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Synthesis method of tris(2,2,2-trifluoroethyl)phosphate

A technology of trifluoroethyl and synthesis method, which is applied in the field of synthesis of phosphoric acid triester, can solve the problems of low yield, high moisture content, difficulty in meeting battery grade, etc., achieve high yield, high purity, and simple synthesis method Effect

Pending Publication Date: 2021-06-04
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current method for preparing tris(2,2,2-trifluoroethyl) phosphate has low yield and high water content, which is difficult to meet the requirements of battery level and affects its function.

Method used

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  • Synthesis method of tris(2,2,2-trifluoroethyl)phosphate
  • Synthesis method of tris(2,2,2-trifluoroethyl)phosphate
  • Synthesis method of tris(2,2,2-trifluoroethyl)phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Under the protection of nitrogen, take 330g of trifluoroethanol, and add 303.6g of triethylamine into 460mL of solvent THF, control the reaction temperature at -6°C, add 153.3g of phosphorus oxychloride dropwise, dropwise for 4 hours, and return to the solution naturally after dropping. Warm to 0°C, keep warm for 1.5h, and stop the reaction. After the obtained reaction solution is suction-filtered, the filtrate is first washed with 10% saline for 30 minutes. After liquid separation, the organic phase is washed with 1% aqueous sodium bicarbonate solution for 20 minutes. After liquid separation, , take the organic phase to dry, dry with anhydrous magnesium sulfate, then add activated carbon for decolorization, filter, collect the filtrate, control the vacuum degree to 0.093MPa, concentrate at a temperature of 45°C for 1h, and then concentrate at 60°C for 1h to obtain 319.26 g of product, colorless transparent liquid.

[0025] The above product was detected by gas chromato...

Embodiment 2

[0028] Under the protection of nitrogen, take 350g of trifluoroethanol, and add 276.5g of pyridine into 1000mL of solvent toluene, control the reaction temperature at -7°C, add 153.3g of phosphorus oxychloride dropwise, dropwise for 5h, and naturally warm to 0°C, keep warm for 2 hours, stop the reaction, after the obtained reaction solution is suction filtered, the filtrate is first washed with 10% saline solution for 40 minutes, after liquid separation, the organic phase is washed with 1% aqueous sodium bicarbonate solution for 30 minutes, after liquid separation, take the organic phase The phase was dried, dried with anhydrous magnesium sulfate, then decolorized by adding activated carbon, filtered, and the filtrate was collected, controlled at a vacuum of 0.093MPa, concentrated at a temperature of 50°C for 1.5h, and then concentrated at 63°C for 2h to obtain 320.75g The product is a colorless transparent liquid.

[0029] Adopt gas chromatograph to detect above-mentioned pro...

Embodiment 3

[0032] Under the protection of nitrogen, take 360g of trifluoroethanol and add 323.2g of triethylamine into 1300mL of solvent DCM, control the reaction temperature at -8°C, add 153.3g of phosphorus oxychloride dropwise, dropwise for 3.5h, and drop naturally Return the temperature to 0°C, keep it warm for 1.5h, stop the reaction, after suction filtration of the obtained reaction solution, wash the filtrate with 10% saline solution for 35min, after liquid separation, wash the organic phase with 1% aqueous sodium bicarbonate solution for 25min, and separate the liquid Finally, take the organic phase and dry it with anhydrous magnesium sulfate, then add activated carbon for decolorization, filter, collect the filtrate, control the vacuum degree to 0.093MPa, concentrate at a temperature of 55°C for 1.2h, and then concentrate at 62°C for 1.5 h, 319.06g of product was obtained as a colorless transparent liquid.

[0033] The above product is detected by gas chromatography, and the det...

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Abstract

The invention provides a synthesis method of tris(2,2,2-trifluoroethyl)phosphate, and belongs to the technical field of battery electrolytic solution additives. The method comprises the following steps: under the protection of nitrogen, adding trifluoroethanol as a raw material and an acid-binding agent into a solvent, then adding phosphorus oxychloride for reaction, carrying out suction filtration on the obtained reaction liquid, washing, drying, decolorizing, and concentrating to obtain tris(2,2,2-trifluoroethyl)phosphate. The key point is that the reaction temperature is controlled to be less than -5 DEG C when the phosphorus oxychloride is dropwise added, the dropwise adding time is 3.5-5 hours, the temperature is naturally returned to 0 DEG C after dropwise adding, the temperature is kept for 1.5-2 hours, and the reaction is stopped; and during concentration, the vacuum degree is controlled to be 0.093 MPa, concentration is conducted for 1-1.5 h at a temperature of 40-55 DEG C, then concentration is conducted for 1-2 h at a temperature of 60-63 DEG C, and the tris(2,2,2-trifluoroethyl)phosphate is obtained. The synthesis method is simple, and the synthesized product is high in yield and high in purity.

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte additives, and relates to a method for synthesizing battery-grade tris(2,2,2-trifluoroethyl) phosphate. The synthesis method of the invention is simple, adopts low-temperature synthesis, and strictly controls the reaction conditions, so that the yield of the obtained product is high, and the content is as high as 99.99% and the moisture content is low, reaching the application level of batteries. Background technique [0002] With its high specific energy, high voltage, no memory effect, environmental protection, and long life, lithium-ion batteries have been widely used as reliable energy sources in portable electronic products, such as mobile devices, notebook computers, and electric power-driven devices. At present, most of the electrolytes of lithium-ion batteries are organic liquid electrolytes, which are composed of organic solvents and conductive lithium salts. Due to the abuse...

Claims

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Application Information

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IPC IPC(8): C07F9/09
CPCC07F9/091
Inventor 武利斌葛建民闫彩桥王军郝俊张民侯荣雪田丽霞张茜
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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