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Preparation method of phosphate ester or phosphite ester, electrolyte and secondary battery

A phosphite and phosphoric acid ester technology, applied in secondary batteries, chemical instruments and methods, circuits, etc., can solve the problems of high reaction temperature, high cost, and high raw material cost, and achieve a mild synthesis method, production cost control, and applicability wide range of effects

Pending Publication Date: 2019-12-10
MICROVAST POWER SYST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction temperature of this method is high, the raw materials used are large, the yield is low, and the cost of industrialized production is relatively high
[0005] Chinese patent application CN105949233A proposes a new preparation method of tris(trimethylsilyl) phosphate, which uses trimethylchlorosilane to react with phosphate. Although the preparation method has a high yield, the raw material trimethylsilyl The consumption of chlorosilane is too large, the reaction temperature is higher, the reaction time is longer, and the reaction product is also easy to introduce chloride ions, which will affect the performance of the battery when tris(trimethylsilyl) phosphate is used as an electrolyte additive.
[0006] Chinese patent application CN104860986A proposes a method for preparing tris(trimethylsilyl)phosphite, which uses alkali metal silicon alkoxide to react with phosphorus halide. The product obtained by this preparation method has higher purity, but the cost of raw materials used Very high, and the preparation of raw materials is also very difficult, so this method has great limitations and cannot be applied to the preparation of other types of phosphite

Method used

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  • Preparation method of phosphate ester or phosphite ester, electrolyte and secondary battery
  • Preparation method of phosphate ester or phosphite ester, electrolyte and secondary battery
  • Preparation method of phosphate ester or phosphite ester, electrolyte and secondary battery

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0076] Weigh 0.26 mol of 2-pyrrolidone, add 0.26 mol of trimethylsilyl chloride and DMF, react at 50°C for 2 hours, and distill under reduced pressure to obtain 3-trimethylsilylpyrrolidone (0.25 mol).

[0077] Weigh 0.05 mol of lithium dihydrogen phosphate, add 0.1 mol of 3-trimethylsilylpyrrolone, and react at room temperature for 1 h. Distillation under reduced pressure (20 mmHg, 72° C.) yielded 0.029 mol of colorless transparent liquid tris(trimethylsilyl) phosphate, with a yield of 86% and a purity of 99%.

Embodiment 2

[0079] Weigh 0.05mol phosphorous acid, add 0.15mol 3-trimethylsilylpyrrolidone, dissolve in THF, and react at 70°C for 4h. The pyrrolidone solid was obtained by filtration, washed three times with 30 ml of petroleum ether, the petroleum ether phase was combined, the solvent was removed, and the GC-MS test was performed. Distilled under reduced pressure to obtain 9 g, a colorless transparent liquid. Then add sodium metal, react under nitrogen protection at 140°C-150°C for 20h under anhydrous conditions, and then distill under reduced pressure after cooling to obtain 0.13mol of tris(trimethylsilyl)phosphite (20mmHg, 75°C).

Embodiment 3

[0081] Weigh 0.26 mol of pyrrolidine, add 0.26 mol of dimethylvinylchlorosilane and DMSO, react at 50° C. for 10 h, and distill under reduced pressure to obtain 1-(dimethylvinylsilyl)pyrrolidine (0.25 mol).

[0082]Weigh 0.05 mol of sodium dihydrogen phosphate, add 1-(dimethylvinylsilyl)pyrrolidine (0.25 mol) and react at room temperature for 1 h. Distillation under reduced pressure (20 mmHg, 72° C.) yielded 0.045 mol of tris(dimethylvinylsilyl)phosphate as a colorless transparent liquid with a yield of 90% and a purity of 99%.

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Abstract

The invention provides a preparation method of a phosphate ester or a phosphite ester. The preparation method comprises the following step: reacting an inorganic phosphate or an inorganic phosphite with a silicon-substituted cycl-lactam compound shown in a formula 3) to obtain the phosphate ester shown in a formula 1) or the phosphite ester shown in a formula 2). The preparation method provided bythe invention not only can be used for preparing phosphate esters, but also can be used for preparing phosphite esters. The synthetic method disclosed by the invention is mild and stable in reaction,convenient to operate, high in yield, high in purity and low in energy consumption in the reaction process, and is a universal synthetic method for synthesizing phosphate esters or phosphite esters.

Description

technical field [0001] The invention relates to a preparation method of phosphoric acid ester or phosphorous acid ester, electrolyte solution and secondary battery. Background technique [0002] With the development of lithium-ion batteries, the use of phosphate or phosphite as battery electrolyte additives to improve the performance of lithium-ion batteries is becoming more and more widely used. [0003] Chinese patent application CN1840550A discloses a compound tris(trimethylsilyl)phosphate containing a P-O-Si bond, which can suppress the reaction of unreacted polymerizable compounds in the electrode, thereby suppressing the increase in battery resistance and suppressing the decrease in capacity . [0004] Chinese patent application CN101870711A proposes a method for the industrial production of tris(trimethylsilyl) phosphate: at 80-160°C, hexamethyldisilazane reacts with ammonium dihydrogen phosphate for 2-5 hours, Generate tris(trimethylsilyl) phosphate and ammonia gas...

Claims

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Application Information

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IPC IPC(8): C07F9/09C07F9/141H01M10/0567
CPCC07F9/095C07F9/1415H01M10/0567Y02E60/10
Inventor 贺伟董剑费震宇张志刚文娟·刘·麦蒂斯
Owner MICROVAST POWER SYST CO LTD
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