Inthis study, the A/O biological treatment method and the coagulation sedimentation treatment are adopted for wastewater from the production of mineral processing reagents, according to anaerobic-aerobic dislodge organic mechanism mixed flocculation sedimentation,s by controlling technological operational parameters, getting the final result of test research. The results show that the combined method can effectively remove the organic pollutants, turbidity and ammonia nitrogen, and the removal rate reached 97%, 97.2%, 98.7%. The production water qualities completely reach the national integrated wastewater discharge standard (GB8978-2002 secondary standard). According to the condition of the test, the operation parameters and the reasonable layout of A/O technology and coagulation are introduced. Then, it can be used as reference for the design and technical process improvements.