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Method for preparing single iodo perfluoro alkane

A technology of perfluoroalkane and iodide, which is applied in the field of preparation of small molecule monoiodoperfluoroalkane, can solve the problems of cumbersome operation, high price and low yield in the reaction process, and achieve reduced production cost, convenient operation, and high yield. rate-enhancing effect

Inactive Publication Date: 2009-06-17
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem solved by the present invention is to provide a preparation method of monoiodoperfluoroalkane, which avoids the disadvantages of expensive and difficult to prepare iodine pentafluoride or iodine chloride, cumbersome operation of the reaction process and low yield

Method used

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  • Method for preparing single iodo perfluoro alkane
  • Method for preparing single iodo perfluoro alkane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Pass high-purity nitrogen into a 500 ml stainless steel autoclave with electromagnetic stirring to remove the oxygen in the autoclave. After testing to confirm that the autoclave is oxygen-free, add 122g (0.48mol) of iodine and 67.5g (0.5mol) of sulfonyl chloride , 0.68 g (0.01 mol) of boron trifluoride, 100 g (5 mol) of anhydrous hydrofluoric acid and 40 g (0.4 mol) of tetrafluoroethylene. Slowly heat under stirring, raise the temperature to 140±2°C within 1 hour, keep the temperature and continue to react for 5 hours, the reaction product is naturally cooled to 50°C, and the released gas phase mixture passes through the absorption tank of 10wt% sodium hydroxide aqueous solution, and then passes through the A dry bottle of calcium chloride-like calcium chloride, then absorbed in a cold well at -78°C to obtain the crude pentafluoroiodoethane, and the crude product was distilled at low temperature to collect fractions with a boiling point of 12-13°C to obtain 94.4g of pen...

Embodiment 2

[0025] Feed high-purity nitrogen into a 500 ml stainless steel autoclave with electromagnetic stirring to remove oxygen in the autoclave. After testing to confirm that the autoclave is oxygen-free, add 127g (0.5mol) of iodine and 67.5g (0.5mol) of sulfonyl chloride , 13.8g (0.05mol) of tantalum pentafluoride, 200g (10mol) of anhydrous hydrofluoric acid and 40g (0.4mol) of tetrafluoroethylene. Slowly heat under stirring, raise the temperature to 180±2°C within 1 hour, keep the temperature and continue to react for 3 hours, the reaction product is naturally cooled to 50°C, the released gas phase mixture passes through the absorption tank of 10wt% sodium hydroxide aqueous solution, and then passes through the A dry bottle of calcium chloride-like calcium chloride, and then absorbed in a cold well at -78°C to obtain a crude pentafluoroiodoethane. The crude product was distilled at low temperature to collect fractions with a boiling point of 12-13°C to obtain 90.5 g of pentafluoroio...

Embodiment 3

[0027] Feed high-purity nitrogen into a 500 ml stainless steel autoclave with electromagnetic stirring to remove oxygen in the autoclave. After testing to confirm that the autoclave is oxygen-free, add 127g (0.5mol) of iodine and 67.5g (0.5mol) of sulfonyl chloride , 33.1 g (0.08 mol) of aluminum triiodide, 200 g (10 mol) of anhydrous hydrofluoric acid and 40 g (0.4 mol) of tetrafluoroethylene. Slowly heat under stirring, raise the temperature to 160±2°C within 1 hour, keep the temperature and continue to react for 7 hours, the reaction product is naturally cooled to 50°C, the released gas phase mixture passes through the absorption tank of 10wt% sodium hydroxide aqueous solution, and then passes through the A dry bottle of calcium chloride-like calcium chloride, then absorbed in a cold well at -78°C to obtain the crude product of pentafluoroiodoethane, and the crude product was distilled at low temperature to collect the fraction with a boiling point of 12-13°C to obtain 91.5g...

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Abstract

The invention discloses a method for preparing single-iodo perfluoro-alkane. The method takes iodine, chlorine / sulfonic acid chloride and an anhydrous hydrofluoric acid as raw materials, and makes the raw materials react with corresponding perfluoro-olefin under the action of a Lewis acid catalyst in an oxygen-free atmosphere, to obtain the target product. The purity of the single-iodo perfluoro-alkane prepared by the method is more than 99 percent, and the yield of the single-iodo perfluoro-alkane reaches 92 percent or more than 92 percent. Compared with the prior art, the method has low price of the raw materials and low preparation cost, is convenient to operate and easy to control, sieves and optimizes different catalytic systems, strictly controls the reaction conditions, and greatlyimproves the yield of the single-iodo perfluoro-alkane.

Description

technical field [0001] The invention relates to a preparation method of monoiodoperfluoroalkane, in particular to a preparation method of non-telomerized small molecule monoiodoperfluoroalkane. Background technique [0002] Organofluorine compounds are widely used in materials, medicine, military and other fields due to their excellent characteristics. Among them, monoiodoperfluoroalkane is a kind of monoiodoperfluoroalkane compound in which hydrogen atoms are completely replaced by fluorine atoms. It is used as a key intermediate of perfluorinated surfactants, fabric finishing agents and certain drugs, and has a very broad market prospect. The most commercially valuable is C 4 -C 12 monoiodoperfluoroalkane. [0003] In the prior art, the preparation method of monoiodoperfluoroalkane is to synthesize small molecule monoiodoperfluoroalkane, such as trifluoroiodomethane, pentafluoroiodoethane and heptafluoroisoiodopropane, etc., and then the small molecule The telomerizatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/16C07C17/04
Inventor 吴梓新高慧敏许家福唐来安
Owner SHANGHAI HUAYI GRP CO
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