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Environment-friendly preparation process for synthesizing perfluoroalkyl alcohol by solvent method

A technology for perfluoroalkyl ethanol and perfluoroalkyl ethyl is applied in the field of environmental protection preparation technology for synthesizing perfluoroalkyl ethanol by solvent method, which can solve the problems of difficulty in implementation, high reaction temperature and high equipment requirements, and achieves investment cost Small, simple process, low cost effect

Active Publication Date: 2017-03-15
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above routes all require high equipment, high reaction temperature, and industrialization is difficult to implement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 474g of perfluorohexylethyl iodide, 1422g of mixed solvent (711g of DMF, 711g of DMSO), and 5.4g of water to a 5L glass reaction flask equipped with a condenser tube, a magnetic stirrer, and a thermometer. Start stirring, raise the temperature to 140°C, and react for 10 hours. The gas phase detection still contains 1.8% perfluorohexylethyl iodide, stop the reaction, and rectify to obtain 330.4g of perfluorohexylethyl alcohol product, the yield is 90%, and the purity of gas chromatography is 98.5%. .

Embodiment 2

[0028] Add 474g perfluorohexylethyl iodide (C 6 f 13 CH 2 CH 2 1), mixed solvent 2370g (DMF 1580g, DMSO 790g), water 90g. Start stirring, raise the temperature to 145°C, and react for 15 hours. The gas phase detection still contains 1.8% perfluorohexylethyl iodide, stop the reaction, and rectify to obtain the product of perfluorohexylethyl alcohol. The conversion rate is 98.1%, and the yield is 91.3%. Gas chromatography 98.2% purity.

Embodiment 3

[0030] Add 474g perfluorohexylethyl iodide (C 6 f 13 CH 2 CH 2 1), mixed solvent 2370g (DMF 1896g, DMSO 474g), water 144g. Start the stirring, raise the temperature to 150°C, and react for 15 hours. The gas phase detection still contains 1.8% perfluorohexylethyl iodide, stop the reaction, and rectify to obtain the perfluorohexylethyl alcohol product, the conversion rate is 98.9%, and the yield is 93.0%. Gas chromatography 98.3% purity.

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Abstract

The invention discloses an environment-friendly preparation process for synthesizing perfluoroalkyl alcohol by a solvent method. The environment-friendly preparation process comprises the following steps: adding perfluoroalkyl ethyl iodide, a mixed solvent and water in a stirring reaction kettle, wherein the molar ratio of the water and the perfluoroalkyl ethyl iodide is 4-10:1, and the weight ratio of the mixed solvent and the perfluoroalkyl ethyl iodide is 3-10:1; in the temperature of 140-160 DEG C, reacting for 10-20 hours under the normal pressure backflow state; and washing layering, rectifying, and dehydrating the reaction liquid, and obtaining a product. After the end of the reaction, the gas phase detection analysis is performed to the product, the percent conversion of the perfluoroalkyl ethyl iodide is more than 98%, the selectivity of the perfluoroalkyl alcohol is more than 95%, and the yield of the perfluoroalkyl alcohol is more than 90%. The environment-friendly preparation process has the advantages of small device investment cost, simple process, low cost, safety and environment friendliness.

Description

technical field [0001] The invention relates to an environment-friendly preparation process for synthesizing perfluoroalkyl alcohols by a solvent method, in particular to a method for synthesizing perfluoroalkyl alcohols by hydrolyzing a mixed solvent containing N-type organic polarity and S-type solvents. Background technique [0002] Perfluoroalkylethanol is an important intermediate for the synthesis of perfluoroalkyl surfactants and functional materials. Used in various fields such as textile, military industry, electronics, aerospace, anti-corrosion, chemical industry, etc. An industrialized route proposed by Dupont, the method for industrialized preparation of perfluoroalkyl alcohols, has mild hydrolysis reaction conditions, sulfuric acid ester is a good leaving group, and the hydrolysis reaction is relatively thorough. The yield reported in the patent is about 90%. This process is The current industrial scale-up process route has the disadvantage of producing a large...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/124C07C31/38
CPCC07C29/124C07C31/38
Inventor 雷志刚杨建荣
Owner JUHUA GROUP TECH CENT
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