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Method of simultaneously preparing perfluoroamyl ether and perfluoroisobutyl ether

A technology of perfluoroisobutyl ether and perfluoropentyl ether, applied in the field of simultaneous preparation of perfluoropentyl ether and perfluoroisobutyl ether, which can solve the problems of separation and purification, many by-products, and large power consumption , to achieve the effect of mild conditions, simple operation and high conversion efficiency

Inactive Publication Date: 2019-05-10
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Methods (2) and (3) are rarely used in actual production due to the high cost of the preparation process and low product yield
Most reports are method (4) using the addition reaction of fluorine-containing alcohols and fluorine-containing olefins to prepare hydrofluoroethers. The produced hydrofluoroethers are either flammable or have a pungent odor, which does not meet the needs of the electronics and other industries. ; and in the process of preparing hydrofluoroethers by the reaction of fluorine-containing alcohols and fluorinated olefins, there will be the production of double bond by-products close to the boiling point of the target product, so the purification process of the final product is increased, and all chlorine or bromine in the purification process High toxicity, strict operation requirements
In method (5), the method of electrofluorination chemistry is usually used to prepare fluorinated acid fluorides, and further to prepare hydrofluoroethers. However, the electrofluorination chemistry method not only consumes a lot of electricity, has low yield and many by-products in the production process, but also The process requires a large amount of anhydrous hydrogen fluoride; and electrofluorine chemistry usually produces a large number of isomers rather than a specific perfluorinated acid fluoride, which are almost impossible to use due to the same or similar boiling points. Separation and purification by rectification technology, the resulting hydrofluoroether product is also a mixture, which cannot be separated by rectification technology

Method used

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  • Method of simultaneously preparing perfluoroamyl ether and perfluoroisobutyl ether
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  • Method of simultaneously preparing perfluoroamyl ether and perfluoroisobutyl ether

Examples

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Effect test

Embodiment 1

[0030] Embodiment 1: the preparation of hexafluoropropylene trimer raw material: hexafluoropropylene gas is passed through the catalytic reaction tube that NaF / Al2O3 catalyst is housed, and the loading capacity of catalyst is 10%, and the temperature of catalyst catalytic reaction tube is 260 ℃, contacts The time is 0.1s; the reacted mixed gas enters the condenser with a cooling jacket from the air inlet, the temperature of the condensed water is 10°C, and the unreacted hexafluoropropylene is circulated to the catalytic reaction tube of the catalyst through the outlet. The purity of the liquid hexafluoropropylene trimer in the condenser was detected to be 99.3%. The yield of hexafluoropropylene trimer is shown in Table 1.

Embodiment 2

[0031]Example 2: Preparation of raw materials for hexafluoropropylene trimer: pass hexafluoropropylene gas through a catalytic reaction tube equipped with an AgF / C catalyst, the loading of the catalyst is 15%, the temperature of the catalytic reaction tube of the catalyst is 300 ° C, contact The time is 10s; the reacted mixed gas enters the condenser with a cooling jacket from the air inlet, the temperature of the condensed water is 10°C, and the unreacted hexafluoropropylene is circulated to the catalytic reaction tube of the catalyst through the outlet. The purity of the liquid hexafluoropropylene trimer in the condenser was detected to be 99.3%. The productive rate of hexafluoropropylene trimer after applying mechanically is shown in Table 1.

Embodiment 3

[0032] Example 3: Preparation of hexafluoropropylene trimer raw material: Hexafluoropropylene gas is passed through a catalytic reaction tube equipped with a KF / C catalyst, the loading of the catalyst is 20%, and the temperature of the catalytic reaction tube of the catalyst is 320°C. The time is 30s; the reacted mixed gas enters the condenser with a cooling jacket through the air inlet, the temperature of the condensed water is 10°C, and the unreacted hexafluoropropylene is circulated to the catalytic reaction tube of the catalyst through the outlet. The purity of the liquid hexafluoropropylene trimer in the condenser was detected to be 99.3%. The productive rate of hexafluoropropylene trimer after applying mechanically is shown in Table 1.

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Abstract

The invention belongs to the field of fluorine chemical engineering and particularly relates to a method of simultaneously preparing perfluoroamyl ether and perfluoroisobutyl ether. The method includes: 1) subjecting hexafluoropropene trimer to cracking reaction with oxygen in an oxidation furnace under catalyst condition so as to prepare perfluoro five-carbon ketone and perfluoro isobutyryl fluoride; 2) adding an alkylation reagent to the perfluoro five-carbon ketone and perfluoro isobutyryl fluoride, and selectively adding tertiary amine or a phase transfer catalyst into an inert dipolar aprotic organic compound solvent under the action of an alkaline metal fluoride, and allowing to react to prepare perfluoroamyl ether and perfluoroisobutyl ether. The hexafluoropropene trimer is used asa raw material herein to generate perfluoro five-carbon ketone and perfluoro isobutyryl fluoride under the action of a catalyst; no separation is required then; a mixture is directly subjected to reaction with the alkylation reagent to generate perfluoroamyl ether and perfluoroisobutyl ether; the conversion efficiency is high; the conditions are mild; the whole process is simple to perform.

Description

technical field [0001] The invention belongs to the field of fluorine chemical industry, and in particular relates to a method for simultaneously preparing perfluoroamyl ether and perfluoroisobutyl ether. Background technique [0002] Hydrofluoroethers (HFEs) are a class of commercially valuable compounds. Hydrofluoroethers have found use as replacements for chlorofluorocarbons (CFCs) in numerous applications. Unlike chlorofluorocarbons, hydrofluoroethers containing fluorine as the only halogen basically do not affect the Earth's ozone layer. The Ozone Depletion Potential (ODP) exhibited by such hydrofluoroethers (HFEs) is therefore considered to be zero. In addition, this hydrofluoroether is more easily degraded in the earth's atmosphere, and its low global warming potential (GWP) and short atmospheric residence time make it an ideal replacement for chlorofluorocarbons (CFCs). [0003] Hydrofluoroethers generally refer to those ethers in which hydrogen atoms are partiall...

Claims

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Application Information

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IPC IPC(8): C07C41/06C07C43/12
Inventor 姚素梅贺光瑞郭海强李希仑
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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