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The super-microporous microcrystalline MgO-ZrO 2 nanomaterials (pore size 1–2 nm) was prepared successfully via a facile one-pot evaporation-induced self-assembly (EISA) method and employed in the transesterification of soybean oil and methanol. X-ray diffraction, transmission electron microscope, temperature programmed desorption of CO 2 , and N 2 adsorption porosimetry were employed to characterize the nanocomposites. Nitrogen sorption isotherms revealed that these materials had large surface areas of more than 200 m 2 /g. Moreover, the sample with a Mg/Zr molar ratio of 0.5 and calcined at 400 °C showed high biodiesel yield (around 99% at 150 °C). [ABSTRACT FROM AUTHOR]