Versatile semi-batch apparatus for manometric measurement of gas–solid reaction rates

Abstract

We describe the design, construction, operation, and performance of a simple and versatile semi-batch reactor that is especially useful for measurement of gas/solid reaction rates at pressures in the range of 1 mTorr to 1500 Torr. The reactor operates by repeatedly imposing small AC modulations of reactant gas pressure on top of a much larger DC pressure background. Based on the rate of pressure relaxation following each AC pulse, the reaction rate is determined. Our design is characterized by modular construction from off-the-shelf, ultra-high-vacuum-compatible components, which facilitate easy retrofitting and adaptation to a range of experimental conditions. Automated experiment control and data acquisition is accomplished via a custom National Instruments© LabView virtual instrument. Data analysis is automated using a custom series of Mathworks© Matlab scripts. We demonstrate reactor performance through measurements of hydrogenation kinetics for a composite H2 getter material consisting of 1,4-bis(phenylethynyl)benzene mixed with a palladium/carbon catalyst.

Additively Manufactured Silicone Polymer Composite with High Hydrogen Getter Content and Hydrogen Absorption Capacity

“…Hydrogen absorption experiments were performed at low H 2 partial pressures, more representative of the working environments using the home-built reactor systems following the same procedure reported in the literature. , These reactors were constructed entirely from ultrahigh-vacuum-compatible components that were electroplated with gold to minimize the exchange of H 2 between stainless steel and the process gas. Each reactor system was contained within a FrioCell environmental chamber (BMT USA, Monroe, WA), which enabled temperature control to within ±0.05 °C in the range 0–100 °C.…”

Feedback Temperature Controller Design to a Semi-batch Hydrogenation Industrial Reactor - Part A: Modeling, Experimental Validation and Current Control System Evaluation

“…The hydrogenation reaction presents higher importance for different manufacturing fields, being widely employed in several types of industries, such as: (i) food industry, which uses the process to convert polyunsaturated fatty acids into fats as, for example, margarine (Gunstone et al 2009); (ii) energy industry, to stabilize biofuels (Souza et al 2012), in addition to produce light hydrocarbons via biomass (Huber et al 2005;Sotelo et al 2011), to obtain paraffin and naphthenes from alkanes and aromatics (Kong et al 2015) and hydrocracking heavy oil residues (Sahu et al 2015); (iii) In fine chemistry, in oxo (DU et al 2016) and amines processes (Lange et al 2016); (iv) drug processing (Klinger et al 2007).…”