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http://dx.doi.org/10.14478/ace.2015.1109

Optimization of a Crystallization Process by Response Surface Methodology  

Lee, Se-Eun (Department of Chemical and Biomolecular Engineering, Sogang University)
Kim, Jae-Kyeong (Department of Chemical and Biomolecular Engineering, Sogang University)
Han, Sang-Keun (Hanwha R&D center)
Chae, Joo-Seung (Agency for Defense Development)
Lee, Keun-Duk (Agency for Defense Development)
Koo, Kee-Kahb (Department of Chemical and Biomolecular Engineering, Sogang University)
Publication Information
Applied Chemistry for Engineering / v.26, no.6, 2015 , pp. 730-736 More about this Journal
Abstract
Cyclotrimethylene trinitramine (RDX) is a high explosive commonly used for military applications. Submicronization of RDX particles has been a critical issue in order to alleviate the unintended and accidental stimuli toward safer and more powerful performances. The purpose of this study is to optimize experimental variables for drowning-out crystallization applied to produce submicron RDX particles. Effects of RDX concentration, anti-solvent temperature and anti-solvent mass were analyzed by the central composite rotatable design. The adjusted determination coefficient of regression model was calculated to be 0.9984 having the p-value less than 0.01. Response surface plots based on the central composite rotatable design determined the optimum conditions such as RDX concentration of 3 wt%, anti-solvent temperature of $0.2^{\circ}C$ and anti-solvent mass of 266 g. The optimum and experimental diameters of RDX particles were measured to be $0.53{\mu}m$ and $0.53{\mu}m$, respectively. The regression model satisfactorily predicts the average diameter of RDX particles prepared by drowning-out crystallization. Structure of RDX crystals was found to be ${\alpha}$-form by X-ray diffraction analysis and FT-IR spectroscopy.
Keywords
cyclotrimethylene trinitramine; drowning-out; central composite rotatable design;
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