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Optimization of a Crystallization Process by Response Surface Methodology

반응표면분석법을 이용한 결정화 공정의 최적화

  • 이세은 (서강대학교 화공생명공학과) ;
  • 김재경 (서강대학교 화공생명공학과) ;
  • 한상근 ((주)한화대전사업장 종합연구소) ;
  • 채주승 (국방과학연구소) ;
  • 이근득 (국방과학연구소) ;
  • 구기갑 (서강대학교 화공생명공학과)
  • Received : 2015.10.08
  • Accepted : 2015.11.02
  • Published : 2015.12.10

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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