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Method for preparing spherical lithium manganate

A spherical lithium manganate and oxalic acid technology, applied in chemical instruments and methods, lithium compounds, electrode manufacturing, etc., can solve the problems of poor sphericity and particle size distribution of reaction products, poor reaction process stability, and difficult to guarantee product morphology. , to achieve the effect of improving specific capacity and high temperature cycle performance, good morphology and good sphericity

Inactive Publication Date: 2008-05-21
BYD CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The disclosed method of above-mentioned CN1447464A is by manganese salt with OH - (alkaline aqueous solution) precipitation, after drying, obtain spherical trimanganese tetraoxide as the precursor of spherical lithium manganate for the preparation of lithium-ion battery anode materials, wherein when carrying out precipitation reaction with alkaline aqueous solution, the reaction process stability is relatively poor, It is necessary to control the pH value of the reaction solution more precisely to obtain the trimanganese tetraoxide precursor with better sphericity. If the pH value deviates from the control range, the product morphology is difficult to guarantee
In addition, the amount of complexing agent used in this method is on the low side, which may cause the precipitation reaction to proceed too quickly, so that the sphericity and particle size distribution of the reaction product are not good

Method used

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  • Method for preparing spherical lithium manganate
  • Method for preparing spherical lithium manganate
  • Method for preparing spherical lithium manganate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Prepare 1 mol / L manganese nitrate aqueous solution, 2 mol / L oxalic acid aqueous solution, and 2 mol / L ethylenediamine aqueous solution. The three solutions were continuously pumped with a plunger pump at the same speed of 6ml / min into a 10 liter stirred reactor pre-filled with 3 liters of deionized water, and the reaction temperature was controlled to 70°C under continuous stirring. After 3 hours of reaction, the solid-liquid mixture in the reactor began to overflow naturally. After 10 hours, the liquid was stopped and the stirring was continued for 1 hour. The solid-liquid mixture obtained from the reaction was collected for solid-liquid separation, and the solid obtained was washed with deionized water , And then dried to obtain spherical manganese oxalate precursor.

[0034] Weigh 200 grams of lithium carbonate and put it in a ball mill, add 600 ml of ethanol to it, and ball mill for 2 hours to obtain a paste. The paste was completely transferred to a beaker with a volum...

Embodiment 2

[0037] Prepare 3 mol / L manganese sulfate aqueous solution, 1 mol / L sodium oxalate aqueous solution, and 1.5 mol / L ethylenediamine aqueous solution. The three solutions were continuously pumped with a plunger pump into a 12-liter stirred reactor pre-filled with 3 liters of deionized water, and the pumping speeds were: manganese sulfate solution 2ml / min, sodium oxalate solution 10ml / min, ethylenediamine solution 10ml / min, continuous stirring, control the reaction temperature to 60℃, after about 4 hours of reaction, the solid-liquid mixture in the reactor begins to overflow naturally, stop feeding after 10 hours, continue to stir and settle For 1 hour, the solid-liquid mixture obtained from the reaction was collected, and solid-liquid separation was performed. The obtained solid was washed with deionized water and then dried to obtain a spherical manganese oxalate precursor.

[0038] Weigh 200 grams of lithium hydroxide and put it into a ball mill, add 700 ml of ethanol to it, and ba...

Embodiment 3

[0041] A mixed aqueous solution containing 0.8 mol / L of manganese chloride and 1 mol / L of acetic acid is prepared, and a 2.5 mol / L of ammonium oxalate aqueous solution is prepared. The two solutions were continuously pumped with a plunger pump into a stirred reactor with a volume of 10 liters pre-filled with 3 liters of deionized water, and the pumping speeds were: manganese chloride / acetic acid mixed solution 7.5ml / Min, 5ml / min of ammonium oxalate solution, stirring continuously, controlling the reaction temperature to 55℃, after about 5 hours of reaction, the solid-liquid mixture in the reactor began to overflow naturally, after 10 hours, stop the liquid feeding, continue to stir and settle for 1 hour, The solid-liquid mixture obtained from the reaction is collected, solid-liquid separation is performed, and the obtained solid is washed with deionized water and then dried to obtain a spherical manganese oxalate precursor.

[0042] Weigh 200 grams of lithium hydroxide into a bal...

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Abstract

This invention relates to a preparation method for a new spherical LiMnO3 as the positive material of Li ionic cells, which applies a spherical manganous oxalate prepared by the flooding method as the precursor to be mixed with LiCO3 or Li(OH)2 to prepare a mash to be dried and baked to get the spherical LiMnCO3.

Description

【Technical Field】 [0001] The invention relates to a preparation method of spherical lithium manganate, in particular to a preparation method of spherical lithium manganate used as a positive electrode material of a lithium ion battery. 【Background technique】 [0002] The materials that can be used as the positive electrode of lithium-ion batteries mainly include embedded compounds formed by lithium and transition metal elements, such as layered Li x MO 2 Structure and spinel Li x M 2 O 4 Structured oxides (M = Co, Ni, Mn, Cr and other transition metals), of which LiNiO is more studied 2 , LiCoO 2 And LiMn 2 O 4 . At present, almost all commercial lithium-ion batteries use LiCoO 2 Used as cathode material, LiCoO 2 Cobalt has high specific energy, good cycle performance, simple preparation process, but poor safety performance and expensive cobalt, limited resources, and large pollution. Therefore, it is urgent to find alternative materials. LiNiO 2 Although its specific energy is h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/04H01M4/48H01M4/58C01G1/02C01G45/00C01D15/00H01M4/505
CPCY02E60/12Y02E60/10
Inventor 荣强姜占锋刘会权孙美红
Owner BYD CO LTD