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Synthetic method of oxalate lithium phosphate salt compound

A salt compound, lithium phosphate technology, 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 the performance of non-aqueous electrolyte batteries and difficulty in industrialization, Achieve the effects of low cost, high reaction yield and simple reaction operation

Active Publication Date: 2020-11-17
微宏先进材料公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the by-products produced in its manufacturing method are HCl and silicon tetrafluoride or silicon tetrachloride, which will adversely affect the performance of non-aqueous electrolyte batteries.
In addition, the large amount of heat generated during the reaction and the strong corrosiveness of HCl also make this synthesis difficult to industrialize

Method used

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  • Synthetic method of oxalate lithium phosphate salt compound
  • Synthetic method of oxalate lithium phosphate salt compound
  • Synthetic method of oxalate lithium phosphate salt compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Add 0.124mol ammonium hexafluorophosphate, 0.254mol bistrimethylsilyl oxalate, 0.150mol lithium hydride and anhydrous diethyl carbonate to a 500ml round bottom flask in a glove box, and react at 80°C for 24h until Gas is no longer produced. The solvent was then removed to obtain a white solid with a yield of 94%. NMR test results show that the ratio of LiDFBOP:LiTFOP is 72:1, and the molar percentage of LiDFBOP is 98.6%.

Embodiment 2

[0040] Add 0.124mol ammonium hexafluorophosphate, anhydrous diethyl carbonate, and 0.273mol bistrimethylsilyl oxalate to a 500ml round bottom flask in a glove box, and react at 100°C for 1h until no gas is produced . Then add 0.118mol lithium hydride to continue the reaction, and react at 100°C for 1h. The solvent was then removed to give a white solid with a yield of 89%. NMR test results show that the ratio of LiDFBOP:LiTFOP is 20:1, and the molar percentage of LiDFBOP is 95.2%.

Embodiment 3

[0042] Same as Example 2, except that the addition amounts of ammonium hexafluorophosphate and bistrimethylsilyl oxalate are 0.124mol and 0.254mol respectively, and the product yield is 88%. The NMR test results show that the ratio of LiDFBOP:LiTFOP is 72:1, the molar percentage of LiDFBOP is 98.6%.

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Abstract

The invention discloses a synthetic method of an oxalate lithium phosphate salt compound. The synthetic method has the advantages of low reaction temperature and high product yield, and comprises thefollowing steps: mixing ammonium hexafluorophosphate or amine salt, silicon-based oxalate and lithium hydride in a non-aqueous solvent, and conducting reacting to obtain the oxalate lithium phosphatesalt compound. No chloride ions are introduced in the synthesis process, purity can reach 99%, and the produced compound can be directly used as an electrolyte additive without further treatment.

Description

technical field [0001] The invention relates to a method for synthesizing lithium oxalatophosphate compounds. Background technique [0002] Lithium oxalatophosphate compounds are generally used as additives for nonaqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors. Commonly used lithium oxalatophosphate compounds include lithium difluorobis(oxalato)phosphate, and the Japanese patent with the publication number JP2003137890A discloses a manufacturing method of lithium difluorobis(oxalato)phosphate in an organic solvent Lithium hexafluorophosphate containing SiCl 4 Reaction under the reaction aid. However, HCl and silicon tetrafluoride or silicon tetrachloride are by-products generated in its manufacturing method, which adversely affect the performance of the nonaqueous electrolyte battery. In addition, the large amount of heat generated during the reaction and the strong corrosiveness of HCl also make this synthesis difficult to industri...

Claims

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Application Information

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IPC IPC(8): C07F9/6574H01M10/0525H01M10/0567
CPCC07F9/65742H01M10/0567H01M10/0525Y02E60/10
Inventor 贺伟董剑文娟·刘·麦蒂斯熊亚丽郑宣鸣张志刚
Owner 微宏先进材料公司
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