本发明属于电解技术领域，具体为一种烧碱和正磷酸铁的联产方法。本发明联产方法包括：电解法制备NaOH和三价铁离子，将阳离子交换膜和/或微孔膜作为阴极、阳极的分隔膜，含有钠离子的水溶液作为阴极电解液，含有亚铁离子和钠离子的水溶液作为阳极电解液；化学沉淀法制备正磷酸铁；采用三价铁离子溶液作为原料，添加含有磷酸根离子水溶液作为沉淀剂，生成正磷酸铁。与传统的氯碱工艺，本发明具有以下优点：1该烧碱工艺能够避免氯气生成，克服由于烧碱生产造成的氯气产能过剩；Fe2+的氧化电位(0.771V vs SHE)远低于氯离子(1.36V vs SHE)，因此可以减少能耗；所产FePO4可用于制备锂离子或钠离子电池电极材料。
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