Graphite-oxide/TiO2 (GO/TiO2) composite materials were prepared by heterocoagulation method from Brodie’s graphite-oxide (GO) in order to test them as catalysts in the methanol photocatalytic reforming reaction in liquid phase. The preparation of the composite itself resulted in only little changes in the structure of GO as it was indicated by attenuated total reflection infrared (ATR-IR) and 13C magic-angle spinning nuclear magnetic resonance (13C MAS NMR) spectroscopic measurements. However, during the photocatalytic reaction, all of the GO/TiO2 samples darkened strongly indicating structural changes of GO. X-ray photoelectron spectroscopy along with NMR confirmed the loss of oxygen functionalities and emergence of graphitic species in the samples recovered from the photocatalytic reaction. Model experiments were designed to identify the key factors determining the activity of the GO/TiO2 derived photocatalysts. It was found that the emergence of a pronounced coupling between TiO2 and the graphite-like carbonaceous material is the most important contribution to get active and stable photocatalysts.
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