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The desulfurater (BaAl2O4) was successfully synthesized with BaCO3 and Al(OH)3 powders as raw materials by microwave sintering method. The mass loss of raw materials and the characterization of the outcome were investigated by means of TG-DSC, XRD and optical microscopy. The reaction mechanism was discussed. The experimental results show that synthesized BaAl2O4 by microwave sintering method is feasible. Compared with conventional sintering method, microwave sintering is a better way to synthesize BaAl2O4 with advantages of low temperature sintering, short time sintering and high synthesis rate.