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Method for preparing battery grade lithium dihydrogen phosphate with high-purity lithium carbonate lithium depositing mother solution

A technology of lithium dihydrogen phosphate and high-purity lithium carbonate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., to achieve stable quality, broad market prospects, and high purity

Active Publication Date: 2013-10-30
GANFENG LITHIUM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The traditional method of mother liquor treatment is to use hydrogen fluoride to extract lithium from the lithium-precipitated mother liquor to prepare lithium fluoride. The lithium extraction rate is only about 70%.

Method used

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  • Method for preparing battery grade lithium dihydrogen phosphate with high-purity lithium carbonate lithium depositing mother solution
  • Method for preparing battery grade lithium dihydrogen phosphate with high-purity lithium carbonate lithium depositing mother solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (A) Add 500L of 99.9% high-purity lithium carbonate mother liquor into the reaction tank, heat it to 90±5℃, start dripping 85% phosphoric acid solution, and control the pH after the reaction = 5. Obtain preliminary lithium extraction products;

[0053] (B) After the reaction solution in step (a) is fully stirred, slowly add the disodium hydrogen phosphate solution dropwise, the temperature is controlled at 80-85 ℃, fully stirred, the end pH value is controlled to pH=7, and the temperature is kept for 1 hour Then a mixed slurry of lithium phosphate and dilithium hydrogen phosphate is obtained;

[0054] (C) Separate the lithium salt and mother liquor in the mixed slurry of lithium phosphate and dilithium hydrogen phosphate while it is hot, with a lithium extraction rate of 90%;

[0055] (D) Wash the separated mixture of lithium phosphate and dilithium hydrogen phosphate with hot water;

[0056] (E) Add a small amount of purified water to the mixture of lithium phosphate and dili...

Embodiment 2

[0062] (A) Add 500L of 99.9% high-purity lithium carbonate mother liquor into the reaction tank, heat it to 90±5℃, start to add 60% phosphoric acid solution dropwise, and control the pH=6 after the reaction , Get the initial lithium extraction product;

[0063] (B) After the reaction solution in step (a) is fully stirred, slowly add the disodium hydrogen phosphate solution dropwise, the temperature is controlled at 80 ~ 85 ℃, fully stirred, the end pH value is controlled to pH=9, and after holding for 1 hour Obtain a mixed slurry of lithium phosphate and dilithium hydrogen phosphate;

[0064] (C) Separate the lithium salt and mother liquor in the mixed slurry of lithium phosphate and dilithium hydrogen phosphate while it is hot, with a lithium extraction rate of 92%;

[0065] (D) Wash the separated mixture of lithium phosphate and dilithium hydrogen phosphate with hot water;

[0066] (E) Add a small amount of purified water to the mixture of lithium phosphate and dilithium hydrogen p...

Embodiment 3

[0072] (A) Add 500L of 99.9% high-purity lithium carbonate mother liquor into the reaction tank, heat it to 90±5℃, start dripping 40% phosphoric acid solution, and control the pH after the reaction = 7. Obtain preliminary lithium extraction products;

[0073] (B) After the reaction solution in step (a) is fully stirred, slowly add the disodium hydrogen phosphate solution dropwise, the temperature is controlled at 80 ~ 85 ℃, fully stirred, the end pH value is controlled to pH = 10, and after 1 hour Obtain a mixed slurry of lithium phosphate and dilithium hydrogen phosphate;

[0074] (C) Separate the lithium salt and mother liquor in the mixed slurry of lithium phosphate and dilithium hydrogen phosphate while it is hot, with a lithium extraction rate of 91%;

[0075] (D) Wash the separated mixture of lithium phosphate and dilithium hydrogen phosphate with hot water;

[0076] (E) Add a small amount of purified water to the mixture of lithium phosphate and dilithium hydrogen phosphate ob...

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Abstract

The invention relates to a method for preparing battery grade lithium dihydrogen phosphate with a high-purity lithium carbonate lithium depositing mother solution. The method comprises the steps of: conducting preliminary lithium extraction and deep lithium extraction to a lithium carbonate lithium depositing mother solution with phosphoric acid and phosphate so as to obtain a mixture of lithium phosphate and dilithium hydrogen phosphate, reacting the mixture with phosphoric acid to generate a lithium dihydrogen phosphate solution, then carrying out concentration and evaporation, cooling and crystallization, centrifugation, saturation washing, drying, air-stream crushing and packaging, thus obtaining the battery grade lithium dihydrogen phosphate. The method of preparing battery grade lithium dihydrogen phosphate in the invention fully makes use of the mother solution generated during high-purity lithium carbonate production, and has the advantages of simple process, easy operation, low production cost, over 90% of lithium recovery rate, and stable quality of the obtained battery grade lithium dihydrogen phosphate product, and is also suitable for preparing the lithium ion battery positive material lithium iron phosphate. Therefore, the method provided in the invention boasts broad market prospects, as well as good economic and social benefits.

Description

Technical field [0001] The invention belongs to the field of inorganic materials and relates to a method for preparing battery-grade lithium dihydrogen phosphate by using high-purity lithium carbonate lithium precipitation mother liquor. Background technique [0002] In recent years, lithium and lithium compounds have been used more and more widely in people's lives. For example, lithium ion secondary batteries have been widely used in portable computers, mobile communications, and power tools. At present, the commonly used cathode materials for lithium batteries include lithium cobalt oxide, lithium nickel cobalt oxide, lithium nickel cobalt manganese oxide, lithium manganese oxide, etc., but their common disadvantages are poor safety performance, high production costs, and limited cobalt resources. Its price has a trend of continuous increase. As a new type of lithium ion battery cathode material, lithium iron phosphate has attracted more and more attention and attention. Lit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/30
Inventor 李良彬马木林白有仙刘明朱志全李芳芳晏婷婷
Owner GANFENG LITHIUM CO LTD
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