A kind of method of synthesizing perfluoroisobutyronitrile

A technology of perfluoroisobutyronitrile and heptafluoroisobutyramide, applied in chemical instruments and methods, preparation of organic compounds, dehydration preparation of carboxylic acid amides, etc., can solve the difficulty of separation and purification of perfluoroisobutyryl fluoride, perfluoro There are no commercial supply of isobutyryl fluoride, complex electrolytic fluorination process and other problems, so as to achieve the effect of easy separation, high product purity and low cost

Active Publication Date: 2021-09-17
昊华气体有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problem of this method is that there is no commercial supply of perfluoroisobutyryl fluoride, and its synthesis requires a special electrolytic fluorination supporting device, the electrolytic fluorination process is complicated, the separation and purification of perfluoroisobutyryl fluoride is difficult, and the yield is low. Difficult to prepare in large quantities

Method used

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  • A kind of method of synthesizing perfluoroisobutyronitrile
  • A kind of method of synthesizing perfluoroisobutyronitrile

Examples

Experimental program
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Embodiment 1

[0022] (1) Preparation of ethyl heptafluoroisobutyrate intermediate Add ethyl chloroformate 50g (460.73mmol), hexafluoropropylene 82.94g (552.88mmol), anhydrous potassium fluoride 58.89g (1.01 mol) and 300 mL of diethylene glycol dimethyl ether were stirred and reacted at 50° C. for 3 h, and the reaction mixture was distilled to obtain 95.80 g of a colorless transparent liquid product. The product purity is 90.5%, and the yield is 80.31%. 1 H NMR (500 MHz, CDCl 3 )δ4.49~4.45(m, 2H), 1.40~1.37(t, 3H); 19 F NMR (471MHz, CDCl 3 )δ -74.94~-74.96 (d, J=9.42Hz, 6F), -182.09~-182.17 (m, 1F).

[0023] (2) Preparation of heptafluoroisobutyramide intermediate Dissolve 100g (413.07mmol) of ethyl heptafluoroisobutyrate in 500mL of methanol, lower the internal temperature of the reaction kettle to -20°C, and slowly pass Add 7.03g (413.07mmol) of ammonia gas. After the feeding was completed, the temperature of the kettle was slowly raised to room temperature. After continuing the react...

Embodiment 2

[0026] (1) Preparation of methyl heptafluoroisobutyrate intermediate Add methyl chloroformate 45.00g (476.21mmol), hexafluoropropylene 142.88g (952.41mmol) and tetrabutylammonium fluoride 243.28 g ( 1.19mol) and anhydrous acetonitrile 500mL, stirred at 120°C for 10h. The resulting reaction mixture was distilled to obtain 83.90 g of a colorless transparent liquid product. The product purity is 91.34%, and the yield is 70.56%. 1 H NMR (500MHz, CDCl 3 )δ4.01(s, 3H); 19 F NMR (471MHz, CDCl 3 ) δ -75.11 ~ -75.13 (d, J=9.42Hz, 6H), -182.29 ~ -182.39 (m, 1H).

[0027] (2) Preparation of Heptafluoroisobutyramide Intermediate Add ethyl heptafluoroisobutyrate (100.00 g, 438.47 mmol) into a 250 mL dry three-necked flask. Slowly add ammonia methanol solution 125.28 mL (7M, 876.94 mmol) dropwise into the system under stirring, and control the system temperature not higher than 20°C during the addition. After the addition was completed, the reaction was continued for 2 hours, and the ...

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Abstract

The invention discloses a method for synthesizing perfluoroisobutyronitrile, which is prepared by using industrial products hexafluoropropylene and chloroformate as raw materials. The reaction route is: chloroformate and hexafluoropropylene under the action of fluoride salt One-pot reaction synthesis of heptafluoroisobutyrate; heptafluoroisobutyrate reacts with ammonia to obtain heptafluoroisobutyramide; heptafluoroisobutyramide is dehydrated with a dehydrating agent and purified by rectification to obtain perfluoroisobutyronitrile ( 2,3,3,3-tetrafluoro-2-trifluoromethylpropionitrile). The raw materials selected in the method are all commercially available, and the main raw materials chloroformate and hexafluoropropylene are low in cost and can be supplied in large quantities; the reaction conditions are mild, and the reaction conversion rate and yield are high; the products of each step are easy to separate, and the product purity is high. High, simple and safe process operation, easy to industrial production.

Description

technical field [0001] The present invention relates to the synthesis method of perfluoroisobutyronitrile. Background technique [0002] Perfluoroisobutyronitrile, namely 2,3,3,3-tetrafluoro-2-trifluoromethylpropionitrile, is a class of perfluoronitrile compounds with a boiling point of -4.7°C. It is a colorless gas at normal temperature and pressure. It has the characteristics of low boiling point, high volatility, excellent electrical insulation properties and good environmental protection performance, and can be used as a gas dielectric material and a dielectric composition for insulators in electrical devices. The greenhouse effect index (GWP) of perfluoroisobutyronitrile is only 2210, which is far lower than that of sulfur hexafluoride (GWP=23500). It can be used to replace the traditional sulfur hexafluoride insulating gas and greatly reduce the problem of atmospheric greenhouse effect. Perfluoroisobutyronitrile has received widespread attention from the global elect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C253/20C07C255/10
CPCC07C67/347C07C231/02C07C253/20C07C255/10C07C233/05C07C69/63
Inventor 宋新巍黄晓磊任章顺牛鹏飞高克利张金彪牛学坤鲍金强吴旭飞张松林
Owner 昊华气体有限公司
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