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Proper utilization of the FeSO4·7H2O waste slag generated from TiO2 industry is an urgent need, and Fe3O4 particles are currently being widely used in the wastewater flocculation field. In this work, magnetite was recovered from ferrous sulphate by a novel co-precipitation method with calcium hydroxide as the precipitant. Under optimum conditions, the obtained spherical magnetite particles are well crystallized with a Fe3O4 purity of 88.78%, but apt to aggregate with a median particle size of 1.83μm. Magnetic measurement reveals the obtained Fe3O4 particles are soft magnetic with a saturation magnetization of 81.73 A·m2/kg. In addition, a highly crystallized gypsum co-product is obtained in blocky or irregular shape. Predictably, this study would provide additional opportunities for future application of low-cost Fe3O4 particles in water treatment field.