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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 complex process, complicated operation, many three wastes and the like, and achieves the effects of simple process and high operation safety.

Active Publication Date: 2014-01-22
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, heat up to 115°C under stirring, and continuously feed vinylidene fluoride gas into the autoclave for reaction, control the reaction pressure at 0.5MPa, After 93 g of the vinyl fluoride gas, stop feeding the vinylidene fluoride gas until the reaction pressure no longer drops, then finish the reaction. The reaction product is rectified to reclaim unreacted perfluorobutyl iodide, and the sampling gas chromatographic analysis shows that 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, heat up to 105°C under stirring, and continuously feed vinylidene fluoride gas into the autoclave for reaction. After 130 g of vinyl fluoride gas, stop feeding the vinylidene fluoride gas until the reaction pressure no longer drops, and then finish the reaction. The reaction product is rectified to reclaim unreacted perfluorobutyl iodide, and the sampling gas chromatographic analysis shows that 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, heat up to 125°C under stirring, and continuously feed vinylidene fluoride gas into the autoclave for reaction, control the reaction pressure at 0.65MPa, After 167 g of vinyl fluoride gas, stop feeding the vinylidene fluoride gas until the reaction pressure no longer drops, then finish the reaction. The reaction product is rectified to reclaim unreacted perfluorobutyl iodide, and the sampling gas chromatographic analysis shows that 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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PUM

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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 synthesis method of perfluoroalkane iodide, in particular to a synthesis method of 1,1-dihydroperfluoroalkane iodide. Background technique [0002] 1,1-Dihydroperfluoroalkanes are important chemical raw materials used in fluorine-containing surfactants, fluorine-containing fabric finishing agents, fluorine-containing surface treatment agents and other fluorine-containing fine chemicals. Compared with perfluoroalkyl iodide, the iodine on 1,1-dihydroperfluoroalkyl iodide is more active, and various fluorine intermediates such as corresponding alcohols, thiols and sulfuryl chlorides can be prepared, and various fluorine surfaces can be further synthesized. Activators, fluorine surface treatment agents and other fluorine-containing fine chemicals. These fluorine fine chemicals have excellent and unique properties such as low surface tension, high heat resistance stability, high chemical stability, and water and oil repellency, s...

Claims

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Application Information

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Patent Type & Authority Applications(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