Levulinic acid is a platform chemical obtained from acid-catalyzed hydrothermal conversion of cellulose-rich biomass. The low amounts of solid biomass which can be handled in the reactor limit the levulinic acid concentration in the aqueous stream, making the economic viability of the aqueous phase process unsuitable for large scale applications. Now a novel approach to biphasic process has been proposed, where a mineral oil has been used as non-solvent for levulinic acid, thus concentrating it in the water phase, reducing the water volume to be processed downstream but at the same time maintaining enough liquid phase to sustain the slurry processability. The work has studied: i) the optimization of the biphasic hydrolysis of corn grain to levulinic acid; ii) the characterization of the recovered oil; iii) the evaluation of the energetic properties of the recovered hydrochar for its exploitation, thus smartly closing the biorefinery cycle.