Process for preparing layered lithium manganate

A layered lithium manganate and process technology, applied in manganate/permanganate and other directions, can solve the problems of cumbersome steps, inability to mass-produce, uneven distribution, etc., and achieves simple and fast process operation, short reaction time, Environmentally friendly effect

Inactive Publication Date: 2015-12-16
LIUZHOU HAOXIANGTE SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the processes of layered lithium manganate include hydrothermal method, ion exchange method, solid phase synthesis method, sol-gel method, etc. In these methods, such as solid phase synthesis method, there are insufficient reactions and uneven pr

Method used

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Examples

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preparation example Construction

[0023] The preparation process of the layered lithium manganate of the present invention is described in detail below, which includes:

[0024] MnSO 4 solution and NH 4 HCO 3 The solution is added to the reactor to stir the reaction, and the reaction product is washed and filtered to obtain MnCO 3 ;MnSO 4 The concentration is 0.8—1.2mol / L, NH 4 HCO 3 The concentration is 0.8—1.2mol / L, of which NH 4 HCO 3 The solution is preferably in excess, and a larger concentration can be used to increase the saturation of the solution. The increase of the crystal nucleation rate in the reaction system is much higher than the increase of the crystal formation rate, and the generated precipitate particles are smaller; the solution is added to the reaction The speed of the kettle is 10-14mL / min, which can make the particle distribution smaller; the pH value during the reaction process is controlled to be 7, and the reaction temperature is 50--70°C. Under this temperature condition, the...

Embodiment 1

[0029] 0.8mol / L of MnSO 4 The solution is the base solution, which will be relative to the MnSO 4 The total molar excess of 20% of 1mol / L NH 4 HCO 3 The solution was added to the reaction kettle at a rate of 10mL / min to stir the reaction. The reaction temperature was controlled at 50°C, the stirring speed was 500r / min, and the pH value was 7. After the reaction was completed, it was aged for 2h, then washed and filtered to obtain MnCO 3 , followed by MnCO 3 Calcined at 500°C for 10 h under an oxygen atmosphere, and then mixed the product with Na at a molar ratio of Na to Mn of 1:1 2 CO 3 Mix, and add ethanol as a control agent at a solid-to-liquid mass ratio of 1:1 to ensure a ball-to-material ratio of 30:1; take out the ball-milled material after 1 hour and calcinate it at 700°C for 22 hours under a carbon-reducing atmosphere; then mix the calcined product with LiOH ·H 2 O is added with water and stirred, then placed in an autoclave and sealed; pressurized to 25MPa with...

Embodiment 2

[0031] 1mol / L MnSO 4 The solution is the base solution, which will be relative to the MnSO 4 The total molar excess of 20% of 1.2mol / L NH 4 HCO 3 The solution was added to the reaction kettle at a rate of 12mL / min to stir the reaction, the reaction temperature was controlled at 60°C, the stirring speed was 600r / min, and the pH value was 7. After the reaction was completed, it was aged for 3h, then washed and filtered to obtain MnCO 3 , followed by MnCO 3 Calcined at 550°C for 9h under an oxygen atmosphere, and then mixed the product with Na 2 CO 3 Mix, and add ethanol as a control agent at a solid-to-liquid mass ratio of 3:1 to ensure a ball-to-material ratio of 20:1; after 2 hours, take out the ball-milled material and calcinate it at 720°C for 22 hours under a carbon-reducing atmosphere; then mix the calcined product with LiOH ·H 2 O was added with water and stirred, then placed in an autoclave and sealed; pressurized to 26MPa within 13min, heated to 370°C, and reacted...

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Abstract

The invention belongs to the field of preparation of lithium manganate, and specifically relates to a process for preparing layered lithium manganate. The process comprises: adding a solution of MnSO4 and a solution of NH4HCO3 into a reaction kettle, and performing stirring for reaction; washing and filtering the reaction product to obtain MnCO3; calcining MnCO3 to Mn2O3; mixing Mn2O3 and anhydrous Na2CO3, and adding ethanol for ball milling; calcining the product obtained from ball milling; stirring the calcined product and LiOH.H2O with water, putting the obtained mixture into an autoclave, and performing sealing; performing pressurization and heating of the autoclave, and then performing quick cooling; taking the obtained product out of the autoclave; and performing filtering and washing to obtain layered lithium manganate. According to the invention, firstly, MnSO4 is taken as a base solution to prepare MnCO3; then, MnCO3 is calcined to a manganese oxide; the manganese oxide and Na2CO3 is subjected to ball milling to produce a precursor of sodium manganate; and finally, a high-temperature and high-pressure reaction is carried out to prepare layered lithium manganate. The process is simple and fast to operate and short in reaction time, and is environment-friendly. The prepared lithium manganate is good in quality.

Description

technical field [0001] The invention relates to the field of preparation of lithium manganate, in particular to a preparation process of layered lithium manganate. Background technique [0002] In order to alleviate the global energy crisis and environmental crisis, some countries focus on the new energy industry, and the development of electric vehicles is the focus of the new energy industry; therefore, more and more attention has been paid to providing clean and environmentally friendly power lithium batteries for electric vehicles . At present, for power lithium batteries, there is a great market and development prospect in terms of production technology and application. Strengthening the technology and application research of power lithium manganese oxide batteries is of great significance to promote the rapid development of new energy industries. [0003] At present, the processes of layered lithium manganate include hydrothermal method, ion exchange method, solid pha...

Claims

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Application Information

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IPC IPC(8): C01G45/12
Inventor 易鉴荣林荔琍唐臻吴坚林荔珊
Owner LIUZHOU HAOXIANGTE SCI & TECH
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