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Method for preparing battery grade lithium phosphate composite material

A composite material and lithium phosphate technology, applied in the field of preparation of lithium phosphate composite materials, can solve the problems of large water consumption, strong acidity, equipment corrosion, etc., and achieve good equipment reliability, mild reaction conditions, and high tap density. Effect

Active Publication Date: 2015-06-17
GUANGZHOU LIBODE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The disadvantages of the above-mentioned preparation method are: the production process is cumbersome; the reaction process has high temperature, strong acidity, and great corrosion to equipment; at the same time, in order to wash off the impurities in lithium dihydrogen phosphate, it needs to consume a large amount of water resources, resulting in A large amount of waste liquid seriously pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 41.87g of lithium carbonate (purity 99.5%), 129.07g of ammonium dihydrogen phosphate (chemically pure) (the molar ratio of lithium source and phosphorus source is about 1.025:1), use 70ml of deionized water as a solvent to mix lithium carbonate and diphosphate Ammonium hydrogen is uniformly dispersed and ground for 8 hours before spray drying; set the spray drying parameters, the inlet temperature is 350°C, the outlet temperature is 130°C, and the atomization disk speed is 10000 rpm, and then the spherical material obtained by spray drying is subjected to high temperature in oxygen. For sintering, the oxygen flow rate is controlled to be 10 cubic meters per hour, the sintering temperature is 700°C, and the battery-grade lithium phosphate composite material is obtained after sintering for 6 hours.

Embodiment 2

[0017] Take 47.31g of lithium hydroxide (purity 99.0%), 148.10g of diammonium hydrogen phosphate (chemically pure) (the molar ratio of lithium source and phosphorus source is about 1.025:1), use 290ml of deionized water as a solvent to mix lithium hydroxide and Diammonium hydrogen phosphate is uniformly dispersed and ground for 2 hours before spray drying; set the spray drying parameters, the inlet temperature is 300°C, the outlet temperature is 120°C, the rotation speed of the atomizing disc is 20000 rpm, and then the spherical material obtained by spray drying is placed in the air Carry out high-temperature sintering, control the air flow rate to 25 cubic meters per hour, and the sintering temperature to 500°C. After sintering for 16 hours, a battery-grade lithium phosphate composite material is obtained.

Embodiment 3

[0019] Take 19.91g lithium carbonate (purity 99.5%), 22.51g lithium hydroxide (purity 99.0%), 167.00g ammonium phosphate (chemically pure) (the molar ratio of lithium source and phosphorus source is about 0.975:1), use 300ml deionized Water is used as a solvent to uniformly disperse and grind lithium carbonate, lithium hydroxide, and ammonium phosphate for 4 hours, and then spray dry; set the spray drying parameters, the inlet temperature is 200 ° C, the outlet temperature is 100 ° C, the atomization disc speed is 8000 rpm, and then The spherical material obtained by spray drying is sintered at high temperature in oxygen, the oxygen flow rate is controlled to be 15 cubic meters per hour, the sintering temperature is 650°C, and the battery-grade lithium phosphate composite material is obtained after sintering for 10 hours.

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Abstract

The invention discloses a method for preparing a battery grade lithium phosphate composite material. The method comprises the following steps of: adding a lithium source and a phosphorus source into deionized water, and fully blending and grinding for 2 to 8 hours, wherein a molar ratio of the lithium source to the phosphorus source is (0.97-1.03):(0.97-1.03); performing spray drying to obtain a spherical lithium phosphate complex precursor; and sintering the spherical lithium phosphate complex precursor at high temperature of between 500 and 700 DEG C for 4 to 16 hours in air or oxygen to obtain the battery grade lithium phosphate composite material, wherein the lithium source is one or more of lithium carbonate, lithium hydroxide and lithium acetate, and the phosphorus source is one or more of phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate and ammonium phosphate. The preparation method has the advantages of middle reaction conditions, high equipment reliability and no waste liquor pollution.

Description

technical field [0001] The invention relates to a preparation method of a lithium phosphate composite material. Background technique [0002] Since the first report in 1997 that olivine ferrous phosphate has the function of reversible lithium intercalation, LiMPO, an olivine-type phosphate-based lithium intercalation material, has been 4 (M=Mn, Fe, Co, Li) Because of its high structural stability, as a new type of lithium-ion battery cathode material, LiMPO 4 Homologs especially LiFePO 4 It has received extensive attention and in-depth research. In the field of power batteries, there are very strict requirements on battery materials, the first is safety, because LiFeMO 4 The stability of its own structure does not release oxygen at high temperatures, which completely eliminates the safety problems caused by traditional cathode materials and improves the safety of power batteries; secondly, it has excellent electrochemical performance, and the material is coated with carbo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 蒋华锋骆宏钧
Owner GUANGZHOU LIBODE NEW MATERIAL
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