A valorization process of spent coffee grounds (SCG) was studied. Thus, a two-stage process, a stage of extraction of the polyphenols and a stage of obtaining activated carbon (AC) by a carbonization process, was performed. The extraction was carried out with a hydro-alcoholic solution in a pressure reactor, modifying time and temperature. To optimize the extraction of polyphenols, a two-level factorial design with three replications at the central values was used. The best results were obtained by performing the extraction at 80 °C during 30 min, using a mixture of EtOH:H2O 1:1 (v/v) as extraction solution. Caffeine and chlorogenic acid were the most abundant compounds in the analyzed extracts, ranging from 0.09 to 4.8 mg∙g^-1 and 0.06 to 9.7 mg∙g^-1, respectively. The precursor obtained in the extraction stage were transformed into AC. An experimental design was realized in order to analyze the influence of different variables in the AC obtained process (reaction time and amount of potassium hydroxide used). Actived carbons with BET specific surface (SBET) comprised between 1600 m^2∙g^-1 and 2330 m²∙g^-1 had a microporous surface. Under the optimum conditions, the obtained AC presented a maximum adsorption capacity of methylene blue (qm) between 411 mg∙g^-1 and 813 mg∙g^-1.