The morphology and mechanical properties of the in situ microfibrillar blend based on isotactic polypropylene (iPP) and poly (phenylene sulfide) (PPS) were examined. The microfibrillar PPS/iPP blend was prepared through a slit-die extrusion, hot stretching, and water quenching process. Morphological observation indicated that the well-defined PPS microfibrils were achieved by the method used in this study, which provided a promising method for both PPS and PP recycling. The morphology study showed that the minimum diameter of PPS phase was independent of PPS concentration. The diameter of most PPS fibrils in the microfibrillar blend was unexpectedly comparable to that of the PPS particles in the common blend at the same PPS content. The tensile strength of microfibrillar blend was higher than that of common blend, indicating the mechanical enhancement of microfibrillar processing to the PPS/iPP blend. The tensile strength of the microfibrillar blend also increased with stretching.