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Article(id=1169295844869153593, tenantId=1146029695717560320, journalId=1146120122248306696, issueId=1169295841580819245, articleNumber=1009-2617(2025)03-0301-08, orderNo=null, doi=10.13355/j.cnki.sfyj.2025.03.003, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1738857600000, receivedDateStr=2025-02-07, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1756711453883, onlineDateStr=2025-09-01, pubDate=1750348800000, pubDateStr=2025-06-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1756711453883, onlineIssueDateStr=2025-09-01, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1756711453883, creator=13701087609, updateTime=1756711453883, 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=301, endPage=308, ext={EN=ArticleExt(id=1169295845104034618, articleId=1169295844869153593, tenantId=1146029695717560320, journalId=1146120122248306696, language=EN, title=Discussion on Process Mineralogical Characteristics and Cobalt Leaching of Copper-Cobalt Oxide Ores in Kambove Mining Area,Congo(DRC), columnId=1152626641181700664, journalTitle=Hydrometallurgy of China, columnName=Experiment Research, runingTitle=null, highlight=null, articleAbstract=

In response to the issue of low cobalt leaching rate from oxidized copper-cobalt ore in the Kambove mining area of Congo(DRC), the mineralogical characteristics of the ore were analyzed by Mineral Liberation Analysis (MLA), polarized light microscopy, and Scanning Electron Microscopy (SEM). Based on the findings, leaching of cobalt from the ore with sodium pyrosulfite, Fe powder and SO2 as reducing agents was studied. The influence of different reducing agents and dosage on the leaching effect was investigated. The resluts reveal that the primary copper minerals in the ore are pseudomalachite, malachite, and libethenite, while the main cobalt minerals are copper-cobalt-bearing manganese oxide and heterogenite. The gangue minerals predominantly consist of siltstone, quartz, sericite, and chlorite. The occurrence states of copper and cobalt in the ore are complex, with cobalt minerals being fine-grained and mostly occurring as inclusions. The theoretical leaching rate of cobalt is calculated to be 92.82%. Compared with the three reducing agents, the leaching effect of SO2 is better. Under the optimal conditions of liquid volume to solid mass ratio of 3∶1, sulfuric acid dosage of 26.7 g/L, SO2 amount at 1.7 times the theoretical amount, reaction temperature of 38 ℃, and reaction duration of 3 h, the cobalt leaching rate can reach 85.48%, approaching the theoretical maximum. The research results can provide both theoretical and technical support for the efficient utilization of cobalt resources in the Kambove mining area of Congo(DRC).

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针对刚果(金)Kambove矿区氧化铜钴矿钴浸出率不高的问题,采用MLA、偏光显微镜、SEM等手段对该氧化铜钴矿的矿物学特征进行分析,并在此基础上,分别研究了以焦亚硫酸钠、Fe粉、SO2气体为还原剂浸出该矿石中的钴,考察了不同还原剂及用量对浸出效果的影响。结果表明:矿石中主要的铜矿物为假孔雀石、孔雀石、磷铜矿;主要的钴矿物为铜钴硬锰矿和水钴矿,主要的脉石矿物为粉砂岩、石英、绢云母、绿泥石;矿石中铜、钴赋存状态复杂,钴矿物粒度细小且多为包裹体,钴理论浸出率为92.82%;3种还原剂对钴浸出效果中SO2的浸出效果最好,在液固体积质量比3∶1、硫酸用量26.7 g/L、SO2通入量为理论量的1.7倍、反应温度38 ℃、反应时间3 h最佳浸出条件下,钴浸出率为85.48%,接近理论浸出率。研究结果可为Kambove矿区钴资源的高效利用提供理论和技术支持。

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肖发新(1980—),男,博士,副教授,主要研究方向有色金属冶金、固废资源化、纳米材料。E-mail:。
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赵亚茹(2000—),女,硕士研究生,主要研究方向有色金属冶金。

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赵亚茹(2000—),女,硕士研究生,主要研究方向有色金属冶金。

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赵亚茹(2000—),女,硕士研究生,主要研究方向有色金属冶金。

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Minerals Engineering, 2019, 137:277-289., articleTitle=Mineralogical reconciliation of cobalt recovery from the acid leaching of oxide ores from five deposits in Katanga (DRC), refAbstract=null), Reference(id=1172888212851802704, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, doi=null, pmid=null, pmcid=null, year=2022, volume=38, issue=2, pageStart=32, pageEnd=34, url=null, language=null, rfNumber=[16], rfOrder=25, authorNames=舒方霞, 詹光, 姜超, journalName=有色矿冶, refType=null, unstructuredReference=舒方霞, 詹光, 姜超, 等. 非洲低品位氧化铜钴矿硫酸体系下SO2强化还原浸出工艺研究[J]. 有色矿冶, 2022, 38(2):32-34., articleTitle=非洲低品位氧化铜钴矿硫酸体系下SO2强化还原浸出工艺研究, refAbstract=null), Reference(id=1172888212914717265, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, doi=null, pmid=null, pmcid=null, year=2022, volume=38, issue=2, pageStart=32, pageEnd=34, url=null, language=null, rfNumber=[16], rfOrder=26, authorNames=SHU Fangxia, ZHAN Guang, JIANG Chao, journalName=Non-Ferrous Mining and Metallurgy, refType=null, unstructuredReference=SHU Fangxia, ZHAN Guang, JIANG Chao, et al. 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tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=图1, caption=氧化铜钴矿的XRD图谱, figureFileSmall=1h7dJ/mleVZvR4dAdWzi9g==, figureFileBig=24WNqNEkw+iJUoH1lUEboA==, tableContent=null), ArticleFig(id=1172888208653304353, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=EN, label=Fig.2, caption=MLA backscatter particle map of partial particle size, figureFileSmall=bj2Pv4uGW66tt2vmlt1m3Q==, figureFileBig=xsPn8AeS0Cx7r+4eriLoXQ==, tableContent=null), ArticleFig(id=1172888208804299298, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=图2, caption=部分粒级的MLA背散射颗粒图, figureFileSmall=bj2Pv4uGW66tt2vmlt1m3Q==, figureFileBig=xsPn8AeS0Cx7r+4eriLoXQ==, tableContent=null), ArticleFig(id=1172888209001431587, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=EN, label=Fig.3, 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tableContent=null), ArticleFig(id=1172888209940955690, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=图6, caption=SO2还原浸出渣的SEM及EDS分析结果

a—SEM,放大2 000倍;b—SEM,放大5 000倍;c—SEM,放大1 000倍;d~g—1#~4#样点,EDS。

, figureFileSmall=zNRkglYVvXuG3g+KxQB+nw==, figureFileBig=ks9myrp4PeoZgxfBxa+Deg==, tableContent=null), ArticleFig(id=1172888209995481643, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=EN, label=Fig.7, caption=Infrared spectrum of copper cobalt oxide (a) and reduction leaching residue by SO2 (b), figureFileSmall=ylYzyWaxsYAmVP67KgZT+g==, figureFileBig=6TNM59w9KXFp7jagjPv6nA==, tableContent=null), ArticleFig(id=1172888210050007596, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=图7, caption=氧化铜钴矿(a)、SO2还原浸出渣(b)的红外光谱, figureFileSmall=ylYzyWaxsYAmVP67KgZT+g==, figureFileBig=6TNM59w9KXFp7jagjPv6nA==, tableContent=null), ArticleFig(id=1172888210100339245, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=EN, label=Table 1, caption=

Chemical multi-element analysis results of copper-cobalt oxide ore %

, figureFileSmall=null, figureFileBig=null, tableContent=
Cu Co Fe S Mn Ti
2.30 0.274 3.14 0.139 0.190 0.635
Cr Ni Zn Pb SiO2 Al2O3
0.012 0.033 0.012 <0.000 1 61.63 12.77
CaO MgO P2O5 K2O Na2O
0.090 7.02 0.780 2.18 0.090
), ArticleFig(id=1172888210175836718, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=表1, caption=

氧化铜钴矿的化学多元素分析结果

, figureFileSmall=null, figureFileBig=null, tableContent=
Cu Co Fe S Mn Ti
2.30 0.274 3.14 0.139 0.190 0.635
Cr Ni Zn Pb SiO2 Al2O3
0.012 0.033 0.012 <0.000 1 61.63 12.77
CaO MgO P2O5 K2O Na2O
0.090 7.02 0.780 2.18 0.090
), ArticleFig(id=1172888210247139887, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=EN, label=Table 2, caption=

Composition of main minerals in copper-cobalt oxide ore

, figureFileSmall=null, figureFileBig=null, tableContent=
矿物名称 占比/% 矿物名称 占比/%
假孔雀石 2.533 粉砂岩 32.629
孔雀石 0.797 铜钴硬锰矿 0.787
磷铜矿 0.471 水钴矿 0.197
硅孔雀石 0.011 褐铁矿 2.812
赤铜矿 0.018 石英 29.547
黑铜矿 0.006 绢云母 12.341
辉铜矿 0.035 绿泥石 15.883
斑铜矿、黄铜矿 0.018 其他 1.915
), ArticleFig(id=1172888210322637360, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=表2, caption=

氧化铜钴矿中主要矿物组成

, figureFileSmall=null, figureFileBig=null, tableContent=
矿物名称 占比/% 矿物名称 占比/%
假孔雀石 2.533 粉砂岩 32.629
孔雀石 0.797 铜钴硬锰矿 0.787
磷铜矿 0.471 水钴矿 0.197
硅孔雀石 0.011 褐铁矿 2.812
赤铜矿 0.018 石英 29.547
黑铜矿 0.006 绢云母 12.341
辉铜矿 0.035 绿泥石 15.883
斑铜矿、黄铜矿 0.018 其他 1.915
), ArticleFig(id=1172888210398134833, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=EN, label=Table 3, caption=

Balance calculation results of cobalt in various minerals

, figureFileSmall=null, figureFileBig=null, tableContent=
矿物名称 矿物占比/
%		 矿物中w(钴)/
%		 矿物中钴
赋存率/%
假孔雀石 2.533 0.21 1.91
孔雀石 0.797 0.29 0.83
磷铜矿 0.471 0.05 0.08
水钴矿 0.197 50.34 35.41
铜钴硬锰矿 0.787 7.22 20.29
褐铁矿 2.812 0.54 5.42
辉铜矿 0.035 0.07 0.01
绿泥石 15.883 0.44 24.96
绢云母 12.341 0.04 1.76
粉砂岩 32.629 0.08 9.33
合计 68.485 59.28 100.00
), ArticleFig(id=1172888210452660786, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=表3, caption=

钴在各矿物中的平衡计算结果

, figureFileSmall=null, figureFileBig=null, tableContent=
矿物名称 矿物占比/
%		 矿物中w(钴)/
%		 矿物中钴
赋存率/%
假孔雀石 2.533 0.21 1.91
孔雀石 0.797 0.29 0.83
磷铜矿 0.471 0.05 0.08
水钴矿 0.197 50.34 35.41
铜钴硬锰矿 0.787 7.22 20.29
褐铁矿 2.812 0.54 5.42
辉铜矿 0.035 0.07 0.01
绿泥石 15.883 0.44 24.96
绢云母 12.341 0.04 1.76
粉砂岩 32.629 0.08 9.33
合计 68.485 59.28 100.00
), ArticleFig(id=1172888210532352563, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=EN, label=Table 4, caption=

Thermodynamic data of reaction equations (1) at different temperatures

, figureFileSmall=null, figureFileBig=null, tableContent=
温度/K ΔrH/
(kJ·mol-1)		 ΔrS/
(J·mol-1·K-1)		 ΔrG/
(kJ·mol-1)
298.15 -427.189 292.205 -514.310
323.15 -455.376 239.918 -532.905
348.15 -493.950 148.880 -545.783
), ArticleFig(id=1172888210586878516, tenantId=1146029695717560320, journalId=1146120122248306696, articleId=1169295844869153593, language=CN, label=表4, caption=

不同温度下式(1)的热力学数据

, figureFileSmall=null, figureFileBig=null, tableContent=
温度/K ΔrH/
(kJ·mol-1)		 ΔrS/
(J·mol-1·K-1)		 ΔrG/
(kJ·mol-1)
298.15 -427.189 292.205 -514.310
323.15 -455.376 239.918 -532.905
348.15 -493.950 148.880 -545.783
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刚果(金)Kambove矿区氧化铜钴矿的工艺矿物学特征及钴浸出探讨
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赵亚茹 1 , 肖发新 1 , 李辉 2 , Dessy Purbandari 1 , 单连军 3 , 杨翠霞 1 , 郑彬 2 , 许卫 2 , 王硕 2 , 涂赣峰 1
湿法冶金 | 试验研究 2025,44(3): 301-308
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湿法冶金 | 试验研究 2025, 44(3): 301-308
刚果(金)Kambove矿区氧化铜钴矿的工艺矿物学特征及钴浸出探讨
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赵亚茹1, 肖发新1 , 李辉2, Dessy Purbandari1, 单连军3, 杨翠霞1, 郑彬2, 许卫2, 王硕2, 涂赣峰1
作者信息
  • 1 东北大学 冶金学院,辽宁 沈阳 110819
  • 2 中国有色创新研究院(天津)有限公司,天津 300380
  • 3 沈阳有色金属研究院有限公司,辽宁 沈阳 110141

    • 赵亚茹(2000—),女,硕士研究生,主要研究方向有色金属冶金。

通讯作者:

肖发新(1980—),男,博士,副教授,主要研究方向有色金属冶金、固废资源化、纳米材料。E-mail:。
Discussion on Process Mineralogical Characteristics and Cobalt Leaching of Copper-Cobalt Oxide Ores in Kambove Mining Area,Congo(DRC)
Yaru ZHAO1, Faxin XIAO1 , Hui LI2, Purbandari DESSY1, Lianjun SHAN3, Cuixia YANG1, Bin ZHENG2, Wei XU2, Shuo WANG2, Ganfeng TU1
Affiliations
  • 1 School of Metallurgy, Northeastern University, Shenyang 110819, China
  • 2 China Nonferrous Metal Innovation Research Institute (Tianjin) Co., Ltd., Tianjin 300380, China
  • 3 Shenyang Research Institute of Nonferrous Metals Co., Ltd., Shenyang 110141, China
出版时间: 2025-06-20 doi: 10.13355/j.cnki.sfyj.2025.03.003
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摘要
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针对刚果(金)Kambove矿区氧化铜钴矿钴浸出率不高的问题,采用MLA、偏光显微镜、SEM等手段对该氧化铜钴矿的矿物学特征进行分析,并在此基础上,分别研究了以焦亚硫酸钠、Fe粉、SO2气体为还原剂浸出该矿石中的钴,考察了不同还原剂及用量对浸出效果的影响。结果表明:矿石中主要的铜矿物为假孔雀石、孔雀石、磷铜矿;主要的钴矿物为铜钴硬锰矿和水钴矿,主要的脉石矿物为粉砂岩、石英、绢云母、绿泥石;矿石中铜、钴赋存状态复杂,钴矿物粒度细小且多为包裹体,钴理论浸出率为92.82%;3种还原剂对钴浸出效果中SO2的浸出效果最好,在液固体积质量比3∶1、硫酸用量26.7 g/L、SO2通入量为理论量的1.7倍、反应温度38 ℃、反应时间3 h最佳浸出条件下,钴浸出率为85.48%,接近理论浸出率。研究结果可为Kambove矿区钴资源的高效利用提供理论和技术支持。

氧化铜钴矿  /  刚果(金)  /  Kambove矿区  /  工艺矿物学  /  钴  /  浸出  /  SO2  /  还原剂

In response to the issue of low cobalt leaching rate from oxidized copper-cobalt ore in the Kambove mining area of Congo(DRC), the mineralogical characteristics of the ore were analyzed by Mineral Liberation Analysis (MLA), polarized light microscopy, and Scanning Electron Microscopy (SEM). Based on the findings, leaching of cobalt from the ore with sodium pyrosulfite, Fe powder and SO2 as reducing agents was studied. The influence of different reducing agents and dosage on the leaching effect was investigated. The resluts reveal that the primary copper minerals in the ore are pseudomalachite, malachite, and libethenite, while the main cobalt minerals are copper-cobalt-bearing manganese oxide and heterogenite. The gangue minerals predominantly consist of siltstone, quartz, sericite, and chlorite. The occurrence states of copper and cobalt in the ore are complex, with cobalt minerals being fine-grained and mostly occurring as inclusions. The theoretical leaching rate of cobalt is calculated to be 92.82%. Compared with the three reducing agents, the leaching effect of SO2 is better. Under the optimal conditions of liquid volume to solid mass ratio of 3∶1, sulfuric acid dosage of 26.7 g/L, SO2 amount at 1.7 times the theoretical amount, reaction temperature of 38 ℃, and reaction duration of 3 h, the cobalt leaching rate can reach 85.48%, approaching the theoretical maximum. The research results can provide both theoretical and technical support for the efficient utilization of cobalt resources in the Kambove mining area of Congo(DRC).

oxidized copper-cobalt ore  /  Congo(DRC)  /  Kambove mining area  /  process mineralogy  /  cobalt  /  leaching  /  SO2  /  reductant
赵亚茹, 肖发新, 李辉, Dessy Purbandari, 单连军, 杨翠霞, 郑彬, 许卫, 王硕, 涂赣峰. 刚果(金)Kambove矿区氧化铜钴矿的工艺矿物学特征及钴浸出探讨. 湿法冶金, 2025 , 44 (3) : 301 -308 . DOI: 10.13355/j.cnki.sfyj.2025.03.003
Yaru ZHAO, Faxin XIAO, Hui LI, Purbandari DESSY, Lianjun SHAN, Cuixia YANG, Bin ZHENG, Wei XU, Shuo WANG, Ganfeng TU. Discussion on Process Mineralogical Characteristics and Cobalt Leaching of Copper-Cobalt Oxide Ores in Kambove Mining Area,Congo(DRC)[J]. Hydrometallurgy of China, 2025 , 44 (3) : 301 -308 . DOI: 10.13355/j.cnki.sfyj.2025.03.003
正文
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钴是一种关键战略金属,因具有卓越的耐热性、耐腐蚀性和磁性而广泛应用于新能源、航空航天、机械制造、国防军工等领域[1]。但钴的独立钴矿物极为稀少,通常伴生于铜钴矿、镍钴矿、砷钴矿和黄铁矿矿床中[2-3]。从全球钴资源分布来看,非洲的氧化铜钴资源占据着举足轻重的地位[4-5],其中刚果(金)的钴储量最为丰富,约占全球的48%[4]。作为加中非成矿带的关键组成部分[6-7],刚果(金)Kambove 矿区位于赞比亚—刚果(金)铜矿带的北西部,是非洲中部卢菲利(Lufilian)弧形构造带北西段的一部分,加丹加弧形成矿带中部[8]。区内已发现多处世界级铜钴矿床,如Kamove、Kamoya、Kamfunduwa、Msesa等[9]。该矿区铜钴矿储量可观,矿床类型多样,矿体形态复杂,矿体分布具有一定的规律性和集群性,开采历史悠久且开发潜力较大。
目前,从低品位氧化铜钴矿石中提取钴的方法主要为湿法,典型的工艺流程为浸出—萃取—电积—沉淀钴。直接酸浸法应用较为广泛,但只能溶解以二价钴元素存在的钴矿物。为提高浸出效率和适应不同矿石性质,常结合使用搅拌强化浸出。但无论是单独搅拌浸出还是与浮选预处理结合后的搅拌浸出都存在一定缺陷,如对设备要求高、能耗大、选择性不高等,尤其是随矿石不断开采,矿石性质也会发生变化,从而影响浸出效率。相较而言,强化还原浸出法技术成熟,对矿石的适应性强,可将矿石中难以浸出的三价钴还原为二价钴,从而提高钴浸出率,同时通过控制反应条件可减少杂质干扰,提高产品纯度。当前,Kambove矿区企业大多采用焦亚硫酸钠作为还原剂还原浸出钴,但钴浸出率仅在60%~75%之间,浸出效果不够理想[10-13]。氧化铜钴矿具有成矿作用和产物复杂、矿石种类繁多等特点,矿物特征会影响铜钴资源浸出工艺的设计[14-15],而目前对Kambove 矿区氧化铜钴矿的矿物学特征研究鲜见报道。因此,试验针对刚果(金)Kambove矿区的某氧化铜钴矿的矿物学特征进行了研究,深度解析了其化学成分及物相组成、铜钴的赋存状态、嵌布特征及嵌布粒度,根据矿物学特征及当地企业的钴浸出生产实践进一步用不同还原剂开展钴浸出研究,确定了最佳还原剂和用量,以期为刚果(金)Kambove矿区氧化铜钴矿高效利用提供有益借鉴。
1 试验部分
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1.1 原料、试剂与仪器
原料:刚果(金)某企业的氧化铜钴矿石,取自Kambove矿区,分矿石和粉体2类样品。其中,矿石粒径为3~10 cm,用于工艺矿物学研究;粉体样品粒度为0.075 mm通过率60%。样品呈灰白色粉状,质轻。
由矿样的XRD分析结果(图1)可知:主要物相结构为石英、绿泥石、碱式碳酸铜、云母和辉铜矿;钴矿石可能因含量较低,在XRD图谱中未发现含钴矿物。
试验用试剂为焦亚硫酸钠(国药,分析纯)、硫酸(国药,分析纯)、SO2(沈阳气体制造有限公司,一级)等。
工艺矿物学分析所用设备为全自动矿物分析仪(MLA 650)、偏光显微镜(蔡司,axioskop40)、扫描电镜(FEI 650)、XRD(德国布鲁克,D8 ADVANCE)。浸出试验所用设备为集热式恒温加热水浴锅(DF-101S,邦西仪器),采用ICP(AVIO500,PE)分析浸出渣中钴含量,采用XRD、SEM(日本电子,JSM-7800F)和IR(日本岛津,Tracer)对浸出渣进行结构表征。
1.2 试验方法
1.2.1 矿物学特征分析
采用MLA及其软件表征矿石的矿物组成及含量、粉体样品中主要矿物的连生类型,铜钴元素在各矿物中的赋存占比;采用偏光显微镜和扫描电镜对矿石中主要矿物产出特征,矿物之间共生关系进行表征;采用偏光显微镜线段法对其工艺粒度进行测定和统计。
1.2.2 最佳还原剂的选择
根据前期研究结果可知,还原剂对氧化铜钴矿浸出影响较大,因此,分别用焦亚硫酸钠、Fe粉、 SO 2 为还原剂考察了不同还原剂对钴浸出率的影响,从而确定最佳还原剂及其用量。
试验方法:量取60 mL水置于200 mL烧杯中,将烧杯放入集热式恒温加热水浴锅中,开启搅拌,加入20 g氧化铜钴矿,同时缓慢加入1.6 g硫酸及理论用量1.5倍的还原剂,升温至38 ℃并持续搅拌3 h;待反应结束后抽滤并用少量水洗涤,滤渣烘干后称重并测定其中钴含量,计算钴浸出率。通过前期优化浸出条件探索试验确定了适宜的浸出条件,在液固体积质量比3∶1、硫酸用量26.7 g/L、反应温度38 ℃、反应时间3 h、磨矿粒度0.075 μm通过率60%条件下确定最佳还原剂。并在此条件下进一步试验,确定最佳还原剂用量。此外,对优化条件下所得浸出渣进行成分分析,计算钴浸出率,同时对浸出渣进行表征。
2 Kambove铜钴矿的工艺矿物学分析
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2.1 原矿的分布状态与化学组成
采用矿物自动定量检测系统(FEI,MLA650)对矿石的分布状态进行分析,结果如图2所示。
由图2看出:经过分散预处理后,基本消除了细颗粒相互接触团聚、凝絮现象,颗粒分散性良好,保证了后续测量数据的可靠性和真实性。矿石化学多元素分析结果见表1。
由表1可知:该矿石中可供选矿回收的有价组分为铜和钴,质量分数分别为2.30%、0.274%;其他组分主要为硅、镁、铝和铁等,硫、钙含量较低。为达到富集有用矿物的目的,需通过选矿排除的脉石组分主要是SiO2、Al2O3、MgO、K2O及P2O5,质量分数分别为61.63%、12.77%、7.02%、2.18%及0.780%,共计84.38%。
2.2 矿物组成分析
采用矿物自动定量检测系统(MLA)测定矿石的矿物组成,结果见表2。
由表2可知:原矿中铜矿物以氧化铜矿物为主,主要为假孔雀石、孔雀石和磷铜矿,占比分别为2.533%、0.797%和0.471%,并含有少量硅孔雀石、赤铜矿,微量黑铜矿,而硫化铜矿物主要为辉铜矿、斑铜矿和黄铜矿等;钴矿物主要为铜钴硬锰矿和水钴矿,占比分别为0.787%、0.197%;铁矿物主要为褐铁矿,占比为2.812%,硫化物含量较低;脉石矿物主要来自粉砂岩的矿物,砂屑成分主要为石英,占比为29.547%,杂基成分包含绢云母、绿泥石和微晶石英等。
2.3 主要有用矿物的嵌布特征
矿石中的主要有用矿物为假孔雀石、孔雀石、磷铜矿、铜钴硬锰矿和水钴矿等。采用MLA、偏光显微镜和SEM-EDS针对这些矿物的嵌布特征进行研究,结果表明:1)假孔雀石主要与磷铜矿、褐铁矿和孔雀石等金属矿物,及粉砂岩、石英、绿泥石和绢云母等脉石矿物连生;2)孔雀石主要与假孔雀石、褐铁矿、黑铜矿及硫化铁矿物等金属矿物连生,并与石英、绿泥石、粉砂岩等脉石矿物连生;3)磷铜矿矿物主要与假孔雀石、粉砂岩、石英、绿泥石和褐铁矿等铜矿物连生;4)铜钴硬锰矿主要与褐铁矿、水钴矿等金属矿物连生,并与绿泥石、粉砂岩、石英和绢云母等脉石矿物连生,少量与假孔雀石、孔雀石等铜矿物连生;5)水钴矿物主要与铜钴硬锰矿、褐铁矿等铁锰矿物连生,并与粉砂岩、镁绿泥石、石英和绢云母等脉石矿物连生,少量与铜矿物连生。
2.4 矿石中铜和钴的赋存状态
通过铜矿物和钴矿物的矿物量和电子探针分析数据,经元素配分计算,得出铜和钴在矿石矿物中的赋存状态。其中,矿石中钴元素的分配及平衡计算结果见表3。
由表3可知,钴赋存在多种矿物中,赋存状态十分复杂:55.70%的钴赋存在水钴矿和铜钴硬锰矿中,2.83%的钴赋存在假孔雀石、孔雀石和磷铜矿等铜矿物中,以上赋存形式的钴可通过浸出回收;9.33%的钴赋存在粉砂岩中,24.96%的钴赋存在绿泥石中,部分粉砂岩和绿泥石中的钴可被浸出。根据矿物学特征,理论上可被浸出的钴质量分数为92.82%,剩余5.42%的钴赋存在氧化铁矿物中,1.76%的钴赋存在绢云母中,这部分钴较难浸出回收,易造成损失。
3 浸出探索试验结果与讨论
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3.1 还原剂的选择
在液固体积质量比3∶1、硫酸用量26.7 g/L、还原剂用量为理论量的1.5倍、反应温度38 ℃、反应时间3 h、磨矿粒度0.075 μm通过率60%条件下,分别以焦亚硫酸钠、Fe粉、SO2为还原剂浸出氧化铜钴矿中的钴,考察不同还原剂对钴浸出率的影响,结果如图3所示。
由图3可知,还原剂对Kambove矿区氧化铜钴矿中钴浸出率影响明显:当以Fe粉为还原剂时,钴浸出率最低;以SO2为还原剂时,钴浸出率最高;焦亚硫酸钠比SO2对钴的浸出效果更弱,这与其矿物特征有一定关系。该矿物中55.70%的钴赋存在铜钴硬锰矿和水钴矿中,SO2气体以小气泡形式通入到溶液中,能与矿物表面持续接触,对钴的还原浸出时间更长,效果更好;而焦亚硫酸钠是一次性加入到溶液中,还原过程所分解的SO2气体利用率更低,因此钴浸出效果不及SO2气体;此外,加入SO2后,溶液酸度显著增大,有利于钴的浸出。由于该矿物中钴被褐铁矿包裹的较少,仅占5.42%,因此,Fe粉还原浸出的效果反而更差。
3.2 SO2还原浸出钴
3.2.1 SO2通入量对钴浸出率的影响
为进一步探讨SO2用量对Kambove矿区氧化铜钴矿中钴浸出的影响,在液固体积质量比3∶1、硫酸用量26.7 g/L、反应温度38 ℃、反应时间3 h、磨矿粒度0.075 μm通过率60%条件下,分别通入理论用量的1.1、1.3、1.5、1.7、2.0、2.25倍的SO2气体作为还原剂浸出钴,考察SO2通入量(理论量的倍数)对氧化铜钴矿中钴浸出率的影响,结果如图4所示。
由图4可知:随SO2通入量增大,钴浸出率缓慢升高,SO2通入量升至理论量的1.7倍时,钴浸出率为85.48%;随SO2通入量进一步增加,钴浸出率几乎不变。考虑到SO2过量会导致气体逸出污染环境,还会增加还原剂成本,故SO2通入量以控制在理论量的1.7倍为宜。需要注意的是,在企业实际生产实践中,SO2气体的利用率低于实验室,钴浸出率也低于预期,这可能与其加入方式有关,有待进一步优化改进。
3.2.2 浸出机制分析
以SO2为还原剂时,SO2将氧化铜钴矿浆中的不溶性三价钴化合物还原为可溶性二价钴进入溶液[16]。主要反应如下:
$\begin{array}{c} 2 \mathrm{CoOOH}+2 \mathrm{H}^{+}+\mathrm{SO}_{2}=2 \mathrm{Co}^{2+}+ \\ \mathrm{SO}_{4}^{2-}+2 \mathrm{H}_{2} \mathrm{O} \end{array}$
根据《高温水溶液热力学数据手册》[17]提供的H+、SO2、Co2+、 SO 4 2 -、H2O在不同温度下的热力学数据,采用经典热力学公式分别计算得到不同温度下CoOOH的标准生成热力学数据。并在此基础上,进一步计算得到式(1)的热力学数据,结果见表4。
由表4可知:在25~75 ℃范围内,水钴矿浸出反应的吉布斯自由能ΔrG均为负值,说明反应能够自发进行;且随反应温度升高,ΔrG逐渐减小,说明升高温度有利于反应发生。
采用X射线衍射仪对最佳条件下SO2还原浸出渣进行分析,结果如图5所示。可知,浸出渣的物相主要为石英、云母、绿泥石、褐铁矿。对比浸出前矿样的XRD图谱(图2)可看出,浸出前后,矿石中的主要物相基本不变,但浸出渣中石英的衍射峰略有增强,原因可能是含铜钴较多的水钴矿和铜钴硬锰矿等矿物被浸出,使得石英等物相在矿物中占比有所上升。
采用场发射扫描电子显微镜对浸出渣进行表面形貌和点扫描,结果如图6所示。
由图6(a)看出:浸出渣较粗糙,存在不规则的孔洞及裂纹,颗粒大小不一。由图6(b)看出:孔隙内部结构复杂,这些孔洞和裂纹可能是由更深层次的金属离子溶解造成的。由图6(c)~(g)看出:浸出渣的主要元素为O、Si、Fe,还含有少量Mg、Al、Co;在不同形状处做打点分析显示,元素分布不均匀,如较亮的块状处(样点1#、4#)的主要元素为Fe、O等物质,结合XRD推测其可能为褐铁矿;较暗的块状处(样点2#)的主要元素为Si、O等物质,结合XRD推测其可能为石英;棒状处(样点3#)的主要元素为O、Si及少量的金属元素,结合XRD推测其可能为石英或绿泥石等物质。
氧化铜钴矿及氧化铜钴矿的SO2还原浸出渣的红外光谱如图7所示。可以看出:在3 567.36、3 422.15及1 622.43 cm-1处的吸收峰是—OH的伸缩振动峰;1 882.82 cm-1处有较弱的吸收峰出现,推测是绢云母、绿泥石等蚀变矿物产生所致;997.31 cm-1处的吸收峰与Si—O键的伸缩振动有关,这与XRD显示含有大量石英的结论一致;在785.98和678.63 cm-1较低波数处出现的吸收峰与Me—O键的弯曲振动有关;467.96 cm-1处的吸收峰可能为金属-金属或金属-氧键的振动,Co—O或Cu—O键的拉伸振动等。对比可知,浸出前后的官能团基本不变,但浸出渣的吸收峰有所增强,推测可能为部分铜钴硬锰矿、水钴矿及少量的褐铁矿中的钴进入溶液,从而使得其他物相占比增加、透过率降低、吸收峰更加明显。
4 结论
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1)通过对刚果(金)Kambove矿区某氧化铜钴矿的矿物学特征进行系统解析,明确了矿石中主要铜、钴矿物和脉石矿物组成,共存状态及其工艺粒度特征。根据钴赋存状态计算得知,矿石中钴的理论浸出率为92.82%,而7.18%的钴赋存在氧化铁矿物和绢云母中,难以通过常规工艺浸出。
2)分别以焦亚硫酸钠、Fe粉、SO2气体为还原剂浸出该氧化铜钴矿中的钴时,SO2气体的浸出效果更好,在液固体积质量比3∶1、硫酸用量26.7 g/L,SO2气体通入量为理论量的1.7倍、反应温度38 ℃、反应时间3 h的优化条件下,渣计钴浸出率为85.48%,与理论值接近。SO2还原浸出渣结构表征结果表明,水钴矿、铜钴硬锰矿等矿物中的钴被浸出,少部分绢云母、粉砂岩中的钴未被浸出。
3)对氧化铜钴矿的矿物学特征和浸出工艺协同研究,可为提高钴浸出率提供理论和技术参考。该强化浸出工艺条件下所得钴浸出率接近工艺矿物学表征的理论钴浸出率,可为Kambove矿区氧化铜钴矿的高效处理提供可行的理论指导技术支持。后续建议对实际生产实践中SO2的加入方式进行优化改进研究,以提高还原剂的利用率。
基金
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  • 中国有色集团科技项目(2023KJZX027)
  • 国家重点研发计划(2020YFC1909003)
文献
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doi: 10.13355/j.cnki.sfyj.2025.03.003
  • 接收时间：2025-02-07
  • 首发时间：2025-09-01
  • 出版时间：2025-06-20
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  • 收稿日期：2025-02-07
基金
中国有色集团科技项目(2023KJZX027)
国家重点研发计划(2020YFC1909003)
作者信息
    1 东北大学 冶金学院,辽宁 沈阳 110819
    2 中国有色创新研究院(天津)有限公司,天津 300380
    3 沈阳有色金属研究院有限公司,辽宁 沈阳 110141

通讯作者:

肖发新(1980—),男,博士,副教授,主要研究方向有色金属冶金、固废资源化、纳米材料。E-mail:。
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https://castjournals.cast.org.cn/joweb/sfyj/CN/10.13355/j.cnki.sfyj.2025.03.003
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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