Purification method of trifluoromethanesulfonic anhydride

A technology of trifluoromethanesulfonic anhydride and a purification method, which is applied in the field of purification of trifluoromethanesulfonic anhydride, can solve the problems of low product purity and complicated process, and achieves the effects of high purification efficiency, simple operation and improved economic benefits.

Active Publication Date: 2013-12-18
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] For existing trifluoromethanesulfonic anhydride purification process technology is more complicated, and the defect that the product purity that obtains is lower, the o

Method used

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  • Purification method of trifluoromethanesulfonic anhydride
  • Purification method of trifluoromethanesulfonic anhydride
  • Purification method of trifluoromethanesulfonic anhydride

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Raw materials: The crude product of trifluoromethanesulfonic anhydride is obtained by the reaction of trifluoromethanesulfonic acid and phosphorus pentoxide, and its main components are shown in Table 3.

[0030] Table 3 trifluoromethanesulfonic anhydride crude product composition list

[0031]

[0032] Rectification device: rectification kettle 1 is a 1000ml round-bottom flask, glass rectification tower 2 has an inner diameter of 25mm, and is equipped with 3mm×3mmθ mesh ring packing, and the number of trays is 10.

[0033] Rectification process: 1200g trifluoromethanesulfonic anhydride crude product (its composition is shown in Table 3) is joined in the round-bottomed flask, vacuumizes the rectification system, makes pressure be-0.025MPa, starts heating, and opens the cooling of reflux device 3 The water starts to reflux completely, and the total reflux time is 1h, so that the impurity component with a boiling point lower than that of trifluoromethanesulfonic anhydr...

Embodiment 2

[0040] Raw material: with embodiment 1

[0041]Rectification device: rectification kettle with 1000ml round bottom flask, glass rectification tower 2 with inner diameter of 25mm, 3mm×3mmθ ring packing inside, 30 trays.

[0042] Rectification process: 1200g trifluoromethanesulfonic anhydride crude product (its composition is shown in Table 3) is joined in the round bottom flask, vacuumizes the rectification system, makes pressure be-0.065MPa, starts heating, and opens the cooling of reflux device 3 The water starts to fully reflux, and the total reflux time is 5 hours, so that the impurity component with a boiling point lower than that of trifluoromethanesulfonic anhydride is enriched at the top of the rectifying tower 2 . Then, when the rectifying still 1 temperature is 50 DEG C, the rectifying tower 2 tower top temperature is 40 DEG C, collect the front fraction with the reflux ratio of 10, and recycle in the front fraction receiving tank 5 through the condensate in the conde...

Embodiment 3

[0048] Raw material: with embodiment 1

[0049] Rectification device: rectification kettle with 1000ml round bottom flask, glass rectification tower 2 with inner diameter of 25mm, inner packing of 3mm×3mmθ mesh ring, 20 trays.

[0050] Rectification process: 1200g trifluoromethanesulfonic anhydride crude product (its composition is shown in Table 3) is joined in the round-bottomed flask, vacuumizes the rectification system, makes pressure be-0.05MPa, starts heating, and opens the cooling of reflux device 3 The water starts to reflux completely, and the total reflux time is 3 hours, so that the impurity component with a boiling point lower than that of trifluoromethanesulfonic anhydride is enriched at the top of the rectifying tower 2 . Then, when the temperature of the rectifying tank 1 is 55°C and the temperature of the top of the rectifying tower 2 is 50°C, the front fraction is collected with a reflux ratio of 12, and the condensate in the condenser 4 is recycled to the fro...

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Abstract

The invention discloses a purification method of trifluoromethanesulfonic anhydride, and belongs to the field of fine chemicals. The method comprises the following steps: introducing a trifluoromethanesulfonic anhydride crude product into a rectification kettle with a rectification tower, vaccumizing a rectification system, starting to heat the rectification kettle after the vacuum degree is stable, and performing total reflux for 1-5 hours; collecting a front fraction at the reflux ratio of 10-15 when the temperature of the rectification kettle is 50-65 DEG C and the temperature at the tower top of the rectification tower is 40-60 DEG C; collecting a medium fraction at the reflux ratio of 4-6 when the temperature of the rectification kettle is 65-70 DEG C and the temperature at the tower top of the rectification tower is 60-68 DEG C; collecting a back fraction at the reflux ratio of 6-8 when the temperature of the rectification kettle increases by 2 DEG C and the temperature at the tower top of the rectification tower is 66-71 DEG C; stopping the collection of the back fraction, stopping heating, stopping vaccumizing and finishing rectification when the temperature of the rectification kettle is not less than 120 DEG C, wherein the medium fraction is a trifluoromethanesulfonic anhydride fine product. The method has the advantages of simplicity in operation and higher product purity.

Description

technical field [0001] The invention relates to a method for purifying trifluoromethanesulfonic anhydride, which is suitable for the industrial production of trifluoromethanesulfonic anhydride prepared from trifluoromethanesulfonic acid and phosphorus pentoxide, and belongs to the field of fine chemicals. Background technique [0002] Trifluoromethanesulfonic anhydride ((CF 3 SO 2 ) 2 O) is a derivative of trifluoromethanesulfonic acid and has a wide range of uses: it is a commonly used intermediate in the pharmaceutical industry and can be used to synthesize nucleosides, antibiotics, steroids, proteins, vitamins, etc. It can also be used as a catalyst for reactions such as polymerization, esterification, and alkylation, and is widely used in plastics industry, electronic chemical industry, sugar industry and other fields. [0003] Trifluoromethanesulfonic anhydride has a variety of preparation methods: the reaction method of trifluoromethanesulfonic acid and phosphorus p...

Claims

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Application Information

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IPC IPC(8): C07C309/06C07C303/44
Inventor 李翔宇吴飞超杨献奎张净普彭立培沙婷
Owner PERIC SPECIAL GASES CO LTD
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