Manganous-manganic oxide preparation method for battery positive pole material lithium manganate and product thereof

A technology of trimanganese tetroxide and lithium manganese oxide, which is applied in the direction of battery electrodes, circuits, electrical components, etc., can solve the problems of low tap density, high content of metal impurities, and low median particle size, and achieve compaction density High, good cycle performance, good capacity performance

Active Publication Date: 2012-12-26
SINOSTEEL ANHUI TIANYUAN TECH
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Problems solved by technology

[0004] As the preparation of lithium manganate (LiMn 2 o 4 ) The main raw material of the positive electrode material, the median particle size, specific surface area, tap density, impurity content, etc. of trimanganese tetroxide directly affect the performance of lithium manganese oxide material. At present, the main method of preparing trimanganese tetraoxide for soft ferrite It adopts the suspension catalytic oxidation method, and the median particle size of the products produced by this process is relatively low (≤10μm), and the specific surface area is relatively high (≥4 m 2 / g), low tap density (≤1.6 g / cm 3 ), the particle shape is irregular, and the content of metal impurities is high, which ultimately affects the capacity performance, cycle performance and processability of lithium manganate batteries

Method used

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  • Manganous-manganic oxide preparation method for battery positive pole material lithium manganate and product thereof
  • Manganous-manganic oxide preparation method for battery positive pole material lithium manganate and product thereof
  • Manganous-manganic oxide preparation method for battery positive pole material lithium manganate and product thereof

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preparation example Construction

[0016] The preparation method of trimanganese tetraoxide for lithium manganese oxide, the battery cathode material of the present invention, the specific steps are: after the high-purity metal manganese powder is crushed to a certain particle size distribution by dry method, water and ammonium salt are added to the reactor, and then the air is ventilated Oxidation, the air flow rate in the initial stage of the reaction is 20~100 m 3 / h, the air flow is adjusted to 40~300m after the 5th hour of reaction 3 / h, the air flow rate is adjusted to 20~100m after the 12th hour of reaction 3 / h until the end of the reaction, the stirring speed is controlled at 250r / min~450r / min, the time required for the reaction process is 18~28h, and the pH value at the end of the reaction is controlled at 6.4±0.2. After the reaction is complete, it is prepared after washing and drying Trimanganese tetraoxide products.

[0017] Among them, the particle size distribution of manganese metal powder aft...

Embodiment 1

[0021] Dry crush 1000kg of high-purity manganese metal powder to a median particle size of 6μm~8μm, and put it into the reactor that has been added with pure water and 80kg of ammonium salt (a mixture of ammonium chloride and ammonium sulfate), and the stirring speed is controlled at 360r / min . Oxidation by air, the air flow rate in the initial stage of the reaction is 80 m 3 / h, the air flow is adjusted to 200 m after the reaction reaches the fifth hour 3 / h, the air flow rate is adjusted to 40 m after the reaction reaches the 12th hour 3 / h until the end of the reaction. After reacting for 27 hours, the slurry was washed and dried to obtain trimanganese tetraoxide product.

[0022] The trimanganese tetraoxide product obtained in this embodiment: the median particle size is 27 μm, and the specific surface area is 1.65 μm 2 / g, tap density 2.2 g / cm 3 .

Embodiment 2

[0024] Dry crush 500kg of high-purity manganese metal powder to a median particle size of 15μm~20μm, and put it into a reactor that has been added with pure water and 15kg of ammonium chloride, and the stirring speed is controlled at 280r / min. Oxidation by air, the air flow rate in the initial stage of the reaction is 50 m 3 / h, the air flow is adjusted to 150 m after the reaction reaches the fifth hour 3 / h, the air flow rate is adjusted to 50 m after the reaction reaches the 12th hour 3 / h until the end of the reaction. After reacting for about 20 hours, the slurry is washed and dried to obtain trimanganese tetraoxide product.

[0025] Manganese manganese tetraoxide product obtained in this embodiment: the median particle size is 18 μm, and the specific surface area is 1.24m 2 / g, tap density 2.8 g / cm 3 .

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Abstract

The invention discloses a manganous-manganic oxide preparation method for battery positive pole material lithium manganate and a product thereof. After high pure manganese metal powder is crushed in a dry method to a certain particle size distribution, and air is added into a reactor for oxidation after water and ammonium salts are added. In an early stage of reaction, air flow is 20-100 cubic meters per hour; after five hours of the reaction, the air flow is regulated to 40-300 cubic meters per hour; after twelve hours of the reaction, the air flow is regulated to 20-100 cubic meters per hour; and when the reaction is finished, a stirring rate is controlled to be 250-450 revolutions per minute. Time needed for the reaction is 18-28 hours, and a potential of hydrogen (pH) value at a finishing point of the reaction is controlled to be 6.4 +/-0.2. After the reaction is finished completely, a manganous-manganic oxide product can be prepared after being washed and dried. The manganous-manganic oxide product prepared by means of the method is 15-30 micrometers in a particle diameter, 1.0-4.0 square meters per gram in specific surface area, and 2.0-3.0 grams per cubic centimeter in tap density. With the manganous-manganic oxide preparation method, the lithium manganate positive pole material has the advantages of being good in capacity performance, high in compaction density, goof in cycle performance and the like.

Description

technical field [0001] The invention relates to a preparation method of trimanganese tetraoxide as a raw material used in lithium manganese oxide, a positive electrode material of batteries, and a product thereof. Background technique [0002] Lithium manganate (LiMn 2 o 4 ) is one of the more promising lithium-ion cathode materials. Compared with traditional cathode materials such as lithium cobalt oxide, lithium manganese oxide has the advantages of abundant resources, low cost, no pollution, good safety, and good rate performance. It is an ideal power source. battery cathode material. [0003] Lithium manganate (LiMn 2 o 4 ) and trimanganese tetroxide (Mn 3 o 4 ) are spinel structures. Manganese tetraoxide (Mn 3 o 4 ) instead of electrolytic manganese dioxide (MnO 2 ) to prepare lithium manganate, there is no drastic structural change, lithium manganate (LiMn 2 o 4 ) is relatively easy to form, therefore, with trimanganese tetroxide (Mn 3 o 4 ) to synthesize...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/505
CPCY02E60/122Y02E60/10
Inventor 马金保王志鹏陈思学杨洋余进
Owner SINOSTEEL ANHUI TIANYUAN TECH
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