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Synthesis method of a lithium hexafluorophosphate non-aqueous solvent method

A technology of lithium hexafluorophosphate and non-aqueous solvent, applied in the field of synthesis of lithium hexafluorophosphate, can solve the problems of inability to obtain lithium hexafluorophosphate, affecting the quality of lithium hexafluorophosphate, side effects of lithium fluoride, etc., and achieve the effects of improving product quality, reducing impurities and inhibiting decomposition

Inactive Publication Date: 2011-08-17
张家港市亚源高新技术材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The main disadvantages of the above synthesis process are: since lithium hexafluorophosphate is sensitive to temperature, it will start to decompose when the temperature is higher than 60°C, and lithium fluoride, which has side effects on the battery, will be produced after decomposition; and there will be impurities in the reaction product. Lithium oxyfluorophosphate; Therefore, the traditional synthesis process cannot obtain lithium hexafluorophosphate with high purity, which affects the quality of lithium hexafluorophosphate

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Embodiment 1

[0017] see figure 1 As shown, 50 liters of lithium fluoride anhydrous hydrogen fluoride solution with a concentration of 10% is added in advance in the reaction device 3, and gaseous phosphorus pentafluoride is passed into the reaction device 3 from the inlet 2, and the reaction temperature is controlled to be 10° C. to - 10°C, after reacting for about 240 minutes, freeze the reaction device 3 to -30°C while stirring continuously, and the reactant containing lithium hexafluorophosphate generated by the reaction is transferred from the output channel 4 to the solid product sedimentation device 5 for separation, and the separated mother liquor Through output channel 6, return to reaction device 3 by input channel 1 and continue to participate in the next batch of reactions. The solid product is transferred to drying device 9 by output channel 7. The temperature is 80 ° C and the volume ratio is nitrogen: phosphorus pentafluoride: The mixed gas of fluorine gas=96:2:2 enters the b...

Embodiment 2

[0019] see figure 1 As shown, 50 liters of lithium fluoride anhydrous hydrogen fluoride solution with a concentration of 10% is added in advance in the reaction device 3, and gaseous phosphorus pentafluoride is passed into the reaction device 3 from the inlet 2, and the reaction temperature is controlled to be 10° C. to - 10°C, after reacting for about 240 minutes, freeze the reaction device 3 to -25°C while stirring continuously, and the reactant containing lithium hexafluorophosphate generated by the reaction is transferred from the output channel 4 to the solid product sedimentation device 5 for separation, and the separated mother liquor Through the output channel 6, return to the reaction device 3 by the input channel 1 and continue to participate in the next batch of reactions. The solid product is transferred to the drying device 9 by the output channel 7. The temperature is 120 ° C, and the volume ratio is argon: phosphorus pentafluoride The mixed gas of =95:5 enters t...

Embodiment 3

[0021] see figure 1 As shown, 50 liters of lithium fluoride anhydrous hydrogen fluoride solution with a concentration of 10% is added in advance in the reaction device 3, and gaseous phosphorus pentafluoride is passed into the reaction device 3 from the inlet 2, and the reaction temperature is controlled to be 10° C. to - 10°C, after reacting for about 240 minutes, freeze the reaction device 3 to -22°C while stirring continuously, and the reactant containing lithium hexafluorophosphate generated by the reaction is transferred from the output channel 4 to the solid product sedimentation device 5 for separation, and the separated mother liquor Return to the reaction device 3 by the input channel 1 through the output channel 6 and continue to participate in the next batch of reactions. The solid product is transferred to the drying device 9 by the output channel 7. The temperature is 120 ° C and the volume ratio is argon: fluorine = 95 The mixed gas of :5 enters the bottom of the...

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Abstract

The invention discloses a synthesis method of a lithium hexafluorophosphate non-aqueous solvent method, which includes the steps of allowing gaseous phosphorus pentafluoride to react with anhydrous hydrogen fluoride solution of lithium fluoride to generate reaction product containing lithium hexafluorophosphate; freezing and crystallizing the reaction product after the reaction is finished; then separating the reaction product containing the lithium hexafluorophosphate by a solid product sedimentation device; and transferring the obtained solid product to a drying device for drying treatment. The drying treatment method includes the steps of heating the mixed gas of inert gas and fluorine or phosphorus pentafluoride gas which presents chemical reaction inertness with the lithium hexafluorophosphate, the hydrogen fluoride and the phosphorus pentafluoride, then introducing the mixed gas into the drying device to contact with the solid product so as to carry out the hydrogen fluoride remaining on the surface of the solid product, and finally obtaining a solid product, namely lithium hexafluorophosphate solid. The synthesis method has the advantages of effectively reducing impurities or restricting the generation of the impurities and being beneficial to the improvement of the product quality when the product carrying out drying.

Description

Technical field [0001] The present invention relates to a method for synthesizing lithium hexafluorophosphate, and in particular to a technology for synthesizing lithium hexafluorophosphate using a non-aqueous solvent method. Background technique [0002] Since the advent of lithium-ion batteries in the 1980s, they have become the first choice for high-performance secondary batteries due to their many superior properties, such as large specific energy, low self-discharge, long cycle life, fast charge and discharge, and no memory effect. [0003] Lithium salts known to be useful as electrolytes for secondary lithium ion batteries include LiAsF 6 ,LiPF 6 ,LiBF 4 ,LiClO 4 ,LiCF 3 SO 3 ,Li(CF 3 SO 3 ) 2 N, etc. Among them, lithium hexafluorophosphate is widely used commercially due to its good comprehensive properties, and its output is increasing day by day. [0004] Lithium-ion secondary batteries have high technical requirements for lithium hexafluorophosphate. Moist...

Claims

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Application Information

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IPC IPC(8): C01B25/455
Inventor 杨瑞甫
Owner 张家港市亚源高新技术材料有限公司
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