Hydrothermal carbonization of two-phase olive mill waste (alperujo): Effect of aqueous phase recycling

Hydrothermal carbonization (HTC) is a promising technique for the conversion of lignocellulosic biomass, such as two-phase olive mill waste (TPOMW). However, the resulting generated aqueous phase (AP) rich in organic compounds is harmful if directly discharged in the environment. In this work, the use of recycled aqueous phase from the HTC process of TPOMW is evaluated as a reactive medium. The evolution of products yields, quality, morphology chemical structure, and composition with AP recycling runs are investigated by different analytical methods (Nuclear Magnetic Spectroscopy 1H and solid state 13C, Scanning Electron Microscopy, Elemental analysis, Proximate analysis, Fourier Infrared Transform spectroscopy, Total organic carbon, and total nitrogen). The results revealed significant improvement in the hydrochar yield and energy yield that increase 47.4 wt% to 53.0 wt% and 72.8%–81.3%, respectively. The increase in the number of recycling experiments promotes the lignin condensation as well as the polymerization of AP intermediates into microspheres. These phenomena lead to the increase in hydrochar yield as well as the modification of its micro-surface into a smooth porous surface through the recycling runs. Additionally, FT-IR and the solid state 13C NMR analysis demonstrated that AP recycling has no noticeable effect on the chemical structure of the produced hydrochars. Further analysis of the AP demonstrated that the total organic carbon and total nitrogen increase significantly after the first recycling run from 17.3 to 26.5 g/L and 0.4–0.6 g/L, respectively. The 1H NMR analysis revealed that AP is mainly formed by aliphatic and aromatic compounds.