Mianyang 621999, China

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    Abstract:

    3,4‐Bis(3'‐aminofurazan‐4'‐yl)furazan(BATF)was synthesized by reduction with stannous chloride in glycerol using 3,4‐bis(3'‐aminofurazan‐4'‐yl)furoxan(BAFF) as raw material. 3,4‐Bis(3'‐nitrofurazan‐4'‐yl)furazan(BNTF) was prepared from BAFF by using hydrogen peroxide as oxidantwith total yield of 59.0%. The structures of BATF and BNTF were characterized by 1H NMR,13C NMR,IR,MS spectra and elemental analysis,and the single crystal structure data of BNTF was obtained successfully. The crystal belongs to orthorhombic system,space group P212121 with crystal parameters a=0.71437(10) nm, b=0.96839(11)nm,c=51555(17)nm,V=1.0484(2)nm3,Z=4,Dc=1.876 g·cm-3,F(000)=592. The influence of molar ratio,reaction time,and reaction temperature on the yield of BNTF was investigated. Results show that the optimum conditions are as follows:n(BATF)∶n(35% H2O2)∶n(98% H2SO4 )∶n(Na2WO4?2H2O)=1∶60∶40∶0.86,the reaction time is 3 h,the reaction temperature is 30 ℃ and the yield of BNTF is 93.3%. The thermal stability of BNTF was determined by DSC and TG‐DTG methods. Apparent activation energy Ea(147.83 kJ·mol-1),pre‐exponential factor A(9.33×1015 min-1)and decomposition rate constant k (2.18×10-44)of thermal decomposition reaction for BNTF were calculated by Kissinger method,Rogers method and Arrenhis method,respectively. The detonation velocity(8.3 km·s-1)and detonation pressure(31.3 GPa)of BNTF were estimated by Ka‐mlet‐Jacobs equation. Characteristic drop height of impact sensitivity(H50=43.0 cm)and friction sensitivity(36.0%)for BNTF were measured according to GJB772A-1997 methods 601.2 and 602.1,respectively.

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王珀会,曾炼,谌思嘉,等. BNTF的合成、单晶结构和性能[J].含能材料,2021,29(1):70-77.
WANG Po-hui, ZENG Lian, SHEN Si-jia, et al. Synthesis, Crystal Structure and Performances of BNTF[J]. Chinese Journal of Energetic Materials,2021,29(1):70-77.

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History
  • Received:July 20,2020
  • Revised:November 18,2020
  • Adopted:November 03,2020
  • Online: November 12,2020
  • Published: January 25,2021