Trifluoromethanesulfonic acid preparation method

A kind of technology of trifluoromethanesulfonic acid and sodium trifluoromethanesulfonate

Active Publication Date: 2015-06-24
JIANGXI GUOHUA IND CO LTD
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  • Application Information

AI Technical Summary

Benefits of technology

This patented technology helps reduce harmful chemical substances produced during making certain types of compounds that are used in medicine or other industries like electronics manufacturing processes without generating unwanted side products. It also improves the quality of these final products while reducing their chlorine content compared with previous techniques.

Problems solved by technology

Technological Problem addressed in this patented technical problem involves finding ways to make highly pure trichromoacetic acid (TCA) without containing harmful impurities like triphenyltriazenium ion(PTZ). Current methods involve expensive starting materials and complex manufacturing processes involving multiple reactors.

Method used

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preparation example Construction

[0025] The preparation method of trifluoromethanesulfonic acid of the present invention comprises the following steps:

[0026] 1. Preparation of trifluoromethyl zinc halide: under the protection of nitrogen, mix zinc powder with tetrahydrofuran solvent at room temperature, and after obtaining the suspension, feed part of trifluorohalomethane gas, add a catalytic amount of elemental iodine as a catalyst, and heat slowly When the temperature rises to 40°C, after the reaction starts, slowly feed the remaining halotrifluoromethane gas, control the temperature below 50°C and stir for 5 hours to obtain the trifluoromethylzinc halide reaction solution.

[0027] 2. Preparation of zinc halide trifluoromethanesulfonate: adding solid sulfur trioxide to the prepared zinc trifluoromethanesulfonate halide reaction liquid, stirring and reacting for 2.0 h to obtain zinc halide trifluoromethanesulfonate reaction liquid.

[0028] 3. Preparation of sodium trifluoromethanesulfonate: In the prepa...

Embodiment 1

[0031] Under the protection of nitrogen, 66g of trifluorochloromethane liquid was passed into 1L tetrahydrofuran suspension of 212g of zinc powder, and then a catalytic amount of elemental iodine was added, and slowly heated to 40°C. After the reaction should occur, slowly passed into 198g of trifluoromethane Fluorochloromethane, control the temperature not to exceed 50°C. After stirring and reacting for 5 hours, slowly add 260 g of solid sulfur trioxide, and stir and react for 2 hours after feeding is completed. The reaction solution was neutralized with 30% aqueous sodium hydroxide solution, and when no precipitation occurred, the solid was filtered off, and the filtrate was evaporated and dried to obtain sodium trifluoromethanesulfonate as a solid. Mix and stir the sodium salt and 240g of concentrated sulfuric acid, react at 100°C for 5h, and rectify to obtain 160.7g of trifluoromethanesulfonic acid. (Content: 99.98%; F - :5ppm; Cl - : 0ppm; SO 4 2- :9ppm)

Embodiment 2

[0033] Under the protection of nitrogen, 100 g of bromotrifluoromethane liquid was passed into 1 L of tetrahydrofuran suspension of 212 g of zinc powder, and then a catalytic amount of elemental iodine was added, and slowly heated to 40 ° C. After the reaction should start, 300 g of trifluoromethane was slowly passed into For methyl bromide, the temperature should not exceed 50°C. After stirring and reacting for 5 hours, slowly add 260 g of solid sulfur trioxide, and stir and react for 2 hours after feeding is completed. The reaction solution was neutralized with 30% aqueous sodium hydroxide solution, and when no precipitation occurred, the solid was filtered off, and the filtrate was evaporated and dried to obtain sodium trifluoromethanesulfonate as a solid. Mix and stir the sodium salt and 240g of concentrated sulfuric acid, react at 100°C for 5h, and rectify to obtain 167.5g of trifluoromethanesulfonic acid. (Content: 99.97%; F - : 7ppm; Cl - : 0ppm; SO 4 2- :8ppm)

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Abstract

The invention relates to a trifluoromethanesulfonic acid preparation method. The method includes: taking halogenated trifluoromethane as a raw material, adding zinc powder and terahydrofuran under the environment of nitrogen protection and feeding trifluoro bromomethane gas prior to adding catalytic amount to obtain lodine; obtaining trifluoromethyl zinc halide through temperature control reaction, adding sulfur trioxide for continuous reaction to generate halogenated trifluoromethane sulfonic acid zinc; adding reaction liquid into alkali liquid for neutralization, evaporating filter liquid to dryness to obtain solid sodium trifluoromethanesulfonate salt prior to acidizing and rectifying to obtain trifluoromethanesulfonia acid. With the method, generation of accessory substances during the production is effectively reduced; the situation about higher fluorinion, chloridion and sulfate ion in trifluoromethanesulfonia acid products in a traditional technology is avoided. In addition, the purity of the trifluoromethanesulfonia acid obtained from distillation and purification can reach 99.95% above, and the yield can reach 83%.

Description

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Claims

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Application Information

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Owner JIANGXI GUOHUA IND CO LTD
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