The present invention discloses a process for recovering ammonia from vanadium preparation for ammonium preparation and recycling wastewater. A conventional vanadium extraction process is complex, and the most difficult to control and treat are ammonia emissions and wastewater treatment. The present process can directly extract ammonium metavanadate and ammonium polyvanadate from the beginning of mining and smelting, and gather all emitted ammonia to prepare ammonium in the process of preparing high-purity vanadium pentoxide by using the ammonium metavanadate or the ammonium polyvanadate, thereby ensuring zero emission of the exhaust gas, and effectively treat all wastewater generated in the above process by using a polyacid ester flocculation technology, thereby ensuring that the wastewater is not discharged but recycled, and realizing that the purity of all products reaches 99.5-99.99%.