The study aimed to investigate the effect of processing temperature and the content of multi-wall carbon nanotubes (MWCNTs) on the rheological, thermal, and electrical properties of polyphenylene sulfide (PPS)/MWCNT nanocomposites. It was observed that the increase in MWCNT content influenced the increase of the complex viscosity, storage modulus, and loss modulus. The microscopic observations showed that with an increase in the amount of MWCNTs, the areal ratio of their agglomerates decreases. Thermogravimetric analysis showed no effect of processing temperature and MWCNT content on thermal stability; however, an increase in stability was observed as compared to neat PPS. The differential scanning calorimetry was used to assess the influence of MWCNT addition on the crystallization phenomenon of PPS. The calorimetry showed that with increasing MWCNT content, the degree of crystallinity and crystallization temperature rises. Thermal diffusivity tests proved that with an increase in the processing temperature and the content of MWCNTs, the diffusivity also increases and declines at higher testing temperatures. The resistivity measurements showed that the conductivity of the PPS/MWCNT nanocomposite increases with the increase in MWCNT content. The processing temperature did not affect resistivity.