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The residence-time distribution (RTD) studies are needed to characterize mixing conditions, flow patterns, and the extent of conversions and reactions of the biopolymers in any plasticating or cooking extruder. For the supercritical fluid extrusion process (SCFX), mixing of the fluid and starch-based biopolymers is an important step affecting cell nucleation and growth. RTD was studied in the mixing zone of the extruder, where CO 2 and gelatinized starch are brought together. Three levels of each of the process variables (screw speed and CO 2 injection pressure) were investigated, using specially designed apparatus for color-dye injection, and a die-restrictor to change the pressure profile and holdup volume in the extruder. Control RTD plots were for no CO 2 injection conditions at the same pressure, and the RTD of the full extruder section. Experimental RTDs were evaluated by: (1) the Wolf-White model, (2) a cascade of continuously stirred reactors (CSTR) model and (3) a model based on plug-flow in series with cascade of CSTRs. The last approach was most successful in capturing all aspects of the observed RTD curves including their tails. Injection of CO 2 at the highest pressure (110.3 bar) increased the RTD compared to no CO 2 -injection conditions. There were significant differences in the plug flow component of the RTD as well as differences in average residence time as a function of both screw speed and CO 2 injection pressure conditions.

The effect of pressure on diffusivity in binary or multicomponent systems such as gas−liquid or gas−solid systems has rarely been reported. The diffusivity of carbon dioxide in extruded gelatinized starch has been measured in this study at pressures of up to 117 bar (1700 psi). Such data are fundamentally not only useful in the understanding of the supercritical carbon dioxide (SC-CO2)/starch systems but also can be useful for the design and control of processes utilizing carbon dioxide injection or mixing in starch-based matrices. The methodology developed here was an improvement over a previously reported technique, enabling high-pressure data to be obtained. The diffusivity of carbon dioxide in the melt was found to be a strong function of pressure but not of moisture content in the range of 34.5−39% (w/w) studied. This diffusivity value decreased from 7.5 × 10-10 to 0.9 × 10-10 m2/s as pressure was increased from atmospheric to 115 bar. The low-pressure diffusivity value was only an order of magnitude...

Using supercritical carbon dioxide (SC-CO2) as the solvent, the solubility of methyl esters, ethyl esters, fatty acids, triglycerides, and fats and oils were studied over a range of temperature and pressures. Equilibrium data from the literature were correlated using the Peng-Robinson equation of state. With the van der Waals (VDW) and Panagiotopoulos and Reid (PR) mixing rules. The data were also correlated using statistical methods and the solubilities predicted by various models were compared with experimental solubilities at the temperature and pressure conditions studied. The equation of state method provided good agreement of theory with experiment for the solubilities of fatty acids and their esters, but less so for the triglycerides, fats and oils. The statistical methods on the other hand, not only predicted the solubilities of fatty acids and fatty acid esters well, but also gave good agreement with the solubilities of triglycerides, fats and oils. Chain length, degree of unsaturation, and functional groups in compounds are known to affect the vapor pressures of these compounds which in turn influence their solubilities in SCCO2. As expected solubilities decreased in going from fatty acid esters, to fatty acids, to triglycerides.