Influence of the bed geometry on the kinetics of rosemary compounds extraction with supercritical CO2

Bed geometry plays an important role in supercritical fluid extraction kinetics. Thus, the objective of this study was to compare the overall extraction curves (OEC's) of rosemary compounds obtained in two beds of 1 L each with different geometries (in terms of height to bed (H-B) diameter (D-B) ratios, H-B/D-B). A scale-up study was carried out maintaining the solvent mass to feed mass (S/F) ratio equal for both beds. Other process variables, such as bed porosity, apparent and true densities of the raw material, particle average size, temperature, pressure and time of extraction, were also maintained constant. The kinetic parameters were obtained by fitting the OEC to a spline model. The results revealed differences of mass transfer rates, mass ratios of solute in the fluid phase and yields of extract in the constant extraction rate period. The evaluation of the OEC's and kinetic parameters indicated that the bed with lower HB/DB ratio (H-B/D-B = 2.7) was more favorable for obtaining rosemary extract. The kinetics of extraction of oxygenated monoterpenes (i.e., 1,8-cineole and camphor) and phenolic diterpenes (i.e., camosic acid) were also different for both bed geometries. These behaviors suggest that the bed geometry presents a pronounced influence in the mass transport properties in supercritical media. Thus, in spite of the scale-up criterion be successful for several botanic matrices such as clove buds, sugarcane residue and grape seeds residue, the criterion applied in this study (maintaining a constant S/F ratio for a given time of extraction) was not suitable for this raw material. (C) 2014 Elsevier B.V. All rights reserved.