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WO2012045211A1 - Procédé de fabrication d'un matériau d'électrode positive à base d'un double sel de phosphate ferreux de lithium et matériau d'électrode positive obtenu - Google Patents

Procédé de fabrication d'un matériau d'électrode positive à base d'un double sel de phosphate ferreux de lithium et matériau d'électrode positive obtenu Download PDF

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Publication number
WO2012045211A1
WO2012045211A1 PCT/CN2010/077619 CN2010077619W WO2012045211A1 WO 2012045211 A1 WO2012045211 A1 WO 2012045211A1 CN 2010077619 W CN2010077619 W CN 2010077619W WO 2012045211 A1 WO2012045211 A1 WO 2012045211A1
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WIPO (PCT)
Prior art keywords
lithium
iron
ferrous
solution
phosphate
Prior art date
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Ceased
Application number
PCT/CN2010/077619
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English (en)
Chinese (zh)
Inventor
赵林治
李中东
李荣富
冯祥明
李春生
赵培正
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HENAN HUANYU GROUP CO Ltd
Original Assignee
HENAN HUANYU GROUP CO Ltd
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Publication date
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Priority to PCT/CN2010/077619 priority Critical patent/WO2012045211A1/fr
Publication of WO2012045211A1 publication Critical patent/WO2012045211A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00—Phosphorus; Compounds thereof
    • C01B25/16—Oxyacids of phosphorus; Salts thereof
    • C01B25/26—Phosphates
    • C01B25/45—Phosphates containing plural metal, or metal and ammonium
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the invention relates to a novel method for preparing lithium ferrous phosphate double salt cathode material by using iron filings, phosphoric acid and lithium hydroxide, belonging to the field of new energy materials.
  • Lithium-ion secondary battery is a new generation of green energy. It is mainly composed of three materials: positive electrode, negative electrode and electrolyte. It has the advantages of high energy density, high cycle performance, low self-discharge rate, no memory effect and wide operating temperature range. It has been widely used in mobile phones, laptops, video cameras, power tools, etc., and is rapidly entering the field of electric vehicles.
  • LiCo0 2 , LiNi0 2 , LiMn 2 0 4 . 1 ⁇ 0 ⁇ 2 is a relatively large-scale commercialized cathode material.
  • the research is mature and the comprehensive performance is excellent, but the price is high and the capacity is low.
  • LiNi0 2 has lower cost and higher capacity, but it is difficult to prepare, and the consistency and reproducibility of material properties are poor, and there are serious safety problems.
  • Spinel LiMn 2 0 4 has low cost and good safety, but its capacity is low.
  • the Tahti- Teller effect occurs during deep discharge, which affects the stability of the material structure and the high temperature cycle performance of the material.
  • the layered LiMn0 2 has a large specific capacity, but it belongs to the thermodynamic metastable state, the structure is unstable, and there is a Jahn-Teller effect and the cycle performance is poor.
  • Layered LiNi x Co y Mn 1-xy 0 2 series materials such as LiNi 1/3 Co 1/3 Mn 1/3 0 2 better combine the advantages of the three, make up for their respective shortcomings With high specific capacity, low cost, stable cycle performance and good safety performance, it is a strong competitor for the next generation of lithium ion battery cathode materials, but there are still many industrial synthesis processes, poor preparation repeatability, powder The filling property of the body is not ideal, and the expensive Ni and Co elements have a high proportion.
  • the Goodenough working group found that the olivine olivine structure of LiFeP0 4 has an oxidation-reduction potential of 3.4 V, good cycle performance, and a theoretical capacity of 170 mAh/g, which has attracted great interest from scientists and many companies.
  • the olivine structure of LiFeP0 4 I has stable voltage, excellent platform characteristics, high capacity, stable structure, high temperature performance and cycle performance, safety, non-toxicity and low cost. From the current development situation, and from the long-term perspectives of cost performance, resources and environment, LiFeP0 4 is a promising cathode material for a new generation of lithium ion secondary batteries.
  • the object of the present invention is to provide a novel method for preparing a lithium ferrous phosphate double salt cathode material which has a long life, a low tap density and a low specific capacity, which is prepared from iron filings, phosphoric acid and lithium hydroxide.
  • the invention provides a novel method for preparing lithium ferrous phosphate double salt cathode material by using iron filings, phosphoric acid and lithium hydroxide, which comprises the following steps:
  • the phosphoric acid solution reacts with the iron filings.
  • the pH of the reaction solution is 1.5, the specific gravity is 1.25 ⁇ 1.32, the reaction liquid is collected; under the inert gas protection condition, the reaction liquid is concentrated by vacuum evaporation, and the crystal is cooled to obtain solid dihydrogen phosphate.
  • Iron and mother liquor
  • the solid dihydrogen phosphate is dissolved in water to obtain solution B under inert gas protection conditions, and the solution B is sufficiently reacted with the lithium hydroxide solution to form a colloidal suspension C;
  • the suspension D is spray-dried to obtain a lithium iron phosphate precursor E;
  • the lithium iron phosphate precursor E is calcined twice under a weak reducing atmosphere, the first calcination temperature is 450-500 ° C, and the second calcination temperature is 650-750 ° C, and the ferrous iron is directly obtained.
  • Synthetic lithium ferrous iron phosphate double salt microcrystals and ferric iron pyrolysis carbon reduction method lithium ferrous phosphate double salt crystallites and pyrolytic carbon crystallites uniformly mixed lithium ion battery cathode material.
  • a novel method for preparing a lithium ferrous phosphate double salt cathode material using iron filings, phosphoric acid or lithium hydroxide according to the present invention the concentration of the phosphoric acid solution is 2.7 to 3.2 moles / liter.
  • a novel method for preparing a lithium ferrous phosphate double salt cathode material using iron filings, phosphoric acid or lithium hydroxide according to the present invention the temperature at which the phosphoric acid solution reacts with the iron filings is maintained at 50 to 70 °C.
  • a novel method for preparing a lithium ferrous phosphate double salt cathode material using iron filings, phosphoric acid, and lithium hydroxide according to the present invention the solid ferrous dihydrogen phosphate, the lithium hydroxide, the iron hydroxide, and pyrolytic carbon
  • the molar ratio is (1.00): (2.00-2.05): (0.96-1.00): (0.9-1.8).
  • the invention discloses a novel method for preparing a lithium ferrous phosphate double salt cathode material by using iron filings, phosphoric acid and lithium hydroxide:
  • the weak reducing atmosphere is a mixed gas of 5-15% hydrogen and 95-85% nitrogen or argon or 100 parts of ammonia decomposition gas and 400 to 67 parts of a mixed gas of nitrogen or argon.
  • the pyrolytic carbon source is selected from any one of sucrose, glucose, citric acid, starch, and polyvinyl alcohol. kind or any of several.
  • Figure 1 is an X-ray diffraction pattern of a positive electrode material
  • Fig. 2 shows a 18650 type 1200mAh cylindrical lithium ion battery prepared by using a positive electrode material as a positive electrode active material. 1. 0C charge, respectively, 0. 2C, 1C, 5C discharge curve.
  • Figure 3 is a 18650 type 1200mAh cylindrical lithium ion battery prepared by using a positive electrode material as a positive electrode active material. IOC discharge cycle curve.
  • Scrap iron scraps Scrap iron scraps from hardware factories producing battery components in the battery industry, porous scrap iron strip materials such as Baosteel's BDCK or SPCC: The impurities contained therein are only slightly higher in manganese (Mn ⁇ 0.3%), but manganese is harmless and beneficial. Doping element.
  • the scrap iron scrap is filled from the top feed port to the vertical reactor, and the 2.9 mol/L phosphoric acid solution enters from the lower part of the reactor until the full immersion iron scrap is near the upper reaction liquid overflow port, and the 2.9 mol/L phosphoric acid solution is commercially available.
  • % phosphoric acid and water are mixed according to a volume ratio of 1:4; the jacket is heated to keep the temperature of the lower part of the reactor at 50-60 ° C.
  • the reaction liquid flows from the upper reaction liquid overflow port (10 cm lower than the liquid surface) through the solid-liquid separator to continuously remove the solid impurities, and then continuously flows into the inert gas protection liquid storage tank; the hydrogen generated by the reaction is vented from the top exhaust pipe to the outside, The condensed water in the tube flows back to the reaction tank.
  • reaction liquid Under inert gas protection conditions, the reaction liquid is sucked from the liquid storage tank into a vacuum evaporator, and concentrated by vacuum evaporation, and the crystal is cooled, centrifuged and dried to obtain solid dihydrogen phosphate and mother liquor, and the separated mother liquid is used for recycling with the phosphoric acid solution. Under the inert gas protection condition, the solid dihydrogen phosphate is redissolved in water to obtain solution B.
  • Fe Chemical analysis knows Fe:
  • the system is in a colloidal suspension C state
  • the colloidal suspension C was added with 25.7 g of sucrose per mole according to the contained ferrous dihydrogen phosphate, and completely dissolved; the colloidal suspension C was continuously added to the original equimolar iron dihydrogen phosphate under stirring. Preparation of the iron hydroxide colloid to obtain a colloidal suspension D;
  • the above molar ratio of solid ferrous dihydrogen phosphate, lithium hydroxide, iron hydroxide and pyrolytic carbon is 1.00: 2.00: 1.00: (0.5+0.4), wherein 0.5 mole of pyrolytic carbon is used for high temperature reduction of ferric iron, 0.4
  • the molar pyrolysis carbon retains the conductive carbon as a product in the product.
  • the colloidal suspension D has a very homogeneous phase.
  • the suspension D was spray-dried to obtain a spherical particle precursor E, and the spray was rapidly dried so that the chemical composition of each spherical particle in the precursor E maintained the uniform consistency of the colloidal suspension D.
  • a weak reducing atmosphere 100 parts by volume of ammonia decomposition gas and 100 parts by volume of nitrogen
  • calcination at 500 ° C for 8 hours and calcination at 700 ° C for 15 hours
  • two reaction principles of the same raw material system were obtained simultaneously to form LiFeP0 4 nanocrystallite particles.
  • the submicron particles uniformly coated and bridged by the pyrolytic carbon, thereby obtaining a lithium ferrous phosphate double salt lithium ion battery cathode material having a high tap density and a high capacity.
  • Fig. 1 is an X-ray diffraction spectrum of a lithium ferrous phosphate double salt cathode material
  • Fig. 2 and Fig. 3 are electrochemical performance diagrams of a lithium ferrous phosphate double salt cathode material. Since the direct synthesis contains ferrous salts and ferric LiFeP0 4 hot synthesis LiFeP0 4 carbon reduction, so that the normal single principle XRD pattern obtained LiFeP0 4 are not identical, but only because LiFeP0 4 orthorhombic a crystalline form of The difference is only in the difference in grain shape and cell parameter values, which is manifested by the fact that the order of the peaks of the strongest diffraction peaks is different.
  • Scrap iron scraps Scrap iron scraps from hardware factories producing battery components in the battery industry, porous scrap iron strip materials such as Baosteel's BDCK or SPCC: The impurities contained therein are only slightly higher in manganese (Mn ⁇ 0.3%), but manganese is harmless and beneficial. Doping element.
  • the scrap iron scrap is filled from the top feed port to the vertical reactor, and the 2.7 mol/L phosphoric acid solution enters from the lower part of the reactor until the full immersion iron scrap is near the upper reaction liquid overflow port, and the 2.7 mol/L phosphoric acid solution is commercially available.
  • reaction liquid flows from the upper reaction liquid overflow port (10 cm lower than the liquid surface) through the solid-liquid separator to remove solid impurities and continuously flows into the inert gas protection liquid storage tank;
  • the hydrogen is vented from the top exhaust pipe to the outside, and the condensed water in the pipe flows back to the reaction tank.
  • reaction liquid Under inert gas protection conditions, the reaction liquid is sucked from the liquid storage tank into a vacuum evaporator, and concentrated by vacuum evaporation, and the crystal is cooled, centrifuged and dried to obtain solid dihydrogen phosphate and mother liquor, and the separated mother liquid is used for recycling with the phosphoric acid solution. Under the inert gas protection condition, the solid dihydrogen phosphate is redissolved in water to obtain solution B.
  • Fe Chemical analysis knows Fe:
  • the colloidal suspension C was added with 50g of sucrose per mole of ferrous phosphate containing hydrogen under stirring and completely dissolved; the colloidal suspension C was continuously added to the original prepared 0.98-fold molar of dihydrogen phosphate.
  • Iron hydroxide colloid obtained colloidal suspension D;
  • LiFeP0 4 is prepared by the high temperature carbon reduction method with Li3 ⁇ 4P0 4 :
  • the colloidal suspension D has a very homogeneous phase. It is known that all components are equimolar Li + +Fe 2+ P0 4 3 _ (synthetic LiFeP0 4 ) and equimolar Li + +Fe 3+ +P0 4 3 _ (synthesis LiFeP0 4 , but the ferric iron is firstly reduced by hot carbon) uniformly mixed multiphase system; spray suspension D is sprayed to obtain spherical particle precursor E, and the spray is rapidly dried to maintain the chemical composition of each spherical particle in the precursor E Uniform consistency of the colloidal suspension D.
  • Example 3 Scrap iron scraps: Waste iron scraps from hardware factories producing battery components in the battery industry, porous scrap iron strip materials such as Baosteel's BDCK or SPCC: the impurities contained therein are only slightly higher in manganese (Mn ⁇ 0.3%), but manganese It is a harmless and beneficial doping element.
  • the scrap iron scrap is filled from the top feed port to the vertical reactor, and the 3.2 mol/L phosphoric acid solution enters from the lower part of the reactor until the full immersion iron scrap is near the upper reaction liquid overflow port, and the 3.2 mol/L phosphoric acid solution is commercially available.
  • the reaction liquid flows from the upper reaction liquid overflow port (10 cm lower than the liquid surface) through the solid-liquid separator to continuously remove the solid impurities, and then continuously flows into the inert gas protection liquid storage tank; the hydrogen generated by the reaction is vented from the top exhaust pipe to the outside, The condensed water in the tube flows back to the reaction tank.
  • the reaction liquid is sucked from the liquid storage tank into a vacuum evaporator, and concentrated by vacuum evaporation, and the crystal is cooled, centrifuged and dried to obtain solid dihydrogen phosphate and mother liquor, and the separated mother liquid is used for recycling with the phosphoric acid solution.
  • the solid ferrous dihydrogen phosphate is redissolved in water to obtain solution B.
  • F e: P 1.4501 mol / L: 2.9588 mol / L, solution B under stirring and dihydrogen phosphate Ferrous (in terms of P0 4 ) 2.02 times mole
  • the lithium hydroxide solution is fully reacted, and the reactions that may occur here are
  • the system is in a colloidal suspension C state
  • the colloidal suspension C was added with 32.8 g of sucrose per mole of ferrous iron dihydrogen phosphate under stirring and completely dissolved;
  • the colloidal suspension C is continuously added to the colloid suspension D which is the newly prepared iron hydroxide colloid containing the equimolar amount of dihydrogen phosphate dihydrogen;
  • the above molar ratio of solid ferrous dihydrogen phosphate, lithium hydroxide, ferric hydroxide and pyrolytic carbon is 1.00: 2.04: 1.00: (0.5+0.65), wherein 0.5 mole of pyrolytic carbon is used for reducing ferric iron, 0.65 mole Pyrolytic carbon retains the conductive carbon in the product as a product.
  • the colloidal suspension D has a very homogeneous phase. It is known that all components are equimolar Li + +Fe 2+ P0 4 3 _ (synthetic LiFeP0 4 ) and equimolar Li + +Fe 3+ +P0 4 3 _ (synthesis a multiphase system in which LiFeP0 4 , but trivalent iron is first reduced by hot carbon);
  • the suspension D was spray-dried to obtain a spherical particle precursor E, and the spray was rapidly dried so that the chemical composition of each spherical particle in the precursor E maintained the uniform consistency of the colloidal suspension D.
  • the carbon is evenly coated and bridged by submicron particles, thereby obtaining a lithium ferrous ferrous phosphate double salt lithium ion battery cathode material with uniform product.
  • the invention discloses a novel method for preparing lithium ferrous phosphate double salt cathode material by using iron filings, phosphoric acid and lithium hydroxide, and is a wet solution solution precipitation method lithium ferrous phosphate double salt crystal nucleus and hot carbon reduction method in the same raw material system.
  • Lithium ferrous iron phosphate complex salt nucleus and conductive agent pyrolyze carbon crystal nucleus, or simultaneously generate co-growth, thereby forming a uniform body of lithium ferrous phosphate double salt microcrystals coated and bridged by pyrolytic conductive carbon, Very good electrical conductivity, electrochemical performance and processing properties.

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

L'invention concerne un procédé de fabrication d'un matériau d'électrode positive à base d'un double sel de phosphate ferreux de lithium et le matériau d'électrode positive obtenu. Le procédé comprend les étapes suivantes : la mise en réaction d'une solution d'acide phosphorique avec des déchets de fer et le recueillement de la solution réactionnelle lorsque le pH de la solution réactionnelle est ≥ 1,5 et la densité de la solution réactionnelle est de 1,25 à 1,32 ; l'évaporation sous vide et la concentration de la solution réactionnelle sous la protection d'un gaz inerte, puis le refroidissement et la cristallisation, afin d'obtenir un dihydro-phosphate ferreux solide et une liqueur mère ; la dissolution du dihydro-phosphate ferreux solide dans de l'eau sous la protection d'un gaz inerte, afin d'obtenir une solution B, la mise en réaction totale de ladite solution B avec une solution d'hydroxyde de lithium, afin d'obtenir une suspension colloïdale C ; l'ajout d'hydroxyde ferrique et d'une source de carbone de pyrolyse dans ladite suspension colloïdale C, afin d'obtenir une solution de suspension D ; le séchage par pulvérisation de ladite solution de suspension D, afin d'obtenir un précurseur E de phosphate de lithium ferreux ; la calcination dudit précurseur E de phosphate de lithium ferreux dans une atmosphère de réduction faible à deux reprises, la température de la première calcination étant de 450 à 500 °C, et la température de la seconde calcination étant de 650 à 750 °C, afin d'obtenir le matériau d'électrode positive à base d'ion lithium. Le procédé assure l'homogénéité du précurseur et du produit. Le produit présente une bonne conductivité et de bonnes propriétés électrochimiques.
PCT/CN2010/077619 2010-10-09 2010-10-09 Procédé de fabrication d'un matériau d'électrode positive à base d'un double sel de phosphate ferreux de lithium et matériau d'électrode positive obtenu Ceased WO2012045211A1 (fr)

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PCT/CN2010/077619 WO2012045211A1 (fr) 2010-10-09 2010-10-09 Procédé de fabrication d'un matériau d'électrode positive à base d'un double sel de phosphate ferreux de lithium et matériau d'électrode positive obtenu

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PCT/CN2010/077619 WO2012045211A1 (fr) 2010-10-09 2010-10-09 Procédé de fabrication d'un matériau d'électrode positive à base d'un double sel de phosphate ferreux de lithium et matériau d'électrode positive obtenu

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110436432A (zh) * 2019-07-22 2019-11-12 贵州大学 一种纳米片状磷酸铁锂颗粒的低温制备方法
CN111326725A (zh) * 2020-03-05 2020-06-23 青海民族大学 一种锂离子有机正极材料、制备方法及应用
CN113086959A (zh) * 2021-02-26 2021-07-09 雅安锂盛新能企业管理中心(有限合伙) 高压实低温型磷酸铁锂材料、锂电池正极片及其制备方法

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CN101552331A (zh) * 2009-05-01 2009-10-07 徐州海天绿色能源科技有限公司 锂离子电池阳极材料磷酸亚铁锂的制备工艺
KR20100019105A (ko) * 2008-08-08 2010-02-18 전남대학교산학협력단 졸-겔법을 이용한 저가형 리튬 2차 전지용 ＬｉＦｅＰＯ4 양극 물질의 제조방법
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CN1706057A (zh) * 2002-10-18 2005-12-07 国立九州大学 二次电池用阴极材料的制备方法和二次电池
KR20100019105A (ko) * 2008-08-08 2010-02-18 전남대학교산학협력단 졸-겔법을 이용한 저가형 리튬 2차 전지용 ＬｉＦｅＰＯ4 양극 물질의 제조방법
WO2010023194A1 (fr) * 2008-08-26 2010-03-04 Basf Se Synhtèse de lifepo4 dans des conditions hydrothermiques
CN101442117A (zh) * 2008-12-22 2009-05-27 上海电力学院 碳包覆磷酸铁锂的制备方法
CN101552331A (zh) * 2009-05-01 2009-10-07 徐州海天绿色能源科技有限公司 锂离子电池阳极材料磷酸亚铁锂的制备工艺

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110436432A (zh) * 2019-07-22 2019-11-12 贵州大学 一种纳米片状磷酸铁锂颗粒的低温制备方法
CN111326725A (zh) * 2020-03-05 2020-06-23 青海民族大学 一种锂离子有机正极材料、制备方法及应用
CN113086959A (zh) * 2021-02-26 2021-07-09 雅安锂盛新能企业管理中心(有限合伙) 高压实低温型磷酸铁锂材料、锂电池正极片及其制备方法
CN113086959B (zh) * 2021-02-26 2022-03-01 云南航开科技有限公司 高压实低温型磷酸铁锂材料、锂电池正极片及其制备方法

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