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Method for purifying lithium hexafluorophosphate and special device thereof

A lithium hexafluorophosphate and purification method technology, which is applied in the field of lithium hexafluorophosphate purification, can solve problems such as increased production costs, corrosion of body tissues, and complicated operations, and achieve the effects of reasonable device structure, corrosion avoidance, and convenient use

Active Publication Date: 2011-09-14
JIANGSU JIUJIUJIU TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Lithium hexafluorophosphate is white powder or fine grains in appearance. It is easily soluble in DEC (diethyl carbonate), EC (ethylene carbonate) and other organic solvents. It has good chemical stability and does not react with most organic and inorganic substances. However, it is a toxic chemical reagent, which decomposes into acid when it meets water, has a corrosive effect on human body tissue, and cannot be directly contacted. It must be stored in an airtight container and must be operated in a dry atmosphere with an absolute humidity of <10ppm when used. prevent decomposition
However, this method is more complicated to operate and cannot be produced continuously, and when using LiPF 6 While being purified, the recrystallized product will carry a certain amount of organic solvent, which will affect the purity of the product, and the use of a large amount of organic solvent in the purification will increase the production cost, so it is difficult to apply to LiPF 6 mass production
In addition, CN1462722 discloses a method of using acid gas to remove LiPF 6 The method of medium moisture, on the one hand, this method cannot remove LiPF 6 Hydrogen fluoride in the crude product, and the introduction of acid gas impurities

Method used

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  • Method for purifying lithium hexafluorophosphate and special device thereof
  • Method for purifying lithium hexafluorophosphate and special device thereof
  • Method for purifying lithium hexafluorophosphate and special device thereof

Examples

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Effect test

Embodiment 1

[0035] A method for purifying lithium hexafluorophosphate. First, the vibrating reaction furnace is evacuated and repeatedly cleaned with dry nitrogen, and the Al 2 o 3 Activate the adsorption column and molecular sieve adsorption column, and cool the condenser and molecular sieve adsorption column to -180~-140°C, assemble the gas circulation loop, Al 2 o 3 The adsorption column and the molecular sieve adsorption column are connected to the gas circulation loop, and 0.06MPa dry inert gas is added to the gas circulation loop at the same time; under the protection of dry inert gas in the glove box, the crude product of lithium hexafluorophosphate is added to the hopper of the vibration reaction furnace , this material contains free acid HF600ppm and water 100ppm, start the vibration reaction furnace, inject the mixed gas of dry inert gas and fluorine gas into the gas circulation circuit at the same time, by controlling the rotation frequency of the screw feeder of the vibration...

Embodiment 2

[0044] In the glove box, add 1 kg of crude lithium hexafluorophosphate product to the feeding funnel of the spiral stirring reaction furnace in advance. This material contains 620 ppm of free acid HF and 130 ppm of water. Vacuumize the gas circulation loop, then feed 0.06MPa high-purity argon into the gas circulation loop, and repeat the above process 3 times. Cool the molecular sieve adsorption column to -180 to -140°C, and then start the compressor to circulate the gas in the gas circulation loop. Start the screw feeder of the vibration reaction furnace, push the crude product of lithium hexafluorophosphate onto the tray of the vibration reaction furnace, and at the same time slowly feed the mixed gas of fluorine gas and argon gas into the gas circulation loop until the pressure in the gas circulation loop is 0.1MPa, stop feeding the mixed gas of fluorine gas and argon gas into the gas circulation loop, and keep the gas circulation for 3 hours, then stop the gas circulation ...

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Abstract

The invention discloses a method for purifying lithium hexafluorophosphate, which comprises the following steps of: with the protection of dry inactive gas, adding coarse lithium hexafluorophosphate in a feed hopper of a vibration reacting furnace in a glove box, starting the vibration reacting furnace and simultaneously injecting the mixed gas of the dry inactive gas and fluorine gas in a gas circulating circuit, and controlling the adding speed and adding amount of the coarse lithium hexafluorophosphate through controlling rotation frequency and feeding time of the spiral feeder of the vibration reacting furnace; and starting a compressor to circulate the mixed gas of the dry inactive gas and the fluorine gas, evacuating the system through an Al2O3 absorption column, evacuating the gas circulating circuit through a molecular sieve absorption column, re-injecting dry inactive gas in the gas circulating circuit at last, and discharging. The invention has the advantages of high reliability, simple purifying process, and realizable continuous production.

Description

technical field [0001] The invention relates to a method for purifying lithium hexafluorophosphate and a special device thereof. Background technique [0002] Lithium hexafluorophosphate is white powder or fine grains in appearance. It is easily soluble in DEC (diethyl carbonate), EC (ethylene carbonate) and other organic solvents. It has good chemical stability and does not react with most organic and inorganic substances. However, it is a toxic chemical reagent, which decomposes into acid when it meets water, has a corrosive effect on human body tissue, and cannot be directly contacted. It must be stored in an airtight container and must be operated in a dry atmosphere with an absolute humidity of <10ppm when used. Prevent decomposition. [0003] Lithium hexafluorophosphate has been the most dominant electrolyte lithium salt used in commercial lithium-ion batteries for more than 10 years. Lithium hexafluorophosphate mainly has the following advantages as the lithium s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M4/1397
CPCY02E60/122Y02E60/10
Inventor 庄全超周新基秦银平朱建军郑晓兵
Owner JIANGSU JIUJIUJIU TECH
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