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Battery grade iron and manganese phosphate and preparation method thereof

An iron manganese phosphate and iron manganese phosphate chemical technology, applied in battery electrodes, circuits, electrical components, etc., can solve the problems of not forming an olivine structure, affecting the electrical properties of products, and affecting the molar ratio, so as to achieve easy large-scale production. , reduce the variety and quantity, and ensure the effect of adjustability

Inactive Publication Date: 2015-04-15
杨志宽
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this invention does not add oxidizing agent or reducing agent, and the substances formed by the reaction are relatively complicated, and phosphates of ferric manganese and ferric iron will not be formed
This will have a great impact on the molar ratio of iron, manganese and phosphorus in the final lithium iron manganese phosphate product, and will not form a stable olivine structure, thereby affecting the electrical properties of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] According to the chemical composition of battery grade iron manganese phosphate Mn 0.1 Fe 0.9 PO 4 , Weigh 251gMn(NO 3 ) 2 4H 2 O, 3634.6gFe(NO 3 ) 3 9H 2 O, 115.29g concentrated phosphoric acid (mass fraction is 85%), join in the reactor of 200L and add deionized water to dissolve completely, add 0.5g sodium hexadecylsulfonate, stir and mix evenly under the speed of 150r / min, Use nitric acid, control the pH value of the system at 3-3.5, control the temperature of the reaction kettle solution to 150°C, continue to stir at a speed of 150r / min for 5h, Mn 2+ Oxidized to Mn by nitric acid 3+ , Mn 3+ and Fe 3+ with PO 4 3- combined to form Mn 0.1 Fe 0.9 PO 4 ·yH 2 O precipitation. get Mn 0.1 Fe 0.9 PO 4 The suspension of yH2O precipitation is naturally cooled to room temperature, and the suspension is filtered and washed with a filter press to obtain a nitrate-free filter cake, which is then roasted at 350°C to remove free water and crystal water. Get ba...

Embodiment 2

[0028] According to the chemical composition of battery grade iron manganese phosphate Mn 0.7 Fe 0.3 PO 4 , weigh 1.76kgMnCl 2 4H 2 O, 1.667kg FeSO 4 ·7H 2 O, 2.30kgNH 4 h 2 PO 4, add deionized water to a 200L reactor to dissolve completely, add 2g cetyl amino acid, stir and mix evenly at a speed of 500r / min, use nitric acid to adjust the pH value of the solution to 1-1.2, and control the temperature of the reactor solution To 200°C, continue to stir at a speed of 500r / min for 40h to obtain Mn-containing 0.7 Fe 0.3 PO 4 ·yH 2 O precipitated suspension, naturally cooled to room temperature, the suspension was filtered and washed with a filter press to obtain a filter cake free of nitrate, sulfate, chloride, ammonium and other impurity ions, and then heated at 500 ° C Roasting at the bottom to remove free water and crystal water to obtain battery-grade Mn 0.7 Fe 0.3 PO 4 .

Embodiment 3

[0030] According to the chemical composition of battery grade iron manganese phosphate Mn 0.4 Fe 0.6 PO 4 , Weigh 1.014kgMnSO 4 ·H 2 O, 3.634kgFe(NO 3 ) 3 9H 2 O, 1.8kgNaH 2 PO 4 , add it to a 200L reactor, add deionized water to dissolve completely, add 1g of cetyl ammonium sulfonate, stir and mix evenly at a speed of 250r / min, use nitric acid to adjust the pH value of the solution at 1.5-2, and control the reactor When the temperature of the solution reaches 120°C, continue to stir at a speed of 250r / min to carry out the reaction for 20h to obtain a solution containing Mn 0.4 Fe 0.6 PO 4 ·yH 2 O precipitated suspension, cooled naturally to room temperature, the suspension was filtered and washed with a filter press to obtain a filter cake free of impurity ions, and then roasted at 650 ° C to remove free water and crystal water to obtain Battery grade Mn 0.4 Fe 0.6 PO 4 .

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PUM

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Abstract

The invention relates to battery grade iron and manganese phosphate and a preparation method thereof. The chemical composition of the battery grade iron and manganese phosphate is MnxFe(1-x)PO4, wherein x is greater than or equal to 0.1 and smaller than or equal to 0.9; the preparation method comprises the steps of adopting a hydrothermal oxidation-coprecipitation technology, putting a soluble phosphorus source, iron source and manganese source solution into a reaction kettle according to the chemical composition MnxFe(1-x)PO4 of the iron and manganese phosphate, adding a surfactant and nitric acid, controlling the system pH value to be within 1 to 4, stirring for 2 to 48 h at 100 to 250 DEG C, so as to perform hydrothermal reaction, obtaining turbid liquid containing MnxFe(1-x)PO4.yH2O precipitate, naturally cooling the turbid liquid to room temperature, filtering, washing and drying, obtaining MnxFe(1-x)PO4.yH2O, performing high-temperature roasting at 250 to 700 DEG C, and then obtaining the battery grade iron and manganese phosphate not containing crystal water. The method is simple and practicable, and is easy to realize scale production, the prepared iron and manganese phosphate has the advantages that size distribution is uniform, the purity is high, and iron and manganese elements realize atomic-scale uniform distribution, and the battery grade iron and manganese phosphate a belongs to the optimal precursor for preparing lithium ferric manganese phosphate battery materials.

Description

technical field [0001] The invention belongs to the field of new energy materials, and particularly prepares battery-grade iron-manganese phosphate through an oxidation-co-precipitation process under the condition of a hydrothermal method, which is the best precursor for preparing lithium iron-manganese phosphate cathode materials. Background technique [0002] Lithium iron phosphate batteries have been widely used in new energy vehicles, large-scale energy storage and other fields due to their high safety, no pollution, long life and other characteristics. Compared with battery materials such as lithium cobalt oxide, lithium manganese oxide, and nickel-cobalt lithium manganese oxide, lithium iron phosphate with an olivine structure has attracted attention due to its safety, long cycle life, and low cost. Automobiles have become popular, and they have been vigorously promoted in major cities with government subsidies. The backup power supply of wind power generation energy ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCH01M4/5825Y02E60/10
Inventor 杨志宽
Owner 杨志宽
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