Lithium ferromanganese phosphate and preparation method thereof

A technology of lithium iron manganese phosphate and ferromanganese hydrogen phosphate, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of complex recovery process, complex process, and high equipment requirements, and achieve high atomic economy and technology. simple effect

Active Publication Date: 2019-04-19
GUANGDONG GUANGHUA SCI TECH +1
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  • Abstract
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  • Claims
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Problems solved by technology

However, this method will use an organic solvent on the one hand, and an autoclave on the other hand. Again, the amount of lithium used in solvent hydrothermal synthesis is three times the theoretical amount, and the excess lithium requires a complicated recovery process.
This method has high requirements on equipment, complicated process, and difficulty in material recovery, resulting in high production costs, which is not conducive to the large-scale production of lithium iron phosphate
[0004] According to reports, there are also researchers who use ion iron source and ion manganese source to prepare lithium manganese iron phosphate, for example, use ferrous sulfate, ferrous nitrate or ferrous acetate as iron source and use manganese nitrate or manganese oxalate as manganese source as a reaction Raw material, then add lithium source and carbon source to syn

Method used

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  • Lithium ferromanganese phosphate and preparation method thereof
  • Lithium ferromanganese phosphate and preparation method thereof
  • Lithium ferromanganese phosphate and preparation method thereof

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preparation example Construction

[0038] A preparation method for lithium manganese iron phosphate, comprising the following steps:

[0039] (1) mixing elemental iron, manganese dioxide and phosphoric acid aqueous solution to obtain mixture A, and ball milling said mixture A to obtain ferromanganese phosphate;

[0040] (2) Contact the ferromanganese phosphate, lithium carbonate and glucose, sand-mill until the particle size D50 of the product is 0.2 μm-1 μm, dry, and calcinate to obtain lithium ferromanganese phosphate.

[0041] Wherein, the "ball milling" and "sand milling" can be carried out in a wide temperature range, the preferred temperature range is 10-60°C, and the milling time depends on whether the D50 particle size of the product has reached the required range, The preferred grinding time is 10h-50h.

[0042] The drying described in step (2) includes but is not limited to vacuum freeze drying, heating drying under nitrogen or inert gas protection, microwave drying, spray drying or flash drying, etc...

Embodiment 1

[0047] Step 1, take by weighing 0.3 mole of iron powder (Fe content > 99%), 0.2 mole of electrolytic manganese powder (Mn content > 99.8%), 0.5 mole of electrolytic manganese dioxide powder (MnO 2 Content > 99%) mixed with phosphoric acid aqueous solution (mass concentration 50%) containing 1.03 moles of phosphoric acid, placed in a ball mill for reaction at 25°C, after 15 hours, the particle size D50 of ferromanganese phosphate was measured to be 5 microns, and the ball milling was terminated . Carry out X-ray diffraction test (XRD) to ferromanganese phosphate powder, test pattern such as figure 1 shown.

[0048]Step 2. Transfer the above-mentioned ferromanganese phosphate to a sand mill for reaction. Add 1.05 moles of lithium carbonate and 0.1 moles of glucose at 20°C. After 30 hours, it is detected that the particle size D50 of the material is 0.6 microns, and the sand milling is terminated. The slurry is spray-dried, the drying temperature is 250°C, and the drying time i...

Embodiment 2

[0050] Step 1, take by weighing 0.3 mole of iron powder (Fe content > 99%), 1.5 mole of electrolytic manganese dioxide powder (MnO 2 Content > 99%) mixed with phosphoric acid aqueous solution (mass concentration 10%) containing 3.06 moles of phosphoric acid, placed in a ball mill for reaction at 40°C, after 40 hours, the particle size D50 of ferromanganese phosphate was measured to be 2 microns, and the ball milling was terminated .

[0051] Step 2. Transfer the above-mentioned ferromanganese phosphate to a sand mill for reaction, add 3 moles of lithium carbonate and 1 mole of glucose at 35°C, and after 50 hours, it is detected that the particle size D50 of the material is 0.2 microns, and the sand milling is terminated. The slurry is spray-dried, the drying temperature is 200°C, and the drying time is 10 seconds. The dried powder is calcined at 700°C under the protection of nitrogen, and the calcining time is 8 hours. After cooling, take it out and put it in gloves. Make a b...

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Abstract

The invention relates to a preparation method of lithium ferromanganese phosphate. The method comprises the steps of: (1) mixing elemental iron, manganese dioxide and a phosphoric acid aqueous solution to obtain a mixture A, and subjecting the mixture A to ball milling to obtain ferromanganese hydrogen phosphate; and (2) mixing the ferromanganese hydrogen phosphate, lithium carbonate and glucose,and performing sand milling to a product particle size D50 of 0.2microm-1microm, and conducting drying and calcination to obtain lithium ferromanganese phosphate. The method has the characteristics ofsimple equipment and process, good atomic economy, small environmental pressure and low manufacturing cost, is easy for industrial production, and by controlling the particle size of the final product, the specific discharge capacity of lithium ferromanganese phosphate serving as a battery cathode material is increased.

Description

technical field [0001] The invention relates to the field of preparation of positive electrode materials for lithium ion batteries, in particular to lithium manganese iron phosphate and a preparation method thereof. Background technique [0002] With the continuous development of electronic equipment such as spacecraft, electric vehicles, medical equipment, and communication equipment, relatively mature binary lithium batteries, such as lithium iron phosphate and lithium manganese phosphate batteries, have gradually improved in terms of charge and discharge voltage, conductivity and service life. Show limitations. Nowadays, the use of a new generation of ternary material lithium manganese iron phosphate as the positive electrode of the battery has the advantage of higher rate performance and cycle performance. Therefore, lithium manganese iron phosphate material is more and more valued by various battery manufacturers. [0003] According to reports, some researchers used so...

Claims

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Application Information

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IPC IPC(8): C01B25/45H01M4/58H01M10/0525
CPCC01B25/45C01P2002/72C01P2004/61H01M4/5825H01M10/0525H01M2004/021H01M2004/028Y02E60/10
Inventor 曾德文王耀南谭泽
Owner GUANGDONG GUANGHUA SCI TECH
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