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Multi-ion doped battery-grade iron phosphate material and preparation method thereof

An ion doping, iron phosphate technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry and other directions, can solve the problem of not effectively improving doping uniformity, and achieve improved electrochemical performance and energy utilization efficiency, The effect of strong operability, excellent discharge capacity and cycle performance

Pending Publication Date: 2022-07-15
BTR (TIANJIN) NANO MATERIAL MFG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The electrical properties of lithium iron phosphate can be improved by doping, but the doping uniformity cannot be effectively improved

Method used

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  • Multi-ion doped battery-grade iron phosphate material and preparation method thereof
  • Multi-ion doped battery-grade iron phosphate material and preparation method thereof
  • Multi-ion doped battery-grade iron phosphate material and preparation method thereof

Examples

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Effect test

Embodiment A1

[0027] A method for preparing a multi-ion doped battery-grade iron phosphate material, comprising the following steps:

[0028] (1) add 1000L pure water in the reaction kettle, add 300kg technical grade ferrous sulfate heptahydrate, be warming up to the temperature of 60 ℃, add 2.5kg reduced iron powder, hydrolysis reaction 3 hours, adjust pH to 4.5~5.0, then Add 0.5kg ammonium fluoride and ammonium sulfide (mass ratio 1:1) mixture, add 0.05% mass fraction of cationic polyacrylamide 2L after 1 hour of reaction, stir well and filter; add 55% mass fraction of hydrogen to the filtrate dropwise 2 L of hydrofluoric acid, stirred and incubated at 60°C for 2 hours and filtered; 4 L of 85% phosphoric acid was added to the filtrate under stirring, and after stirring for 2 hours, let stand for 2 hours, and filtered to obtain a pure ferrous sulfate solution; It is 6kg metatitanic acid and 6kg ammonium metavanadate; add 180L hydrogen peroxide with a mass fraction of 27.5% in the above-men...

Embodiment A2

[0031] A method for preparing a multi-ion doped battery-grade iron phosphate material, comprising the following steps:

[0032](1) add 1000L pure water in the reaction kettle of , add 300kg technical grade ferrous sulfate heptahydrate, be warming up to temperature is 60 ℃, add 2.5kg reduced iron powder, hydrolysis reaction is 3 hours, pH is adjusted to 4.5~5.0, Then add 0.5kg of ammonium fluoride and ammonium sulfide (mass ratio 1:1) mixture, add 0.05% mass fraction of cationic polyacrylamide 2L after 1 hour of reaction, stir well and filter; add 55% mass fraction to the filtrate dropwise 2 L of hydrofluoric acid, stirred and incubated at 60°C for 2 hours and filtered; 4 L of 85% phosphoric acid was added to the filtrate under stirring, and after stirring for 2 hours, let stand for 2 hours, and filtered to obtain a pure ferrous sulfate solution; Add 9kg of metatitanic acid and 9kg of ammonium metavanadate; add 180L hydrogen peroxide with a mass fraction of 27.5% in the above-m...

Embodiment A3

[0035] A method for preparing a multi-ion doped battery-grade iron phosphate material, comprising the following steps:

[0036] (1) add 1000L pure water in the reaction kettle of , add 300kg technical grade ferrous sulfate heptahydrate, be warming up to temperature is 60 ℃, add 2.5kg reduced iron powder, hydrolysis reaction is 3 hours, pH is adjusted to 4.5~5.0, Then add 0.5kg of ammonium fluoride and ammonium sulfide (mass ratio 1:1) mixture, add 0.05% mass fraction of cationic polyacrylamide 2L after 1 hour of reaction, stir well and filter; add 55% mass fraction to the filtrate dropwise 2 L of hydrofluoric acid, stirred and incubated at 60°C for 2 hours and filtered; 4 L of 85% phosphoric acid was added to the filtrate under stirring, and after stirring for 2 hours, let stand for 2 hours, and filtered to obtain a pure ferrous sulfate solution; Add 9kg metatitanic acid and 12kg ammonium metavanadate; add 180L hydrogen peroxide with a mass fraction of 27.5% in the above-menti...

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Abstract

The invention provides a multi-ion doped battery grade iron phosphate material and a preparation method thereof, the iron phosphate material is prepared by a one-step synthesis method, drying and dehydration, the mass ratio of doped V ions is 0.2%-0.5%, and the mass ratio of doped Ti ions is 0.2%-0.5%. According to the present invention, the iron phosphate preparation process is simple, the operability is strong, the doped particles of the prepared multi-ion doped battery grade iron phosphate material are reduced, the specific surface area is increased, the chemical activity is improved, the grinding efficiency during the lithium iron phosphate preparation process is improved, and the co-doping of V and Ti does not change the crystal form structure of the iron phosphate, optimizes the crystal structure, and further improves the lithium iron phosphate preparation efficiency. The diffusion impedance of lithium ions is reduced, the exchange current density is increased, and the conductivity of a material body is improved. And multiple ions are doped into iron phosphate crystal lattices, so that the interplanar spacing is increased, Li < + > de-intercalation is facilitated, the transfer rate of lithium ions among particles is increased, the impedance among the particles is reduced, the exchange current density is increased, and the electrochemical performance of lithium iron phosphate is improved.

Description

technical field [0001] The invention belongs to the technical field of electrode material synthesis, in particular to a multi-ion-doped battery-grade iron phosphate material and a preparation method thereof. Background technique [0002] Lithium Iron Phosphate (LiFePO 4 ) as a new-generation lithium-ion battery cathode material with a theoretical specific capacity of 170mAh g -1 , the actual specific capacity of the product can exceed 140mAh / g (0.2C, 25℃), and the voltage platform is 3.4V (relative to Li / Li + ), has the advantages of low price, good thermal stability, and does not contain any heavy metal elements that are harmful to human body, environmental protection, high safety, it also has excellent cycle performance, under 100% deep discharge conditions, can be charged and discharged 2000 times above. Therefore, lithium iron phosphate is considered to be an ideal cathode material for lithium-ion batteries. At present, the preparation of lithium iron phosphate mostl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
CPCC01B25/375C01P2004/62C01P2004/61C01P2006/12C01P2006/40C01P2002/52
Inventor 朱振文席小兵石洪建张威孙禾孟少敏刘又勇
Owner BTR (TIANJIN) NANO MATERIAL MFG CO LTD
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