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Dry reforming of methane (DRM) is an important way to produce synthesis gas, requiring the use of catalysts stable at high temperatures and capable of resisting coke formation. In this work, Ni/Al2O3 and Ni/Mg‐Al2O3 catalysts were synthesized with calcined aluminas at different temperatures (623, 773, 923, and 1073 K) to evaluate the effect of calcination temperature on catalyst properties and performance. The synthesis of catalysts was performed by wet impregnation with predicted levels of Ni (10% w/w) and Mg (5% w/w) in the treated supports. The DRM assays were conducted in an experimental laboratory unit (continuous fixed bed reactor with in‐situ catalyst activation) using a 1:1 (v/v) CH4:CO2 mixture, a weight basis gas hourly space velocity (WGHSV) of 15 L h−1 gcat−1, and operation at 973 K. The reaction product was evaluated by gas chromatography. Variations in CH4 and CO2 conversions and H2/CO ratio were observed, indicating that these catalysts have different physical and chemical characteristics attributed to different effects caused by calcinating the supports (Al2O3 and Mg‐Al2O3) at different temperatures.

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