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Preparation method of trifluoromethane sulfonic acid

A technology of trifluoromethanesulfonic acid and trifluoromethanesulfonic acid base, applied in the field of preparation of trifluoromethanesulfonic acid, can solve the problems of limited potassium fluoride removal ability, equipment corrosion, equipment corrosion and the like, and achieves The effect of reducing drying and water removal requirements, improving operational flexibility, and extending service life

Active Publication Date: 2016-06-22
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In patent CN101885691A, the potassium fluoride produced during the synthesis of trifluoromethanesulfonic acid alkali metal salt solution from trifluoromethanesulfonyl fluoride can ionize a large amount of fluoride ions, which are the root cause of corrosion of equipment. Treatment by crystallization increases the complexity of the process, and the crystallization process has a limited ability to remove potassium fluoride; the residual potassium fluoride also severely corrodes the equipment during the acidification process, and the hydrogen fluoride formed during the acidification process enters the The follow-up process results in high fluoride ions in the product, which reduces the stability and quality of the product; in this patent, only concentrated sulfuric acid is used to acidify the alkali metal trifluoromethanesulfonate, and its water content is as high as 2%~5%. High is another major factor causing poor product stability and serious equipment corrosion

Method used

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  • Preparation method of trifluoromethane sulfonic acid
  • Preparation method of trifluoromethane sulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 793g of potassium hydroxide aqueous solution with a concentration of 49.4%, 560g of calcium hydroxide and 774g of high-purity water in sequence in a 304 stainless steel reaction kettle, heat up to 70°C, mix and stir for 2 hours; then continuously feed trifluoromethanesulfonyl fluoride gas quantitatively , control the reaction pressure between 0.2MPa~1.0MPa; stop the ventilation when the ventilation quality is 980g trifluoromethanesulfonyl fluoride, the ventilation time is 3 hours, then keep the temperature for 2 hours, and then cool down to 25 °C; the above reaction solution Filter to obtain potassium trifluoromethanesulfonate aqueous solution, the concentration of potassium trifluoromethanesulfonate is 46.81%, pH=14, F - =5ppm, ICP detection: Fe: 0.5ppm, Ni: 0.1ppm. Fluoride ion concentration

[0035] The aqueous solution of above-mentioned potassium trifluoromethanesulfonate was evaporated to dryness to obtain potassium trifluoromethanesulfonate 1201g, w...

Embodiment 2

[0037] Add 793g of potassium hydroxide aqueous solution with a concentration of 49.4%, 434g of calcium hydroxide and 774g of high-purity water into a 304 stainless steel reaction kettle in sequence, raise the temperature to 70°C, mix and stir for 2 hours; then continuously feed trifluoromethanesulfonyl fluoride gas quantitatively , control the reaction pressure between 0.2MPa~1.0MPa; stop the ventilation when the ventilation quality is 980g trifluoromethanesulfonyl fluoride, the ventilation time is 3 hours, then keep the temperature for 2 hours, and then cool down to 25 °C; the above reaction solution Filter to obtain potassium trifluoromethanesulfonate aqueous solution, the concentration of potassium trifluoromethanesulfonate is 48.74%, pH=14, F - =4ppm, ICP detection: Fe: 0.4ppm, Ni: 0.09ppm. Fluoride ion concentration

[0038] The aqueous solution of above-mentioned potassium trifluoromethanesulfonate was evaporated to dryness to obtain potassium trifluoromethanes...

Embodiment 3

[0040] Add 875g of 32.0% aqueous sodium hydroxide solution, 424g of calcium oxide and 580g of high-purity water in sequence in a 316L stainless steel reaction kettle, raise the temperature to 85°C, and mix and stir for 3 hours; Control the reaction pressure between 0.2MPa and 1.0MPa; stop the ventilation when the ventilation mass is 980g trifluoromethanesulfonyl fluoride, the ventilation time is 4 hours, then keep the temperature for 2.5 hours, and then lower the temperature to 25°C; carry out the above reaction solution Filter to obtain sodium trifluoromethanesulfonate aqueous solution, the concentration of sodium trifluoromethanesulfonate is 47.55%, pH=14, F - =7ppm, ICP detection: Fe: 0.5ppm, Ni: 0.14ppm. Fluoride ion concentration

[0041] The aqueous solution of above-mentioned sodium trifluoromethanesulfonate is evaporated to dryness to obtain sodium trifluoromethanesulfonate 1100g, moisture content 9200ppm, F - =15ppm; Then add 105% oleum of 1100g to carr...

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Abstract

The invention relates to a preparation method of trifluoromethane sulfonic acid. According to the preparation method, trifluoromethanesulphonyl fluoride and alkali metal hydroxide are subjected to a neutralizing hydrolysis reaction under existence of a fluorine fixing agent, after the reaction is completed, reaction liquid is filtered and dried, and fluorinated methyl sulfonic acid alkali metal salt is obtained; the fluorinated methyl sulfonic acid alkali metal salt and fuming sulphuric acid are subjected to acidizing treatment, then rectification is conducted multiple times, and high-purity trifluoromethane sulfonic acid is obtained. Through improvement of the preparation method, operating flexibility, production efficiency and product stability are improved, the comprehensive yield is raised, product purity can reach 99.90% or above, and the preparation method is suitable for industrial production.

Description

technical field [0001] The present invention specifically relates to a kind of preparation method of trifluoromethanesulfonic acid. Background technique [0002] Trifluoromethanesulfonic acid is a strong proton-donating (H + ) super organic acid, its trifluoromethanesulfonate (CF 3 SO 3 - ) has extremely strong thermodynamics and chemical stability, and even under the action of strong nucleophiles, the dissociation of C-F bonds will not occur. Trifluoromethanesulfonic acid is used in industrial catalysis, organic synthesis, biopharmaceuticals, high-performance materials, It has a very wide range of applications in new energy and other fields. [0003] The current Simons electrolytic fluorination is currently the methyl (CH 3 - ) Synthesis of trifluoromethyl (CF 3 - ) is the most effective industrialized process route, which uses methanesulfonyl chloride or methanesulfonyl fluoride as a raw material, electrolytically synthesizes trifluoromethanesu...

Claims

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Application Information

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IPC IPC(8): C07C303/32C07C303/02C07C309/06
CPCC07C303/02C07C303/32C07C309/06
Inventor 邹凯任齐都何永刚钱晓兵李建中
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS