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Preparation method of lithium tetrafluorooxalatophosphate and lithium difluorodioxalatophosphate

A technology of lithium difluorobisoxalate phosphate and lithium tetrafluorooxalate phosphate, which is applied in chemical instruments and methods, lithium compounds, alkali metal compounds, etc., can solve problems such as high energy consumption and safety risks, hidden safety hazards, and risks. Achieve the effect of reducing energy consumption, increasing productivity and increasing safety

Active Publication Date: 2019-06-07
武汉海斯普林科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, the common preparation methods of tetrafluorolithium oxalate phosphate and lithium difluorobisoxalate phosphate have certain defects. For example, the method of CN 105218348 uses hydrogen fluoride and phosphorus pentafluoride as raw materials, and this method has certain hidden dangers in safety. and risk
In US2010267984, phosphorus pentafluoride not only participates in the reaction, but also requires high temperature in the reaction operation, so the energy consumption and safety risk of this route are higher

Method used

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  • Preparation method of lithium tetrafluorooxalatophosphate and lithium difluorodioxalatophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Bottom liquid configuration: under the protection of nitrogen, take 45.02g oxalic acid, 200g dimethyl carbonate and stir, take 79.1g pyridine dissolved in 100g dimethyl carbonate and stir evenly, slowly drop the pyridine solution into the oxalic acid solution, after the titration Stirring was continued for 30 min.

[0020] Configuration of titration solution: Under the protection of nitrogen, take 76g of lithium hexafluorophosphate and add it to 227.85g of dimethyl carbonate in batches, and stir while adding. After a uniform solution is formed, drop 108.64g of trimethylchlorosilane into the solution, and the titration is completed After forming a uniform solution, drop the titration solution into the bottom solution for the next step of reaction.

[0021] Set the temperature to -10°C. After the flask reaches the set temperature, slowly add the prepared titration solution into the bottom liquid. The dropping process takes 90 minutes. After the dropwise addition, continu...

Embodiment 2

[0024] Bottom liquid configuration: under the protection of nitrogen, take 99.07g oxalic acid, 200g dimethyl carbonate and stir, take 174.02g pyridine and dissolve it in 200g dimethyl carbonate, slowly drop the pyridine solution into the oxalic acid solution, after the titration Stirring was continued for 30 min.

[0025] Configuration of titration solution: Under the protection of nitrogen, take 76g of lithium hexafluorophosphate and add it to 227.85g of dimethyl carbonate in batches, and stir while adding. After a uniform solution is formed, drop 108.64g of trimethylchlorosilane into the solution, and the titration is completed After forming a uniform solution, drop the titration solution into the bottom solution for the next step of reaction.

[0026] Set the temperature to -10°C. After the flask reaches the set temperature, slowly add the prepared titration solution into the bottom liquid. The dropping process takes 90 minutes. After the dropwise addition, continue the he...

Embodiment 3

[0029] Bottom liquid configuration: Under nitrogen protection, take 99.04g oxalic acid, stir with 350g acetonitrile, take 74.91g imidazole and dissolve in 300g acetonitrile, slowly drop the imidazole solution into the oxalic acid solution, continue stirring for 30min after the titration is completed.

[0030] Configuration of titration solution: Under the protection of nitrogen, take 76g of lithium hexafluorophosphate and add it to 227.85g of acetonitrile in batches, and stir while adding. After a uniform solution is formed, 108.64g of trimethylchlorosilane is dropped into the solution. After the solution, the titration solution was dropped into the bottom solution to carry out the next step of reaction.

[0031] Set the temperature at 25°C. After the flask reaches the set temperature, slowly add the prepared titration solution into the bottom liquid, and the dropping process takes 60 minutes. As the reaction progresses, the bubbles in the solution gradually become more intens...

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Abstract

The invention relates to a preparation method of lithium tetrafluorooxalatophosphate and lithium difluorodioxalatophosphate. The method comprises the following steps: preparation of a titration solution: dissolving lithium hexafluorophosphate in an organic solvent, and adding trimethylchlorosilane into the solution; preparation of a base solution: dissolving oxalic acid into an organic solvent, preparing an organic alkali solution in the same way, adding the organic alkali into the oxalic acid solution, and stirring the solution; slowly dropwise adding the prepared titration solution into thereaction base solution, and when the molar ratio of lithium hexafluorophosphate to oxalic acid is 1:1.8-1:2.5 and the reaction temperature is 15-40 DEG C, carrying out a reaction to generate the lithium tetrafluorooxalatophosphate; when the molar ratio of lithium hexafluorophosphate to oxalic acid is 1:1.8-1:2.5 and the reaction temperature is 15-40 DEG C, carrying out a reaction to generate the lithium difluorodioxalatophosphate; after the reaction is finished, adjusting the temperature of the reaction system, continuously stirring the reaction product for a period of time, and filtering andrecrystallizing the reaction product to obtain the required products. The method is mild in reaction condition and easy to control, the solvent can be repeatedly used, the cost is saved, and the yieldis further increased.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a method for preparing lithium tetrafluorooxalate phosphate and lithium difluorobisoxalate phosphate. Background technique [0002] Lithium tetrafluorooxalate phosphate and lithium difluorobisoxalate phosphate can be used as excellent battery electrolyte additives. They can improve the thermal stability and hydrolytic stability of the electrolyte, even after the battery ages. Still in good shape. Therefore, for the electrolyte industry, lithium tetrafluorooxalate phosphate and lithium difluorobisoxalate phosphate are a class of substances that are expected to further reduce the use of lithium hexafluorophosphate, reduce costs, and improve battery performance. After the electrolyte formula matures, the market will respond to such substances Demand will increase. [0003] However, the common preparation methods of tetrafluorolithium oxalate phosphate and lithium difluo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/00
Inventor 周永妍周宜海王文潘君周国武
Owner 武汉海斯普林科技发展有限公司
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