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A kind of method for preparing trifluoromethanesulfonic acid by continuous hydrolysis

A technology of trifluoromethanesulfonic acid and trifluoromethanesulfonyl fluoride is applied in the field of continuous hydrolysis to prepare trifluoromethanesulfonic acid, which can solve the problems of affecting economic benefits, high energy consumption, and high preparation cost of trifluoromethanesulfonic acid, and achieves the The effect of avoiding by-products, low energy consumption, and saving preparation costs

Active Publication Date: 2022-08-09
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the preparation method of above-mentioned trifluoromethanesulfonic acid can obtain high-purity trifluoromethanesulfonic acid, because the energy consumption in the preparation process is higher, the preparation cost of trifluoromethanesulfonic acid is higher, affects economic benefit

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Select a sodium hydroxide solution with a mass fraction of 35% as a raw material for neutralizing the hydrolysis reaction, and inject trifluoromethanesulfonyl fluoride gas and sodium hydroxide solution into the falling film reactor through the feed port, and the falling film A falling film shell and tube reactor is used in the reactor. A redistributor is set at the top of the falling film shell and tube reactor. The trifluoromethanesulfonyl fluoride gas enters from the middle of each shell tube, and the alkali metal hydroxide solution runs along the inner wall of each shell tube. Inflow; the molar ratio of trifluoromethanesulfonyl fluoride gas to sodium hydroxide is 1:1.1, and the pressure inside the falling film shell and tube reactor is controlled at an absolute pressure of 0.15MPa, and the temperature is controlled at 45°C. At the same time, the trifluoromethanesulfonyl fluoride gas and the sodium hydroxide solution flow in parallel through the pipes inside the fa...

Embodiment 2

[0028] (1) Select a potassium hydroxide solution with a mass fraction of 30% as a raw material for neutralizing the hydrolysis reaction, and inject trifluoromethanesulfonyl fluoride gas and potassium hydroxide solution into the falling film reactor through the inlet, and the falling film reactor A falling-film shell-and-tube reactor is used, and a redistributor is set at the top of the falling-film shell-and-tube reactor, the trifluoromethanesulfonyl fluoride gas enters from the middle of each shell, and the alkali metal hydroxide solution flows along the inner wall of each shell; According to the molar ratio of trifluoromethanesulfonyl fluoride gas and potassium hydroxide solution of 1:1.12, the pressure inside the falling film shell and tube reactor was controlled at an absolute pressure of 0.18MPa, and the temperature was controlled at 47°C. The trifluoromethanesulfonyl fluoride gas and the potassium hydroxide solution flow in parallel in the pipes inside the falling film sh...

Embodiment 3

[0033] (1) Select a potassium hydroxide solution with a mass fraction of 40% as the raw material for the neutralization hydrolysis reaction, and inject trifluoromethanesulfonyl fluoride gas and potassium hydroxide solution into the falling film reactor through the inlet, and the falling film reactor A falling-film shell-and-tube reactor is used, and a redistributor is set at the top of the falling-film shell-and-tube reactor, the trifluoromethanesulfonyl fluoride gas enters from the middle of each shell, and the alkali metal hydroxide solution flows along the inner wall of each shell; Trifluoromethanesulfonyl fluoride gas and potassium hydroxide solution are in a molar ratio of 1:1.15, and the pressure inside the falling film tubular reactor is controlled at an absolute pressure of 0.20 MPa, and the temperature is controlled at 50 °C. At the same time, the trifluoromethanesulfonyl fluoride gas and the potassium hydroxide solution flow in parallel through the pipes inside the fa...

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Abstract

The invention relates to a method for preparing trifluoromethanesulfonic acid by continuous hydrolysis, and belongs to the technical field of fine chemicals. First, the trifluoromethanesulfonyl fluoride gas and the alkali metal hydroxide solution are sent into the falling film reactor from the feed port for continuous neutralization and hydrolysis, and the reaction liquid is obtained at the discharge port of the falling film reactor; then The reaction solution is pumped into a drying tower for drying, the dried solid is initially dissolved in a solvent, and the initially dissolved liquid enters the extraction tower through a diaphragm pump and is extracted by an extractant to obtain an alkali metal trifluoromethanesulfonic acid salt. ; Add the trifluoromethanesulfonic acid alkali metal salt and the concentrated sulfuric acid into the acidifying tower to carry out acidification reaction, obtain the trifluoromethanesulfonic acid crude product, and obtain a kind of high-purity trifluoromethanesulfonic acid after purification. The method realizes continuous production of trifluoromethanesulfonic acid, avoids the generation of by-products in the preparation of traditional production of trifluoromethanesulfonic acid, and the continuous hydrolysis method consumes less energy and can effectively save costs.

Description

technical field [0001] The invention relates to a method for preparing trifluoromethanesulfonic acid by continuous hydrolysis, and belongs to the technical field of fine chemicals. Background technique [0002] Trifluoromethanesulfonic acid is one of the strongest known organic acids, and the trifluoromethanesulfonic acid ion contained in it has extremely strong thermodynamic and chemical stability. This property makes trifluoromethanesulfonic acid play an important role in the field of organic chemical reactions. [0003] In Chinese patent application 201510173116.X a kind of preparation method of trifluoromethanesulfonic acid, halogenated trifluoromethane is used as raw material, in the environment of nitrogen protection, zinc powder and tetrahydrofuran are added, and after passing trifluorobromomethane gas A catalytic amount of elemental iodine is added, and the temperature-controlled reaction is performed to obtain a trifluoromethyl zinc halide reagent, and sulfur triox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/02C07C309/06
CPCC07C303/02C07C309/06Y02P20/10
Inventor 李林李柄缘李虹嶙吕灵华罗建志郝春辉滕鑫胜张明杰郭君袁瑞玲
Owner PERIC SPECIAL GASES CO LTD
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