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Method for preparing spherical iron phosphate for lithium iron phosphate cell material

A lithium iron phosphate battery and manufacturing method technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problem of poor rate discharge performance, low LFP gram capacity, and product quality that does not meet the requirements of battery-grade products, etc. problem, to achieve a highly dispersed and fluid effect

Active Publication Date: 2011-10-05
HUBEI HAOYUAN MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The resulting LFP has low gram capacity, poor rate discharge performance, and the product quality cannot meet the requirements of battery-grade products, so it cannot meet the requirements of LFP battery raw materials.

Method used

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  • Method for preparing spherical iron phosphate for lithium iron phosphate cell material
  • Method for preparing spherical iron phosphate for lithium iron phosphate cell material
  • Method for preparing spherical iron phosphate for lithium iron phosphate cell material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Weigh 1000KG ferrous sulfate crystals, add water to dissolve and filter, transfer to a clean 5000L reactor, fully

[0031] Stir and raise the temperature to about 50 degrees, add about 5KG of acid to stabilize the pH value at about 1.0~2.0, then add 200~350KG of industrial hydrogen peroxide and stir for about 60 minutes to make the solution turn brownish red. Then slowly add industrial ammonia water to adjust the pH value to about 4.5~6, so that iron can form ferric hydroxide precipitation. After continuing to raise the temperature to 80-95 degrees, filter under high pressure (about greater than 10KG pressure) while it is hot, and fully wash the ferric hydroxide filter cake with pure water at about 80 degrees until the pH value of the filter cake is stable at 6-7. The filter cake is transferred to the PP storage tank for use.

[0032] 2. Prepare a 5-18% dilute phosphoric acid solution, transfer it to a 5000L reactor, start stirring at a speed of 80r / min, and raise t...

Embodiment 1

[0041] The ferric phosphate SEM figure that embodiment 1 obtains is as follows image 3 As shown, the laser particle size distribution map of the finished product is as follows Figure 4 shown.

Embodiment 2

[0043] 1. Weigh 800KG iron oxide and 300KG iron flakes, add 30% by-product hydrochloric acid or sulfuric acid 2000KG and heat up to 80~95 degrees to dissolve the iron source. The reaction is accompanied by metathesis reaction, redox reaction and replacement reaction. It can be filtered when it is green, transfer the filtrate to a clean 5000L reactor, stir well and raise the temperature to about 50 degrees, add about 5KG of acid to stabilize the pH value at about 1.0~2.0, and then add industrial hydrogen peroxide 200~ 350KG was fully stirred for about 60 minutes to make the solution turn brownish red. Then slowly add industrial ammonia water to adjust the pH value to about 4.5~6, so that the iron salt forms iron hydroxide precipitation. After continuing to raise the temperature to 80-95 degrees, filter under high pressure (approximately greater than 10KG pressure) while hot, and fully wash the iron hydroxide filter cake with pure water at about 80 degrees until the pH value of ...

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Abstract

The invention relates to a method for preparing spherical iron phosphate for lithium iron phosphate cell material. In the method, sheet iron, scrap iron, inorganic ferric salt, oxide of ferrum or organic iron is used for preparing ultra-pure high-density spherical iron phosphate for lithium iron phosphate cell material. Iron phosphate products produced by using the method have high main content of over 99.5%, extremely low impurity content, high dispersibility and high flowability, and oscillation ratios are all higher than 0.95; size distribution is in a narrow range, wherein D50 is stabilized at about 3 mum; the shapes of the products are shown to be sphere-like under an SEM (Scanning Electron Microscope), XRD (X-Ray Diffraction) also shows that the obtained iron phosphate products are pure phases, namely iron phosphate products with dehydrate structures. TG-DTA (Thermal Gravimetric-Differential Thermal Analysis) proves that iron phosphate produced by using the method disclosed by the invention is standard iron phosphate with two crystal waters.

Description

technical field [0001] The invention relates to a method for manufacturing ultra-high-purity and high-density spherical iron phosphate for lithium iron phosphate battery materials, in particular to a method for preparing ultra-high-purity and high-density spherical iron phosphate for lithium iron phosphate battery materials using common iron sources and phosphorus sources Spherical ferric phosphate method. Background technique [0002] Traditionally, iron phosphate is prepared by directly adding ferrous sulfate or ferric chloride into an oxidizing agent, and adding hydrogen phosphate to the oxidized ferric salt. Its sulfate, potassium, sodium and other impurities and heavy metal impurities (Co, Ni, Pb, etc.) have a high content, and these impurities will directly affect or reduce the battery capacity and rate discharge performance of lithium iron phosphate batteries. In theory, these impurities are as low as possible. The content of sulfate, potassium, sodium, etc. in ferr...

Claims

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Application Information

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IPC IPC(8): C01B25/37
Inventor 常开军
Owner HUBEI HAOYUAN MATERIAL TECH
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