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Different samples of graphite oxide (GrO) were prepared by modification of the Improved Hummers Method reported in the literature. Graphite was used as the raw material and KMnO4 and H2SO4 were used as chemical reagents. GrO samples were analyzed by Raman spectroscopy, SEM, TEM, elemental analysis, X-ray diffraction, N2 adsorption–desorption, and thermogravimetric analysis. The results indicate that, after optimizing the synthesis method, the oxidation time was reduced from 12 to 3 h, coagulation step was removed, wash step was halved, use of H3PO4 during the oxidation step was no longer necessary, the production of graphite oxide per batch was increased, and the amount of graphite that could be processed was increased five times. Therefore, synthesis costs were significantly lower than those related to the published Improved Hummers Method. An economic assessment for the industrial scale demonstrated that this process could be viable from the third year after its implementation.