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

DUAN Shaojun; SUN Yuzhu; SONG Xingfu; YU Jianguo

doi:10.11949/j.issn.0438-1157.20170461

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

更新时间：2025-12-10

- Optimization of reactive-crystallization process of lithium carbonate based on response surface methodology
- CIESC Journal Issue 11, Pages: 4169-4177(2017)
- 作者机构：
  
  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
- 作者简介：
- 基金信息：
- DOI：10.11949/j.issn.0438-1157.20170461
  CLC： Q131.1+1
- Online First：05 November 2017，
  
  Published：05 November 2017
- 稿件说明：
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DUAN Shaojun, SUN Yuzhu, SONG Xingfu, et al. Optimization of reactive-crystallization process of lithium carbonate based on response surface methodology[J]. CIESC Journal, 2017, (11): 4169-4177.
DOI：

DUAN Shaojun, SUN Yuzhu, SONG Xingfu, et al. Optimization of reactive-crystallization process of lithium carbonate based on response surface methodology[J]. CIESC Journal, 2017, (11): 4169-4177. DOI： 10.11949/j.issn.0438-1157.20170461.

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）。

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).

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