Developing novel filtering materials with both high permeation flux and rejection rate presents an enticing prospect for oil/water separation. In this paper, robust porous poly(melamine formaldehyde) (PMF) sponges with superwettability and controlled pore sizes through introducing layered double hydroxides (LDH) and SiO 2 electrospun nanofibers are reported. The LDH nanoscrolls endow the sponge with inherent superhydrophilicity and the SiO 2 nanofibers act as pore size regulators by overlapping the PMF mainframe. This approach allows the intrinsic large pores in the pristine sponge to decrease quickly from 109.50 to 23.35 µm, while maintaining porosity above 97.8%. The resulting modified sponges with varied pore sizes can effectively separate a wide range of oil/water mixtures, including the surfactant-stabilized emulsions, solely by gravity, with ultrahigh permeation flux (maximum of 3 × 10 5 L m −2 h −1 bar −1 ) and satisfactory oil rejection (above 99.46%). Moreover, separation of emulsions stabilized by different surfactants, such as anionic, nonionic, and cationic surfactants has been investigated for further practical evaluation. It is expected that such a pore size tuning technology can provide a low cost and easily scaled-up method to construct a series of filtering materials for high-efficient separation of target oil/water mixtures.
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