Triple graphite nitrate cointercalation compounds (GNCCs) with acetic acid were synthesized, characterized by powder XRD and SEM methods, and used as a source of the thermally expanded graphite (TEG). Structural reorganization of graphite nitrate-acetate and triple GNCCs with acetic acid as a result of their exposition in air is discussed on the base of powder XRD data. Dispersions of carbon nanoparticles were prepared by liquid phase exfoliation of TEGs obtained from the GNCCs. It was demonstrated by TEM method that using of the studied TEGs as a source of carbon nanoparticles favours formation of few-layered graphene.