Method for preparing lithium hexafluorophosphate

A technology of lithium hexafluorophosphate and hexafluorophosphoric acid, applied in chemical instruments and methods, phosphorus compounds, lead-acid batteries, etc., can solve the problems of low purity of lithium hexafluorophosphate, difficult purification, etc. Effect

Active Publication Date: 2009-11-04
DO FLUORIDE CHEM CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The lithium hexafluorophosphate produced by t...

Method used

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Examples

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Effect test

Embodiment 1

[0019] The method of the present invention specifically comprises the following steps: in a closed container, 572g of phosphorus pentoxide is added under the protection of nitrogen, and 1306g of liquid anhydrous hydrogen fluoride is slowly added under stirring and cooling, and the temperature of the system is kept at about 0°C. for 4 hours. Get the hexafluorophosphoric acid generated in the step (1), slowly add 1635g of fuming sulfuric acid under cooling and stirring. After adding the oleum, put the system in a dry environment at 150°C and react for 1 hour. The generated phosphorus pentafluoride gas passes through a cooler at -40°C to remove impurities and collect them. 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 phosphorus pentafluoride gas reacts, ...

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 Lithium in anhydrous hydrogen fluoride solution. The reaction process of Example 1 was repeated. Obtain 300g of lithium hexafluorophosphate product. Test results product purity greater than 99.9%, product free acid (in HF) 95ppm, moisture (Karl Fischer method) 5ppm, alkali metal ion content (in K, Na) 4ppm, heavy metal ion content (in Fe) 2ppm, Insoluble matter content 500ppm.

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Abstract

The invention relates to a method for preparing lithium hexafluorophosphate. The method comprises the following steps: (1), enabling anhydrous hydrogen fluoride and phosphorus pentoxide to react underthe protection of inert gas to prepare hexafluorophosphoric acid; (2), adding oleum to the hexafluorophosphoric acid under cooling stirring to prepare phosphorus pentafluoride gas; (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 the phosphorus pentafluoride gas at 40DEG C below zero, guiding the phosphorus pentafluoride gas to the anhydrous hydrogen fluoride solution containing the lithium fluoride, and reacting, crystallizing, separating and drying the phosphorus pentafluoride gas to obtain a pure lithium hexafluorophosphate product; and (5), continuously pumping the unreacted cooled phosphorus pentafluoride gas 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 has rich material resources and easily obtainable raw materials, low production cost, high reaction rate, high product quality and thorough reaction and can realize semi-continuous production by the series connection of double kettles.

Description

technical field [0001] The invention relates to a method for preparing lithium hexafluorophosphate, in particular to a method for preparing lithium hexafluorophosphate used as an electrolyte solution for 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. And when the lithium-ion secondary battery is charged, l...

Claims

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Application Information

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