Long-term accumulation of cobalt-containing wastewater may also pollute groundwater and cause a large amount of loss of valuable metals. Therefore, the comprehensive utilization of cobalt-containing wastewater must be realized, especially as cobalt itself is a very important strategic resource. This paper proposes a membrane electroconversion method to separate cobalt ions from cobalt-containing wastewater and prepare cobalt hydroxide. In addition, the electrolysis process was optimized, and single-factor experiments such as the initial concentration, cobalt ions, current density, temperature etc., and economic calculations such as current efficiency were explored. The electrolysis product was calcined as the precursor to obtain the oxide Co3O4, and the calcination experiment was also optimized. In this concentration range, more than 90% of cobalt can be recovered within 2 h.