An innovative environmently friendly hydrolysis process for recycling waste aluminum with the generation of high-pressure hydrogen has been proposed and experimentally validated. The effect of the concentration of sodium hydroxide solution on hydrogen generation rate was the main focus of the study. In the experiments, distilled water and aluminum powder were placed in the pressure-resistance reactor made of Hastelloy, and was compressed to a desired constant water pressure using a liquid pump. The sodium hydroxide solution was supplied by liquid pump with different concentrations (from 1.0 to 5.0 mol/dm3) at a constant flow rate into the reactor by replacing the distilled water, and the rate of hydrogen generated was measured simultaneously. The liquid temperature in the reactor increased due to the exothermic reaction given by Al + OH(-) + 3H2O = 1.5H2 + Al(OH)4(-) + 415.6 kJ. Therefore, a high-pressure hydrogen was generated at room temperature by mixing waste aluminum and sodium hydroxide solution. As the hydrogen compressor used in this process consumes less energy than the conventional one, the generation of hydrogen having a pressure of almost 30 MPa was experimentally validated together with Al(OH)3, a useful byproduct.