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Method for preparing high purity lithium hexafluorophosphate

A lithium hexafluorophosphate, high-purity technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high production cost, corrosion of battery materials, high energy consumption, etc., and achieves fast reaction speed, no pollution to the environment, simple craftsmanship

Inactive Publication Date: 2009-03-25
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the biggest disadvantage of this process is that HF ​​is complexed with LiPF 6 The form of HF remains in the product, and the general method is extremely difficult to reduce the HF content in the product to less than 10ppm, because the residual HF will corrode the battery material, thus affecting the battery electrical performance; in addition, this process will affect the anti-corrosion measures and materials of the equipment The requirements and production safety measures are high; and the process is a cryogenic process, which consumes a lot of energy
These series of reasons have directly led to the high requirements on production equipment for the preparation of lithium hexafluorophosphate by the HF solvent method, which makes the production cost high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh industrial calcium fluoride and phosphorus pentoxide at a mass ratio of 0.5:1.0, seal them in a ceramic ball mill mixer, ball mill and mix them for 2 hours under the protection of argon, and quickly transfer the mixture into a stainless steel airtight pressure heating furnace ( In the phosphorus pentafluoride generation furnace), the air in the furnace is driven away by argon gas, the furnace temperature is controlled at 280°C±5°C, the heating time is 4h, and the phosphorus pentafluoride generated by the reaction is drawn out under pressure; the solid high-purity nano-lithium fluoride and The anhydrous acetonitrile purified by rectification is put into another stainless steel airtight pressure heating furnace (lithium hexafluorophosphate production furnace) at the same time, and after the air in the furnace is driven away with argon, it is stirred under airtight conditions to form a suspension, and the five products generated in the previous step are mixed. Phospho...

Embodiment 2

[0023] Industrial calcium fluoride and phosphorus pentoxide were weighed according to the mass ratio of 0.3:1.0, sealed in a ceramic ball mill mixer, ball milled and mixed for 5 hours under the protection of argon, and the mixture was quickly transferred into a stainless steel airtight pressure heating furnace ( In the phosphorus pentafluoride generation furnace), the air in the furnace is driven away with argon, the furnace temperature is controlled at 300°C±5°C, the heating time is 8h, and the phosphorus pentafluoride generated by the reaction is extracted under pressure; the solid high-purity nano-lithium fluoride and The anhydrous acetonitrile purified by rectification is put into another stainless steel airtight pressure heating furnace (lithium hexafluorophosphate production furnace) at the same time, and after the air in the furnace is driven away with argon, it is stirred under airtight conditions to form a suspension, and the five products generated in the previous step...

Embodiment 3

[0026] According to the conditions described in Example 2, after the reaction is completed, the product obtained by vacuum drying is then dissolved and recrystallized by acetonitrile, the dissolution temperature is 70°C, the dissolution time is 6h, and the filtrate is filtered while it is hot, cooled and crystallized at -20°C, and then filtered to obtain The cake was vacuum-dried at 60°C to obtain the product.

[0027] The reaction yield is more than 98%, and the obtained product lithium hexafluorophosphate can meet the requirements for the use of lithium-ion battery electrolyte, and the specific indicators can be met: the product is high-purity grade, LiPF 6 The content is greater than 99.95%, the water content is less than 10ppm, the HF content is less than 5ppm, and the total impurity metal content is less than 10ppm.

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Abstract

The invention discloses a lithium hexafluorophosphate preparation method, which comprises the following steps: anhydrous acetonitrile is put into a sealed pressure heating furnace, simultaneously solid high-pure nano lithium fluoride is added into the furnace, and after dried inert gas is adopted to drive air out from the furnace a suspension is formed under sealed stirring condition; compressed phosphorus pentafluoride gas is introduced in and the lithium hexafluorophosphate is synthesized continually under the sealed stirring condition. The product prepared by the method has high purification, the content of LiPF<6> is greater than 99.9 percent, the water content is less than 10ppm, the content of HF is less than 50ppm and the content of total impurity metal is less than 50ppm; moreover, the technique is simple, the preparation process is environment-friendly, thus having extremely high industrial popularization value.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to the preparation of electrolyte lithium salts. Background technique [0002] Lithium hexafluorophosphate (LiPF 6 ) is the most widely used electrolyte lithium salt in commercial lithium-ion batteries. Its main advantages are: (1) it can form a proper SEI film on the electrode, especially on the carbon negative electrode; (2) it can effectively passivate the positive current collector to prevent its dissolution; (3) it has a wide Electrochemical stability window; (4) appropriate solubility and high conductivity in various non-aqueous solvents; (5) relatively good environmental friendliness. [0003] At present, the global demand for lithium hexafluorophosphate has reached 1,500 tons, and the supply of three Japanese companies, Stella, Morita, and Kanto, which are capable of providing lithium hexafluorophosphate on a large scale in the world, has far failed to keep up with the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
Inventor 李新海刘建文王志兴郭华军彭文杰胡启阳
Owner CENT SOUTH UNIV
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