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Preparation method for perfluoroisobutyronitrile

A technology of heptafluoroisobutyronitrile and heptafluoroisobutyramide is applied in the field of preparation of heptafluoroisobutyronitrile, can solve the problems of high cost, difficult to store in the system, low yield and the like, and achieves mild reaction conditions and no three wastes Effect

Pending Publication Date: 2020-01-03
GUANGDONG POWER GRID CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In view of this, the application discloses a preparation method of heptafluoroisobutyronitrile, which can effectively solve the technical defects of low yield, high cost and difficulty in storing in the system in the current method for preparing heptafluoroisobutyronitrile

Method used

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  • Preparation method for perfluoroisobutyronitrile
  • Preparation method for perfluoroisobutyronitrile
  • Preparation method for perfluoroisobutyronitrile

Examples

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Embodiment 1

[0037] The embodiment of the present application provides the first preparation method of heptafluoroisobutyronitrile, the specific steps are as follows:

[0038] The autoclave used in the examples of the present application has a volume of 1 L, and the autoclave is equipped with stirring, a thermometer and a heat exchange jacket. Add 0.3 kg of methyl tert-butyl ether, 0.21 kg of p-toluenesulfonyl chloride, and 0.21 kg of heptafluoroisobutyramide into the autoclave, then cool down the autoclave, and add 0.12 kg of triethylamine. Incubate at -30°C for 1 hour; finally analyze the product of the autoclave, the product contains p-toluenesulfonate and the target product heptafluoroisobutyronitrile, and record the p-toluenesulfonate and target product heptafluoroisobutyronitrile Changes in content (deducting the content of other substances). The result is as figure 1 shown.

Embodiment 2

[0040] The embodiment of the present application provides the second preparation method of heptafluoroisobutyronitrile, the specific steps are as follows:

[0041] The autoclave used in the examples of the present application has a volume of 1 L, and the autoclave is equipped with stirring, a thermometer and a heat exchange jacket. Add 0.3 kg of methyl tert-butyl ether, 0.21 kg of p-toluenesulfonyl chloride, and 0.21 kg of heptafluoroisobutyramide into the autoclave, then cool down the autoclave, and add 0.12 kg of triethylamine. Incubate at -20°C for 1 hour; finally analyze the product of the autoclave, the product contains p-toluenesulfonate and the target product heptafluoroisobutyronitrile, and record the p-toluenesulfonate and target product heptafluoroisobutyronitrile Changes in content (deducting the content of other substances). The result is as figure 1 shown.

Embodiment 3

[0043] The embodiment of the present application provides the third preparation method of heptafluoroisobutyronitrile, the specific steps are as follows:

[0044] The autoclave used in the examples of the present application has a volume of 1 L, and the autoclave is equipped with stirring, a thermometer and a heat exchange jacket. Add 0.3 kg of methyl tert-butyl ether, 0.21 kg of p-toluenesulfonyl chloride, and 0.21 kg of heptafluoroisobutyramide into the autoclave, then cool down the autoclave, and add 0.12 kg of triethylamine. Incubate at -10°C for 1 hour; finally analyze the product of the autoclave, the product contains p-toluenesulfonate and the target product heptafluoroisobutyronitrile, and record the p-toluenesulfonate and target product heptafluoroisobutyronitrile Changes in content (deducting the content of other substances). The result is as figure 1 shown.

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Abstract

The present application belongs to the technical field of inorganic chemistry, and particularly relates to a preparation method for perfluoroisobutyronitrile. The method includes the following steps:step 1, in the presence of an organic solvent and an alkaline solution, performing condensation on heptafluoroisobutyramide and p-toluenesulfonyl chloride to obtain heptafluoroisobutyryl p-toluenesulfonate; and step 2, performing a reaction on the heptafluoroisobutyryl p-toluenesulfonate at the temperature of -30 DEG C to 20 DEG C to produce the perfluoroisobutyronitrile and p-toluenesulfonate. The preparation method for the perfluoroisobutyronitrile disclosed by the present application can effectively solve the technical defects that a current method for preparing perfluoroisobutyronitrile has a low yield and high costs, and the generated perfluoroisobutyronitrile is difficult to store in the system.

Description

technical field [0001] The application belongs to the technical field of inorganic chemistry, in particular to a preparation method of heptafluoroisobutyronitrile. Background technique [0002] With the continuous development and innovation of the global energy Internet, gas-insulated enclosed switchgear (GIS) and gas-insulated transmission line (GIL) have been widely used in power grids. SF as the internal insulating medium of GIS and GIL 6 , is considered to be an almost ideal insulating gas because of its excellent insulation and arc extinguishing properties and low liquefaction temperature. However, SF 6 It is a strong greenhouse gas, and its greenhouse potential (GWP) is about CO 2 23500 times of that, the atmospheric lifetime is about 3200a. Therefore, the development of SF 6 Alternative gases become an urgent task. [0003] Heptafluoroisobutyronitrile (C 4 f 7 N) is a potential insulating gas, the gas GWP value is 2400, about SF 6 1 / 10, low toxicity, excellen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/00C07C255/10C07C303/26C07C309/73
CPCC07C253/00C07C303/26C07C309/73C07C255/10
Inventor 李丽唐念周永言张曼君黎晓淀樊小鹏
Owner GUANGDONG POWER GRID CO LTD
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