Hybrid Preceramic Aerogels for Oil and Solvent Cleanup

This study presents the first synthesis and characterization of monolithic hybrid preceramic aerogels using distinct drying techniques: ambient pressure (ambigels) and CO₂ supercritical drying. Polymeric ambi/aerogels, derived from polyhydromethlysiloxane (PHMS) and divinylbenzene (DVB), are processed at 200 °C, while hybrid ceramic‐polymer (ceramer) is produced through pyrolysis at 600 °C. Despite variations in drying methods, polymer and ceramer ambi/aerogels exhibit comparable microstructural characteristics, bulk density, pore size and volume, and specific surface area (542–841 m² g⁻¹). Polymeric and ceramer ambigel with 90 vol% total porosity yield a compressive strength, reaching 2.5 MPa, demonstrating a low thermal conductivity of 0.046 W m⁻¹ K⁻¹. Sorption tests are conducted using oil and organic solvents in aqueous media to benefit their high hydrophobicity (112° < θ < 142°). Aerogels exhibit high sorption capacities: 13.17 g g⁻¹ for sesame oil, 11.74 g g⁻¹ for toluene, and 9.19 g g⁻¹ for n‐hexane. The sorption rate for the oil is nearly 10 times slower than that for toluene and n‐hexane. Regarding regeneration and reusability, polymer and ceramer aerogels show consistent sorption properties cycles tested for n‐hexane and toluene.