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A kind of iron phosphate material and its preparation method and application

A technology of iron phosphate and iron salt, applied in chemical instruments and methods, phosphorus compounds, structural parts, etc., can solve the problems of difficult filtration, precipitation, long process time, and difficulty in ensuring the complete reaction of calcium phosphate powder.

Active Publication Date: 2022-05-06
HUNAN YACHENG NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When this method is applied on a large scale, two production lines for large particle iron phosphate slurry and small particle iron phosphate slurry need to be established at the same time, and the production efficiency is low.
Moreover, the intermediate product of the preparation of small-particle ferric phosphate slurry by this method—ferric hydroxide is a metastable colloid, which not only has a strong adsorption capacity for impurity ions, but is also extremely difficult to filter and precipitate, resulting in a long process time.
In addition, the invention utilizes ferric iron source and calcium phosphate powder to react to prepare large-particle iron phosphate slurry. The reaction conditions are relatively harsh, and it is difficult to ensure that the calcium phosphate powder is completely reacted. The prepared iron phosphate particles are easy to trap calcium phosphate

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  • A kind of iron phosphate material and its preparation method and application
  • A kind of iron phosphate material and its preparation method and application
  • A kind of iron phosphate material and its preparation method and application

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Embodiment 1

[0064] Embodiment 1 of the present invention is: a kind of preparation method of iron phosphate material, comprises the following steps:

[0065] S1. Preparation of iron phosphate slurry Ⅰ:

[0066] Ingredients: Prepare ammonium monohydrogen phosphate solution with a concentration of 1.2mol / L and ferric sulfate solution with a concentration of 0.5mol / L.

[0067] Seed crystal reaction: 49g mass concentration is that the phosphoric acid solution of 80% is diluted with water to 1L as bottom liquid, is added in the reaction kettle; Under the stirring rate of 240rpm, with the feed mode of concurrent flow, 2L ammonium hydrogen phosphate solution (1.2 mol / L) and 2L ferric sulfate solution (0.5mol / L) were added to the reactor; after the addition was completed, the temperature was raised to 88°C, and the reaction was continued at this temperature for 3h to obtain a white slurry; among them, ammonium monohydrogen phosphate The feeding rate of solution and ferric sulfate solution is 30m...

Embodiment 2

[0072] Embodiment 2 of the present invention is: a kind of preparation method of iron phosphate material, comprises the following steps:

[0073] S1. Preparation of iron phosphate slurry Ⅰ:

[0074] Ingredients: prepare ammonium monohydrogen phosphate solution with a concentration of 1.1mol / L and ferric sulfate solution with a concentration of 0.5mol / L.

[0075] Seed crystal reaction: 73.5g mass concentration is that the phosphoric acid solution of 80% is diluted with water to 1L as bottom liquid, is added in the reactor; Under the stirring speed of 200rpm, with the feeding mode of co-current, 2L ammonium hydrogen phosphate solution ( 1.1mol / L) and 2L ferric sulfate solution (0.5mol / L) were added to the reactor; after the addition was completed, the temperature was raised to 88°C, and the reaction was continued at this temperature for 3 hours to obtain a white slurry; among them, monohydrogen phosphate The feed rate of ammonium solution and ferric sulfate solution is 40mL / min...

Embodiment 3

[0080] Embodiment 3 of the present invention is: a kind of preparation method of iron phosphate material, comprises the following steps:

[0081] S1. Preparation of iron phosphate slurry Ⅰ:

[0082] Ingredients: Prepare ammonium monohydrogen phosphate solution with a concentration of 0.65mol / L and ferric nitrate solution with a concentration of 0.5mol / L.

[0083] Seed crystal reaction: 20g mass concentration is that the phosphoric acid solution of 80% is diluted with water to 1L as bottom liquid, is added in the reactor; Under the stirring rate of 200rpm, with the feed mode of co-current, 2L ammonium hydrogen phosphate solution (0.65 mol / L) and 2L ferric sulfate solution (0.5mol / L) were added to the reactor; after the addition was completed, the temperature was raised to 88°C, and the reaction was continued at this temperature for 3h to obtain a white slurry; among them, ammonium monohydrogen phosphate The feeding rate of solution and ferric sulfate solution is 30mL / min.

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Abstract

The invention discloses an iron phosphate material and its preparation method and application. The iron phosphate material is composed of a large-grain iron phosphate material and a small-grain iron phosphate material; the preparation method comprises the following steps: preparing a phosphorus salt raw material solution, The iron salt raw material solution and phosphoric acid solution are mixed, heated and reacted to produce iron phosphate seed crystals; then the iron salt raw material solution and phosphorus salt raw material solution are continuously added for crystallization reaction, so that the ferric phosphate seed crystals grow continuously, and iron phosphate slurry is obtained Ⅰ; mix the iron phosphate slurry I and the iron salt raw material solution, add the phosphate salt raw material solution to react, and obtain the iron phosphate slurry II; press-filter, wash and dry the iron phosphate slurry II to obtain the iron phosphate Material. The process of the invention is simple and can be used in industrialized production, and the method of the invention can control the particle diameter of large particle iron phosphate and the ratio between large particles and small particles. The lithium iron phosphate synthesized by the iron phosphate obtained by the method of the present invention as a precursor has a compacted density exceeding 2.4g / cm 3 .

Description

technical field [0001] The invention relates to the technical field of lithium batteries, in particular to an iron phosphate material and a preparation method and application thereof. Background technique [0002] Lithium batteries made of olivine-structured lithium iron phosphate are widely used in new energy vehicles, communication base stations, energy storage equipment and other fields due to their advantages such as large discharge capacity, long cycle life, high safety, and environmental friendliness. However, the energy density of the battery system using lithium iron phosphate as the cathode material is low, which limits the application of lithium iron phosphate in power batteries. Research and practice have shown that increasing the capacity, voltage platform or compaction density of lithium iron phosphate can effectively increase the energy density of lithium iron phosphate batteries. At present, the capacity and voltage platform of lithium iron phosphate are clos...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37C01B25/45H01M4/58H01M10/052
CPCC01B25/375C01B25/45H01M4/5825H01M10/052H01M2004/028C01P2004/03C01P2004/61C01P2004/62Y02E60/10
Inventor 林奕彭超颜志雄万文治
Owner HUNAN YACHENG NEW MATERIAL CO LTD