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Preparation method of battery grade iron phosphate micropowder

An iron phosphate, battery-grade technology, applied in battery electrodes, secondary batteries, chemical instruments and methods, etc., can solve the problems of poor product quality stability, unstricken temperature control requirements, etc., to prevent product particle size from being too large, particle size Evenly distributed, fine-grained effect

Inactive Publication Date: 2017-06-23
河南省净寰新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method of ferric phosphate that has been publicly reported at present generally uses an ordinary kettle-type reactor, and the requirements for temperature control and post-reaction material liquid treatment are not strict, resulting in poor product quality stability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A preparation method of battery-grade iron phosphate micropowder, comprising the following steps:

[0022] (1), according to the amount of substance P:Fe=0.7~1.3 and H 2 o 2 : The ratio of Fe=0.5~0.55, take FeSO 4 、Na 2 HPO 4 and H 2 o 2 ,spare;

[0023] (2), the FeSO 4 Add deionized water to dissolve completely, so that the concentration of iron ions in the solution is 0.5mol / L, then add surfactant and mix evenly to form solution A, the amount of surfactant added is 0.1% of the theoretically generated iron phosphate mass;

[0024] (3), the Na 2 HPO 4 Add deionized water to dissolve completely, use phosphoric acid to adjust the pH value to 1, and the total concentration of the solution is 0.1mol / L to obtain solution B;

[0025] (4), the H 2 o 2 Add it into deionized water to make the solution concentration reach 10%, and obtain solution C;

[0026] (5) Add solution A and solution B into the reactor, stir and heat up, when the temperature rises to 55°C, add ...

Embodiment 2

[0029] A preparation method of battery-grade iron phosphate micropowder, comprising the following steps:

[0030] (1), according to the amount of substance P:Fe=0.7~1.3 and H 2 o 2 : The ratio of Fe=0.5~0.55, take FeCl 2 , NH 4 h 2 PO 4 and H 2 o 2 ,spare;

[0031] (2), the FeSO 4 Add deionized water to dissolve completely, so that the concentration of iron ions in the solution is 2.0mol / L, then add surfactant and mix evenly to form solution A. The amount of surfactant added is 5% of the theoretically generated iron phosphate mass;

[0032] (3), the Na 2 HPO 4 Add deionized water to dissolve completely, use phosphoric acid to adjust the pH value to 2, the total concentration of the solution is 1mol / L, and obtain solution B;

[0033] (4), the H 2 o 2 Add it into deionized water to make the solution concentration reach 30%, and obtain solution C;

[0034] (5) Add solution A and solution B into the reactor, stir and heat up, when the temperature rises to 75°C, add s...

Embodiment 3

[0037] A preparation method of battery-grade iron phosphate micropowder, comprising the following steps:

[0038] (1), according to the amount of substance P:Fe=0.7~1.3 and H 2 o 2 : The ratio of Fe=0.5~0.55, take FeCl 2 、K 2 HPO 4 and H 2 o 2 ,spare;

[0039] (2), the FeSO 4 Add deionized water to dissolve completely, so that the concentration of iron ions in the solution is 1.0mol / L, then add surfactant and mix evenly to form solution A, the amount of surfactant added is 2% of the theoretically generated iron phosphate mass;

[0040] (3), the Na 2 HPO 4 Add deionized water to dissolve completely, use phosphoric acid to adjust the pH value to 1, the total concentration of the solution is 0.5mol / L, and obtain solution B;

[0041] (4), the H 2 o 2 Add it into deionized water to make the solution concentration reach 20%, and obtain solution C;

[0042] (5) Add solution A and solution B into the reactor, stir and heat up, when the temperature rises to 70°C, add solut...

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Abstract

The invention relates to a preparation method of battery grade iron phosphate micropowder. The preparation method comprises the following steps: (1) taking an iron raw material, a phosphorus raw material and H2O2; (2) adding the iron raw material into deionized water, and then adding a surfactant to form a solution A; (3) adding the phosphorus raw material into the deionized water and adjusting the pH to 1-2 to obtain a solution B; (4) adding H2O2 into the deionized water to obtain a solution C; (5) adding the solution A and the solution B into a reactor, stirring and heating the solution to 55-75 DEG C, and adding the solution C into the reactor; and (6) after reaction, performing separation, washing and water removal on the surface to obtain the battery grade iron phosphate micropowder. According to the preparation method provided by the invention, the reaction is controlled to be quickly performed at specific pH and temperature, and the iron phosphate micropowder is quickly crystallized and quickly grows. As a result of quickness of the reaction and the demand of the product on index control, a lithium ion battery anode material precursor, iron phosphate powder, which is uniform in granular distribution and fine in granules can be prepared.

Description

technical field [0001] The invention relates to the technical field of preparation of positive electrode materials for lithium batteries, in particular to a method for preparing battery-grade iron phosphate micropowder. Background technique [0002] For lithium-ion batteries, its wide application mainly depends on the battery's capacity, charge and discharge performance, price and safety. The further improvement of the performance of lithium-ion batteries depends to a large extent on the improvement of the performance of cathode materials, and the reduction of the manufacturing cost of lithium-ion batteries also depends on the reduction of the cost of cathode materials to a large extent. Therefore, the development of positive electrode materials with excellent performance, price and safety has become the focus of lithium-ion battery research. As an important member of lithium-ion batteries, lithium iron phosphate batteries have unparalleled advantages and are known as the s...

Claims

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Application Information

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IPC IPC(8): C01B25/37H01M4/58H01M10/0525
CPCC01B25/375H01M4/5825H01M10/0525Y02E60/10
Inventor 孔令师任宏伟蒋志昌周景龙刘鑫桢
Owner 河南省净寰新能源科技有限公司