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Lithium tetrafluorooxalatophosphate preparation method

A technology of lithium tetrafluorooxalate phosphate and lithium oxalate, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as adverse effects on battery performance and product quality degradation, and achieve Overcome the effect of large reaction consumption, short reaction time and improvement of product quality

Inactive Publication Date: 2019-04-23
TIANJIN JINNIU POWER SOURCES MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the product prepared by this method will have a certain content of chloride ions, resulting in a decline in product quality, which will adversely affect battery performance.

Method used

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  • Lithium tetrafluorooxalatophosphate preparation method
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  • Lithium tetrafluorooxalatophosphate preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] At room temperature, 101.9 g of lithium oxalate and 800 g of DMC were added to the jacketed reaction vessel 2 and stirred for 1 hour to form a uniform suspension of lithium oxalate and DMC. Add 65.17g of red phosphorus to the reaction vessel 1 in advance, then slowly pass in 200g of fluorine gas, pass a low-temperature cooling medium into the jacket to control the temperature, and then pass the phosphorus pentafluoride produced in the process into the reaction vessel 2 , The gas outlet rate is controlled to 2L / Min. During the process, always pay attention to temperature changes, and control the temperature below 30°C. After the gas is introduced, continue to stir for 4 hours. After filtration, after concentration and crystallization, 174.43 g of product was obtained, of which the theoretical output was 202 g, and the product yield reached 86.35%. The product purity of the obtained product is 99.96%, the water content is 4.8 ppm, and the acid content is 28 ppm.

[0035] Ta...

Embodiment 2

[0038] At room temperature, 110.2 g of lithium oxalate and 850 g of DMC were added to a jacketed reaction vessel 2 and stirred for 1 hour to form a uniform suspension of lithium oxalate and DMC. Into the reaction vessel 1, 72g of red phosphorus was introduced in advance, and then 200g of fluorine gas was slowly introduced, and a low-temperature cooling medium was introduced into the jacket to control the temperature, and then the phosphorus pentafluoride produced in the process was introduced into the reaction vessel 2 In the process, the gas outlet rate is controlled to 2L / Min. During the process, pay attention to temperature changes at all times, and control the temperature below 30°C. After the gas is introduced, continue to stir for 4 hours. After filtration, after concentration and crystallization, 175.23g of product was obtained, of which the theoretical output was 210g, and the product yield reached 86.74%. The product purity of the obtained product is 99.8%, the water c...

Embodiment 3

[0042] At room temperature, 105 g of lithium oxalate and 820 g of DMC were added to the jacketed reaction vessel 2 and stirred for 1 hour to form a uniform suspension of lithium oxalate and DMC. Add 68g of white phosphorus to the reaction vessel 1 in advance, and then slowly pass in 200g of fluorine gas, pass a low-temperature cooling medium into the jacket to control the temperature, and then pass the phosphorus pentafluoride produced in the process into the reaction vessel 2. The export rate is controlled to 2L / Min. During the process, keep an eye on the temperature change, and control the temperature below 30°C. After the gas is introduced, continue to stir for 4 hours. After filtration, after concentration and crystallization, 174.52 g of product was obtained, of which the theoretical output was 205 g, and the product yield reached 86.4%. The product purity of the obtained product is 99.90%, the water content is 5.2 ppm, and the acid content is 20 ppm.

[0043] Table Three

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Abstract

The invention discloses a lithium tetrafluorooxalatophosphate preparation method, which specifically comprises: introducing phosphorus pentafluoride generated by a reaction of elemental phosphorus andfluorine gas into a reaction kettle with a suspension formed from lithium oxalate and an organic solvent through a buffer tank, and carrying out a reaction, wherein the gas flow rate is controlled at1-5 L / min, preferably 2 L / min, the pressure change and the temperature change of the reaction kettle are real-timely monitored during the reaction, the temperature is maintained at 10-40 DEG C duringthe reaction, preferably 30 DEG C, the pressure is maintained at 0-0.5 MPa, preferably 0.1 MPa, a molar ratio of phosphorus pentafluoride to lithium oxalate is 2.2-2:1, preferably 2.05:1, a completestirring reaction is performed for 1-3 h, preferably 2 h, concentration crystallization is performed after filtering, and filtering and drying are sequentially performed to obtain the desired product.A purpose of the present invention is to improve the lithium tetrafluorooxalatophosphate preparation method based on the problems and the disadvantages of the existing process so as to reduce the preparation cost of the lithium tetrafluorooxalatophosphate and improve the quality of the product.

Description

Technical field [0001] The invention relates to the technical field of lithium ion battery material manufacturing, and more specifically to a method for preparing lithium tetrafluorooxalate phosphate, an additive used for non-aqueous electrolyte of lithium ion batteries. Background technique [0002] Lithium tetrafluorooxalate phosphate is mainly used as an additive for non-aqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors. This kind of additive can form a more stable SEI film structure on the surface of the battery cathode material, effectively improving the cycle performance and high temperature performance of the battery. The currently known preparation methods of such additives mainly include the following. [0003] US20100267984 mentions mixing lithium hexafluorophosphate and lithium oxalate in a pressure vessel, and heating to 150°C to 180°C for reaction, then dissolving the obtained product in acetonitrile, filtering, removing the solven...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65742
Inventor 王坤赵庆云刘大凡安峰袁莉张丽红张冬青
Owner TIANJIN JINNIU POWER SOURCES MATERIAL
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