The need and preparation of spherical 1,1-diamino-2,2-dinitroethene
(FOX-7) particles to meet certain special applications in high explosives
and propellant formulation have been illustrated. Preparation of spherical
FOX-7 particles by using a microemulsion technique has not been reported
in the literature. In the present study, the preparation of spherical
FOX-7 particles has been described using the novel concept of a micelle-based
nanoreactor. Micelle-based nanoreactors have been prepared using a
microemulsion of Triton X-100, cyclohexane, and water. Formation of
spherical FOX-7 particles in the reverse micelle reactors have been
described in the subsequent sections of this article. It is observed
that spherical particles of FOX-7 are formed within 2 h in the microemulsion
media. Analysis of the experimental results revealed that the particle
size and shape of FOX-7 can be varied by changing the water/surfactant
molar ratio in the microemulsion. Spherical particles synthesized
by this method have diameters that are generally in the submicrometer
to nanometer range. Impact sensitivity (h
50) of the spherical particles obtained by the fall-hammer method is
around 45 cm compared to regular synthesized FOX-7 (i.e., 50 ±
5 cm) without any change in friction sensitivity, i.e. 36 kg. Loadability
of the explosive charges can be enhanced by using these spherical
particles of FOX-7.
A thermally stable, insensitive, high-explosive 1,3,5-triamino-2,4,6-trinitrobenzene
(TATB) is manufactured by amination of 1,3,5-trichloro-2,4,6-trinitrobenzene
in toluene with NH3 gas. An orange–red, sensitive
impurity, 1,3,5-triamino-2-chloro-4,6-dinitrobenzene (TACDNB), was
found forming with product TATB in the pilot-plant process. This impurity
was isolated and characterized by single-crystal XRD, NMR, FTIR, DSC,
and sensitivity test. The chemical reactivity of this impurity with
aqueous sodium hydroxide solution was also studied. The process anomalies
which led to the formation of this impurity with product TATB were
investigated. This TACDNB impurity was formed due to amination of
1,3,5,6-tetrachloro-2,4-dinitrobenzene (T4) when excess
NH3 gas was fed into the reactor.
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