Sodium alginate, a biopolymer extracted from brown algae, has shown great potential for many applications, mainly due to its remarkable biocompatibility and biodegradability. To broaden its fields of applications and improve material characteristics, the use of nanoreinforcements to prepare nanocomposites with enhanced properties, such as carbonaceous structures which could improve thermal and mechanical behavior and confer new functionalities, is being studied. In this work, graphene oxide was obtained from graphite by using modified Hummers' method and exfoliation was assisted by sonication and centrifugation, and it was later used to prepare sodium alginate/graphene oxide nanocomposites. The effect that different variables, during preparation of graphene oxide, have on the final properties has been studied. Longer oxidation times showed higher degrees of oxidation and thus larger amount of oxygen-containing groups in the structure, whereas longer sonication times and higher centrifugation rates showed more exfoliated graphene sheets with lower sizes. The addition of graphene oxide to a biopolymeric matrix was also studied, considering the effect of processing and content of reinforcement on the material. Materials with reinforcement size-dependent properties were observed, showing nanocomposites with large flake sizes, better thermal stability, and more enhanced mechanical properties, reaching an improvement of 65.3% and 83.3% for tensile strength and Young's modulus, respectively, for a composite containing 8 wt % of graphene oxide.