This work aimed to study the thermal and crystalline properties of poly (1,4-phenylene sulfide)@carbon char nanocomposites. Coagulation-processed nanocomposites of polyphenylene sulfide were prepared using synthesized mesoporous nanocarbon of coconut shell as reinforcement. The mesoporous reinforcement was synthesized using a facile carbonization method. The investigation of the properties of nanocarbon was done by SAP, XRD, and FESEM analysis. The research was further propagated via the synthesis of nanocomposite by the addition of characterized nanofiller into poly (1,4-phenylene sulfide) at five different combinations. The coagulation method was utilized for the nanocomposite formation. The obtained nanocomposite was analyzed using FTIR, TGA, DSC, and FESEM analysis. The BET surface area and average pore volume of bio-carbon prepared from coconut shell residue were calculated to be 1517 m2/g and 2.51 nm respectively. The addition of nanocarbon to poly (1,4-phenylene sulfide) has led to an increase in thermal stability and crystallinity up to 6% loading of filler. The minimum achievable glass transition temperature is for 6 % doping of filler into the polymer matrix. It was established that the thermal, morphological, and crystalline properties have been tailored by synthesizing their nanocomposites with mesoporous bio-nanocarbon obtained from coconut shells. So, the loading of filler into poly (1,4-phenylene sulfide) can be optimized to enhance its thermoplastic properties for surface applications.