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Method for preparing battery-level ferrous oxalate for production of lithium iron phosphate material

A technology of ferrous oxalate and lithium iron phosphate, which is applied in the direction of battery electrodes, carboxylate preparation, circuits, etc., can solve the problems of insufficient product quality, low LFP gram capacity, and inability to meet the raw material requirements for LFP battery production, etc.

Active Publication Date: 2011-10-26
HUBEI HAOYUAN MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The LFP thus synthesized has low gram capacity and poor rate discharge performance, and the product quality cannot meet the requirements of battery-grade ferrous oxalate products required by lithium iron phosphate, so it cannot meet the raw material requirements for LFP battery production.

Method used

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  • Method for preparing battery-level ferrous oxalate for production of lithium iron phosphate material
  • Method for preparing battery-level ferrous oxalate for production of lithium iron phosphate material
  • Method for preparing battery-level ferrous oxalate for production of lithium iron phosphate material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh 1500Kg of iron filings, add 2500L of industrial by-product 30% hydrochloric acid into a 5000L reactor, heat up to about 90 degrees, the reaction begins to intensify, and a large number of bubbles are generated. After maintaining the reaction liquid level for about 4 hours, the pH reached 2.5~3.5 and the reaction was almost terminated.

[0036] After plate and frame filtration, the iron salt solution is about 25 °Be', and the filtrate is pumped into a 6000L reactor and kept at 55-75 °C for use;

[0037] Prepare an oxalic acid solution with a concentration of 10-30%, filter it through a plate and frame, keep it warm and store it in a PP tank for use.

[0038] Turn on the iron salt stirring, and the stirring speed can be controlled by the frequency converter to about 50r / min, and the oxalic acid solution is quantitatively passed through the metering tank

[0039] (The amount of oxalic acid or oxalate added can be calculated by measuring the ferric ion content in the...

Embodiment 2

[0047] Weigh 1500Kg scrap iron scraps, add 2500L of industrial by-product 30% hydrochloric acid into a 5000L reactor, heat up to about 90 degrees, the reaction begins to intensify, and a large number of bubbles are generated. After maintaining the reaction liquid level for about 4 hours, the pH reached 2.5~3.5. The reaction was almost terminated.

[0048] After plate and frame filtration, the iron salt solution is about 25 °Be', and the filtrate is pumped into a 6000L reactor and kept at 55-75 °C for use;

[0049] Prepare an oxalic acid solution with a concentration of 10-30%, filter it through a plate and frame, keep it warm and store it in a PP tank for use.

[0050] Turn on the iron salt stirring, and control the stirring speed by the frequency converter to about 50r / min, and quantitatively pass the oxalic acid solution through the metering tank (the amount of oxalic acid or oxalate added can be calculated by measuring the ferrous ion content in the iron salt solution ) is s...

Embodiment 3

[0057] After weighing 1000Kg of waste iron oxide and 500KG of iron flakes or iron filings, add 2500L of industrial by-product 30% hydrochloric acid into a 5000L reactor, and raise the temperature to about 90 degrees, the reaction begins to intensify, and a large number of bubbles are generated. The reaction is accompanied by metathesis reactions and redox reactions and displacement reactions. Keeping the reaction liquid level for about 3 hours is faster than simply adding iron flakes, and the pH can reach 3.0~4.5, and the reaction is almost terminated at this time.

[0058] After the reaction solution with this ingredient is filtered through the plate frame, the iron salt solution can reach about 28 °Be', and the filtrate is pumped into a 6000L reactor and kept at 55-75 °C for use;

[0059] Prepare an oxalic acid solution with a concentration of 10-30%, filter it through a plate and frame, keep it warm and store it in a PP tank for use.

[0060] Turn on the iron salt stirring...

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Abstract

The invention discloses a method for preparing battery-level ferrous oxalate for production of a lithium iron phosphate material. The method is characterized by dissolving a iron source through a acid, carrying out a filtering through a plate frame after pH value of the solution is stabilized; then pumping the resulting filtrate in a reactor, followed by adjusting a baume degree of the iron salt solution to 5-30<0>Be<,> and maintaining a temperature of the iron salt solution to 30-120 DEG C; adding a oxalic acid solution or a oxalate solution to the iron salt solution under stirring, carrying out centrifuging or sucking filtering after completing the holding reaction; carrying out pure washing and drying for the filter cake to obtain the battery-level ferrous oxalate having a uniform granularity. The ferrous oxalate products prepared by the present invention has a average main content more than 99.5%, a S content less than and equal to 50 ppm, a Na content less than and equal to 30 ppm, heavy metal contents of Pb, Cd, Cr and the like less than and equal to 10 ppm, contents of Cu, Ca, Mg and Ni less than and equal to 50 ppm, Mn content less than and equal to 200 ppm, a stable D50 of about 3 micrometers, a lamelliform or tip ice-shaped morphology, a polarization ratio more than 0.97, a glossiness and golden yellow appearance, high dispersibility and fluidity.

Description

technical field [0001] The invention relates to a method for manufacturing battery-grade ferrous oxalate used in the production of lithium iron phosphate materials, in particular to a method for producing ferrous oxalate using scrap iron or by-product iron sludge, iron slag and by-product acid or recovered acid using a special production process for A method for producing battery-grade ferrous oxalate from a lithium iron phosphate material. . Background technique [0002] Ferrous oxalate is usually prepared by adding ferrous sulfate, ferrous chloride or ferrous nitrate directly to oxalate or oxalic acid. Its sulfate, potassium, sodium, ammonium 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 f...

Claims

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Application Information

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IPC IPC(8): C07C55/07C07C51/41H01M4/139
CPCY02E60/10
Inventor 常开军
Owner HUBEI HAOYUAN MATERIAL TECH
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