Preparation method of precursor iron phosphate of cathode material lithium iron phosphate of lithium ion battery

A technology for lithium-ion batteries and cathode materials, applied in electrode manufacturing, battery electrodes, circuits, etc., can solve problems such as harsh production conditions, difficult control of product components, and complicated process flow

Inactive Publication Date: 2010-02-03
CENT SOUTH UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

At present, the industrial iron phosphate preparation method is synthesized by high-temperature reaction of ferrite and phosphat

Method used

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  • Preparation method of precursor iron phosphate of cathode material lithium iron phosphate of lithium ion battery
  • Preparation method of precursor iron phosphate of cathode material lithium iron phosphate of lithium ion battery

Examples

Experimental program
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Embodiment 1

[0015] (1) Weigh 55.604g of ferrous sulfate heptahydrate, weigh 23.004g of ammonium dihydrogen phosphate, dissolve it in 0.2L deionized water respectively, stir to dissolve it; mix ferrous sulfate solution and ammonium dihydrogen phosphate solution At the same time, it was added to the reactor at a speed of 800mL / h, and the stirrer was turned on for strong stirring. The reaction temperature was controlled at 80°C, and the reaction time was 0.5h under the condition of a stirring speed of 800r / min, and gray ferrous phosphate was obtained. suspension;

[0016] (2) Take 11.4 mL of hydrogen peroxide and add it to the above suspension, a large amount of white precipitates will appear immediately, continue to react for 0.5 h, and after aging for 6 h, filter and wash repeatedly to obtain the precipitate iron phosphate, which is white in color. The total iron content (Fe) of gained ferric phosphate is 29.8%, P is 16.5%, particle diameter is about 300nm, D 50 = 2.5 μm.

[0017] (3) Pu...

Embodiment 2

[0019] (1) Weigh 55.604g of ferrous sulfate heptahydrate, weigh 23.004g of ammonium dihydrogen phosphate, dissolve it in 2L of deionized water respectively, stir to dissolve it; mix ferrous sulfate solution and ammonium dihydrogen phosphate solution simultaneously Add it into the reactor at a speed of 600mL / h, and turn on the stirrer for strong stirring, control the reaction temperature at 60°C, and under the condition of stirring speed of 1000r / min, the reaction time is 1h to obtain light gray ferrous phosphate suspension;

[0020] (2) Take 15.6 mL of hydrogen peroxide and add it to the above suspension, a large amount of white precipitates will appear immediately, continue to react for 1 hour, and after aging for 8 hours, filter and wash repeatedly to obtain precipitated ferric phosphate, which is light yellow in color. The total iron content (Fe) of gained ferric phosphate is 31.8%, and P is 17.2%, and particle size is about 100nm, D 50 = 1.8 μm.

[0021] (3) Put the iron...

Embodiment 3

[0023] (1) Weigh 55.604g of ferrous sulfate heptahydrate, weigh 23.004g of ammonium dihydrogen phosphate, dissolve it in 0.1L deionized water respectively, stir to dissolve it; mix ferrous sulfate solution and ammonium dihydrogen phosphate solution At the same time, it was added to the reactor at a speed of 1000mL / h, and the stirrer was turned on for stirring, and the reaction temperature was controlled to be 90°C. Under the condition of a stirring speed of 600r / min, the reaction time was 0.3h, and light gray ferrous phosphate was obtained. suspension;

[0024] (2) Take 11.4mL of hydrogen peroxide and add it to the above suspension, a large amount of white precipitates will appear immediately, continue to react for 0.3h, and after aging for 4h, filter and wash repeatedly to obtain precipitate iron phosphate, which is white in color. The total iron content (Fe) of the obtained ferric phosphate is 25.2%, P is 13.7%, particle size is about 1 μm, D 50 = 4.3 μm.

[0025] (3) Acco...

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Abstract

The invention discloses a preparation method of precursor iron phosphate of cathode material lithium iron phosphate of a lithium ion battery, which comprises the following steps: simultaneously addingferrous ion aqueous solution with the concentration of 0.05-2mol/L and phosphate radical aqueous solution into a reactor according to the stoichiometric ratio of ferrous ions and phosphate radical ions of 0.8-1.2: 1 and at the speed of 400-1000mL/h, and reacting for 0.2-2h under the conditions that the reaction temperature is 50-90 DEG C and the stirring speed is 400-1200rpm; adding hydrogen peroxide with excessive stoichiometry and reacting for 0.2-2h, and ageing for 2-8h, filtering, washing and drying to obtain iron phosphate powder with two crystallization water; and in the obtained iron phosphate, the total ferric content (Fe) is 29.5-30.5 percent, the P content is 16.0-16.9 percent, the particle size is 0.1-1Mum, and D50 is 1-5Mum. The invention has simple and convenient operation process, simple device, easy control, low energy consumption, even and fine particle size distribution and high reaction activity and is suitable for preparing the lithium ion battery cathode material lithium iron phosphate.

Description

technical field [0001] The invention relates to a preparation method of iron phosphate, a lithium iron phosphate precursor, which is a cathode material of a lithium ion battery. Background technique [0002] Because of its cheap price and no pollution to the environment, iron phosphate has great advantages as a cathode material for lithium batteries. Prosini et al. obtained amorphous FePO by co-precipitation 4 1.5H 2 O; Hong et al. studied the amorphous FePO 4 synthesis conditions. Croce et al. prepared hexagonal FePO by wet chemical method 4 . FePO 4 2H 2 O is a pink monoclinic crystal, which can be used as a food and feed additive, especially for the preparation of lithium iron phosphate, a cathode material for lithium-ion batteries. At present, the industrial iron phosphate preparation method is synthesized by high-temperature reaction of ferrite and phosphate, which has problems such as complicated process flow, harsh production conditions, and difficult control o...

Claims

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Application Information

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IPC IPC(8): H01M4/04H01M4/58
CPCY02E60/12Y02E60/10
Inventor 张宝张佳峰沈超彭春丽
Owner CENT SOUTH UNIV
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