无机盐工业
主管:中海油天津化工研究设计院有限公司
主办:中海油天津化工研究设计院有限公司
   中海油炼油化工科学研究院(北京)有限公司
   中国化工学会无机酸碱盐专业委员会
ISSN 1006-4990 CN 12-1069/TQ

无机盐工业 ›› 2021, Vol. 53 ›› Issue (8): 60-65.doi: 10.19964/j.issn.1006-4990.2020-0527

• 研究与开发 • 上一篇    下一篇

田口实验设计法优化碳酸锂反应结晶制备工艺

王斌1,2,3,4(),邓小川1,2(),史一飞1,2,董超超1,2,3,樊发英1,2,朱朝梁1,2,樊洁1,2,马婉霞1,2,左方涛1,2   

  1. 1.中国科学院青海盐湖研究所,中国科学院盐湖资源综合高效利用重点实验室,青海西宁 810008
    2.青海省盐湖资源综合利用工程技术中心
    3.中国科学院大学
    4.国家能源集团科学技术研究院有限公司银川分公司
  • 收稿日期:2020-09-25 出版日期:2021-08-10 发布日期:2021-08-11
  • 作者简介:王斌(1994— ),男,硕士研究生,主要研究方向为无机化工材料制备及工艺研究;E-mail: wangbin181@mails.ucas.ac.cn

Optimizing preparation process of lithium carbonate reaction crystallization by Taguchi experimental design method

Wang Bin1,2,3,4(),Deng Xiaochuan1,2(),Shi Yifei1,2,Dong Chaochao1,2,3,Fan Faying1,2,Zhu Chaoliang1,2,Fan Jie1,2,Ma Wanxia1,2,Zuo Fangtao1,2   

  1. 1. Key Laboratory of Comprehensive and Highly Efficient Utilization of Salt Lake Resources,Qinghai Institute of Salt Lakes,Chinese Academy of Sciences,Xining 810008,China
    2. Qiughai Engineering and Technology Research Center of Comprehensive Utilization of Salt Lake Resources
    3. University of Chinese Academy of Sciences
    4. Yinchuan Branch of State Power Science & Research Institute Co.,Ltd.
  • Received:2020-09-25 Published:2021-08-10 Online:2021-08-11

摘要:

单因素实验无法全面、可靠地研究各因素对反应结晶过程制备高品质碳酸锂的影响,田口设计有利于全面研究各因素对制备高品质碳酸锂的影响,实验周期较短,实验成本较低。以东台吉乃尔盐湖精制卤水为原料,设计田口实验,采用聚焦光束反射测量仪FBRM G400实时在线研究反应温度、搅拌速率、卤水加料速度、碳酸钠浓度等因素对反应结晶工艺中碳酸锂粒径和纯度的影响。通过田口实验表明搅拌速率对碳酸锂的粒径影响最大,碳酸锂的纯度对反应温度最敏感。研究结果表明,反应温度为85 ℃、搅拌速率为200 r/min、卤水加料速度为2 mL/min、碳酸钠质量浓度为201.6 g/L时得到的碳酸锂品质最优,其粒度为3.71 μm,纯度高达99.62%。

关键词: 碳酸锂, 反应结晶, 田口实验设计法, 粒径, 纯度

Abstract:

Single-factor experiment cannot comprehensively and reliably study the influence of various factors on the pre-paration of high-quality lithium carbonate during the reaction crystallization process.Taguchi′s design is conducive to the comprehensive study of various factors to prepare high-quality lithium carbonate.The experiment cycle is shorter and the experiment cost is lower.Using the refined brine of Dongtai Jinel Salt Lake as the raw material,Taguchi experiment was designed,and the focused beam reflection measuring instrument FBRM G400 was used to study effect of the reaction temperature,stirring rate,brine feed rate,Na2CO3 concentration and other factors on the reaction crystallization process in real-time on-line study of the lithium carbonate particle size and purity.Taguchi experiments showed that the stirring rate had the greatest influence on the particle size of lithium carbonate,and the purity of lithium carbonate was most sensitive to the reaction temperature.The results of the study showed that when the reaction temperature was 85 ℃,the stirring rate was 200 r/min,the brine feed rate was 2 mL/min,and the mass concentration of Na2CO3 was 201.6 g/L,the quality of obtained lithium carbonate was the best with particle size of 3.71 μm and purity of 99.62%.

Key words: Li2CO3, reaction crystallization, Taguchi experimental design method, particle size, purity

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