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Preparation method of lithium hexafluorophate

A technology of lithium hexafluorophosphate and hexafluorophosphate, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of low yield and achieve the effects of environmental friendliness, mild reaction conditions and low corrosion

Inactive Publication Date: 2012-09-12
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Prepare lithium hexafluorophosphate by this method, although no toxic gas such as hydrogen fluoride is used in the preparation process, the safety is improved, but the yield of this method is low, and only an organic solution of lithium hexafluorophosphate can be obtained

Method used

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  • Preparation method of lithium hexafluorophate
  • Preparation method of lithium hexafluorophate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Potassium hexafluorophosphate and lithium chloride with a molar ratio of 2.2:1 were dissolved in acetonitrile respectively to form solutions with a concentration of 10% and 20%; In the reaction kettle of the reactor, in dry air and under normal pressure, react at a temperature of 30°C for 8h; filter the above-mentioned feed liquid to remove insoluble matter, and evaporate the solution under reduced pressure at a temperature of 65°C to remove part of the solvent, and then dry In the air, cool and crystallize at a temperature of 10°C, filter, recrystallize, and recover the mother liquor to obtain the complex Li(CH 3 EN) 4 PF 6 , to obtain pure lithium hexafluorophosphate after vacuum drying. According to the alkali titration method, HF was not detected, and the moisture content measured by the Karl Fischer method was 15ppm. The impurity indicators detected by ICP spectroscopy met the requirements of HG / T 4066-2008, and the obtained lithium hexafluorophosphate had a puri...

Embodiment 2

[0036] Dissolve sodium hexafluorophosphate and lithium chloride with a molar ratio of 3:1 in ethylene glycol dimethyl ether and ethanol respectively to form solutions with a concentration of 30% and 25%; add the above two solutions with In a reactor with a stirrer, a thermometer and a reflux condenser, react at a temperature of 25°C for 2 hours under a nitrogen atmosphere and at normal pressure; filter the above-mentioned feed liquid to remove insoluble matter, and evaporate the solution under reduced pressure at a temperature of 65°C. Remove part of the solvent, cool and crystallize at -20°C under a nitrogen atmosphere, filter, recrystallize, and recover the mother liquor to obtain the complex LiPF of lithium hexafluorophosphate and ethylene glycol dimethyl ether 6 (C 4 h 10 o 2 ) 2 , to obtain pure lithium hexafluorophosphate after vacuum drying. According to the alkaline titration method, HF was not detected, and the moisture content measured by the Karl Fischer method ...

Embodiment 3

[0038]Dissolve ammonium hexafluorophosphate and lithium chloride with a molar ratio of 2.05:1 in acetone and acetonitrile respectively to form solutions with a concentration of 15% and 40%; and a reflux condenser reaction kettle, under a nitrogen atmosphere, in a normal pressure environment, react at a temperature of 0°C for 5.5h; filter the above-mentioned feed liquid to remove insoluble matter, and evaporate the solution under reduced pressure at a temperature of 20°C to remove part of the solvent , under a nitrogen atmosphere, cooled and crystallized at a temperature of -30°C, filtered, recrystallized, recovered the mother liquor, and obtained the complex Li(CH 3 EN) 4 PF 6 , to obtain pure lithium hexafluorophosphate after vacuum drying. According to the alkaline titration method, HF was not detected, and the moisture content was 16ppm according to the Karl Fischer method. The impurity indicators detected by ICP spectroscopy met the requirements of HG / T 4066-2008, and th...

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Abstract

The invention discloses a preparation method of lithium hexafluorophate, which is characterized in that the preparation method comprises the following steps of respectively dissolving dry hexafluorophosphate and dry lithium chloride into an organic solvent according to a molar ratio of 0.5-3.5:1 and preparing into solution with a concentration of 10-40 percent; adding the organic solvent and the solution into a reaction kettle with an agitator, a thermometer and a reflux condenser, reacting for 2-8 hours at a temperature of 0-40 DEG C under the inert atmosphere and the constant-pressure environment; filtering feed liquid under the inert atmosphere, removing undissolved substances, carrying out pressure reduction and evaporation on the solution at a temperature of 20-100 DEG C, removing a part of solvents, cooling and crystallizing at a temperature of 30 below zero-10 DEG C, filtering and recovering mother liquor to obtain a lithium hexafluorophate monomer or a complex of the lithium hexafluorophate monomer with the solvent; and re-crystallizing and vacuum-drying to obtain obtaining the lithium hexafluorophate with a purity of 99.92-99.97 percent.

Description

technical field [0001] The invention relates to a preparation method of lithium hexafluorophosphate, belonging to the technical field of preparation of lithium hexafluorophosphate. Background technique [0002] The current industrialized lithium hexafluorophosphate preparation method is the hydrogen fluoride solvent method or its improved method, which uses phosphorus pentafluoride or phosphorus pentachloride, lithium fluoride or lithium chloride as raw materials, dissolves and reacts in anhydrous hydrogen fluoride medium. After the reaction is completed, the insoluble matter is filtered out, and the remaining solution is subjected to low-temperature crystallization and dried to obtain the lithium hexafluorophosphate product. Lithium hexafluorophosphate prepared by this method often contains a large amount of hydrogen fluoride, because lithium hexafluorophosphate and hydrogen fluoride form adducts during the preparation process, it is difficult to remove the hydrogen fluorid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455H01M10/056
CPCY02E60/10
Inventor 王辛龙李宣丽张志业杨林傅玉信
Owner SICHUAN UNIV
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