The hydrotalcite-based NiAl mixed oxides were synthesized by coprecipitation and urea hydrolysis approaches and employed for SO₂ removal. The samples were well characterized by inductively coupled plasma (ICP) elemental analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and N₂ adsorption/desorption isotherm analyses. The acid-base properties were characterized by pyridine chemisorption and CO₂ temperature-programmed desorption (TPD). The calcined NiAlO from the urea method showed excellent SO₂ adsorption and its adsorption equilibrium showed a type I isotherm, which significantly improved the adsorption performance for low-concentration SO₂. Both the physical structure and the acidic-basic sites were found to play important roles in the SO₂ adsorption process. In situ Fourier transform infrared spectroscopy (FTIR) investigation revealed that adsorbed SO₂ molecules formed surface bisulfite, sulfite, and bidentate binuclear sulfate. The mechanisms for SO₂ adsorption and transformation are discussed in detail.

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