This study examined how pH hydrolysis affects the recovery process for antimony extracted from spent electrolytes. Various OH−reagents were used to adjust the pH levels. The findings reveal that pH plays a crucial role in determining the optimal conditions for extracting antimony. The results show that NH4OH and NaOH are more effective compared to water, with optimal conditions at pH 0.5 for water and pH 1 for NH4OH and NaOH, resulting in average antimony extraction yields of 90.4%, 96.1%, and 96.7%, respectively. Furthermore, this approach helps to improve both crystallography and purity related to recovered antimony samples obtained through recycling processes. The solid precipitates obtained lack a crystalline structure, making it difficult to identify the compounds formed, but element concentrations suggest the presence of oxychloride or oxide compounds. Arsenic is incorporated into all solids, affecting the purity of the product, and water showing higher antimony content (68.38%) and lower arsenic values (8%) compared to NaOH and NH4OH. Bismuth integration into solids is less than arsenic (less than 2%) and remains unaffected by pH levels except in tests with water, where a bismuth hydrolysis product is identified at pH 1, accounting for the observed reduction in antimony extraction yields.