Acetylene purification wastewater (APW) usually contains high concentrations of ammonia nitrogen (NH4-N), which is generated during the production of acetylene in a polyvinylchloride manufacturing plant. In this study, a struvite precipitation method was selected to remove NH4-N from the APW. Laboratory-scale batch experiments were performed to investigate the effects of the initial APW pH, phosphate (PO43−) concentration, magnesium (Mg2+) concentration, and sources of PO43− and Mg2+ on NH4-N removal. The results indicated that the initial APW pH had a significant effect on the removal of NH4-N, while the other factors had relatively minor effect. The NH4-N could be effectively removed at an optimum initial APW pH of 9.5, when Na2HPO4·12H2O and MgSO4·7H2O were both applied to NH4-N at a ratio of 1.2. Under these conditions, the efficiency of removal of NH4-N, total nitrogen and chemical oxygen demand were 85%, 84% and 18%, respectively. The X-ray diffraction analysis indicated that the precipitates were dominated by struvite. The scanning electron microscopy analysis of the precipitates showed a typical morphology of stick-like and prismatic crystals with coarse surface. The energy dispersive spectroscopy analysis indicated that the precipitates contained P, O, Mg and Ca.