We report a method for achieving controlled dispersion of graphene oxide (GO) in poly(methyl methacrylate) (PMMA) via the precipitation polymerization process in a water/methanol mixture. GO acts as a surfactant and adsorbs on the interface between polymerized PMMA particles and solvent mixture. Scanning electron and transmission electron microscopy confirmed that the precipitate consists of polymer particles (<1 μm) surrounded by the GO sheets. Compression molding of the precipitate yields a polymer nanocomposite with the GO organized into a regularly spaced 3D network which percolates at 0.2 wt % GO. Simple thermal reduction of the GO sheets dispersed in PMMA at relatively low temperature (210 °C) achieved electrical conductivity higher than 10 -2 S/m at 0.4 wt % of GO. Parallel dielectric and rheological characterization demonstrated that the thermal reduction is a quite fast process without significant degradation of the polymer. The study should open up new opportunities in the design of GO-based polymer nanocomposites.