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Method for preparing lithium-manganese phosphate positive material by adopting wet-chemical method

A technology of lithium manganese phosphate and cathode material, applied in battery electrodes, electrical components, circuits, etc., can solve problems such as low yield per unit of equipment and separation of by-products

Active Publication Date: 2015-06-10
天津赫维科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a method for preparing lithium manganese phosphate positive electrode material by wet chemical method, using lithium phosphate and manganese phosphate as raw materials, preparing lithium manganese phosphate material through hydrothermal reaction, and solving the separation of by-products prepared by hydrothermal method And the problem of low yield per unit of equipment, while maintaining the advantages of hydrothermal method for preparing lithium manganese phosphate materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) Mix 118.1g of lithium phosphate (Shanghai Zhongli Industrial Co., Ltd., purity 98%) and 412.1g of manganese phosphate crystals (analytically pure, purity 99%) into a mortar, then add 62.5g of absolute ethanol to grind After 3 hours ethanol volatilized completely, the mixture became powder;

[0015] (2) Add 6.25g of pharmaceutical grade ascorbic acid, grind it evenly, then add 625g of 4% polyvinyl alcohol (molecular weight 6000) solution, and stir it evenly on a small disperser to form a slurry;

[0016] (3) Pour the slurry into a hydrothermal reaction kettle, seal it well, heat it to 180°C and keep it for 10 hours, then cool down to room temperature, open the reaction kettle and pour out all the materials, and carry out blast drying at 105°C to form a lump;

[0017] (4) Use a tubular experimental electric furnace to raise the temperature of the block to 450°C at a rate of 5°C / min under the protection of high-purity nitrogen, keep it warm for 2 hours, and then heat i...

Embodiment 2

[0020] (1) Mix 118.1g of lithium phosphate (Shanghai Zhongli Industrial Co., Ltd., purity 98%) and 412.1g of manganous phosphate crystals (analytically pure, purity 99%) into a mortar, then add 62.5g of absolute ethanol to grind After 1.2 hours, the ethanol evaporated completely, and the mixture became powder;

[0021] (2) Add 6.25g of pharmaceutical grade ascorbic acid, grind evenly, then add 625g of 4% polyvinyl alcohol (molecular weight: 15,000) solution, and use a small dispersion disc to stir evenly into a slurry;

[0022] (3) Pour the slurry into a hydrothermal reaction kettle, seal it well, heat it to 180°C and keep it for 10 hours, then cool down to room temperature, open the reaction kettle and pour out all the materials, and carry out blast drying at 105°C to form a block;

[0023] (4) Use a tube-type experimental electric furnace to raise the temperature of the block to 450°C at a rate of 5°C / min under the protection of high-purity nitrogen, keep it for 2 hours, and...

Embodiment 3

[0026] (1) Mix 120.5g of lithium phosphate (Shanghai Zhongli Industrial Co., Ltd., purity 98%) and 412.1g of manganese phosphate crystals (analytically pure, purity 99%) into a mortar, then add 62.5g of absolute ethanol to grind After 3 hours ethanol volatilized completely, the mixture became powder;

[0027] (2) Add 6.25g of pharmaceutical grade ascorbic acid, grind evenly, then add 625g of 4% polyvinyl alcohol (molecular weight 10000) solution, stir evenly to form a slurry;

[0028] (3) Pour the slurry into a hydrothermal reaction kettle, heat to 180°C for 10 hours, then cool down to room temperature, open the reaction kettle, pour out all the materials, and carry out blast drying at 105°C to form lumps;

[0029] (4) Use a tube-type experimental electric furnace to raise the temperature of the block to 450°C at a rate of 5°C / min under the protection of high-purity nitrogen, keep it for 2 hours, and then raise the temperature to 700°C at a rate of 5°C / min for 4 hours. Natura...

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Abstract

The invention discloses a method for preparing a lithium-manganese phosphate positive material by adopting a wet-chemical method. The method comprises the following steps: (1) mixing analytically-pure lithium phosphate and analytically-pure manganous phosphate in a grinding bowl according to the molar ratio of Li to Mn being.(1.0-1.02) to 1, then adding absolute ethyl alcohol, grinding for 1-3 hours till the mixture becomes powder; (2) adding ascorbic acid, grinding uniformly, then adding 4% of a polyvinyl alcohol solution, stirring uniformly to be in a pulpy state; (3) heating the pulpy materials to 180 DEG C, maintaining for 10 hours, then cooling to room temperature and pouring all the materials in a reaction kettle, blowing at the temperature of 105 DEG C, and drying into blocked materials; and (4) heating the blocked materials to 450 DEG C at the speed of 5 DEG C / min under the protection of high-pure nitrogen, maintaining the temperature for 2 hours, then heating to 700 DEG C at the speed of 5 DEG C / min, maintaining the temperature for 4 hours, cooling to room temperature, grinding into powder, and sieving by a 100-mesh sieve so as to obtain the lithium-manganese phosphate material.

Description

technical field [0001] The invention belongs to the field of novel chemical energy storage, and in particular relates to a method for preparing lithium manganese phosphate cathode material by a wet chemical method. Background technique [0002] Lithium manganese phosphate material is a positive electrode material for lithium-ion batteries. It has the advantages of low price, abundant raw materials, non-toxicity, good thermal stability, high specific energy, long cycle life, long shelf life, outstanding safety performance and no pollution to the environment. Its theoretical specific capacity is 170mAh / g, and its theoretical operating voltage is about 4.1 V. It is a new type of lithium-ion battery cathode material with the most potential. However, lithium manganese phosphate cathode materials still have some shortcomings, such as low electrical conductivity, low ion diffusion coefficient, poor low temperature performance, and poor rate discharge capability, which lead to many ...

Claims

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Application Information

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IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 郝德利叶丽光
Owner 天津赫维科技有限公司