Crystallization of phenanthrene from toluene with carbon dioxide by the GAS process

The crystallization of phenanthrene from toluene with carbon dioxide as the antisolvent gas is described. In the GAS process, a pressurized gas is dissolved into a liquid solvent, where it causes a volumetric expansion and lowers the solubility of the solute. Theoretical models ave presented for the liquid-phase expansion and the solubility as a function of pressure and temperature. The Nyvlt theory for batch crystallization is adapted to predict the pressure profile in the crystallizer needed to maintain a constant supersaturation and growth rate. Generation of seeds is accomplished via a pressure pulse at the saturation pressure. The average particle size of the phenanthrene could be varied from 160 to 540 mu m. Creation of seeds doubles the particle size and reduces the coefficient of variation significantly. The residual amount of toluene in the crystals without treatment is approximately 70 ppm. The particles are agglomerates of phenanthrene crystals.