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Article(id=1240648788793160047, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240648781595725960, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.05.010, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1711641600000, receivedDateStr=2024-03-29, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773723321388, onlineDateStr=2026-03-17, pubDate=1727712000000, pubDateStr=2024-10-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773723321388, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773723321388, creator=13701087609, updateTime=1773723321388, updator=13701087609, issue=Issue{id=1240648781595725960, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='5', pageStart='1', pageEnd='184', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773723319672, creator=13701087609, updateTime=1773824608750, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241073618831078097, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240648781595725960, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241073618831078098, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240648781595725960, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=51, endPage=56, ext={EN=ArticleExt(id=1240648790403772812, articleId=1240648788793160047, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Synergistic Oxidation of NaClO and KMnO4 on Flotation Separation of Chalcopyrite and Pyrite and Mechanism Therein, columnId=1236276106932842717, journalTitle=Mining and Metallurgical Engineering, columnName=MINERAL PROCESSING, runingTitle=null, highlight=null, articleAbstract=

The effects of separate and combined usage of NaClO and KMnO4 on the flotation separation of chalcopyrite and pyrite were investigated by performing flotation and adsorption tests, infrared spectroscopy (IR) and XPS analysis. The results show that selective separation of chalcopyrite and pyrite can be achieved with NaClO and KMnO4 in a ratio of 10∶1, the total oxidant dosage of 70 mg/L, pulp pH of 10, and oxidation time of 3 min. It is shown that the recovery of chalcopyrite can exceed 92%, while the recovery of pyrite is less than 8%. The IR and XPS analyses show that a combined usage of NaClO and KMnO4 obviously changes the surface property of pyrite, resulting in hydrophilic oxidized substances on the surface, such as iron oxide, iron hydroxide and iron sulfate, which impedes the adsorption of collectors, thus reducing floatability of pyrite. The chalcopyrite surface remains mildly inert to NaClO and KMnO4 under certain conditions. Consequently, the adsorption of xanthate on chalcopyrite is remarkably higher than that on pyrite, which favors their flotation separation.

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通过浮选试验、吸附实验、红外光谱和XPS分析等研究了NaClO和KMnO4单独使用以及组合使用对黄铜矿和黄铁矿浮选分离的影响。结果表明，在NaClO与KMnO4质量比10∶1、总质量浓度70 mg/L，矿浆pH=10，氧化时间3 min条件下，黄铜矿回收率达到92%以上，黄铁矿回收率低于8%，较好地实现了黄铜矿与黄铁矿的选择性分离。红外光谱和XPS分析结果表明，组合药剂明显改变了黄铁矿的表面性质，使其表面氧化为氧化铁、氢氧化铁和硫酸铁等亲水性物质，并阻碍捕收剂的吸附，从而降低黄铁矿的可浮性。黄铜矿表面在一定处理条件下对NaClO和KMnO4保持温和惰性，因此黄铜矿表面吸附的黄药量远大于黄铁矿表面，这有利于黄铜矿与黄铁矿的浮选分离。

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印万忠（1970—），男，浙江杭州人，博士，教授，主要从事矿物浮选理论与技术研究。E-mail：
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龙逸云（2000—），男，湖南湘潭人，硕士研究生，主要研究方向为矿物浮选理论与技术。E-mail：

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龙逸云（2000—），男，湖南湘潭人，硕士研究生，主要研究方向为矿物浮选理论与技术。E-mail：

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龙逸云（2000—），男，湖南湘潭人，硕士研究生，主要研究方向为矿物浮选理论与技术。E-mail：

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Minerals Engineering, 2015, 72: 94-100., articleTitle=Floatability and oxidation of pyrite with different spatial symmetry, refAbstract=null)], funds=[Fund(id=1240648801992634568, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, awardId=52174239, language=CN, fundingSource=国家自然科学基金(52174239), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1240648793457226387, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, xref=null, ext=[AuthorCompanyExt(id=1240648793461420693, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, companyId=1240648793457226387, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zijin School of Geology and Mining, Fuzhou University, Fuzhou 350000, Fujian, China), AuthorCompanyExt(id=1240648793465614998, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, companyId=1240648793457226387, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=福州大学　紫金地质与矿业学院，福建　福州　350000)])], figs=[ArticleFig(id=1240648799383778258, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=EN, label=null, caption=null, figureFileSmall=+KLPNJ+6Hk0NUKOz6tAgWA==, figureFileBig=LlR+Mcfq77nYamGu1WF9Yw==, tableContent=null), ArticleFig(id=1240648799467664348, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=CN, label=图1, caption=浮选试验流程, figureFileSmall=+KLPNJ+6Hk0NUKOz6tAgWA==, figureFileBig=LlR+Mcfq77nYamGu1WF9Yw==, tableContent=null), ArticleFig(id=1240648799731905521, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=EN, label=null, caption=null, figureFileSmall=mK+qhyzvQfITtXNNFPJ3qw==, figureFileBig=074P3pAHOYJbE2pM3R6Yuw==, tableContent=null), ArticleFig(id=1240648799857734649, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=CN, label=图2, caption=乙基黄药质量浓度对矿物可浮性的影响, figureFileSmall=mK+qhyzvQfITtXNNFPJ3qw==, figureFileBig=074P3pAHOYJbE2pM3R6Yuw==, tableContent=null), ArticleFig(id=1240648800004534277, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=EN, label=null, caption=null, figureFileSmall=so7PJVca19CrSs7KHuvq8w==, figureFileBig=SBGlvhUphz/VUd6DFUqwJg==, tableContent=null), ArticleFig(id=1240648800109391886, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=CN, label=图3, caption=NaClO和KMnO4质量浓度对黄铜矿与黄铁矿可浮性的影响

（a）NaClO；（b）KMnO4

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（a）组合药剂用量配比；（b）组合药剂质量浓度

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（a）黄铜矿；（b）黄铁矿

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（a）全谱；（b）Fe2p；（c）S2p；（d）O1s

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氧化剂种类产品名称产率/%品位/%回收率/%分离效率/%
CuSCuS
无精矿41.9022.1240.5458.7931.9029.67
尾矿58.1012.2043.9041.2168.10
原矿100.0016.7042.17100.00100.00
KMnO4精矿79.1019.5539.0786.6462.0624.00
尾矿20.907.2945.3813.3637.94
原矿100.0016.7042.17100.00100.00
NaClO精矿70.3122.5638.4778.6545.1336.03
尾矿26.696.6145.9521.3554.87
原矿100.0016.7042.17100.00100.00
KMnO4+NaClO精矿66.2024.0436.2380.6737.9547.02
尾矿33.805.0848.2419.3362.05
原矿100.0016.7042.17100.00100.00
), ArticleFig(id=1240648801371877525, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=CN, label=表1, caption=

人工混合矿浮选试验结果

, figureFileSmall=null, figureFileBig=null, tableContent=
氧化剂种类产品名称产率/%品位/%回收率/%分离效率/%
CuSCuS
无精矿41.9022.1240.5458.7931.9029.67
尾矿58.1012.2043.9041.2168.10
原矿100.0016.7042.17100.00100.00
KMnO4精矿79.1019.5539.0786.6462.0624.00
尾矿20.907.2945.3813.3637.94
原矿100.0016.7042.17100.00100.00
NaClO精矿70.3122.5638.4778.6545.1336.03
尾矿26.696.6145.9521.3554.87
原矿100.0016.7042.17100.00100.00
KMnO4+NaClO精矿66.2024.0436.2380.6737.9547.02
尾矿33.805.0848.2419.3362.05
原矿100.0016.7042.17100.00100.00
), ArticleFig(id=1240648801497706656, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
氧化剂种类乙基黄药吸附量/（mg·g-1）
黄铜矿黄铁矿
无1.840.39
KMnO41.690.08
NaClO1.600.09
KMnO4+NaClO1.710.02
), ArticleFig(id=1240648801598369959, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=CN, label=表2, caption=

不同药剂制度下乙基黄药在黄铜矿和黄铁矿表面的吸附量

, figureFileSmall=null, figureFileBig=null, tableContent=
氧化剂种类乙基黄药吸附量/（mg·g-1）
黄铜矿黄铁矿
无1.840.39
KMnO41.690.08
NaClO1.600.09
KMnO4+NaClO1.710.02
), ArticleFig(id=1240648801736782005, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称Cu2pFe2pS2pO1sC1s
黄铜矿12.9711.1226.6023.1426.17
黄铜矿+KMnO412.0911.0226.3223.3827.19
黄铜矿+NaClO11.0010.3121.5224.6632.51
黄铜矿+KMnO4+NaClO11.7110.1224.7023.9729.50
黄铁矿—10.3431.1226.9931.55
黄铁矿+KMnO4—9.9718.7434.8636.43
黄铁矿+NaClO—5.4120.0041.7132.88
黄铁矿+KMnO4+NaClO—4.4918.6144.0932.81
), ArticleFig(id=1240648801862611134, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240648788793160047, language=CN, label=表3, caption=

药剂作用前后矿物表面元素相对含量（原子分数）

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称Cu2pFe2pS2pO1sC1s
黄铜矿12.9711.1226.6023.1426.17
黄铜矿+KMnO412.0911.0226.3223.3827.19
黄铜矿+NaClO11.0010.3121.5224.6632.51
黄铜矿+KMnO4+NaClO11.7110.1224.7023.9729.50
黄铁矿—10.3431.1226.9931.55
黄铁矿+KMnO4—9.9718.7434.8636.43
黄铁矿+NaClO—5.4120.0041.7132.88
黄铁矿+KMnO4+NaClO—4.4918.6144.0932.81
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NaClO和KMnO4协同氧化对黄铜矿与黄铁矿浮选分离的影响及其机理
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龙逸云 , 印万忠 , 龙恺云
矿冶工程杂志 | 选矿 2024,44(5): 51-56
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矿冶工程杂志 | 选矿 2024, 44(5): 51-56
NaClO和KMnO4协同氧化对黄铜矿与黄铁矿浮选分离的影响及其机理
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龙逸云 , 印万忠 , 龙恺云
作者信息
  • 福州大学　紫金地质与矿业学院，福建　福州　350000

    • 龙逸云（2000—），男，湖南湘潭人，硕士研究生，主要研究方向为矿物浮选理论与技术。E-mail：

通讯作者:

印万忠（1970—），男，浙江杭州人，博士，教授，主要从事矿物浮选理论与技术研究。E-mail：
Synergistic Oxidation of NaClO and KMnO4 on Flotation Separation of Chalcopyrite and Pyrite and Mechanism Therein
Yiyun LONG , Wanzhong YIN , Kaiyun LONG
Affiliations
  • Zijin School of Geology and Mining, Fuzhou University, Fuzhou 350000, Fujian, China
出版时间: 2024-10-01 doi: 10.3969/j.issn.0253-6099.2024.05.010
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摘要
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通过浮选试验、吸附实验、红外光谱和XPS分析等研究了NaClO和KMnO4单独使用以及组合使用对黄铜矿和黄铁矿浮选分离的影响。结果表明，在NaClO与KMnO4质量比10∶1、总质量浓度70 mg/L，矿浆pH=10，氧化时间3 min条件下，黄铜矿回收率达到92%以上，黄铁矿回收率低于8%，较好地实现了黄铜矿与黄铁矿的选择性分离。红外光谱和XPS分析结果表明，组合药剂明显改变了黄铁矿的表面性质，使其表面氧化为氧化铁、氢氧化铁和硫酸铁等亲水性物质，并阻碍捕收剂的吸附，从而降低黄铁矿的可浮性。黄铜矿表面在一定处理条件下对NaClO和KMnO4保持温和惰性，因此黄铜矿表面吸附的黄药量远大于黄铁矿表面，这有利于黄铜矿与黄铁矿的浮选分离。

黄铜矿  /  黄铁矿  /  表面氧化  /  浮选  /  抑制剂  /  捕收剂  /  氧化剂  /  铜硫分离

The effects of separate and combined usage of NaClO and KMnO4 on the flotation separation of chalcopyrite and pyrite were investigated by performing flotation and adsorption tests, infrared spectroscopy (IR) and XPS analysis. The results show that selective separation of chalcopyrite and pyrite can be achieved with NaClO and KMnO4 in a ratio of 10∶1, the total oxidant dosage of 70 mg/L, pulp pH of 10, and oxidation time of 3 min. It is shown that the recovery of chalcopyrite can exceed 92%, while the recovery of pyrite is less than 8%. The IR and XPS analyses show that a combined usage of NaClO and KMnO4 obviously changes the surface property of pyrite, resulting in hydrophilic oxidized substances on the surface, such as iron oxide, iron hydroxide and iron sulfate, which impedes the adsorption of collectors, thus reducing floatability of pyrite. The chalcopyrite surface remains mildly inert to NaClO and KMnO4 under certain conditions. Consequently, the adsorption of xanthate on chalcopyrite is remarkably higher than that on pyrite, which favors their flotation separation.

chalcopyrite  /  pyrite  /  surface oxidation  /  flotation  /  depressant  /  collector  /  oxidant  /  Cu/S separation
龙逸云, 印万忠, 龙恺云. NaClO和KMnO4协同氧化对黄铜矿与黄铁矿浮选分离的影响及其机理. 矿冶工程杂志, 2024 , 44 (5) : 51 -56 . DOI: 10.3969/j.issn.0253-6099.2024.05.010
Yiyun LONG, Wanzhong YIN, Kaiyun LONG. Synergistic Oxidation of NaClO and KMnO4 on Flotation Separation of Chalcopyrite and Pyrite and Mechanism Therein[J]. Mining and Metallurgical Engineering, 2024 , 44 (5) : 51 -56 . DOI: 10.3969/j.issn.0253-6099.2024.05.010
正文
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铜是重要的有色金属资源[1]，而黄铜矿是主要的提铜矿物之一[2]。黄铜矿通常与其他硫化矿伴生，尤其是黄铁矿[3]，因此黄铜矿与黄铁矿的有效分离对铜资源的高效利用至关重要。黄铁矿天然可浮性较差，黄铜矿/黄铁矿分离通常采用抑制黄铁矿、浮选黄铜矿的方法。黄铁矿常用的无机抑制剂[4]包括石灰、氰化物、硫氧化物和氧化剂类等，因具有价格便宜、原料来源广泛以及选择性良好等优点，这类抑制剂在多金属硫化矿浮选实践中得到了广泛应用[5]。氧化剂类抑制剂具有对伴生金属影响较小、能适用于较宽泛的pH值范围并简化矿浆处理和降低环境污染等优点，受到大家的青睐。
表面氧化通常通过在表面产生亲水性氧化物来降低某些硫化矿物的可浮性[4]。有研究[6]发现，NaClO和KMnO4是黄铁矿的有效氧化剂，可通过使黄铁矿表面形成亲水膜抑制黄铁矿，而对黄铜矿浮选影响很小。然而，单一药剂往往不能达到理想的浮选分离效果。在硫化矿选矿过程中，药剂与药剂之间相互作用，将药剂间各自特有的功能和性能进行协调（药剂之间协同效应），可以表现出更好的物理和化学性能[7]，达到比单一药剂更好的综合浮选效果，以获得更好的浮选精矿指标，还可以减少药剂用量[8]。本文通过一系列浮选试验和表面分析技术，探讨NaClO、KMnO4单独使用以及两者组合作为氧化剂对黄铜矿和黄铁矿浮选分离的影响，并对其作用机理进行了分析，可为铜硫分离提供参考。
1　试验原料及试验方法
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1.1　试验原料及药剂
试验矿样为-38 μm粒级黄铜矿和黄铁矿，黄铜矿纯度95.67%，黄铁矿纯度98.56%，符合单矿物浮选试验要求。
试验所用捕收剂乙基黄药（SEX）、起泡剂甲基异丁基甲醇（MIBC）、pH值调整剂盐酸（HCl）和氢氧化钠（NaOH）、氧化剂高锰酸钾（KMnO4）和次氯酸钠（NaClO）均为分析纯试剂。试验用水为去离子水。
1.2　试验方法
1.2.1　浮选试验
采用XFG型挂槽式浮选机进行单矿物和人工混合矿浮选试验。浮选流程如图1所示。浮选结束后将泡沫产品和槽内产品分别烘干、称重并计算浮选回收率。
人工混合矿浮选试验中，采用分离效率SE来评价黄铜矿和黄铁矿的浮选分离效果：
式中：SE为分离效率，%；γ为浮选精矿产率，%；α和β分别为原矿和精矿中的Cu品位，%；δ为黄铜矿单矿物的Cu品位，%。
1.2.2　检测方法
采用残余浓度法计算乙基黄药在矿物表面的吸附量；利用傅里叶变换红外光谱仪（德国Bruker）测定药剂处理前后矿物的红外光谱；采用1063 XPS光谱仪（美国Thermo Fisher Scientific公司）测量样品电子能谱。
2　试验结果与讨论
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2.1　单矿物浮选试验
2.1.1　捕收剂质量浓度试验
起泡剂MIBC质量浓度10 mg/L、矿浆pH值10时，考察了捕收剂乙基黄药质量浓度对黄铜矿和黄铁矿可浮性的影响，结果如图2所示。由图2可知，两种矿物的可浮性均随着乙基黄药质量浓度增加而升高，乙基黄药质量浓度20～24 mg/L时，黄铜矿回收率稳定在96%附近。综合考虑，确定适宜的乙基黄药质量浓度为20 mg/L。
2.1.2　氧化剂单独使用及组合使用效果研究
MIBC质量浓度10 mg/L、乙基黄药质量浓度20 mg/L、矿浆pH值10、氧化时间3 min条件下，分别考察了NaClO和KMnO4质量浓度对黄铜矿和黄铁矿可浮性的影响，结果如图3所示。由图3（a）可知，随着NaClO质量浓度增加，黄铜矿回收率略有降低，而黄铁矿回收率逐渐下降，NaClO氧化预处理对黄铁矿有较强的抑制作用，而对黄铜矿浮选影响较小。这表明使用NaClO预处理可以实现铜硫有效分离。由图3（b）可知，随着KMnO4质量浓度增加，黄铁矿回收率呈现下降趋势，而黄铜矿回收率在KMnO4质量浓度0～5 mg/L时略有下降，KMnO4质量浓度大于5 mg/L后，黄铜矿回收率急速下降。综合考虑，NaClO质量浓度50 mg/L或KMnO4质量浓度5 mg/L时，两种单矿物分离效果较好，该条件下它们的回收率差值分别为77.80个百分点和82.85个百分点。
MIBC质量浓度10 mg/L、乙基黄药质量浓度20 mg/L、NaClO和KMnO4总质量浓度70 mg/L、矿浆pH值10、氧化时间3 min条件下，考察了NaClO与KMnO4质量配比对黄铜矿和黄铁矿可浮性的影响，结果如图4（a）所示。由图4（a）可见：随着NaClO质量增加，黄铜矿浮选回收率先增加后略有减少，黄铁矿回收率略有增加；NaClO与KMnO4质量比10∶1时黄铜矿与黄铁矿分离效果较好，此时黄铜矿回收率为93.60%、黄铁矿回收率为3.50%。
NaClO与KMnO4质量比10∶1，其他条件不变，组合药剂质量浓度对黄铜矿和黄铁矿浮选回收率的影响如图4（b）所示。由图4（b）可知：组合药剂质量浓度40～70 mg/L时，随着组合药剂质量浓度增大，黄铜矿回收率基本不变，黄铁矿回收率直线下降；组合药剂质量浓度70～90 mg/L时，随着组合药剂质量浓度增大，黄铜矿回收率下降，黄铁矿回收率基本不变。黄铜矿与黄铁矿回收率差值最大时组合药剂质量浓度为70 mg/L，确定适宜的组合药剂总质量浓度为70 mg/L。
2.1.3　矿浆pH值试验
MIBC质量浓度10 mg/L、乙基黄药质量浓度20 mg/L、氧化时间3 min，单独使用时KMnO4质量浓度5 mg/L、NaClO质量浓度50 mg/L，组合使用时NaClO与KMnO4质量比10∶1、总质量浓度70 mg/L，考察了pH值对黄铜矿和黄铁矿可浮性的影响，结果如图5所示。由图5可知，黄铜矿在pH=4～12范围内可浮性都很好；黄铁矿在碱性条件下可浮性很差，pH>8后，黄铁矿回收率低于40%。KMnO4作用下，pH=4～12范围内黄铜矿可浮性变化很小；NaClO及组合药剂作用下，黄铜矿回收率在pH=4～8时略有增加，在pH=8～10时保持平稳，在pH=10～12时有所降低。以KMnO4为氧化剂时，pH值从4升至6，黄铁矿回收率降低了21.81个百分点，在pH=6～8时略有增加，pH值从8升至12，回收率降低了17.88个百分点；以NaClO为氧化剂时，pH值从4升至8，黄铁矿回收率降低了32个百分点，在pH=8～12时黄铁矿回收率略有降低，稳定在20%左右。以NaClO+KMnO4为组合氧化剂时，pH值从4升至6，黄铁矿回收率降低了31.60个百分点，pH值从6升至12，黄铁矿回收率从7.08%缓慢降低至1.90%。这充分说明，组合药剂比单用NaClO或KMnO4对黄铁矿有更强的抑制能力，且不抑制黄铜矿。综合考虑，在pH值为10时能较好地分离黄铜矿与黄铁矿。
2.2　人工混合矿浮选试验
pH=10、乙基黄药质量浓度20 mg/L、MIBC质量浓度10 mg/L、氧化时间3 min，单独使用时KMnO4质量浓度5 mg/L、NaClO质量浓度50 mg/L，组合加药时NaClO与KMnO4质量比10∶1、总质量浓度70 mg/L，进行了人工混合矿浮选分离试验，结果如表1所示。由表1可知，KMnO4和NaClO组合时，可获得产率66.20%、铜品位24.04%、铜回收率80.67%、硫品位36.23%、硫回收率37.95%的精矿，分离效率达到47.02%，分离效果显著。这说明组合药剂对黄铁矿具有选择性抑制作用，能达到强化黄铜矿和黄铁矿浮选分离的目的。
2.3　作用机理分析
2.3.1　捕收剂吸附量测定
pH=10、捕收剂乙基黄药质量浓度20 mg/L、起泡剂MIBC质量浓度20 mg/L条件下，不同药剂制度（与浮选试验条件一致）对黄铜矿和黄铁矿表面乙基黄药吸附量的影响如表2所示。由表2可以看出：与空白组相比，单独使用或组合使用KMnO4和NaClO对乙基黄药在黄铜矿表面吸附量的影响不大；单独添加KMnO4或NaClO后，乙基黄药在黄铁矿表面的吸附量分别下降了0.31 mg/g和0.30 mg/g，组合加药后，乙基黄药在黄铁矿表面的吸附量下降至0.02 mg/g。这表明KMnO4和NaClO对黄铁矿表面有一定抑制效果，两种药剂组合添加时这种抑制效果更显著。
2.3.2　红外光谱分析
图6为矿物与药剂作用前后的红外光谱。查文献可知，乙基黄药的—CH3和—CH2拉伸振动峰位于2 959 cm-1和1 446 cm-1处，位于1 106～1 174 cm-1的拉伸振动峰属于C—O—C，而的拉伸振动峰位于1 061 cm-1左右[9]。由图6（a）可知，与乙基黄药作用后，黄铜矿在2 923.70 cm-1、1 386.19 cm-1、1 093.53 cm-1和1 039.28 cm-1处出现了4个峰，分别为—CH3、—CH2、C—O—C和的对称伸缩振动吸收峰，表明乙基黄药在黄铜矿表面发生了化学吸附。经KMnO4和NaClO单独或组合作用后继续加入乙基黄药对黄铜矿进行处理，所得红外光谱未发生明显变化，这说明氧化剂对黄铜矿影响不大，乙基黄药对黄铜矿的吸附依然有效。由图6（b）可知，经乙基黄药处理后，黄铁矿在2 923.70 cm-1和2 849.47 cm-1处同样出现了—CH3和—CH2的对称伸缩振动吸收峰，这说明乙基黄药能在黄铁矿表面发生化学吸附。但经KMnO4及NaClO单独或组合处理后，黄铁矿表面的乙基黄药伸缩振动峰消失，在600 cm-1和1 000 cm-1左右出现了Fe—O和SO42-的新峰[10]，这说明添加氧化剂后，黄铁矿表面被氧化，导致乙基黄药在黄铁矿表面吸附较差，这时黄铁矿可浮性变差。KMnO4和NaClO可以选择性抑制乙基黄药在黄铁矿表面的吸附，从而实现黄铁矿和黄铜矿的浮选分离。
2.3.3　X射线光电子能谱（XPS）分析
药剂作用前后矿物表面的元素含量如表3所示。可以看出，经KMnO4和NaClO单独或组合处理后，黄铜矿表面主要元素原子分数几乎没有变化，这表明KMnO4及NaClO与黄铜矿表面的相互作用非常弱；而经KMnO4和NaClO单独或组合处理后，黄铁矿表面主要元素原子分数发生了显著变化，表明随着药剂的加入，黄铁矿表面性质发生了显著变化，矿物表面的氧化铁和氢氧化物（711～712 eV宽带）[11]比例增加，导致黄铁矿疏水性降低。组合药剂作用下黄铁矿表面相对原子分数变化幅度较单独药剂作用后更大，此时黄铁矿表面氧化程度更剧烈、浮选回收率也更低。这与浮选试验结果一致。
图7为KMnO4和NaClO组合作用前后黄铁矿的XPS图谱。经组合药剂作用后，矿物表面各元素结合能及峰强都有一定变化。药剂作用前，黄铁矿Fe2p3/2图谱在707.30 eV、709.02 eV和711.60 eV有3个峰，分别代表黄铁矿晶格中Fe原子（Fe（II）-S）、表面结合的Fe原子与硫（Fe（III）-S）以及氧化产物，主要是Fe（III）-O/OH；720.10 eV处的结合能对应于Fe2p1/2的自旋轨道[12]。药剂作用后，Fe（III）-S和Fe（III）-O/OH中Fe的结合能分别偏移至711.40 eV和713.80 eV，且两峰的强度明显增加，在725.60 eV处也出现了一个新的Fe（III）-O/OH强峰，说明与药剂作用后黄铁矿表面发生了明显的氧化。组合药剂促使黄铁矿表面铁向羟基铁转变，从而阻止乙基黄药在其表面吸附。药剂作用前，黄铁矿S2p图谱在162.00 eV、162.90 eV、164.50 eV和169.20 eV有4个峰，分别对应于单硫化物（S2-）、二硫化物（S22-）、多硫化物和元素硫（Sn2-/S0）以及硫酸盐（SO42-）[12]。药剂作用后，S2-结合能位置由162.90 eV偏移到162.70 eV，S22-的强度峰消失，Sn2-/S0结合能位置由164.50 eV偏移到165.90 eV。这说明组合药剂的添加促进了黄铁矿表面硫的氧化，改变了黄铁矿表面的化学环境。在S总量大幅下降的同时，多硫化物和元素硫Sn2-/S0量减少，硫酸盐量增加，单硫化物S2-消失。这些都有利于提高黄铁矿表面的亲水性，使黄铁矿受到严重抑制。药剂作用前，黄铁矿O1s图谱在533.40 eV和532.00 eV有2个峰，分别对应于吸附水和OH-[11]。药剂作用后，上述两峰的位置都有一定偏移且出现了一个新的O2-峰，这表明黄铁矿表面被氧化生成了高价态的亲水性化合物。综上所述，在一定条件下，KMnO4和NaClO组合使用可以选择性氧化黄铁矿而对黄铜矿影响较小，在此条件下可以实现黄铜矿与黄铁矿的选择性分离。这一过程的机理模型如图8所示。
3　结论
收起
1）以乙基黄药为捕收剂时，KMnO4和NaClO组合使用对黄铁矿的抑制作用远大于对黄铜矿的抑制作用，人工混合矿浮选分离试验结果表明，组合药剂的添加可使精矿铜品位提升1.92个百分点、回收率提高21.88个百分点，分离效率达到47.02%。
2）红外光谱和XPS分析结果表明，经KMnO4和NaClO组合处理，乙基黄药在黄铜矿表面的吸附量远大于在黄铁矿表面的吸附量。经组合药剂处理后，黄铁矿表面被严重氧化，并覆盖有亲水性Fe（OH）3、Fe2O3、FeOOH和Fe2（SO4）3。黄铜矿在一定条件下经KMnO4和NaClO组合处理后，矿物表面对该药剂表现为轻度惰性。
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  • 国家自然科学基金(52174239)
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2024年第44卷第5期
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doi: 10.3969/j.issn.0253-6099.2024.05.010
  • 接收时间：2024-03-29
  • 首发时间：2026-03-17
  • 出版时间：2024-10-01
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  • 收稿日期：2024-03-29
基金
国家自然科学基金(52174239)
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    福州大学　紫金地质与矿业学院，福建　福州　350000

通讯作者:

印万忠（1970—），男，浙江杭州人，博士，教授，主要从事矿物浮选理论与技术研究。E-mail：
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鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
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