Microwave (MW) treatment promotes homogeneous heating compared to conventional methods, thus increasing the recovery of high-added-value compounds and leading to a considerably lower amount of both by-products and side reactions. Therefore, the main goal of this work is to valorize almond hull (AH) via microwave (MW)-assisted radiation (0–200 W, 0–300 psi, 100–190 °C, 10–40 min). In this context, two different pathways were evaluated. Firstly, the transformation of AH into levulinic acid (LA), one of the major bio-based chemicals obtained from lignocellulosic biomass. The so-called almond hull extractives-free biomass (AH-EFB) led to the best results after using both Lewis (AlCl 3 ⋅6 H 2 O, 1 mol/L, 87 % molar yield) and Brønsted ( p -toluenesulfonic ( p -TsOH), 0.25 mol/L, 91 % molar yield) acids, at 190 °C for 20 min. This latter not only provides a sustainable system in contrast to mineral acids such as H 2 SO 4 or HCl, but also the possibility of being recovered and recycled for further transformations. In a parallel secondary experiment, the recovery of biologically active compounds (BACs) was studied separately. For this purpose, antioxidant assays and phenolic profiling were carried out, which demonstrated that MW was more efficient than traditional methods (i.e. soaking) based on obtained values in terms of scavenging activity and polyphenols. Overall, this valorization approach involves most of the Green Chemistry principles, thus contributing to the development of almond biorefineries. • Bioenergy and biofuels can be obtained from almond by-products. • Almond hull can provide high-added-value chemicals. • MW treatment increased the extraction of polyphenols and antioxidant activity.
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