Abstract: A process for the separation of carbon dioxide from gas mixtures is disclosed in which a metal oxide sorbent, which is used to capture and release carbon dioxide, is recycled. The process incorporates the regeneration of the carbon dioxide capture capacity of the metal oxide to maintain a high capture capacity over many cycles. The regeneration involves hydrating the metal oxide and then heating the resulting metal hydroxide under a gas atmosphere that is effective to suppress the dehydration of the hydroxide so that dehydration occurs at an elevated temperature. The regeneration may also be used independently from the carbon dioxide separation process to produce, from a metal hydroxide, a metal oxide having an enhanced resistance to attrition and fragmentation.