In this work, toluene and carbon disulfide have been employed as solvents to obtain sulfur out of sulfur concentrate. Sulfur concentrate is produced as residue in the flotation of zinc industry, coming from the leaching process of zinc concentrate. Up to 86.7% of sulfur is recovered using toluene at 100 °C, and a 96.3% of high purity sulfur recovered at room temperature using carbon disulfide as solvent. The X-ray diffraction of the obtained sulfur is very similar to the commercial sulfur, and the diffraction data of the residue show no peak of sulfur. The results are compared to the evaporation-condensation method previously used with similar samples.