Abstract: A process for recovering antimony and sodium compounds from antimony-containing spent ethylene glycol residues resulting from the manufacture of polyethylene-terephthalate polyester, which comprises combusting the spent glycol residues to produce an ash, and then contacting the ash with water to form an ash-water mixture having a liquid phase and a solid phase, the water-soluble sodium compounds being essentially contained in the liquid phase and the water-insoluble antimony compounds being essentially contained in the solid phase. The liquid phase and solid phase are then separated in order to recover therefrom sodium and antimony compounds, respectively.