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Preparation method of tris(trimethylsilyl)phosphate ester

A technology of trimethylsilyl, phosphate ester, applied in the direction of phosphorus organic compounds, etc., can solve the problems of high reaction temperature, large dosage, and high production cost, and achieve the effects of reducing reaction temperature, improving product yield, and reducing energy consumption

Inactive Publication Date: 2015-09-23
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction temperature of this method is high, the excessive amount of hexamethyldisilazane is 50%, the consumption is relatively large, and the product molar yield is below 80%, so the production cost is relatively high

Method used

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  • Preparation method of tris(trimethylsilyl)phosphate ester

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Experimental program
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Effect test

Embodiment 1

[0021] In a 500mL three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 115g of ammonium dihydrogen phosphate, 255g of hexamethyldisilazane, and 3.7g of tetrabutylammonium bromide, and stir at 78°C for 3 Hours, the reaction process was carried out under nitrogen protection. After the reaction, filter to obtain the filtrate crude product of tris(trimethylsilyl) phosphate; then carry out vacuum distillation on the filtrate, collect the fraction at 126~128°C / 30mmHg to obtain 285g of tris(trimethylsilyl)phosphate . Based on hexamethyldisilazane, the molar yield is 86.1%.

Embodiment 2

[0023] In a 1000mL three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 230g of ammonium dihydrogen phosphate, 520g of hexamethyldisilazane, and 7.5g of dodecyltrimethylammonium chloride. The reaction was stirred for 5 hours, and the reaction process was carried out under the protection of nitrogen. After the reaction, filter to obtain the crude filtrate tris(trimethylsilyl) phosphate; then carry out vacuum distillation on the filtrate, collect the fraction at 126~128°C / 30mmHg to obtain 580g of tris(trimethylsilyl)phosphate . Based on hexamethyldisilazane, the molar yield is 85.8%.

Embodiment 3

[0025] In a 2000mL three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 460g of ammonium dihydrogen phosphate, 1040g of hexamethyldisilazane, and 45g of trioctylmethylammonium bromide, and stir the reaction at 68°C After 4 hours, the reaction process was carried out under the protection of argon. After the reaction, filter to obtain the crude filtrate tris(trimethylsilyl) phosphate; then carry out vacuum distillation on the filtrate, collect the fraction at 126~128°C / 30mmHg to obtain 1175g of tris(trimethylsilyl)phosphate . Based on hexamethyldisilazane, the molar yield is 86.9%.

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Abstract

The invention discloses a preparation method of tris(trimethylsilyl)phosphate ester. According to the preparation method, reaction temperature is low, and yield of products is high. The preparation method comprises the following steps: pouring hexamethyldisilazane and ammonium dihydrogen phosphate into a reaction vessel, adding a phase transfer catalyst into the reaction vessel, heating to 30-78 DEG C, reacting under inert gas protection, and filtering after the reaction so as to obtain a filtrate, namely a tris(trimethylsilyl)phosphate ester crude product; and rectifying the filtrate and collecting a fraction to obtain tris(trimethylsilyl)phosphate ester. By the above method, yield can reach more than 85%. The high-purity tris(trimethylsilyl)phosphate ester obtained after synthesis and rectification by the above method can be directly used as a lithium-ion battery electrolyte additive.

Description

technical field [0001] The invention relates to a preparation method of tri(trimethylsilyl) phosphate. Background technique [0002] The present invention relates to the preparation method of tris(trimethylsilyl) phosphate of following structural formula (I). [0003] [0004] Tris(trimethylsilyl)phosphate can be used as an electrolyte additive for lithium-ion batteries to improve the performance of lithium-ion batteries. Publication number is pointed out in the Chinese patent literature of CN1840550A that the compound tris (trimethylsilyl) phosphate ester of P-O-Si bond can suppress the reaction of unreacted polymerizable compound in the electrode, can suppress the battery resistance increase and can Inhibition of capacity reduction. [0005] Publication No. CN101217204A pointed out in the Chinese patent literature that when sultone and tris(trimethylsilyl)phosphate with unsaturated hydrocarbon groups are contained in the non-aqueous electrolyte, a low-resistance coati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
Inventor 陈晓华王峰秦虎岳立刘祖锋刘磊赵世勇
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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