A kind of synthetic method of three (trimethylsilyl) phosphites

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 the problem of expensive, easy hydrolysis, and increased post-processing steps and other problems, to achieve the effect of simple post-processing steps, mild reaction conditions and little environmental pollution

Active Publication Date: 2022-05-17
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The defect of this method is: the by-product triethylamine hydrochloride can be difficult to remove, and cause adverse effect to subsequent steps
The defect of this method is: one, there will be inorganic salt to generate after the reaction, and this has increased the step of aftertreatment
2. The raw material trimethyl alkali metal silicon alkoxide is highly corrosive, easy to hydrolyze and expensive, which is not conducive to industrial production

Method used

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  • A kind of synthetic method of three (trimethylsilyl) phosphites

Examples

Experimental program
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Effect test

Embodiment 1

[0018] In a 2000mL three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 650g of hexamethyldisilazane, 10g of D002 type strong acidic styrene-based cationic resin, raise the temperature to 80°C, and add phosphorous acid-acetonitrile dropwise The solution (200 g of phosphorous acid, 300 g of acetonitrile) was added dropwise in 2 hours. After the dropwise addition, it was kept at 90° C. for 1 hour to complete the reaction. 1090 g of reaction liquid was obtained, including 670 g of tris(trimethylsilyl)phosphite, and the conversion rate was 92.2%.

Embodiment 2

[0020] In a 2000mL three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 600g of hexamethyldisilazane, 20g of D62 type strong acidic styrene-based cation exchange resin, raise the temperature to 50°C, and dropwise add phosphorous acid- N,N-dimethylformamide solution (phosphorous acid 200g, N,N-dimethylformamide 400g), the dropwise addition was completed in 2 hours, after the dropwise addition, it was kept at 50° C. for 2 hours, and the reaction was completed. 1147 g of reaction liquid was obtained, including 618 g of tris(trimethylsilyl)phosphite, and the conversion rate was 85.0%.

Embodiment 3

[0022] In a 5000mL three-necked flask equipped with an electric stirrer, a reflux condenser, and a thermometer, add 500g of hexamethyldisilazane, 7g of 734-type strong acidic styrene-based cation exchange resin, raise the temperature to 90°C, and dropwise add phosphorous acid- Diethylene glycol dimethyl ether solution (phosphorous acid 200g, diethylene glycol dimethyl ether 200g), was added dropwise in 1 hour. After the dropwise addition was completed, it was incubated at 90° C. for 1 hour, and the reaction was completed. 850 g of reaction liquid was obtained, including 537 g of tris(trimethylsilyl)phosphite, and the conversion rate was 87.0%.

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Abstract

The invention discloses a method for synthesizing tris(trimethylsilyl)phosphite, which comprises the following steps: dissolving phosphorous acid in an organic solvent and adding it dropwise into hexamethyldisilazane; Carry out the reaction to obtain tris(trimethylsilyl)phosphite; the mass ratio of phosphorous acid to hexamethyldisilazane is 1:2.2~1:4.4, and the temperature is controlled at 20°C~120°C during the dropping process , after the dropwise addition, keep warm at 20°C to 120°C for reaction, and the catalyst is a strongly acidic cation exchange resin. The invention has the advantages of: 1. The raw materials are easy to obtain, the reaction conditions are mild, and the conversion rate can be as high as 90%. 2. After the reaction is completed, it can be directly rectified, and the post-treatment steps are simple and the yield is high. 3. No waste is generated in the whole synthesis process, and the environmental pollution is small.

Description

technical field [0001] The invention relates to the technical field related to the synthesis of electrolyte additives, in particular to a method for synthesizing tris(trimethylsilyl)phosphite. Background technique [0002] Tris(trimethylsilyl)phosphite can be used to prepare bis(trimethylsilyl)phosphate gently by Arbuzow reaction, and can also be used as an electrolyte additive. [0003] From the published reports, the commonly used method is to react trimethylchlorosilane and phosphorous acid in the presence of acid-binding agent triethylamine and solvent to synthesize tris(trimethylsilyl)phosphite. The defect of this method is: by-product triethylamine hydrochloride can be difficult to remove, and cause adverse effect to subsequent steps. [0004] Another CN106046046A discloses a method for synthesizing tris(trimethylsilyl) phosphite with trimethylsilicon alkali metal alkoxide and phosphorus trichloride. The disadvantages of this method are: 1. Inorganic salts will be ge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/141
CPCC07F9/1415
Inventor 陈晓华岳立刘栋成程勇张明亮周铭柯
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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