Converting Glycerol into Valuable Trioses by Cuδ+‐Single‐Atom‐Decorated WO3 under Visible Light

Abstract Photocatalytic selective oxidation under visible light presents a promising approach for the sustainable transformation of biomass‐derived wastes. However, achieving both high conversion and excellent selectivity poses a significant challenge. In this study, two valuable trioses, glyceraldehyde and dihydroxyacetone, are produced from glycerol over Cu δ+ ‐decorated WO 3 photocatalyst in the presence of H 2 O 2 . The photocatalyst exhibits a remarkable five‐fold increase in the conversion rate (3.81 mmol ⋅ g −1 ⋅ h −1 ) while maintaining a high selectivity towards two trioses (46.4 % to glyceraldehyde and 32.9 % to dihydroxyacetone). Through a comprehensive analysis involving X‐ray photoelectron spectroscopy measurements with and without light irradiation, electron spin resonance spectroscopy, and isotopic analysis, the critical role of Cu + species has been explored as efficient hole acceptors. These species facilitate charge transfer, promoting glycerol oxidation by photoholes, followed by coupling with OH ‐ , which are subsequently dehydrated to yield the desired glyceraldehyde and dihydroxyacetone.