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Calcium oxalates are naturally occurring biominerals and can be found as a byproduct of some industrial processes. Recently, a new and green method for carbon capture and sequestration in stable calcium oxalate from oxalic acid produced by carbon dioxide reduction was proposed. The reaction resulted in high-quality weddellite crystals. Assessing the stability of these weddellite crystals is crucial to forecast their reuse as solid-state reservoir of pure CO2 and CaO in a circular economy perspective or, eventually, their disposal. The thermal decomposition of weddellite obtained from the new method of carbon capture and storage was studied by coupling in-situ high-temperature X-ray powder diffraction and thermogravimetric analysis, in order to evaluate the dehydration, decarbonation, and the possible production of unwanted volatile species during heating. At low temperature (119–255 °C), structural water release was superimposed to an early CO2 feeble evolution, resulting in a water-carbon dioxide mixture that should be separated for reuse. Furthermore, the storage temperature limit must be considered bearing in mind this CO2 release low-temperature event. In the range 390–550 °C, a two-component mixture of carbon monoxide and dioxide is evolved, requiring oxidation of the former or gas separation to reuse pure gases. Finally, the last decarbonation reaction produced pure CO2 starting from 550 °C.

Thermal Stability of Calcium Oxalates from CO2 Sequestration for Storage Purposes: An In-Situ HT-XRPD and TGA Combined Study