The effects of pyrite and diaspore with different particle sizes on the rheological properties of pulp with butyl xanthate added as a collector were studied, and the mechanism for rheological pyrite separation from diaspore by flotation was probed. The apparent viscosity of the diaspore pulp with different particle sizes was higher than that of pyrite, especially for -30 μm diaspore. Microfine diaspore was an important component affecting the apparent viscosity and yield stress of the diaspore-pyrite mixed pulp, and the pulp became a non-Newtonian fluid when the mass fraction of fine-grained diaspore in the mixed pulp was high. In this study, sodium hexametaphosphate (SHMP) was used to control the rheology of the mixed pulp and improve the pyrite flotation, and the S (sulfur) recovery rate first increased and then decreased with increasing SHMP concentration. The apparent viscosity of the pulp decreased by 3.01% and the S recovery rate increased by 34.83% when the amount of added SHMP was 0.05 mg/kg. The apparent viscosity with 0.50 mg/kg SHMP was 21.76% lower than that seen with the addition of 0.05 mg/kg SHMP, but the S recovery rate was also reduced by 14.94%. Further research showed that the increased SHMP concentration led to increases in the electronegativities of the particle surface and the repulsive force between particles, which prevented agglomeration of the particles, reduced the apparent viscosity and yield stress of the mixed pulp, promoted collisions between the pyrite particles and the bubbles, and reduced the resistance of the air bubbles to flotation.