Method for preparing high-purity lithium fluoride and lithium hexafluorophosphate by utilization of organo tin fluoride

A technology of lithium hexafluorophosphate and organotin, applied in chemical instruments and methods, lithium halides, phosphorus compounds, etc., can solve the problems of multiple production links, low product yield and purity, high equipment and environmental protection requirements, and achieve the effect of avoiding use

Active Publication Date: 2013-08-21
中山市华玮新能源科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the invention is to prepare LiPF in order to overcome prior art 6 There are many production links, low temperature operation is required, the process is complicated, the equipment and environmental protection requirements are high, and the product yield and purity are not high. It provides a simple and controllable technology, simple process conditions, and reduces equipment corrosion. Method for preparing high-purity lithium fluoride and lithium hexafluorophosphate from tin fluoride

Method used

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preparation example Construction

[0054] The specific preparation method of LiF among the present invention comprises: under normal temperature condition, under dry nitrogen atmosphere, LiX and organotin fluoride R n SnF 4-n Add it to the reaction kettle and suspend it in a dry organic solvent, heat up and stir for 5-10 hours until R n SnF 4-n disappear completely, during which the reaction temperature is 20 to 150°C, preferably 30 to 82°C. The produced LiF is a nano-scale solid, which is suspended in an organic solvent, and the mother liquor is removed by filtration, and the high-purity LiF solid is separated to be used as the raw material for the next step of the reaction; the suspension can also be used directly for the next step of the reaction without separation.

[0055] PF in the present invention 5The specific preparation method includes: PCl 5 Dissolved in a dry organic solvent, under the protection of nitrogen, the organotin fluoride R n SnF 4-n Add to the reaction kettle to suspend and stir fo...

Embodiment 1

[0066] In a closed reaction kettle, under the protection of nitrogen, 42.4g (1mol) LiCl was dissolved in 500mL of anhydrous methanol at room temperature, and then 182.9g (1mol) Me 3 The SnF solid was suspended in the solution, and the Me 3 The SnF solid gradually disappeared, and at the same time, a very fine LiF solid was formed and suspended in the solution. After 10 hours of reaction, the solid was collected by filtration, washed with an appropriate amount of methanol, concentrated and dried in vacuo to obtain 25.4 g of LiF solid with a purity of 99.95%.

Embodiment 2

[0068] In a closed reactor, under the protection of nitrogen, 86.84g (1mol) LiBr was dissolved in 800mL of anhydrous methanol at room temperature, and then 182.9g (1mol) Me 3 The SnF solid was suspended in the solution, heated to 80°C and stirred, Me 3 The SnF solid gradually disappeared, and at the same time, a very fine LiF solid was formed and suspended in the solution. After reacting for 10 hours, cool to room temperature, collect the solid by filtration, and wash the solid with an appropriate amount of ethanol. After vacuum concentration and drying, 25.6g of LiF solid was obtained, with a purity of 99.95%. .

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Abstract

The invention discloses a method for preparing high-purity lithium fluoride and lithium hexafluorophosphate by the utilization of organo tin fluoride. As for preparation of lithium fluoride, a fluorine/halogen exchange reaction between lithium halide and organo tin fluoride is carried out to generate lithium fluoride. As for preparation of lithium hexafluorophosphate, a fluorine/halogen exchange reaction between phosphorus pentahalide and organo tin fluoride is firstly carried out to generate phosphorus pentafluoride, and a contact reaction between phosphorus pentafluoride and lithium fluoride is carried out to generate lithium hexafluorophosphate; or, lithium halide and phosphorus pentahalide are firstly dissolved in an organic solvent until a clear intermediate solution, and then the intermediate solution reacts with organo tin fluoride to generate lithium hexafluorophosphate, wherein lithium halide is lithium chloride or lithium bromide. The lithium fluoride prepared in the invention has high purity. Meanwhile, adoption of highly corrosive HF as a fluorinated reagent is avoided so as to avoid the possibility of introducing impurities and guarantee that high-quality LiPF6 can be prepared in the next step.

Description

【Technical field】 [0001] The invention relates to a method for preparing lithium fluoride and lithium hexafluorophosphate, in particular to a method for preparing high-purity lithium fluoride and lithium hexafluorophosphate by using organic tin fluoride. 【Background technique】 [0002] In recent years, the basic research and application development of lithium-ion batteries have become one of the hot spots in the field of new energy, and all developed countries in the world regard it as the breakthrough point of the next emerging industry for development and research. Lithium hexafluorophosphate (LiPF 6 ) has been widely used in commercial lithium-ion batteries due to its good electrical conductivity and stable electrochemical performance, and is one of the key materials for manufacturing lithium-ion batteries. LiPF 6 It is a white powdery solid, which is not only easy to decompose due to moisture absorption, but also has poor thermal stability. LiPF as an electrolyte for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/04C01B25/455
Inventor 余佩华余佩娟
Owner 中山市华玮新能源科技有限公司
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