Rapeseed and sunflower meals are the co-products of the pressing and de-oiling process of rapeseed and sunflower seeds and are usually used as animal feed. Rapeseed and sunflower hulls are other minor co-product of the oil industry. Among other major components (lignin, proteins, polysaccharides) these co-products contain a relatively high content of phenolic compounds which can be valorized. Most of the phenolic compounds remain in the meals (and the hulls) after processing the seeds. The aim of this work was to separate these meals and hulls into its major components using dry fractionation and separation technologies. More specifically, the combination of the ultrafine milling (UFM) with the electrostatic separation and the turbo separation technologies was studied. The different fractions obtained were analyzed in terms of total phenolic compounds (TPC), chemical composition, yield and energy consumption. Then, we studied the enzymatic pretreatment of the different raw materials and fractions containing the most interesting chemical composition. This step was done to try to enhance the extractability of the phenolic compounds or their bioavailability. Following, we developed and optimized the extraction methodologies. To do this, we compared the classic extractions methodology using methanol at 75 °C, the ultrasound assisted extractions (UAE) and the microwave assisted extractions (MAE). Their efficiency in terms of yield, selectivity and preservation of the phenolic compounds was studied.