Method for preparing ferric pyrophosphate used for lithium ion battery by utilizing iron-bearing raffinate

A lithium ion battery, iron orthophosphate technology, applied in battery electrodes, chemical instruments and methods, circuits, etc., can solve the problems of increasing the production cost of iron phosphate, coarse extraction of ferrous salt solution, and low concentration of active ingredients, and saving The effect of raw materials, improving utilization rate and improving production efficiency

Active Publication Date: 2015-11-04
常州锂源新能源科技有限公司
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Problems solved by technology

[0003] The raw material of industrial production iron phosphate usually comprises iron source, phosphorus source, oxidizing agent and lye, iron source usually adopts ferric salt or ferrous salt at present, and the iron source disclosed as CN102491302A and CN102555725B is ferrous sulfate (FeSO 4 ), ferrous chloride (FeCl 2 ), ferric nitrate (FeNO 3 ) and ferric chloride (FeCl 3 ), etc., by adding an oxidant to oxidize the ferrous salt to ferric salt, the disadvantage of this method is the use of non-renewable resources, and the use of ferric salt, oxidant and lye increases the production cost of ferric phosphate
CN104409...

Method used

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  • Method for preparing ferric pyrophosphate used for lithium ion battery by utilizing iron-bearing raffinate

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Effect test

Embodiment 1

[0042] (1) Add hydrogen peroxide solution in the iron-containing raffinate, the quality of the hydrogen peroxide is 10% of the iron-containing raffinate quality, stir for 2h, control the reaction temperature of the solution to be 20°C, and the pH value to be 2; add organic phosphoric acid The extractant P204 is used for multi-stage extraction, the mass ratio of extractant and solution in each stage of extraction tank is 1:200, the extraction temperature is 20°C, the pH value is 2, the extraction is 1h, the organic phase is separated and washed with inorganic acid to obtain iron salt solution;

[0043] (2) Use the iron salt solution recovered in step (1) as an iron source, add phosphoric acid, stir, the reaction temperature is 55 ° C, add a pH regulator to a pH value of 2, react for 2 hours, cool, and then undergo solid-liquid separation and washing 1. Obtain iron orthophosphate powder material for lithium ion battery after drying.

Embodiment 2

[0045] (1) Add sodium hypochlorite solution in iron-containing raffinate, the quality of described sodium hypochlorite is 30% of iron-containing raffinate quality, stir 3h, the reaction temperature of control solution is 40 ℃, pH value is 1.5; Add organophosphoric acid The extractant P507 is used for multi-stage extraction, the mass ratio of extractant and solution in each stage of extraction tank is 1:400, the extraction temperature is 10°C, the pH value is 1.5, the extraction is 1.5h, the organic phase is separated and washed with inorganic acid Obtain iron salt solution;

[0046] (2) Use the iron salt solution recovered in step (1) as an iron source, add ammonium dihydrogen phosphate, stir, the reaction temperature is 65°C, add a pH regulator to a pH value of 2, react for 5 hours, cool, and then undergo solid-liquid After separation, washing and drying, iron orthophosphate powder materials for lithium ion batteries are obtained.

Embodiment 3

[0048] (1) add sodium peroxide solution in iron-containing raffinate, the quality of described sodium peroxide is 100% of iron-containing raffinate quality, stir 5h, the reaction temperature of control solution is 70 ℃, and pH value is 3 Add organic phosphoric acid extractant N290 for multi-stage extraction, the mass ratio of extractant and solution in each stage of extraction tank is 1:800, the extraction temperature is 70°C, the pH value is 1.5, the extraction is 2.5h, and the organic phase is separated through Obtain iron salt solution after mineral acid washing;

[0049] (2) Use the iron salt solution recovered in step (1) as an iron source, add ammonium dihydrogen phosphate, stir, the reaction temperature is 72°C, add a pH regulator to a pH value of 2, react for 8 hours, cool, and then undergo solid-liquid After separation, washing and drying, iron orthophosphate powder materials for lithium ion batteries are obtained.

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Abstract

The invention relates to a method for preparing ferric pyrophosphate used for a lithium ion battery by utilizing iron-bearing raffinate. The method comprises the following steps of (1) adding oxidizing agent solution in the iron-bearing raffinate, stirring, adding the raffinate to carry out multistage extraction, and washing a separated organic phase through inorganic acid to obtain ferric salt solution; and (2) taking the ferric salt solution in the step (1) as an iron source, adding a phosphorus source, stirring, adding a pH regulator to react, cooling, carrying out solid-liquid separation, washing and drying to obtain a battery-level ferric pyrophosphate powder material. According to the method, the ferric salt solution recycled from the iron-bearing raffinate is taken as the iron source to prepare ferric pyrophosphate, so that the scrap metallic iron is recycled to the greatest extent, the economic benefit is improved, the environmental pollution is reduced; the whole preparation process is greatly simplified, and the production cost is reduced.

Description

technical field [0001] The invention relates to the field of lithium-ion battery materials, in particular to a method for iron orthophosphate for lithium-ion batteries, and in particular to a method for preparing iron orthophosphate for lithium-ion batteries by using iron elements recovered from iron-containing raffinate as an iron source method Background technique [0002] Since iron orthophosphate (FePO 4 ) has a rich chemical structure and has a wide range of applications in the fields of lithium-ion battery materials, catalysis, ceramic glass, and agriculture. After market selection and development of R&D technology, lithium iron phosphate (LiFePO 4 ) The mainstream preparation process has gradually shifted from the ferrous oxalate process to the iron phosphate process. The lithium iron phosphate material produced by this method usually has better performance and is suitable for the preparation of high-end lithium battery products. The synthesis process has the follo...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/139C01B25/37
CPCC01B25/375H01M4/139H01M4/5825Y02E60/10
Inventor 王长伟杨顺毅陈万超
Owner 常州锂源新能源科技有限公司
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