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2 Central European Journal of Energetic Materials

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Statistical Optimization of a Novel Approach for the Reductive Debenzylation of 2,4,6,8,10,12-Hexabenzyl-2,4,6,8,10,12-hexaazaisowurtzitane Using Pd@SiO2 Nano Catalyst

Zarandi M., Bayat Y., Zebardasti A., Khayrabadi A. A.

Central European Journal of Energetic Materials

2017

Vol. 14, no. 4

984--995

The synthesis of 2,6,8,12-tetraacetyl-4,10-dibenzyl-2,4,6,8,10,12-hexaazaisowurtzitane (TADB), from 2,4,6,8,10,12-hexabenzyl-2,4,6,8,10,12-hexaazaisowurtzitane(HBIW) is a key step in the preparation of 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (HNIW or CL-20). In this study, a novel highly efficient nano catalyst based on Pd@SiO2 was used for the reductive debenzylation of HBIW. It is notable that an orthogonal array design OA9 was applied as a statistical optimization method for the synthesis of TADB. The current application of the Taguchi method in optimizing the experimental parameters of the TADB synthetic procedure was successful. TADB was synthesized by investigating the effect of the reaction conditions, such as catalyst percentage, time (h) and temperature (°C). The effects of these factors on the yield of TADB were evaluated quantitavely by the analysis of variance (ANOVA). The Pd@SiO2 nano catalyst, consisting of a palladium core with SiO2 monolayer shells, was synthesized and characterized by SEM, TEM and IR spectroscopy. The optimum condition indicated that the use of fresh Pd@SiO2 nano catalyst provides a high yield (90%). The use of Pd@SiO2 nano catalyst after recovery gave a yield of 65%.

Statistical Optimization of the Preparation of HNIW Nanoparticles via Oil in Water Microemulsions

Bayat Y., Zarandi M., Khadiv-Parsi P., Salimi Beni A.

Central European Journal of Energetic Materials

2015

Vol. 12, no. 3

459--472

HNIW (2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane) is a family member of high-energy density cage nitramines which have so many versatile applications. In this paper, HNIW nanoparticles were prepared by the oil in water microemulsion route. The effects of various experimental parameters on this reaction were investigated using the Taguchi method. The effects of different variables: organic phase, water/organic phase (W1/W2), organic phase/ propanol (W3/W4) and HNIW weight percent, on the particle size of the HNIW were investigated at three distinct levels. Optimal conditions for obtaining HNIW nanoparticles were determined. Performing the process under the optimal conditions proposed by the Taguchi method leads to the production of HNIW nanoparticles with an average size of about 80 nm. The HNIW nanoparticles were characterized using Scanning Electron Microscopy (SEM), Dynamic Light Scattering (DLS), Differential Thermal Analysis (DTA) and X-Ray Diffraction (XRD).