(437f) Real-Time Analysis of Process Conditions During a Super-Saturation Controlled Recrystallization

As part of a parametric study in particle size control, 3-Nitro-1,2,4-triazol-5-one is being recrystallization under a condition of constant super-saturation level. A super-saturated solution is one in which the concentration of a solute dissolved in a solvent is higher than the saturation concentration of that solute in the same solvent at a given temperature. Super-saturation level is the difference in concentration between the supersaturated concentration and the equilibrium concentration (saturation concentration) at a given temperature. In order to maintain a constant super-saturation level, real-time analysis of process conditions within the reactor such as temperature, particle size, and dissolved energetic concentration are constantly measured and relayed back to the control system to automatically adjust reactor temperature along the desired cooling curve. This paper will discuss the results of how real-time analytical tools were used to control process parameters and effect particle size and distribution control.