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为了降低铜电解副产品粗硫酸镍溶液中Cu、Fe和Zn等杂质含量并减少镍损失，研究了采用Na2S2O3选择性沉淀铜—萃取深度除锌铁—蒸发结晶工艺深度净化粗硫酸镍溶液，并优化了关键工艺参数。结果表明：以Na2S2O3作沉淀剂时，在Na2S2O3过量系数2.0、溶液pH=5.0、反应温度85℃、反应时间2 h最佳工艺条件下，Cu沉淀率可达99.89%,Ni损失率仅为1.22%;选择P204作萃取剂时，在控制萃原液pH=3.0、P204体积分数25%、皂化率50%、相比VO/VA=1.5/1、萃取温度25℃、萃取时间10 min优化条件下，Zn、Fe萃取率可分别达99.87%和99.98%,Ni损失率为2.24%;深度净化后的硫酸镍溶液经蒸发结晶得到电镀级硫酸镍晶体产品，质量符合国家标准(GB/T 26524—2023)的Ⅱ类指标，可以用作电镀及其他工业用途的优质原料。
Abstract：In order to reduce the content of impurities such as Cu, Fe, Zn and reduce the loss of Ni in crude nickel sulfate solution of copper electrolysis by-products, the process of selective precipitation of copper by Na2S2O3—deep extraction of zinc removal iron—evaporation crystallization was studied for deep purification of the solution, and the key process parameters were optimized.The results show that the precipitation rate of Cu can reach 99.89% and the loss rate of Ni is only 1.22% using Na2S2O3 as precipitator under the optimum conditions of Na2S2O3 excess coefficient of 2.0,solution pH of 5.0,reaction temperature of 85 ℃ and reaction time of 2 h.Using P204 as extracant, the extraction rates of Zn and Fe can reach 99.87% and 99.98%,respectively, and the loss rate of Ni is 2.24% under the optimal conditions of pH=3.0,P204 volume fraction of 25%,saponification rate of 50%,VO/VA=1.5/1,extraction temperature of 25 ℃ and extraction time of 10 min.Electroplating grade nickel sulfate crystal products are obtained by evaporation and crystallization of the deeply purified nickel sulfate solution.The quality can meet the national standard GB/T 26524—2023 Class Ⅱ indicators, and can be used as high-quality raw materials for electroplating and other industrial uses.
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基本信息:
DOI：10.13355/j.cnki.sfyj.2025.03.014
中图分类号:TF811
引用信息:
[1]杨永明,朱文云,蒋学先等.铜电解副产品粗硫酸镍的深度净化工艺研究[J].湿法冶金,2025,44(03):398-405.DOI:10.13355/j.cnki.sfyj.2025.03.014.
基金信息:
广西科技重大专项(桂科AA22067077,桂科AB21196046); 崇左市科技计划项目(崇科20220601)