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Phosphate rocks are a critical resource for the European Union, and alternative sources to assure the future production of a new generation of fertilizers are to be assessed. In this study, a statistical approach, combined with a sustainability evaluation for the recovery of materials from waste containing phosphorus (P), is presented. This work proposes a strategy to recover P and silica (SiO2) from rice husk poultry litter ash (RHPLA). The design of experiment (DoE) method was applied to maximize the P extraction using hydrochloric acid (HCl), with the aim to minimize the contamination that can occur by leachable heavy metals present in RHPLA, such as zinc (Zn). Two independent variables, the molar concentration of the acid, and the liquid-to-solid ratio (L/S) between the acid and RHPLA, were used in the experimental design to optimize the operating parameters. The statistical analysis showed that a HCl concentration of 0.34 mol/L and an L/S ratio of 50 are the best conditions to recover P with low Zn contamination. Concerning the SiO2, its content in RHPLA is too low to consider the proposed recovery process as advantageous. However, based on our analysis, this process should be sustainable to recover SiO2 when its content in the starting materials is more than 80%.