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Method for producing lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and lithium fluoride, which is applied in chemical instruments and methods, phosphorus compounds, lead-acid batteries, etc., can solve the problems of many production links of lithium hexafluorophosphate, the reaction yield does not exceed 65%, and the production cost remains high. Easy to popularize and apply, high product quality, good social value and economic value

Inactive Publication Date: 2009-11-04
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently, because of the preparation of lithium hexafluorophosphate (LiPF 6 ) has many production links, complicated process and high equipment requirements, so the production cost remains high
[0003] Japanese Patent Application Publication No. Ping 5-279003 discloses a method for preparing lithium hexafluorophosphate, which comprises reacting phosphorus pentachloride with hydrogen fluoride gas to generate phosphorus pentafluoride and hydrogen chloride gas, and then making the resulting phosphorus pentafluoride and hydrogen chloride The gas passes through a cooling tower with a tower temperature of -40 to -80°C, and then enters a reactor containing a hydrofluoric acid solution of lithium fluoride to prepare lithium hexafluorophosphate. The disadvantage of this method is that the reaction yield does not exceed 65%.
[0004] The Chinese Patent Gazette discloses an application for an invention patent with the application number: 200610013957.5, and its name is: the method for preparing lithium hexafluorophosphate. Phosphorus pentachloride reacts with anhydrous hydrogen fluoride solution to prepare a mixed gas of phosphorus pentafluoride and hydrogen chloride, then introduces the mixed gas of phosphorus pentafluoride and hydrogen chloride into anhydrous hydrogen fluoride solution of lithium fluoride, reacts, crystallizes, separates, and dries The pure lithium hexafluorophosphate product is obtained, the disadvantage of this method is that the continuity is not good enough

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0019] The method of the present invention comprises the steps of: adding 500 g of phosphorus pentachloride to a 5 L airtight reaction vessel with magnetic stirring, jacket insulation, and a cooler at the gas outlet, cooling to -40° C., and protecting the reaction vessel under nitrogen protection Slowly add 300g of anhydrous hydrogen fluoride with a water content of less than 10ppm after rectification and purification to make it react with phosphorus pentachloride to generate a mixed gas of phosphorus pentafluoride and hydrogen chloride, and the mixed gas passes through a cooler (-40°C) at the gas outlet ) to remove some impurities and residual acid after cooling. In the 1# reaction kettle with magnetic stirring and cooling jacket, dissolve 55g of high-purity lithium fluoride in 1000g of anhydrous hydrogen fluoride to form anhydrous hydrogen fluoride solution of lithium fluoride, and introduce cooled pentafluoride under stirring The mixed gas of phosphorus fluoride and hydroge...

Embodiment 2

[0023] Return 1250 g of mother liquor after crystallization and filtration in 1# and 2# reactors in Example 1 to 1# and 2# reactors respectively, and add 55 g of high-purity lithium fluoride and anhydrous hydrogen fluoride solution under stirring to form fluoride Anhydrous hydrogen fluoride solution of lithium, repeat the reaction process of embodiment 1, obtain 300g lithium hexafluorophosphate product. The test result product purity is greater than 99.9%, the product free acid (calculated by HF) 95ppm, moisture (Karl Fischer method) 5ppm, alkali metal ion content (calculated by K, Na) 4ppm, heavy metal ion content (calculated by Fe) 2ppm , Insoluble matter content 500ppm.

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PUM

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Abstract

The invention relates to a method for producing lithium hexafluorophosphate. The method comprises the following steps: (1), rectifying and purifying industrial anhydrous hydrogen fluoride and removing moisture and heavy metal impurities therein; (2), enabling the rectified anhydrous hydrogen fluoride and phosphorus pentachloride to react to prepare the mixed gas of phosphorus pentafluoride and chlorine hydride; (3), dissolving high-pure lithium fluoride in an anhydrous hydrogen fluoride solution to form an anhydrous hydrogen fluoride solution containing the lithium fluoride; (4), cooling and guiding the mixed gas of the phosphorus pentafluoride and the chlorine hydride to the anhydrous hydrogen fluoride solution containing the lithium fluoride, reacting, crystallizing, separating and drying to obtain a pure lithium hexafluorophosphate product; and (5), continuously guiding the unreacted gas of the phosphorus pentafluoride and the chlorine hydride after a reaction to the other anhydrous hydrogen fluoride solution containing the lithium fluoride and continuously reacting to obtain a lithium hexafluorophosphate finished product. The invention uses the industrial anhydrous hydrogen fluoride, the phosphorus pentachloride and the high-pure lithium fluoride as raw materials to prepare the lithium hexafluorophosphate product, has rich raw material resources, low production cost, high reaction rate, high product quality and thorough reaction and can realize semi-continuous production.

Description

technical field [0001] The invention relates to a method for producing lithium hexafluorophosphate, belonging to the technical field of lithium ion batteries. Background technique [0002] In recent years, lithium hexafluorophosphate (LiPF 6 ) is selected as the electrolyte of the lithium-ion secondary battery, and lithium hexafluorophosphate is dissolved in some non-aqueous organic solvents to form the electrolyte of the lithium-ion secondary battery. Lithium-ion secondary batteries are internationally recognized as ideal chemical energy sources. They are small in size, large in capacity, can be charged and discharged 500 times, and their capacity is only reduced by 3%. They are widely used in mobile phones, laptop computers, and camcorders. It is used as a dopant for making wafers in the electronics industry and as a catalyst for organic synthesis. Currently, because of the preparation of lithium hexafluorophosphate (LiPF 6 ) has many production links, complex process a...

Claims

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Application Information

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IPC IPC(8): C01B25/455H01M10/08
CPCY02E60/126Y02E60/10
Inventor 皇甫根利侯红军闫春生贾雪枫马小芬
Owner DO FLUORIDE CHEM CO LTD
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