Extraction of Caprolactam with an Alternative Benign Solvent in a Pulsed Disc and Doughnut Column

Abstract

Caprolactam is obtained by extraction using organic solvents like benzene, toluene, or chlorinated hydrocarbons. As an alternative solvent, the mixed solvent heptane‐heptanol (40 mass %) was selected in previous studies based on a relatively high distribution ratio of caprolactam, a low mutual solvent solubility, beneficial physical properties, and a low distribution ratio of impurities. Now, the hydraulic and mass transfer characteristics of the extraction of caprolactam in a pulsed disc and doughnut column (PDDC) were investigated using the benign solvent. The results were compared to those for toluene. The PDDC showed qualitatively comparable operational characteristics for both solvents. In the hydraulic experiments the mixed solvent showed smaller drop diameters and hold‐ups, required lower pulsation intensities for regime transitions, but the operational windows are slightly smaller. For both solvents, mass transfer resulted in increasing drop diameters and pulsation intensities required for regime transition. In the forward extraction the mixed solvent was superior, where HETS/m=0.26 to 0.37, compared to 0.42 to 0.67 for toluene, while less theoretical stages are required as well. For the back‐extraction HETS/m=0.33 to 0.40 for the mixed solvent compared to 0.30 to 0.37, but toluene requires the lower amount of theoretical stages. The hydraulic characteristics at equilibrium and concentration profiles in both the forward and back‐extraction were described accurately using the developed models.