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Synthesis method of 1,1-dihydroperfluoroalkyl iodide

A technology of perfluoroiodoalkane and a synthesis method, which is applied in the field of synthesis of perfluoroiodoalkane, can solve the problems of poor product composition distribution, complicated operation, complicated process and the like, and achieves good product composition distribution, high operation safety, simple craftsmanship

Active Publication Date: 2015-05-06
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the process is complicated, the amount of additives such as solvents, initiators, and acid absorbers is large, and there are many three wastes. At the same time, the use of a large amount of initiators is likely to cause safety problems
The disadvantages are complicated operation, high content of by-products and poor distribution of product composition

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Put 1000g of perfluorobutyl iodide and 20g of reduced copper powder into a 1L autoclave. The temperature is raised to 115°C under stirring. Vinylidene fluoride gas is continuously introduced into the autoclave for reaction. The reaction pressure is controlled to 0.5MPa, and partial After 93 g of vinyl fluoride gas, the flow of vinylidene fluoride gas was stopped until the reaction pressure no longer dropped, and the reaction was terminated. The reaction product is rectified to recover the unreacted perfluorobutyl iodide, sampled and analyzed by gas chromatography, and the main composition is CF 3 CF 2 CF 2 CF 2 CF 2 CH 2 I content 96.3%, CF 3 CF 2 CF 2 CF 2 CH 2 CF 2 I content 0.5%, CF 3 CF 2 CF 2 CF 2 (CF 2 CH 2 ) 2 The I content is 2.6%, and the target product yield is 97.3%.

Embodiment 2

[0026] Put 1000g of perfluorobutyl iodide and 35g of reduced copper powder into a 1L autoclave. The temperature is raised to 105°C under stirring. Vinylidene fluoride gas is continuously introduced into the autoclave for reaction. The reaction pressure is controlled to 0.8MPa and the After 130 g of vinyl fluoride gas, the flow of vinylidene fluoride gas was stopped until the reaction pressure no longer dropped, and the reaction was terminated. The reaction product is rectified to recover the unreacted perfluorobutyl iodide, sampled and analyzed by gas chromatography, and the main composition is CF 3 CF 2 CF 2 CF 2 CF 2 CH 2 I content 96.2%, CF 3 CF 2 CF 2 CF 2 CH 2 CF 2 I content 0.6%, CF 3 CF 2 CF 2 CF 2 (CF 2 CH 2 ) 2 The I content is 2.9%, and the target product yield is 96.5%.

Embodiment 3

[0028] Put 1000g of perfluorobutyl iodide and 50g of reduced copper powder into a 1L autoclave. The temperature is raised to 125°C under stirring. Vinylidene fluoride gas is continuously introduced into the autoclave for reaction. The reaction pressure is controlled to 0.65MPa and the partial After 167 g of vinyl fluoride gas, the flow of vinylidene fluoride gas was stopped until the reaction pressure no longer dropped, and the reaction was terminated. The reaction product is rectified to recover the unreacted perfluorobutyl iodide, sampled and analyzed by gas chromatography, and the main composition is CF 3 CF 2 CF 2 CF 2 CF 2 CH 2 I content 96.1%, CF 3 CF 2 CF 2 CF 2 CH 2 CF 2 I content 1.7%, CF 3 CF 2 CF 2 CF 2 (CF 2 CH 2 ) 2 The I content is 2.9%, and the target product yield is 96.5%.

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Abstract

The invention discloses a synthesis method of 1,1-dihydroperfluoroalkyl iodide. Perfluoroalkyl iodide reacts with vinylidene fluoride in the presence of a catalyst at the reaction temperature of 85-150 DEG C under the reaction pressure of 0.2-1.6 MPa according to the mass ratio of 1:0.01-0.2 to obtain 1,1-dihydroperfluoroalkyl iodide, wherein the mass ratio of perfluoroalkyl iodide to the catalyst is 1:0.005-0.1. The synthesis method has the advantages of simple process, high safety in operation, good product composition distribution and the like.

Description

Technical field [0001] The invention relates to a method for synthesizing perfluoroalkane iodide, in particular to a method for synthesizing 1,1-dihydroperfluoroalkane iodide. Background technique [0002] The 1,1-dihydroperfluoroalkane iodide series are an important class of chemical raw materials used in fluorinated surfactants, fluorinated fabric finishing agents, fluorinated surface treatment agents and other fluorinated fine chemicals. Compared with perfluoroalkyl iodide, 1,1-dihydroperfluoroalkyl iodide has higher iodine activity, and can prepare various fluorine intermediates such as corresponding alcohols, mercaptans and sulfonyl chlorides, and further synthesize various fluorine surfaces Active agent, fluorine surface treatment agent and other fluorine-containing fine chemicals. These fluorine fine chemicals have excellent and unique properties such as low surface tension, high heat stability, high chemical stability, and water and oil repellency, so they have been wide...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/16C07C17/278
Inventor 耿为利周强王树华兰喜平胡正吕秉达
Owner JUHUA GROUP TECH CENT