Synthesis method of lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and its synthesis method, which is applied in the fields of phosphorus compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as strong corrosion, great environmental hazards, safety accidents, etc., and achieve the effect of low cost

Active Publication Date: 2010-05-26
ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently, there are two methods commonly used in the synthesis of lithium hexafluorophosphate (LiPF6): one is to react phosphorus pentachloride (PCl5) and hydrogen fluoride (HF) to generate phosphorus pentafluoride (PF5) and hydrogen chloride (HCl), and then use hydrogen fluoride ( HF) is a solvent, and phosphorus pentafluoride (PF5) reacts with LiF to generate lithium hexafluorophosphate (LiPF6), wherein hydrogen fluoride (HF) and hydrogen chloride (HCl) are very corrosive, equipment investment and maintenance costs are high, and a large amount of waste salt is generated in recycling. It is harmful to the environment and prone to safety accidents;
[0004] The other is to generate phosphorus pentafluoride (PF5) by the reaction of phosphorus (P) and fluorine gas (F2), and then use hydrogen fluoride (HF) as a solvent to react phosphorus pentafluoride (PF5) and LiF to generate lithium hexafluorophosphate (LiPF6), Among them, hydrogen fluoride (HF) is very corrosive, and the equipment investment and maintenance costs are high, and a large amount of waste salt is produced after recycling, which is harmful to the environment, and the reaction of phosphorus (P) and fluorine gas (F2) is prone to safety accidents.
[0005] Therefore, the deficiencies in the prior art are: solvents are highly corrosive, equipment investment and maintenance costs are high, environmental hazards are large, and safety accidents are likely to occur

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] First, with dried 8.5g lithium chloride and 36.8g potassium hexafluorophosphate as raw materials, add 125g dimethyl carbonate (moisture is 3.1ppm) as organic solvent and stir in the reaction vessel; Add 4.1 g of tetraethylammonium bromide as a catalyst in the reaction vessel; again, heat while stirring, the control temperature is 30 degrees, and the heating time is 6 hours; after the solution is cooled, the insoluble matter is filtered to obtain an organic solution containing lithium hexafluorophosphate, The whole process is protected with high-purity nitrogen (99.998%). The content of lithium hexafluorophosphate in the solution was detected to be 1.4%.

Embodiment 2

[0022] First, with dried 8.5g lithium chloride and 76.3g potassium hexafluorophosphate as raw materials, add 165g diethyl carbonate (moisture is 4.3ppm) as organic solvent and stir in the reaction vessel; Add 2.1g of tetraethylammonium bromide in the reaction vessel as a catalyst; again, heat while stirring, control the temperature to 70 degrees, and heat for 16 hours; finally, filter the insoluble matter after the solution is cooled, and the organic solution containing lithium hexafluorophosphate , The whole process was protected with high-purity (99.99%) argon. The content of lithium hexafluorophosphate in the solution was detected to be 2.2%.

Embodiment 3

[0024] First, with dried 17g lithium chloride and 36.8g potassium hexafluorophosphate as raw materials, add 185g diethyl carbonate (moisture is 5.1ppm) as organic solvent and stir in the reaction vessel; Add 30g of tetramethylammonium bromide in the container as a catalyst; again, heat while stirring, control the temperature to 55 degrees, and the heating time is 10 hours; finally, filter the insoluble matter after the solution is cooled, and the organic solution containing lithium hexafluorophosphate, the whole The process was carried out in a drying room (the moisture content of the drying room was 98 ppm). The content of lithium hexafluorophosphate in the solution was detected to be 1.8%.

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Abstract

The invention discloses a synthesis method of lithium hexafluorophosphate, aiming to provide a lithium hexafluorophosphate synthesis method with low cost, safety and high efficiency. The method comprises the following steps of: firstly, adding dried lithium chloride and potassium hexafluorophosphate to an organic solvent and stirring; secondly, adding a catalyst to the organic solvent; then, heating while stirring at a controlled temperature of 30-80 DEG C for 2-16 h, controlling the temperature to 20-80 DEG C and the heating time of 2-16 h; and finally, filtering insoluble matter to obtain an organic lithium hexafluorophosphate solution. The invention can be applied to the preparation field of the lithium hexafluorophosphate in a lithium ion battery electrolyte.

Description

technical field [0001] The invention relates to a synthesis method of lithium hexafluorophosphate. Background technique [0002] Lithium hexafluorophosphate (LiPF6) relative molecular mass: 190.11, white crystal or powder, relative density 1.50. Strong deliquescence; easily soluble in water, also soluble in low-concentration methanol, ethanol, acetone, carbonates and other organic solvents. Decomposes on exposure to air or heating. When exposed to air or heated, lithium hexafluorophosphate decomposes rapidly in the air due to the action of water vapor, releasing PF5 and producing white smoke. Lithium hexafluorophosphate is mainly used as an electrolyte material for lithium-ion batteries. Lithium hexafluorophosphate electrolyte is mainly used in the manufacture of lithium-ion batteries. [0003] Currently, there are two methods commonly used in the synthesis of lithium hexafluorophosphate (LiPF6): one is to react phosphorus pentachloride (PCl5) and hydrogen fluoride (HF) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
Inventor 戴晓兵
Owner ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS
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