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    李丽君, 刘程琳, 宋兴福, 于建国. 碱性溶液体系制备磷酸锂结晶过程优化[J]. 华东理工大学学报(自然科学版), 2020, 46(5): 598-607. DOI: 10.14135/j.cnki.1006-3080.20190430003
    引用本文: 李丽君, 刘程琳, 宋兴福, 于建国. 碱性溶液体系制备磷酸锂结晶过程优化[J]. 华东理工大学学报(自然科学版), 2020, 46(5): 598-607. DOI: 10.14135/j.cnki.1006-3080.20190430003
    LI Lijun, LIU Chenglin, SONG Xingfu, YU Jianguo. Optimization of Crystallization Process for Preparation of Lithium Phosphate in Alkaline Solution System[J]. Journal of East China University of Science and Technology, 2020, 46(5): 598-607. DOI: 10.14135/j.cnki.1006-3080.20190430003
    Citation: LI Lijun, LIU Chenglin, SONG Xingfu, YU Jianguo. Optimization of Crystallization Process for Preparation of Lithium Phosphate in Alkaline Solution System[J]. Journal of East China University of Science and Technology, 2020, 46(5): 598-607. DOI: 10.14135/j.cnki.1006-3080.20190430003

    碱性溶液体系制备磷酸锂结晶过程优化

    Optimization of Crystallization Process for Preparation of Lithium Phosphate in Alkaline Solution System

    • 摘要: 鉴于锂辉石中低温碱浸技术浸出液中锂浓度低、杂质离子浓度高、碳酸锂结晶难等问题,测定了磷酸锂在碱性体系中的溶解度;系统研究了磷酸锂反应结晶过程中多工艺参数对磷酸锂收率和粒径的影响;着重考察了K、Si、Al这3种常见杂质元素对磷酸锂粒径和形貌的影响,认为杂质离子的作用机理为离子选择性吸附在晶面和离子嵌入晶格的共同作用。采用中心复合设计(CCD)响应曲面法优化工艺参数,当反应温度为80 ℃,锂离子初始质量浓度为1.60 g/L,磷酸钠用量为130%(即理论化学计量数的1.3倍),加料速率为10 mL/min时,得到晶体产物收率和平均粒径的预测值分别为97.37%和18.57 μm,相应的实验值分别为96.85%和18.70 μm。预测值与实验值接近,误差较小。

       

      Abstract: The medium-temperature or low-temperature alkaline leaching method of spodumene ore is an environmentally friendly laboratory technology being explored. The low concentration of lithium and high concentration of impurity ions in the leaching solution make it impossible to prepare lithium carbonate. Herein, the preparation of low-solubility and high-value lithium phosphate (\rmL\rmi_\rm3\rmP\rmO_\rm4) is proposed. The solubility of \rmL\rmi_\rm3\rmP\rmO_\rm4 in alkaline solution system was determined. The effect of process conditions on the yield and particle size of \rmL\rmi_\rm3\rmP\rmO_\rm4 was investigated, as well as the influences of impurity including K, Si, Al on the purity, morphology and size of \rmL\rmi_\rm3\rmP\rmO_\rm4. The mechanism indicates that the synergy of ion-selective-adsorption on the crystal surface and ion-intercalation in the crystal lattice are responsible for the effects. Central composite design (CCD), a kind of response surface methodology, was employed to explore the effects of reaction temperature, lithium concentration, dosage of sodium phosphate and feeding rate. The optimal conditions were 80 ℃, 1.60 g/L of Li+ concentration, 130% of Na3PO4 dosage and 10 mL/min of feed speed, respectively. Under the conditions, the optimal yield and the average particle size were predicted to be 97.37% and 18.57 μm, respectively, while the corresponding experimental results were 96.85% and 18.70 μm, respectively. The errors between the predicted and experimental values were small.

       

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