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Synthesis method of 3,3,3-trifluoropropene carbonate

A technology of propylene trifluorocarbonate and a synthesis method, which is applied in directions such as organic chemistry, can solve the problems of complex process, low product yield, high cost and the like, and achieves the effects of simple operation and high purity

Inactive Publication Date: 2020-11-06
SHIJIAZHUANG SAN TAI CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, as far as the existing 3,3,3-trifluoropropylene carbonate synthesis technology is concerned, there are problems such as complicated process, difficult to realize industrialized production, high cost and low product yield in the synthesis process, especially when 3,3,3-trifluoropropylene carbonate is used. The yield of 3-trifluoro-1,2-propanediol and triphosgene synthesis generally can only reach 60-70%

Method used

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  • Synthesis method of 3,3,3-trifluoropropene carbonate
  • Synthesis method of 3,3,3-trifluoropropene carbonate

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Mix 112g of 3,3,3-trifluoro-1,2-propylene oxide and 110mL of 0.1mol / L hydrochloric acid aqueous solution, add 0.2g of perfluorosulfonic acid resin, react at 40°C for 4 hours, and cool naturally to At room temperature, add potassium hydroxide solution with a mass fraction of 10%, pH 7.0, react for 35 minutes, distill under reduced pressure, filter, and fractionate to obtain 3,3,3-trifluoro-1,2-propanediol with a yield of 93.54 %;

[0023] Add 110 g of 3,3,3-trifluoro-1,2-propanediol obtained above and 84 g of triphosgene into 1200 mL of tetraethylene glycol dimethyl ether and mix, add 545 g of tetrabutylammonium bromide, and place in an ice bath at 0°C 250g of triethylamine was added dropwise with stirring, followed by GC until 3,3,3-trifluoro-1,2-propanediol disappeared, filtered, and the filtrate was rectified under reduced pressure to obtain the total yield of 3,3,3-trifluoropropylene carbonate The rate is 85.7%.

Embodiment 2

[0025] Mix 112g of 3,3,3-trifluoro-1,2-propylene oxide and 130mL of 0.1mol / L hydrochloric acid aqueous solution, add 0.3g of perfluorosulfonic acid resin, react at 42°C for 3.5 hours, and cool naturally to At room temperature, add sodium hydroxide solution with a mass fraction of 10% to it, pH 7.0, react for 45 minutes, distill under reduced pressure, filter, and fractionate to obtain 3,3,3-trifluoro-1,2-propanediol with a yield of 93.77 %;

[0026] Add 110g of 3,3,3-trifluoro-1,2-propanediol and 51g of triphosgene obtained above into 1500mL of tetraethylene glycol dimethyl ether and mix, add 800g of tetrabutylammonium bromide, and place in an ice bath at 0°C 172 g of triethylamine was added dropwise with stirring, followed by GC until 3,3,3-trifluoro-1,2-propanediol disappeared, filtered, and the filtrate was rectified under reduced pressure to obtain the total yield of 3,3,3-trifluoropropylene carbonate The rate is 86.3%.

Embodiment 3

[0028] Mix 112g of 3,3,3-trifluoro-1,2-propylene oxide and 120mL of 0.1mol / L hydrochloric acid aqueous solution, add 0.4g of perfluorosulfonic acid resin, react at 45°C for 5 hours, and cool naturally to At room temperature, add potassium hydroxide solution with a mass fraction of 10%, pH 7.0, react for 55 minutes, distill under reduced pressure, filter, and fractionate to obtain 3,3,3-trifluoro-1,2-propanediol with a yield of 94.15 %;

[0029] Add 110g of 3,3,3-trifluoro-1,2-propanediol obtained above and 62g of triphosgene into 1200mL of tetraethylene glycol dimethyl ether and mix, add 610g of tetrabutylammonium bromide, and place in an ice bath at 0°C 190g of triethylamine was added dropwise with stirring, followed by GC until the disappearance of 3,3,3-trifluoro-1,2-propanediol, filtered, and the filtrate was rectified under reduced pressure to obtain the total yield of 3,3,3-trifluoropropylene carbonate The rate is 87.1%.

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Abstract

The invention discloses a synthesis method of 3,3,3-trifluoropropene carbonate, belonging to the technical field of cosolvents or additives for battery electrolytes. 3,3,3-trifluoropropene carbonate is prepared from 3,3,3-trifluoro-1,2-epoxypropane. The method comprises the following steps: A, mixing 3,3,3-trifluoro-1,2-epoxypropane with an aqueous hydrochloric acid solution having a concentrationof 0.1 mol / L, adding perfluorosulfonic acid resin, carrying out a reaction at 35-45 DEG C for 3-5 h, conducting natural cooling to room temperature, then adding an alkaline solution with a pH value of 7.0, carrying out a reaction for 30-60 min, and carrying out reduced-pressure distillation, and performing filtration and fractionation to obtain 3,3,3-trifluoro-1,2-propanediol; and B, adding the 3,3,3-trifluoro-1,2-propanediol obtained in the step A and triphosgene into tetraethylene glycol dimethyl ether, conducting mixing, adding tetrabutylammonium bromide, performing stirring and dropwise adding triethylamine at 0 DEG C under an ice bath condition, conducting GC tracking until the 3,3,3-trifluoro-1,2-propanediol disappears, carrying out filtering, and rectifying a filtrate under reducedpressure to obtain the 3,3,3-trifluoropropene carbonate. The method has the advantages of cheap and easily-accessible raw materials, simple operation and environment friendliness, and the obtained 3,3,3-trifluoropropene carbonate has the advantages of high purity (up to 99.95%) and high yield (up to 85% or above).

Description

technical field [0001] The invention belongs to the technical field of battery electrolyte co-solvent or additive, and relates to a synthesis method of 3,3,3-trifluoropropylene carbonate which will be used as battery electrolyte co-solvent or additive. Background technique [0002] Lithium-ion batteries have been widely used in electric vehicles, hybrid vehicles, aerospace and other fields due to their advantages such as long life, large specific capacity, and no memory effect. However, with the widespread application of lithium-ion batteries in electric vehicles, energy storage and other fields, people put forward higher requirements for lithium-ion batteries, such as: higher energy density, wider operating temperature, better safety, etc. In order to solve this problem, it is necessary to design and synthesize new functional electrolytes or find suitable electrolyte additives to meet the application of lithium-ion batteries in special cases. [0003] 3,3,3-trifluoropropyl...

Claims

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Application Information

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IPC IPC(8): C07D317/36
CPCC07D317/36
Inventor 王军闫彩桥葛建民郝俊张民武利斌侯荣雪
Owner SHIJIAZHUANG SAN TAI CHEM CO LTD
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