Method for equal molar preparation of lithium iron phosphate by hydrothermal method

A lithium iron phosphate, equimolar technology, applied in the field of lithium-ion battery cathode materials, can solve the problems of raw material cost waste, high reaction impurity content, complicated operation, etc., and achieve the effect of maintaining charge balance and refining lithium iron phosphate particles

Active Publication Date: 2016-06-15
RIZHAO HUAXUAN NEW ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example: wang et al. (ElectrochemActa, 2005, 50, 14) used a solid-state reaction method to prepare Fe-site-doped cathode material LiFe 0.9 Mg 0.1 PO 4 ; Jin et al. (JPowerSources, 2008, 178) synthesized LiFePO by hydrothermal method 4 , with LiOH, FeSO 4 , H 3 PO 4 As raw material, the molar ratio is 3:1:1, first mix phosphoric acid and ferrous sulfate, add a small amount of distilled water to stir, then add lithium hydroxide solution to the mixed solution, stir and then transfer to the reaction kettle, in the dry box at 180 Heating at ℃ for 5 hours; in this method, lithium source: iron source: phosphorus source is 3:1:1, a large amount of lithium source in the solution neutralizes redundant anions, resulting in waste of raw material costs, and metal iron ions are easy to react with phosphate Agglomeration occurs and precipitates at the bottom of the autoclave, and insufficient contact with lithium ions leads to high content of reaction impurities, high cost and complicated operation

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  • Method for equal molar preparation of lithium iron phosphate by hydrothermal method
  • Method for equal molar preparation of lithium iron phosphate by hydrothermal method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) First weigh 400g of ammonium pyrophosphate and dissolve in 1L of deoxygenated distilled water, and slowly add 1mol of FeSO with electromagnetic stirring 4 ·7H 2 O, heated to 80°C and kept warm for 30min to form mixed solution A;

[0026] (2) Weigh 1molLiH 2 PO 4 , dissolved in 1L deoxygenated distilled water, and stirred to form solution B; LiH 2 PO 4 Weigh the standard as Fe 2+ : Li + =1:1; that is, the ratio of the added substances is the molar ratio Li:Fe:P=1:1:1;

[0027] (3) Mix and stir the mixed solution A and solution B, add it to the high-pressure reactor, and adjust the pH to 6 with 1mol / L ammonia water; feed high-purity nitrogen gas, heat the reactor to 160°C for 6 hours in waves, and cool naturally to At room temperature, filter, wash, dry in a vacuum oven at 80°C for 4 hours, and pulverize to obtain the positive electrode material LiFePO 4 .

[0028] In the prior art, iron ions in the solution easily react with phosphate ions, and agglomerate t...

Embodiment 2

[0032] (1) First weigh 200g of zwitterionic polyacrylamide into 1L of deoxygenated distilled water, and slowly add 1mol of ferrous oxalate with electromagnetic stirring to form a mixed solution A;

[0033] (2) Weigh 1molLiH 2 PO 4 Dissolve in 1L deoxygenated distilled water and stir to form solution B; LiH 2 PO 4 Weigh the standard as Fe 2+ : Li + =1:1; that is, the ratio of the added substances is the molar ratio Li:Fe:P=1:1:1;

[0034] (3) Mix and stir the mixed solution A and solution B, then add it to the high-pressure reactor, adjust the pH to 7 with 1mol / L ammonia water; feed high-purity nitrogen, heat the reactor to 200°C for 4 hours in a wave type, and cool naturally to room temperature, filter, wash, dry in a vacuum oven at 80°C for 4 hours, and pulverize to obtain the positive electrode material LiFePO 4 .

[0035] Wherein the selected iron phosphate stabilizer is zwitterionic polyacrylamide, and the ferrous source is ferrous oxalate. Zwitterionic polyacrylam...

Embodiment 3

[0037] (1) Weigh 200g of soluble starch and dissolve it in 1L of deoxygenated distilled water, heat to 60°C to form gelatinized starch, slowly add 1mol of FeSO with electromagnetic stirring 4 ·7H 2 O, forming a mixed solution A;

[0038] (2) Weigh 1molLiH 2 PO 4 Dissolve in 1L deoxygenated distilled water and stir to form solution B;

[0039] (3) Mix and stir the mixed liquid A and solution B, add it to the high-pressure reactor, and adjust the pH to 8 with ammonia water; feed high-purity argon, heat the reactor to 180°C for 5 hours in a wave manner, cool naturally to room temperature, and filter , washing, drying in a vacuum oven at 80°C for 4 hours, and crushing to obtain the positive electrode material LiFePO 4 .

[0040] Among them, the iron phosphate stabilizer selected is soluble starch. Since the soluble starch is heated and gelatinized and reversed, the starch molecules in the granules stretch and diffuse in all directions, dissolve out of the granules, and the ex...

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Abstract

The invention discloses a method for equal molar preparation of lithium iron phosphate by a hydrothermal method. The method comprises the following steps: (1) dissolving weighed iron phosphate stabilizer into deoxidized distilled water, stirring the deoxidized distilled water and adding an iron ferrous source to form a mixed solution A; (2) dissolving weighed LiH<2>PO<4> at the ratio of Fe<2+> to Li<+> being 1 to 1 to form a solution B; and (3) mixing the mixed solution A with the solution B evenly, adding the mixture to a high-pressure reaction kettle, adjusting the pH to be 6-8, introducing an inert gas, heating the reaction kettle to 160-200 DEG C for heat preservation for 4-6 hours in a wave mode, naturally cooling the reaction kettle to a room temperature, carrying out filtering, washing and vacuum drying to obtain a cathode material LiFePO<4>. The cathode material LiFePO<4> prepared by the method is excellent in performance; and the specific discharge capacity at 0.2C reaches 152mAh / g.

Description

technical field [0001] The invention relates to the field of positive electrode materials for lithium ion batteries, in particular to a method for preparing lithium iron phosphate in equimolar quantities by a hydrothermal method. Background technique [0002] In recent years, the application of lithium-ion batteries in the field of new energy has attracted more and more attention. Subsequently, as one of the core parts of lithium-ion batteries, cathode materials have become a research hotspot. The lithium iron phosphate material has the advantages of wide sources, low cost, low toxicity, easy recycling, good safety performance, long service life and high specific capacity, and is currently one of the most popular and reliable candidate cathode materials. [0003] At present, in many preparation methods and electrochemical performance improvement of lithium iron phosphate, solid-phase method, sol-gel method, hydrothermal method, carbon coating, metal ion doping, etc. occupy a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525
CPCH01M4/5825H01M10/0525Y02E60/10
Inventor 王海峰
Owner RIZHAO HUAXUAN NEW ENERGY
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