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Synthesis method of trifluoroethoxy vinyl phosphate

A technology of vinyl trifluoroethoxy phosphate and synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., which can solve the problems of poor purity, lower reaction efficiency, and influence on reaction Yield and other issues, to achieve the effect of reducing the violent occurrence of side reactions, mild reaction process, and simple reaction process

Pending Publication Date: 2021-12-07
SHIJIAZHUANG SAN TAI CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that a two-step reaction is required to obtain the final product, and the chlorinated cyclic phosphate intermediate has poor stability and is not easy to purify and store, which will eventually affect the subsequent reaction yield and reduce the overall reaction efficiency
[0004] At present, the production and purification methods of trifluoroethoxy vinyl phosphate are not perfect enough, and the uncertainty of various parameters in the manufacturing process leads to low production capacity and relatively poor purity

Method used

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  • Synthesis method of trifluoroethoxy vinyl phosphate
  • Synthesis method of trifluoroethoxy vinyl phosphate
  • Synthesis method of trifluoroethoxy vinyl phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The synthetic method of trifluoroethoxy vinyl phosphate, its synthetic steps are as follows:

[0022] Disperse 0.3 g of nano-aluminum phosphate in 20 mL of dichloromethane to obtain a nano-aluminum phosphate dispersion;

[0023] Take 15.33g (0.1mol) of phosphorus oxychloride and 17.05g (0.105mol) of hexamethyldisiloxane, stir and mix them and carry out pre-reaction at 30°C for 1h, then add nano-aluminum phosphate dispersion at 30°C, and then maintain for 30 Slowly add 6.83g (0.11mol) ethylene glycol and 11g (0.11mol) trifluoroethanol dropwise at °C, slowly raise the temperature to 80°C, maintain 80°C for esterification reaction for 6h, filter, concentrate under reduced pressure to remove volatile solvents, and pass Vigreux Fractional distillation in the fractionating column yielded 19.01g trifluoroethoxy vinyl phosphate (also known as 2-trifluoroethoxy-2-oxo-1,3,2-dioxaphospholane), yield 92.25% , with a purity of 99.7%, the specific chemical reaction formula is as fol...

Embodiment 2

[0026] The synthetic method of trifluoroethoxy vinyl phosphate, its synthetic steps are as follows

[0027] Disperse 0.46g of nano-aluminum phosphate in 20mL of dichloromethane to obtain a nano-aluminum phosphate dispersion;

[0028] Take 15.33g (0.1mol) of phosphorus oxychloride and 17.86g (0.11mol) of hexamethyldisiloxane, stir and mix them and carry out pre-reaction at 25°C for 1.2h, then add nano-aluminum phosphate dispersion at 25°C, and then maintain Slowly add 7.14g (0.115mol) ethylene glycol and 11.5g (0.115mol) trifluoroethanol dropwise at 25°C, slowly raise the temperature to 85°C, maintain 85°C for esterification for 5 hours, filter, concentrate under reduced pressure to remove volatile solvents, and then Vigreux fractionation column fractionation, namely get 18.97g trifluoroethoxy vinyl phosphate (also known as 2-trifluoroethoxy-2-oxo-1,3,2-dioxaphospholane), yield 92.06%, purity 99.5%.

Embodiment 3

[0030] The synthetic method of trifluoroethoxy vinyl phosphate, its synthetic steps are as follows:

[0031] Disperse 0.15 g of nano-aluminum phosphate in 15 mL of dichloromethane to obtain a nano-aluminum phosphate dispersion;

[0032] Take 15.33g (0.1mol) of phosphorus oxychloride and 17.54g (0.108mol) of hexamethyldisiloxane and stir and mix them at 20°C for 1.4h, then add nano-aluminum phosphate dispersion at 20°C, and then maintain Slowly add 7.01g (0.113mol) ethylene glycol and 12g (0.12mol) trifluoroethanol dropwise at 20°C, slowly raise the temperature to 83°C, maintain 83°C for esterification reaction for 4h, filter, concentrate under reduced pressure to remove volatile solvents, and then Vigreux fractionation column fractionation, obtains 19.12g trifluoroethoxy vinyl phosphate (also known as 2-trifluoroethoxy-2-oxo-1,3,2-dioxaphospholane), yield 92.79 %, purity 99.6%.

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Abstract

The invention discloses a synthesis method of trifluoroethoxy vinyl phosphate, and relates to the technical field of battery electrolyte additives. The synthesis method comprises the following steps: taking phosphorus oxychloride and hexamethyldisiloxane for pre-reaction, dropwise adding ethylene glycol and trifluoroethanol, and carrying out esterification reaction to obtain the trifluoroethoxy vinyl phosphate. According to the invention, the phosphorus oxychloride, the ethylene glycol and the trifluoroethanol are taken as raw materials and are directly subjected to cyclization reaction, and dichloromethane is added as a solvent to disperse a reaction system, so that severe side reaction can be reduced, and the reaction is promoted to proceed towards a required reaction direction. According to the method, the reaction process is simple, raw materials used in the reaction are easy to obtain, the reaction process is milder and safer compared with the prior art, and the yield of the product is further improved by reasonably controlling the dosage of the reaction raw materials and the reaction process, so that the yield reaches 32.61% or above, and the purity reaches 99.5% or above.

Description

technical field [0001] The invention relates to the technical field of battery electrolyte additives, in particular to a synthesis method of trifluoroethoxy vinyl phosphate. Background technique [0002] Lithium-ion batteries are currently the most common electrical energy storage devices. Compared with traditional batteries, they have higher storage capacity and more stable performance. The key factors affecting the performance of lithium-ion batteries lie in the performance of organic electrolytes. Adding an electrolyte additive containing trifluoroethoxyethylene phosphate to the electrolyte during battery production can effectively prevent thermal runaway of the battery and improve the safety performance of the lithium-ion battery. [0003] In the prior art, the preparation process of vinyl trifluoroethoxy phosphate is mainly through the reaction of phosphorus oxychloride and ethylene glycol to generate a chlorinated cyclic phosphoric acid ester intermediate, which is pur...

Claims

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Application Information

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IPC IPC(8): C07F9/6574
CPCC07F9/65742
Inventor 赵光华高山林胜赛李庆占邢艳召刘鹏田丽霞张茜张民彭鹏鹏郝俊侯荣雪王军葛建民武利斌闫彩桥许晓丹闫朋飞杨世雄牛庾鑫张利辉
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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