Coal Fly Ash (CFA) is a hazardous waste from coal-fired power plants, but has increasingly become a popular supplementary cementitious material for cement in the construction industry. As a secondary resource of REE, its main advantage lies in its fine particle size that eliminates the need for costly and energy-intensive comminution. In this study, the potential of CFA from the Philippines as a secondary REE resource was investigated by direct leaching of REEs with hydrochloric acid (HCl). The CFA sample came from a coal-fired power plant with a circulating fluidized bed combustion (CFBC) technology. For the leaching tests, the effects of HCl concentration, leaching time and leaching temperature on REE extractions were elucidate optimized via Response Surface Methodology (RSM). The RSM results showed that the optimum leaching occurred at 3M HCl, 65 °C and 270 min with extractions of Nd, Er, Eu, Tb and Dy at 70.8%, 76.34%, 88.02%, 90.01% and 73.38%, respectively. According to these results, the CFA from the Philippines is a promising secondary resource of REE and the extraction method employed was effective in achieving a relatively high REE dissolution. Moreover, the empirical model that was established accurately predicted the dissolution of REE with an accuracy of 98.20%, 96.66%, 97.09%, 98.17% and 97.78% for Nd, Er, Eu, Tb and Dy, respectively.