There is 0.032% cobalt and 0.56% sulfur in the cobalt-bearing V–Ti tailings in the Panxi Region, with the metal sulfide minerals mainly including FeS2
, and (Fe,Co)S2
, and the gangue minerals mainly including aluminosilicate minerals. The flotation process was used to recover cobalt and sulfur in the cobalt-bearing V–Ti tailings. The results showed that an optimized cobalt–sulfur concentrate with a cobalt grade of 2.08%, sulfur content of 36.12%, sulfur recovery of 85.79%, and cobalt recovery and 84.77% were obtained by flotation process of one roughing, three sweeping, and three cleaning under roughing conditions, which employed pulp pH of 8, grinding fineness of <0.074 mm occupying 80%, flotation concentration of 30%, and dosages of butyl xanthate, copper sulfate, and pine oil of 100 g/t, 30 g/t, and 20 g/t, respectively. Optimized one sweeping, two sweeping, and three sweeping conditions used a pulp pH of 9, and dosages of butyl xanthate, copper sulfate, and pine oil of 50 g/t, 15 g/t, 10 g/t; 25 g/t, 7.5 g/t, 5 g/t; 20 g/t, 5 g/t, 5 g/t, respectively. Optimized one cleaning, two cleaning, and three cleaning condition dosages of sodium silicate of 200 g/t, 100 g/t, 50 g/t, respectively. Study of analysis and characterization of cobalt–sulfur concentrate by X-ray diffraction (XRD), automatic mineral analyzer (MLA), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS) showed that the main minerals in cobalt–sulfur concentrate are FeS2,
, of which FeS2
accounted for 65.64% and Co3
for 22.64%. Gangue minerals accounted for 11.72%. The element Co in (Fe,Co)S2
is closely related to pyrite in the form of isomorphism, and the flotability difference between cobalt and pyrite is very small, which makes it difficult to separate cobalt and sulfur. Cobalt–sulfur concentrate can be used as raw material for further separation of cobalt and sulfur in smelting by pyrometallurgical or hydrometallurgical methods.