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Method for synthesizing graphene-doped nanometer manganese-rich lithium iron phosphate under conditions of normal pressure and water phase

A manganese-rich lithium iron phosphate and graphene technology, applied in nanotechnology, electrical components, electrochemical generators, etc., can solve the problems of long process, large equipment investment, poor product consistency, etc., and achieve mild reaction conditions and particle size. The effect of uniform and controllable, reducing production cost

Active Publication Date: 2014-07-30
JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the main problem of the high-temperature solid-phase method is that the batch stability of the product is poor, which directly leads to the short-plate reaction of the battery pack; the precursor obtained by the sol-gel method and the solution co-precipitation method is not lithium iron phosphate, but more The mixture of various substances, the components of the mixture are difficult to be consistent, and the obtained precursor needs to be calcined at a high temperature again to obtain the lithium iron phosphate crystal, which makes the process long, the product consistency is poor, and the equipment investment is large; hydrothermal Although the method and the solvothermal method can directly obtain lithium ferrous phosphate crystals, they require high temperature and high pressure reaction equipment, and the investment is huge, which is not suitable for large-scale industrial production, and the pure lithium ferrous phosphate has low capacity and poor rate performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for synthesizing graphene-doped nano manganese-rich lithium iron phosphate in an aqueous phase under normal pressure, comprising the following steps:

[0020] (1) Add 4800L of lithium sulfate solution containing 0.2mol / L lithium to a 6300L enamel reaction kettle, start stirring, add 36.9kg of 85% phosphoric acid, and raise the temperature to 70°C, then add sodium hydroxide solution under stirring , adjust the pH value to 11, and then carry out solid-liquid separation and washing to obtain lithium phosphate solid;

[0021] (2) Add 3.0 kg of graphene into 3000L of pure water, and fully disperse it into a graphene water suspension with ultrasonic waves;

[0022] (3) Add lithium phosphate to the graphene aqueous suspension obtained in step (2), and fully disperse it mechanically to obtain a 3000L graphene lithium phosphate suspension containing 1.0 g / L of graphene and 0.1 mol / L of lithium phosphate liquid;

[0023] (4) Dissolve manganese sulfate and ferrous sulfa...

Embodiment 2

[0028] A method for synthesizing graphene-doped nano manganese-rich lithium iron phosphate in an aqueous phase under normal pressure, comprising the following steps:

[0029] (1) Add 4800L lithium chloride solution containing 0.4mol / L lithium to a 6300L enamel reaction kettle, start stirring, add 73.8kg85% phosphoric acid, and raise the temperature to 70°C, then add sodium hydroxide under stirring solution, adjust the pH value to 9.5, and then carry out solid-liquid separation and washing to obtain lithium phosphate solid;

[0030] (2) Add 3.0 kg of graphene into 3000L of pure water, and fully disperse it into a graphene water suspension with ultrasonic waves;

[0031] (3) Add lithium phosphate to the graphene aqueous suspension obtained in step (2), and fully disperse it mechanically to obtain a 3000L graphene lithium phosphate suspension containing 1.0 g / L of graphene and 0.2 mol / L of lithium phosphate liquid;

[0032] (4) Dissolve manganese nitrate and ferrous chloride in...

Embodiment 3

[0037] A method for synthesizing graphene-doped nano manganese-rich lithium iron phosphate in an aqueous phase under normal pressure, comprising the following steps:

[0038] (1) Add 3000L lithium nitrate solution containing 3mol / L lithium to a 5000L enamel reaction kettle, start stirring, add 346kg85% phosphoric acid, and raise the temperature to 30°C, then add sodium hydroxide solution while stirring, and adjust pH value to 10, then solid-liquid separation and washing, to obtain lithium phosphate solid;

[0039] (2) Add 4.8 kg of graphene oxide into 3000L of pure water, and fully disperse it into a graphene oxide aqueous suspension with ultrasonic waves;

[0040](3) Add lithium phosphate to the graphene oxide aqueous suspension obtained in step (2), and fully disperse it mechanically to obtain 3000L graphene oxide phosphoric acid containing 1.6g / L of graphene and 0.5mol / L of lithium phosphate Lithium suspension;

[0041] (4) Dissolve manganese sulfate and ferrous chloride ...

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Abstract

The invention discloses a method for synthesizing graphene-doped nanometer manganese-rich lithium iron phosphate under conditions of normal pressure and water phase. The method comprises the following steps: preparing lithium phosphate, preparing a graphene or graphene oxide water suspension, preparing a lithium phosphate and graphene or graphene oxide mixed suspension, preparing a divalent manganese salt and ferrite mixed solution, preparing graphene-doped or graphene oxide-doped nano manganese-rich lithium iron phosphate, and recycling lithium from a mother solution. Compared with the prior art, the method has the advantages that the method for synthesizing graphene-doped nanometer manganese-rich lithium iron phosphate under conditions of normal pressure and water phase is mild in reaction conditions and low in equipment cost; the prepared product is high in electrical property and capacity, good in rate capability, stable in batch and uniform and controllable in granularity; the lithium in the mother solution can be recycled, so that the production cost is lowered, and the requirement of industrialized production is met.

Description

technical field [0001] The invention relates to the preparation of positive electrode materials for lithium ion batteries, in particular to a method for synthesizing graphene-doped nano manganese-rich ferrous phosphate in an aqueous phase at normal pressure. Background technique [0002] As a cathode material for lithium-ion batteries, lithium iron phosphate is popular because of its safe olivine structure, low-cost raw materials, and environmental protection. It is considered to be one of the ideal cathode materials for lithium-ion batteries. At present, the methods for synthesizing lithium ferrous phosphate mainly include: high-temperature solid-phase method, solution-gel method, hydrothermal method, solvothermal method, solution co-precipitation method, etc. Among them, the main problem of the high-temperature solid-phase method is that the batch stability of the product is poor, which directly leads to the short-plate reaction of the battery pack; the precursor obtained ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/1397B82Y40/00
CPCB82Y40/00H01M4/58H01M10/0525Y02E60/10
Inventor 何国端李南平葛建敏蒋燕锋
Owner JIANGSU RONGHUI GENERAL LITHIUM IND CO LTD
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