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Porous hollow carbonaceous microspheres (PHCMs) fabricated from yeast cells by hydrothermal treatment have stimulated interest because of their outstanding chemical and physical properties. Herein, the functionalizations of PHCMs by further coating of α-Fe2O3 nanoparticles onto the surface were carried out. The structure of resulted α-Fe2O3@PHCMs products were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive spectrometry (EDS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), and BET specific surface area measurements (BET), respectively. Its promising application was evaluated by the Fenton-like degradation of fluorescent whitening agent-VBL from aqueous solutions.<br>In this work, novel α-Fe2O3@porous hollow carbonaceous microspheres (α-Fe2O3@PHCMs) were synthesized through a combination of hydrothermal method and calcinations route and achieved excellent removal efficiency for fluorescent whitening Agent-VBL.<br><br>Display Omitted<br>• The hybrid α-Fe2O3@ porous hollow microspheres (PHCMs) were firstly fabricated. • The formation mechanism of α-Fe2O3@PHCMs microspheres was proposed and verified. • Dithizone played a key role in the synthesis of α-Fe2O3@PHCMs composites. • A favorable removal for the fluorescent whitening agent-VBL were achieved.