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Lithium hexafluorophosphate preparation method

A technology of lithium hexafluorophosphate and potassium hexafluorophosphate, applied in the direction of phosphorus halide/oxyhalide and the like, can solve the problems of many processing steps and high production cost, and achieve the effects of easy processing, ensuring safety, and reducing requirements and operation difficulty.

Inactive Publication Date: 2016-06-22
庄祥荣
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity of lithium hexafluorophosphate produced by this method is relatively high, but at the same time, it has the disadvantages of high production cost and many pretreatment steps for material purification.

Method used

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Examples

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Effect test

preparation example Construction

[0020] The invention discloses a preparation method of lithium hexafluorophosphate, and those skilled in the art can learn from the content of this article and appropriately improve the process parameters to realize it. In particular, it should be pointed out that all similar replacements and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The preparation method and application of the present invention have been described through preferred embodiments, and those skilled in the art can obviously make changes or appropriate changes and combinations to the method and application described herein without departing from the content, spirit and scope of the present invention , to realize and apply the technology of the present invention.

[0021] Unless otherwise specified, the test materials involved in the specific embodiments can be purchased freely from the market.

Embodiment 1

[0024] (1) Add 103.76g of high-purity lithium fluoride powder with a purity of 99.99% into a reaction kettle with a volume of 2L. The vacuum Hastelloy reactor is made of Cr-Ni-Mo stainless steel. Adjust the temperature of the reaction kettle to 5°C, slowly add 60g of anhydrous hydrogen fluoride into the reaction kettle to form porous lithium fluoride, and then pass in dry nitrogen and argon mixed gas, and in the dry dry nitrogen and argon mixed gas Slowly add 1L of anhydrous organic solvent obtained by mixing ethyl acetate or methyl formate in a ratio of 1:1 under the protection of the solvent, stir and mix evenly to form a suspension;

[0025] (2) Add tetramethylammonium bromide and 18-crown ether-6 catalyst configured in 1:1 while stirring the suspension, and add 732.74g potassium hexafluorophosphate reactor at the same time, and the material in the reactor drops to After continuing the reaction at 5°C for 5 hours, adjust the temperature of the reactor to 0°C;

[0026] (3)...

Embodiment 2

[0029] (1) Add 103.76g of high-purity lithium fluoride powder with a purity of 99.99% into a reaction kettle with a volume of 2L. Vacuum Hastelloy reactor, the inner wall of which is coated with polyethylene, made of iron-based Cr-Ni. Adjust the temperature of the reaction kettle to 5°C, slowly add 70g of anhydrous hydrogen fluoride into the reaction kettle to form porous lithium fluoride, and then pass through dry argon and helium mixed gas, in the dry dry argon, helium Under the protection of mixed gas, slowly add 1L of anhydrous organic solvent prepared by mixing ethyl acetate or methyl formate in a ratio of 1:2, stir and mix evenly to form a suspension;

[0030] (2) While stirring the suspension, add tetraethylammonium bromide and 14-crown ether-2 as a catalyst configured in 1:2, and add 1104.35g potassium hexafluorophosphate reactor at the same time, and the material in the reactor drops to After continuing the reaction at 5°C for 6 hours, adjust the temperature of the r...

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PUM

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Abstract

The invention relates to a lithium hexafluorophosphate preparation method. The method comprises the following steps: processing highly pure lithium fluoride by anhydrous hydrogen fluoride to obtain porous lithium fluoride and release a large amount of heat, using the heat to catalyze dissolving of potassium hexafluorophosphate and lithium fluorine in an anhydrous organic solvent, and absorbing too high heat by the anhydrous organic solvent to form a high efficiency reaction system; and reducing the relative density of a fluorine-containing gas generated in the reaction by the volatilized anhydrous organic solvent, easily processing discharged exhaust gas, reacting gaseous phosphorus pentafluoride with lithium fluoride incompletely reacted in the reaction system, and carrying out reduced pressure distillation to obtain lithium hexafluorophosphate. The method avoids the reaction at an ultralow temperature (-30DEG C or below), reduces the requirements and the operating difficulty of a device, and guarantees the safety.

Description

technical field [0001] The invention relates to the field of lithium ion battery electrolyte salt production, in particular to a preparation method of lithium hexafluorophosphate. Background technique [0002] Lithium-ion battery is a secondary battery (rechargeable battery). In lithium-ion battery materials, the electrolyte is one of the four indispensable materials (positive electrode, negative electrode, diaphragm, electrolyte). The lithium salt used in the electrolyte includes LiAsF 6 、LiPF 6 、LiCF 3 SO 3 , LiClO 4 、LiBF 4 , LiAg 2 CrO 4 etc., where LiPF 6 (Lithium hexafluorophosphate) has been widely used commercially due to its good comprehensive performance. [0003] With the national "Twelfth Five-Year Plan", my country has listed new materials, new energy, and new energy vehicles as strategic emerging industries cultivated and developed by the country. At the same time, consumers have shown great enthusiasm for new energy vehicles such as pure electric veh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/10
Inventor 庄祥荣
Owner 庄祥荣
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