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Battery-grade ferric orthophosphate as well as preparation method and application thereof

An iron orthophosphate, battery-level technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of poor low-temperature performance, unclear crystal structure, and disjointed preparation of lithium iron phosphate, and achieve good fluidity and packaging The effect of excellent coating effect and excellent low temperature performance

Inactive Publication Date: 2020-10-30
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Domestic ferric orthophosphate technology is based on the early low-level ceramic-grade and food-grade product models, which have problems of fluctuating purity and unclear crystal structure, and many manufacturers are out of touch with the preparation of positive electrode materials in the stage of product and technology development. Can solve the defect of poor low temperature performance of lithium iron phosphate from the source

Method used

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  • Battery-grade ferric orthophosphate as well as preparation method and application thereof
  • Battery-grade ferric orthophosphate as well as preparation method and application thereof
  • Battery-grade ferric orthophosphate as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A battery grade ferric orthophosphate, which is prepared as follows:

[0028] S1, in the kettle that is equipped with 2.2mol / L ferrous sulfate solution and is continuously stirred at a frequency of 75Hz, a peristaltic pump is used to add a concentration of 80% phosphoric acid solution at a flow rate of 50L / h. After the addition, stir for 3.5h, and then Use a peristaltic pump to inject 22% ammonia water at a flow rate of 110L / h and adjust the pH value of the reaction solution to 2.2, control the temperature of the reaction system to 80°C, and then use a gas flow meter to 3 The flow rate / h added concentration is 2.5×10 5 ppm ozone, finally add flocculant ferric sulfate, after complete addition, stir for 3.5h, and let stand for 1.2h after stirring.

[0029] S2, then press-filter and wash the reaction product in S1 to obtain ferric phosphate dihydrate;

[0030] S3. Physicochemically granulate ferric phosphate dihydrate, calcining at 620° C. for 4.5 hours to obtain anhydro...

Embodiment 2

[0035] A battery grade ferric orthophosphate, which is prepared as follows:

[0036] S1. Use a peristaltic pump to add a phosphoric acid solution with a concentration of 75% at a flow rate of 40L / h to the kettle equipped with 2mol / L ferrous sulfate solution and continuously stirred at a frequency of 70Hz. After the addition, stir for 3h, and then use peristaltic The pump injects 20% sodium hydroxide at a flow rate of 100L / h and adjusts the pH value of the reaction solution to 2.0, controls the temperature of the reaction system to be 75°C, and then uses a gas flow meter to 3 The flow rate / h added concentration is 2×10 5 ppm ozone, finally add the flocculant ferric chloride, stir for 3 hours after complete addition, and let stand for 1 hour after stirring.

[0037] S2, then press-filter and wash the reaction product in S1 to obtain ferric phosphate dihydrate;

[0038] S3. Physicochemically granulate ferric phosphate dihydrate, calcining at 600° C. for 4 hours to obtain anhydr...

Embodiment 3

[0041] A battery grade ferric orthophosphate, which is prepared as follows:

[0042]S1. Use a peristaltic pump to add a phosphoric acid solution with a concentration of 85% at a flow rate of 60L / h into a kettle equipped with a 2.5mol / L ferrous sulfate solution and continuously stirred at a frequency of 80Hz. After the addition, stir for 4h, and then use The peristaltic pump injects 25% sodium hydroxide with a flow rate of 120L / h and adjusts the pH value of the reaction solution to 2.5, controls the temperature of the reaction system to be 85°C, and then uses a gas flow meter to 3 The flow rate / h added concentration is 3×10 5 ppm ozone, finally add flocculant ferric sulfate, after complete addition, stir for 4 hours, and let stand for 1.5 hours after stirring.

[0043] S2, then press-filter and wash the reaction product in S1 to obtain ferric phosphate dihydrate;

[0044] S3. Physicochemically granulate ferric phosphate dihydrate, calcining at 650° C. for 5 hours to obtain an...

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Abstract

The invention discloses battery-grade ferric orthophosphate as well as a preparation method and application thereof, and relates to the energy storage material technical field. The preparation methodcomprises the following steps: adding a phosphoric acid solution into a ferrous sulfate solution, stirring, adjusting the pH value of a reaction system to 2.0-2.5, controlling the temperature of the reaction system to 75-85 DEG C, introducing a gas oxidant, then adding a flocculating agent, stirring, and aging after the reaction is completed; carrying out filter pressing and washing on the reaction product to obtain iron phosphate dihydrate; and carrying out physicochemical granulation and calcination on the iron phosphate dehydrate to obtain the anhydrous ferric orthophosphate. The ferric orthophosphate is prepared by adopting a coprecipitation method, and ultrafine iron phosphate particles with small particle size and narrow particle size distribution are prepared by utilizing the characteristics of low solubility, high nucleation speed, low growth speed and easiness in obtaining high-dispersion colloid of the ferrous phosphate through the steps of controlling the pH and temperatureof the reaction system, adding the flocculating agent, ageing and the like. The lithium iron phosphate material prepared from the iron phosphate shows excellent low-temperature performance.

Description

technical field [0001] The invention relates to the technical field of energy storage materials, in particular to a battery-grade ferric orthophosphate and a preparation method and application thereof. Background technique [0002] With the wide application of lithium iron phosphate lithium ion batteries in new energy vehicles, wind energy storage, communication base stations, large database storage and other industries, the production and manufacturing of lithium iron phosphate cathode materials have also been vigorously developed. There are a variety of technological routes for the preparation of lithium iron phosphate cathode materials, and the technical routes that have been industrialized include iron oxide red route, oxalate ferrous route, hydrothermal synthesis route, and orthophosphate iron route. After the practice and verification of the industry and market after 2012, the lithium iron phosphate prepared by the orthophosphate railway line has outstanding advantages...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37C01B25/45H01M4/58
CPCC01B25/375C01B25/45H01M4/5825H01M2004/028C01P2004/32C01P2004/62C01P2004/80C01P2006/40Y02E60/10
Inventor 万宁李萍萍陈峰汪伟伟杨茂萍
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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