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A kind of preparation method of battery grade ferric phosphate hydrate

A hydrated phosphoric acid, battery-level technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of limited raw material sources, iron source and phosphorus source raw material purity requirements are very high, to expand raw material sources, reduce cost The cost of auxiliary materials and the effect of reducing supersaturation

Active Publication Date: 2021-12-14
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the one hand, lithium iron phosphate and iron phosphate are the final two-phase structure in the charging and discharging process of lithium iron phosphate. When iron phosphate is used to prepare lithium iron phosphate, the structure and morphology of iron phosphate affect the performance of the final product, so the shape The preparation of ferric phosphate with controllable appearance is very important; on the other hand, in the process of preparing ferric phosphate hydrate, the existing technology has very high requirements on the purity of raw materials of iron source and phosphorus source, which greatly limits the source of raw materials for the preparation of ferric phosphate hydrate. Controlling the distribution behavior of impurity components in the preparation process of ferric phosphate hydrate is also very important for expanding the source of raw and auxiliary materials for the preparation of ferric phosphate hydrate

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  • A kind of preparation method of battery grade ferric phosphate hydrate
  • A kind of preparation method of battery grade ferric phosphate hydrate
  • A kind of preparation method of battery grade ferric phosphate hydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1 (scheme A):

[0053] Weigh 27.8g ferrous sulfate heptahydrate and dissolve it in 100ml boiled deionized water to form a 1.0mol / L ferrous sulfate solution. Weigh 13.8g ammonium dihydrogen phosphate and dissolve it in 100ml deionized water to form a 1.2mol / L solution. L ammonium dihydrogen phosphate solution, add the ammonium dihydrogen phosphate solution to the reactor containing the ferrous sulfate solution at a certain rate, after adding ammonium dihydrogen phosphate, use 1:1 dilute sulfuric acid to adjust the pH value of the solution 0.1, slowly add 1.5 times the theoretical amount of 30% hydrogen peroxide solution dropwise to oxidize ferrous iron to ferric iron, after the hydrogen peroxide is added dropwise, react at a constant temperature of 50°C for 1.0h, and then raise the temperature of the reaction system to 95°C ℃, constant temperature reflux reaction for 36.0h, the reaction is completed, vacuum filtration, washing and drying to obtain the hydrated...

Embodiment 2

[0055] Embodiment 2 (scheme A):

[0056] Measure 150ml of ferrous sulfate solution produced by dissolving high-purity iron flakes in dilute sulfuric acid, add 1:1 dilute ammonia water to adjust the pH of the solution to 4.2, heat up to 45°C, and react at a constant temperature for 1.0h to hydrolyze and purify to remove impurities such as silicon / aluminum in the solution After standing still, the ferrous sulfate purification solution was obtained by vacuum filtration, and the concentration of ferrous ions in the ferrous sulfate purification solution was measured. Take 100ml of the ferrous sulfate purification solution in a 250ml conical flask, and add 1.2 times the theoretical amount at a certain speed. Ammonium dihydrogen phosphate solution with a concentration of 1.2mol / L, after adding ammonium dihydrogen phosphate, use 1:1 dilute sulfuric acid to adjust the pH value of the solution to 0.45, and slowly add 1.2 times the theoretical amount of 30% hydrogen peroxide dropwise Sol...

Embodiment 3

[0058] Embodiment 3 (scheme B):

[0059] Weigh 278 grams of titanium dioxide by-product ferrous sulfate particles, dissolve in 1000ml pure water, stir until completely dissolved, add 1:1 dilute ammonia water, adjust the pH value of the solution to 4.5, react at a constant temperature of 50°C for 1.5h, and hydrolyze Purify and remove impurity components such as titanium / aluminum / silicon in the solution, and vacuum filter after standing for stratification to obtain ferrous sulfate purification solution. Take 100ml of the above-mentioned ferrous sulfate purification solution in a 250ml conical flask, add 1.2 times the theoretical amount of ammonium dihydrogen phosphate to the above-mentioned ferrous sulfate solution, stir until the ammonium dihydrogen phosphate is completely dissolved, and then adjust the reaction system with concentrated ammonia water pH to 8.5, the temperature was raised to 60° C. for 2.0 h at a constant temperature, and after standing for stratification, the f...

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Abstract

The invention discloses a method for preparing battery-grade hydrated ferric phosphate, including scheme A or B: scheme A: mixing ferrous source solution and phosphorus source solution into a mixed solution, and strictly controlling pH, reaction temperature and time and other conditions, Oxidize ferrous ions and convert them into hydrated ferric phosphate; plan B: first convert the solution of phosphorus source and ferrous source into ferrous phosphate precipitate; Conditions such as reaction temperature and time, the ferrous ion is oxidized and converted into hydrated ferric phosphate. The method can produce battery-grade ferric phosphate hydrate in terms of purity, density, and particle size, and can use chemically pure or low-purity iron source or phosphorus source materials, breaking through the limitations of the prior art on raw material purity requirements, and solving the problem at the same time. The technical defect of the existing hydrated ferric phosphate product is that the tap density is relatively low.

Description

technical field [0001] The invention relates to a method for preparing battery-grade hydrated ferric phosphate, in particular to a method for utilizing high-acidity ionization precipitation technology to realize battery-grade hydrated ferric phosphate with high purity, high tap density and good appearance, belonging to lithium-ion battery materials field of preparation. Background technique [0002] Since it was first reported in 1997 that lithium ions in olivine-structured lithium iron phosphate can be intercalated / extracted and used as cathode materials for lithium-ion batteries, based on the olivine structure (LiMPO 4 , M represents Fe, Mn, Ni, Co, etc.) lithium-ion battery cathode materials, especially LiFePO 4 Cathode materials have the advantages of high safety, long cycle life, and low manufacturing cost, and are one of the most potential cathode materials for lithium-ion batteries. With the application of lithium iron phosphate batteries in new energy vehicles, win...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/32C01P2006/80C01P2004/03C01P2002/72C01P2004/51C01P2006/11
Inventor 周康根胡振光彭长宏陈伟张雪凯江洋吴业惠子李嘉
Owner CENT SOUTH UNIV
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