This study presents a rapid and efficient laboratory-scale process for removing lead from Pb–Sb alloy melts using a composite H3PO4–(NaPO3)6 flux. Thermodynamic analysis was combined with experimental investigation to elucidate the influence of key parameters on lead removal behavior. The Wilson equation was employed to describe the non-ideal behavior of the Pb–Sb system, enabling estimation of equilibrium lead contents and providing theoretical support for interpreting experimental trends. Under the investigated conditions (1073 K, H3PO4/(NaPO3)6 mass ratio of 2:1, and a holding time of 10 min), the Pb mass fraction was reduced from 10.0 wt.% to 0.018 wt.%, corresponding to a lead removal efficiency of 99.86%. Compared with the traditional refining processes, this method shortens the processing time and avoids the use of volatile gas reagents, demonstrating its potential for lead–antimony separation. The results provide thermodynamic and experimental insight into phosphate-based refining of crude antimony.
Tan et al. (Fri,) studied this question.