含锂工业废料制备电池级碳酸锂工艺研究

doi:10.11962/1006-4990.2019-0221

Abstract

Abstract:

The market demand for battery-grade lithium carbonate is increasing with the rapid development of the battery industry.The lithium-containing industrial waste from a company was used as raw material,and it was purified by carbonization decomposition method,and the filtrate filter cake cycle was repeated,and finally the battery-grade lithium carbonate meeting the requirement of the industry standard was obtained.The reaction conditions of the carbonization process was as follows：the solid-liquid mass-volume ratio was 1:50,the stirring speed was 300 r/min,the CO₂ flow rate was 10 L/min,the reaction tem-perature was 20 ℃ and the reaction time was 60 min.The reaction conditions of the thermal decomposition process was as follows： the stirring speed was 300 r/min,the reaction temperature was 95 ℃ and the reaction time was 60 min.After a five-stage filtrate cake cycle for the Li₂CO₃ obtained by the carbonization-and decomposition-processes,the final purified Li₂CO₃ product can fully meets the requirement of battery-grade lithium carbonate industry standard.The content of Li₂CO₃ in the product was 99.71%,the mass fractions of Mg,Ca and K were reduced to 0.005 3%,0.005 0% and 0.000 9%,respectively.The yield was maintained above 55%,and the product had a rod shape,uniform size and good dispersion.

Key words: battery-grade lithium carbonate, carbonization reaction, thermal decomposition reaction, purification

CLC Number:

TQ131.11

Hu Min,Gong Hanzhang,Wu Huadong,Guo Jia,Zhang Linfeng,Zhou Yuxin. Preparation of battery-grade lithium carbonate from lithium-containing industrial waste[J]. Inorganic Chemicals Industry, 2020, 52(3): 80-84.

Figures/Tables 7

References 20

[1]	魏昊, 田欢, 张梦龙 , 等. 电池级碳酸锂制备与提纯的研究进展[J]. 现代化工, 2018,38(8):33-37.
[2]	刘光启, 马连湘, 刘杰 . 化学化工物性数据手册[M]. 北京: 化学工业出版社, 2002.
[3]	尹记帅, 孙文亮, 郝如斯 , 等. 沉锂反应条件对碳酸锂纯度及杂质影响的研究[J]. 无机盐工业, 2019,51(3):29-33.
[4]	乜贞, 卜令忠, 王云生 , 等. 盐湖卤水资源锂镁分离的工艺技术[J]. 无机盐工业, 2013,45(5):1-4.
[5]	Arikan M, Sobolev K, Ertün T , et al. Properties of blended cements with thermally activated kaolin[J]. Construction & Building Materi-als, 2009,23(1):62-70.
[6]	Scrosati B, Garche J . Lithium batteries:Status,prospects and fut-ure[J]. Journal of Power Sources, 2010,195(9):2419-2430.
[7]	李燕茹, 朱亮, 袁建军 , 等. 粗级碳酸锂提纯工艺过程研究[J]. 无机盐工业, 2013,45(8):15-17.
[8]	赵春龙, 孙峙, 郑晓洪 , 等. 碳酸锂的制备及其纯化过程的研究进展[J]. 过程工程学报, 2018,18(1):20-28.
[9]	祁双文, 李积仓 . 粗级碳酸锂提纯工艺过程分析[J]. 化工管理, 2016(31):221.
[10]	Kesler S E, Gruber P W, Medina P A , et al. Global lithium resour-ces:Relative importance of pegmatite,brine and other deposits[J]. Ore Geology Reviews, 2012,48(5):55-69.
[11]	Yi W T, Yan C Y, Ma P H . Crystallization kinetics of Li₂CO₃ from LiHCO₃ solutions[J]. Journal of Crystal Growth, 2010,312(16/17):2345-2350.
[12]	王珂 . 从锂云母中提取碱金属化合物[D]. 上海:华东理工大学, 2013.
[13]	刘人生, 田礼平, 熊铜兴 . 高杂质碳酸锂提纯工艺研究[J]. 化工技术与开发, 2018,47(7):5-7.
[14]	王运其 . 浅谈高纯碳酸锂的制备方法[J]. 新疆有色金属, 2009,32(z1):92-93.
[15]	Wu H, Cui Y . Designing nanostructured Si anodes for high energy lithium ion batteries[J]. Nano Today, 2012,7(5):414-429.
[16]	陈宁 . 盐湖卤水碳化沉锂过程研究及工艺优化[D]. 北京:中国科学院大学(中国科学院过程工程研究所), 2017.
[17]	汪发波, 王林生, 文小强 . 碳化分解法提纯碳酸锂的研究[J]. 有色金属科学与工程, 2013,4(2):41-45.
[18]	赵泉峰, 吴鉴, 姚耀春 . 碳化分解法制备电池级碳酸锂的研究[J]. 材料导报, 2014,28(10):75-77.
[19]	周启立, 王莫飞 . 碳化法制备高纯碳酸锂[J]. 无机盐工业, 2012,44(7):36-37.
[20]	GB/T 11064.1—2013 碳酸锂、单水氢氧化锂、氯化锂化学分析方法第1部分:碳酸锂量的测定(酸碱滴定法)[S].

主要成分	质量分数/%	主要成分	质量分数/%
Li₂CO₃	97.00	K	0.008 5
Na	0.185 1	Fe	0.030 0
Mg	0.056 1	SO₄^2-	0.163 8
Ca	0.063 4	Cl^-	0.159 6

碳酸锂	w（Na）	w（Mg）	w（Ca）	w（K）	w（Fe）	w（Zn）	w（Cu）
电池级	≤ 0.025	≤ 0.008	≤ 0.005	≤ 0.001	≤ 0.001	≤ 0.000 3	≤ 0.000 3
实验产品	0.023 6	0.005 3	0.005	0.000 9	0.000 5	0.000 28	0.000 3
碳酸锂	w （Pb）	w （Si）	w （Al）	w （Mn）	w （Ni）	w（SO₄^2-）	w （Cl）
电池级	≤ 0.000 3	≤ 0.003	≤ 0.001	≤ 0.000 3	≤ 0.001	≤ 0.08	≤ 0.003
实验产品	0.000 27	0.001 9	0.000 9	0.000 26	0.000 5	0.071 9	0.002 8

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Preparation of battery-grade lithium carbonate from lithium-containing industrial waste

RichHTML

PDF (PC)

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 7

References 20

Related Articles 15

Metrics

Comments

Recommended 10

[1]	Zhang Yan,Zhao Zhenzhong,Ma Zhaohui,Zhao Yancai,Chen Zhiyu,Ma Zhengqiang. Optimization of process for preparation of battery grade lithium carbonate by carbonization [J]. Inorganic Chemicals Industry, 2020, 52(3): 68-71.
[2]	Li Wenqing,Zou Ping. Progress in preparation and research of high purity polyaluminium chloride [J]. Inorganic Chemicals Industry, 2020, 52(1): 30-34.
[3]	Guo Ju. Study on preparation of battery-grade ferrous sulfate by purification of titanium white slag [J]. Inorganic Chemicals Industry, 2019, 51(8): 48-51.
[4]	Wang Ben,Chen Mengmeng,Zhang Fan. Research progress on purification technology of hydrogen peroxide [J]. Inorganic Chemicals Industry, 2019, 51(6): 1-4.
[5]	Zhang Pinghua,Yan Yunjie,Chen Jianjun,Wang Hongyan,Zhang Chunli,Wu Ning. Preparation of nanometer calcium carbonate from high-Ca-Mg phosphorus tailings by acid leaching [J]. Inorganic Chemicals Industry, 2019, 51(3): 63-66.
[6]	TAN Ming-Yang, ZHANG Xi-Xing, XIANG Li-Xue, YU Xin. Research progress of phosphorus gypsum as cement retarder [J]. INORGANICCHEMICALSINDUSTRY, 2016, 48(7): 4-.
[7]	CAI Zhuang-Hong, HE Su-Jiao. Study on continuous preparation of potassium ferrate by electrolytic process [J]. INORGANICCHEMICALSINDUSTRY, 2016, 48(7): 51-.
[8]	YANG Tie-Jian, YAN Xin. Research on CPAM coagu-flocculation mechanism in brine purification process [J]. INORGANICCHEMICALSINDUSTRY, 2016, 48(6): 32-.
[9]	LI Xin-Zhu, GUO Zong-Duan, JIA Liang, JIA Hong-Xiu, HU Zhao-Ping, WANG Zhou. Preparation of industrial mono-ammonium phosphate from wet process phosphoric acid purified by methanol precipitation method [J]. INORGANICCHEMICALSINDUSTRY, 2016, 48(2): 40-.
[10]	LIU Fei, LI Tian-Xiang, JIE Tian, SHI Lian-Jun. Study on purification of purified wet-process phosphoric acid [J]. INORGANICCHEMICALSINDUSTRY, 2016, 48(2): 42-.
[11]	YAN Xin, LU Yun-Feng, YANG Tie-Jian. New technology of lime and flue-gas brine purification with waste-slurry zero discharge [J]. INORGANICCHEMICALSINDUSTRY, 2016, 48(11): 44-.
[12]	CHEN De-Qing, WANG Na, ZHANG Min, SHEN Xing-Ming, LIU Peng. Study on preparation of industrial grade MAP by WPA [J]. INORGANICCHEMICALSINDUSTRY, 2016, 48(1): 38-.
[13]	XIE Zi-Nan, WANG Jiao, SHEN Jia-Guo. Research on purification of Ca(Ⅱ) and Mg(Ⅱ) in industrial manganese sulfate [J]. INORGANICCHEMICALSINDUSTRY, 2015, 47(5): 48-.
[14]	KUANG Jia-Ling. Desilication of artificial cryolite products with high molecular ratio [J]. INORGANICCHEMICALSINDUSTRY, 2015, 47(2): 49-.
[15]	ZHANG Zhi-Qiang, ZHANG Cai-Mian, SUN Ying-Bo, TANG Qiang. Research on purification of wet process phosphoric acid by methyl isobutyl ketone [J]. INORGANICCHEMICALSINDUSTRY, 2014, 46(7): 20-.