Oil spill accidents are presented as a severe environmental problem because they cause ecological damage in the short and long term, especially in the aquatic environment. For this reason, the development of efficient materials to separate oil/water mixtures is fundamental. Studies have been performed using aerogels to fulfill this purpose because they are materials with a high porosity and high surface area, formed by solid particle networks and interconnected pores; these properties make them ideal for application as petroleum adsorbents. In this study, a simpler synthesis process using only renewable and environmentally friendly reagents for obtaining hollow carbon fiber/carbon quantum dots composite aerogels (CF-QD) is presented. Sorbent materials were prepared using an easy dip-coating technique and pyrolysis. Analyzing the effect of the concentration of carbon quantum dots (CQDs) in aerogels on the properties and adsorption capacity. CF-QD manifested remarkable characteristics, including a high surface area (up to 360.7 m2/g), hydrophobic surface, excellent buoyancy, and good adsorption capacity (up to 84.1 g/g). These features make them a viable option for application as sorbents for organic liquids, including oil.