A simple and efficient method was developed for fabricating spherical granules of CuO catalyst via a three-step procedure. In the first step, copper oxide nanoparticles were synthesized by hydrothermal decomposition of copper nitrate solution under supercritical condition. Then, they were immobilized in the polymeric matrix of calcium alginate, and followed by high-temperature calcination in an air stream as the third step, in which carbonaceous materials were oxidized, to result in a pebble-type catalyst of high porosity. The produced CuO nanoparticles were characterized by transmission electron microscopy (TEM) that revealed an average size of 5 nm, X-ray diffractometry (XRD), and thermo gravimetric (TG) analysis. The catalysts were further investigated by BET test for measurement of their surface area, and by temperature-programmed reduction analysis (H2-TPR) for determination of catalytic activity. The results demonstrated that immobilization of the CuO nanoparticle in the polymeric matrix of calcium alginate, followed by calcination at elevated temperatures, could result in notable mechanical strength and enhanced catalytic activity due to preservation of the high surface area, both valuable for practical applications. A simple and efficient method was developed for fabricating spherical granules of CuO catalyst via a three-step procedure. In the first step, copper oxide nanoparticles were synthesized by hydrothermal decomposition of copper nitrate solution under supercritical conditions. matrix of calcium alginate, and followed by high-temperature calcination in an air stream as the third step, in which carbonaceous materials were oxidized, to result in a pebble-type catalyst of high porosity. The produced CuO nanoparticles were characterized by transmission electron microscopy (TEM) that revealed an average size of 5 nm, X-ray diffractometry (XRD), and thermo gravimetric (TG) analysis. The catalysts were further tested by BET test for measurement of their surface area, and by temperature-programmed reduction analysis (H2-TPR) for determination of catalytic activity. The results demonstrated that immobilization of the CuO nanoparticle in the polymeri c matrix of calcium alginate, followed by calcination at elevated temperatures, could result in not able mechanical strength and enhanced catalytic activity due to preservation of the high surface area, both valuable for practical applications.