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The hydration of phenylacetylene in near-critical water, assisted with additives (NaHSO4, ZnCl2, FeCl3), has been successfully conducted with temperature and residence time ranges of 220-300 ℃ and 60-180 min, respectively. The results showed the catalytic ability is FeCl3 > ZnCl2 > NaHSO4. The maximum yield of product acetophenone was 96.68% at 260 ℃, 120 min. Based on the results found, a possible mechanism of hydration of phenylacetylene in near-critical water was proposed.