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Hydrothermal synthesis method for lithium ferromanganese phosphate anode material of lithium ion battery

A technology of lithium manganese iron phosphate and lithium-ion batteries, which is applied in the direction of battery electrodes, phosphorus compounds, chemical instruments and methods, etc., can solve the problems of not having high capacity and specific energy, and achieve the purpose of increasing specific capacity and specific energy, reducing The effect of cost and great application prospect

Inactive Publication Date: 2011-11-23
朱鸥鹭
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The material has technical problems such as high capacity and specific energy

Method used

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  • Hydrothermal synthesis method for lithium ferromanganese phosphate anode material of lithium ion battery
  • Hydrothermal synthesis method for lithium ferromanganese phosphate anode material of lithium ion battery
  • Hydrothermal synthesis method for lithium ferromanganese phosphate anode material of lithium ion battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Reactor: The effective volume is 1000L, heated by heat conduction oil jacket.

[0039] The first step, hydrothermal synthesis reaction to prepare the basic material LiMn 0.6 Fe 0.4 PO 4 (Li:M:P=3.00:1.00:1.03, x=0.6)

[0040] Weigh 44.5kg or 0.16kmol of FeSO4 ·7H 2 O and 40.56kg or 0.24kmol of MnSO 4 ·H 2 O is dissolved in water and diluted to 400L. After standing for 2 hours, filter with a precision filter to remove a small amount of insoluble matter; weigh 47.5kg of 85% phosphoric acid, which is 0.412kmol of phosphoric acid, and 44.2kg of 1.05kmol of LiOH. h 2 O is dissolved in water and diluted to 400L. Filter with a precision filter for later use.

[0041] Vacuum first, then pass nitrogen gas to purge the reactor to remove the air in it, add water seal to the air outlet to seal the autoclave, open the feeding valve, at room temperature, first add phosphoric acid, then add ferrous sulfate and manganese sulfate mixture. Stirring was started at a speed of 200...

Embodiment 2

[0066] The first step, hydrothermal synthesis reaction to prepare the basic material LiMn 0.8 Fe 0.2 PO 4

[0067] Weigh 2.22kg or 0.008kmol of FeSO 4 ·7H 2 O and 5.41kg or 0.032kmol of MnSO 4 ·H 2 O was dissolved in water and diluted to 400L. After standing for 10 hours, filtered to remove a small amount of insoluble matter; weighed 5.3kg of 85% phosphoric acid (0.046kmol of phosphoric acid), and 5.37kg of 0.128kmol of LiOH·H 2 O is dissolved in water and diluted to 400L. Filter and set aside.

[0068] Vacuum first, then pass nitrogen gas to purge the reactor to remove the air in it, add water seal to the air outlet to seal the autoclave, at room temperature, first add phosphoric acid, then add lithium hydroxide solution. Stirring was started at a speed of 300 rpm, and the mixed solution of ferrous sulfate and manganese sulfate was added into the reaction kettle, and the feeding time was 2 minutes. Then seal the autoclave, set the temperature of the heat transfer oil...

Embodiment 3

[0082] The first step, hydrothermal synthesis reaction to prepare the basic material LiMn 0.3 Fe 0.7 PO 4

[0083] Weigh 40.1kg or 0.144kmol of FeSO 4 ·7H 2 O and 56.76kg or 0.336kmol of MnSO 4 ·H 2 O was dissolved in water and diluted to 400L. After standing for 12 hours, filtered to remove a small amount of insoluble matter; weighed 58.1kg of 85% phosphoric acid (0.504kmol of phosphoric acid), and 62.4kg of 1.49kmol of LiOH·H 2 O is dissolved in water and diluted to 400L. Filter and set aside.

[0084] Vacuum first, then pass nitrogen gas to purge the reactor to remove the air in it, add water seal to the air outlet to seal the autoclave, at room temperature, first add the mixed solution of ferrous sulfate and manganese sulfate into the reactor from the feeding port , then add phosphoric acid, start stirring, the rotating speed is 300rpm, then add lithium hydroxide solution, and the feeding time is 5 minutes. Then seal the autoclave, set the temperature of the heat tr...

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Abstract

The invention relates to a hydrothermal synthesis method for lithium ferromanganese phosphate anode material of a lithium ion battery, belonging to the technical field of lithium ion batteries. The method has the following processing steps of: step 1, preparing LiMnxFe1-xPO4 through a hydrothermal synthesis reaction: mixing an aqueous lithium hydroxide solution, an aqueous ferrous sulfate solution and phosphoric acid under a stirring condition, after sealing, heating to 150 DEG C to 180 DEG C within 0.5 to 2 h, reacting for 0.5-4 h under the pressure of 0.48-1.0 Mpa, cooling to less than 80 DEG C, and filtering; step 2, mixing with organic matters and drying: mixing a wet filter cake with a soluble carbon source organic matter, and carrying out spray drying or expansion drying; and step 3, carrying out carbon-coated processing: roasting LiMnxFe1-xPO4 carbon source compound powder at a temperature between 600 DEG C and 750 DEG C for 4-6 h under an insert gas condition, and cooling to less than 150 DEG C to obtain a carbon-coated lithium ferromanganese phosphate anode material of the lithium ion battery. The hydrothermal synthesis method disclosed by the invention has the advantages of simple and controllable technology, convenience for operation, low cost, high crystallization degree of products, uniform dispersion, high specific capacity, high conservation rate of the cycling capacity, and the like.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, in particular to a hydrothermal synthesis method of lithium manganese iron phosphate, a cathode material of lithium ion batteries. Background technique [0002] At present, the positive electrode materials with olivine structure represented by lithium iron phosphate are characterized by safety, low cost, and environmental friendliness. With the adjustment of the energy structure, the field of energy storage puts forward higher requirements on the performance of cathode materials, that is, materials must not only have high specific capacity, but also have high specific energy. Among the existing methods for modifying lithium iron phosphate, a transition metal is used as a dopant to improve its electrochemical performance. But the resulting material has only one discharge platform. For example, CN1785799A proposes a preparation method of transition element lithium doped lithium iron...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/1397B82Y40/00
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 朱鸥鹭
Owner 朱鸥鹭
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