Phosphate as well as preparation method and application thereof

A phosphate ester and reaction technology, applied in the field of phosphate ester and its preparation, can solve the problems of inability to suppress side reactions, single function, increase battery internal resistance, etc., achieve low impedance, less dosage, and inhibit contact reaction effects

Active Publication Date: 2021-08-03
湖州永兴锂电池技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the function of the above additives is relatively single, and when the amount is small, it cannot inhibit the side reaction, and when the amount is increased, it will increase the internal resistance of the battery, which is unfavorable.

Method used

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  • Phosphate as well as preparation method and application thereof
  • Phosphate as well as preparation method and application thereof
  • Phosphate as well as preparation method and application thereof

Examples

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preparation example Construction

[0057] A kind of preparation method of above-mentioned phosphoric acid ester, comprises the steps:

[0058] S1: by alcohol R 1 OH and phosphorus pentachloride (PCl 5 ) reaction to obtain the intermediate The H required for this step reaction 2 O is moisture in the air or additionally added;

[0059] S2: by alcohol R 2 OH reacts with it to obtain the target product

[0060] S3: by alcohol R 3 OH reacts with it to give the product

[0061] As preferably, the mol ratio of alcohol and PCI5 in S1 is 1: (3~10); The mol ratio of alcohol and intermediate in S2 is 1: (2~5); The mol ratio of alcohol and intermediate in S3 has no special requirement, is generally 1:1.

[0062] Preferably, the reaction temperature of S1, S2 and S3 is 0-60° C., and the reaction time is 0.5-10 h.

[0063] S1, S2 and S3 are performed in a solvent; the solvent is selected from ethers, hydrocarbons and aromatic hydrocarbon solvents, such as diethyl ether, furan, n-hexane, cyclohexane and toluene,...

Embodiment 1

[0079] Preparation of Compound A: The first step reaction: add 208.0g of phosphorus pentachloride (PCl 5 ) and 2L n-hexane solvent, and stirred evenly at room temperature. Then slowly add methoxymethanol containing 6.2g (methoxymethanol and PSCl 3 The substance mass ratio is 1:10) n-hexane solution, after the addition, continue to stir for 1 h to obtain the reaction solution. 15.8 g of intermediate were obtained by distillation under reduced pressure The yield was 88.3%.

[0080] The second step reaction: 12.5g of the above-mentioned product is transferred to a single-necked round bottom flask, 0.05L of ether is added, and 2.0g of allyl alcohol (the mass ratio of allyl alcohol to the intermediate is 1:2) is added, and the mixture is heated at room temperature Stirred for 2h, purified by distillation under reduced pressure to obtain 5.8g intermediate The yield was 82.5%.

[0081] The third step reaction: transfer 4.9g of the above product to a single-necked round botto...

Embodiment 2

[0094] Preparation of Compound B:

[0095] The first step reaction: add 208.0g of PCl to the reaction vessel 5 and 2L of solvent cyclohexane, and stirred evenly at 0°C. Then slowly add 25.3g 2-methoxyethanol (2-methoxyethanol and PSCl 3 The substance mass ratio is 1:3) cyclohexane solution, after the addition, continue to stir the reaction solution for 0.5h. 50.5 g intermediate was obtained by distillation under reduced pressure The yield was 78.7%.

[0096] The second step reaction: transfer 48.3 g of the above intermediate to a single-necked round bottom flask, add diethyl ether and start stirring at 0°C. Then slowly add a toluene solution containing 2.8 g of propargyl alcohol (the mass ratio of propargyl alcohol to the intermediate is 1:5), and continue stirring for 5 h after the addition to obtain a reaction solution. 8.7 g of intermediate were obtained by distillation under reduced pressure The yield was 81.5%.

[0097] The third reaction step: transfer 8.7 g o...

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Abstract

The invention relates to the field of lithium batteries, and discloses phosphate as well as a preparation method and application thereof. In the phosphate, R1 is alkyl with the carbon atom number of 1-8, or fluorine-substituted alkyl with the carbon atom number of 1-8, or fluorine-substituted aryl or fluorine-free aryl; R2 is a hydrocarbon group having 1-8 carbon atoms and containing an alkenyl group or an alkynyl group; and R3 is a group containing a cyano group. The preparation method comprises the following steps: S1, reacting alcohol R1OH with phosphorus pentachloride in a solvent to obtain an intermediate; S2, reacting another alcohol R2OH with the intermediate to obtain a product or another intermediate; S3, reacting a third alcohol R3OH with the intermediate in the second step to obtain a product. The electrolyte prepared from the phosphonate can improve the cycling stability, safety performance and storage stability of the secondary battery.

Description

technical field [0001] The invention relates to the field of lithium batteries, in particular to a phosphoric acid ester and its preparation method and application. Background technique [0002] In the application field of lithium-ion secondary batteries, how to improve the cycle life, storage stability and safety performance of batteries has always been the goal and pursuit of scientific researchers. Optimizing the cell design of lithium-ion batteries and applying high-performance battery materials are two commonly used ideas. Among them, as the core material of the battery, the electrolyte has an important impact on the safety performance and electrical performance of the battery cell. Therefore, the improvement of the electrolyte is an important way to improve the overall performance of the battery. In particular, the development and application of new additives has the advantages of less dosage, obvious effect, relatively low cost, low process requirements, and easy in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0567H01M10/42H01M10/0525
CPCH01M10/0567H01M10/4235H01M10/0525H01M2300/0025Y02P70/50
Inventor 臧旭峰夏会玲郑卓群
Owner 湖州永兴锂电池技术有限公司
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