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A kind of preparation method of perfluoroalkane

A technology of perfluoroalkane and perfluoroalkane, which is applied in the field of preparation of perfluoroalkane, can solve the problems of narrow application range and inability to be used in the synthesis of series of perfluoroalkane, so as to achieve accelerated reaction speed, high yield of target product, The effect of high dissolution rate

Active Publication Date: 2019-05-14
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Limited by raw materials, this method can only obtain perfluoroalkanes with specific chain lengths such as perfluorooctane, perfluorododecane and perfluorohexadecane, which cannot be used to synthesize a series of perfluoroalkanes, and the application range is narrow

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 3.2mol of anhydrous potassium fluoride into a 2L 316L material high-pressure reactor, and feed 1% fluorine-nitrogen mixed gas under stirring at room temperature. The fluorine-nitrogen mixed gas contains 0.096mol fluorine gas, and continue to stir for half an hour; Add 2 mol of perfluorohexyl iodide and 20 mol of anhydrous sulfolane under residual pressure, raise the temperature to 170°C with stirring, react for 7 hours, and finish the reaction, and the reaction product is cooled to room temperature. The reaction product was distilled to obtain 1.91 mol of perfluorohexane with a yield of 95.5%.

Embodiment 2

[0029] Put 3.6mol of anhydrous potassium fluoride into a 2L 316L material high-pressure reactor, and feed 2% fluorine-nitrogen mixed gas under stirring at room temperature. The fluorine-nitrogen mixed gas contains 0.108mol fluorine gas, and continue to stir for half an hour; Add 2 mol of perfluorooctyl iodide and 20 mol of anhydrous sulfolane under residual pressure, heat up to 180°C with stirring, react for 8 hours, and end the reaction. The reaction product is cooled to room temperature. The reaction product was distilled to obtain 1.896 mol of perfluorooctane with a yield of 94.8%.

Embodiment 3

[0031] Put 3.6mol of anhydrous potassium fluoride into a 2L 316L material high-pressure reactor, and feed 5% fluorine-nitrogen mixed gas under stirring at room temperature. The fluorine-nitrogen mixed gas contains 0.108mol fluorine gas, and continue to stir for half an hour; Under residual pressure, 2mol perfluorobutyl bromide and 24mol anhydrous sulfolane were added, the temperature was raised to 160°C under stirring, and the reaction was completed for 6h. The reaction product was cooled to room temperature. The reaction product was distilled to obtain 1.81 mol of perfluorobutane with a yield of 90.5%.

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PUM

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Abstract

The invention discloses a preparation method for perfluoroalkane. The preparation method comprises the following steps: adding a fluorination reagent into a reaction vessel, stirring the fluorination reagent at room temperature, introducing fluorine-nitrogen gas mixture into the reaction vessel for activation of the fluorination reagent and continuing stirring for half an hour, wherein the concentration of fluorine gas in the fluorine-nitrogen gas mixture is 0.5 to 10%, and the molar weight of the fluorine-nitrogen gas mixture is 1 to 5% of the molar weight of the fluorination reagent; after completion of stirring, relieving residual pressure in the reaction vessel, and adding perfluoroalkyl halide and a solvent into the reaction vessel for a reaction at 150 to 200 DEG C for 5 to 10 h, wherein a mol ratio of perfluoroalkyl halide to the fluorination reagent is (1: 1) to (1: 2), and a mol ratio of perfluoroalkyl halide to the solvent is (1: 5) to (1: 15); and after a reaction product is obtained upon completion of the reaction, cooling the reaction product to room temperature and distilling the reaction product to obtain perfluoroalkane. The method provided by the invention has the advantages of simple equipment, high operation security, etc.

Description

technical field [0001] The invention relates to the field of preparation of chemical agents, in particular to a preparation method of perfluoroalkane. Background technique [0002] Perfluoroalkanes are alkane compounds in which hydrogen atoms are completely replaced by fluorine atoms, and are used in refrigerants, solvents, lubricants, insulating materials, etc. It is often used as a solvent for synthetic reactions in industry, and used as a second-generation artificial blood and MRI contrast agent in medicine. At present, the production method of perfluoroalkane is to prepare perfluoroalkane through radical reaction or fluorination reaction using perfluoroalkyl haloalkanes as reactants. The method for preparing perfluoroalkane by free radical reaction has problems such as violent reaction and poor controllability, which reduces production safety; the method for preparing perfluoroalkane by fluorination reaction uses F2, which is prone to explosion and is very dangerous. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/20C07C19/08
CPCC07C17/20C07C19/08
Inventor 耿为利周强吴庆王宗令
Owner JUHUA GROUP TECH CENT