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A kind of preparation method of lithium manganate precursor

A technology of precursor and lithium manganate, which is applied in the field of preparation of lithium manganate precursor, can solve the problems of less research on precursors and restrictions on the research of lithium manganate, and achieve the effect of short process flow, low cost and easy process control

Active Publication Date: 2018-06-29
LIUZHOU HAOXIANGTE SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, when preparing spinel lithium manganate, the formation of its precursor MnOOH directly affects the quality of lithium manganate. Due to the limitations of existing technologies, there are few studies on the precursor, which has always restricted the research of lithium manganate.

Method used

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Examples

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Effect test

preparation example Construction

[0019] The preparation method of the lithium manganate precursor of the present invention is described in detail below, which includes:

[0020] MnSO 4 solution and NH 4 HCO 3 The solution was added to the reactor to stir the reaction, and the reaction solution was 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,...

Embodiment 1

[0024] 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 Roast at a temperature of 950°C for 6 hours in an oxygen atmosphere, and after the product is cooled, follow H 2 o 2 with Mn 3 o 4 Add H at a molar ratio of 4:1 2 o 2 In , after reacting at room temperature and pH value of 8.7 for 45 min, aging at 95 ° C for 7 h to obtain the precursor. Sampling analysis shows that the sample is clear linear MnOOH with uniform particle size distribution.

Embodiment 2

[0026] 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 Roast at 1000°C for 5 hours in an oxygen atmosphere, and after the product is cooled, follow H 2 o 2 with Mn 3 o 4 Add H at a molar ratio of 5:1 2 o 2 In , after reacting at room temperature and pH value of 8.7 for 40 min, aging at 100 ° C for 6 h to obtain the precursor. Sampling analysis shows that the sample is clear linear MnOOH with uniform particle size distribution.

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Abstract

The invention belongs to the preparation field of lithium manganate, and particularly a preparation method for a lithium manganate precursor, comprising: adding an MnSO4 solution and a NH4HCO3 solution into a reaction kettle to stir and react; washing and filtering the reaction product to obtain MnCO3; roasting the MnCO3 into Mn3O4; adding the Mn3O4 into H2O2 to react; then aging to obtain a precursor MnOOH. According to the preparation method, the MnSO4 is used as a base solution to prepare the MnCO3, the MnCO3 is roasted into manganese oxide, and then hydrogen peroxide is added to obtain the precursor. The whole technological process is short, the process is easy to control, and the preparation method is lower in cost, so that a foundation for the preparation of spinel lithium manganese oxide is established.

Description

technical field [0001] The invention relates to the field of preparation of lithium manganate, in particular to a preparation method of lithium manganate precursor. 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, when preparing spinel lithium manganate, the formation of its precursor MnOOH directly affects the qu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/505H01M10/0525
CPCY02E60/10
Inventor 易鉴荣林荔琍唐臻吴坚林荔珊
Owner LIUZHOU HAOXIANGTE SCI & TECH
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