We presented a novel bi-functional catalyst composed of HxWO3 and carbon composites, which exhibits excellent catalytic activity in biomass conversion and has the ability to effectively purify water via a wide range of wavelengths in the light spectrum. The HxWO3/carbon composites were effectively produced from commercially available monoclinic tungsten trioxide (WO3) and polypropylene (PP) powders to a single-step mechanochemical reaction employing high-energy ball milling. We systemically investigated how different synthesis parameters, such as rotation speed, processing duration, and ball diameter, affect the mechanochemically-induced phase transformation to either tetragonal or cubic HxWO3 during planetary ball milling. The crystal phase of HxWO3 was controllable by altering the total impact energy in the ball milling. In addition, real-time monitoring of the pressure increment inside the pot and evaluation of the evolved gas revealed the degassing behavior through the oxidative degradation of PP assisted by WO3. The CV and Rietveld analysis proved that HxWO3 exhibited significant enhancement by two orders of magnitude in the rate of H+ diffusion compared to monoclinic WO3. This enhancement would be attributed to the expansion of a mechanically-formed tunnel along the a-axis, which facilitates the migration of H+ ions. The HxWO3/carbon composites performed approximately 12-fold higher efficiency in generating soluble solids (glucose and furfural derivatives) compared to untreated WO3 through the catalytic hydrolysis of cellulose, owing to the enhanced Brønsted acidity. Moreover, the composite particles showed broad light absorption in the UV–Vis–NIR range and demonstrated a considerable enhancement of over three orders of magnitude in the photocatalytic degradation of methyl orange pollutants when exposed to NIR and visible light.
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