Catalyst performance is a relevant factor in biodiesel production because it can affect the efficiency of the process. This work provides a study of the performance of heterogeneous catalysts for biodiesel production derived from thermal-treated hydrocalumite-type compounds. This work aimed to synthesize and characterize hydrocalumite-type compounds intercalated with chloride and nitrate, evaluate the effect of thermal treatments at different temperatures (500, 600, and 750 °C) on these materials, and assess the performance of these materials as catalysts in the transesterification reactions using soybean oil and methanol. The materials were characterized by X-ray diffraction (XRD), vibrational spectroscopy (Fourier transform infrared with attenuated total reflectance (FTIR-ATR)), thermogravimetric analysis coupled to mass spectrometry (TGA DSC-MS), specific surface area, and X-ray photoelectron spectroscopy (XPS). The results of the transesterification reactions showed that the thermal-treated materials from the hydrocalumite intercalated with chloride presented high catalytic activity, among them, the thermal-treated material at 750 °C presented the highest conversion to methyl esters. process thermaltreated treated hydrocalumitetype type nitrate 500, 500 (500 600 75 C methanol Xray X ray XRD, XRD , (XRD) Fourier FTIRATR, FTIRATR FTIR ATR (FTIR-ATR)) TGA DSCMS, DSCMS DSC MS DSC-MS) area XPS. XPS . (XPS) activity them esters 50 (50 60 7 (XRD (FTIR-ATR) DSC-MS (XPS 5 (5 6 (FTIR-ATR (