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Preparation method for perfluoroalkyl iodide

A technology of perfluoroalkyl and iodide, which is applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve the problems of high price of dihalogenated perfluoroalkanes, increase of production cost and danger, and achieve improvement Effects of production safety, improvement of uniformity and stability, and reduction of production cost

Active Publication Date: 2010-07-14
太仓中化环保化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The Chinese invention patent with the patent number ZL200610068952.2 discloses a telomerization method for synthesizing medium-chain-length perfluoroalkyl iodides. The method uses tetrafluoroethylene as the main chain, and R f I is a telogen, with active copper, nickel or their alloy as a catalytic initiator, dihalogenated perfluoroalkane as a chain transfer agent, and the polymerization is regulated at a temperature of 80 to 180 ° C and the autogenous pressure of the system. The method used The chain transfer agent dihalogenated perfluoroalkane is expensive and highly toxic, which increases the production cost and danger. At the same time, in order to achieve better results, the reaction still needs to be carried out at a relatively high temperature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 10g of 300-mesh copper powder and 10g of Span 85 into a 5L vertical stainless steel reactor, seal the reactor and evacuate it. Replace with high-purity nitrogen so that the oxygen content in the kettle is less than 10ppm, and the moisture content is less than 100ppm. The reactor was then evacuated to -0.1MPa, and 5 kg of pentafluoroiodoethane was added into the reactor through an auxiliary pump. Then 45 g of tetrafluoroethylene gas was slowly introduced, stirring was started and the temperature was raised to 120° C., and tetrafluoroethylene was introduced again when the reaction pressure no longer changed. The tetrafluoroethylene addition was repeated until a total of 677 g was added, and the reaction was carried out until the pressure did not drop any more. Condensate and recover unreacted pentafluoroiodoethane. The liquid phase product was analyzed by chromatography after alkali washing and dehydration, and its composition ratio was measured in Table 1.

[0018...

Embodiment 2

[0021] Add 30g of 800-mesh nickel powder and 40g of Span 80 to a 5L vertical stainless steel reactor, seal the reactor and evacuate it. Replace with high-purity nitrogen so that the oxygen content in the kettle is less than 10ppm, and the moisture content is less than 100ppm. The reactor was then evacuated to -0.1MPa, and 5 kg of pentafluoroiodoethane was added into the reactor through an auxiliary pump. Then, 45 g of tetrafluoroethylene gas was slowly introduced, stirring was started and the temperature was raised to 150° C., and tetrafluoroethylene was introduced again when the reaction pressure no longer changed. The addition of tetrafluoroethylene was repeated until a total of 508 g was added, and the reaction was carried out until the pressure did not drop any more. Condensate and recover unreacted pentafluoroiodoethane. The liquid phase product was subjected to alkali washing and dehydration and then chromatographically analyzed. The measured composition ratios are sho...

Embodiment 3

[0025] Add 40g of 1000-mesh copper-zinc powder and 25g of polyvinylpyrrolidone (K-30) into a 5L vertical stainless steel reactor, seal the reactor and evacuate it. Replace with high-purity nitrogen so that the oxygen content in the kettle is less than 10ppm, and the moisture content is less than 100ppm. The reactor was then evacuated to -0.1MPa, and 5 kg of pentafluoroiodoethane was added into the reactor through an auxiliary pump. Then, 45 g of tetrafluoroethylene gas was slowly introduced, stirring was started and the temperature was raised to 110° C., and tetrafluoroethylene was introduced again when the reaction pressure no longer changed. The addition of tetrafluoroethylene was repeated until a total of 1016 g was added, and the reaction was carried out until the pressure did not drop any more. Condensate and recover unreacted pentafluoroiodoethane. The liquid phase product was analyzed by chromatography after alkali washing and dehydration, and the measured composition...

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Abstract

The invention relates to a method for preparing perfluoroalkyl iodide through telomerization reaction. The reaction system of the telomerization reaction comprises tetrafluoroethylene used as telomerization monomer, RfI used as telogen and metal powder used as catalyst, wherein Rf denotes perfluoroalkyl with the carbon number of 1-6 and the structure of a linear chain or branched chains, the molar ratio of the dosed tetrafluoroethylene and RfI is 1:1-6, the used amount of the metal powder is 0.1-5 percent of the mass of the dosed RfI, and nonionic surfactant with weight which is 0.1-10 times of the weight of the metal powder is added in the reaction system of the telomerization reaction. In the perfluoroalkyl iodide product, the proportion of low-polymerization-degree perfluoroalkyl iodide is more than 90 percent, the safety is good and the production cost is low.

Description

technical field [0001] The invention belongs to the field of perfluorinated fine chemical intermediates, in particular to a preparation method of perfluoroalkyl iodides. Background technique [0002] Perfluoroalkyl iodide (general formula: R f (CF 2 CF 2 ) n I, where Rf is a perfluoroalkyl group with 1 to 6 carbons and a straight or branched structure) is a class of monoiodoperfluoroalkane compounds in which hydrogen atoms are completely replaced by fluorine atoms, and is used for the production of fluorine fine chemicals It is widely used in the production of fluorine-containing finishing agents, fluorine-containing surfactants and other fluorine-containing fine chemicals. The ones with industrial application value are mainly perfluoroalkyl iodides with 6 to 12 carbon atoms, among which Perfluorooctyl iodide with 8 carbon atoms has the best performance. [0003] In the prior art, perfluoroalkyl iodides are mainly prepared by telomerization. The so-called telomerizatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C19/16C07C17/278
Inventor 胡开达郭艳红梁成锋张海兵
Owner 太仓中化环保化工有限公司
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