Fabricating effective oil/water separation materials to cope with significant industrial organic pollutants and oil spills requires procedures that are not only inexpensive and environmentally benign, but also simple to scale up. In this article, we describe a simple and efficient way of fabricating titanium disulfide (TiS2)-anchored candle-soot (CS)-decorated carbon nanofiber (CNF) membrane by a series of electrospinning, carbonization, and solvothermal growth techniques. The prepared TiS2/CS:CNF membrane is well characterized using SEM, EDS, XRD, Raman, AFM, and a contact angle goniometer. The NF membrane had an exceptional hydrophobic and oleophilic characteristics, with a water contact angle (WCA) of similar to 133 degrees and oil contact angle (OCA) of similar to 3 degrees, respectively. Different oil/water mixtures were subsequently separated using the membrane, and after 15 cycles, the separation efficiency was recorded to be similar to 99% for gasoline. Because of its superior multicycle efficiency as well as its stability, the TiS2/CS:CNF membrane plays a significant role in the implementation of oil/water separation in real-world conditions.