Preparation method of silicon-based ester compound, silicon-based ester compound, electrolyte containing silicon-based ester compound and secondary battery

An amine compound and compound technology are applied in the fields of silicon-based ester compound preparation, silicon-based ester compound, electrolyte containing the same, and secondary battery, and can solve the problems of complicated operation process, difficult handling and purification, complicated operation, etc. , to achieve the effects of convenient operation in the preparation process, long reaction time and mild reaction conditions.

Active Publication Date: 2020-06-02
微宏先进材料公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 1980, Hergott et al. reported the synthesis of trialkylsilyl oxalate (Synthesis, 1980, 8, 626–627), which prepared trialkylsilyl oxalate through the reaction of trimethylchlorosilane and oxalic acid, but the The reaction time is as long as 64 hours, and the by-product is HCl; in addition, because the by-product of the reaction is HCl, which is not easy to process and purify, it is easy to corrode metal utensils or equipment, and will also cause pollution to the environment
In 1981, C.Palomo proposed an improved two-step sy

Method used

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  • Preparation method of silicon-based ester compound, silicon-based ester compound, electrolyte containing silicon-based ester compound and secondary battery
  • Preparation method of silicon-based ester compound, silicon-based ester compound, electrolyte containing silicon-based ester compound and secondary battery
  • Preparation method of silicon-based ester compound, silicon-based ester compound, electrolyte containing silicon-based ester compound and secondary battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Add oxalic acid (0.2mol) and DMSO (150mL) to the flask, then add monomethylamine (0.44mol), react at room temperature for 1h overnight and let stand for 12h; then add trimethylbromosilane (0.22mol), then add DMSO (130ml) , heated at 70° C. for 8 h; after the reaction, suction filtration and vacuum distillation (20 mmHg) gave white solid bis(trimethylsilyl) oxalate with a purity of 97% and a yield of 81%.

Embodiment 2

[0069] Add oxalic acid (0.15mol) and acetonitrile (150mL) to the flask, add trimethylamine (0.05mol), and react at room temperature for 1h; then add dimethylvinylchlorosilane (0.15mol), and heat at 50°C for 2h; Suction filtration and vacuum distillation (20mmHg) after the end, to obtain a colorless liquid bis(dimethylvinylsilyl) oxalate with a purity of 97% and a yield of 85%.

Embodiment 3

[0071] Add oxalic acid (0.2mol) and carbon tetrachloride (150mL) to the flask, then add monopropylamine (0.44mol), and react at room temperature for 1h; then add dimethylisopropylbromosilane (1mol), and heat the reaction at 100°C 6h; after the reaction, suction filtration and vacuum distillation (20mmHg) gave a colorless liquid bis(dimethylisopropylsilyl) oxalate with a purity of 97% and a yield of 55%.

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Abstract

The invention relates to a preparation method of a silicon-based ester compound, the silicon-based ester compound, an electrolyte containing the silicon-based ester compound and a secondary battery. The preparation method of the silicon-based ester compound comprises the following steps: adding organic alkali and organic acid into a solvent and carrying out reacting to obtain an intermediate, andthen, adding halogenated silane to react with the intermediate to obtain the silicon-based ester compound, wherein the intermediate is ionic liquid. The preparation method provided by the invention can relieve the problems of long reaction time, difficult treatment of byproducts, complex operation caused by step-by-step reaction, high cost, difficult industrial scale-up production and the like inthe existing synthesis method.

Description

technical field [0001] The invention relates to a preparation method of a silicon-based ester compound, a silicon-based ester compound, an electrolyte containing the silicon-based ester compound, and a secondary battery. Background technique [0002] Silicon-based ester compounds have potential application prospects in lithium-ion batteries. In 1967, Von G. Schott and G.Henneberg studied the preparation method and thermal stability of bis(triarylsilyl) oxalate (Liber dieStabilitat von Bis(triorgano-silyl)-oxalaten, Zeitschrift fur anorganische undallgemeine Chemie, 1967, 352, 45-52). In 1980, Hergott et al. reported the synthesis of trialkylsilyl oxalate (Synthesis, 1980, 8, 626–627), which prepared trialkylsilyl oxalate through the reaction of trimethylchlorosilane and oxalic acid, but the The reaction time is as long as 64 hours, and the by-product is HCl; in addition, because the by-product produced by the reaction is HCl, which is difficult to process and purify, it is ...

Claims

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Application Information

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IPC IPC(8): C07F7/18H01M10/0525H01M10/0567
CPCC07F7/1896H01M10/0567H01M10/0525Y02E60/10
Inventor 贺伟郑宣鸣熊亚丽张志刚董剑
Owner 微宏先进材料公司
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