nav emailalert searchbtn searchbox tablepage yinyongbenwen piczone journalimg journalInfo searchdiv qikanlogo popupnotification paper paperNew
2024, 08, v.39 12-16
二水磷酸铁陈化过程对磷酸铁品质及形貌的影响研究
基金项目(Foundation): 贵州省科技计划项目(黔科合战略找矿[2022ZD006)
邮箱(Email): 18920416836@163.com;
DOI:
摘要:

磷酸铁作为制备磷酸铁锂正极材料的重要前驱体,目前采用硫酸亚铁和磷酸通过均相沉淀法制备,反应后得到无定形磷酸铁,需要进行陈化转晶。陈化过程包含无定型磷酸铁溶解重排以及二水磷酸铁晶型的生长和凝聚,对磷酸铁的品质及形貌影响很大。研究结果表明,经过陈化转晶重排以后的磷酸铁为致密的类球状单斜FePO4·2H2O颗粒。在物料洗涤过程中控制物料与洗涤水质量比为1.0∶1.5、陈化温度70℃、陈化搅拌转速300~500 r/min、补加磷酸至p H 1.5条件下协同调控,可得到低杂质含量、高比表面积的多孔网状结晶体,从而提高下游磷酸铁锂的产品性能。

Abstract:

As an important precursor for the preparation of lithium iron phosphate cathode materials, iron phosphate is currently prepared by homogeneous co-precipitation of ferrous sulfate and phosphoric acid. The amorphous iron phosphate after reaction needs to be aged, which includes dissolution and recrystallization and has great influence on the quality and morphology of iron phosphate. The results show that the aged iron phosphate is compact spheroidal monoclinic FePO4·2H2O particles. After aging at 70 ℃, whose stirring speed is between 300 and 500 r/min and added phosphoric acid to pH 1.5, then washing under 1.5 times water, porous iron phosphate with low impurity and high specific surface area can be obtained, which can serve as an excellent precursor for high-performance lithium iron phosphate.

参考文献

[1]郑俊超,李新海,王志兴,等.制备过程pH值对FePO4·x H2O及LiFePO4性能的影响[J].中国有色金属学报,2008,18(5):867-872.ZHENG J C,LI X H,WANG Z X,et al. Effect of pH value on performance of FePO4·x H2O and LiFePO4in synthesis process[J].The Chinese Journal of Nonferrous Metals,2018,18(5):867-872.

[2] HE W D,LIANG Y C,LIU J N,et al. A facile and low-cost industrial method to optimize LiFePO4[J]. Journal of University of Electronic Science and Technology of China,2016,45(4):659-663.

[3]孙少先,应皆荣.氧化沉淀-陈化晶化法制备FePO4·2H2O及LiFePO4[J].电源技术,2018,42(10):1473-1476.SUN S X,YING J R. Preparation of FePO4·2H2O via oxidizing precipitation followed aging crystallization and downstream products LiFePO4[J]. Chinese Journal of Power Sources,2018,42(10):1473-1476.

[4]陈召勇,王文华,朱华丽,等.沉淀法制备FePO4的形貌控制[J].长沙理工大学学报(自然科学版),2013,10(2):82-88.CHENG Z Y,WANG W H,ZHU H L,et al. Morphology control of FePO4synthesized by co-precipitation[J]. Journal of Changsha University of Science&Technology(Natural Science),2013,10(2):82-88.

[5]张永晴.盐酸法硫铁矿烧渣制备磷酸铁工艺研究[D].武汉:武汉工程大学,2023.ZHANG Y Q. Study on preparation of iron phosphate from pyrite cinder by hydrochloric acid process[D]. Wuhan:Wuhan Institute of Technology,2023.

[6]董虹,叶红齐,韩凯,等.前驱体制备工艺条件对FePO4·2H2O和LiFePO4性能的影响[J].中南大学学报(自然科学版),2014,45(3):695-702.DONG H, YE H Q, HAN K, et al. Effect of precursor preparation condition on FePO4·2H2O and performance of LiFePO4[J]. Journal of Central South University(Science and Technology),2014,45(3):695-702.

[7]郭举,贾双珠.类球形低硫磷酸铁的制备技术研究[J].无机盐工业,2020,52(5):31-34.GUO J,JIA S Z. Study of the method for the preparation of spherical-like and low sulfur FePO4[J]. Inorganic Chemicals Industry,2020,52(05):31-34.

[8] SONG Y N,ZAVALIJ P Y,SUZUKI M,et al. New iron(Ш)phosphate phases:crystal strucyure and elecetrochemical magnetic properties[J]. Inorganic Chemistry:A Research Journal that Includes Bioinorganic,Catalytic,Organometallic,Solid-state,and Synthetic Chemistry and Reaction Dynamics,2002,41(22):5778-5786.

[9]严鹏,谢刚,张春明,等.非晶态磷酸铁的沉淀反应机理及性能[J].电池,2015,45(5):241-243.YAN P,XIE G,ZHANG C M,et al. Precipitation reaction mechanism and performance of amorphous ferric phosphate[J].Battery Bimonthly,2015,45(5):241-243.

[10]李立平,李煜乾.不同晶体类型磷酸铁的制备及电化学性能的研究进展[J].化工技术与开发,2022,51(8):27-32.LI L P, LI Y Q. Research process on preparation and electrochemical properties of several crystal forms of iron phosphate[J]. Technology&Development of Chemical Industry,2022,51(8):27-32

[11]李健,余奔,岳有涛,等.形貌控制剂对磷酸铁振实密度的影响[J].现代机械,2020(2):100-102.LI J,YU B,YUE Y T,et al. Effect of morphology control agent on tap density of iron phosphate[J]. Modern Machinery,2020,(2):100-102.

基本信息:

DOI:

中图分类号:TM912;TQ138.11

引用信息:

[1]盛国臣,彭海南,李绍清等.二水磷酸铁陈化过程对磷酸铁品质及形貌的影响研究[J].生态产业科学与磷氟工程,2024,39(08):12-16.

基金信息:

贵州省科技计划项目(黔科合战略找矿[2022ZD006)

检 索 高级检索

引用

GB/T 7714-2015 格式引文
MLA格式引文
APA格式引文