One-Pot Steam-Assisted Synthesis of BiOCl/TiO2/Zn-In-Modified Mg-Al LDHs Catalyst and Its Photocatalytic Degradation of Methylene Blue

A series of Mg-Al LDH-based photocatalysts were synthesized via a one-pot steam-assisted method, including pure Mg-Al LDH (MA), Zn-In ion-exchange-modified Mg-Al LDH (MAZ), BiOCl-loaded pristine Mg-Al LDH (MAB), and Zn-In-modified Mg-Al LDH co-loaded with TiO2 and BiOCl (MA/Zn-In/TiO2/BiOCl, MAZB). The one-pot synthesis facilitated the in situ intercalation and uniform loading of BiOCl/TiO2/Zn-In, while Zn2+/In3+ modified the MA layers via ion exchange, leading to an expansion of the interlayer spacing. The innovation of this work is reflected in two aspects: first, all raw materials are added via a one-pot strategy to achieve in situ preparation of modified hydrotalcite; second, this synthetic route features simple post-treatment without complicated washing, pressure filtration, and other tedious operations. The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and N2 adsorption–desorption isotherms. The bismuth chloride oxide/TiO2/LDHs exhibited a layered structure, with the active components uniformly distributed between the layers and on the MA surface. Under simulated sunlight irradiation, MAZB achieved 97.5% degradation of 20 mg/L MB within 120 min, with an apparent rate constant of 0.0297 min−1, which is 7.2 times, 2.4 times, and 2.9 times that of MA, MAZ, and MAB, respectively. The degradation rate of MAZB still remained at 89.5% after five cycles, demonstrating excellent stability and reusability. Compared with traditional hydrothermal methods, this steam-assisted system features mild reaction conditions (180 °C, atmospheric pressure), sodium-free raw materials, no washing requirement, and zero waste discharge, showing prominent green advantages.