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Article(id=1241406725832634923, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241406711219680205, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.06.021, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1718121600000, receivedDateStr=2024-06-12, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773904027660, onlineDateStr=2026-03-19, pubDate=1732982400000, pubDateStr=2024-12-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773904027660, onlineIssueDateStr=2026-03-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773904027660, creator=13701087609, updateTime=1773904027660, updator=13701087609, issue=Issue{id=1241406711219680205, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='6', pageStart='1', pageEnd='174', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773904024176, creator=13701087609, updateTime=1773911273793, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241437118384362345, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241406711219680205, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241437118388556650, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1241406711219680205, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=99, endPage=103, ext={EN=ArticleExt(id=1241406726239482455, articleId=1241406725832634923, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Leaching Test Based on Occurrence State of Fluoride in Barite, columnId=1236276106727321817, journalTitle=Mining and Metallurgical Engineering, columnName=METALLURGY, runingTitle=null, highlight=null, articleAbstract=

Based on the investigation of occurrence state, fluoride associated with barite was leached with HCl-AlCl3 by using Plackett-Burman design, and influences of HCl concentration, AlCl3 concentration, reaction temperature, reaction time, and liquid-to-solid ratio on fluorine leaching rate were investigated. It is found that the fluorine in barite mainly exists in the form of disseminated and banded fluorite. By using HCl at a concentration of 3 mol/L and AlCl3 at a concentration of 0.4 mol/L, after 30 min leaching reaction of ore sample with grain size of 48-75 μm, liquid-to-solid ratio of 10 mL/g, and stirring speed at 300 r/min, the leaching rate of fluorine can reach 93.20%, and the mass fraction of barite is 95.91%. Results show that all factors that influence fluorine leaching rate are arranged in descending order of importance as follows: reaction temperature > HCl concentration > reaction time > AlCl3 concentration > liquidto-solid ratio.

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研究了重晶石伴生氟化物赋存状态，结合Plackett-Burman试验法，采用HCl-AlCl3浸出重晶石伴生氟化物，考察HCl浓度、AlCl3浓度、反应温度、反应时间和液固比对氟浸出率的影响。结果表明：重晶石中氟元素主要以萤石形式存在，呈浸染状和条带状分布；HCl浓度3 mol/L、AlCl3浓度0.4 mol/L、反应温度80 ℃、反应时间30 min、液固比10 mL/g、矿样粒度48～75 μm、搅拌速度300 r/min条件下，氟浸出率可达93.20%，浸出后重晶石质量分数95.91%；各因素影响氟浸出率的显著性排序为：反应温度>HCl浓度>反应时间>AlCl3浓度>液固比。

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李维娟（1966—），女，辽宁锦州人，博士研究生，教授，主要研究方向为高性能金属材料组织与性能调控。E-mail：
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范智禹（1997—），男，辽宁鞍山人，博士研究生，主要研究方向为矿物材料加工及资源综合利用。E-mail：

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范智禹（1997—），男，辽宁鞍山人，博士研究生，主要研究方向为矿物材料加工及资源综合利用。E-mail：

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范智禹（1997—），男，辽宁鞍山人，博士研究生，主要研究方向为矿物材料加工及资源综合利用。E-mail：

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重晶石主要矿物组成及含量（质量分数）

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重晶石萤石石英生石膏铝镁尖晶石
87.997.961.461.390.02
方解石磁铁矿天青石白云石钙长石
1.060.030.030.010.05
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水平因素
X1X2X3X4X5
-120.265208
140.6954012
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Plackett-Burman试验设计因素和水平

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水平因素
X1X2X3X4X5
-120.265208
140.6954012
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试验组X1X2X3X4X5氟浸出率/%
1-1-1-1-1-137.16
2-111-1168.63
3-1-11-1160.05
41-1-1-1154.83
5111-1-180.99
6-1-1-11-157.63
7-11-11161.82
8-1111-173.94
911-1-1-160.12
101-111-189.60
1111-11176.51
121-111190.87
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Plackett-Burman试验方案和结果

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试验组X1X2X3X4X5氟浸出率/%
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2-111-1168.63
3-1-11-1160.05
41-1-1-1154.83
5111-1-180.99
6-1-1-11-157.63
7-11-11161.82
8-1111-173.94
911-1-1-160.12
101-111-189.60
1111-11176.51
121-111190.87
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项目平方和自由度均方F值P值
模型2 606.345521.2757.45<0.000 1**
X1731.481731.4880.62<0.000 1**
X284.64184.649.33<0.022 4*
X31 121.5311 121.53123.61<0.000 1**
X4654.021654.0272.08<0.000 1**
X514.67114.671.62<0.250 5
残差54.4469.07——
总离差2 660.7811———
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项目平方和自由度均方F值P值
模型2 606.345521.2757.45<0.000 1**
X1731.481731.4880.62<0.000 1**
X284.64184.649.33<0.022 4*
X31 121.5311 121.53123.61<0.000 1**
X4654.021654.0272.08<0.000 1**
X514.67114.671.62<0.250 5
残差54.4469.07——
总离差2 660.7811———
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重晶石氟化铝石英生石膏天青石其他
95.910.251.731.950.030.13
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酸浸后重晶石主要矿物含量（质量分数）

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重晶石氟化铝石英生石膏天青石其他
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重晶石伴生氟化物的赋存状态及浸出试验研究
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范智禹 1 , 聂登攀 2 , 李维娟 1 , 王一雍 1 , 李继东 1 , 庞启航 1
矿冶工程杂志 | 冶金 2024,44(6): 99-103
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矿冶工程杂志 | 冶金 2024, 44(6): 99-103
重晶石伴生氟化物的赋存状态及浸出试验研究
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范智禹1 , 聂登攀2, 李维娟1 , 王一雍1, 李继东1, 庞启航1
作者信息
  • 1.辽宁科技大学　材料与冶金学院，辽宁　鞍山　114051
  • 2.贵州民族大学　化学工程学院，贵州　贵阳　550025

    • 范智禹（1997—），男，辽宁鞍山人，博士研究生，主要研究方向为矿物材料加工及资源综合利用。E-mail：

通讯作者:

李维娟（1966—），女，辽宁锦州人，博士研究生，教授，主要研究方向为高性能金属材料组织与性能调控。E-mail：
Leaching Test Based on Occurrence State of Fluoride in Barite
Zhiyu FAN1 , Dengpan NIE2, Weijuan LI1 , Yiyong WANG1, Jidong LI1, Qihang PANG1
Affiliations
  • 1.School of Materials and Metallurgy, University of Science and Technology Liaoning, Anshan 114051, Liaoning, China
  • 2.School of Chemical Engineering, Guizhou Minzu University, Guiyang 550025, Guizhou, China
出版时间: 2024-12-01 doi: 10.3969/j.issn.0253-6099.2024.06.021
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摘要
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研究了重晶石伴生氟化物赋存状态，结合Plackett-Burman试验法，采用HCl-AlCl3浸出重晶石伴生氟化物，考察HCl浓度、AlCl3浓度、反应温度、反应时间和液固比对氟浸出率的影响。结果表明：重晶石中氟元素主要以萤石形式存在，呈浸染状和条带状分布；HCl浓度3 mol/L、AlCl3浓度0.4 mol/L、反应温度80 ℃、反应时间30 min、液固比10 mL/g、矿样粒度48～75 μm、搅拌速度300 r/min条件下，氟浸出率可达93.20%，浸出后重晶石质量分数95.91%；各因素影响氟浸出率的显著性排序为：反应温度>HCl浓度>反应时间>AlCl3浓度>液固比。

重晶石  /  氟化物  /  赋存状态  /  HCl-AlCl3  /  浸出  /  Plackett-Burman试验法  /  氟

Based on the investigation of occurrence state, fluoride associated with barite was leached with HCl-AlCl3 by using Plackett-Burman design, and influences of HCl concentration, AlCl3 concentration, reaction temperature, reaction time, and liquid-to-solid ratio on fluorine leaching rate were investigated. It is found that the fluorine in barite mainly exists in the form of disseminated and banded fluorite. By using HCl at a concentration of 3 mol/L and AlCl3 at a concentration of 0.4 mol/L, after 30 min leaching reaction of ore sample with grain size of 48-75 μm, liquid-to-solid ratio of 10 mL/g, and stirring speed at 300 r/min, the leaching rate of fluorine can reach 93.20%, and the mass fraction of barite is 95.91%. Results show that all factors that influence fluorine leaching rate are arranged in descending order of importance as follows: reaction temperature > HCl concentration > reaction time > AlCl3 concentration > liquidto-solid ratio.

barite  /  fluoride  /  occurrence state  /  HCl-AlCl3  /  leaching  /  Plackett-Burman design  /  flouorine
范智禹, 聂登攀, 李维娟, 王一雍, 李继东, 庞启航. 重晶石伴生氟化物的赋存状态及浸出试验研究. 矿冶工程杂志, 2024 , 44 (6) : 99 -103 . DOI: 10.3969/j.issn.0253-6099.2024.06.021
Zhiyu FAN, Dengpan NIE, Weijuan LI, Yiyong WANG, Jidong LI, Qihang PANG. Leaching Test Based on Occurrence State of Fluoride in Barite[J]. Mining and Metallurgical Engineering, 2024 , 44 (6) : 99 -103 . DOI: 10.3969/j.issn.0253-6099.2024.06.021
正文
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重晶石（BaSO4）是含钡的非金属矿石，具有无毒、密度大、耐酸碱、填充性和防辐射性好等优点，常用作涂染料、加重剂、防射线混凝土以及聚合填充材料等，广泛应用于石油、化工、采矿、建筑等领域[1-4]。天然重晶石常与萤石（CaF2）、方解石（CaCO3）等脉石矿物伴生[5]。重晶石产品BaSO4品位须达到90%以上才能进入市场销售[6]。采用重选[7]、磁选[8]和浮选[9]等选矿方法难以彻底脱除伴生的脉石矿物，为提高重晶石产品质量，浸出提纯是一种高效方法[10]。
重晶石伴生的萤石与盐酸和硫酸反应均会生成有毒的氟化氢气体，与水互溶后形成氢氟酸，对设备腐蚀严重。盐酸-硼酸-硫酸混合可有效浸出CaF2[11]，此方法氟浸出率虽然较高，但同样对设备产生腐蚀，且浸出后的含氟废液难以处理，容易造成环境污染。有研究曾使用络合法浸出混合稀土精矿中的氟化物[12]，添加Al3+能与F-形成络合离子[AlFn]3-n，用于生产冰晶石，但在重晶石提质除氟工艺中未见相关报道。
本文采用HCl-AlCl3浸出重晶石中的氟化物，考察了HCl浓度、AlCl3浓度、反应温度、反应时间和液固比对氟浸出率的影响，并在单因素实验基础上，结合Plackett-Burman试验设计，确定各因素影响氟浸出率的显著性，旨在为重晶石提质降杂工业化放大试验提供指导。
1　试验
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1.1　试验原料
试验所用重晶石矿样取自贵州赛博盟微粉工业有限公司。采用X射线荧光光谱仪（XRF，荷兰PANalytical Axios）分析重晶石矿样化学成分，结果见表1。从表1可看出，重晶石矿样中主要成分为BaO和SO3，所含杂质元素主要有钙、氟、锶和硅，其中氟含量（质量分数）达5.29%。
采用X射线衍射仪（XRD，日本Rigaku Ultima IV）测定了重晶石矿样的XRD图谱，结果见图1。由图1可知，矿样主要物相为重晶石（BaSO4）、萤石（CaF2）、方解石（CaCO3）、石英（SiO2）和石膏（CaSO4）。
采用矿物解离分析仪（MLA，美国FEI MLA 650）分析重晶石矿样的背散射电子图像，结果如图2所示。由图2可观测到重晶石、萤石和生石膏的存在，萤石有富集现象，且CaF2含量较高。矿样的主要矿物组成及含量见表2。由表2可知，重晶石中还伴有铝镁尖晶石、方解石、磁铁矿、天青石、白云石和钙长石，其中重晶石含量（质量分数，下同）87.99%、萤石含量7.96%。
重晶石矿样薄片偏光显微分析结果见图3。由图3可见，重晶石主体呈白色，细小的萤石颗粒呈现浸染状构造，疏散、不均匀分布在重晶石矿体中，且有部分隐晶质存在。而有富集现象的萤石在一个方向延伸，以条带状分布夹杂在重晶石矿体中，呈现暗黄色，纯萤石矿物本身应为无色，结合XRF分析结果可知，其呈现颜色的原因主要是混入了铁、铝等杂质元素。
采用X射线光电子能谱仪（XPS，美国Thermo ESCALAB 250XI）测定重晶石矿中的微量含氟物相，结果如图4所示。图4（a）中存在6个强峰，说明Ba、O、S、Ca和F是重晶石矿样中含量较多的元素，这与XRF分析结果一致。图4（b）中存在683.74、684.86、686.67和687.88 eV共4个特征峰，查询美国国家标准技术研究所XPS数据库进行数据匹配与对照，结合XRF分析，F（1s）分谱图中，结合能683.74 eV附近的相关结构为Ba—F，684.86 eV附近的相关结构为Ca—F与Sr—F，686.67 eV附近的相关结构为Si—F，687.88 eV附近的相关结构为Al—F。可见重晶石矿中还存在Ba—F、Sr—F、Si—F和Al—F结合形态的氟化物。
1.2　浸出试验
以500 mL三口烧瓶为反应器，采用水浴加热和机械搅拌，配置冷凝管，搅拌速度300 r/min。在反应器中加入一定量HCl和AlCl3溶液，加热至设定温度。再投入20 g研磨至48～75 μm的重晶石矿样。反应一段时间后进行液固分离、洗涤，测定浸出液和浸出渣中氟含量，计算氟浸出率：
式中：η为氟浸出率，%；p为浸出液中F-质量浓度，g/mL；V为浸出液体积，mL；m为重晶石质量，g；w为重晶石初始氟含量（质量分数），%。
试验试剂盐酸（HCl）由重庆川东化工（集团）有限公司生产，氯化铝（AlCl3）由上海麦克林生化科技有限公司生产，均为分析纯。试验用水为从实验室去离子纯水机接取的超纯水，其电阻率为18.25 MΩ。
1.3　Plackett-Burman试验设计
基于单因素实验结果，采用Design-Expert 8.0.6.1软件，对HCl浓度（X1，mol/L）、AlCl3浓度（X2，mol/L）、反应温度（X3，℃）、反应时间（X4，min）、液固比（X5，mL/g）5个因素进行氟浸出率的显著性考察，建立Plackett-Burman因素水平表如表3所示，比较各因素与整体差异的显著性。其中每个因素选取单因素实验较好结果的高低两个水平，分别用-1和1表示。
2　试验结果与讨论
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2.1　重晶石伴生氟化物浸出单因素实验
2.1.1　盐酸浓度试验
AlCl3浓度0.2 mol/L、反应温度95 ℃、反应时间40 min、液固比12 mL/g、矿样粒度48～75 μm、搅拌速率300 r/min条件下，考察了HCl浓度对重晶石中氟浸出率的影响，结果如图5所示。结果表明，较高的HCl浓度可加速氟的浸出；HCl浓度从1 mol/L增加到3 mol/L，氟浸出率显著提高，HCl浓度从3 mol/L增加到4 mol/L，氟浸出率只有细微提高。适宜的HCl浓度为3 mol/L。
2.1.2　氯化铝浓度试验
HCl浓度3 mol/L，其他条件不变，考察了AlCl3浓度对重晶石中氟浸出率的影响，结果如图6所示。结果表明，AlCl3浓度从0.2 mol/L增加到0.4 mol/L，氟浸出率明显提高；AlCl3浓度从0.4 mol/L增加到0.6 mol/L，氟浸出率达到平衡；AlCl3浓度继续增加到1.0 mol/L，氟浸出率反而降低。氟化物的分解是HCl和AlCl3共同作用于矿物颗粒表面的结果，Al3+浓度过高会阻碍氟化物与HCl的碰撞概率，导致氟浸出率降低。适宜的AlCl3浓度为0.4 mol/L。
2.1.3　反应温度试验
AlCl3浓度0.4 mol/L，其他条件不变，考察了反应温度对重晶石中氟浸出率的影响，结果如图7所示。结果表明：氟浸出率随着反应温度升高而增大；反应温度65 ℃以下时，氟浸出率较低；反应温度从80 ℃增加到95 ℃，氟浸出率细微增加。温度升高能使能量较低的分子变成活化分子，增加反应物中的活化分子数，同时分子热运动加快，使分子间有效碰撞次数增加，加快反应速率；温度过高会导致盐酸快速挥发，不仅浪费原料，还会造成环境污染。适宜的反应温度为80 ℃。
2.1.4　反应时间试验
反应温度80 ℃，其他条件不变，考察了反应时间对重晶石中氟浸出率的影响，结果如图8所示。结果表明，氟浸出率随着反应时间延长而增大，反应30 min后，氟浸出率没有明显变化。适宜的反应时间为30 min。
2.1.5　液固比试验
反应时间30 min，其他条件不变，考察了液固比对重晶石中氟浸出率的影响，结果如图9所示。结果表明，随着液固比增加，氟浸出率提高，液固比超过10 mL/g后，氟浸出率没有明显变化。液固比较低时，浆料黏度和浸出液离子浓度较大，液固传质速率较低，浸出率较小。适宜的液固比为10 mL/g。
2.2　各因素影响氟浸出率的显著性分析
Plackett-Burman试验结果见表4。根据Plackett-Burman试验结果，采用Design-Expert 8.0.6.1软件自动计算得到重晶石中氟浸出率的回归方程系数以及影响因素的显著性，结果如表5所示。由表5可知，反应温度、HCl浓度和反应时间对氟浸出率的影响极显著，液固比对氟浸出率的影响不显著。根据F值可得到各因素显著性大小排序依次为：反应温度>HCl浓度>反应时间>AlCl3浓度>液固比。
2.3　酸浸后的矿物特征
在HCl浓度3 mol/L、AlCl3浓度0.4 mol/L、反应温度80 ℃、反应时间30 min、液固比10 mL/g、矿样粒度48～75 μm、搅拌速率300 r/min的优化条件下酸浸重晶石，氟浸出率可达93.20%。对优化条件下酸浸后的重晶石矿样进行了XRD分析，结果如图10所示。由图10可看出，浸出后矿样主要物相为BaSO4，未见CaF2和CaCO3晶相峰，但XRD光谱并不平滑，小峰很多，峰强较弱，说明重晶石中还含有多种微量物相。对比浸出前后的重晶石矿样图可知，浸出后矿样白度显著提高。
进一步对浸出后的重晶石矿样进行MLA分析，结果如图11所示。由图11可知，酸浸后矿样中主要矿物组成为重晶石、石英和生石膏，未检测到萤石矿物。酸浸后重晶石矿样主要矿物含量如表6所示。酸浸后重晶石中BaSO4含量（质量分数）为95.91%，较酸浸前有了显著提高，获得了能市场销售的合格产品；酸浸后生成了少量氟化铝和天青石。
3　结论
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1）重晶石矿样中氟元素主要以萤石形式存在，呈浸染状和条带状分布，同时还存在少量以Ba—F、Fe—F、Sr—F、Si—F和Al—F结构形态赋存的氟。重晶石矿样还伴有萤石、石英、生石膏、铝镁尖晶石、方解石、磁铁矿、天青石、白云石和钙长石，其中重晶石质量分数为87.99%，萤石质量分数为7.96%。
2）HCl-AlCl3溶液可有效浸出重晶石中伴生氟化物，提高重晶石产品质量。在HCl浓度3 mol/L、AlCl3浓度0.4 mol/L、反应温度80 ℃、反应时间30 min、液固比10 mL/g、矿样粒度48～75 μm、搅拌速度300 r/min条件下，氟浸出率可达93.20%，浸出后重晶石质量分数95.91%。各因素影响氟浸出率的显著性顺序为：反应温度>HCl浓度>反应时间>AlCl3浓度>液固比。
基金
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  • 辽宁省教育厅重点攻关项目(JYTZD2023091)
  • 贵州省科技计划项目(黔科合支撑[2021]一般484; 黔科合支撑[2020]4Y014; 黔科合基础[2020]1Y406)
  • 贵州省科协专项及调研课题(YZ2023001)
文献
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2024年第44卷第6期
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doi: 10.3969/j.issn.0253-6099.2024.06.021
  • 接收时间：2024-06-12
  • 首发时间：2026-03-19
  • 出版时间：2024-12-01
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  • 收稿日期：2024-06-12
基金
辽宁省教育厅重点攻关项目(JYTZD2023091)
贵州省科技计划项目(黔科合支撑[2021]一般484; 黔科合支撑[2020]4Y014; 黔科合基础[2020]1Y406)
贵州省科协专项及调研课题(YZ2023001)
作者信息
    1.辽宁科技大学　材料与冶金学院，辽宁　鞍山　114051
    2.贵州民族大学　化学工程学院，贵州　贵阳　550025

通讯作者:

李维娟（1966—），女，辽宁锦州人，博士研究生，教授，主要研究方向为高性能金属材料组织与性能调控。E-mail：
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https://castjournals.cast.org.cn/joweb/kygczz/CN/10.3969/j.issn.0253-6099.2024.06.021
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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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