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Synthesis method of low-carbon-chain perfluoroalkyl iodine

A technology for the synthesis of perfluoroalkyl iodides, which is applied in chemical instruments and methods, preparation of halogenated hydrocarbons, organic chemistry, etc., can solve problems such as inability to recycle catalysts, difficulty in controlling telomerization reactions, and accumulation of reaction heat. The effect of good product composition distribution, simple process and high selectivity

Active Publication Date: 2018-01-19
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is the use of intermittent production, cumbersome operation and low efficiency
The disadvantage is that the product discharged from the reactor in liquid state contains a large amount of catalyst, which needs to be separated from liquid and solid, and the catalyst cannot be recycled, and the cost is high. The tubular reactor is easy to cause the accumulation of reaction heat, which makes it difficult to control the telomerization reaction.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Mix pentafluoroethane and iodine vapor and preheat it to 200°C, and then continuously pass it into a stainless steel tube with a diameter of 1cm and a length of 150cm The reaction was carried out while maintaining 300°C in the reactor. The flow molar ratio of fluorine gas in pentafluoroethane, tetrafluoroethylene, iodine vapor, and fluorine-nitrogen mixed gas is 1:8:1.2:0.005, and the residence time is 10s. The mixed gas obtained from the reaction is washed with alkali, dried, and analyzed by gas chromatography. The composition of the product (excluding the raw material pentafluoroethane) is: 75.7% pentafluoroiodoethane, 13.4% perfluorobutyl iodide, and 3.5% perfluorohexyl iodide , perfluorooctyl iodide and long-chain alkyl iodide 1%, diiodide, perfluoroalkane and other components total 6.4%, pentafluoroethane conversion rate 87.3%.

Embodiment 2

[0027] Mix pentafluoroethane and iodine vapor and preheat it to 200°C, then continuously pass it into a stainless steel tube with a diameter of 1cm and a length of 150cm The reaction was carried out while maintaining 350°C in the reactor. The molar ratio of fluorine gas flow in pentafluoroethane, tetrafluoroethylene, iodine vapor, and fluorine-nitrogen mixed gas is 1:10:1.5:0.008, and the residence time is 7s. The mixed gas obtained from the reaction is washed with alkali, dried, and analyzed by gas chromatography. The composition of the product (excluding the raw material pentafluoroethane) is: 71.9% pentafluoroiodoethane, 16.2% perfluorobutyl iodide, and 3.8% perfluorohexyl iodide , perfluorooctyl iodide and long-chain alkyl iodide 1.2%, diiodide, perfluoroalkane and other components total 6.9%, pentafluoroethane conversion rate 89.7%.

Embodiment 3

[0029] Mix pentafluoroethane and iodine vapor and preheat it to 200°C, then continuously pass it into a stainless steel tube with a diameter of 1cm and a length of 150cm The reaction was carried out while maintaining 280°C in the reactor. The molar ratio of fluorine gas flow in pentafluoroethane, tetrafluoroethylene, iodine vapor, and fluorine-nitrogen mixed gas is 1:15:2:0.01, and the residence time is 15s. The mixed gas obtained from the reaction is washed with alkali, dried, and analyzed by gas chromatography. The composition of the product (excluding the raw material pentafluoroethane) is: 75.6% pentafluoroiodoethane, 9.7% perfluorobutyl iodide, and 2.3% perfluorohexyl iodide , perfluorooctyl iodide and long-chain alkyl iodide 0.5%, diiodide, perfluoroalkane and other components total 11.9%, pentafluoroethane conversion rate 84.8%.

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PUM

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Abstract

The invention discloses a synthesis method of low-carbon-chain perfluoroalkyl iodine. The synthesis method includes the steps of: continuously feeding pentafluoroethane, iodine vapor, tetrafluoroethylene and a fluorine / nitrogen gas mixture together into a tubular reactor to perform a reaction to produce a gas mixture; and alkaline-washing, drying and separating the gas mixture to prepare a mixtureof various perfluoroalkyl iodine products. In the method, molar ratio of the pentafluoroethane to the iodine vapor is 1:1-2; the molar ratio of the pentafluoroethane to the tetrafluoroethylene is 1:5-20; the molar ratio of the pentafluoroethane to the fluorine gas in the fluorine / nitrogen gas mixture is 1:0.001-1:0.01. Reaction temperature is 250-380 DEG C and reaction retention time is 1-15 s. The method has simple processes and high efficiency, is safe and controllable, and has good product component distribution.

Description

technical field [0001] The invention relates to the field of perfluoroalkyl iodides, in particular to a method for synthesizing low-carbon chain perfluoroalkyl iodides. Background technique [0002] Perfluoroalkyl iodide can be used in the production of fluorine-containing fine chemicals such as fluorine-containing pharmaceutical intermediates. The fluorine-containing fabric finishing agent prepared with perfluoroalkyl iodide as the basic raw material has water and oil repellent properties unmatched by other types of fabric finishing agents, and is the mainstream of water and oil repellent fabric finishing agents. However, with the implementation of the EU ban, the market has to turn to the development of low-carbon paraffin products. [0003] In the prior art, perfluoroalkyl iodides with 6 to 12 carbon numbers are mainly prepared, usually by telomerization of short carbon chain perfluoroalkyl iodides and tetrafluoroethylene. The telomerization reaction mostly adopts a tan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/10C07C19/16
Inventor 耿为利吴庆王宗令王树华张文革戴宏文张会学
Owner JUHUA GROUP TECH CENT
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