trimethyl benzene (TMB) was used as organic swelling agent in O/W emulsions to template ul-tra-large mesoporous materials using the hydrothermal method. The silicas with well-defined mesopores and hydro-thermally robust framework were characterized by X-ray diffraction, transmission electron microscopy and BET surface area analysis. The influence of the quantity of TMB during preparation was studied. It has been found that the TMB/CTAB ratio must be controlled for producing high pore volume materials. Polysulfone (PSU), as the usual extraction agent, was coated on the silicas with the solvent evaporation method to produce a solid separation medium. The adsorptivity and the surface area of the coated MCM were determined: 10% PSU coated MCM adsorbed twice as much phenol as the un-coated material, reaching 0.5 mg/g silica. It was found that the surface area of the coated material decreased rapidly with an increase of the PSU loading. trimethyl benzene (TMB) was used as organic swelling agent in O / W emulsions to template ul-tra-large mesoporous materials using the hydrothermal method. The silicas with well-defined mesopores and hydro-thermally robust framework were characterized by X-ray diffraction , The transmission electron microscopy and BET surface area analysis. The influence of the quantity of TMB during preparation was studied. It has been found that the TMB / CTAB ratio must be controlled for producing high pore volume materials. Polysulfone (PSU), as the usual extraction agent, was coated on the silicas with the solvent evaporation method to produce a solid separation medium. The adsorptivity and the surface area of ​​the coated MCM were determined: 10% PSU coated MCM adsorbed twice as much phenol as the un-coated material, reaching 0.5 mg / g silica. It was found that the surface area of ​​the coated material was rapidly with an increase of the PSU loading.