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Optimization of the Process Parameters for the Synthesis of High Purity 4,6‐Dinitrobenzofuroxan (4,6‐DNBF)
Author(s) -
Li JinShuh,
Chen FuJen,
Yang HsiuWen,
Lu KaiTai
Publication year - 2020
Publication title -
propellants, explosives, pyrotechnics
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.56
H-Index - 65
eISSN - 1521-4087
pISSN - 0721-3115
DOI - 10.1002/prep.201900413
Subject(s) - yield (engineering) , analytical chemistry (journal) , taguchi methods , fourier transform infrared spectroscopy , differential scanning calorimetry , materials science , thermogravimetry , scanning electron microscope , nitric acid , mass spectrometry , nuclear chemistry , chemistry , chromatography , inorganic chemistry , optics , physics , composite material , thermodynamics , metallurgy
4,6‐Dinitrobenzofuroxan (4,6‐DNBF) is explosive and can also be used as an important intermediate in the synthesis of other explosives. It can be prepared by nitrating benzofuroxan (BF) with mixed nitric/sulfuric acid. However, little is known about its optimal synthesis parameters in the preparation process. In this study, Taguchi's experimental design method was used to improve the yield of 4,6‐DNBF. A L 9 (3 4 ) orthogonal array with four control factors and three levels of each control factor was used to design nine experimental conditions. The experimental data were transformed into a signal‐to‐noise (S/N) ratio to analyze and evaluate the experimental conditions of the optimal parameter combination for the maximum yield of 4,6‐DNBF. The verification results indicated that the optimal synthesis parameters were as follows: nitration temperature was 40 °C, mass ratio of BF to H 2 SO 4 , was 1 : 15, volume ratio of HNO 3 to H 2 SO 4 was 1 : 2.0 and reaction time was 4 hours, and then the maximum crude yield and the maximum yield after purification could reach 73.2 % and 49.0 %, respectively. Furthermore, the synthesized 4,6‐DNBF was identified by scanning electron microscopy (SEM), nuclear magnetic resonance spectrometer (NMR), Fourier transform infrared spectrometer (FTIR), elemental analyzer (EA), ultraviolet‐visible spectrometer (UV‐Vis) and thermogravimetry‐differential scanning calorimetry (TG‐DSC), and its sensitivity was determined using BAM fallhammer, BAM friction tester, and electrostatic spark sensitivity tester.