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Preparation method of lithium difluorobisoxalate phosphate solution

A technology of lithium difluorobisoxalate phosphate and oxalic acid solution, which is applied in the field of electrolyte, can solve the problems of large environmental pollution of by-products, unsuitability for industrialization, complicated preparation methods, etc., and achieve simple post-reaction treatment, increase feasibility, and reaction Effects in simple steps

Active Publication Date: 2019-09-06
DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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Problems solved by technology

[0004] Aiming at the problems in the prior art of preparing lithium difluorobisoxalate phosphate products such as complex preparation method, difficulty in removing impurities, great environmental pollution by by-products and unsuitability for industrialization, the present invention provides a method for preparing lithium difluorobisoxalate phosphate solution, The obtained solution can be directly used as a lithium salt electrolyte material for a lithium-ion battery without purification, and the reaction raw materials of this method are cheap and easy to obtain, the operation is simple, and the by-products are environmentally friendly, and are suitable for industrial production

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  • Preparation method of lithium difluorobisoxalate phosphate solution
  • Preparation method of lithium difluorobisoxalate phosphate solution
  • Preparation method of lithium difluorobisoxalate phosphate solution

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[0040] 2. Preparation of lithium difluorobisoxalate phosphate solution

[0041] Add lithium hexafluorophosphate to the above-mentioned two (N-succinimidyl) oxalic acid solution, react, and process after the reaction to obtain difluorobisoxalate lithium phosphate solution, the reaction equation is as follows:

[0042]

[0043] In some embodiments, the molar ratio of lithium hexafluorophosphate to bis(N-succinimidyl)oxalic acid is 1:2-2.2, for example: 1:2, 1:2.1, 1:2.2.

[0044] The operation of adding lithium hexafluorophosphate needs to be carried out in an inert gas environment with a moisture content of less than 10 ppm, such as in a glove box. The temperature at the time of addition was controlled at 0°C.

[0045] The reaction temperature is 30-80° C., and the reaction time is 4-8 hours.

[0046] In some embodiments, the reaction temperature is 50-80°C, for example: 50°C, 55°C, 60°C, 65°C, 70°C, 75°C, 80°C, etc.

[0047] Non-limiting examples of the reaction time inclu...

Embodiment 1

[0054] In a 500mL three-necked flask, add 200g of dimethyl carbonate, 57.5g (0.504mol) of N-hydroxysuccinimide and 63g (0.496mol) of oxalyl chloride, and react at 60°C for 9h under the protection of nitrogen to produce The tail gas can be absorbed by a low-concentration sodium hydroxide solution; after the reaction is completed, feed dry nitrogen into the reaction solution at 80°C for 5 hours to remove excess oxalyl chloride and HCl to obtain bis(N-succinimidyl)oxalic acid solution. Then, the reaction flask containing bis(N-succinimidyl) oxalic acid solution (containing 0.248mol bis(N-succinimidyl) oxalic acid) was transferred to the glove box, and 19 g (0.125 mol) Lithium hexafluorophosphate, after the lithium hexafluorophosphate is completely dissolved, transfer the flask to an oil bath at a temperature of 50°C, and react for 5 hours under the protection of nitrogen. 5-diketone, after filtration, a lithium difluorobisoxalate phosphate solution was obtained.

[0055] The ob...

Embodiment 2

[0060] In a 1000mL three-necked flask, add 500g of dimethyl carbonate, 172.6g (1.514mol) of N-hydroxysuccinimide and 126g (0.992mol) of oxalyl chloride, and react at 80°C for 9h under the protection of nitrogen to produce The tail gas can be absorbed by a low-concentration sodium hydroxide solution; after the reaction is completed, feed dry nitrogen into the reaction solution at 80°C for 5 hours to remove excess oxalyl chloride and HCl to obtain bis(N-succinimidyl)oxalic acid solution. Then, the reaction flask containing bis(N-succinimidyl) oxalic acid solution (containing 0.757mol bis(N-succinimidyl) oxalic acid) was transferred to the glove box, and 56.9 g (0.374 mol) lithium hexafluorophosphate, after the lithium hexafluorophosphate is completely dissolved, transfer the flask to an oil bath at a temperature of 60°C, and react for 5 hours under the protection of nitrogen, after the reaction, cool the reaction solution to 0°C, and precipitate solid 1-fluoropyrrolidine-2, 5-d...

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Abstract

The invention provides a preparation method of a lithium difluorobisoxalate phosphate solution, and the method comprises the following steps: 1) reacting N-hydroxysuccinimide and oxalyl chloride in anon-aqueous solvent to obtain a di (N-succinimido) oxalic acid solution; and 2) adding lithium hexafluorophosphate into the di (N-succinimido) oxalic acid solution, and reacting to obtain the lithiumdifluorobisoxalate phosphate solution. According to the preparation method, the obtained solution can be directly used for lithium salt electrolyte materials of lithium ion batteries without further purification, and the method has the advantages of cheap and easily available reaction raw materials, simple operation, environmental friendliness of byproducts, and suitability for industrial production.

Description

technical field [0001] The invention belongs to the technical field of electrolytes, and in particular relates to a preparation method of lithium difluorobisoxalate phosphate solution. Background technique [0002] Lithium difluorobisoxalate phosphate is mainly used as an additive for nonaqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors. After adding this kind of additive, the electrolyte has excellent low temperature resistance, and a more stable solid electrolyte interfacial film structure can be formed on the surface of the positive electrode material, improving the cycle performance of the battery. [0003] Currently, four methods for synthesizing lithium difluorobisoxalate phosphate are disclosed in the prior art. For example, CN102216311, WO2013180174, WO2014097772, and JP2016201244 all use lithium hexafluorophosphate to react with oxalic acid, and add silicon tetrachloride; the high chlorine compounds and free acids in the solutio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574H01M10/0567
CPCC07F9/65748H01M10/0567Y02E60/10
Inventor 冯天明朱辉余意
Owner DONGGUAN DONGYANG SOLAR SCI RES & DEV CO LTD
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