Synthesis method of tris(trimethylsilyl) phosphate

A technology based on a trimethylsilyl group and a synthesis method, which is applied to phosphorus organic compounds, electrochemical generators, electrical components, etc., can solve the problems of long reaction time, high reaction temperature, and low product yield, and achieves easy control of the reaction. , The effect of high reaction yield and good product purity

Active Publication Date: 2010-10-27
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[Zh.Obshch.Khim., 1985, 55(8): 1674] The raw material hexamethyldisilathane used in this method is highly toxic and has no industrial products. Another raw material P 4 o 10 It is also very dangerous, not easy to operate, and the reaction temperature is high and the time is long, so this method is not suitable for industrial production
[0007] 2. Hexamethyldisilazane and P 4 o 10 Heating and reacting for 2 hours, but the yield is only within 20%, [Zh.Obshch.Khim., 1985,55(8):1883]. This method also uses the dangerous and difficult raw material P 4 o 10 , and the yield of the reaction is extremely low, so this method is not suitable for industrial production
[0009] The methods reported in the above literature have the disadvantages of high toxicity of raw materials, danger, long reaction time or low product yield.

Method used

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  • Synthesis method of tris(trimethylsilyl) phosphate
  • Synthesis method of tris(trimethylsilyl) phosphate

Examples

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Embodiment 1

[0024] A 500ml three-necked flask is equipped with an electric stirrer, a reflux condenser, and a thermometer. Add 58g (0.5mol) of ammonium dihydrogen phosphate and 320ml (1.5mol) of hexamethyldisilazane, and heat and stir at 120°C for 3 hours. After the reaction was finished, the reflux device was changed to a fractionation device for fractionation and purification. The vacuum fractionation method was used to collect fractions at 126-128° C. / 30 mmHg to obtain 126 g of tris(trimethylsilyl) phosphate.

Embodiment 2

[0026] A 1000ml three-necked flask is equipped with an electric stirrer, a reflux condenser, and a thermometer. Add 200g (1.72mol) of ammonium dihydrogen phosphate and 590ml (1.58mol) of hexamethyldisilazane, and heat and stir at 130°C for 3 hours. After the reaction, the reflux device was changed to a fractionation device for fractionation and purification. The vacuum fractionation method was used to collect fractions at 118-119° C. / 25 mmHg to obtain 541 g of tris(trimethylsilyl) phosphate.

Embodiment 3

[0028] A 5000ml three-necked flask is equipped with an electric stirrer, a reflux condenser, and a thermometer. Add 1000g (8.6mol) of ammonium dihydrogen phosphate and 2950ml (13.6mol) of hexamethyldisilazane, and heat and stir at 100°C for 5 hours. After the reaction was finished, the reflux device was changed to a fractionation device for fractional distillation and purification. The vacuum fractional distillation method was used to collect fractions at 120-121° C. / 27 mmHg to obtain 2210 g of tris(trimethylsilyl) phosphate.

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Abstract

The invention relates to a synthesis method of a tris(trimethylsilyl) phosphate, which comprises the following steps: reacting hexamethyldisilazane with a phosphate for 2 to 5 hours at the temperature of 80 to 160 DEG C so as to form a tris(trimethylsilyl) phosphate and ammonia; then carrying out rectification and purification on the obtained crude product so as to obtain a fine product of the tris(trimethylsilyl) phosphate. The method has the advantages of simple operation, easy-taking raw material and simple post-processing, is suitable for industrial production, and can synthesize high quality product.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a synthesis method of tris(trimethylsilyl)phosphate. Tris(trimethylsilyl)phosphate can be used as electrolyte additive for lithium-ion batteries. Background technique [0002] The three (trimethylsilyl) phosphates referred to in the present invention have the following structure: [0003] [0004] Research has found that tris(trimethylsilyl) phosphate can be used as an electrolyte additive for lithium-ion batteries to improve the performance of lithium-ion batteries. In US20080166637A1, tris(trimethylsilyl) phosphate is used as an electrolyte additive for power batteries. In Chinese patent CN1840550A it is pointed out that tris(trimethylsilyl) phosphate is a composition for electrolyte and a polymer electrolyte capable of suppressing a decrease in capacity when the battery is stored in a charged state. The high-molecular-weight electrolyte includes an electrolytic solution...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09H01M10/40
Inventor 吴茂祥卢碧强
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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