Process Design to Preserve Particle Properties during Crystallization of Energetic Material

Obtaining desired particle size and morphology of isolated material from a quenched crystallization can be challenging during scale up. This work focuses on the scale-up of a quenched crystallization of an energetic compound while maintaining a large blocky morphology of the isolated material. The compound has low solubility in most solvents, therefore recrystallization options were limited. In this case, the key to obtaining the desired particle size and morphology was quenching the reaction mixture into a nitrate salt solution. This talk will discuss the process optimization and the effects of mixing, temperature, and salt concentration on this quenched crystallization. Optimization and development efforts were performed in the 1-L Mettler Toledo OptiMax reactor before being scaled up to the pilot plant.