New hybrid composite materials were prepared by polymerization of resorcinol–formaldehyde resins in the presence of bentonite with various contents of polymer and water, and then exposed to pyrolysis in an inert atmosphere at 800 °C. The influence of the filler and synthesis method on the morphological, textural and structural characteristics has been described. The materials were characterized using low temperature nitrogen adsorption–desorption, small angle X-ray scattering, scanning electron microscopy, Raman spectroscopy, differential scanning calorimetry (DSC), and thermogravimetry analysis (TGA). The maximal values of the specific surface area of organo-bentonite and carbonized samples were 254 and 200 m2/g, respectively, which is much larger than that of the initial bentonite. The TGA and DSC experiments showed changes in the thermal stability of samples depending on their composition. The obtained data could provide a better understanding of the principles of preparing hybrid bentonite-containing composites that may provide an additional incentive to develop advanced technologies.
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