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Method of preparing perfluoro-3-methyl-2-butanone

A technology of methyl and butanone, which is used in the preparation of carbonyl compounds by condensation, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of difficult preparation of solid-phase catalysts and achieve fast reaction speed. , the reaction conditions are mild, and the effect of improving product yield

Active Publication Date: 2019-05-03
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this method, solid-phase catalysts are difficult to prepare

Method used

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  • Method of preparing perfluoro-3-methyl-2-butanone

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Experimental program
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Effect test

Embodiment 1

[0052] Embodiment 1, the preparation of catalyst Cat1

[0053]In a three-necked flask equipped with a reflux condenser, a constant pressure dropping funnel, and a magnetic stirrer, add 1.2 g of potassium fluoride, 5.3 g of octadecadexadecyl ether, and 18.9 g of diethylene glycol dimethyl ether, and set the temperature at 50 °C, start stirring and heating, and slowly add 2.8 g of perfluoro-4-methyl-2-pentene dropwise. After the addition, continue stirring for 1 hour, stop stirring and cool down to room temperature to obtain liquid phase catalyst Cat1.

Embodiment 2

[0054] Embodiment 2, the preparation of catalyst Cat2

[0055] In a three-necked flask equipped with a reflux condenser, a constant pressure dropping funnel, and a magnetic stirrer, add 1.2 g of potassium fluoride, 5.3 g of octadecadexadecyl ether, and 18.9 g of diethylene glycol dimethyl ether, and set the temperature at 50 °C, start stirring and heating, stir for 1 hour, stop stirring and cool down to room temperature to obtain liquid phase catalyst Cat2.

Embodiment 3

[0056] Embodiment 3, the preparation of catalyst Cat3

[0057] In a three-neck flask equipped with a reflux condenser, a constant pressure dropping funnel, and a magnetic stirrer, respectively add 1.2 g of potassium fluoride and 18.9 g of diethylene glycol dimethyl ether, set the temperature at 50 ° C, start stirring and heating slowly 2.8 g of perfluoro-4-methyl-2-pentene was added dropwise, and the stirring was continued for 1 hour after the addition was completed, then the stirring was stopped and the temperature was lowered to room temperature to obtain a liquid phase catalyst Cat3.

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Abstract

The invention discloses a method of preparing perfluoro-3-methyl-2-butanone through a reaction of hexafluoropropylene and trifluoroacetyl fluoride under effect of a liquid-phase catalyst which includes a main catalyst, a cocatalyst, an additive and an organic solvent, wherein the main catalyst is selected from metal fluorides and / or metal bifluorides; the cocatalyst is selected from C6-C9 perfluoroolefines; the additive is selected from crown ether and / or crown ether-like compound; the organic solvent is selected from polar aprotic solvents. The preparation method can achieve one-step reaction, is high in reaction speed, and is high in product yield.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing ketone, in particular to a preparation method of perfluoro-3-methyl-2-butanone. Background technique [0002] Perfluoro-3-methyl-2-butanone is a perfluorinated ketone compound with an ODP of 0 and a GWP of 1. It is an environmentally friendly compound and has certain applications in the fields of fire extinguishing, smelting and refrigeration. application potential. In addition, perfluoro-3-methyl-2-butanone also has excellent insulating properties, so it also has potential application in the field of insulation. [0003] For the preparation method of perfluoro-3-methyl-2-butanone, there are those prepared by liquid phase reaction in the prior art, and some are prepared by gas-solid phase reaction, and the following reports are arranged: [0004] (1) Document J.Fluorine.Chem., 89, (1998) 5. discloses the preparation method of perfluoro-3-methyl-2-butanone, under the action of hexaet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/45C07C49/167B01J31/26
Inventor 王飞倪航张洁明
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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