Article(id=1169295844034490463, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1169295841580819245, articleNumber=1009-2617(2025)03-0398-08, orderNo=null, doi=10.13355/j.cnki.sfyj.2025.03.014, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1722960000000, receivedDateStr=2024-08-07, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1756711453684, onlineDateStr=2025-09-01, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1756711453684, onlineIssueDateStr=2025-09-01, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1756711453684, creator=13701087609, updateTime=1756711453684, updator=13701087609, issue=Issue{id=1169295841580819245, tenantId=1146029695717560320, journalId=1146120122248306696, year='2025', volume='44', issue='3', pageStart='283', pageEnd='431', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1756711453097, creator=13701087609, updateTime=1756711962360, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1169297977647571041, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1169295841580819245, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1169297977647571042, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1169295841580819245, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=398, endPage=405, ext={EN=ArticleExt(id=1169295844265177184, articleId=1169295844034490463, tenantId=1146029695717560320, journalId=1146120122248306696, language=EN, title=Deep Purification Process of Crude Nickel Sulfate as By-product of Copper Electrolysis, columnId=1152626641181700664, journalTitle=Hydrometallurgy of China, columnName=Experiment Research, runingTitle=null, highlight=null, articleAbstract=
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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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。
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杨永明(1985—),男,本科,工程师,主要研究方向为有色金属冶金及资源回收利用。
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杨永明(1985—),男,本科,工程师,主要研究方向为有色金属冶金及资源回收利用。
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2 Department of Materials Science and Engineering, Guilin University of Technology, Guilin 541004, China
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2 桂林理工大学 材料科学与工程学院,广西 桂林 541004
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Deep purification test flow of crude nickel sulfate solution, figureFileSmall=YgE3tiNlRFgi63OlWVZUQg==, figureFileBig=BSiBWutiSQQh5gSouhjE1A==, tableContent=null), ArticleFig(id=1172888183537808207, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图1, caption=
粗硫酸镍溶液的深度净化试验流程, figureFileSmall=YgE3tiNlRFgi63OlWVZUQg==, figureFileBig=BSiBWutiSQQh5gSouhjE1A==, tableContent=null), ArticleFig(id=1172888183613305683, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.2, caption=
Effect of excess coefficient of Na2S2O3 on precipitation separation of Cu and Ni, figureFileSmall=nxGMRYuepVXqcRiadgG8WQ==, figureFileBig=QbzShR+jXa2d5es1OCV63A==, tableContent=null), ArticleFig(id=1172888183676220245, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图2, caption=
Na2S2O3过量系数对Cu、Ni沉淀分离效果的影响, figureFileSmall=nxGMRYuepVXqcRiadgG8WQ==, figureFileBig=QbzShR+jXa2d5es1OCV63A==, tableContent=null), ArticleFig(id=1172888183726551894, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.3, caption=
Effect of solution pH on precipitation separation of Cu and Ni, figureFileSmall=fVYvlaU5kWbcVvzLg7KRcw==, figureFileBig=pTFopiyhlidck6lqs9+fBA==, tableContent=null), ArticleFig(id=1172888183785272152, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图3, caption=
溶液pH对Cu、Ni沉淀分离效果的影响, figureFileSmall=fVYvlaU5kWbcVvzLg7KRcw==, figureFileBig=pTFopiyhlidck6lqs9+fBA==, tableContent=null), ArticleFig(id=1172888183869158237, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.4, caption=
Effect of reaction temperature on precipitation separation of Cu and Ni, figureFileSmall=VIrD4ThoU4aWwsK2vK4j8w==, figureFileBig=C/Njr+Qx0tmtqbxTjn22gw==, tableContent=null), ArticleFig(id=1172888183932072797, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图4, caption=
反应温度对Cu、Ni沉淀分离效果的影响, figureFileSmall=VIrD4ThoU4aWwsK2vK4j8w==, figureFileBig=C/Njr+Qx0tmtqbxTjn22gw==, tableContent=null), ArticleFig(id=1172888183986598751, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.5, caption=
Effect of reaction time on precipitation separation of Cu and Ni, figureFileSmall=sJcUfgLASqvY3zKztGlb+w==, figureFileBig=b8ZhGKdD4bkUVE9FX6ghmQ==, tableContent=null), ArticleFig(id=1172888184083067747, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图5, caption=
反应时间对Cu、Ni沉淀分离效果的影响, figureFileSmall=sJcUfgLASqvY3zKztGlb+w==, figureFileBig=b8ZhGKdD4bkUVE9FX6ghmQ==, tableContent=null), ArticleFig(id=1172888184204702565, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.6, caption=
Extraction effects of different extractants on Zn,Fe and Ni, figureFileSmall=oWa6nJrL/g9zxMDdEOGeYQ==, figureFileBig=WfCthqcbU4CZ8xyMUttpiw==, tableContent=null), ArticleFig(id=1172888184280200039, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图6, caption=
不同萃取剂对Zn、Fe和Ni的萃取效果, figureFileSmall=oWa6nJrL/g9zxMDdEOGeYQ==, figureFileBig=WfCthqcbU4CZ8xyMUttpiw==, tableContent=null), ArticleFig(id=1172888184330531688, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.7, caption=
Effect of VO/VA on extraction and separation of Zn,Fe and Ni, figureFileSmall=dv5ul8dZW52jMyz1cvw05w==, figureFileBig=3rh32uar6JnW2fVGG1V/Kg==, tableContent=null), ArticleFig(id=1172888184393446250, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图7, caption=
VO/VA对Zn、Fe和Ni萃取分离效果的影响, figureFileSmall=dv5ul8dZW52jMyz1cvw05w==, figureFileBig=3rh32uar6JnW2fVGG1V/Kg==, tableContent=null), ArticleFig(id=1172888184456360812, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.8, caption=
Effect of extraction temperature on extraction separation of Zn,Fe and Ni, figureFileSmall=yKuS4I5aDY8haMim0IaGYw==, figureFileBig=O16KZgdpJ1UfOZhJjdwXMw==, tableContent=null), ArticleFig(id=1172888184527663982, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图8, caption=
萃取温度对Zn、Fe和Ni萃取分离效果的影响, figureFileSmall=yKuS4I5aDY8haMim0IaGYw==, figureFileBig=O16KZgdpJ1UfOZhJjdwXMw==, tableContent=null), ArticleFig(id=1172888184594772848, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Fig.9, caption=
Effect of extraction time on extraction separation of Zn,Fe and Ni, figureFileSmall=kHLBu/29azdrjqT6HZTLOA==, figureFileBig=pKVdDAHw/na9INBkdQrksg==, tableContent=null), ArticleFig(id=1172888184653493106, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=图9, caption=
萃取时间对Zn、Fe和Ni萃取分离效果的影响, figureFileSmall=kHLBu/29azdrjqT6HZTLOA==, figureFileBig=pKVdDAHw/na9INBkdQrksg==, tableContent=null), ArticleFig(id=1172888184724796276, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Table 1, caption=
Main chemical components of crude nickel sulfate crystals %
, figureFileSmall=null, figureFileBig=null, tableContent=
| Ni | Cu | Fe | Zn | Co | Ca | Mg |
| 15.79 | 0.18 | 0.31 | 0.91 | 0.075 | 0.08 | 0.031 |
), ArticleFig(id=1172888184808682358, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=表1, caption=
粗硫酸镍结晶的主要化学成分
, figureFileSmall=null, figureFileBig=null, tableContent=
| Ni | Cu | Fe | Zn | Co | Ca | Mg |
| 15.79 | 0.18 | 0.31 | 0.91 | 0.075 | 0.08 | 0.031 |
), ArticleFig(id=1172888184875791224, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Table 2, caption=
Comprehensive verification test results of removal of copper by precipitation
, figureFileSmall=null, figureFileBig=null, tableContent=
| 试验编号 | Cu沉淀率/% | Ni损失率/% |
| 1 | 99.89 | 1.25 |
| 2 | 99.78 | 1.14 |
| 3 | 100.00 | 1.29 |
| 平均 | 99.89 | 1.22 |
), ArticleFig(id=1172888184980648825, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=表2, caption=
沉淀除铜综合验证试验结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 试验编号 | Cu沉淀率/% | Ni损失率/% |
| 1 | 99.89 | 1.25 |
| 2 | 99.78 | 1.14 |
| 3 | 100.00 | 1.29 |
| 平均 | 99.89 | 1.22 |
), ArticleFig(id=1172888185068729211, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Table 3, caption=
Comprehensive verification test results of extraction of zinc-removed iron by P204 %
, figureFileSmall=null, figureFileBig=null, tableContent=
| 试验编号 | Zn萃取率 | Fe萃取率 | Ni损失率 |
| 1 | 99.78 | 100.00 | 1.92 |
| 2 | 99.95 | 99.94 | 2.06 |
| 3 | 99.89 | 100.00 | 1.99 |
| 平均 | 99.87 | 99.98 | 1.99 |
), ArticleFig(id=1172888185161003901, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=表3, caption=
P204萃取除锌、铁综合验证试验结果
, figureFileSmall=null, figureFileBig=null, tableContent=
| 试验编号 | Zn萃取率 | Fe萃取率 | Ni损失率 |
| 1 | 99.78 | 100.00 | 1.92 |
| 2 | 99.95 | 99.94 | 2.06 |
| 3 | 99.89 | 100.00 | 1.99 |
| 平均 | 99.87 | 99.98 | 1.99 |
), ArticleFig(id=1172888185261667199, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=EN, label=Table 4, caption=
Comparison between chemical composition content of nickel sulfate products and GB/T 26524—2023 standard requirements %
, figureFileSmall=null, figureFileBig=null, tableContent=
| 项目 | GB/T 26524—2023标准 | 硫酸镍产品中wB |
| I类 | Ⅱ类 |
| 镍 | ≥22.08 | ≥22.20 | 22.24 |
| 钴 | ≤0.05 | ≤0.001 | 0.000 3 |
| 铜 | ≤0.000 5 | ≤0.000 5 | 0.000 1 |
| 铁 | ≤0.000 5 | ≤0.000 5 | 0.000 2 |
| 锌 | ≤0.000 5 | ≤0.000 5 | 0.000 1 |
| 钙 | ≤0.003 | ≤0.002 | 0.001 7 |
| 镁 | ≤0.003 | ≤0.002 | 0.000 9 |
| 水不溶物 | ≤0.001 | — | — |
), ArticleFig(id=1172888185332970369, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844034490463, language=CN, label=表4, caption=
硫酸镍产品化学成分含量与GB/T 26524—2023标准要求的对比
, figureFileSmall=null, figureFileBig=null, tableContent=
| 项目 | GB/T 26524—2023标准 | 硫酸镍产品中wB |
| I类 | Ⅱ类 |
| 镍 | ≥22.08 | ≥22.20 | 22.24 |
| 钴 | ≤0.05 | ≤0.001 | 0.000 3 |
| 铜 | ≤0.000 5 | ≤0.000 5 | 0.000 1 |
| 铁 | ≤0.000 5 | ≤0.000 5 | 0.000 2 |
| 锌 | ≤0.000 5 | ≤0.000 5 | 0.000 1 |
| 钙 | ≤0.003 | ≤0.002 | 0.001 7 |
| 镁 | ≤0.003 | ≤0.002 | 0.000 9 |
| 水不溶物 | ≤0.001 | — | — |
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