Prototype high-throughput system for hydrothermal synthesis and X-ray diffraction of microporous and mesoporous materials

Abstract

In the hydrothermal synthesis of microporous and mesoporous materials a large number of parameters including chemical composition of the mixture, reagent sources, organic templates, temperature, and time play a role. The high-throughput experimental approach facilitates screening of this multi-parameter space for conditions favoring formation of desired zeolite phases and ordered mesoporous materials. A critical issue in the development of a high-throughput system for hydrothermal synthesis is the avoidance of cross-contamination between the individual synthesis volumes. Further important issues are automation of reactant dosing, product filtration, calcination and identification. In this work, a prototype multi-clave was designed with three 5 mL synthesis vials for operation at temperatures up to 200 °C under autogenous pressure. The multi-clave is equipped with a sample tray for filtration, washing and drying of all of the synthesis products at the same time. This multi-filter also serves as the sample holder for X-ray diffraction characterization. The innovation resides in the multi-clave concept and the integration of the entire process from synthesis over product workup to XRD characterization without necessitating individual sample transfer. The performance of the prototype was evaluated with the synthesis of the mesoporous–microporous hybrid material zeotile-2, and of clathrasils.