Oil/water separation using membrane technology has gained a tremendous attention in the recent years. In the present study, a nanohybrid consisting of carboxylated carbon nanotubes and graphene oxide nanosheets (CNTs/GO) was embedded in polysulfone hollow fiber membranes (P HFMs) with an aim to improve their physicochemical properties, mainly surface functionality, hydrophilicity, mechanical strength and surface charge, and separation performance including antifouling property, water permeation flux and oil/water separation. It was found that the blending of nanohybrid in HFMs showed the positive effect on the properties of HFMs with high hydrophilic nature (water contact angle of ∼51.4°), high mechanical strength (Young’s modulus of 510.2 ± 12.4 MPa) and high negative surface charge (zeta potential of – 35.9 ± 2.5 mV). Notably, high pure water permeability (487.9 ± 25.4 mL/m²/h/mmHg), superior antifouling property with 90.5% flux recovery, and significantly high oil/water separation (98.7 ± 1.2%) were measured for Psf composite HFMs with 1 wt.% CNTs/GO nanohybrid. Thus, this study, through the above-obtained experimental results, demonstrated the potential efficacy of the polysulfone-CNTs/GO composite HFMs for efficient oil/water separation.