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Synthetic method of di(trimethylsilyl)phosphite

A technology of trimethylsilyl and phosphite, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as long reaction time, low purity, and high energy consumption problem, to achieve the effect of reducing energy consumption and cost, and lowering the reaction temperature

Active Publication Date: 2017-06-20
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of long reaction time, high energy consumption, low yield and low purity in the process of preparing bis(trimethylsilyl)phosphite in the prior art, the present invention provides a bis(trimethylsilyl) The synthetic method of base) phosphite solves the above problems, and is easy to operate, mild in reaction and stable

Method used

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  • Synthetic method of di(trimethylsilyl)phosphite

Examples

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Effect test

Embodiment 1

[0021] The humidity in the operating room is controlled at 46%-56%, and the temperature is about 25°C.

[0022] First remove the water from the phosphorous acid, put the phosphorous acid and toluene in the container, heat and reflux in the oil bath, divide the water for 4 hours, remove the water, and concentrate the toluene by rotary evaporation (water pump, vacuum degree 0.095MPa, temperature 60°C) After 2 hours to constant weight, the phosphorous acid after dehydration is obtained.

[0023] Weigh 29.2g (0.356mol) of dehydrated phosphorous acid and 90mL formamide (102g) into a 500mL four-neck flask, blow in nitrogen, control the flow rate of nitrogen to 2ml / min, stir vigorously for about 20min, the phosphorous acid is completely After the solution was dissolved, a colorless transparent liquid was obtained, and the nitrogen gas was continued to be passed in, and the gas was exhausted for 30 minutes.

[0024] Add 140mL (120g, 1.1mol) trimethylchlorosilane (slightly brown) drop...

Embodiment 2

[0029] The humidity in the operating room is controlled at 46%-56%, and the temperature is about 25°C.

[0030] First remove the water from the phosphorous acid, put the phosphorous acid and toluene in the container, heat and reflux in the oil bath, divide the water for 4 hours, remove the water, and concentrate the toluene by rotary evaporation (water pump, vacuum degree 0.095MPa, temperature 60°C) After 2 hours to constant weight, the phosphorous acid after dehydration is obtained.

[0031] Weigh 29.2g (0.356mol) of dehydrated phosphorous acid and 90mL formamide (102g) into a 500mL four-neck flask, blow in nitrogen, control the flow rate of nitrogen to 2ml / min, stir vigorously for about 20min, the phosphorous acid is completely After the solution was dissolved, a colorless transparent liquid was obtained, and the nitrogen gas was continued to be passed in, and the gas was exhausted for 30 minutes.

[0032] Add 140mL (120g, 1.1mol) trimethylchlorosilane (slightly brown) drop...

Embodiment 3

[0038] The humidity of the operating room is controlled at 35%-45%, and the temperature is about 25°C.

[0039] First remove the water from the phosphorous acid, put the phosphorous acid and toluene in the container, heat and reflux in the oil bath, divide the water for 4 hours, remove the water, and concentrate the toluene by rotary evaporation (water pump, vacuum degree 0.095MPa, temperature 60°C) After 2 hours to constant weight, the phosphorous acid after dehydration is obtained.

[0040] Weigh 29.2g (0.356mol) of dehydrated phosphorous acid and 90mL formamide (102g) into a 500mL four-neck flask, blow in nitrogen, control the flow rate of nitrogen to 5ml / min, stir vigorously for about 15min, the phosphorous acid is completely After dissolving, a colorless transparent liquid was obtained, and nitrogen gas was continuously passed in, and exhausted for 20 minutes.

[0041] Add 180mL (152g, 1.4mol) trimethylchlorosilane (slightly brown) dropwise to this colorless transparent ...

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Abstract

A synthetic method of di(trimethylsilyl)phosphite belongs to the technical field of compound synthesis. Trimethylchlorosilane and orthophosphorous acid which are adopted as raw materials undergo a reaction to obtain the di(trimethylsilyl)phosphite. The method comprises the following steps: placing orthophosphorous acid in methanamide, introducing nitrogen, stirring the orthophosphorous acid in methanamide for 15-20 min, adding the trimethylchlorosilane, simultaneously adding benzyltriethylammonium chloride and / or tetrabutylammonium hydrogen sulfate, continuously introducing nitrogen, controlling the reaction temperature to be less than 40 DEG C, and carrying out a one-step reaction to obtain the di(trimethylsilyl)phosphite. The synthetic method has the advantages of simplicity, easiness in operation, mild and stable reaction process, and high yield and high purity of the obtained di(trimethylsilyl)phosphite.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and relates to a synthesis method of bis(trimethylsilyl) phosphite. The synthesis method of the present invention is simple, has been operated, and the reaction process is mild and stable. The obtained bis(trimethylsilyl) The yield of phosphite is high and the purity is high. Background technique [0002] Bis(trimethylsilyl)phosphite can be used as an electrolyte additive for lithium-ion batteries to improve the performance of lithium-ion batteries. Bis(trimethylsilyl)phosphite is a composition for an electrolyte and a polymer electrolyte capable of suppressing a decrease in capacity when a battery is stored in a charged 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 an unreacted polymerizable compound from reacting in an electrode, suppressing an increase in battery resista...

Claims

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Application Information

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IPC IPC(8): C07F9/141
CPCC07F9/1415
Inventor 郝俊刘鹏梅银平
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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