Synthesis of layered double hydroxides: Investigating the impact of stirring conditions and reactor design parameters

Abstract

The synthesis by coprecipitation of Layered Double Hydroxides (LDHs) is governed by the stages of nucleation and crystal growth associated with the efficiency of the mixing and dispersion process of the reagents. Mixing efficiency is related to process variables, such as agitation speed, type of impeller and baffles presence, among others. In this context, this work proposes an analysis of these variables in a batch reactor, using a 23 factorial design employing the factors: acceleration speed (200 and 1000 rpm), mixing time (2 and 18 h) and presence or absence of baffles. The results were evaluated quantitatively (amount of LDH produced, time and amount of base for the formation of LDHs to begin) and qualitatively (mixing aspects, sedimentation ad grinding). The significant factors affecting the amount of LDH produced (51.94–80.81 g) were agitation speed and aging time. These factors were also correlated with the structural characteristics of the materials produced, such as crystallinity, crystallite size (70.99–174.79 nm), surface area (69.81–97.62 m2/g), pore volume (0.28–0.59 cm3/g), and pore diameter (11.40–34.66 nm). LDHs produced at higher agitation rates (1000 rpm) and longer aging times (18 h) yielded higher quantities of materials (80.81 g) with improved structural characteristics. The study highlights the importance of systematically exploring the synergistic effect between process variables, emphasizing the research potential in this area.