Exploring the wet mechanochemical synthesis of Mg-Al, Ca-Al, Zn-Al and Cu-Al layered double hydroxides from oxides, hydroxides and basic carbonates

Abstract

The synthesis of Mg-Al, Ca-Al, Zn-Al and Cu-Al layered double hydroxides (LDHs) was investigated with a one-step wet mechanochemical route. The research aims to expand on the mechanochemical synthesis of LDH using a mill designed for wet grinding application. A 10% slurry of solids was added to a Netzsch LME 1 horizontal bead mill and milled for 1 h at 2000 rpm. Milling conditions were selected according to machine limitations and as an initial exploratory starting point. Precursor materials selected consisted of a mixture of oxides, hydroxides and basic carbonates. Samples obtained were divided such that half was filtered and dried at 60 °C for 12 h. The remaining half of the samples were further subjected to ageing at 80 °C for 24 h as a possible second step to the synthesis procedure. Synthesis conditions, such as selected precursor materials and the MII:MIII ratio, were adapted from existing mechanochemical methods. LDH synthesis prior to ageing was successful with precursor materials observably present within each sample. No Cu-Al LDH was clearly identifiable. Ageing of samples resulted in an increase in the conversion of raw materials to LDH product. The research offers a promising green method for LDH synthesis without the production of environmentally harmful salt effluent. The synthesis technique warrants further exploration with potential for future commercial up-scaling.