Herein, we report a single-step carbonization approach for fabricating high-performance three-dimensional (3D) porous and superhydrophobic carbon-aerogel (S-CA) from edible sugar. S-CA has been used here to remove many substances, including various solvents (polar protic and aprotic, nonpolar, and oily), oils (crude, engine, waste cooking oil, etc.), and nitroaromatics (p-nitrophenol, dinitrophenol, 3-nitroaniline, and 4-nitroaniline) compounds based on their adsorption abilities. The superhydrophobic nature of porous S-CA has been supported by a static contact angle of ∼155° and the formation of a silver mirror-like surface when contacted with the surface of the water. S-CA adsorption capabilities were used to separate crude petroleum oil, waste engine oil, and a few other types of waste oil (waste cooking, silicon oil, and mustard oil) from the aqueous medium. Moreover, absorption analyses were extended to the adsorption and recovery of the toxic nitroaromatic pollutants from the aqueous medium. The nitroaromatics were recovered from the S-CA using ethyl acetate with a percentage recovery of more than 95%. Kinetic and intraparticle diffusion studies are being studied to understand the type and various stages of adsorption.