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Preparation process of a pollution-free and low-cost lithium manganese iron phosphate crystal material

A technology of lithium iron manganese phosphate and crystalline materials, applied in inorganic chemistry, phosphorus compounds, structural parts, etc., can solve the problems of unsolved safety problems, limited energy density, difficult charging and discharging, etc., to achieve synthesis Low cost, increase synthesis cost, improve the effect of overall level

Active Publication Date: 2021-12-14
南阳逢源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

Although the energy density of ternary materials is high, the safety problem has not been well solved so far, and its preparation requires a large amount of rare element cobalt
Although the traditional lithium iron phosphate has a series of advantages such as environmental friendliness, safety, low cost, and long life, its 3.2V voltage limits its energy density.
Although lithium manganese phosphate has an olivine stable structure similar to lithium iron phosphate and has a voltage platform of 4.1V, its conductivity is particularly poor and it is an insulator, which makes it difficult to effectively charge and discharge, which limits its commercial use.

Method used

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  • Preparation process of a pollution-free and low-cost lithium manganese iron phosphate crystal material
  • Preparation process of a pollution-free and low-cost lithium manganese iron phosphate crystal material
  • Preparation process of a pollution-free and low-cost lithium manganese iron phosphate crystal material

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Effect test

Embodiment 1

[0032] A preparation process of pollution-free and low-cost lithium manganese iron phosphate crystal material, comprising the following steps:

[0033] 1) Weigh iron powder, manganese powder and phosphoric acid according to the molar ratio of 0.3:0.7:1, and the diluted concentration of phosphoric acid is 40%;

[0034] 2) Put the substance weighed in step 1) into the acid-resistant reactor to control the temperature of the reaction system between 30°C, feed oxygen to start the pre-reaction, and the reaction time is 24 hours;

[0035] 3) Step 2) Add lithium hydroxide solution after the reaction, lithium hydroxide and phosphoric acid are mixed at a ratio of 1:1, after mixing evenly, the precursor is transferred into an autoclave, and the reaction is sealed. The temperature during the synthesis process is 120-260 ° C, high pressure The pressure of the kettle is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled within 3-24...

Embodiment 2

[0039] A preparation process of pollution-free and low-cost lithium manganese iron phosphate crystal material, comprising the following steps:

[0040] 1) Weigh iron powder, manganese powder, and phosphoric acid according to the molar ratio of 0.5:0.5:1-1.2, and the diluted concentration of phosphoric acid is 35%;

[0041] 2) Put the substance weighed in step 1) into the acid-resistant reactor to control the temperature of the reaction system between 25 and 80°C, feed oxygen to start the pre-reaction, and the reaction time is 18 hours;

[0042] 3) Step 2) After the reaction, add lithium hydroxide solution, lithium hydroxide and phosphoric acid are mixed at a ratio of 1-1.2:1, after mixing evenly, the precursor is transferred into an autoclave, and the reaction is sealed. The temperature during the synthesis process is 120-260°C , the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled within...

Embodiment 3

[0046] A preparation process of pollution-free and low-cost lithium manganese iron phosphate crystal material, comprising the following steps:

[0047] 1) Weigh iron powder, manganese powder, and phosphoric acid according to the molar ratio of 0.4:0.6:1-1.2, and the diluted concentration of phosphoric acid is 30%;

[0048] 2) Put the substance weighed in step 1) into the acid-resistant reactor to control the temperature of the reaction system between 25 and 80°C, feed oxygen to start the pre-reaction, and the reaction time is 18 hours;

[0049]3) Step 2) After the reaction, add lithium hydroxide solution, lithium hydroxide and phosphoric acid are mixed at a ratio of 1-1.2:1, after mixing evenly, the precursor is transferred into an autoclave, and the reaction is sealed. The temperature during the synthesis process is 120-260°C , the pressure of the autoclave is 0.2-4.7MPa, the whole reaction process is continuously dispersed and stirred, the reaction time is controlled within ...

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Abstract

The invention discloses a process for preparing a pollution-free and low-cost lithium manganese iron phosphate crystal material, which is completed through the following steps: select iron powder and manganese powder with high purity, and the particle size is selected between 20 mesh and 20000 mesh; according to a certain quality Select manganese powder, iron powder, phosphoric acid and lithium source solution, after dilution, put them in an acid-resistant reactor and stir to fully react iron powder, manganese powder and phosphoric acid; add lithium source solution to the obtained reaction precursor slurry and stir well , the selected lithium source solution is a soluble lithium source lithium hydroxide or lithium acetate; the obtained slurry is transferred into the reactor to start the hydrothermal reaction; the obtained slurry after the reaction is subjected to solid-liquid separation, and the separated solid lithium manganese iron phosphate Carry out clathrate carbonization annealing treatment, prepare lithium manganese iron phosphate crystal material. Compared with the prior art, the invention has lower cost and convenient process operation, and not only the manufactured lithium manganese iron phosphate crystal material has higher commercial value, but also has no pollution in the manufacturing process and meets the current environmental protection requirements.

Description

technical field [0001] The invention relates to the technical field of chemical material synthesis, in particular to a preparation process of a pollution-free and low-cost lithium manganese iron phosphate crystal material. Background technique [0002] With the rapid development of electric vehicles and the gradual expansion of 3C and energy storage market demand, higher requirements are placed on the energy density of materials. Although the energy density of ternary materials is high, the safety problem has not been well resolved so far, and its preparation requires a large amount of rare element cobalt. Although traditional lithium iron phosphate has a series of advantages such as environmental friendliness, safety, low cost, and long life, its 3.2V voltage limits its energy density. Although lithium manganese phosphate has an olivine stable structure similar to lithium iron phosphate and has a voltage platform of 4.1V, its electrical conductivity is particularly poor, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/45H01M4/58
CPCH01M4/5825C01B25/45C01P2006/40C01P2004/62C01P2004/01C01P2002/72Y02E60/10
Inventor 孙青林魏宏政贾庆煜白兵
Owner 南阳逢源新能源科技有限公司
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