Research progress on preparation of high purity lithium carbonate through hydrogenation-decomposition technology

doi:10.16085/j.issn.1000-6613.2024-1671

Abstract

Abstract:

High purity lithium carbonate is used as essential raw material in the fields of magnetic materials, atomic energy and optoelectronics. Considering the increasing demand of high purity lithium carbonate, the purification technologies of crude lithium carbonate have been given widespread concern. Hydrogenation-decomposition have recently emerged with good potential application in Li₂CO₃ purification. Herein, recent developments in the field of hydrogenation-decomposition covering optimization of process parameters and macroscopic kinetics of hydrogenation process, crystal growth and agglomeration control during pyrolysis were summarized. Meanwhile, the application studies of process strengthening technology as well as the deep removal technology of trace impurities in hydrogenation pyrolysis were highlighted. The future development direction was further prospected. Overall, this review intended to provide a theoretical support and further guide the industrial application of high purity Li₂CO₃ generated by hydrogenation-decomposition method.

Key words: high purity lithium carbonate, hydrogenation-decomposition, purification, trace impurities separation

摘要：

高纯碳酸锂作为磁性材料行业、原子能工业、电子工业和光学仪器行业的重要原料，市场需求量逐年提升。以大宗粗碳酸锂为原料纯化精制高纯碳酸锂的相关技术备受关注。其中，氢化热解法因可操作强、收率高等特点在制备高纯碳酸锂方面展现出广阔应用前景。本文围绕氢化过程和热解过程介绍了近年来制备高纯碳酸锂的最新研究进展，包括氢化过程的传质反应机理和宏观动力学，分析了CO₂流速和液固比等工艺参数对氢化率的影响，总结了关键工艺参数优化范围；探讨了热解过程中晶体生长与团聚控制等关键科学问题，重点关注了近年来过程强化技术和微量杂质深度脱除技术在氢化热解制备高纯碳酸锂工艺中的具体应用，并对其未来发展方向提出进一步展望。本文旨在为氢化热解法纯化粗碳酸锂制备高纯碳酸锂的工业化应用提供理论支撑和技术支持。

关键词: 高纯碳酸锂, 氢化热解, 纯化, 微量杂质脱除

CLC Number:

TQ131.1

LI Yahui, LIU Taoran, ZHU Ruisong, CAO Jing, LIU Minghui, LI Yingwen, HU Xuesheng, GAO Fei. Research progress on preparation of high purity lithium carbonate through hydrogenation-decomposition technology[J]. Chemical Industry and Engineering Progress, 2025, 44(11): 6133-6143.

李亚辉, 刘陶然, 朱瑞松, 曹靖, 刘铭晖, 李应文, 胡雪生, 高飞. 氢化热解法制备高纯碳酸锂的研究进展[J]. 化工进展, 2025, 44(11): 6133-6143.

Figures/Tables 11

References 64

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方法名称	方法描述	方法评价
Zintl-Harder-Dauth法	将粗碳酸锂溶于醋酸中，以(NH₄)₂C₂O₄沉淀Ca²⁺，以Ba(OH)₂沉淀Mg²⁺，再以H₂SO₄除去Ba²⁺，所得混合液经过滤干燥后灼热除去铵盐，剩余固体溶于盐酸后碳化得到精制Li₂CO₃^[26]	该法需要投加大量化学试剂且伴产固废，增加了固废处置的费用，环境友好性差
苛化法	向粗碳酸锂浆料中加入精制石灰乳，将Ca²⁺、Mg²⁺等杂质沉淀后过滤去除，碳化	收率较低、产生固废
电解法	以粗碳酸锂氢化或酸溶后的溶液为阳极液，LiOH溶液为阴极液，两者间以离子选择性渗透膜隔开，电解	所需膜材料价格昂贵，工业应用前景较差
重结晶法	利用碳酸锂在水中的溶解度随温度的升高而降低、大部分杂质溶解度随温度升高而增大的差异，通过调控温度，反复进行溶解-结晶过程提升产品纯度	该方法对产品纯度的提升程度非常有限，且由于碳酸锂具有一定的水溶性，收率普遍低于75%^[27-28]
氢化热解法	以粗碳酸锂料浆为原料，通入CO₂将Li₂CO₃氢化，使微溶的Li₂CO₃转变为可溶性的LiHCO₃，将杂质去除后升温热解制备高纯碳酸锂	流程简单，CO₂的利用和回收是关键问题，应用前景广阔

方法名称	方法描述	方法评价
Zintl-Harder-Dauth法	将粗碳酸锂溶于醋酸中，以(NH₄)₂C₂O₄沉淀Ca²⁺，以Ba(OH)₂沉淀Mg²⁺，再以H₂SO₄除去Ba²⁺，所得混合液经过滤干燥后灼热除去铵盐，剩余固体溶于盐酸后碳化得到精制Li₂CO₃^[26]	该法需要投加大量化学试剂且伴产固废，增加了固废处置的费用，环境友好性差
苛化法	向粗碳酸锂浆料中加入精制石灰乳，将Ca²⁺、Mg²⁺等杂质沉淀后过滤去除，碳化	收率较低、产生固废
电解法	以粗碳酸锂氢化或酸溶后的溶液为阳极液，LiOH溶液为阴极液，两者间以离子选择性渗透膜隔开，电解	所需膜材料价格昂贵，工业应用前景较差
重结晶法	利用碳酸锂在水中的溶解度随温度的升高而降低、大部分杂质溶解度随温度升高而增大的差异，通过调控温度，反复进行溶解-结晶过程提升产品纯度	该方法对产品纯度的提升程度非常有限，且由于碳酸锂具有一定的水溶性，收率普遍低于75%^[27-28]
氢化热解法	以粗碳酸锂料浆为原料，通入CO₂将Li₂CO₃氢化，使微溶的Li₂CO₃转变为可溶性的LiHCO₃，将杂质去除后升温热解制备高纯碳酸锂	流程简单，CO₂的利用和回收是关键问题，应用前景广阔

名称	类型	官能团	颗粒尺寸/mm	交换容量	参考文献
TOKEM 308	强酸性磺酸阳离子交换	—SO₃H	0.2~0.3	1.9mg/cm³	[50]
TOKEM 200	弱酸性羧酸阳离子交换	—COOH	0.3~1.6	4.3mg/cm³	[50]
Purolite S930	亚氨基羧基阳离子交换剂	—N(CH₂COOH)₂	0.4~1.0	1.5mg/cm³	[50]
Amberlite IRC 748	亚氨基羧基阳离子交换剂	—N(CH₂COOH)₂	0.5~0.65	≥1.35mg/cm³	[50]
AXIONIT 3S	亚氨基羧基阳离子交换剂	—N(CH₂COOH)₂	0.3~0.8	1.3~1.4mg/cm³	[50]
D412	—	—	—	0.014mg/cm³（以Ca计）	[49]
Dowex G26	强酸性阳离子交换树脂	—	—	80mg/g（吸附容量）	[37]
Amberlite IRC 747	螯合树脂	—CH₂NHCH₂PO₃Na₂	0.52~0.66	≥1.75×10^-3mg/cm³（以Na计）	[21]
AG 50W-X8	磺化聚苯乙烯树脂	—SO₃H	—	—	[3]

名称	类型	官能团	颗粒尺寸/mm	交换容量	参考文献
TOKEM 308	强酸性磺酸阳离子交换	—SO₃H	0.2~0.3	1.9mg/cm³	[50]
TOKEM 200	弱酸性羧酸阳离子交换	—COOH	0.3~1.6	4.3mg/cm³	[50]
Purolite S930	亚氨基羧基阳离子交换剂	—N(CH₂COOH)₂	0.4~1.0	1.5mg/cm³	[50]
Amberlite IRC 748	亚氨基羧基阳离子交换剂	—N(CH₂COOH)₂	0.5~0.65	≥1.35mg/cm³	[50]
AXIONIT 3S	亚氨基羧基阳离子交换剂	—N(CH₂COOH)₂	0.3~0.8	1.3~1.4mg/cm³	[50]
D412	—	—	—	0.014mg/cm³（以Ca计）	[49]
Dowex G26	强酸性阳离子交换树脂	—	—	80mg/g（吸附容量）	[37]
Amberlite IRC 747	螯合树脂	—CH₂NHCH₂PO₃Na₂	0.52~0.66	≥1.75×10^-3mg/cm³（以Na计）	[21]
AG 50W-X8	磺化聚苯乙烯树脂	—SO₃H	—	—	[3]