Catalyst-type mixed metal oxides with different compositions and Co/Fe ratios were obtained from layered double hydroxides to be used as heterogeneous catalysts in the production of biodiesel. The effect of the Co/Fe ratio on the precursors of the catalysts was analyzed, considering their thermal, textural and structural properties. The physicochemical properties of the catalysts were determined by thermogravimetric analysis (differential scanning calorimetry and thermogravimetric), X-ray diffraction, Fourier-transform infrared spectroscopy, Scanning Electron Microscopy-Energy Dispersive X-ray spectroscopy and N2-physisorption. The conversion to biodiesel using the different catalysts obtained was determined by diffuse reflectance infrared Fourier-transform spectroscopy and 1H-Nuclear magnetic resonance spectroscopy, allowing us to correlate the effect of the catalyst composition with the catalytic capacity. The conditions for obtaining biodiesel were optimized by selecting the catalyst and varying the percentage of catalyst, the methanol/oil ratio and the reaction time. The catalysts reached yields of conversion to biodiesel of up to 96% in 20 min of reaction using only 2% catalyst. The catalyst that showed the best catalytic activity contains a mixture of predominant crystalline and amorphous phases of CoFe2O4 and NaxCoO2. The results suggest that cobalt is a determinant in the activity of the catalyst when forming active sites in the crystalline network of mixed oxides for the transesterification of triglycerides, with high conversion capacity and selectivity to biodiesel.