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Purification method of tri (trimethylsililyl) phosphite ester and tri (trimethylsililyl) phosphate ester

A technology of trimethylsilyl and phosphite, which is applied in chemical instruments and methods, phosphorus organic compounds, compounds of Group 5/15 elements of the periodic table, etc. High-purity products, unstable product quality, etc., to achieve the effect of being conducive to stable storage or long-distance transportation, environment-friendly, and not easy to decompose

Active Publication Date: 2012-09-19
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing purification process, tris(trimethylsilyl)phosphite and phosphoric acid ester products contain many impurities, it is difficult to obtain high-purity products, and the product quality is unstable and cannot meet the requirements of electronic grade indicators, thus Limits the application of products in the electronic field

Method used

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  • Purification method of tri (trimethylsililyl) phosphite ester and tri (trimethylsililyl) phosphate ester
  • Purification method of tri (trimethylsililyl) phosphite ester and tri (trimethylsililyl) phosphate ester

Examples

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Embodiment 1

[0022] Under the protection of nitrogen, add 1680g of tris(trimethylsilyl)phosphate with a content of 60% to a 2000mL three-necked flask, the water content is 2600ppm, add 168g of phenothiazine, and pass through a rectification device with an adjustable reflux ratio under normal pressure. Carry out fractional distillation and purification, collect fractions at 115~120°C / 0.2~5KPa to obtain 825g of tris(trimethylsilyl)phosphate, and the content of the product measured by gas chromatography (GC-2014, purchased from Shimadzu company) is 99.9035% , The content of phenothiazine is 112ppm.

Embodiment 2

[0024] Under nitrogen protection, add 1550g of tris(trimethylsilyl)phosphate with a content of 90% to a 2000mL three-necked flask with a water content of 800ppm, add 1.6g of 2,6-di-tert-butyl p-cresol, and adjust the The rectification device with the reflux ratio conducts fractional distillation and purification under reduced pressure, collects the fraction at 125~128°C / 5~10KPa, and obtains 1182g of tris(trimethylsilyl)phosphate, which is passed through a gas chromatograph (GC-2014, purchased from Shimadzu Company) measured that the content of the product was 99.9216%, and the content of 2,6-di-tert-butyl-p-cresol was 18ppm.

Embodiment 3

[0026] Under nitrogen protection, 758g of tris(trimethylsilyl)phosphite with a content of 96% was added to a 1000mL three-necked flask, and the water content was 128ppm. 7g of butylhydroxyanisole and 5g of tert-butylhydroquinone were added, Fractional distillation and purification were carried out under reduced pressure through a rectification device with an adjustable reflux ratio, and the fraction at 80~86°C / 2~5KPa was collected to obtain 662g of tris(trimethylsilyl)subite, which was passed through a gas chromatograph (GC-2014 , purchased from Shimadzu company) measured product content is 99.9525%, butylated hydroxyanisole content is 21ppm, tertiary butyl hydroquinone content is 45ppm.

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Abstract

The invention discloses a purification method of tri (trimethylsililyl) phosphite ester and tri (trimethylsililyl) phosphate ester. The purification method is characterized in that crude products containing tri (trimethylsililyl) phosphite ester and tri (trimethylsililyl) phosphate ester is subjected to dehydration until the water content is lower than or equal to 3000ppm, free radical stabilizers containing benzene ring structures are added, then, the reduced pressure rectification and the purification are carried out, and the tri (trimethylsililyl) phosphite ester or the tri (trimethylsililyl) phosphate ester with the purity higher than or equal to 99.9 percent are obtained. According to the technical scheme disclosed by the invention, the free radical stabilizers containing the benzene ring structures are added, the product is more stable in the purification process, in addition, the decomposition is not easy to occur, or other side reactions cannot be caused, meanwhile, the product carries ppm-grade stabilizers after the rectification and purification, and the stable storage or the long-distance transportation is more favorably realized. Compared with the traditional purification process, the purification method has the advantages that no three wastes are generated, the environment-friendly effect is realized, in addition, the unit consumption is low, the yield of the purification method is high, the purity of the obtained product is higher than or equal to 99.9 percent, and the electronic grade application requirements are met.

Description

technical field [0001] The invention relates to a method for purifying electronic-grade tris(trimethylsilyl)phosphite and phosphoric acid ester. Background technique [0002] Tris(trimethylsilyl)phosphite and phosphate can be used as electrolyte additives for lithium-ion batteries to improve the performance of lithium-ion batteries. A composition and a polymer electrolyte capable of suppressing the decrease in battery capacity of a lithium-ion battery in a charged storage state. The high-molecular-weight electrolyte includes an electrolytic solution including a compound having a P-O-Si bond or a B-O-Si bond, thereby suppressing a reaction of an unreacted polymerizable compound in an electrode, suppressing an increase in battery resistance, and a high-molecular-weight compound. Capacity reduction can be suppressed. When the non-aqueous electrolyte contains sultone and tris(trimethylsilyl)phosphate compound with a saturated hydrocarbon group at the same time, a low-resistanc...

Claims

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Application Information

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IPC IPC(8): C07F9/141C07F9/09
Inventor 张先林杨志勇周立新吴国栋沈鸣
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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