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Method for preparing perfluoro alkyl ethylene

A technology of perfluoroalkylethylene and perfluoroalkylethyl, which is applied in the field of preparation of perfluoroalkylethylene, can solve the problems of increased manufacturing cost, cumbersome post-processing, solvent loss, etc., and achieves high purity and simple preparation method , the effect of rapid response

Inactive Publication Date: 2009-10-28
山东中氟化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem is that the presence of excess inorganic base will make the post-treatment cumbersome; solution washing will cause a large amount of solvent loss, which will increase the manufacturing cost and bring harm to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 800g (1.39mol) of perfluorooctylethyl iodide, 215g of methanol solution with a mass fraction of 28% sodium methoxide, wherein the mass of sodium methoxide is 60.2g (1.115mol) and 8g (0.44mol) of water are added with a thermometer , Condenser tube, in a mechanically stirred 1L four-neck flask, start stirring, heat up, and reflux the solution for 18h. Then connect a 1.2m rectification column, after methanol is distilled off at normal pressure, use an oil pump to draw negative pressure on the system, adjust the vacuum degree to 120mmHg, and collect fractions with a top temperature of 85-89°C. After the residue of the kettle was suction filtered, the filtrate (excessive perfluorooctylethyl iodide) was recovered.

[0021] 380 g of perfluorooctylethylene was obtained, the purity detected by gas chromatography was 98.5%, and the yield was 76.41%.

Embodiment 2

[0023] With 800g (1.39mol) perfluorooctylethyl iodide, 75g mass fraction is the methanol solution of 10% sodium methylate, wherein the quality of sodium methylate is 7.5g (0.139mol) and 2.16g (0.12mol) water is added with Thermometer, condenser, in a mechanically stirred 1L four-neck flask, start stirring, raise the temperature, and reflux the solution for 12 hours. Then connect a 1.2m rectification column, after methanol is distilled off at normal pressure, use an oil pump to draw negative pressure on the system, adjust the vacuum degree to 120mmHg, and collect fractions with a top temperature of 85-89°C. After the residue of the kettle was suction filtered, the filtrate (excessive perfluorooctylethyl iodide) was recovered.

[0024] 50.5 g of perfluorooctylethylene was obtained, the purity detected by gas chromatography was 98.5%, and the yield was 81.5%.

Embodiment 3

[0026] With 800g (1.39mol) perfluorooctylethyl iodide, 291.9g mass fraction is the ethanol solution of 20% potassium ethylate, wherein the quality of potassium ethylate is 58.38g (0.695mol) and 4g (0.22mol) water is added with Thermometer, condenser, in a mechanically stirred 1L four-neck flask, start stirring, raise the temperature, and reflux the solution for 18 hours. Then connect a 1.2m rectification column, after methanol is distilled off at normal pressure, use an oil pump to draw negative pressure on the system, adjust the vacuum degree to 120mmHg, and collect fractions with a top temperature of 85-89°C. After the residue of the kettle was suction filtered, the filtrate (excessive perfluorooctylethyl iodide) was recovered.

[0027] 268.0 g of perfluorooctylethylene was obtained, the purity detected by gas chromatography was 98.27%, and the yield was 86.45%.

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Abstract

The invention relates to a method for preparing perfluoro alkyl ethylene. The method comprises the following steps that: in a container provided with a mechanical stirrer, a condenser and a heating system, a solution of organic alkali and perfluoro alkyl ethyl iodide which is more than stoichiometric amount are mixed; the mixing solution is catalyzed by adding a catalyst and then subjected to heating backflow to generate the perfluoro alkyl ethylene; and the solvent and the perfluoro alkyl ethylene with higher purity are separated in modes of normal pressure rectification and pressure reduction rectification respectively. The method has the advantages that: the preparation method is simple, and the reaction is quick; the obtained product is easily separated and high in purity; the solvent can be recycled; and the use equipment is simple, so that the costs on energy and equipment investment are saved.

Description

technical field [0001] The invention relates to a preparation method of perfluoroalkylethylene. Background technique [0002] At present, the commonly used method for preparing perfluoroalkylethylene is to react perfluoroalkylethyl iodide with an excessive amount of alcohol solution of inorganic base, under mechanical stirring, reflux for a certain period of time, filter to remove solid salt after the reaction, and wash the solution with water to obtain Perfluoroalkylethylene. [0003] In this method, an excess of inorganic base is used to neutralize hydrogen iodide generated in the elimination reaction of perfluoroalkylethyl iodide, and neutralization will generate equimolar water at the same time. The existing problem is that the existence of excessive inorganic base will make the post-treatment cumbersome; solution washing will cause a large amount of solvent loss, which will increase the manufacturing cost and bring harm to the environment. Contents of the invention ...

Claims

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Application Information

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IPC IPC(8): C07C21/18C07C17/25
Inventor 肖玉岭张立亭毛震
Owner 山东中氟化工科技有限公司
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