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Process for preparing lithium hexafluorophosphate by organic solvent method

A technology of lithium hexafluorophosphate and organic solvent, applied in the field of preparing lithium hexafluorophosphate by organic solvent method, can solve the problems of low efficiency, low yield, low purity and the like, and achieve the effects of low production cost, abundant sources and high reaction efficiency

Inactive Publication Date: 2011-09-14
CENT SOUTH UNIV +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Therefore, the present invention provides a new process for preparing lithium hexafluorophosphate by an organic solvent method, and avoids technical problems (low yield, low purity, low efficiency, etc.) and energy consumption problems in traditional methods

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] In a closed dry nitrogen-protected glove box, take 21g (0.1mol) of phosphorus pentachloride and 120mL of propylene carbonate and mix them evenly in reactor A, take 2.1g (0.08mol) of lithium fluoride and 0.06g of PVP- 40000 and 100mL acetonitrile were mixed and stirred evenly in reactor B.

[0044] After connecting the reaction device, pass high-purity nitrogen into it for 10 minutes to discharge the air. The temperatures of reactors A and B were controlled at -20°C and 0°C, respectively, and a total of 20 g (1 mol) of anhydrous hydrofluoric acid was slowly added dropwise to reactor A while stirring magnetically, and the drops were completed within 3 hours. After reacting for 15 hours, slowly pass nitrogen into the reaction device for 20 minutes to discharge the residual acid gas therein.

[0045] After the reaction, the solid residue in the reaction slurry was filtered out. Collect the filtrate, take it out of the glove box after sealing, and cool and crystallize at -...

Embodiment 2

[0048] In a closed dry nitrogen-protected glove box, take 33g (0.16mol) of phosphorus pentachloride and 150mL of dimethyl carbonate and mix them evenly in reactor A, take 3.6g (0.14mol) of lithium fluoride and 0.09g of PEO Mix -6000 and 150mL acetonitrile in reactor B and stir evenly.

[0049] After connecting the reaction device, pass high-purity nitrogen into it for 10 minutes to discharge the air. The temperatures of reactors A and B were controlled at 0°C and 20°C respectively, and a total of 28 g (1.4 mol) of anhydrous hydrofluoric acid was slowly added dropwise to reactor A while stirring magnetically, and the drops were completed within 3 hours. After reacting for 12 hours, slowly pass nitrogen into the reaction device for 20 minutes to discharge the residual acid gas therein.

[0050] After the reaction, the solid residue in the reaction slurry was filtered out. Collect the filtrate, take it out of the glove box after sealing, and cool and crystallize at -30°C. The ...

Embodiment 3

[0053] In a closed dry nitrogen-protected glove box, take 19g (0.09mol) phosphorus pentachloride and 120mL diethyl carbonate and mix them evenly in reactor A, take 1.6g (0.06mol) lithium fluoride and 0.06g PEO Mix -6000 and 100mL acetonitrile in reactor B and stir evenly.

[0054] After connecting the reaction device, pass high-purity nitrogen into it for 10 minutes to discharge the air. The temperatures of reactors A and B were controlled at -20°C and 0°C respectively, and 18 g (0.9 mol) of anhydrous hydrofluoric acid was slowly added dropwise to reactor A while stirring magnetically, and the drops were completed within 3 hours. After reacting for 15 hours, slowly pass nitrogen into the reaction device for 20 minutes to discharge the residual acid gas therein.

[0055] After the reaction, the solid residue in the reaction slurry was filtered out. Collect the filtrate, take it out of the glove box after sealing, and cool and crystallize at -35°C. The crystals were filtered ...

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Abstract

The invention discloses a process for preparing lithium hexafluorophosphate by adopting an organic solvent and solubilizer method. The process comprises the following steps of: reacting liquid anhydrous hydrofluoric acid with phosphorus pentachloride to generate phosphorus pentafluoride gas; reacting the phosphorus pentafluoride with lithium fluoride in an organic solvent dissolved with less solubilizer to generate lithium hexafluorophosphate; and filtering reaction slurry to obtain the residual lithium fluoride, cooling down a filtrate for crystallizing, filtering and vacuum drying to obtain a high-purity lithium hexafluorophosphate product. In the process for preparing the lithium hexafluorophosphate by adopting the organic solvent and solubilizer method disclosed by the invention, various raw materials are cheap and easy to obtain, and the production cost is low; the organic solvent with a few dissolved solubilizers is taken as a reaction medium, thus continuous production is easy to implement due to the reaction conditions, the reaction efficiency is high, the yield of the lithium hexafluorophosphate product is over 92%, and the purity of the lithium hexafluorophosphate product can reach more than 99.9%; in addition, the lithium hexafluorophosphate product prepared by the process disclosed by the invention is suitable for being used as an electrolyte of lithium ion batteries and the like.

Description

technical field [0001] The invention relates to a process for preparing lithium hexafluorophosphate by an organic solvent method, in particular to a new process for preparing lithium hexafluorophosphate as an electrolyte material of a lithium ion secondary battery by an organic solvent method. Background technique [0002] The organic electrolyte of lithium-ion secondary batteries is mainly composed of three parts: (1) electrolyte lithium salt; (2) organic solvent; (3) additives. The electrolyte lithium salt used in the electrolyte of lithium-ion secondary batteries must have high electrical conductivity, good chemical and electrochemical stability, wide usable temperature range, and good safety. Lithium hexafluorophosphate (LiPF 6 ) has good electrical conductivity and electrochemical stability, and the disposal of waste batteries is simple, has little impact on the ecological environment, and also has very outstanding oxidation resistance stability. Therefore, lithium hex...

Claims

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Application Information

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IPC IPC(8): C01B25/455
Inventor 潘春跃肖跃龙喻桂朋唐新村程邦宇
Owner CENT SOUTH UNIV
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