Battery-grade iron phosphate, preparation method and application thereof

An iron phosphate, battery-level technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of high enterprise cost, complicated process, environmental pollution, etc., and achieve less impurity content, lower impurity content, and low cost Effect

Pending Publication Date: 2021-04-09
GUANGDONG BRUNP RECYCLING TECH +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the main problems faced by the preparation of ferric phosphate are: 1. The preparation of ferrous phosphate needs to consume a large amount of oxidant, and the cost of the enterprise is high; 2. Due to the small particle size and high viscosity of ferric phosphate, the SO in the product 4 2- Difficult to wash, requires multiple washes Uses a two-step process to produce acceptable impurity content
The ferric phosphate prepared by these methods has high cost and complex process, and if the operation steps are improper, it will also cause pollution to the environment

Method used

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  • Battery-grade iron phosphate, preparation method and application thereof
  • Battery-grade iron phosphate, preparation method and application thereof
  • Battery-grade iron phosphate, preparation method and application thereof

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Embodiment 1

[0051] The preparation method of the battery grade iron phosphate of the present embodiment specifically comprises the following steps:

[0052] (1) 50kg of ferric phosphate dihydrate waste was roasted at 350°C for 3h to remove the crystal water. The roasted material was about 40kg. At 200rpm, the material was put into a sulfuric acid solution kettle with 270L and 1.5mol / L and stirred. Heat to 50°C to dissolve for about 5 hours, then let it stand still, use a precision filter to filter out the filter residue and transfer it to a storage tank to obtain Fe-containing 3+ and PO4 3- The solution, the content of iron and phosphorus in the detection solution is respectively 39.70g / L, 22.36g / L, Fe:P molar ratio=1:1.016;

[0053] (2) Use 10L deionized water as the base solution, which will contain Fe 3+ and PO4 3- The solution and NaOH are injected into the reactor from the bottom of the reactor in parallel at a feeding speed of 7:1, and are fully stirred at a stirring speed of 100...

Embodiment 2

[0061] The preparation method of the battery grade iron phosphate of the present embodiment specifically comprises the following steps:

[0062] (1) 50kg of ferric phosphate dihydrate waste was roasted at 350°C for 3h to remove the crystal water. The roasted material was about 40kg. At 200rpm, the material was put into a 340L, 1.2mol / L sulfuric acid solution tank and stirred. Heat to 50°C to dissolve for about 5 hours, then let it stand still, use a precision filter to filter out the filter residue and transfer it to a storage tank to obtain Fe-containing 3+ and PO4 3- solution, the content of iron and phosphorus in the detection solution is respectively 41.05g / L, 23.55g / L, Fe:P molar ratio=1:1.035;

[0063] (2) 10L deionized water is used as the bottom liquid, which will contain Fe 3+ and PO4 3- The solution and NaOH are injected into the reactor from the bottom of the reactor in parallel at a feed rate of 9:1, and are fully stirred at a stirring speed of 100rpm. The feed ...

Embodiment 3

[0072] The preparation method of the battery grade iron phosphate of the present embodiment specifically comprises the following steps:

[0073] (1) 50kg of ferric phosphate dihydrate waste was roasted at 350°C for 3h to remove the crystal water. The roasted material was about 40kg. At 200rpm, the material was put into a 340L, 1.2mol / L sulfuric acid solution tank and stirred. Heat to 40°C and dissolve for about 5 hours, then let it stand still, use a precision filter to filter out the filter residue and transfer it to a storage tank to obtain Fe-containing 3+ and PO4 3- solution, the content of iron and phosphorus in the detection solution is respectively 41.74g / L, 24.26g / L, Fe:P molar ratio=1:1.048;

[0074] (2) 10L deionized water is used as the bottom liquid, which will contain Fe 3+ and PO4 3- The solution and NaOH are injected into the reactor from the bottom of the reactor in parallel at a feed rate of 8:1, and are fully stirred at a stirring speed of 100rpm. The feed...

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Abstract

The invention belongs to the field of battery materials, and discloses battery-grade iron phosphate, a preparation method and application thereof. The preparation method comprises the following steps: roasting iron phosphate waste, adding into acid liquor, dissolving, and filtering to obtain a solution A containing an iron element and a phosphorus element; stirring the solution A and alkali liquor, adjusting the pH value to be acidic, and reacting to obtain iron phosphate slurry; heating the iron phosphate slurry, adding phosphoric acid, stirring for aging reaction, washing and filtering to obtain an iron phosphate dihydrate filter cake, and drying to obtain iron phosphate dihydrate powder; and roasting, dehydrating and cooling the iron phosphate dihydrate powder to obtain the battery-grade iron phosphate. According to the invention, recovered ferrophosphorus waste is used as a raw material, NaOH is used for precipitating amorphous iron phosphate, phosphoric acid is used as an aging agent under the high-temperature stirring condition, and battery-grade iron phosphate with the impurity content smaller than or equal to 1.0% is prepared through a one-step method.

Description

technical field [0001] The invention belongs to the field of battery materials, and in particular relates to a battery-grade iron phosphate and its preparation method and application. Background technique [0002] Lithium iron phosphate batteries are widely used because of their good safety performance, long cycle life, low price, and abundant raw material reserves without causing too much pollution to the environment. Iron phosphate is an important precursor material in the production of lithium iron phosphate battery cathode materials, and its quality will directly affect the performance of lithium iron phosphate batteries. In the current technology, it has been reported that ferrous salt is used as the iron source, and hydrogen peroxide is added as the oxidant to oxidize ferrous iron to ferric iron, which needs to consume more hydrogen peroxide as the oxidant, which increases the production cost and reduces the enterprise benefit. . Others disclose a regeneration method...

Claims

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Application Information

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IPC IPC(8): C01B25/37H01M4/58
CPCC01B25/375H01M4/5825C01P2006/80C01P2006/82C01P2006/11C01P2006/12C01P2004/62C01P2004/61Y02E60/10
Inventor 秦存鹏殷磊刘更好阮丁山李长东
Owner GUANGDONG BRUNP RECYCLING TECH
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