Preparation process of trifluoromethanesulfonic anhydride

A technology of trifluoromethanesulfonic anhydride and trifluoromethanesulfonic acid, which is applied in the field of trifluoromethanesulfonic anhydride preparation technology, can solve the problem of multiple trifluoromethanesulfonic acid salt steps, reduce the preparation efficiency, and improve the overall yield of trifluoromethanesulfonic anhydride No high problems, to reduce time consumption, simplify the preparation process, improve efficiency and overall yield

Inactive Publication Date: 2020-09-22
JIANGXI GUOHUA IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Compared with CN201910769924.0, CN201210467020.0 has more steps for preparing trifluoromethanesulfonate, which increases the cost and reduces the efficiency of preparation, and the trifluoromethanesulfonic anhydride prepared by the above two patents has an overall yield not high problem

Method used

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  • Preparation process of trifluoromethanesulfonic anhydride

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Comparison scheme
Effect test

Embodiment 1

[0024] see figure 1 , the present invention provides a kind of technical scheme: a kind of trifluoromethanesulfonic anhydride preparation process comprises the steps:

[0025] Step 1: raw material preparation: trifluoromethanesulfonic acid, phosphorus pentoxide; the dosage of trifluoromethanesulfonic acid is 1.0 times of phosphorus pentoxide; trifluoromethanesulfonic acid generates viscous phosphoric acid after being dehydrated by phosphorus pentoxide Esters, part of trifluoromethanesulfonic anhydride doped in it, can not be evaporated, resulting in low overall yield, the amount of trifluoromethanesulfonic acid is 1.0 times that of phosphorus pentoxide, which helps to improve the overall yield;

[0026] Step 2: Mixing and stirring: under the protection of nitrogen, add phosphorus pentoxide and trifluoromethanesulfonic acid in sequence to the dry reaction kettle equipped with a thermometer, a distillation device and a stirring device. The reaction temperature is 20°C, which hel...

Embodiment 2

[0031] see figure 1 , the present invention provides a kind of technical scheme: a kind of trifluoromethanesulfonic anhydride preparation process comprises the steps:

[0032] Step 1: raw material preparation: trifluoromethanesulfonic acid, phosphorus pentoxide; the amount of trifluoromethanesulfonic acid is 1.4 times that of phosphorus pentoxide; trifluoromethanesulfonic acid generates viscous phosphoric acid after dehydration of phosphorus pentoxide Esters, part of the trifluoromethanesulfonic anhydride doped therein, can not be evaporated, resulting in a low overall yield, the amount of trifluoromethanesulfonic acid is 1.4 times that of phosphorus pentoxide, which helps to improve the overall yield;

[0033] Step 2: Mixing and stirring: under the protection of nitrogen, add phosphorus pentoxide and trifluoromethanesulfonic acid in turn to the dry reaction kettle equipped with a thermometer, a distillation device and a stirring device. The reaction temperature is 25 °C, whic...

Embodiment 3

[0038] see figure 1 , the present invention provides a kind of technical scheme: a kind of trifluoromethanesulfonic anhydride preparation process comprises the steps:

[0039] Step 1: raw material preparation: trifluoromethanesulfonic acid, phosphorus pentoxide; the amount of trifluoromethanesulfonic acid is 1.8 times that of phosphorus pentoxide; trifluoromethanesulfonic acid generates viscous phosphoric acid after dehydration of phosphorus pentoxide Esters, part of trifluoromethanesulfonic anhydride doped therein, can not be evaporated, resulting in low overall yield, the amount of trifluoromethanesulfonic acid is 1.8 times of phosphorus pentoxide, which helps to improve the overall yield;

[0040] Step 2: Mixing and stirring: under the protection of nitrogen, add phosphorus pentoxide and trifluoromethanesulfonic acid in sequence to the dry reaction kettle equipped with a thermometer, a distillation device and a stirring device. The reaction temperature is 30 °C, which helps...

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Abstract

The invention discloses a preparation process of trifluoromethanesulfonic anhydride. The preparation process comprises the following steps of: raw material preparation: preparing trifluoromethanesulfonic acid and phosphorus pentoxide; mixing and stirring: under the protection of nitrogen, sequentially adding phosphorus pentoxide and trifluoromethanesulfonic acid into a drying reaction kettle provided with a thermometer, a distillation device and a stirring device, and performing stirring under normal temperature and normal pressure; crude product preparation: carrying out reduced pressure distillation to obtain a trifluoromethanesulfonic anhydride crude product; and purification: under the protection of nitrogen, putting the trifluoromethanesulfonic anhydride crude product into a flask, connecting a distillation device, conducting vacuumizing and heating, and carrying out reduced pressure distillation to obtain refined trifluoromethanesulfonic anhydride. The beneficial effects of the invention are that: according to the method, trifluoromethanesulfonic acid and phosphorus pentoxide are adopted as the raw materials, the dosage of trifluoromethanesulfonic acid is 1.0-1.8 times that of phosphorus pentoxide, high-purity trifluoromethanesulfonic anhydride is obtained through the preparation process of mixing, stirring, distillation and purification, the preparation process is simplified, the preparation time is reduced, and the preparation efficiency and the overall yield are improved.

Description

technical field [0001] The invention belongs to the technical field of trifluoromethanesulfonic anhydride preparation, and in particular relates to a preparation process of trifluoromethanesulfonic anhydride. Background technique [0002] Trifluoromethanesulfonic anhydride is a derivative of trifluoromethanesulfonic acid. It is a colorless transparent liquid with a strong pungent odor. It reacts violently with water and produces smoke. It will cause corrosion and burns when it contacts the eyes or skin. Stimulate the respiratory tract and cause emphysema; trifluoromethanesulfonic anhydride is widely used in the chemical and pharmaceutical fields, and as an important chemical intermediate and catalyst, it has broad application prospects and market demand. [0003] The application number is CN201210467020.0, which discloses the preparation method of trifluoromethanesulfonic anhydride. Trifluoromethanesulfonyl fluoride is reacted with alkali metal hydroxide to prepare trifluoro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/00C07C303/44C07C309/06
CPCC07C303/00C07C303/44C07C309/06
Inventor 陈红斌祝金玲黄素玉
Owner JIANGXI GUOHUA IND CO LTD
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