Synthesis of high purity Li2CO3 and MgCO3·3H2O in a homogeneous-like organic phase

doi:10.1016/j.cjche.2019.02.009

摘要/Abstract

摘要： Herein, three kinds of Li₂CO₃ and two kinds of MgCO₃·3H₂O crystals are easily synthesized in a homogeneouslike organic phase. The morphology and size of synthesized crystals are controllable and adjustable in the single organic phase, with the morphology of Li₂CO₃ ranging from micro-flaky, flower to nanobranch, MgCO₃·3H₂O ranging from nanosphere to nanorod. Compared with coupled reaction and solvent extraction process, of which the crystallization process occurred in the interface of two phase, our proposed method made it possible that the crystallization process occurred in the single organic phase, which resulted in better crystal morphology. Moreover, the formation mechanism of different crystal morphologies is discussed, the results showed that the crystals in micron size and nano size are involved in two crystallization mechanism, the micron particles in the form of flake and flower-like is a typical radial growth, which means that the growth occurs by diffusion around a nucleus as starting point, while the reaction model for small particles should be similar to a water-in-oil structure. As the reaction carried out, the crystal should be restricted in a constrained organic structure.

关键词: Li₂CO₃, MgCO₃· 3H₂O, Morphology, Crystallization mechanism

Abstract: Herein, three kinds of Li₂CO₃ and two kinds of MgCO₃·3H₂O crystals are easily synthesized in a homogeneouslike organic phase. The morphology and size of synthesized crystals are controllable and adjustable in the single organic phase, with the morphology of Li₂CO₃ ranging from micro-flaky, flower to nanobranch, MgCO₃·3H₂O ranging from nanosphere to nanorod. Compared with coupled reaction and solvent extraction process, of which the crystallization process occurred in the interface of two phase, our proposed method made it possible that the crystallization process occurred in the single organic phase, which resulted in better crystal morphology. Moreover, the formation mechanism of different crystal morphologies is discussed, the results showed that the crystals in micron size and nano size are involved in two crystallization mechanism, the micron particles in the form of flake and flower-like is a typical radial growth, which means that the growth occurs by diffusion around a nucleus as starting point, while the reaction model for small particles should be similar to a water-in-oil structure. As the reaction carried out, the crystal should be restricted in a constrained organic structure.

Key words: Li₂CO₃, MgCO₃· 3H₂O, Morphology, Crystallization mechanism

Lang Li, Jinsong Sui, Wei Qin. Synthesis of high purity Li₂CO₃ and MgCO₃·3H₂O in a homogeneous-like organic phase[J]. 中国化学工程学报, 2019, 27(5): 1230-1234.

Lang Li, Jinsong Sui, Wei Qin. Synthesis of high purity Li₂CO₃ and MgCO₃·3H₂O in a homogeneous-like organic phase[J]. Chinese Journal of Chemical Engineering, 2019, 27(5): 1230-1234.

参考文献

[1] C.L. Zeng, P.Y. Guo, W.T. Wu, Electrochemical impedance spectra for the corrosion of two-phase Cu-15Al alloy in eutectic (Li, K)₂CO₃ at 650℃ in air, Electrochim. Acta 49(2004) 1445-1450.
[2] A.J. Smith, S.H. Kim, N.K. Duggirala, J. Jin, L. Wojtas, J. Ehrhart, B. Giunta, J. Tan, M.J. Zaworotko, R.D. Shytle, Improving lithium therapeutics by crystal engineering of novel ionic cocrystals, Mol. Pharm. 10(2013) 4728-4738.
[3] T.D. Gould, A.M. Picchini, H. Einat, H.K. Manji, Targeting glycogen synthase kinase-3 in the CNS:implications for the development of new treatments for mood disorders, Curr. Drug Targets 7(2006) 1399-1409.
[4] Y.D.D.C. Sorescu, Density functional theory studies of the structural, electronic, and phonon properties of Li₂O, and Li₂CO₃:Application to CO₂ capture reaction, Phys. Rev. B 79(2009) 4301.
[5] L. Ji, Z. Lin, M. Alcoutlabi, X. Zhang, Recent developments in nanostructured anode materials for rechargeable lithium-ion batteries, Energy Environ. Sci. 4(2011) 2682-2699.
[6] J. Luo, W. Zhang, H. Yuan, C. Jin, L. Zhang, H. Huang, C. Liang, Y. Xia, J. Zhang, Y. Gan, X. Tao, Pillared structure design of MXene with ultralarge interlayer spacing for high-performance lithium-ion capacitors, ACS Nano 11(2017) 2459-2469.
[7] Lang Li, Jinsong Sui, Wei Qin, Superior capacity, rate, long cycle life and high temperature performance of multilayered porous ultralong LiMn₂O₄ nanorods for lithium ion batteries, J. Electroanal. Chem. 833(2019) 304-312.
[8] P.G. Bruce, B. Scrosati, J. Tarascon, Nanomaterials for rechargeable lithium batteries, Angew. Chem. Int. Ed. 47(2008) 2930-2946.
[9] B. Scrosati, J. Garche, Lithium batteries:Status, prospects and future, J. Power Sources 195(2010) 2419-2430.
[10] P.G. Bruce, S.A. Freunberger, L.J. Hardwick, J. Tarascon, Li-O₂ and Li-S batteries with high energy storage, Nat. Mater. 11(2011) 19-29.
[11] Lang Li, Jinsong Sui, Rui Huang, Wei Xiang, Wei Qin, Dependence of electrochemical properties of spinel LiMn₂O₄ on Li₂CO₃ with micro-flaky, micro-flower and nanorod morphologies, RSC Adv. 7(2017) 42289-42295.
[12] Wenting Cheng, Zhibao Li, Nucleation kinetics of nesquehonite (MgCO₃·3H₂O) in the MgCl₂-Na₂CO₃, J. Cryst. Growth 312(2010) 1563-1571.
[13] W. Xiang, S. Liang, Z. Zhou, W. Qin, W. Fei, Extraction of lithium from salt lake brine containing borate anion and high concentration of magnesium, Hydrometallurgy. 166(2016) 9-15.
[14] Z. Zhou, S. Liang, W. Qin, W. Fei, Extraction equilibria of lithium with tributyl phosphate, diisobutyl ketone, acetophenone, methyl isobutyl ketone, and 2-heptanone in kerosene and FeCl₃, Ind. Eng. Chem. Res. 52(2013) 7912-7917.
[15] X. Liu, G. Zhu, K. Yang, J. Wang, A mixture of LiNi_1/3Co_1/3Mn_1/3O₂ and LiCoO₂ as positive active material of LIB for power application, J. Power Sources 174(2007) 1126-1130.
[16] H. Dixit, W. Zhou, J. Idrobo, J. Nanda, V.R. Cooper, Facet-dependent disorder in pristine high-voltage lithium-manganese-rich cathode material, ACS Nano 8(2014) 12710-12716.
[17] F. Lin, I.M. Markus, D. Nordlund, T. Weng, M.D. Asta, H.L. Xin, M.M. Doeff, Surface reconstruction and chemical evolution of stoichiometric layered cathode materials for lithium-ion batteries, Nat. Commun. 5(2014) 3529.
[18] J. Cho, LiNi_0.74Co_0.26-xMg_xO₂ cathode material for a Li-ion cell, Chem. Mater. 12(2000) 3089-3094.
[19] B.C. Sun, X.M. Wang, J.M. Chen, Synthesis of nano-CaCO₃ by simultaneous absorption of CO₂ and NH₃ into CaCl₂ solution in a rotating packed bed, Chem. Eng. J. 168(2011) 731-736.
[20] Y. Li, X. Song, G. Chen, et al., Preparation of calcium carbonate and hydrogen chloride from distiller waste based on reactive extraction-crystallization process, Chem. Eng. J. 278(2015) 55-61.
[21] L. Xin, W. Wang, W. Man, et al., Experimental study of CO₂ mineralization in Ca²⁺-rich aqueous solutions using tributylamine as an enhancing medium, Energy Fuel 28(2014) 2047-2053.
[22] W. Wang, L. Xin, W. Peng, et al., Enhancement of CO₂ mineralization in Ca²⁺-/Mg²⁺-rich aqueous solutions using insoluble amine, Ind. Eng. Chem. Res. 52(2013) 8028-8033.
[23] Guilan Chen, Xingfu Song, Chunhua Dong, Mineralizing CO₂ as MgCO₃·3H₂O using abandoned MgCl₂ based on a coupled reaction-extraction-alcohol precipitation process, Energy Fuel 30(2016) 7551-7559.
[24] Z. Zhou, F. Liang, Q. Wei, et al., Coupled reaction and solvent extraction process to form Li₂CO₃:Mechanism and product characterization, AICHE J. 60(2014) 282-288.
[25] Xin X, Zhu T. Coupled process of reaction and solvent extraction I. The reaction between CO₂, and SrCl₂, coupled with solvent extraction of HCl. Hydrometallurgy. 76(2005) 11-17.
[26] Y. Lu, Y. Liu, C. Zhou, G. Luo, Preparation of Li₂CO₃ nanoparticles by carbonation reaction using a microfiltration membrane dispersion microreactor, Ind. Eng. Chem. Res. 53(2014) 11015-11020.
[27] W. Yi, C. Yan, P. Ma, Removal of calcium and magnesium from LiHCO₃ solutions for preparation of high-purity Li₂CO₃ by ion-exchange resin, Desalination. 249(2009) 729-735.
[28] Y. Sun, X. Song, J. Wang, J. Yu, Preparation of Li₂CO₃ by gas-liquid reactive crystallization of LiOH and CO₂, Cryst. Res. Technol. 47(2012) 437-442.
[29] Y. Sun, X. Song, J. Wang, J. Yu, Preparation of lithium carbonate hollow spheres by spray pyrolysis, Cryst. Res. Technol. 46(2011) 173-177.
[30] Y. Li, X. Song, G. Chen, S. Sun, Y. Xu, Extraction of hydrogen chloride by a coupled reaction-solvent extraction process, Front. Chem. Sci. Eng. 9(2015) 479-487.
[31] G. Chen, X. Song, C. Dong, S. Sun, Z. Sun, Mineralizing CO₂ as MgCO₃·3H₂O using abandoned MgCl₂ based on a coupled reaction-extraction-alcohol precipitation process, Energy Fuel 30(2016) 7551-7559.
[32] F. Chen, X. Wang, W. Liu, et al., Selective extraction of nitric and acetic acids from etching waste acid using N235 and MIBK mixtures, Sep. Purif. Technol. 169(2016) 50-58.
[33] Y. Li, X. Song, S. Sun, et al., Extraction equilibrium of hydrochloric acid at low concentrations between water and N235 in isoamyl alcohol solution:experiments and simulation, J. Chem. Eng. Data 60(2015) 3000-3008.
[34] L. Pastero, F.R. Massaro, D. Aquilano, Experimental and theoretical morphology of single and twinned crystals of Li₂CO₃(Zabuyelite), Cryst. Growth Des. 7(2007) 2749-2755.
[35] S. Chen, S. Yu, J. Jiang, F. Li, Y. Liu, Polymorph discrimination of CaCO₃ mineral in an ethanol/water solution:Formation of complex vaterite superstructures and aragonite rods, Chem. Mater. 18(2006) 115-122.

Synthesis of high purity Li₂CO₃ and MgCO₃·3H₂O in a homogeneous-like organic phase

Synthesis of high purity Li₂CO₃ and MgCO₃·3H₂O in a homogeneous-like organic phase

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价

[1]	Qiaoqiao Liu, Guihong Lin, Jian Zhou, Liangliang Huang, Chang Liu. Hydrogen-bond mediated and concentrate-dependent NaHCO₃ crystal morphology in NaHCO₃–Na₂CO₃ aqueous solution: Experiments and computer simulations[J]. 中国化学工程学报, 2023, 55(3): 49-58.
[2]	Fang Chen, Tao Zhou, Lijie Li, Chongwei An, Jun Li, Duanlin Cao, Jianlong Wang. Morphology prediction of dihydroxylammonium 5,5'-bistetrazole-1,1'-diolate (TKX-50) crystal in different solvent systems using modified attachment energy model[J]. 中国化学工程学报, 2023, 53(1): 181-193.
[3]	Jialu Zhang, Xiang Liu, Shuai Liu, Yuxing Li, Qihui Hu, Wuchang Wang. Microscopic morphology evolution of the crystal structure of tetrahydrofuran hydrate under flowing condition[J]. 中国化学工程学报, 2022, 45(5): 103-110.
[4]	Xin Jiang, Baojiang Sun, Zhiyuan Wang, Wantian Zhou, Jiakai Ji, Litao Chen. Methane hydrate crystal growth on shell substrate[J]. 中国化学工程学报, 2022, 43(3): 50-61.
[5]	Zuhong Lin, Fushuai Xu, Lili Wang, Liyang Hu, Lingfu Zhu, Jie Tan, Zhifeng Li, Tingting Zhang. Characterization of oil component and solid particle of oily sludge treated by surfactant-assisted ultrasonication[J]. 中国化学工程学报, 2021, 34(6): 53-60.
[6]	Xuke Ruan, Xiao-Sen Li. Investigation of the methane hydrate surface area during depressurization-induced dissociation in hydrate-bearing porous media[J]. 中国化学工程学报, 2021, 32(4): 324-334.
[7]	Qihui Hu, Xiaoyu Wang, Wuchang Wang, Yuxing Li, Shuai Liu. Growth and aggregation micromorphology of natural gas hydrate particles near gas-liquid interface under stirring condition[J]. 中国化学工程学报, 2021, 40(12): 65-77.
[8]	Xueyi Guo, Chenlin Yang, Jinxiu Chen, Qinghua Tian, Hongmei Zhang, Guoyong Huang. Facile synthesis of spinel LiNi_0.5Mn_1.5O₄ as 5.0 V-class high-voltage cathode materials for Li-ion batteries[J]. 中国化学工程学报, 2021, 39(11): 247-254.
[9]	Xuewen Cao, Chenyang Fu, Zhenqiang Xie, Chao Wu, Xiaoyang Sun. Simulation and experimental study on the surface morphology and energy lost of the target material under non-overlapping impact of angular particles[J]. 中国化学工程学报, 2021, 29(1): 47-56.
[10]	Xiaokai Xing, Zhonghua Zhao, Jianhang Wu. Direct image-based fractal characterization of micromorphology of calcium carbonate fouling crystals[J]. 中国化学工程学报, 2020, 28(2): 466-476.
[11]	Xinmei Zhao, Huanhuan You, Faming Gao. DNA-assisted rational design of BaF₂ linear and erythrocyte-shaped nanocrystals[J]. Chinese Journal of Chemical Engineering, 2018, 26(7): 1581-1585.
[12]	Jian Sun, Lisheng Wang, Dongfang Zhao. Polymorph and morphology of CaCO₃ in relation to precipitation conditions in a bubbling system[J]. , 2017, 25(9): 1335-1342.
[13]	Lei Yang, Yangyang Zhang, Hua Li, Hezhou Liu. Controllable synthesis of metallic Bi from commercial Bi₂O₃ via one-pot solvothermal reduction method[J]. , 2017, 25(9): 1202-1206.
[14]	Qi Zhang, Xuhua Yan, Peng Zheng, Zhengbao Wang. Influence factors on activity of Ru-Zn catalysts in selective hydrogenation of benzene[J]. , 2017, 25(3): 294-300.
[15]	Lin Yang, Jianxin Cao, Caiyu Li. Enhancing the hydration reactivity of hemi-hydrate phosphogypsum through a morphology-controlled preparation technology[J]. , 2016, 24(9): 1298-1305.