Synthesis of nanocrystalline molybdenum carbide materials and their characterization

• A method to produce precursors to generate Mo2C materials was developed.
• C/Mo ratio, temperature, H2 or lack of H2 control the Mo2C phases formed.
• Nanocrystalline Mo2C can be prepared with the cubic or hexagonal phases.
• Mo2C phases were shown to be active for hydrogenation of toluene at 423 K.

A convenient and practical method for the preparation of precursors to form molybdenum carbide materials using solutions of ammonium heptamolybdate and sucrose is presented. Depending on the temperature-programmed reaction protocol employed [i.e., low temperature and long times (523 K for 24 h, 598 K for 24 h and 673 K for 72 h) or high temperature and short times (1073 K for 30 min)], the C/Mo ratio of the precursors (i.e., 6.3, 3.6, 2.0, 1.0 and 0.6) and the presence or not of H2, it is possible to produce nanocrystalline molybdenum carbide materials with the cubic or hexagonal phases. The two prepared phases of molybdenum carbide showed activity for the hydrogenation of toluene at 423 K to selectively produce methyl-cyclohexane. In the tested conditions, the hexagonal molybdenum carbide phase showed an initial higher activity but the deactivation of the catalyst was more pronounced than in the cubic molybdenum carbide catalyst.

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