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Method for continuously preparing ethyl trifluoromethanesulfonate

A technology of ethyl trifluoromethanesulfonate and trifluoromethanesulfonic acid, which is applied in the field of preparation of ethyl trifluoromethanesulfonate, can solve the problems of long production cycle, high energy consumption, low yield, etc. Short, low energy consumption, simple process effect

Active Publication Date: 2014-06-25
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The disadvantages of the above synthesis process are: long production cycle, high energy consumption, many side reactions, by-products such as ethylene and trifluoromethanesulfonic acid monohydrate, and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] (1) Put 300g of trifluoromethanesulfonic acid and 154g of diethyl sulfate into a 5L glass reactor, start stirring, then raise the temperature of the reactor to 80°C, and keep it warm for 5 hours; (2) Raise the temperature of the reactor to 110-130°C , open the rectifying tower valve, control the reflux ratio to be 1: 1; Simultaneously, add trifluoromethanesulfonic acid and diethyl sulfate continuously in the reactor, trifluoromethanesulfonic acid is added into the reactor continuously with the rate of 30g / min In the process, diethyl sulfate is continuously added to the reaction kettle at a rate of 15g / min. After the reaction rectification, the temperature at the top of the rectification tower is stabilized at about 115±3°C. The distillate is collected and condensed. The chromatographic purity of ethyl methanesulfonate is as high as 99.3%, and the product enters the finished product collection tank. In this test, 3Kg of trifluoromethanesulfonic acid and 1.54Kg of diethyl...

Embodiment 2

[0016] (1) Put 300g of trifluoromethanesulfonic acid and 154g of diethyl sulfate into a 5L glass reactor, start stirring, then raise the temperature of the reactor to 50°C, and keep it warm for 2 hours; (2) Raise the temperature of the reactor to 100-120°C , open the rectifying tower valve, control the reflux ratio to be 1: 1; Simultaneously, add trifluoromethanesulfonic acid and diethyl sulfate continuously in the reactor, trifluoromethanesulfonic acid is added into the reactor continuously with the rate of 35g / min In the process, diethyl sulfate is continuously added to the reaction kettle at a rate of 32g / min. After the reaction rectification, the temperature at the top of the rectification tower is stabilized at about 115±3°C. The distillate is collected and condensed. The chromatographic purity of ethyl methanesulfonate is as high as 99.2%, and the product enters the finished product collection tank. This test drops into trifluoromethanesulfonic acid 3Kg altogether, dieth...

Embodiment 3

[0019] (1) Put 300g of trifluoromethanesulfonic acid and 154g of diethyl sulfate into a 5L glass reactor, start stirring, then raise the temperature of the reactor to 60°C, and keep it warm for 2 hours; (2) Raise the temperature of the reactor to 120-140°C , open the rectifying tower valve, control the reflux ratio to be 3: 1; Simultaneously, add trifluoromethanesulfonic acid and diethyl sulfate continuously in the reactor, trifluoromethanesulfonic acid is added into the reactor continuously with the speed of 30g / min In the process, diethyl sulfate is continuously added to the reaction kettle at a rate of 15g / min. After the reaction rectification, the temperature at the top of the rectification tower is stabilized at about 115±3°C. The distillate is collected and condensed. The chromatographic purity of ethyl methanesulfonate is as high as 99.4%, and the product enters the finished product collection tank. This test drops into trifluoromethanesulfonic acid 3Kg altogether, diet...

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PUM

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Abstract

A disclosed method for continuously preparing ethyl trifluoromethanesulfonate comprises the following steps: (1) adding trifluoromethanesulfonic acid and diethyl sulfate with the molar ratio of (1-2):1 into a reaction kettle, switching on a stirring apparatus, raising the temperature of the reaction kettle to 50-100 DEG C, and keeping the temperature for reacting for 2-6 h; and (2) raising the temperature of the reaction kettle to 100-150 DEG C, switching on a rectifying apparatus, controlling the reflux ratio of the rectifying apparatus at (1-3):(3-1), continuously introducing trifluoromethanesulfonic acid and diethyl sulfate into the reaction kettle, controlling the speed of trifluoromethanesulfonic acid introduced into the reaction kettle at 30-70 g / min, controlling the speed of diethyl sulfate introduced into the reaction kettle at 10-50 g / min, and collecting a distillation fraction and condensing to obtain ethyl trifluoromethanesulfonate. The preparation method is short in production period and low in energy consumption, and prepared ethyl trifluoromethanesulfonate has the purity larger than 99%, the yield is 90% or more, and industrialized production can be realized.

Description

technical field [0001] The present invention relates to the preparation method of ethyl trifluoromethanesulfonate. Background technique [0002] Ethyl trifluoromethanesulfonate is a derivative of trifluoromethanesulfonic acid, which is widely used as an intermediate in chemical, pharmaceutical and other industries. [0003] At present, the synthesis process of ethyl trifluoromethanesulfonate is mainly to react with ethanol or ether and trifluoromethanesulfonic acid to obtain a mixture of ethyl trifluoromethanesulfonate and water, and then go through post-treatment procedures such as liquid separation and drying. [0004] The disadvantages of the above synthesis process are: long production cycle, high energy consumption, many side reactions, and by-products such as ethylene and trifluoromethanesulfonic acid monohydrate will be generated, and the yield is low. Contents of the invention [0005] The purpose of this invention is to provide a kind of technique simple, short p...

Claims

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Application Information

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IPC IPC(8): C07C309/65C07C303/26C01B17/90
Inventor 徐晓强李建中郭军施苏萍钱晓兵何永刚余三宝杨升
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS