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The development of heterogeneous Fenton catalysts with good performance and stability is a challenge in the field of wastewater treatment. In this work, MgAlFe hydrotalcite-like compounds (MgAlFe-HTLcs) were prepared by solid phase reaction at room temperature and modified via a hydrothermal process. The experimental results showed that MgAlFe-HTLcs had a good layered structure with the same proportion of iron and aluminium, 18 h of crystallisation time and 110°C of crystallisation temperature and the lamellar structure was more uniform by solid grinding. Furthermore, the addition of iron can activate H2O2 more effectively to generate active oxygen which is •OH. The degradation experiments demonstrated that nearly 99.0% degradation efficiency was achieved for 10 mg/L Malachite Green (MG) solution within 60 min at the conditions of 0.10 g·L−1 MgAlFe-HTLcs, 0.10 mol·L-1 H2O2 and a natural pH of 6.3. Total organic carbon (TOC) removal reached 72.2% in a 70 min reaction. BET and XRD were measured to further discuss the stability and durability. Finally, a possible mechanism for the degradation of MG was presumed. [ABSTRACT FROM AUTHOR]