Supercritical Fluids Laboratories

Studies in the supercritical fluids (SCF) labs include fundamentals and applications of SCF's in polymer processing, nano-materials synthesis, organic waste destruction, surfactants and micro-emulsions, reaction engineering and pharmaceutical processing. These labs are fully equipped laboratories and fitted with appropriate fume hoods, utilities, safety equipment and instrumentation, including vacuum ovens, balances, rotary evaporators, etc. The SCF's labs are equipped with a custom high-pressure continuous flow reactor available for the study of catalytic reactions under supercritical fluid conditions. This reactor is equipped with a solvent delivery system (both Isco syringe pumps and HPLC metering pumps), gaseous reactant delivery systems (Brooks mass flow controllers), a downflow fixed bed catalytic reactor (HIP tube reactor), a back pressure regulator, high temperature and low temperature separator traps, and automated injection systems into two Gas Chromatographs (Varian 3300 FID gas chromatograph and a Varian 3800 TCD gas chromatograph) for full product analysis from C1 to C30 products. This system is also equipped with several safety devices including CO and H2 detector systems, shut off valves, power failure shut off valves, etc.

This reactor system is utilized to evaluate long-term activity and stability of the proposed catalysts, reactant conversions, product selectivies, etc. Spectroscopic studies under high pressure conditions are performed using a Varian Cary 3E UV-vis spectrophotometer, a Perkin Elmer Spectra 2000 FTIR spectrophotometer and a Nicolet Avatar FTIR spectrometer, along with custom built high pressure optical cells. FTIR experiments can be conducted in both transmittance and reflectance mode. Also available is an Ocean Optics Fiber Optics based UV-vis spectrometer system that can be used with the high pressure vessels in-situ.

The SCF labs have several high pressure vessels (custom) fitted with optical windows for both UV-vis and IR work with on- line sampling ports. Multiple Isco 260D and Isco 500D high pressure syringe pumps are available along with several Heise digital pressure gauges, Omega pressure transducers, and temperature controllers. The SCF labs also have several high pressure variable volume view cell devices for measurement of phase behavior of SCF systems.

Two supercritical water oxidation systems can be used to study chemical processing in supercritical water for environmental (e.g., oxidation of wastes) and nanotechnology (e.g., production of metal oxide nano-particles) applications. Pressure of up to 5000 psi and temperature of up to 500°C can be achieved in these systems, which are equipped with high-pressure Inconel reactors and HPLC pumps. A Water's HPLC system and dynamic light scattering device is available for product analysis. Two supercritical antisolvent systems employ supercritical carbon dioxide as an antisolvent to produce micro- and nano-particles of various compounds including pharmaceuticals. Enhanced mass transfer can be achieved using a Sonics and Material's ultrasound horn.

Last Updated: Feb 09, 2011