工程科学学报，第41卷，第4期：447-453,2019年4月 Chinese Journal of Engineering,Vol.41,No.4:447-453,April 2019 DOI:10.13374/j.issn2095-9389.2019.04.004:http://journals.ustb.edu.cn 铷云母矿资源的综合利用 邢鹏，王成彦⑧，马保中，陈永强 北京科技大学治金与生态工程学院，北京100083 ☒通信作者，Emai:chywang(@yeah.net 摘要针对目前铷矿提取工艺污染严重、资源综合利用率低的现状，本文提出采用酸浸一溶剂萃取工艺提取物云母矿中的 物.研究了浸出温度、硫酸浓度及浸出时间对铷浸出率的影响，并借助X射线衍射、扫描电镜、能谱分析等手段，研究了浸出过 程中蜘云母矿的物相转变.实验结果表明，铷云母矿酸浸的最佳条件为浸出温度250℃、H,S0,质量浓度200gL'、浸出时间 1.5,在此条件下铷浸出率达85.2%.X射线衍射图谐表明铷云母矿的主要矿物组成为石英、黑云母、白云母、正长石及钠长 石，扫描电镜一能谱分析结果表明矿石中的铷主要以类质同象取代钾的位置分别存在于黑云母及白云母中.浸出过程中发生 的主要反应为载物云母的溶解.在萃取剂浓度1ol·L1、有机相与水相的体积比0/A=3:1、萃取级数为3级条件下进行逆流 萃取实验，萃余液中的铷质量浓度为0.003gL,铷的萃取率达98%.在HCl浓度1molL、相比0/A=4:1、反萃级数为2 级条件下反萃负载铷的有机相，蜘反萃率达99%.以浸出渣为原料，采用碱熔一中和沉淀工艺制备出了白炭黑产品，实现了资 源的综合利用.采用X射线衍射、红外光谱分析技术对白炭黑进行了表征，结果表明产品成分为水合二氧化硅，符合非晶态白 炭黑的特征.化学定量分析结果表明白炭黑产品含S0,质量分数91.65%，所制备的白炭黑满足国家化工行业标准. 关键词铷云母矿：酸浸：溶剂萃取：铷：白炭黑 分类号TF826.4 Comprehensive utilization of rubidium mica ore XING Peng,WANG Cheng-yan,MA Bao-zhong,CHEN Yong-giang School of Metallurgical and Ecological Engineering,University of Science and Technology Beijing,Beijing 100083,China Corresponding author,E-mail:chywang@yeah.net ABSTRACT In light of the serious environmental pollution caused by the conventional roasting processes and the corresponding low comprehensive utilization of rubidium resources,a novel acid leaching and solvent extraction process was developed to extract rubidium from rubidium mica ore.The effects of leaching temperature,sulfuric acid concentration,and time on the leaching of rubidium were in- vestigated,and the phase transformations during the leaching were analyzed through X-ray diffraction (XRD),scanning electron micro- scope (SEM),and energy dispersive spectrometry (EDS).The experimental results show that the optimum conditions of acid leaching for rubidium mica ore are as follows:leaching temperature of 250C,HSO concentration of 200gL,and leaching time of 1h.Un- der these conditions,the leaching ratio of rubidium increases up to 85.2%.The XRD patterns of the raw ore indicate that quartz,bio- tite,muscovite,orthoclase,and albite are the major phases.Further SEM-EDS analysis shows that the Rb is scatted in biotite and muscovite in the form of isomorphism.Furthermore,the main reaction in the leaching process was the dissolution of the rubidium-rich micas.The countercurrent extraction experiment was conducted under the following conditions:extractant concentration of 1 mol.L-1, phase ratio (O/A)of 3:1,and extraction stage 3.The concentration of rubidium in the raffinate was 0.003gL,and the extraction ratio of rubidium was 98%.After performing the 2-stage countercurrent stripping with I mol'L-HCI at a phase ratio (O/A)of 4:1, 收稿日期：20180104 基金项目：国家自然科学基金资助项目(U1802253,51674026):国家重点研发计划资助项目(2018Y℃1900304)：北京市自然科学基金资助项 目(2182040)：中央高校基本科研业务费专项资金资助项目(230201606500018)工程科学学报，第 41 卷，第 4 期: 447--453，2019 年 4 月 Chinese Journal of Engineering，Vol． 41，No． 4: 447--453，April 2019 DOI: 10． 13374 /j． issn2095--9389． 2019． 04． 004; http: / /journals． ustb． edu． cn 铷云母矿资源的综合利用 邢 鹏，王成彦，马保中，陈永强 北京科技大学冶金与生态工程学院，北京 100083 通信作者，E-mail: chywang@ yeah． net 摘 要 针对目前铷矿提取工艺污染严重、资源综合利用率低的现状，本文提出采用酸浸—溶剂萃取工艺提取铷云母矿中的 铷． 研究了浸出温度、硫酸浓度及浸出时间对铷浸出率的影响，并借助 X 射线衍射、扫描电镜、能谱分析等手段，研究了浸出过 程中铷云母矿的物相转变． 实验结果表明，铷云母矿酸浸的最佳条件为浸出温度 250 ℃、H2 SO4质量浓度 200 g·L － 1、浸出时间 1. 5 h，在此条件下铷浸出率达 85. 2% ． X 射线衍射图谱表明铷云母矿的主要矿物组成为石英、黑云母、白云母、正长石及钠长 石． 扫描电镜--能谱分析结果表明矿石中的铷主要以类质同象取代钾的位置分别存在于黑云母及白云母中． 浸出过程中发生 的主要反应为载铷云母的溶解． 在萃取剂浓度 1 mol·L － 1、有机相与水相的体积比 O/A = 3∶ 1、萃取级数为 3 级条件下进行逆流 萃取实验，萃余液中的铷质量浓度为 0. 003 g·L － 1，铷的萃取率达 98% ． 在 HCl 浓度 1 mol·L － 1、相比 O/A = 4∶ 1、反萃级数为 2 级条件下反萃负载铷的有机相，铷反萃率达 99% ． 以浸出渣为原料，采用碱熔—中和沉淀工艺制备出了白炭黑产品，实现了资 源的综合利用． 采用 X 射线衍射、红外光谱分析技术对白炭黑进行了表征，结果表明产品成分为水合二氧化硅，符合非晶态白 炭黑的特征． 化学定量分析结果表明白炭黑产品含 SiO2质量分数 91. 65% ，所制备的白炭黑满足国家化工行业标准． 关键词 铷云母矿; 酸浸; 溶剂萃取; 铷; 白炭黑 分类号 TF826. 4 收稿日期: 2018--01--04 基金项目: 国家自然科学基金资助项目( U1802253，51674026) ; 国家重点研发计划资助项目( 2018YFC1900304) ; 北京市自然科学基金资助项 目( 2182040) ; 中央高校基本科研业务费专项资金资助项目( 230201606500018) Comprehensive utilization of rubidium mica ore XING Peng，WANG Cheng-yan ，MA Bao-zhong，CHEN Yong-qiang School of Metallurgical and Ecological Engineering，University of Science and Technology Beijing，Beijing 100083，China Corresponding author，E-mail: chywang@ yeah． net ABSTＲACT In light of the serious environmental pollution caused by the conventional roasting processes and the corresponding low comprehensive utilization of rubidium resources，a novel acid leaching and solvent extraction process was developed to extract rubidium from rubidium mica ore． The effects of leaching temperature，sulfuric acid concentration，and time on the leaching of rubidium were in￾vestigated，and the phase transformations during the leaching were analyzed through X-ray diffraction ( XＲD) ，scanning electron micro￾scope ( SEM) ，and energy dispersive spectrometry ( EDS) ． The experimental results show that the optimum conditions of acid leaching for rubidium mica ore are as follows: leaching temperature of 250 ℃，H2 SO4 concentration of 200 g·L － 1，and leaching time of 1 h． Un￾der these conditions，the leaching ratio of rubidium increases up to 85. 2% ． The XＲD patterns of the raw ore indicate that quartz，bio￾tite，muscovite，orthoclase，and albite are the major phases． Further SEM--EDS analysis shows that the Ｒb is scatted in biotite and muscovite in the form of isomorphism． Furthermore，the main reaction in the leaching process was the dissolution of the rubidium-rich micas． The countercurrent extraction experiment was conducted under the following conditions: extractant concentration of 1 mol·L － 1， phase ratio ( O/A) of 3∶ 1，and extraction stage 3． The concentration of rubidium in the raffinate was 0. 003 g·L － 1，and the extraction ratio of rubidium was 98% ． After performing the 2-stage countercurrent stripping with 1 mol·L － 1 HCl at a phase ratio ( O/A) of 4∶ 1