Turbulent flow cycle synthesis and characterization of super-fine lithium phosphate

doi:10.3969/j.issn.0438-1157.2014.03.046

CIESC Journal ›› 2014, Vol. 65 ›› Issue (3): 1099-1103.DOI: 10.3969/j.issn.0438-1157.2014.03.046

Previous Articles Next Articles

Turbulent flow cycle synthesis and characterization of super-fine lithium phosphate

HU Yi¹, AI Changchun², LIU Yang¹, WU Yuanxin^1,3

1 School of Chemical Engineering and Pharmacy, Wuhan Institute of Technology, Wuhan 430073, Hubei, China;
2 National Engineering Research Center for Development and Utilization of Phosphorus Resources, Wuhan Institute of Technology, Wuhan 430073, Hubei, China;
3 Key Laboratory of Novel Chemical Process of Ministry of Education, Wuhan 430073, Hubei, China

Received:2013-07-08 Revised:2013-10-28 Online:2014-03-05 Published:2014-03-05
Supported by:
supported by the National Engineering Research Center for Development and Utilization of Phosphorus Resources (2012-Z001).

紊流循环法合成超细磷酸锂及表征

胡意¹, 艾常春², 刘洋¹, 吴元欣^1,3

1 武汉工程大学化工与制药学院, 湖北武汉 430073;
2 武汉工程大学国家磷资源开发利用工程技术研究中心, 湖北武汉 430073;
3 绿色化工过程省部共建教育部重点实验室, 湖北武汉 430073

通讯作者: 艾常春
作者简介:胡意（1987—），男，硕士研究生。
基金资助:
国家磷资源开发利用工程技术研究中心开放基金项目（2012-Z001）。

Abstract

Abstract: A new technology is proposed for the preparation of lithium phosphate by the co-precipitation method in a turbulent flow cycle equipment. The reaction conditions of lithium hydroxide and phosphoric acid in turbulent flow circulation kettle for the preparation of super-fine lithium phosphate were investigated. X-Ray powder diffraction (XRD), laser granularity instrument, scanning electron microscopy (SEM), specific surface and porosity analyzer and thermal analyzer were used to characterize the crystal structure, particle size distribution, morphology, specific surface area and thermal stability of the products. The lithium phosphate prepared by this method had good thermal stability, a narrow particle size distribution of D₅₀=3.25 mm, and a specific BET surface of 13.38 m²·g^-1. As a uniformly dispersed super-fine powder material, the lithium phosphate is expected to be a highly active raw material of cathode materials for lithium ion battery or an additive for lithium ion battery electrolyte.

Key words: super-fine, lithium phosphate, turbulent flow cycle, characterization

摘要： 采用共沉淀法在紊流循环方式下制备超细磷酸锂的一种新工艺，探索了氢氧化锂和磷酸在紊流循环釜中制备超细磷酸锂的反应条件，用X射线粉末衍射、激光粒度仪、扫描电镜、比表面及孔隙分析仪及热分析仪对产物的晶体结构、粒度分布、外观形貌、比表面积以及热稳定性进行了表征。结果表明该方法制得的磷酸锂热稳定性好，粒度分布窄（D₅₀=3.25 mm），比表面积（BET）为13.38 m²·g^-1，为一种分散均匀的超细粉体材料，可望成为一种高活性的锂离子电池正极材料原材料或电解质添加剂。

关键词: 超细, 磷酸锂, 紊流循环, 表征

CLC Number:

TQ131.11

HU Yi, AI Changchun, LIU Yang, WU Yuanxin. Turbulent flow cycle synthesis and characterization of super-fine lithium phosphate[J]. CIESC Journal, 2014, 65(3): 1099-1103.

胡意, 艾常春, 刘洋, 吴元欣. 紊流循环法合成超细磷酸锂及表征[J]. 化工学报, 2014, 65(3): 1099-1103.

References 21

[1]	Hou Qinglie(侯庆烈), Gu Jianfei(顾建飞). Study on the process for preparing the fluorescent grade lithium phosphate[J]. Inorganic Chemicals Industry (无机盐工业), 2007, 39(3): 47-49
[2]	Niu Ben(牛锛), Man Liying(满丽莹), Qi Enlei(齐恩磊), Wang Lei(王磊). Preparation and characterization of lithium phosphate powder[J]. Sulphur Phosphorus and Bulk Materials Handling Related Engineering (硫磷设计与粉体工程), 2011, 2: 27-28
[3]	Ma Weihua(马卫华), Han Qiaofeng(韩巧凤), Lu Lude(陆路德), Yang Xujie(杨绪杰), Wang Xin(汪信). Study of propylene oxide isomerization catalyst[J]. Fine Chemicals (精细化工), 2002, 19(7): 415-417
[4]	Yin Jinhua(尹进华). The study on the catalyst for the isomerization of propylene oxide[D]. Qingdao: Qingdao University of Science and Technology, 2005
[5]	Ma Weihua(马卫华). The study on the catalyst for the isomerization of propylene oxide[D]. Nanjing: Nanjing University of Science and Technology, 2005
[6]	Zhang Li(张莉). Research of preparation of allyl alcohol by propylene oxide catalytic isomerization[D]. Xi'an: Northwest University, 2007
[7]	Ma Weihua(马卫华), Lu Lude(陆路德), Yang Xujie(杨绪杰), Wang Xin(汪信). Catalytic isomerization of propylene oxide and its kinetics[J]. Chemical Reaction Engineering and Technology (化学反应工程与工艺), 2005, 21(5): 397-401
[8]	Ma Weihua(马卫华), Han Qiaofeng(韩巧凤), Lu Lude(陆路德), Yang Xujie(杨绪杰), Wang Xin(汪信). Preparation of allyl alcohol by isomerization of propylene oxide over lithium phosphate catalysts[J]. Industrial Catalysis (工业催化), 2005, 13(4): 40-44
[9]	Zhang Weixin, Chen Lingling, Yang Zeheng, Peng Jing. An optical humidity sensor based on Li3PO4 hollow nanospheres[J]. Sensors and Actuators B: Chemical, 2011, 155: 226-231
[10]	Zhang Long(张龙), Huang Guosong(黄国松), Hu Hefang(胡和方). Nd3+ doped tetraphosphate glass for microchip laser[J]. Journal of Inorganic Materials (无机材料学报), 2001, 16(6): 1062-1068
[11]	Popovic L, Manoun B, de waal D, Nieuwoudt M K, Comins J D. Raman spectroscopic study of phase transitions in Li3PO4[J]. Journal of Raman Spectroscopy, 2003, 34(1): 77-83
[12]	Andrea Gassmann, Christian Melzer, Heinz von Seggern. The Li3PO4/Al electrode: an alternative, efficient cathode for organic light-emitting diodes[J]. Synthetic Metals, 2012, 161: 2575-2579
[13]	Xiao Jie, Chernova Natasha A, Upreti Shailesh, Chen Xilin, Li Zheng, Deng Zhiqun, Choi Daiwon, Xu Wu, Nie Zimin, Graff Gordon L, Liu Jun, Whittingham M Stanley, Zhang Jiguang. Electrochemical performances of LiMnPO4 synthesized from non-stoichiometric Li/Mn ratio[J]. Phys. Chem. Chem. Phys., 2011, 13: 18099-18106
[14]	Ai Xinping, Li Hai, Li Xiaoyan, Liao Qinlin, Liu Bingdong, Yang Haixi. One step ball-milling synthesis of LiFePO4 nanoparticles as the cathode material of Li-ion batteries[J]. Wuhan University Journal of Natural Sciences, 2006, 11(3): 687-690
[15]	Zhao Shixi, Ding Hao, Wang Yanchao, Li Baohua, Nan Cewen. Improving rate performance of LiFePO4 cathode materials by hybrid coating of nano-Li3PO4 and carbon[J]. Journal of Alloys and Compounds, 2013, 566: 206-211
[16]	Liu Zengcai, Fu Wujun, Andrew Payzant E, Yu Xiang, Wu Zili, Dudney Nancy J, Jim Kiggans, Hong Kunlun, Rondinone Adam J, Liang Chengdu. Anomalous high ionic conductivity of nanoporous β-Li3PS4[J]. Journal of the American Chemical Society, 2013, 135: 975-978
[17]	Gong Changsheng(贡长生). The developing direction and prospect of phosphorous chemical industry in our country[J]. Modern Chemical Industry (现代化工), 2011, 31(9): 4-9
[18]	Ai Changchun, Xiao Yong, Wen wen, Yuan Liangjie. Large scale and environmentally friendly preparation of micro-submicron spherical silica and their surface effect in resin materials[J]. Powder Technology, 2011, 210: 323-327
[19]	Liu Qiaoyun, Xiao Yong, Rong Wen, Yuan Liangjie. Large-scale synthesis of monodisperse 2ZnO·2B2O3·3H2O micro/nano single crystals and their effect in polypropylene[J]. Soft Materials, 2009, 7(2): 67-78
[20]	Ai Changchun, Li Yaoji, Wu Yuanxin. The preparation method of nanometer-clusters structure iron phosphate[P]: CN, 102807203 A. 2012-12-05
[21]	Wu Yuan(伍沅). Properties and application of impinging streams[J]. Chemical Industry and Engineering Progress (化工进展), 2001, 20(11): 8-13

Turbulent flow cycle synthesis and characterization of super-fine lithium phosphate

紊流循环法合成超细磷酸锂及表征

PDF (PC)

Knowledge

Cited

Abstract

Cite this article

share this article

References 21

Related Articles 15

Recommended Articles

Metrics

Comments

[1]	Xiaole HUANG, Fu YANG, Lei HAN, Xing NING, Ruiyu LI, Lingxiao DONG, Husheng CAO, Lei DENG, Defu CHE. 3D characterization of pore structure and seepage simulation of tar-rich coal (long flame coal) [J]. CIESC Journal, 2022, 73(11): 5078-5087.
[2]	Liubin SONG, Yixuan WANG, Yinjie KUANG, Yubo XIA, Zhongliang XIAO. Development and prospect of pivotal materials and technologies in sodium-ion batteries [J]. CIESC Journal, 2022, 73(11): 4814-4825.
[3]	HUANG Zhengliang, WANG Chao, GUO Yanni, YANG Yao, SUN Jingyuan, WANG Jingdai, YANG Yongrong. Investigation of secondary flow in helical coils based on residence time distribution [J]. CIESC Journal, 2021, 72(2): 921-927.
[4]	Zhiguo WANG, Yan FENG, Wenzhe YANG, Conghui ZHANG, Dong LI, Lijun LIU. Thermal conductivity analysis model of porous media based on REV [J]. CIESC Journal, 2020, 71(S2): 118-126.
[5]	Jingfang SUN, Chengyan GE, Dongqi AN, Qing TONG, Fei GAO, Lin DONG. Review on characterization methods of oxygen vacancy in rare earth cerium-based catalysts [J]. CIESC Journal, 2020, 71(8): 3403-3415.
[6]	Changyou YU,Bingbing HE,Yanbo LIU,Baohong HOU,Mingyang CHEN,Junbo GONG. Granulation of spherical particles by crystal agglomeration method [J]. CIESC Journal, 2020, 71(11): 4903-4917.
[7]	Cong ZHANG, Jinbo JIANG, Xudong PENG, Wenjing ZHAO, Jiyun LI. Comparison and correction of CO₂ properties model in critical region [J]. CIESC Journal, 2019, 70(8): 3058-3070.
[8]	Yanpei SONG, Xiuzheng ZHUANG, Hao ZHAN, Nantao WANG, Xiuli YIN, Chuangzhi WU. Investigation on synergistic characteristics of sludge and lignite during co-hydrothermal carbonization [J]. CIESC Journal, 2019, 70(8): 3132-3141.
[9]	ZHANG Shuangzheng, CHEN Guo, SU Pengfei. Preparation and characterization of magnetic cross-linked glucoamylase aggregates [J]. CIESC Journal, 2017, 68(7): 2763-2770.
[10]	HU Yanwei, CHENG Gong, LI Haoran, HE Yurong. Synthesis of SiO₂ nanoparticles by chemical precipitation [J]. CIESC Journal, 2016, 67(S1): 379-383.
[11]	GONG Yanjun, LIU Rugeng, ZHAO Xiaomeng, ZHANG Heng. Review on application of small angle X-ray scattering to synthesis and characterization of zeolite [J]. CIESC Journal, 2016, 67(8): 3146-3159.
[12]	HU Yanjun, MA Wenchao, WU Yanan, CHEN Jiang. Characterization on PAHs distributions in pyrolysis bio-oil from different wastewater sewage sludge [J]. CIESC Journal, 2016, 67(7): 3016-3022.
[13]	WANG Yunfang, BU Changjuan, CHI Zhiming, LI Qian. Adsorption of quinoline on zeolite Al-MCM-41 [J]. CIESC Journal, 2015, 66(9): 3597-3604.
[14]	WANG Xuechuan, REN Jing, QIANG Taotao. Synthesis, characterization and application of sulfonic acid type water-based polyurethane chain extender [J]. CIESC Journal, 2015, 66(2): 834-842.
[15]	LIU Jianhua, SHI Tiejun, LI Ming, XU Guomei, WANG Quan, YU Fu. Synthesis, characterization of single benzoxazine contained bis-DOPO based on bisphenol A and flame retardant performance of its copolymer with epoxy [J]. CIESC Journal, 2015, 66(2): 820-826.