Preparation method of trifluoro methanesulfonic anhydride

A technology of trifluoromethanesulfonic anhydride and trifluoromethanesulfonic acid salt, which is applied in the field of preparation of trifluoromethanesulfonic anhydride, can solve the problems of difficult purification, solidification of reaction liquid, and difficult reaction, and achieve simple, convenient and simplified operation process Reaction steps, effects of avoiding by-products

Active Publication Date: 2013-02-06
JIANGXI GUOHUA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The above-mentioned chemical method has a simple process, mild conditions, and is easy to operate, but its raw material, bistrifluoromethyl disulfide, can be used as a chemical warfare agent, which is extremely toxic and is an extremely dangerous substance, and the yield is low, difficult to purify, and difficult to produce. Industrial production; the raw materials of electrochemical fluorination method are cheap and easy to buy, and the process is mature, but hydrogen gas is easy to be generated during the electrolytic reaction process, and there will be accumulation of glassy by-product polyphosphoric acid when anhydride is prepared with phosphorus pentoxide and sulfonic acid , causing the reaction solution to solidify, the reaction solution is difficult to stir, and then the reaction is difficult to carry out. In addition, polyphosphoric acid is not easy to remove and not easy to carry out post-treatment of the reaction, it is difficult to distill and recover trifluoromethanesulfonic acid and diluted polyphosphoric acid, making industrialization exist many problems

Method used

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preparation example Construction

[0020] The preparation method of trifluoromethanesulfonic anhydride of the present invention may further comprise the steps:

[0021] 1. Preparation of trifluoromethanesulfonate: trifluoromethanesulfonyl fluoride gas is mixed with alkali metal hydroxide solution to prepare trifluoromethanesulfonate, and the concentration of alkali metal hydroxide solution is 20%-40% When the concentration is less than 20%, the hydrolysis rate is slow, and the content of trifluoromethanesulfonate is low after the end of hydrolysis, which wastes energy when evaporating and crystallizing. The hydrolysis reaction is difficult to reach the end; the hydrolysis temperature is 20-80°C, when the temperature is 80°C, the vapor pressure of water is too large, resulting in waste, and it is easy to overheat Cause the cracking of trifluoromethanesulfonyl fluoride gas; control the flow rate of trifluoromethanesulfonyl fluoride gas so that the gas content in the gas outlet of the hydrolysis tower is ≤0.5%.

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Embodiment 1

[0026] Prepare 224g of 25% KOH solution, and slowly inject trifluoromethanesulfonyl fluoride gas into the KOH solution until the solution is neutral, then 273.6g of acid fluoride gas is introduced. After evaporation and drying, potassium trifluoromethanesulfonate solid powder was obtained, which was refined with ethanol to obtain 173 g of potassium trifluoromethanesulfonate. Mix 340g of trifluoromethanesulfonyl chloride and the obtained potassium trifluoromethanesulfonate, and stir the reaction for 6 h at 15°C, obtain 253.8g of trifluoromethanesulfonic anhydride by distillation, and the measured main content is 99.92%, F - :10ppm, SO 4 2- : 20ppm, Cl - :15ppm.

Embodiment 2

[0028] Slowly feed trifluoromethanesulfonyl fluoride gas into the LiOH solution with a mass fraction of 18% until the solution is neutral, the consumed LiOH is 48g, and the acyl fluoride gas is 456g. After evaporation and drying, 338.4 g of potassium trifluoromethanesulfonate solid powder is obtained. g, obtained 326.6 g of potassium trifluoromethanesulfonate after refining with acetone. The refined potassium trifluoromethanesulfonate was put into 455g of trifluoromethanesulfonyl chloride for mixed reaction, stirred at 10°C for 5 h, and 486g of trifluoromethanesulfonic anhydride was obtained by distillation. The measured main content is 99.90%, F - :30ppm, SO 4 2- :20ppm, Cl - :20ppm.

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Abstract

The invention provides a preparation method of trifluoro methanesulfonic anhydride. The method comprises the following steps of: firstly reacting trifluoro methanesulphonyl fluoride with alkali metal hydroxide to prepare trifluoro mesylate, purifying trifluoro mesylate by recrystallization by utilizing an organic solvent, reacting trifluoro methane sulfonyl chloride with trifluoro mesylate to generate a trifluoro methanesulfonic anhydride crude product, and finally purifying trifluoro methanesulfonic anhydride by atmospheric distillation. The preparation method of trifluoro methanesulfonic anhydride can be used for not only effectively simplifying reaction steps so that the operation process is simple and convenient and the operation is safe, but also avoiding byproducts generated in the process of the traditional method for producing trifluoro methanesulfonic anhydride, and effectively reducing the contents of F<-> and SO4<2-> in the product; by utilizing recrystallization, atmospheric distillation and other methods for purification, the product purity is up to 99.5%; and more importantly, the yield of anhydride is greatly increased and raised to 88% from original 60%.

Description

technical field [0001] The invention relates to a preparation method of trifluoromethanesulfonic anhydride. Background technique [0002] As the anhydride of trifluoromethanesulfonic acid, a super acid, trifluoromethanesulfonic anhydride is extremely stable in redox. Widely used in plastic processing industry, pharmaceutical industry, synthesis of vitamins and sugar industry. In addition, trifluoromethanesulfonic anhydride is also an intermediate in drug synthesis and agricultural chemicals, and has a wide range of uses. Its derivative lithium trifluoromethanesulfonate is one of the important raw materials for lithium batteries. Known methods for synthesizing trifluoromethanesulfonic anhydride include chemical synthesis and electrochemical fluorination. The chemical synthesis method uses bistrifluoromethyl disulfide as raw material to generate trifluoromethanesulfonic acid, and then dehydrates trifluoromethanesulfonic acid with a certain proportion of phosphorus pentoxide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/06C07C303/00
Inventor 陈红斌魏伟群
Owner JIANGXI GUOHUA IND CO LTD
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