Spinel ferrites have been widely studied owing to their structural, optical, dielectric, and magnetic properties leading to numerous applications. CoFe2O4 nanoparticles have been synthesized directly via the sol-gel method with glycine as a fuel. The Rietveld refinement of the X-ray diffraction patterns revealed the formation of a single cubic structure with a space group, no secondary phase was observed. The lattice parameter and the average crystallite size of powders produced from the standard and alkaline solutions were 8.36/8.38 Å, and 511/1060 Å, respectively. The characteristic vibrations modes of the spinel structure have been revealed by Fourier Transform Infrared spectroscopy. CoFe2O4 powders were tested for Fenton catalysis, and their performance was investigated for dye degradation.