Lithium battery electrolyte additive and preparation method thereof

An electrolyte additive and lithium battery technology, which is applied in secondary batteries, circuits, electrical components, etc., can solve problems such as complex reaction and purification process, difficult product quality control, and highly toxic phosphorus trichloride. Green friendly, excellent solubility, good effect of high rate discharge performance

Pending Publication Date: 2022-04-29
河北松辰医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent CN113130996A discloses a method for preparing lithium-ion battery additives. In this application, the raw material is phosphorus trichloride, which is highly toxic and can generate hydrochloric acid mist in the air, which is highly dangerous and pollutes seriously. , does not conform to the concept of environmental protection
The reaction and purification process of this method are relatively complicated, and the product quality is not easy to control during the preparation process, and more waste liquid will be generated during the entire implementation process, which is not conducive to environmental protection

Method used

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  • Lithium battery electrolyte additive and preparation method thereof
  • Lithium battery electrolyte additive and preparation method thereof
  • Lithium battery electrolyte additive and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0031]

[0032] Preparation of DFTC: Under the protection of nitrogen, add 1 L of dichloromethane, 10 g of compound A (2,2-difluoro-1,3-propanediol), 89.2 mmol, into a dry and anhydrous 2 L reaction flask, and add them in batches under stirring at room temperature CDI 15.92g, 98.1mmol, the mixture was heated to reflux at 40°C and kept to react for 4h, confirmed by TLC that the reaction was complete, cooled to 5°C, added 400ml of 2mol / L HCl aqueous solution to the system to quench the reaction, separated the liquid, and used dichloro Extracted with methane to no product (2 times × 200ml), the combined organic phases were washed once with water × 300ml, washed once with saturated sodium chloride solution × 300ml, dried over anhydrous sodium sulfate, filtered with suction, and the filtrate was concentrated under reduced pressure (vacuum degree -0.098 MPa) to solvent-free to obtain the crude product, and obtain pure DFTC 9.66g as a colorless liquid by distillation under reduced ...

Embodiment 2

[0038]

[0039] Preparation of DFTC: Under the protection of nitrogen, add 100ml of dichloromethane, 5g of compound A (2,2-difluoro-1,3-propanediol), 44.6mmol, into a dry and anhydrous 250ml reaction flask, add in batches under stirring at room temperature Triphosgene 14.8g, 49.1mmol, the mixture was heated to reflux at 40°C and incubated for 4h, confirmed by TLC that the reaction was complete, cooled to 5°C, added 40ml of water to the system to quench the reaction, separated, and the aqueous phase was extracted with dichloromethane to No product (2 times × 30ml), the combined organic phases were washed once with water × 30ml, washed once with saturated sodium chloride solution × 30ml, dried over anhydrous sodium sulfate, filtered with suction, and the filtrate was concentrated under reduced pressure (vacuum degree -0.098MPa) to The crude product was obtained after solvent-free, and 3.4 g of pure DFTC was obtained as a colorless liquid by distillation under reduced pressure....

Embodiment 3

[0045]

[0046]Preparation of DFTC: Under the protection of nitrogen, add 100L of dichloromethane, 5.0kg of compound A (2,2-difluoro-1,3-propanediol), 44.6mol, into a dry and anhydrous 200L reactor, and stir in batches at room temperature Add 7.96kg, 49.1mol of CDI, heat the mixture to reflux at 40°C and keep it warm for 4 hours, confirm the completion of the reaction by TLC, cool down to 5°C, add 2mol / L H to the system 2 SO 4 Quench the reaction with 40L of solution, separate the liquids, extract the aqueous phase with dichloromethane until there is no product (2 times × 20L), wash the combined organic phase with water once × 30L, wash once with saturated sodium chloride solution × 30L, anhydrous sodium sulfate After drying and suction filtration, the filtrate was concentrated under reduced pressure (vacuum degree-0.098MPa) to obtain a crude product after being free of solvent, and 5.175kg of pure DFTC was obtained as a colorless liquid by vacuum distillation.

[0047] Yi...

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PUM

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Abstract

The invention relates to a preparation method of a lithium battery electrolyte additive, which comprises the following steps: under the protection of nitrogen, adding a solvent, a compound 2, 2-difluoro-1, 3-propylene glycol or an initial raw material I into a dry and anhydrous reactor, adding a cyclization agent in batches while stirring at room temperature, heating the mixture to 20-80 DEG C, carrying out reflux heat preservation reaction for 2-4 hours, and confirming that the reaction is complete through thin layer chromatography; after the reaction is completed, washing and concentrating to obtain a product. According to the method, traditional easily available raw materials are adopted, high-risk reactions such as fluorination are avoided, the method is safer and more economical than a common fluorination method, high-risk chemical raw materials such as fluorine gas are avoided, the number of three wastes is reduced, the economic benefit is improved, and a product route is green and friendly.

Description

technical field [0001] The invention relates to the technical field of lithium batteries, in particular to a lithium battery electrolyte additive and a preparation method thereof. Background technique [0002] When mankind enters the 21st century, with the rapid development of the economy, the demand for energy is constantly increasing. In order to promote sustainable development, lithium-ion batteries have attracted more and more attention as a new energy source, and have become one of the key points of high-tech One, significant progress has been made in recent years. As global energy and environmental problems become more and more serious, vehicles have switched to energy storage batteries as the main power source. Lithium-ion batteries are also considered to be the ideal choice for high-capacity and high-power batteries, and will gradually replace nickel hydrogen. Battery. [0003] Adding a small amount of certain substances as additives in the electrolyte of lithium-i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0567
CPCH01M10/0567
Inventor 吴红松邵永亮贾晓旭齐贺军李江潮贾晓茹郅雅琴
Owner 河北松辰医药科技有限公司
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