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Article(id=1241768044716953926, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241768035548205179, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.01.026, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1694793600000, receivedDateStr=2023-09-16, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773990172793, onlineDateStr=2026-03-20, pubDate=1706716800000, pubDateStr=2024-02-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773990172793, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773990172793, creator=13701087609, updateTime=1773990172793, 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=121, endPage=124, ext={EN=ArticleExt(id=1241768045870387569, articleId=1241768044716953926, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Experimental Study on Acid Leaching of Polymetallic Sulphide Ore, columnId=1236276106727321817, journalTitle=Mining and Metallurgical Engineering, columnName=METALLURGY, runingTitle=null, highlight=null, articleAbstract=

An experiment of acid leaching was performed for the concentrate obtained by flotation pretreatment of a refractory sulphide ore. After leaching at 95 ℃ for 2 h, with nitric acid concentration at 9 mol/L, and liquid-solid ratio of 4∶1, the leaching rates of copper and zinc reach 90.46% and 85.34%, respectively, showing no lead leached out. The leaching process is mainly controlled by both solid film and chemical reaction.

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对某难选多金属硫化矿浮选预处理所得精矿进行了酸浸试验研究。在浸出温度95 ℃、硝酸浓度9 mol/L、液固比4∶1及浸出时间2 h条件下进行酸浸试验，铜和锌浸出率分别达到了90.46%、85.34%，铅几乎没有浸出。浸出过程主要受固膜控制和化学反应混合控制。

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郑凯露（1999—），男，山西晋城人，硕士研究生，主要研究方向为矿物分选理论与工艺。E-mail：
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张晋霞（1979—），女，山西晋城人，博士，教授，硕士研究生导师，主要研究方向为复杂难选矿高效分选。E-mail：

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张晋霞（1979—），女，山西晋城人，博士，教授，硕士研究生导师，主要研究方向为复杂难选矿高效分选。E-mail：

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张晋霞（1979—），女，山西晋城人，博士，教授，硕士研究生导师，主要研究方向为复杂难选矿高效分选。E-mail：

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CuPbZnFeSMn
3.5210.2418.9710.3434.280.09
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铜铅锌混合精矿主要化学成分（质量分数）

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某多金属硫化矿酸浸试验研究
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张晋霞 1, 2 , 郑凯露 1 , 牛福生 1, 2
矿冶工程杂志 | 冶金 2024,44(1): 121-124
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矿冶工程杂志 | 冶金 2024, 44(1): 121-124
某多金属硫化矿酸浸试验研究
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张晋霞1, 2 , 郑凯露1 , 牛福生1, 2
作者信息
  • 1.华北理工大学　矿业工程学院，河北　唐山　063210
  • 2.河北省矿业开发与安全技术重点实验室，河北　唐山　063210

    • 张晋霞（1979—），女，山西晋城人，博士，教授，硕士研究生导师，主要研究方向为复杂难选矿高效分选。E-mail：

通讯作者:

郑凯露（1999—），男，山西晋城人，硕士研究生，主要研究方向为矿物分选理论与工艺。E-mail：
Experimental Study on Acid Leaching of Polymetallic Sulphide Ore
Jinxia ZHANG1, 2 , Kailu ZHENG1 , Fusheng NIU1, 2
Affiliations
  • 1.School of Mining Engineering, North China University of Science and Technology, Tangshan 063210, Hebei, China
  • 2.Hebei Key Laboratory of Mining Development and Safety Technology, Tangshan 063210, Hebei, China
出版时间: 2024-02-01 doi: 10.3969/j.issn.0253-6099.2024.01.026
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摘要
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对某难选多金属硫化矿浮选预处理所得精矿进行了酸浸试验研究。在浸出温度95 ℃、硝酸浓度9 mol/L、液固比4∶1及浸出时间2 h条件下进行酸浸试验，铜和锌浸出率分别达到了90.46%、85.34%，铅几乎没有浸出。浸出过程主要受固膜控制和化学反应混合控制。

多金属硫化矿  /  酸浸  /  动力学  /  固膜控制  /  铜  /  铅  /  锌

An experiment of acid leaching was performed for the concentrate obtained by flotation pretreatment of a refractory sulphide ore. After leaching at 95 ℃ for 2 h, with nitric acid concentration at 9 mol/L, and liquid-solid ratio of 4∶1, the leaching rates of copper and zinc reach 90.46% and 85.34%, respectively, showing no lead leached out. The leaching process is mainly controlled by both solid film and chemical reaction.

polymetallic sulphide ore  /  acid leaching  /  kinetics  /  solid film control  /  Cu  /  Pb  /  Zn
张晋霞, 郑凯露, 牛福生. 某多金属硫化矿酸浸试验研究. 矿冶工程杂志, 2024 , 44 (1) : 121 -124 . DOI: 10.3969/j.issn.0253-6099.2024.01.026
Jinxia ZHANG, Kailu ZHENG, Fusheng NIU. Experimental Study on Acid Leaching of Polymetallic Sulphide Ore[J]. Mining and Metallurgical Engineering, 2024 , 44 (1) : 121 -124 . DOI: 10.3969/j.issn.0253-6099.2024.01.026
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复杂多金属硫化矿，如黄铜矿、闪锌矿、方铅矿等矿物中含有丰富的铜、铅、锌等金属元素，是重要的矿产资源，但该类矿石性质复杂，金属共存方式紧密繁杂，金属分离困难[1]。对于构成简单的多金属硫化矿，浮选工艺能有效分选有用矿物；但对于一些难选的复杂多金属矿，特别是在磨矿作业中容易被铜离子活化的闪锌矿拥有了与铜矿接近的可浮性[2]，以及矿石中两种或多种矿物互含严重、嵌布关系紧密时，单体解离难度大，难以通过浮选分离有用矿物。
为了高效回收复杂难选硫化矿中的有用元素，可以采用选冶联合方法[3-5]。选冶联合通常将浮选与湿法冶金结合在一起。目前常用的湿法冶金工艺包括酸浸、氨浸、碱浸、高压氧化浸出等[6-8]。黄铜矿具有独特的晶体结构，其表面在浸出过程中形成的保护层阻隔了浸出剂与矿物的相互接触和进一步扩散，常规浸出时需添加高电位的氧化剂进行辅助浸出，使铜以金属离子形式进入液相中[9]。本文以某复杂多金属硫化矿浮选预处理所得精矿为研究对象，采用加温氧化酸浸法实现难选铜铅锌多金属矿的高效分离，并研究了其浸出过程的动力学。
1　试验
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1.1　试验原料与设备
试验原料为江西某铜铅锌多金属矿经浮选预处理得到的铜铅锌混合精矿，其主要化学成分如表1所示。由表1可知，混合精矿主要成分为锌、铅、铁、铜和硫。
对混合精矿进行了X射线衍射分析，结果见图1。由图1可知，混合精矿主要由黄铁矿、方铅矿、闪锌矿和黄铜矿组成，脉石矿物主要为石英。
试验设备为磁力搅拌器等。试验所用药品为分析纯试剂浓硫酸与浓硝酸。
1.2　试验方法
将浮选预处理所得混合精矿进行缩分，每次称取10.0 g矿样置于烧杯中，按不同液固比将浓硫酸倒入烧杯中，随后采用分批添加的方式加入氧化剂硝酸，轻轻摇晃烧杯防止矿样黏着在烧杯底部；将烧杯置于水浴锅中进行磁力转子搅拌，研究液固比、浸出时间、浸出温度以及硝酸浓度对浸出效果的影响。试验结束后，待溶液冷却后取出浸出渣，烘干、化验，并计算铜、铅、锌浸出率。因试验过程中铅基本不被浸出，本文试验数据仅列出铜和锌浸出率。
1.3　试验原理
浸出过程中，铜铅锌混合精矿主要与硫酸和硝酸发生反应：
2　试验结果与分析
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2.1　液固比对铜、锌浸出率的影响
浸出温度70 ℃、浸出时间1.5 h、硝酸浓度6 mol/L，考察了液固比对铜、锌浸出率的影响，结果见图2。由图2可知，液固比由2∶1增至4∶1时，铜、锌浸出率逐渐增加，在液固比4∶1时达到峰值；继续增大液固比至5∶1后，铜、锌浸出率出现下降趋势，表明继续增大液固比不利于铜、锌的浸出。增大液固比会增加硫酸铅的浸出，过多的硫酸铅覆盖至铜和锌表面以及矿物孔隙结构中，会导致铜、锌与浸出液无法进一步反应，铜、锌浸出率下降。综合考虑，选择液固比4∶1，此时铜和锌浸出率分别为75.31%和63.10%。
2.2　浸出时间对铜、锌浸出率的影响
液固比4∶1、浸出温度70 ℃、硝酸浓度6 mol/L，不同浸出时间下铜、锌浸出率见图3。由图3可知，延长浸出时间能够有效提高铜、锌浸出率，浸出时间由0.5 h延长至2 h时，铜、锌浸出率逐渐提高，在2 h时达到峰值；继续延长浸出时间至2.5 h后，铜、锌浸出率出现下降的趋势，这可能是延长浸出时间，部分浸出的硫酸铅覆盖到铜和锌表面，阻碍了浸出液与铜、锌的接触和反应，铜和锌浸出率降低。适宜的浸出时间为2 h，此时铜和锌浸出率分别为77.34%和65.46%。
2.3　浸出温度对铜、锌浸出率的影响
液固比4∶1、浸出时间2 h、硝酸浓度6 mol/L，不同浸出温度下铜、锌浸出率见图4。由图4可知，升高温度，铜和锌浸出率明显增加。升高温度能够推动化学反应快速进行，使矿物颗粒表面活性增加，铜和锌浸出率随之提升。温度超过95 ℃后，继续升高温度对铜和锌浸出率的影响很小。确定浸出温度为95 ℃，此时铜和锌浸出率分别为84.25%和80.24%。
2.4　硝酸浓度对铜、锌浸出率的影响
液固比4∶1、浸出时间2 h、温度95 ℃，不同硝酸浓度下铜和锌浸出率见图5。由图5可知，提高硝酸浓度促进了硫化物的转化，铜和锌浸出率增加。综合考虑，硝酸浓度选择9 mol/L，此时铜和锌浸出率分别为90.89%和85.60%。
2.5　浸出渣XRD分析
通过单因素实验确定了浸出的适宜条件为：浸出温度95 ℃、硝酸浓度9 mol/L、液固比4∶1、浸出时间2 h，此时铜、锌浸出率分别为90.46%、85.34%。该条件下所得浸出渣XRD图谱如图6所示。经2 h浸出后，浸出渣中主要产物为硫酸铅，同时存在微量石英和闪锌矿。该结果与浸出试验结果一致。
2.6　浸出动力学分析
在浸出过程中，原料与浸出液接触后发生复杂的液固反应，通常使用未反应核收缩模型表示反应过程，整个浸出过程可能由固膜扩散控制、表面化学反应控制或两者混合控制：
式中α为浸出率，%；ka为化学反应速率常数，min-1；kb为扩散速率常数，min-1；kc为混合速率常数，min-1；t为反应时间，min。
将不同温度下铜、锌浸出率数据代入式（5）～（7）进行线性拟合，结果分别见图7～9。
由图7～9可知，采用混合收缩核模型拟合铜浸出率，相关系数大于0.96，高度相关，说明铜在浸出过程中主要由固膜扩散和化学反应扩散共同控制；锌的浸出与铜相似，采用混合收缩核模型的相关系数大于0.93，主要由固膜扩散和化学扩散共同控制。根据阿伦尼乌斯方程：
式中k为反应速率常数；A为频率因子；Ea为表观活化能，J/mol；R为摩尔气体常数；T为反应温度，℃。对式（8）两边取对数，得：
作lnk关于1/T的拟合曲线，如图10所示。由拟合曲线斜率可知，浸出过程中铜和锌表观活化能分别为28.28 kJ/mol和22.87 kJ/mol。铜和锌表观活化能在21～42 kJ/mol范围内，根据动力学理论可得，浸出过程受固膜扩散和化学反应混合控制。
3　结论
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1）对浮选预处理所得铜铅锌混合精矿进行酸浸，适宜的浸出条件为：浸出温度95 ℃、硝酸浓度9 mol/L、液固比4∶1、浸出时间2 h，该条件下，铜和锌浸出率分别达到90.46%和85.34%。
2）浸出渣XRD分析结果表明，浸出渣中主要产物为硫酸铅，同时存在微量石英和闪锌矿。
3）浸出动力学研究结果表明，浸出过程中铜和锌表观活化能分别为28.28和22.87 kJ/mol，主要受固膜扩散和化学反应混合控制。
文献
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doi: 10.3969/j.issn.0253-6099.2024.01.026
  • 接收时间：2023-09-16
  • 首发时间：2026-03-20
  • 出版时间：2024-02-01
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  • 收稿日期：2023-09-16
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作者信息
    1.华北理工大学　矿业工程学院，河北　唐山　063210
    2.河北省矿业开发与安全技术重点实验室，河北　唐山　063210

通讯作者:

郑凯露（1999—），男，山西晋城人，硕士研究生，主要研究方向为矿物分选理论与工艺。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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