Preparation method of lithium tetrafluorooxalate phosphate

A technology of lithium tetrafluorooxalate phosphate and lithium hexafluorophosphate is applied in the field of lithium ion batteries, which can solve the problems of large reaction consumption, danger and complex reaction, and achieve the effects of short reaction time, low risk factor and simple process

Inactive Publication Date: 2018-12-21
中山弘毅新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has complex reactions and many steps, and the product is accompanied by lithium hexafluorophosphate, which is difficult to separate. At the same time, anhydrous hydrofluoric acid is used twice in the preparation process, and the reaction consumes a lot and is dangerous, so it is not suitable for industrial production.

Method used

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  • Preparation method of lithium tetrafluorooxalate phosphate

Examples

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Comparison scheme
Effect test

Embodiment 1

[0034] In a dry argon glove box, 228 g of dry ethyl methyl carbonate (EMC) was added to a three-necked flask, and lithium hexafluorophosphate (LiPF 6 ) 76.0g (0.5mol), dissolve, then drop into the flask 41.6g (0.2mol) of phosphorus pentachloride, one mouth of the flask is connected with a gas conduit with a valve, and the other two mouths are plugged with stoppers. The flask was taken out of the glove box, immersed in an ice-water bath and stirred. After half an hour, argon gas was slowly passed into the flask, and a stopper was opened at the same time, so that the inside of the flask was in an atmosphere protected by argon gas, and 45.0 g (0.5 mol) of anhydrous oxalic acid was quickly added to the flask, and then fully stirred. Slowly increase the temperature of the water bath to above 10°C, the reaction begins, and the generated gas flows into the solution containing sodium hydroxide for absorption. Continue to raise the temperature slowly until the solid dissolves, and the...

Embodiment 2

[0038] In a dry argon glove box, 304.0 g of dry dimethyl carbonate (DMC) was added to a three-necked flask, and lithium hexafluorophosphate (LiPF 6) 38.0g (0.25mol) for dissolution, then put 22.5g (0.25mol) of anhydrous oxalic acid into the flask, take the flask out of the glove box, immerse it in a water bath at 35°C and stir, and keep stirring the mixture. Slowly add 20.8 (0.1 mol) g of phosphorus pentachloride using a solid feeder, and the reaction begins to take place. The generated gas flows into a solution containing sodium hydroxide for absorption. It takes 1.5 hours to add phosphorus pentachloride, and then keep it at 35°C for one hour. No gas is emitted from the reaction, indicating that the reaction is complete. Under the protection of argon flow, 1800 mL of cyclohexane was added into the flask, and stirred slowly until crystals were precipitated. Lower the temperature of the water bath to -10°C, stop stirring, and after the crystals settle, filter, wash with cyclo...

Embodiment 3

[0041] In a dry argon glove box, 152.0 g of dry diethyl carbonate (DEC) was added to a three-necked flask, and lithium hexafluorophosphate (LiPF 6 ) 38.0g (0.25mol) for dissolution, then put 31.0g (0.25mol) of anhydrous ammonium oxalate into the flask, take the flask out of the glove box, immerse it in a water bath at 40°C and stir, and keep stirring the mixture. Phosphorus trichloride 22.9g (0.16mol) was slowly added dropwise using a constant pressure dropping funnel, and the reaction began to take place. The generated gas flows into a solution containing sodium hydroxide for absorption. It takes 1 hour to add phosphorus trichloride dropwise, and then keep the temperature at 40°C for 1 hour. If there is no gas released from the reaction, it means that the reaction is over. Under the protection of argon flow, 800 mL of dichloroethane was added to the flask, and stirred slowly until crystals were precipitated. Lower the temperature of the water bath to 0°C, stop stirring, and...

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Abstract

The invention discloses a preparation method of lithium tetrafluorooxalate phosphate. The method is characterized by comprising the following steps: (1) dissolving lithium hexafluorophosphate in an aprotic solvent, adding oxalic acid or ammonium oxalate, phosphorus pentachloride or phosphorus trichloride, and carrying out a reaction to obtain lithium tetrafluorooxalate phosphate; (2) adding a poorsolvent to enable the generated lithium tetrafluorooxalate phosphate to be crystallized; (3) filtering, washing, and drying to obtain the lithium tetrafluorooxalate phosphate. The method provided bythe invention is simple in process, non-toxic in raw materials, low in danger coefficient, short in reaction time and high in yield, can effectively control the contents of metal ions and anionic impurities, and can be used for preparing the high-purify lithium tetrafluorooxalate phosphate target product.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to a method for preparing lithium tetrafluorooxalate phosphate which can be used as an additive for lithium ion batteries for nonaqueous electrolyte batteries. Background technique [0002] Lithium tetrafluorooxalate phosphate can be used as an additive for lithium-ion batteries. The known preparation method of tetrafluorolithium oxalate phosphate, such as patent document 1 (patent name: preparation method of tetrafluoro(oxalato)phosphate solution; patent number: CN201380028506.7), the method is to dissolve in an organic solvent Lithium hexafluorophosphate is reacted with oxalic acid in the presence of silicon tetrachloride as a reaction aid. In this method, only a solution containing lithium tetrafluorooxalate phosphate can be obtained, and the organic solvent cannot be removed. Chloride ions, free acids and other soluble impurities are difficult to remove, and the product has...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C55/07
CPCC07C51/412C07C55/07
Inventor 周文超赵喜波
Owner 中山弘毅新材料有限公司
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