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Novel octafluorocyclopentene preparation method

A technology of perfluorocyclopentene and hexafluorocyclopentene, which is applied in the field of preparation of perfluorocyclopentene, can solve problems such as unfavorable industrial production, high operating environment requirements, and explosive polymerization, and achieve selectivity High efficiency, simple equipment and low energy consumption

Inactive Publication Date: 2016-03-30
BEIJING YUJI SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using tetrafluoroethylene as a raw material has high requirements on the operating environment and is prone to explosive polymerization, which is not conducive to industrial production

Method used

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  • Novel octafluorocyclopentene preparation method
  • Novel octafluorocyclopentene preparation method
  • Novel octafluorocyclopentene preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 50g of anhydrous potassium fluoride and 100ml of anhydrous DMF in a 500ml three-necked flask, start stirring, and use a peristaltic pump to mix 1,3-dichloro-2,3,4,4,5,5-hexafluorocyclopentene and The mixture of 1,4-dichloro-2,3,3,4,5,5-hexafluorocyclopentene (GC content is respectively 67% and 33%) injects in the there-necked flask with 10ml / h, and the oil bath temperature rises As high as 80°C, the three-necked flask was connected to a rectification device, and the gaseous phase material at the top of the rectification tower was introduced into a cold trap. The temperature of the cold trap was -78°C, and the liquid product was collected.

Embodiment 2

[0039] Add 50g of anhydrous potassium fluoride and 100ml of anhydrous DMSO in a 500ml three-necked flask, start stirring, and use a peristaltic pump to mix 1,3-dichloro-2,3,4,4,5,5-hexafluorocyclopentene and The mixture of 1,4-dichloro-2,3,3,4,5,5-hexafluorocyclopentene (GC content is respectively 67% and 33%) injects in the there-necked flask with 10ml / h, and the oil bath temperature rises As high as 100°C, the three-necked flask was connected to a rectification device, and the gaseous phase material at the top of the rectification tower was introduced into a cold trap. The temperature of the cold trap was -78°C, and the liquid product was collected.

Embodiment 3

[0041]Add 50g of anhydrous potassium fluoride and 100ml of anhydrous DMAc in a 500ml three-necked flask, start stirring, and use a peristaltic pump to mix 1,3-dichloro-2,3,4,4,5,5-hexafluorocyclopentene and The mixture of 1,4-dichloro-2,3,3,4,5,5-hexafluorocyclopentene (GC content is respectively 67% and 33%) injects in the there-necked flask with 10ml / h, and the oil bath temperature rises As high as 110°C, the three-neck flask was connected to a rectification device, and the gaseous phase material at the top of the rectification tower was introduced into a cold trap with a temperature of -78°C. The liquid product was collected, and the composition of organic matter was analyzed by gas chromatography. The results are listed in Table 1.

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PUM

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Abstract

The invention relates to a novel octafluorocyclopentene preparation method. The method comprises steps as follows: fluoro-chloro-cyclopentene is taken as a raw material, anhydrous alkali metal fluoride is taken as a fluorinating reagent, Lewis alkali is taken as a solvent, the components have the fluorinating reaction in a closed stirring type reaction kettle at the temperature of 80-120 DEG C, and octafluorocyclopentene is obtained; the reaction kettle is externally connected with a distillation device, and gas-phase materials at the top of the distillation tower are collected; the fluoro-chloro-cyclopentene is 1,3-dichloro-2,3,4,4,5,5-hexafluorocyclopentene or / and 1,4-dichloro-2,3,3,4,5,5-hexafluorocyclopentene or / and 1,5-dichloro-2,3,4,4,5,5-hexafluorocyclopentene. Octafluorocyclopentene prepared with the method has high sensitivity; the reaction efficiency is high and the octafluorocyclopentene preparation method is suitable for the industrial production.

Description

technical field [0001] The invention relates to a preparation method for perfluorocyclopentene, which belongs to the field of chemical synthesis. Background technique [0002] Perfluorocyclopentene is the basic raw material for the production of fluorine-containing fine chemicals and polymer materials, and perfluorocyclopentene has important economic, environmental and application values. The atmospheric ozone depletion value (ODP) of perfluorocyclopentene is 0, the greenhouse effect value ((GWP100 value) is low (90), non-combustible, environmentally friendly, and excellent etching performance. It is considered to be the most promising electronic etching One of the representative products in gas, it can be widely used in electronics, post and telecommunications, aerospace, light industry, textile, machinery, medical, automobile, precision instrument and other industries. In 2005 patent (EP1498940A2) reported the use of perfluorocyclopentene Used as a composite etching gas c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/20C07C23/08
CPCC07C17/208
Inventor 庆飞要贾晓卿周晓猛权恒道
Owner BEIJING YUJI SCI & TECH