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Electrodeposited antimony can be treated with sulfuration–volatilization technology, which causes antimony to volatilize in the form of antimony sulfide. During this process, gold is enriched in the residue, thereby realizing the value-added use of antimony and the recovery of gold. In this study, the thermodynamic conditions of antimony sulfide were analyzed by the Clausius–Clapeyron equation. Moreover, the volatilization behavior of antimony sulfide and the enrichment law of gold were studied by heat volatilization experiments. The effects of the sulfide temperature and volatilization pressure on the separation efficiency of antimony and gold enrichment were investigated. The results demonstrate that the sulfuration rate was the highest, namely 96.06%, when the molar ratio of sulfur to antimony was 3:1, the sulfur source temperature was 400 °C, the antimony source temperature was 550 °C, and the sulfuration time was 30 min. Antimony sulfide prepared under these conditions was volatilized at 800 °C over 2 h at an evaporation pressure of 0.2 atm, and the volatilization rate was the highest, namely 92.81%. Antimony sulfide with a stibnite structure obtained from the sulfuration–volatilization treatment of electrodeposited antimony meets the ideal stoichiometric ratio of sulfur and antimony in Sb2S3 (3:2), and gold is enriched in the residue.

Preparation of Antimony Sulfide and Enrichment of Gold by Sulfuration–Volatilization from Electrodeposited Antimony