Kenneth J. James, Ph.D.,* Supercritical Fluid Technologies, Inc.
Kenneth R. Krewson, Supercritical Fluid Technologies, Inc
Abstract
The goal of a high pressure laboratory reaction unit is to assess technical feasibility of pressurized reaction applications such as Catalytic Chemistry, Hydrolysis, Polymerization, Synthesis, and investigate Process Development. The High Pressure Laboratory Reaction Unit typically consists of a 50 ml to 4 liter reaction vessel fitted with the appropriate solvent (CO2, Liquid, or Gas) and reagent addition modules, mixing, heating/cooling, temperature controls, safety features, flow meters, sensors, and controls. Typical Operation conditions for these units are up to 10,000 psi (68.9 MPa) and 350 degrees Celsius.
Product samples and data from the laboratory unit feasibility testing can be used to assess product quality, and to research process variables such as:
1) Preparation and solubility of reagents
2) Reaction conditions (temperatures, pressures, use of Co-Solvents to enhance reactant or product solubility.
3) Collection conditions.
The reaction product is analyzed to determine how changes in these parameters change yield, purity, and economics of the proposed process. This information can then be utilized to fine tune the reaction to maximize key parameters for a commercial scale reaction process or simply be used for repetitive laboratory scale applications. Examples demonstrating the utility of a High Pressure Reaction Unit for traditional organic synthesis and supercritical fluid synthesis are presented.