In this study, we aimed to address challenges in thermal management and structural applications by developing composite materials with enhanced thermal conductivity and insulation properties. Our approach involved combining two-dimensional MoS2 2 nanosheets with carbon nanotubes (CNTs), leveraging their respective properties to create synergistic effects. MoS2, 2 , renowned for its remarkable electrical and mechanical attributes, was synthesized via a hydrothermal reaction and subsequently exfoliated using liquid-phase exfoliation techniques. Meanwhile, CNTs were surface-treated to prevent aggregation and ensure optimal dispersion within the composite matrix. These treated CNTs were then entangled with MoS2 2 nanosheets to form layered structures, facilitating the creation of efficient heat transfer pathways. The resulting MoS2-CNT 2-CNT composites were fabricated using a hot-pressing method, with polyphenylene sulfide (PPS) layers integrated for structural integrity. Through experimental investigation and characterization, our composites exhibited substantial improvements in thermal conductivity, achieving an impressive 5.77 W/mK. Additionally, the incorporation of PPS layers endowed the composites with insulation properties, further enhancing their suitability for diverse applications. Notably, the composite demonstrated a tensile strength of 67 MPa, indicating its potential for structural applications. This research underscores the promising potential of MoS2-CNT 2-CNT composites in addressing critical challenges in thermal management and structural engineering across various industries, including automotive and electronics. By offering a comprehensive solution that combines enhanced thermal conductivity, mechanical strength, and insulation properties, our composite material opens avenues for innovation in the development of advanced materials for next-generation technologies.