Method for preparing perfluoro-isobutyronitrile and intermediates thereof

A technology of perfluoroisobutyronitrile and perfluoroisobutyramide is applied in the field of preparation of perfluoroisobutyronitrile, which can solve the problems of difficult treatment and industrial application of trifluoroacetic acid pyridinium salt, and achieves reduction of three wastes and reaction operation. Simple, novel raw material route effect

Inactive Publication Date: 2019-05-14
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The trifluoroacetic acid pyridinium salt generated in the dehydration step is difficult to treat as three wastes, and it is difficult for industrial application

Method used

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  • Method for preparing perfluoro-isobutyronitrile and intermediates thereof
  • Method for preparing perfluoro-isobutyronitrile and intermediates thereof
  • Method for preparing perfluoro-isobutyronitrile and intermediates thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1: Preparation of perfluoroisobutyramide

[0048] At 0°C, 80 grams of perfluoroisobutyryl fluoride and 12 grams of ammonia gas were introduced into 200 grams of acetonitrile under stirring from two pipelines. The reaction vessel was a dry 500 ml four-necked flask. During the reaction, keep the internal temperature of the solution not exceeding 25°C. After the gas was passed through, stirring was continued for 2 hours. Dissolve the resulting reaction liquid in water and use Na 2 CO 3 After the treatment is made basic, acetonitrile is removed under reduced pressure. The remaining aqueous phase was extracted with dichloromethane or ethyl acetate, separated, dried, filtered, and evaporated to obtain 67.2 g of perfluoroisobutyramide. The yield was 85%.

Embodiment 2

[0049] Example 2: Preparation of perfluoroisobutyramide

[0050] At -10°C, 50 g of perfluoroisobutyryl fluoride and 7.5 g of ammonia gas were passed into 100 g of acetonitrile under stirring, and the reaction vessel was a dry 250 ml four-necked flask. The rest of the operation is the same as in Example 1, and 36.0 g of perfluoroisobutyramide is obtained. The yield was 73%.

Embodiment 3

[0051] Example 3: Preparation of perfluoroisobutyramide

[0052] At 0°C, 50 g of perfluoroisobutyryl fluoride and 12 g of ammonia gas were passed into 200 g of acetonitrile under stirring, and the reaction vessel was a dry 500 ml four-necked flask. The other operations were the same as in Example 1, and 40.5 g of perfluoroisobutyramide was obtained. The yield was 82%.

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Abstract

The invention discloses a method for preparing perfluoro-isobutyronitrile. The method includes carrying out reaction on perfluoro-isobutyryl fluoride and ammonia solution or ammonia gas in water or organic solvents to generate perfluoro-isobutyramide at first; dehydrating the perfluoro-isobutyramide by dehydrating agents to obtain the perfluoro-isobutyronitrile. The method has the advantages of novel raw materials and routes, simplicity in reaction operation, high product yield and low waste gas, wastewater and industrial residue quantities.

Description

Technical field [0001] The invention relates to a preparation method of fluorine-containing nitrile, in particular to a preparation method of perfluoroisobutyronitrile. Background technique [0002] Sulfur hexafluoride is the main insulating gas in the high-voltage transmission pipeline system due to its good insulation and arc extinguishing performance. Perfluoroisobutyronitrile has a dielectric strength better than or equivalent to sulfur hexafluoride, and a very low GWP (Global Warming Potential, SF 6 It is 23900, and perfluoroisobutyronitrile is 2100), which has become the main potential substitute for sulfur hexafluoride. [0003] For the preparation method of perfluoroisobutyronitrile, there are the following reports in the prior art: [0004] (1) The literature J. Chem. Soc. Perkin Trans 1 1990, 4, 983 reported the use of photochemical methods to synthesize perfluoroisobutyronitrile compounds with fluoro-1,2,3-triazine compounds as raw materials. This method does not disclos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/05C07C231/02C07C255/10C07C253/20
Inventor 张洁明倪航王飞
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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