Process intensification for the synthesis and purification of battery-grade Li2CO3 with microfluidics--颗粒学报PARTICUOLOGY

Li, H., Zhang, J., Dai, L., Du, L., & Zhu, J. (2024). Process intensification for the synthesis and purification of battery-grade Li2CO3 with microfluidics. Particuology, 90, 106-117. https://doi.org/10.1016/j.partic.2023.12.001

Process intensification for the synthesis and purification of battery-grade Li₂CO₃ with microfluidics

Haodu Li, Jie Zhang, Lin Dai, Le Du^*, Jiqin Zhu^*

The State Key Laboratory of Chemical Resource Engineering, College of Chemical Engineering, Beijing University of Chemical Technology, Beijing 100029, China

10.1016/j.partic.2023.12.001

Volume 90, July 2024, Pages 106-117

Received 18 October 2023, Revised 20 November 2023, Accepted 1 December 2023, Available online 11 December 2023, Version of Record 26 December 2023.

E-mail: dule@mail.buct.edu.cn; zhujq@mail.buct.edu.cn

Highlights

• Battery-grade Li₂CO₃ particles were prepared with microfluidics.

• A membrane dispersion microreactor was used to enhance mass transfer.

• Synthetic systems of Na₂CO₃–LiCl, NH₄HCO₃–LiCl and NH₃·H₂O−CO₂−LiCl were adopted.

• Li₂CO₃ particles with a size of 3–5 μm were prepared.

• A purity of 99.7–99.8 wt% was achieved in the ammonia-based systems.

Abstract

Battery-grade lithium carbonate (Li₂CO₃) with a purity of higher than 99.5 wt% is of great importance as a high value-added lithium salt. However, influences of different reaction systems and process control on product purity remain unclear. Herein, a membrane dispersion microreactor was used to enhance the mass transfer of preparation and purification processes in homogeneous and heterogeneous system. Synthetic systems of Na₂CO₃–LiCl, NH₄HCO₃–LiCl, and NH₃·H₂O−CO₂−LiCl, CO₂purification based on carbonation and decomposition were adopted. The Li₂CO₃ purity was increased by the improvement of mixing performance. The carbonation time was reduced by 62.5% and 58.3% for the NH₃·H₂O−CO₂ and CO₂ purification systems, respectively. In the two ammonia-based systems, Li₂CO₃ particles with a purity of 99.7–99.8 wt% were one-step prepared with a size of 3–5 μm, which also met the requirement of the battery-grade standard. The purity was further increased to 99.9 wt% by CO₂ purification and LiHCO₃ decomposition. The investigation could provide a feasible alternative for the controllable preparation of battery-grade Li₂CO₃ in one or multiple steps.

Graphical abstract

Keywords

Microfluidics; Battery grade; Li₂CO₃; Process intensification; High purity

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