以碳酸钾为原料制备碳酸锂晶体团聚现象及调控方法的研究
收稿日期: 2023-12-13
网络出版日期: 2024-02-04
基金资助
青海省自然科学基金项目(2023-ZJ-712);国家自然科学基金项目(21968026)
Study on agglomeration phenomenon and regulation method of lithium carbonate crystal prepared from potassium carbonate
Received date: 2023-12-13
Online published: 2024-02-04
以氯化锂与碳酸钾为原料进行反应结晶制备碳酸锂,以提高碳酸锂收率、降低其钾含量及获得良好粒径分布为目标,考察反应温度、搅拌转速、晶种加入量及晶种加入的粒径大小对实验的影响。实验结果表明,氯化锂与碳酸钾反应结晶存在着明显的晶体团聚现象,反应温度不同,对晶体形貌有显著影响,低温下晶体呈片状团聚体,较高温度下晶体呈棒状团聚体。剪切力的增加可以减小团聚体尺寸,晶种的加入有利于抑制爆发成核,减轻晶体团聚和黏壁现象。实验结果表明,在反应温度为85 ℃、搅拌转速为400 r/min、氯化锂浓度为3.2 mol/L、晶种加入量为3.0 g/L、晶种粒径控制在小于54 μm、超声功率为100 W、超声时间为150 min条件下,获得的碳酸锂收率高、晶体不易发生聚结、钾含量较低且拥有较好的粒径分布。以碳酸钾为原料制备的碳酸锂与以碳酸钠为原料制备的碳酸锂收率相当,但杂质含量有一定的降低。且在反应结晶过程中加入超声后可有效避免出现大团聚体,在保证碳酸锂收率无明显降低的情况下,钾含量明显降低。通过研究获得的实验条件可以为碳酸锂生产调整工艺参数提供依据,并为产品质量的提高提供指导。
成春春 , 李玉龙 , 张志强 , 左硕 , 覃冬兰 , 周娜 , 王佳琴 . 以碳酸钾为原料制备碳酸锂晶体团聚现象及调控方法的研究[J]. 无机盐工业, 2024 , 56(10) : 47 -54 . DOI: 10.19964/j.issn.1006-4990.2023-0599
Lithium carbonate was prepared by reaction crystallization using lithium chloride and potassium carbonate as raw materials.The experimental conditions such as reaction temperature,stirring speed,seed addition amount,and seed particle size were investigated with the aim of improving the yield of lithium carbonate,reducing its potassium content,and obtaining a good particle size distribution.The experiment showed that there was a significant crystal agglomeration phenomenon in the reaction crystallization of lithium chloride and potassium carbonate.Different reaction temperatures had a significant impact on the crystal morphology,with crystals showing flake⁃like agglomerates at low temperatures and rod⁃like agglomerates at higher temperatures.The increase of shear force could reduce the size of agglomerates,and the addition of seed crystals was beneficial to suppress explosive nucleation,reduced crystal agglomeration and wall sticking.The experimental results showed that when the reaction temperature was 85 ℃,the stirrer speed was 400 r/min,the lithium chloride concentration was 3.2 mol/L,the seed addition amount was 3.0 g/L,the seed particle size was controlled to be less than 54 μm,and the ultrasonic power was 100 W for 150 min,the yield of lithium carbonate was high,the crystals were not prone to coalescence,the potassium content was low,and the particle size distribution was good.The yield of lithium carbonate prepared using potassium carbonate as raw material was comparable to that prepared using sodium carbonate as raw material,but the impurity content was reduced to some extent.Adding ultrasound during the reaction crystallization process could effectively avoid the formation of large agglomerates,and the potassium content was significantly reduced while ensuring the yield of lithium carbonate was not significantly reduced.The experimental conditions obtained through the study could provide a basis for adjusting process parameters in the production of lithium carbonate,and provide guidance for improving product quality.
Key words: lithium carbonate; crystal; agglomeration; seed crystal; ultrasonic
| 1 | GAO Tianming, FAN Na, CHEN Wu,et al.Lithium extraction from hard rock lithium ores(spodumene,lepidolite,zinnwaldite,petalite):Technology,resources,environment and cost[J].China Geology,2023(1):137-153. |
| 2 | 邢凯,朱清,任军平,等.全球锂资源特征及市场发展态势分析[J].地质通报,2023,42(8):1402-1421. |
| XING Kai, ZHU Qing, REN Junping,et al.Research on the characteristics and market development trend of global lithium resourc?es[J].Geological Bulletin of China,2023,42(8):1402-1421. | |
| 3 | SHANG Xiaohong, LIU Jianyun, HU Bin,et al.CNT-strung LiMn2O4 for lithium extraction with high selectivity and stabili? ty[J].Small Methods,2022,6(7):2200508. |
| 4 | HU Bin, SHANG Xiaohong, NIE Pengfei,et al.Lithium ion sieve modified three?dimensional graphene electrode for selective extraction of lithium by capacitive deionization[J].Journal of Colloid and Interface Science,2022,612:392-400. |
| 5 | 乜贞,伍倩,丁涛,等.中国盐湖卤水提锂产业化技术研究进展[J].无机盐工业,2022,54(10):1-12. |
| NIE Zhen, WU Qian, DING Tao,et al.Research progress on industrialization technology of lithium extraction from salt lake brine in China[J].Inorganic Chemicals Industry,2022,54(10):1-12. | |
| 6 | ZHANG Ye, SUN Wei, XU Rui,et al.Lithium extraction from water lithium resources through green electrochemical?battery approaches:A comprehensive review[J].Journal of Cleaner Production,2021,285:124905. |
| 7 | ZHANG Ye, HU Yuehua, WANG Li,et al.Systematic review of lithium extraction from salt?lake brines via precipitation approach? es[J].Minerals Engineering,2019,139:105868. |
| 8 | NGUYEN T, LEE M.A review on the separation of lithium ion from leach liquors of primary and secondary resources by solvent extraction with commercial extractants[J].Processes,2018,6(5): 55. |
| 9 | QIAO Linju, CHEN Hang, YU Jianguo.Recovery of lithium from salt?lake brine by liquid?liquid extraction using TBP-FeCl3 based mixture solvent[J].The Canadian Journal of Chemical Engineering,2023,101(4):2139-2147. |
| 10 | GUO Youhong,BAE J, FANG Zhiwei,et al.Hydrogels and hydrogel?derived materials for energy and water sustainability[J].Chemical Reviews,2020,120(15):7642-7707. |
| 11 | SHANG Xiaohong, HU Bin, NIE Pengfei,et al.LiNi0.5Mn1.5O4-based hybrid capacitive deionization for highly selective adsorption of lithium from brine[J].Separation and Purification Technology,2021,258:118009. |
| 12 | WU Qian, YU Jiangjiang, BU Lingzhong,et al.The application of an enhanced salinity?gradient solar pond with nucleation matrix in lithium extraction from Zabuye salt lake in Tibet[J].Solar Energy,2022,244:104-114. |
| 13 | MULLIN J W.Crystallisation[M].4th ed.London:Elsevier Science,2001. |
| 14 | 刘玉强,张志强,毕秋艳,等.超声波对碳酸锂反应结晶过程的影响[J].无机盐工业,2019,51(4):42-47. |
| LIU Yuqiang, ZHANG Zhiqiang, BI Qiuyan,et al.Influence of ultrasonic on reaction crystallization process of lithium carbon?ate[J].Inorganic Chemicals Industry,2019,51(4):42-47. | |
| 15 | TABORGA P, BRITO I, GRABER T A.Effect of additives on size and shape of lithium carbonate crystals[J].Journal of Crystal Gro? wth,2017,460:5-12. |
| 16 | 王彦飞,王磊鑫,邢红,等.反应结晶制备碳酸锂的粒度及形貌控制[J].无机盐工业,2016,48(9):13-17. |
| WANG Yanfei, WANG Leixin, XING Hong,et al.Size and morphology controlling of lithium carbonate in reactive crystallization process[J].Inorganic Chemicals Industry,2016,48(9):13-17. | |
| 17 | 殷海青,马祎明,万旭兴,等.碳酸锂气液固三相反应结晶过程研究[J].化工学报,2022,73(3):1207-1220. |
| YIN Haiqing, MA Yiming, WAN Xuxing,et al.Research of lithium carbonate three?phase reactive crystallization process[J].CIESC Journal,2022,73(3):1207-1220. | |
| 18 | 曾雄,易丹青,王斌,等.超声对碳酸锂溶液反应结晶成核过程的影响[J].有色金属文摘,2015,30(3):111-113. |
| ZENG Xiong, YI Danqing, WANG Bin,et al.The effects of ultrasound on the process of lithium carbonate solution reaction crystal nucleation[J].Nonferrous Metals Abstract,2015, 30(3): 111-113. | |
| 19 | LI Hong, LI Hairong, GUO Zhichao,et al.The application of power ultrasound to reaction crystallization[J].Ultrasonics Sonochemistry,2006,13(4):359-363. |
| 20 | LI Hong, WANG Jingkang, BAO Ying,et al.Rapid sonocrystallization in the salting?out process[J].Journal of Crystal Growth,2003,247(1/2):192-198. |
| 21 | GAHN C, MERSMANN A.Brittle fracture in crystallization processes Part B.Growth of fragments and scale?up of suspension crystallizers[J].Chemical Engineering Science,1999,54(9):1283-1292. |
| 22 | HOUNSLOW M J, RYALL R L, MARSHALL V R.A discretized population balance for nucleation,growth,and aggregation[J].AIChE Journal,1988,34(11):1821-1832. |
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