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过程工程学报 ›› 2022, Vol. 22 ›› Issue (5): 651-659.DOI: 10.12034/j.issn.1009-606X.221137

• 研究论文 • 上一篇    下一篇

改性电炉钛渣矿相解构法制备富钛料新工艺研究

周育生， 邱冠周， 景建发*， 郑富强*， 王帅， 陈凤， 郭宇峰   

  1. 中南大学资源加工与生物工程学院，湖南 长沙 410083
  • 收稿日期:2021-04-26 修回日期:2021-07-16 出版日期:2022-05-28 发布日期:2022-05-27
  • 通讯作者: 景建发 jingjianfa456@163.com
  • 作者简介:周育生(1976-)，男，广东省广州市人，博士研究生，资源与环境专业，E-mail: 2297233035@qq.com；通讯联系人，景建发，E-mail: jingjianfa456@163.com；郑富强，E-mail: f.q.zheng@csu.edu.cn

A novel process for preparation Ti-rich material from modified electric furnace titanium slag by phase deconstruction method

Yusheng ZHOU,  Guanzhou QIU,  Jianfa JING*,  Fuqiang ZHENG*,  Shuai WANG,  Feng CHEN,  Yufeng GUO   

  1. School of Minerals Processing and Bioengineering, Central South University, Changsha, Hunan 410083, China
  • Received:2021-04-26 Revised:2021-07-16 Online:2022-05-28 Published:2022-05-27
  • Contact: jianfa Jing jingjianfa456@163.com

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摘要： 以氧化后的钛精矿电炉冶炼渣为研究对象，采用一段氟化氢铵浸出-二段盐酸浸出的新工艺制备可用于沸腾氯化生产的富钛料原料，从浸出反应热力学和改性钛渣浸出行为两方面进行了系统的研究。氟化氢铵浸出热力学研究表明，氟化氢铵浸出可分解硅酸盐和部分黑钛石，并形成CaMg2Al2F12, CaF2和AlF3沉淀，浸出后杂质元素硅主要以(NH4)2SiF6的形式进入到浸出液中。氟化氢铵浸出实验表明，在氟化氢铵浓度为15wt%、液固比为10:1、温度20℃、浸出时间2 h的条件下，Si, Al, Ti, Fe, Ca和Mg元素的浸出率分别为93.55wt%, 28.03wt%, 3.88wt%, 20.50wt%, 3.40wt%和2.45wt%。浸出渣中主要的物相为金红石、黑钛石和钙镁氟化盐。氟化浸出残渣的盐酸浸出热力学表明，CaMg2Al2F12, CaF2, AlF3沉淀和剩余的黑钛石可溶解于盐酸溶液中。盐酸浸出实验表明，在盐酸浓度为20wt%、液固比为8:1、温度120℃、浸出时间2 h的条件下，Ca, Al, Mg, Ti, Si和Fe的浸出率分别为86.78wt%, 62.33wt%, 92.31wt%, 18.08wt%, 40.23wt%和75.36wt%。盐酸浸出后浸出渣主要物相为金红石，TiO2品位95.20wt%、CaO含量为0.49wt%、MgO含量为0.48wt%，满足沸腾氯化法对原料成分的要求。

关键词: 富钛料, 氟化氢铵浸出, 盐酸浸出, 改性钛渣, 黑钛石

Abstract: In this study, a novel process for preparation rich-titanium material from modified titanium slag after melting in electric furnace by ammonium hydrogen fluoride leaching and hydrochloric acid leaching was proposed. The thermodynamic analysis of ammonium hydrogen fluoride leaching and hydrochloric acid leaching were investigated. The thermodynamic results of ammonium hydrogen fluoride leaching indicated that a small part of anosovite and the silicate can be decomposed, the silicate react with ammonium hydrogen fluoride leaching to produce sediment (CaMg2Al2F12), CaF2 and AlF3. The element of Si was converted to (NH4)2SiF6 existed in solution. The effects of ammonium hydrogen fluoride leaching conditions on the impurities extraction rate were investigated. The results indicated that the extraction rate of Si, Al, Ti, Fe, Ca and Mg were 93.55wt%, 28.03wt%, 3.88wt%, 20.50wt%, 3.40wt% and 2.45wt% respectively when the concentration of ammonium hydrogen fluoride was 15wt%, the liquid-solid ratio was 10:1, the temperature was 20℃ and the time was 2 h. The XRD results showed that the main phases in residue were rutile, anosovite and sediment (CaMg2Al2F12), the diopside was decomposed by ammonium hydrogen fluoride leaching. The thermodynamic results of hydrochloric acid leaching indicated that the sediment (CaMg2Al2F12), CaF2, AlF3 and the residual anovosite was decomposed by hydrochloric acid leaching. The effects of hydrochloric acid leaching conditions on the impurities extraction rate were investigated. The results of hydrochloric acid leaching indicated that the extraction rate of Ca, Al, Mg, Ti, Si and Fe were 86.78wt%, 62.33wt%, 92.31wt%, 18.08wt%, 40.23wt% and 75.36wt% respectively when the concentration of hydrochloric acid was 20wt%, the liquid-solid ratio was 8:1, the temperature was 120℃ and the time was 2 h. The main phase after hydrochloric acid leaching was rutile. The XRD results indicated that the sediment (CaMg2Al2F12) phase was solute by hydrochloric acid leaching. The titanium dioxide grade in rich-titanium material was 95.20wt%, the content of CaO was 0.49wt%, and the content of MgO was 0.48wt% which meet the need of boiling chlorination charge.

Key words: Ti-rich material, Ammonium bifluoride leaching, Hydrochloric acid leaching, Modified titanium slag, Anosovite.