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WO2025086304A1 - Phosphate de fer modifié, son procédé de préparation et son utilisation - Google Patents

Phosphate de fer modifié, son procédé de préparation et son utilisation Download PDF

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Publication number
WO2025086304A1
WO2025086304A1 PCT/CN2023/127394 CN2023127394W WO2025086304A1 WO 2025086304 A1 WO2025086304 A1 WO 2025086304A1 CN 2023127394 W CN2023127394 W CN 2023127394W WO 2025086304 A1 WO2025086304 A1 WO 2025086304A1
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WO
WIPO (PCT)
Prior art keywords
phosphate
preparation
iron phosphate
zirconium
iron
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/CN2023/127394
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English (en)
Chinese (zh)
Inventor
吴芷菁
李爱霞
谢英豪
余海军
李长东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
Original Assignee
Hunan Brunp Recycling Technology Co Ltd
Guangdong Brunp Recycling Technology Co Ltd
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Filing date
Publication date
Application filed by Hunan Brunp Recycling Technology Co Ltd, Guangdong Brunp Recycling Technology Co Ltd filed Critical Hunan Brunp Recycling Technology Co Ltd
Priority to CN202380011823.1A priority Critical patent/CN117693487B/zh
Priority to PCT/CN2023/127394 priority patent/WO2025086304A1/fr
Publication of WO2025086304A1 publication Critical patent/WO2025086304A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C01B25/37—Phosphates of heavy metals
    • 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
    • C01B25/38—Condensed phosphates
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • 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 present invention belongs to the technical field of battery materials and relates to a modified iron phosphate and a preparation method and application thereof.
  • Lithium iron phosphate a lithium-ion battery material
  • iron phosphate determines the performance of lithium iron phosphate.
  • the existing preparation technologies of iron phosphate include solid phase method, particle size grading method, liquid phase synthesis method, etc.
  • CN105480960A discloses a method for preparing iron phosphate, comprising the following steps: placing iron in a phosphoric acid solution, heating to perform an iron oxidation reaction, and obtaining a reaction liquid containing Fe( H2PO4 ) 2 ; adding hydrogen peroxide to the filtrate of the reaction liquid, performing an oxidation reaction under stirring, and then adding polyethylene glycol and continuing to stir to react Fe( H2PO4 ) 2 to generate iron phosphate, and obtaining an oxidized liquid; adding distilled water to the oxidized liquid to perform a hydrolysis reaction; performing solid-liquid separation on the hydrolyzed liquid, washing the separated solid phase discharge with water until the pH value of the washed liquid reaches a near-neutral value, and drying to obtain solid iron phosphate; and sequentially drying and dehydrating the dried solid iron phosphate to form dehydrated iron phosphate.
  • CN111704121A discloses a method for preparing iron phosphate and lithium iron phosphate, comprising the following steps: S1, preparing an iron source and a phosphorus source, dividing the iron source into two parts F1 and F2, and dividing the phosphorus source into two parts P1 and P2; S2, adding the phosphorus source P1 to the iron source F1, heating to 90-100° C., and keeping the temperature until the material turns white; S3, mixing the iron source F2 with the phosphorus source P2, and adding sulfuric acid to obtain a mixed solution; S4, adding the mixed solution obtained in step S3 to the material treated in step S2, reacting at 90-100° C. for 1-3 hours, and washing the product after the reaction; After calcination, the iron phosphate is obtained.
  • the iron phosphate products obtained by the above scheme mostly present tightly packed secondary agglomerates.
  • greater grinding intensity and longer grinding time are required, which leads to increased costs.
  • the purpose of the present disclosure is to provide a modified iron phosphate and a preparation method and application thereof.
  • the present disclosure uses zirconium phosphotungstate as a seed to prepare iron phosphate, which can promote the generation of secondary particle cracks, make the iron phosphate easier to break, reduce the difficulty of grinding the iron phosphate, and obtain an iron phosphate precursor with a smaller particle size, thereby preparing a high-energy, high-power density lithium iron phosphate positive electrode material.
  • the present invention adopts the following technical solutions:
  • the present disclosure provides a method for preparing modified ferric phosphate, the preparation method comprising the following steps:
  • the modified material is sintered and ground to obtain the modified iron phosphate.
  • the present invention uses zirconium phosphotungstate (Zr 2 WO 4 (PO 4 ) 2 ) as a seed crystal to prepare iron phosphate.
  • zirconium phosphotungstate Zr 2 WO 4 (PO 4 ) 2
  • the core of the iron phosphate precursor can shrink during synthesis and expand after cooling to room temperature, which promotes the appearance of cracks in the secondary agglomerated particles and reduces the grinding intensity and time required for preparing small particles of iron phosphate.
  • the prepared modified iron phosphate is used in the subsequent preparation of lithium iron phosphate.
  • the zirconium and tungsten ions are heated in the lithium iron phosphate sintering process.
  • zirconium ions can be doped into Li ion sites and tungsten ions can be doped into Fe sites, which improves the intrinsic conductivity of the material.
  • the doping of tungsten and zirconium ions can also increase the compaction density of the material.
  • the zirconium salt in step (1) comprises zirconium oxychloride.
  • the hydrogen phosphate includes any one of ammonium hydrogen phosphate, sodium hydrogen phosphate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, sodium dihydrogen phosphate, and disodium hydrogen phosphate, or a combination of at least two thereof.
  • the tungstate salt includes sodium tungstate and/or ammonium tungstate.
  • the molar ratio of zirconium, tungsten and phosphorus in the mixed salt solution of step (1) is (1.8-2.3):1:(2-2.5), for example: 1.8:1:2, 1.9:1:2.1, 2:1:2.2, 2.1:1:2.4 or 2.3:1:2.5, etc.
  • the mixing time in step (1) is 15 to 30 minutes, for example, 15 minutes, 18 minutes, 20 minutes, 25 minutes or 30 minutes.
  • the mixing in step (1) of the present disclosure may be a mixture of zirconium salt, hydrogen phosphate and tungstate with a solvent, or zirconium salt, hydrogen phosphate and tungstate may be separately prepared into solutions in advance and then mixed.
  • the heating reaction in step (1) comprises a microwave hydrothermal reaction.
  • the temperature of the heating reaction is 100-150°C, for example, 100°C, 110°C, 120°C, 140°C or 150°C.
  • the heating reaction time is 20 to 40 minutes, for example, 20 minutes, 25 minutes, 30 minutes, 35 minutes or 40 minutes.
  • the heating reaction is followed by vacuum drying.
  • the vacuum drying treatment is carried out at a temperature of 50 to 80°C, for example, 50°C, 55°C, 60°C, 70°C or 80°C.
  • the vacuum drying treatment time is 12 to 24 hours, for example: 12 hours, 15 hours, 18 hours, 20 hours or 24 hours.
  • the median particle size D50 of the zirconium phosphotungstate is 100-200 nm, for example, 100 nm, 120 nm, 140 nm, 160 nm, 180 nm or 200 nm.
  • the iron salt in step (2) includes any one of ferrous sulfate, ferrous chloride or ferrous oxalate, or a combination of at least two thereof.
  • the phosphate includes any one of sodium phosphate, potassium phosphate or ammonium phosphate, or a combination of at least two thereof.
  • the oxidant includes any one of hydrogen peroxide, sodium peroxide, peracetic acid or ammonium persulfate, or a combination of at least two thereof.
  • the molar ratio of the oxidant to the iron element in the iron source is (1-2):1, for example: 1:1, 1.2:1, 1.5:1, 1.8:1 or 2:1, etc.
  • the mixing in step (2) includes mixing an iron salt solution with an oxidant, adding phosphoric acid to adjust the pH, adding zirconium phosphotungstate seed crystals, and then adding a phosphate solution.
  • the concentration of the iron salt solution is 0.5-1.5 mol/L, for example, 0.5 mol/L, 0.8 mol/L, 1 mol/L, 1.2 mol/L or 1.5 mol/L.
  • the pH is 1 to 3, for example, 1, 1.5, 2, 2.5 or 3.
  • the concentration of the phosphate solution is 0.5-1.5 mol/L, for example, 0.5 mol/L, 0.8 mol/L, 1 mol/L, 1.2 mol/L or 1.5 mol/L.
  • the molar ratio of the iron element in the iron salt solution to the phosphorus element in the phosphate solution is 1:(1-1.5), for example: 1:1, 1:1.1, 1:1.2, 1:1.4 or 1:1.5, etc.
  • the temperature of the synthesis reaction in step (2) is 80-100°C, for example, 80°C, 85°C, 90°C, 95°C or 100°C.
  • the synthesis reaction time is 1 to 3 hours, for example: 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours.
  • the sintering temperature in step (3) is 400-700°C, for example, 400°C, 450°C, 500°C, 600°C or 700°C.
  • the sintering treatment time is 3 to 6 hours, for example: 3 hours, 3.5 hours, 4 hours, 5 hours or 6 hours.
  • the grinding time is 1 to 3 hours, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours.
  • the present disclosure provides a modified iron phosphate, wherein the modified iron phosphate is prepared by the method described in the first aspect.
  • the median particle size D50 of the modified ferric phosphate is 0.5-1 ⁇ m, for example, 0.5 ⁇ m, 0.6 ⁇ m, 0.8 ⁇ m, 0.9 ⁇ m or 1 ⁇ m.
  • the modified iron phosphate disclosed in the present invention is subjected to grinding treatment to obtain modified iron phosphate particles with a median particle size of 0.5 to 1 ⁇ m, and a good crushing effect, which also indirectly illustrates the characteristic that the modified iron phosphate prepared in the present application is easy to crush.
  • the present disclosure provides a lithium iron phosphate positive electrode material, wherein the lithium iron phosphate positive electrode material is prepared by mixing and sintering the modified iron phosphate as described in the second aspect and a lithium source.
  • the present invention has the following beneficial effects:
  • the present invention uses zirconium tungstate phosphotungstate as a seed crystal to prepare iron phosphate, which can promote the generation of secondary particle cracks, making the iron phosphate easier to break, reducing the difficulty of grinding the iron phosphate, and obtaining an iron phosphate precursor with a smaller particle size, thereby preparing a high-energy, high-power density lithium iron phosphate positive electrode material.
  • the compacted density of the modified iron phosphate prepared by the method disclosed in the present invention can reach above 2.57 g/cm 3 , and the 0.1C discharge capacity of the battery prepared can reach above 156.33 mAh/g.
  • the outer layer of the iron phosphate precursor prepared in the present invention is coated with a small amount of zirconium phosphotungstate, which can limit the growth of lithium iron phosphate particles during the synthesis of lithium iron phosphate, which is conducive to obtaining lithium iron phosphate with a smaller particle size.
  • Iron-lithium cathode material Iron-lithium cathode material.
  • FIG. 1 is a SEM image of modified iron phosphate prepared in Example 1 of the present disclosure.
  • This embodiment provides a modified iron phosphate, and the preparation method of the modified iron phosphate is as follows:
  • the modified iron phosphate is used to prepare a lithium iron phosphate positive electrode material, and the D50 of the obtained lithium iron phosphate positive electrode material is about 1 ⁇ m.
  • This embodiment provides a modified iron phosphate, and the preparation method of the modified iron phosphate is as follows:
  • This embodiment provides a modified iron phosphate, and the preparation method of the modified iron phosphate is as follows:
  • microwave hydrothermal in step (1) is replaced by conventional hydrothermal, and the other conditions and parameters are exactly the same as those in embodiment 1.
  • ferrous phosphate was used as a seed crystal to prepare modified iron phosphate, and other conditions and parameters were exactly the same as those in Example 1.
  • the D50 of the obtained modified iron phosphate was 3 ⁇ m, and the lithium iron phosphate positive electrode material was prepared using the modified iron phosphate, and the D50 of the obtained lithium iron phosphate was 5 ⁇ m.
  • Example 1 The only difference between this comparative example and Example 1 is that the ball milling time is 5 h, and the other conditions and parameters are exactly the same as those in Example 1.
  • Example 1 The only difference between this comparative example and Example 1 is that no zirconium source is added, and other conditions and parameters are exactly the same as those in Example 1.
  • Example 1 The only difference between this comparative example and Example 1 is that no tungsten source is added, and other conditions and parameters are exactly the same as those in Example 1.
  • the iron phosphate prepared in the embodiment and the comparative example is mixed with lithium hydroxide and glucose, and the molar ratio of lithium to iron phosphate is 1 to 1.1: 1.
  • the mass of glucose is 2 to 5% of the mass of the theoretically synthesized lithium iron phosphate;
  • the mixed material is placed in a sintering device, and a protective or reducing gas is introduced at a gas flow rate of 0.08 L/min.
  • the temperature is raised from room temperature to 700°C at a rate of 4°C/min, and the temperature is kept for 10 hours.
  • the temperature in the furnace is naturally lowered to room temperature to obtain LiFePO 4 /C.
  • the prepared LiFePO 4 /C was mixed with the conductive agent acetylene black and the binder polyvinylidene fluoride PVDF at a mass ratio of 90:5:5, and N-methylpyrrolidone NMP was used as a solvent.
  • the mixture was evenly coated on aluminum foil, dried, and rolled to form a simulated battery positive electrode.
  • the negative electrode was a metal lithium sheet
  • the separator was Celgard2400
  • the electrolyte was 1 mol/L LiPF 6 /DMC+DEC (volume ratio was 1:1), forming a CR2025 type simulated battery.
  • the charge and discharge voltage range was 2.9 to 3.7V, and the electrochemical performance data of lithium iron phosphate, a positive electrode material of a lithium-ion battery, was obtained.
  • the test results are shown in Table 1:
  • the compaction density of the modified iron phosphate prepared by the method of the present disclosure can reach more than 2.57 g/cm 3
  • the 0.1C discharge capacity of the prepared battery can reach more than 156.33 mAh/g.
  • Example 4 From the comparison between Example 1 and Example 4, it can be seen that the present disclosure can obtain an iron phosphate precursor with a finer particle size through microwave hydrothermal treatment, which is beneficial to the improvement of compaction density and discharge capacity.
  • Example 1 By comparing Example 1 with Comparative Example 1, it can be seen that the present disclosure uses zirconium phosphotungstate as a seed to prepare iron phosphate.
  • zirconium phosphotungstate As a seed to prepare iron phosphate.
  • the core of the iron phosphate precursor can shrink during synthesis and expand after cooling to room temperature, which promotes cracks in the secondary agglomerated particles and reduces the grinding intensity and time required for preparing small particles of iron phosphate.
  • the crushing and grinding of the secondary agglomerated particles can make part of the zirconium phosphotungstate core coated on the particle surface, which can limit the growth of its particles during the synthesis of lithium iron phosphate, and obtain small particles of lithium iron phosphate positive electrode material.
  • Example 1 From the comparison between Example 1 and Comparative Examples 1-2, it can be seen that the method described in the present application can significantly reduce the accumulation of secondary agglomerates in the iron phosphate product, and lithium iron phosphate particles with smaller particle size can be obtained in a shorter grinding time. Compared with Comparative Example 2, the grinding time is increased (exceeding the grinding time of the present application), but the particle size of the material does not change significantly.
  • zirconium and tungsten ions can The doping of zirconium ions to Li ion sites and tungsten ions to Fe sites improves the intrinsic conductivity of the material. In addition, the doping of tungsten and zirconium ions can also increase the compaction density of the material.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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  • Manufacturing & Machinery (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
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  • Battery Electrode And Active Subsutance (AREA)

Abstract

L'invention concerne un phosphate de fer modifié, son procédé de préparation et son utilisation. La méthode de préparation comprend les étapes suivantes consistant à : (1) mélanger un sel de zirconium, un phosphate d'hydrogène et un tungstate avec un solvant pour obtenir une solution de sel mixte, et effectuer une réaction de chauffage, de façon à obtenir un phosphotungstate de zirconium ; (2) mélanger le phosphotungstate de zirconium servant de germe cristallin avec un sel de fer, un phosphate, de l'acide phosphorique et un agent oxydant, et effectuer une réaction de synthèse, de façon à obtenir un matériau modifié ; et (3) fritter le matériau modifié, puis le broyer, de façon à obtenir du phosphate de fer modifié. Dans la présente divulgation, le phosphotungstate de zirconium est utilisé en tant que germe cristallin pour préparer du phosphate de fer, qui peut favoriser la génération de fissures dans des particules secondaires, ce qui rend le phosphate de fer facile à casser et un précurseur de phosphate de fer présentant une taille de particule plus petite ; par conséquent, un matériau d'électrode positive au phosphate de fer-lithium à haute énergie et à haute densité de puissance est préparé.
PCT/CN2023/127394 2023-10-27 2023-10-27 Phosphate de fer modifié, son procédé de préparation et son utilisation Pending WO2025086304A1 (fr)

Priority Applications (2)

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CN202380011823.1A CN117693487B (zh) 2023-10-27 2023-10-27 一种改性磷酸铁及其制备方法和应用
PCT/CN2023/127394 WO2025086304A1 (fr) 2023-10-27 2023-10-27 Phosphate de fer modifié, son procédé de préparation et son utilisation

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US20120058039A1 (en) * 2010-03-02 2012-03-08 Guiqing Huang HIGH PERFORMANCE CATHODE MATERIAL LiFePO4, ITS PRECURSORS AND METHODS OF MAKING THEREOF
CN102897743A (zh) * 2012-10-30 2013-01-30 东华大学 一种磷酸铁锂纳米材料的制备方法
CN113044823A (zh) * 2021-02-24 2021-06-29 湖南雅城新材料有限公司 一种磷酸铁材料及其制备方法与应用
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WO2022267423A1 (fr) * 2021-06-24 2022-12-29 广东邦普循环科技有限公司 Phosphate de fer nanométrique, son procédé de préparation et son utilisation
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CN115367725A (zh) * 2022-08-29 2022-11-22 广东邦普循环科技有限公司 一种掺杂型磷酸铁锂及其制备方法和应用

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