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Lithium difluoro-bis(oxalate)phosphate as well as preparation method and application thereof

A technology of difluorobis-oxalate lithium phosphate and bis-oxalate lithium phosphate, which is applied in chemical instruments and methods, secondary batteries, electrochemical generators, etc. Low problems, to achieve the effect of ensuring purity and quality, avoiding complicated operations, and simple and convenient operation

Active Publication Date: 2021-09-03
SHENZHEN YANYI NEW MATERIALS CO LTD
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Problems solved by technology

[0003] At present, in the preparation methods of lithium difluorobisoxalate phosphate that have been disclosed, most of the preparation methods use lithium hexafluorophosphate and silicon tetrachloride as raw materials to react, but lithium hexafluorophosphate is easily partially decomposed into pentafluorophosphate during the reaction process. Phosphate, or react with other oxygen-containing substances to form lithium difluorophosphate, which is difficult to remove. At the same time, in the process of using silicon additives for the reaction, a large amount of silicon tetrafluoride and hydrogen chloride gas will be produced, which is difficult to separate and utilization, technical solutions have high security risks, causing great difficulties in industrialization
[0004] CN102216311B discloses a kind of manufacture method of lithium difluorobis(oxalato)phosphate solution, it uses hexafluorophosphoric acid, lithium oxalate and silicon tetrachloride as raw material to prepare lithium difluorobisoxalate phosphate, and its described method can produce a large amount of Hydrogen chloride and silicon fluoride, these highly corrosive acidic gases have very high requirements on equipment, and are difficult to separate from the product, and the content of chloride ions and acid value in the product are difficult to control. This method has hidden dangers and risks in terms of safety and reliability. risk
[0005] CN111690010A discloses a preparation method of lithium tetrafluorooxalate phosphate and lithium difluorobisoxalate phosphate, which uses lithium hexafluorophosphate, oxalic acid and silazane to react to prepare lithium difluorobisoxalate phosphate, and the method produces difficult separation of ammonia and fluorine Silane is two kinds of gases, and the post-treatment is cumbersome, and the three wastes are produced in a large amount, which is not conducive to industrial production
[0006] The above-mentioned scheme has the problems of low safety, poor reliability or large output of three wastes, which is not conducive to industrial production. Therefore, the development of a kind of lithium difluorobisoxalate phosphate with high safety and reliability, environmental protection and favorable industrial production is very necessary

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  • Lithium difluoro-bis(oxalate)phosphate as well as preparation method and application thereof
  • Lithium difluoro-bis(oxalate)phosphate as well as preparation method and application thereof

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Embodiment 1

[0057] This embodiment provides a lithium difluorobisoxalate phosphate, the preparation method of the lithium difluorobisoxalate phosphate is as follows:

[0058] (1) In a glove box with a nitrogen atmosphere with a moisture content of less than 10ppm, add 250g of dimethyl carbonate dehydrated to 8ppm into a three-necked reaction flask, and simultaneously add 15.19g (0.1mol) of lithium hexafluorophosphate and 25.38g (0.2mol) of oxalyl chloride ), take the three-necked reaction bottle out of the glove box, place it on a constant temperature magnetic stirring device, heat it to 30°C, and add 64.95g (0.4mol) of hexamethyldisiloxane dropwise to the three-necked reaction via a constant pressure dropping funnel In the bottle, the molar ratio of lithium hexafluorophosphate to oxalyl chloride to hexamethyldisiloxane is 1:2:4, and the reaction is carried out with sufficient stirring, and the trimethylfluorosilane gas generated during the reaction is introduced into alkali such as potass...

Embodiment 2

[0061] This embodiment provides a lithium difluorobisoxalate phosphate, the preparation method of the lithium difluorobisoxalate phosphate is as follows:

[0062] (1) In a glove box with a nitrogen atmosphere with a moisture content of less than 10ppm, add 152g of diethyl carbonate dehydrated to 7ppm into a three-necked reaction flask, and simultaneously add 15.19g (0.1mol) of lithium hexafluorophosphate and 30.46g (0.24mol) of oxalyl chloride ), take the three-necked reaction bottle out of the glove box, place it on a constant temperature magnetic stirring device, heat it to 60°C, and add 73.07g (0.45mol) of hexamethyldisiloxane dropwise to the three-necked reaction via a constant pressure dropping funnel In the bottle, the molar ratio of lithium hexafluorophosphate, oxalyl chloride, and hexamethyldisiloxane is 1:2.4:4.5, fully stirred for reaction, and the trimethylfluorosilane gas generated during the reaction is introduced into alkali such as potassium hydroxide solution A...

Embodiment 3

[0065] This embodiment provides a lithium difluorobisoxalate phosphate, the preparation method of the lithium difluorobisoxalate phosphate is as follows:

[0066] (1) In a glove box with a nitrogen atmosphere with a moisture content of less than 10ppm, add 300g of ethyl methyl carbonate dehydrated to 6ppm into a three-necked reaction flask, and simultaneously add 15.19g (0.1mol) of lithium hexafluorophosphate and 27.92g (0.22mol) of oxalyl chloride ), take the three-necked reaction bottle out of the glove box, place it on a constant temperature magnetic stirring device, heat it to 40°C, and add 68.20 g (0.42 mol) of hexamethyldisiloxane dropwise to the three-necked reaction via a constant pressure dropping funnel In the bottle, the molar ratio of lithium hexafluorophosphate, oxalyl chloride, and hexamethyldisiloxane is 1:2.2:4.2, fully stirred for reaction, and the trimethylfluorosilane gas generated during the reaction is introduced into alkali such as potassium hydroxide solu...

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Abstract

The invention provides lithium difluoro-bis(oxalate)phosphate as well as a preparation method and application thereof. The preparation method comprises the following steps: (1) mixing oxalyl chloride and lithium hexafluorophosphate with a non-aqueous solvent, adding siloxane, and reacting to obtain a lithium difluoro-bis (oxalate)phosphate solution; and (2) adding a poor solvent into the lithium difluoro-bis(oxalate)phosphate solution for crystallization treatment to obtain the lithium difluoro-bis(oxalate)phosphate. According to the method, lithium hexafluorophosphate, oxalyl chloride, hexamethyldisiloxane and other raw materials are adopted for preparing the difluoro-bis (oxalate)phosphate, and the method is few in side reaction, few in impurities, high in product purity and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to lithium difluorobisoxalate phosphate, its preparation method and application. Background technique [0002] Lithium-ion batteries are mainly composed of positive electrodes, negative electrodes, separators, electrolytes, etc. The electrolytes are mainly composed of electrolytes and organic solvents. The electrolyte is an active component that connects the positive and negative electrodes and is an important factor related to battery performance. Electrolyte additives are the most important components in lithium-ion battery electrolytes except for electrolytes and organic solvents. Appropriate additives can play a key role in enhancing the performance of lithium-ion batteries. Lithium difluorobisoxalate phosphate is mainly used in non-aqueous electrolytes such as lithium-ion batteries and lithium-ion capacitors. Lithium difluorobisoxalate phosphate can improve the high t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574H01M10/0567
CPCC07F9/65748H01M10/0567H01M2300/0017Y02E60/10H01M10/052
Inventor 岳敏余意王献明
Owner SHENZHEN YANYI NEW MATERIALS CO LTD
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