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Article(id=1241768040421986484, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241768035548205179, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.01.022, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1691942400000, receivedDateStr=2023-08-14, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773990171771, onlineDateStr=2026-03-20, pubDate=1706716800000, pubDateStr=2024-02-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773990171771, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773990171771, creator=13701087609, updateTime=1773990171771, updator=13701087609, issue=Issue{id=1241768035548205179, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='1', pageStart='1', pageEnd='178', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773990170609, creator=13701087609, updateTime=1773993209826, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241780783011140021, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241768035548205179, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241780783015334326, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241768035548205179, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=100, endPage=104, ext={EN=ArticleExt(id=1241768040879165640, articleId=1241768040421986484, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Enrichment of Nickel and Cobalt by Solid-State Reduction of Limonite-Type Nickel Laterite Ore Enhanced by NaFeS2, columnId=1236276106727321817, journalTitle=Mining and Metallurgical Engineering, columnName=METALLURGY, runingTitle=null, highlight=null, articleAbstract=

The effects of the amount of NaFeS2, which was used as an additive, on solid-state reduction and magnetic separation for enrichment of nickel and cobalt, and also the reduction behavior of nickel laterite ore were studied. The results show that with the increase of NaFeS2 addition, the softening and melting temperature of nickel laterite ore decreases correspondingly during the reduction process; while particles of the Ni-Co-Fe alloy obtained by reduction increase accordingly. The enrichment and recovery effects of nickel and cobalt will be better by adding 10% NaFeS2. The nickel laterite ore, after being pressed into briquettes, was subjected to reduction at 1 100 ℃ for 60 min, followed by a process of grinding and magnetic separation, resulting in a high quality nickel-cobalt-iron powder grading 7.89% Ni, 0.66% Co and 74.01% Fe, at corresponding recoveries of 97.13%, 86.78% and 35.81%.

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以NaFeS2为添加剂，研究了NaFeS2用量对红土镍矿固态还原-磁选富集镍、钴及红土镍矿还原行为的影响。结果表明，随着NaFeS2添加量增加，还原过程红土镍矿的软熔特性温度相应降低，还原所得Ni-Co-Fe合金颗粒随之增大；添加10%NaFeS2时，镍、钴的富集和回收效果好，红土镍矿经压团于1 100 ℃还原60 min，再经磨矿-磁选可获得Ni、Co、Fe品位分别为7.89%、0.66%、74.01%，Ni、Co、Fe回收率分别为97.13%、86.78%、35.81%的优质镍钴铁粉产品。

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饶明军（1984—），男，江西广丰人，博士，教授，主要研究方向为复杂铁矿、二次资源清洁高效利用。E-mail：
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肖仁栋（1998—），男，安徽芜湖人，硕士研究生，主要研究方向为镍钴资源提取和矿产资源高效利用。E-mail：

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肖仁栋（1998—），男，安徽芜湖人，硕士研究生，主要研究方向为镍钴资源提取和矿产资源高效利用。E-mail：

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肖仁栋（1998—），男，安徽芜湖人，硕士研究生，主要研究方向为镍钴资源提取和矿产资源高效利用。E-mail：

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NiCoTFeSiO2MgOAl2O3CaOCr2O3S烧失
1.307 20.1442.439.604.823.440.753.190.2413.02
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红土镍矿主要化学成分（质量分数）

, figureFileSmall=null, figureFileBig=null, tableContent=
NiCoTFeSiO2MgOAl2O3CaOCr2O3S烧失
1.307 20.1442.439.604.823.440.753.190.2413.02
), ArticleFig(id=1241779804882669628, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241768040421986484, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
铁物相含量/%分布率/%
针铁矿中铁42.0399.06
赤铁矿中铁0.150.35
硫化物中铁0.140.33
硅酸盐中铁0.110.26
合计42.43100.00
), ArticleFig(id=1241779804991721534, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1241768040421986484, language=CN, label=表2, caption=

红土镍矿中铁主要赋存状态及含量分布

, figureFileSmall=null, figureFileBig=null, tableContent=
铁物相含量/%分布率/%
针铁矿中铁42.0399.06
赤铁矿中铁0.150.35
硫化物中铁0.140.33
硅酸盐中铁0.110.26
合计42.43100.00
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镍物相含量/%分布率/%
铁氧化物中镍1.2595.62
硅酸盐中镍0.0463.52
硫化镍中镍0.0100.77
硫酸镍中镍0.001 20.09
合计1.307 2100.00
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红土镍矿中镍主要赋存状态及含量分布

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镍物相含量/%分布率/%
铁氧化物中镍1.2595.62
硅酸盐中镍0.0463.52
硫化镍中镍0.0100.77
硫酸镍中镍0.001 20.09
合计1.307 2100.00
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NaFeS2强化褐铁矿型红土镍矿固态还原富集镍钴的研究
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肖仁栋 , 陈靖 , 胡美世 , 许斌 , 罗骏 , 张鑫 , 饶明军
矿冶工程杂志 | 冶金 2024,44(1): 100-104
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矿冶工程杂志 | 冶金 2024, 44(1): 100-104
NaFeS2强化褐铁矿型红土镍矿固态还原富集镍钴的研究
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肖仁栋 , 陈靖, 胡美世, 许斌, 罗骏, 张鑫, 饶明军
作者信息
  • 中南大学　资源加工与生物工程学院，湖南　长沙　410083

    • 肖仁栋（1998—），男，安徽芜湖人，硕士研究生，主要研究方向为镍钴资源提取和矿产资源高效利用。E-mail：

通讯作者:

饶明军（1984—），男，江西广丰人，博士，教授，主要研究方向为复杂铁矿、二次资源清洁高效利用。E-mail：
Enrichment of Nickel and Cobalt by Solid-State Reduction of Limonite-Type Nickel Laterite Ore Enhanced by NaFeS2
Rendong XIAO , Jing CHEN, Meishi HU, Bin XU, Jun LUO, Xin ZHANG, Mingjun RAO
Affiliations
  • School of Minerals Processing & Bioengineering, Central South University, Changsha 410083, Hunan, China
出版时间: 2024-02-01 doi: 10.3969/j.issn.0253-6099.2024.01.022
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摘要
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以NaFeS2为添加剂，研究了NaFeS2用量对红土镍矿固态还原-磁选富集镍、钴及红土镍矿还原行为的影响。结果表明，随着NaFeS2添加量增加，还原过程红土镍矿的软熔特性温度相应降低，还原所得Ni-Co-Fe合金颗粒随之增大；添加10%NaFeS2时，镍、钴的富集和回收效果好，红土镍矿经压团于1 100 ℃还原60 min，再经磨矿-磁选可获得Ni、Co、Fe品位分别为7.89%、0.66%、74.01%，Ni、Co、Fe回收率分别为97.13%、86.78%、35.81%的优质镍钴铁粉产品。

红土镍矿  /  添加剂  /  还原焙烧  /  NaFeS2  /  镍钴铁粉  /  固态还原  /  磁选  /  镍  /  钴

The effects of the amount of NaFeS2, which was used as an additive, on solid-state reduction and magnetic separation for enrichment of nickel and cobalt, and also the reduction behavior of nickel laterite ore were studied. The results show that with the increase of NaFeS2 addition, the softening and melting temperature of nickel laterite ore decreases correspondingly during the reduction process; while particles of the Ni-Co-Fe alloy obtained by reduction increase accordingly. The enrichment and recovery effects of nickel and cobalt will be better by adding 10% NaFeS2. The nickel laterite ore, after being pressed into briquettes, was subjected to reduction at 1 100 ℃ for 60 min, followed by a process of grinding and magnetic separation, resulting in a high quality nickel-cobalt-iron powder grading 7.89% Ni, 0.66% Co and 74.01% Fe, at corresponding recoveries of 97.13%, 86.78% and 35.81%.

nickel laterite ore  /  additive  /  reduction roasting  /  NaFeS2  /  Ni-Co-Fe powder  /  solid state reduction  /  magnetic separation  /  Ni  /  Co
肖仁栋, 陈靖, 胡美世, 许斌, 罗骏, 张鑫, 饶明军. NaFeS2强化褐铁矿型红土镍矿固态还原富集镍钴的研究. 矿冶工程杂志, 2024 , 44 (1) : 100 -104 . DOI: 10.3969/j.issn.0253-6099.2024.01.022
Rendong XIAO, Jing CHEN, Meishi HU, Bin XU, Jun LUO, Xin ZHANG, Mingjun RAO. Enrichment of Nickel and Cobalt by Solid-State Reduction of Limonite-Type Nickel Laterite Ore Enhanced by NaFeS2[J]. Mining and Metallurgical Engineering, 2024 , 44 (1) : 100 -104 . DOI: 10.3969/j.issn.0253-6099.2024.01.022
正文
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镍和钴是新能源产业不可或缺的战略金属，动力电池用镍占比预计从2020年的7%增至2040年的31%，与此同时钴需求年均增长率也将高于13%[1-2]。当前以高压酸浸法为代表的湿法工艺可实现红土镍矿中镍、钴的提取，生产电池级镍钴硫酸盐，但存在酸浸渣排放量大（约120 t渣/t镍）、污染隐患严重、生产控制困难等突出问题[3-4]。
红土镍矿经固态还原-磁选获得的镍钴铁粉是制备镍钴硫酸盐的优质原料，能有效满足动力电池产业的镍钴需求[5-6]。磁选可使大部分脉石和铁氧化物进入尾矿，实现酸浸渣的源头减量；同时镍钴铁粉颗粒小、活性高，常压酸浸即可使镍、钴高效溶出，避免了高压酸浸工艺存在的设备腐蚀、安全隐患等问题，应用前景广阔[7-8]。
已有研究发现，含钠、硫组分的添加剂能强化固态还原的富集效果[9-10]。同时，高硫铝土矿生产氧化铝、铅酸电池碱熔回收铅及其他有色金属冶炼过程产生的多硫铁钠脱硫渣，因碱性大、含硫量高而难以处理，但该特性也使其能用作固态还原添加剂[11-12]。为研究该类废渣作为还原添加剂的可行性，本文通过合成该类渣的主要成分NaFeS2，研究了NaFeS2用量对镍钴铁粉产品的影响，并对NaFeS2强化红土镍矿固态还原的机制进行了探讨，旨在制备高品质镍钴铁粉，为后续工艺改进提供理论支撑。
1　实验
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1.1　实验原料
NaFeS2合成所用九水合硝酸铁、九水合硫化钠、氢氧化钠、无水乙醇和二硫化碳均为分析纯，试验所用氮气纯度为99.99%。还原焙烧所用无烟煤试验前破碎至-74 μm，其固定碳、挥发分、灰分含量分别为83.8%、4.9%、10.2%。
红土镍矿来自印度尼西亚，其主要化学成分见表1。该矿物属于褐铁矿型红土镍矿，使用前磨细至-74 μm粒级占90%。该红土镍矿中铁、镍化学物相分析结果分别见表2～3。铁主要以针铁矿形式存在，占比达99.06%；镍主要赋存于铁氧化物中，分布率达95.62%。
1.2　实验方法
将氢氧化钠溶液倒入硝酸铁溶液中并搅拌均匀，再倒入硫化钠溶液并搅匀，待黑色固体沉淀后，过滤并用无水乙醇和二硫化碳洗涤即可获得NaFeS2。最后将NaFeS2置于卧式管炉中，在氮气气氛下于180 ℃烘干即可[13]。
向红土镍矿中加入4%（质量分数）无烟煤和不同用量NaFeS2，混匀，压制成团块，经真空烘干2 h后，取干燥团块置于带盖石墨坩埚中，于1 100 ℃马弗炉内焙烧60 min。还原试验结束后，将石墨坩埚埋入煤粉中冷却。取部分焙烧矿于矿浆浓度50%条件下湿磨至-43 μm粒级占90%，并使用湿式磁选管（XCGS-73型）于磁场强度80 kA/m条件下对矿浆进行磁选分离。
通过化学分析法测定各样品Fe、Ni和Co含量；采用X射线衍射仪（德国普鲁克Advance D8型）测定还原产物物相组成；采用比饱和磁化强度测量仪（美国LakeShore 7404型）分析还原产物的磁滞回线；采用扫描电镜（捷克TESCAN MIRA3 LMH/LMU型）分析还原产物中各主要元素的分布状态和合金颗粒大小；采用YX-HRD3000型矿物熔点炉测定配加不同用量NaFeS2红土镍矿的还原软熔特性温度。
2　实验结果与讨论
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2.1　NaFeS2的表征
合成NaFeS2产品的X射线衍射分析结果如图1所示。该产品物相组成单一，特征峰与NaFeS2标准峰位一致，说明合成产品纯度高。
2.2　还原焙烧-磁选分离试验
图2为NaFeS2用量对红土镍矿还原焙烧-磁选效果的影响。不添加NaFeS2时，磁选产品镍和钴品位分别为2.52%和0.23%，富集效果差。添加10%NaFeS2后，镍和钴品位分别增至7.89%和0.66%，对应回收率分别为97.13%和86.78%。磁选精矿铁品位随着NaFeS2用量增加呈现上升趋势，NaFeS2用量10%时，铁品位74.01%、回收率35.81%。
NaFeS2用量增加时，铁金属化率下降，表明NaFeS2能抑制铁的金属化，减少Ni-Co-Fe合金中铁的含量。现有研究证明，添加硫化物可使红土镍矿在还原过程中生成低熔点硫化物液相，促进合金颗粒的聚集与生长[14]。过高的NaFeS2用量使较多的脉石矿物和FeS黏附于合金颗粒，影响磨矿和磁选分离效果，导致磁选精矿镍、钴品位下降。
2.3　物相转变规律
采用X射线衍射分析了不同用量NaFeS2还原产物的物相组成，结果如图3所示。
由图3可知，添加NaFeS2后，开始出现FeS，其峰强度随NaFeS2用量升高而增加，Ni-Co-Fe合金的峰强度相应降低，表明添加NaFeS2能抑制金属铁的生成量。由于还原煤用量较少，大部分铁氧化物仅被还原至FeO阶段，只有少量被还原至金属态。不添加NaFeS2时，蛇纹石在焙烧时通过反应（1）形成镁铁橄榄石（（Mg，Fe）2SiO4）；添加NaFeS2后，仍会生成镁铁橄榄石，但原矿中部分硅酸盐在焙烧时转变为霞石（（Na，Al，Si）O4）（反应（2）～（5）），其峰强度随NaFeS2用量增加而升高。原矿所含Cr、Al在还原焙烧后主要以尖晶石形式存在，伴有Mg、Fe元素的固溶。
不同用量NaFeS2还原产物的磁滞回线见图4。还原产物的饱和磁化强度随NaFeS2用量增加逐渐降低，与图2中铁金属化率的变化规律一致。这说明NaFeS2用量提高，金属铁硫化程度加深，铁金属化率下降。
2.4　还原团块元素分布状态
图5为添加10%NaFeS2还原产物的元素分布状态。金属颗粒较少，FeO大量存在，Ni、Co存在于金属铁中；FeS分布广泛，晶粒细长，环绕Ni-Co-Fe合金和FeO，说明FeS在焙烧过程中主要以液相形式存在。因液相的传质速率远高于固相，FeS的广泛分布能促进金属颗粒的聚集与生长。同时，低熔点液相还能堵塞孔隙，抑制还原气体的扩散，抑制金属铁的生成[15]。外层硅酸盐矿物主要为霞石，且与镁铁橄榄石紧密接触，外层硅酸盐因与NaFeS2反应而在焙烧过程转变为霞石，未与NaFeS2反应的内层硅酸盐则转化为镁铁橄榄石。
不同用量NaFeS2还原产物的显微结构见图6。由图6可知，不添加NaFeS2时，合金颗粒微小，矿石内部结构致密，矿石间存在缝隙，说明还原过程无明显液相生成，导致合金颗粒难以聚集长大。添加10%NaFeS2时，Ni-Co-Fe合金颗粒增至30 μm，Ni-Co-Fe合金和FeO颗粒的外形圆润，与脉石矿物的区分界限明显，无独立矿石存在，但有大面积孔洞产生，说明添加NaFeS2加强了还原过程中红土镍矿的流动性，促进了合金颗粒的聚集生长。添加20%NaFeS2时，Ni-Co-Fe合金和FeS颗粒进一步增大，致密的镁铁橄榄石有所减少，霞石物相显著增多，说明NaFeS2用量上升，促进了霞石的生成，进一步提高了还原过程中红土镍矿的流动性。
2.5　还原软熔特性
图7为不同NaFeS2用量条件下红土镍矿还原过程中软熔特性温度的变化情况。从图7可知，随着NaFeS2用量提高，红土镍矿还原过程中软熔特性温度（变形温度、软化温度和流动温度）下降。不添加NaFeS2时，还原过程红土镍矿变形温度为1 210 ℃，远高于试验温度，不利于Ni-Co-Fe合金颗粒的聚集长大；添加10% NaFeS2时，变形温度降至1 112 ℃；添加20% NaFeS2时，变形温度降至960 ℃，软化温度与流动温度也相应地有所下降。添加NaFeS2能有效降低红土镍矿的软熔特性温度[16]。
3　结语
收起
1）针对Ni、Co、Fe含量分别为1.31%、0.14%、42.53%的褐铁矿型红土镍矿，添加10%NaFeS2和4%无烟煤于1 100 ℃焙烧60 min，再经磨矿-磁选分离，能获得Ni、Co、Fe品位分别为7.89%、0.66%、74.01%，对应回收率分别为97.13%、86.78%、35.81%的镍钴铁粉产品。
2）添加NaFeS2后还原过程生成低熔点铁硫化物和霞石，抑制了镁铁橄榄石的形成和铁的金属化，降低了红土镍矿的软熔特性温度，促进了Ni-Co-Fe合金颗粒的聚集生长。
3）通过选择性固态还原-磁选分离可将红土镍矿中大部分脉石矿物和铁氧化物选入尾矿，获得高镍高钴含量的镍钴铁粉。进一步通过常压硫酸浸出、除杂净化可生产电池级硫酸镍、硫酸钴。
基金
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  • 国家自然科学基金(52174288; 51804346)
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2024年第44卷第1期
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doi: 10.3969/j.issn.0253-6099.2024.01.022
  • 接收时间：2023-08-14
  • 首发时间：2026-03-20
  • 出版时间：2024-02-01
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  • 收稿日期：2023-08-14
基金
国家自然科学基金(52174288; 51804346)
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    中南大学　资源加工与生物工程学院，湖南　长沙　410083

通讯作者:

饶明军（1984—），男，江西广丰人，博士，教授，主要研究方向为复杂铁矿、二次资源清洁高效利用。E-mail：
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2种不同金属材料的力学参数
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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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