Perfluoro nitrile preparation method

A technology of fluoronitrile and perfluoroalkene, which is applied in the field of preparation method of perfluoronitrile, can solve the problems of unavailable raw materials, low yield of heptafluoroisobutyronitrile, high cost, etc., achieves shortened synthetic route, novel synthetic route, The effect of increasing the conversion rate

Active Publication Date: 2018-04-20
泉州宇极新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The above-mentioned prior art has the following problems: first, in the first route, the pyrolysis fragmentation reaction of diazine compounds and nitrogen-containing polycyclic compounds is not complete, so the productive rate of heptafluoroisobutyronitrile is low, and three The pyrolysis and fragmentation reaction of azine compounds is very thorough, and the selectivity and yield of heptafluoroisobutyronitrile are very high, but the raw materials are not easy to obtain and the cost is high; the second route has the defect of low yield of heptafluoroisobutyronitrile; Then there is the serious deficiency that the productive rate of heptafluoroisobutyronitrile and the selectivity are very low in the third route; Productive rate is low, has greatly reduced the total yield of whole route heptafluoroisobutyronitrile, thereby greatly increased the production cost of heptafluoroisobutyronitrile,

Method used

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Experimental program
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Effect test

Embodiment 1

[0051] In a 1-liter, 316-material autoclave, first add 0.5 mol of potassium fluoride and 0.1 mol of 18-crown-6, then evacuate, pass through anhydrous acetonitrile, and then put it under stirring conditions at -100°C , quickly feed 1 mol of hexafluoropropylene and 1 mol of carbonyl fluoride, after the feed is completed, keep the temperature at 15°C, and the reaction time is 10 hours. After the reaction, use a 200mL small steel cylinder made of 316 to collect the gas phase in the reaction system The product heptafluoroisobutyryl fluoride was 207.8 g, the purity was 99.7% (GC analysis), and the yield of heptafluoroisobutyryl fluoride was 95.9%.

Embodiment 2

[0053] In a 1-liter, 316-material autoclave, first add 0.5 mol of sodium fluoride and 0.1 mol of 15-crown-5, then evacuate, pass in anhydrous acetonitrile, and then put it under stirring conditions at -100°C , quickly feed 1 mol of hexafluoropropylene and 1 mol of carbonyl fluoride, after the feed is completed, keep the temperature at 15°C, and the reaction time is 10 hours. After the reaction, use a 200mL small steel cylinder made of 316 to collect the gas phase in the reaction system The product heptafluoroisobutyryl fluoride was 203.5 g, the purity was 98.7% (GC analysis), and the yield of heptafluoroisobutyryl fluoride was 93.0%.

Embodiment 3

[0055] In a 1-liter, 316-material autoclave, after vacuuming, 0.5 mol of heptafluoroisobutyryl fluoride and 1.5 mol of methylamine CH 3 NH 2 , after the feed is completed, keep the temperature at 15 ° C, and the reaction time is 20 hours. After the reaction is over, the valve is opened to release the gas in the reaction system to obtain 105.6 grams of solid heptafluoroisobutyramide, with a melting point of 46-51 °C, the purity is 99.5% (GC analysis), and the yield is 98.7%.

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Abstract

The invention discloses a perfluoro nitrile preparation method. The perfluoro nitrile preparation method comprises the following steps: an addition reaction is performed on perfluoroolefine R1R2C=CR3R4 and carbonyl fluoride to obtain acyl fluoride R1R2(COF)C-CFR3R4(the general formula of R1,R2,R3 and R4 is -CnF(2n+1) group, and n is a nonnegative integer set); b, performing a reaction on acyl fluoride R1R2(COF)C-CFR3R4, acyl fluoride and an alkali metal amide or an amino compound R-NH2(R is Li, Na, K, Rb, Cs or -CmH(2m+1) group, and m is a nonnegative integer set) to obtain amide R1R2(CONH2)C-CFR3R4; and c, performing a dehydration reaction on amide R1R2(CONH2)C-CFR3R4 to obtain perfluoro nitrile R1R2(CN)C-CFR3R4. The perfluoro nitrile preparation method has a short reaction path, can easily obtain perfluoroolefine and carbonyl fluoride, is low in cost and high in overall yield of perfluoro nitrile, and the reaction path is easy to industrialize.

Description

technical field [0001] The present invention relates to a kind of preparation method of perfluoronitrile, particularly relate to a kind of perfluoroalkene as starting raw material, firstly in the presence of alkali metal fluoride and cosolvent generation addition reaction with carbonyl fluoride to obtain acyl fluoride, then in The preparation method comprises the reaction of acyl fluoride with alkali metal amide or amino compound to obtain amide under the condition of no solvent or solvent, and finally the dehydration reaction of amide in the presence of dehydrating agent to obtain perfluoronitrile. Background technique [0002] Up to now, various documents have disclosed four routes for the synthesis of heptafluoroisobutyronitrile. [0003] The first route is the pyrolysis of nitrogen-containing aromatic heterocycles at high temperature or under UV irradiation. The document "Journal of the Chemical Society, Perkin Transactions 1: Organic and Bio-Organic Chemistry (1972-199...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/20C07C255/10C07C231/02C07C233/05
CPCC07C51/58C07C231/02C07C253/20C07C255/10C07C233/05C07C53/50
Inventor 权恒道张呈平贾晓卿
Owner 泉州宇极新材料科技有限公司
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