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Process for preparing high-purity trifluoromethyl sulphonic acid

A technology of trifluoromethanesulfonic acid and trifluoromethanesulfonic acid salt, which is applied in the field of preparing high-purity trifluoromethanesulfonic acid, and can solve the problem that the hydrolysis reaction speed of trifluoromethanesulfonyl fluoride gas is slow and the reaction is insufficient. , loss of raw materials, etc.

Active Publication Date: 2009-04-08
PERIC SPECIAL GASES CO LTD
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] In this way, the shortcomings of this process are: the hydrolysis reaction rate of trifluoromethanesulfonyl fluoride gas is slow, and the problem of insufficient reaction will occur, resulting in the loss of raw materials and polluting the environment; the potassium fluoride and hydrogen produced by hydrolysis Potassium oxide and other impurities are not removed in time, resulting in F in potassium trifluoromethanesulfonate - The content is very large, thereby increasing the difficulty of purification of trifluoromethanesulfonic acid; it is difficult to make the F in the crude product by simple distillation method - down to below 10ppm

Method used

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  • Process for preparing high-purity trifluoromethyl sulphonic acid

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Embodiment

[0019] Add 8 kg of 20% KOH aqueous solution into the 10L hydrolysis tower through circulation pump 1, install 5 × 5θ nickel rings in the hydrolysis tower 2, and heat up the temperature of the hydrolysis tower 2 to 90-95 ° C, at this time, the trifluoromethanesulfonyl fluoride gas is discharged from the tower The air inlet at the bottom leads into the hydrolysis tower 2, and the KOH aqueous solution is guaranteed to circulate during the reaction process, and the circulation speed is about 5m 3 / h, the hydrolysis tower 2 is as shown in the accompanying drawing.

[0020] The ventilation flow rate of trifluoromethanesulfonyl fluoride is controlled so that the content of trifluoromethanesulfonyl fluoride in the gas outlet is less than 0.2%. The reaction was carried out for 12 hours, the pH of the solution in the hydrolysis tower 2 reached 11, the inlet valve was closed, the reaction was stopped, and the consumption of trifluoromethanesulfonyl fluoride was 2.2 kg. The hydrolysis so...

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Abstract

The invention relates to a process method for preparing high-purity trifluoromethane sulfonic acid. The process method comprises the following steps: firstly, hydrolyzing trifluoromethane sulfuryl fluoride gas prepared by an electrochemical fluorination method in alkaline metal or alkaline-earth metal hydroxide solution, recrystallizing the generated trifluoromethane sulphonate in a solvent to purify, and then reacting the trifluoromethane sulphonate with 100 percent of sulfuric acid in the presence of silicon dioxide to obtain an initial product of the trifluoromethane sulfonic acid, and finally purifying the trifluoromethane sulfonic acid through reduced pressure distillation. The process method not only effectively improves the hydrolysis speed of the trifluoromethane sulfuryl fluoride gas, leads the trifluoromethane sulfuryl fluoride gas to react more completely, and improves the yield, but also effectively reduces the content of F<-> in the trifluoromethane sulfonic acid product, and improves the purity of the product.

Description

technical field [0001] The invention relates to a process for preparing high-purity trifluoromethanesulfonic acid, which is suitable for preparing trifluoromethanesulfonic acid based on an electrochemical fluorination method. Background technique [0002] As one of the super acids, trifluoromethanesulfonic acid is extremely stable to redox and can be used as a catalyst for polymerization, esterification, coagulation, dehydration and other reactions, and is widely used in plastic industry, fuel industry, pharmaceutical industry, herbicide and growth Synthesis of regulators, synthesis of vitamins and the sugar industry, etc. In addition, trifluoromethanesulfonic acid 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-ion batteries. Known methods for preparing trifluoromethanesulfonic acid mainly include chemical synthesis and ele...

Claims

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Application Information

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IPC IPC(8): C07C309/39C07C303/02C07C303/44C25B3/08C25B3/28
Inventor 杨献奎李绍波李翔宇商洪涛郑秋艳
Owner PERIC SPECIAL GASES CO LTD
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