响应曲面法优化碳酸锂反应结晶工艺

doi:10.11949/j.issn.0438-1157.20170461

化工学报 ›› 2017, Vol. 68 ›› Issue (11): 4169-4177.DOI: 10.11949/j.issn.0438-1157.20170461

响应曲面法优化碳酸锂反应结晶工艺

段绍君, 孙玉柱, 宋兴福, 于建国

华东理工大学国家盐湖综合利用工程技术研究中心, 上海 200237

收稿日期:2017-04-24 修回日期:2017-08-11 出版日期:2017-11-05 发布日期:2017-11-05
通讯作者: 宋兴福
基金资助:
国家自然科学基金项目（51574126）；国家重点研发计划项目（2016YFC0401203）；国家科技支撑项目（2015BAB10B01）。

Optimization of reactive-crystallization process of lithium carbonate based on response surface methodology

DUAN Shaojun, SUN Yuzhu, SONG Xingfu, YU Jianguo

National Engineering Research Center for Integrated Utilization of Salt Lake Resources, East China University of Science and Technology, Shanghai 200237, China

Received:2017-04-24 Revised:2017-08-11 Online:2017-11-05 Published:2017-11-05
Supported by:
supported by the National Natural Science Foundation of China (51574126), the National Key R&D Plan(2016YFC0401203) and the National Science-technology Support Plan Projects(2015BAB10B01).

摘要/Abstract

摘要：

碳酸锂是制备各种锂化合物的基础锂盐，碳酸锂的制备是锂产业链当中的承前启后的关键技术。以察尔汗盐湖老卤为原料，采用响应曲面法中的central composite design（CCD）设计实验，分别考察了温度、碳酸钠加料速度、碳酸钠浓度和锂离子浓度4个因素及交互作用对反应结晶工艺中碳酸锂的收率和粒度的影响，并分别建立了响应值与影响因素之间的回归方程。响应预测最佳值为：碳酸锂收率93.68%、粒径（d₅₀）16.73 μm；相应的实验值分别为94.01%和16.91 μm。预测值与实验值接近，误差较小，说明响应曲面法建立的预测碳酸锂反应结晶的模型可靠，在最佳工艺条件下分析所制得的产品，用ICP-AES分析纯度为99.52%，用XRD分析基本无杂峰，说明反应结晶生成Li₂CO₃晶体，其主要晶面为（-1 1 0）、（-2 2 0）和（0 0 2）。

关键词: 反应结晶, 整体优化, 数学模拟, 纯化, 响应曲面法, 交互作用

Abstract:

Lithium carbonate (Li₂CO₃) is used as raw material to prepare various lithium compounds, so the reactive crystallization of lithium carbonate is the key technique in the lithium industry. Central composite design(CCD), a kind of response surface methodology, was used to explore the effects of temperature, feeding speed of sodium carbonate (Na₂CO₃), concentration of Na₂CO₃ and concentration of lithium chloride(LiCl) on the yield of Li₂CO₃ and the particle size of Li₂CO₃. Based on the regression analysis, regression equations related to response values and factors were established, respectively. The optimal simulated values were found as follows:yield of Li₂CO₃ 93.68%, the median particle sizes (d₅₀) 16.73 μm, while the corresponding experimental results were 94.01% and 16.91 μm, respectively. The errors between the predicted and experimental values were small, which showed that the established models were accurate and reliable for the analysis and prediction of the process of reactive crystallization. In the above conditions, battery-grade Li₂CO₃ were prepared and its purity reached 99.52%. No impurity peak could be observed in the XRD analysis of Li₂CO₃ product, and its main crystal faces were (-1 1 0), (-2 2 0) and (0 0 2).

Key words: reactive crystallization, global optimization, mathematical modeling, purification, response surface methodology, interaction effect

中图分类号:

TQ131.1⁺1

段绍君, 孙玉柱, 宋兴福, 于建国. 响应曲面法优化碳酸锂反应结晶工艺[J]. 化工学报, 2017, 68(11): 4169-4177.

DUAN Shaojun, SUN Yuzhu, SONG Xingfu, YU Jianguo. Optimization of reactive-crystallization process of lithium carbonate based on response surface methodology[J]. CIESC Journal, 2017, 68(11): 4169-4177.

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响应曲面法优化碳酸锂反应结晶工艺

Optimization of reactive-crystallization process of lithium carbonate based on response surface methodology

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