Monitoring and controlling zeolite synthesis via reactor-based solutions: a fed-batch strategy

Abstract

Most conventional zeolite synthesis takes place in closed batch autoclaves that cannot be monitored or controlled during the process. Moreover, the study of time-dependent parameters of the synthesis with the conventional “cooling-opening” procedure not only reduces accuracy as a series of reactors (never 100% identical) needs to be started in parallel (and stopped at different times), it is also labor intense. Furthermore, the classic batch concept does not permit the intermediate addition of species without disrupting synthesis and the cooling-reheating effects. In this study, we developed a technique for zeolite synthesis monitoring in one-pot experiments using the sampling feature of fed-batch (FB) reactors. These one-pot syntheses can save time and ingredients instead of performing plenty of classic batch experiments. In addition, we could control and manipulate the zeolite synthesis by using the feeding function of the FB reactor and the intermediate addition of precursors at operational temperatures and pressures. Stannosilicate and zincosilicate syntheses were carried out via the FB reactor to investigate the intermediate timed-addition and the possibility of optimizing feeding rates of heteroatoms opposed to a classic synthesis, which faces challenges when a high amount of heteroatom precursor presents at the start. Finally, a modified FB platform was further developed to be able to monitor essential kinetic and synthetic parameters on-line (T, P, and also pH) on-line without intervention. For instance, pH profiles can allow one to estimate key events in zeolite synthesis, but in the art, these profiles are always measured ex situ (including cooling effects etc.).