Acidic fermentation (AF) of organic waste/wastewater generates valuable byproducts, including hydrogen, volatile fatty acids, and ethanol; however, its sensitivity to pH drops limits the stability and efficiency of the process. A reversal process, the acidic chemical treatment of concrete waste (CW) to recycle its aggregates, generates calcium hydroxide, which can serve as buffering agent. Meanwhile, integrating both processes can introduce a sustainable win-win approach, which is the aim of this study. To assess this approach, a series of batch AF experiments were conducted at 50 °C and pH 5.5, using glucose as the substrate. Cementitious specimen (1.5 × 1.5 × 0.8 cm) was supplemented to each 200 mL-fermenter. Unamended fermenters, with and without additional NaHCO3-buffering, were used as controls to compare with the amended ones. Introducing cementitious specimens to AF increased H2-production by 2-fold and 1.7-fold compared to controls with and without NaHCO3-addition, respectively, after three consecutive feed-cycles. The surface analysis of incorporated specimen confirmed the Ca, Al, Mg, and Si leaching. The AF efficiency and resulting cementitious mass reduction were further assessed at different organic loads and specimens’ volume, surface area, and porosity (by changing water-to-cement [W/C] ratio). Increasing the organic load from 10 to 20 g-glucose/L resulted in lower H2-production, higher specimen mass reduction (up to ∼32%), and higher Ca2+ release (up to 2 g/L); however, no significant effect was observed when using specimens with higher W/C ratio or surface area. Moreover, the presence of cementitious specimens significantly influenced the microbial composition, leading to notable developments in the abundant genera Thermoanaerobacterium and Bacillus. This study presents a novel approach to sustainably enhancing AF process using CW as both an additive and a treatable substance, with reusable aggregates as a byproduct. It provides valuable insights for optimizing the process and guiding future practical applications. This includes considering various concrete compositions, adjusting organic load conditions, and evaluating long-term stability in larger-scale systems.
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