A novel method for the preparation of stable Pt/C catalysts with size-controlled nanoparticles has been developed. The method is based on in situ synthesis of the nanoparticles (reduction with NaBH4 in the presence of a support and PVP). Compared to the conventional ex situ route (colloidal synthesis followed by impregnation), this in situ route yields smaller nanoparticles (2.5–3.9 nm) of narrower size distribution. The catalysts prepared by the in situ synthesis showed a higher stability in water at 80 °C, indicating a stronger interaction between the support and the metallic phase. Hydrothermal stability tests were also conducted under conditions equivalent to those of aqueous phase reforming (200 °C, 17 bar and water and diluted acetic acid). Hydrothermal treatment proved to be an excellent method to improve the resistance to leaching of the catalysts. Metal loss was negligible while PVP was almost completely removed from the catalyst; hence, most of the porosity was recovered and the dispersion measured by CO chemisorption increased from 5 to 34–75%. Water at 200 °C was more effective than diluted acetic acid for the removal of PVP. TEM images confirmed that the Pt nanoparticles did not undergo significant changes either in size or morphology upon the hydrothermal treatment, and XPS analysis showed a homogeneous distribution of Pt nanoparticles within the catalyst granules.
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