The effect of synthesis variable control during the combustion of urea in solution to obtain a Ni-Co/γ-Al2O3 catalyst with a low metallic loads for producting hydrogen by reforming glycerol was studied. Catalysts with the same urea/metal molar ratio but synthesized by controlled or uncontrolled urea matrix combustion were compared. It has been observed that adopting a urea/metal molar ratio between 2 and 6 and a heating rate of 10 °C∙min−1 results in a catalyst with an active surface and high Ni-Co interaction. This leads to significant improvements in H2 yield (from 34 to 50%), glycerol conversion (from 35 to 50%), and H2 selectivity (from 96 to 99%), while maintaining stability during 420 min of reaction. The repeatability of controlled synthesis has shown differences in results of less than 2%. Controlled synthesis is an attractive approach for scaling up the process for treating glycerinous waters, effluents in biodiesel plants.
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