In this study, the effects of ball milling (BM) technique and carbon nanotube (CNT) content on the thermal and mechanical properties of hybrid reinforced composites were investigated. The composites were prepared using glass fiber (GF), novolac resin (No), and CNTs with different wt% (1, 2, and, 4). Various milling times were used to optimize the entanglement/agglomeration of CNTs in the polymer matrix and subsequently enhance the final thermal and mechanical properties. Through precise investigations, it was found that the nanocomposite with 2 wt% CNT reinforcement, subjected to 2 h of BM, exhibited remarkable enhancements in key properties. The tensile strength was significantly improved to 45.6 MPa, while the elastic modulus reached 3.419 GPa. Hardness was measured at 96 HRM, and thermal conductivity was enhanced to 0.463 W/mK. Moreover, this sample demonstrated a weight loss that was 43.65% lower compared to the sample reinforced with 1 wt% CNT and subjected to 1 h of BM. Overall, this study highlights the importance of optimizing the milling time and CNT content in the preparation of polymer nanocomposites, and it provides valuable insights for the development of advanced materials with superior performance in various applications.