Utilization of Lithium Production Chain Waste
As a Zeolitic Precursor: Influence of Pre-treatments
Physico-chemical in the Synthesis of LTA and FAU of the NAX type.
silicoaluminate residue; LTA zeolite; FAU (NaX) zeolite; alkaline digestion;
alkaline fusion; mechanochemical activation; Lithium.
The processing of lithium-bearing minerals, such as spodumene, generates significant
volumes of silicoaluminous solid residues. Due to the presence of mineral phases with
high thermochemical stability, such as quartz and spodumene, this material represents a
challenging environmental liability, with limited recycling potential. As a valorization
alternative, this study aimed to develop and evaluate methodologies for the synthesis of
LTA and FAU (NaX) zeolites from this residue of the lithium production chain. The
research investigated the influence of different precursor pre-treatment routes—alkaline
digestion and alkaline fusion, with or without mechanical milling—correlating energy
consumption with the crystallinity, morphology, and textural properties of the obtained
materials. The syntheses were compared with commercial standards and characterized by
techniques such as XRD, SEM, and N₂ physisorption. The results demonstrated that
obtaining zeolitic phases from the residue necessarily requires the application of pre-
treatments, as no crystallization of the raw material was observed within 24 hours.
Alkaline digestion, characterized by lower energy demand, enabled the synthesis of LTA
with an optimal time of 4 hours and 37.21% relative crystallinity, but proved ineffective
for NaX formation. In contrast, alkaline fusion showed greater efficiency in dissolving
stable siliceous phases, promoting the formation of more satisfactory zeolitic structures.
Notably, the NaXRF zeolite obtained via alkaline fusion achieved 83.34% crystallinity
and high morphological correspondence to the standard. The milling step was shown to
increase surface area and generate structural defects beneficial to nucleation; however,
excessive mechanical energy favored particle aggregation and the formation of secondaryphases (sodalite), requiring careful optimization of these parameters. It is concluded that
lithium-bearing residue is a viable alternative source of silicon and aluminum. The
selection of the ideal synthesis route depends on the balance between energy consumption
and the structural requirements of the final application, with alkaline digestion being
suitable for less demanding uses, and alkaline fusion combined with optimized milling
recommended for the development of high-purity materials.