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A kind of synthetic method of three (trihydrocarbyl silyl) phosphites

A technology of trihydrocarbyl silicon base and trihydrocarbyl silicon amine, which is applied in the field of triphosphite synthesis to achieve the effects of easy-to-obtain raw materials, simple process route, and safe and environmentally friendly reaction process

Active Publication Date: 2021-08-24
CHANGSHU CHANGJI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem mainly solved by the present invention is to provide a kind of synthetic method of three (trihydrocarbyl silyl) phosphite, can solve the above-mentioned problem that existing method exists when synthesizing tris (trihydrocarbyl silyl) phosphite

Method used

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  • A kind of synthetic method of three (trihydrocarbyl silyl) phosphites
  • A kind of synthetic method of three (trihydrocarbyl silyl) phosphites
  • A kind of synthetic method of three (trihydrocarbyl silyl) phosphites

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Effect test

Embodiment 1

[0037] The reaction device is equipped with an electric heating mantle, a four-neck flask, an electric stirring rod, a thorn-shaped rectification column, a reflux condenser and a receiving bottle, and the nitrogen gas is inserted into the bottom tube to make nitrogen bubbles purge the reaction device to ensure that the device is dry.

[0038] Add 328g of phosphorous acid and 3480g of N,N-diethyl-N-trimethylsilylamine into the reaction flask, and at the same time turn on the -10°C circulating chilled water in the reflux condenser, turn on the heating, and adjust the heating voltage to control the temperature rise Slowly distill off the diethylamine generated by the reaction. When the kettle temperature gradually rises to 155°C, the top temperature is kept at 125°C and basically unchanged, and the distilled fraction is detected by gas chromatography to be substantially free of diethylamine, the heating can be stopped, the temperature is lowered and cooled, and 2396g of the reacti...

Embodiment 2

[0040] The reaction device is equipped with an electric heating mantle, four-neck flask, electric stirring rod, thorn-shaped rectification column, reflux condenser, and receiving bottle. The bottom tube is opened with nitrogen gas, and the reaction device is purged with nitrogen bubbles to ensure that the device is dry.

[0041]Add 328g of phosphorous acid and 4312g of N-vinyldimethylsilylpiperidine to the reaction flask, and at the same time turn on the -10°C circulating chilled water in the reflux condenser, turn on the heating, adjust the heating voltage to control the heating rate, and slowly evaporate The reaction produces piperidine. When the kettle temperature gradually rises above 160°C, the top temperature remains basically constant above 135°C, and when the distilled fraction is substantially free of piperidine as detected by gas chromatography, the heating can be stopped, the temperature is lowered and cooled, and 3239g of the reaction solution is obtained by weighin...

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Abstract

The invention discloses a method for synthesizing tris(trihydrocarbylsiliconyl)phosphite. Phosphorous acid and trihydrocarbylsiliconyl amine are added to a dry reaction bottle, and then reacted and evaporated under the conditions of heating, stirring and reflux condensation. The generated amine, the reaction liquid is subjected to precision filtration and rectification under reduced pressure to obtain high-purity tris(trihydrocarbylsilyl)phosphite. The present invention adopts phosphorous acid to react with trihydrocarbyl silyl amine, and the selectivity of tris (trihydrocarbyl silyl) phosphite product is high, and the obtained tris (trihydrocarbyl silyl) phosphite crude product can be easily purified to more than 99.9%. , to meet the requirements of lithium ion electrolyte additives; and the raw materials of the present invention are easy to obtain, the process route is simple, the reaction process is safer and more environmentally friendly, the energy consumption is low, and the amount of waste discharge is small, and it is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of lithium ion electrolyte additives, in particular to a method for synthesizing tris(trihydrocarbyl silicon-based) phosphite. Background technique [0002] Tris(trihydrocarbylsilyl)phosphite is a kind of elemental organic compound containing two heteroatoms of phosphorus and silicon. It can be used as a trihydrocarbyl silylating agent and has the flame retardant properties of phosphorus and silicon. In recent years, studies have found that tris(trihydrocarbylsilyl)phosphite is used as an additive for lithium-ion battery electrolytes, which can effectively reduce the capacity loss of lithium-ion batteries, prolong the life of the battery, and improve the high-temperature performance of the battery. With the emphasis on green and environmentally friendly new energy, lithium-ion power batteries have become a new type of green and environmentally friendly energy that replaces traditional batteries. Tris(trihydrocarbylsi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/141
CPCC07F9/1415
Inventor 傅人俊林晓文徐伟文郑翔
Owner CHANGSHU CHANGJI CHEM
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