Method for preparing perfluoroalkyl ethanol

A technology of perfluoroalkylethanol and perfluoroalkylethyl, which is applied in the field of preparation of perfluoroalkylethanol, can solve the problems of high reaction temperature, high equipment requirements, and difficult industrial implementation, and achieve simple process and reduce production Cost, low cost effect

Inactive Publication Date: 2017-11-07
JUHUA GROUP TECH CENT
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The disadvantage is that it requires high equipment and high reaction temperature, making it difficult to implement industrially
[0008] The above separation process needs to use a large amount of water for multiple washings in the liquid separation process, so a large amount of waste water is generated; the patent US4219681 needs to add low-carbon chain hydrocarbon alcohols in the azeotropic distillation, and finally produces alcohol waste liquid after separation

Method used

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  • Method for preparing perfluoroalkyl ethanol
  • Method for preparing perfluoroalkyl ethanol
  • Method for preparing perfluoroalkyl ethanol

Examples

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Embodiment 1-17

[0027] Add perfluoroalkyl ethyl iodide, mixed solvent and water into the reaction kettle for reaction, and add the mixture obtained from the reaction containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water into the rectification tower for vacuum distillation, Distillate and still bottom liquid are obtained, the distillate is a mixture of perfluoroalkylethanol, by-product olefins and water, and the still bottom liquid is a solvent salt; the obtained distillate is subjected to azeotropic distillation to obtain by-product olefin and water Mixed liquid, and perfluoroalkyl ethanol products; the mixed liquid of by-product olefin and water obtained by azeotropic distillation is statically separated to obtain the crude product of by-product olefin and water, and the crude product of by-product olefin is dried to obtain the by-product Olefin products are produced, and the water obtained by liquid separation can be recovered for the hydrolysis of perfluoroalkylethyl...

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Abstract

The invention discloses a method for preparing perfluoroalkyl ethanol. The method comprises the following steps: enabling perfluoroalkyl ethyl iodide, a mixed solvent and water to react, and separating and purifying the obtained mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water, thereby obtaining the perfluoroalkyl ethanol product, wherein the separation and purification comprise the following steps: (1) adding a mixture containing perfluoroalkyl ethanol, by-product olefins, solvent salt and water into a rectifying tower for performing reduced pressure distillation, controlling the vacuum degree to be -0.91 to -0.96MPa so as to obtain distillate containing perfluoroalkyl ethanol, by-product olefins and water and bottom liquid, performing strong base treatment on the bottom liquid, and filtering to obtain the recycled mixed solvent; and (2) performing azeotropic distillation on the distillate, thereby obtaining the mixed solution of the by-product olefins and water and the product perfluoroalkyl ethanol. The method disclosed by the invention has the advantages of simplicity in process, greening, environment friendliness, convenience, high efficiency and low cost.

Description

technical field [0001] The invention relates to a preparation method of perfluoroalkyl alcohol, which belongs to the technical field of fluorine-containing fine chemicals. Background technique [0002] Perfluoroalkylethanol is an important intermediate for the synthesis of perfluoroalkyl surfactants and functional materials. It is widely used in various fields such as textile, military industry, electronics, aerospace, anticorrosion, chemical industry, etc., and its preparation method is a research hotspot in recent years. [0003] For example, the patent EP0247614B1 discloses a preparation method of perfluoroalkyl diols. First, the perfluoroalkyl diiodide, copper sulfate, acetonitrile, and water are reacted at 160° C. for 12 hours, and then the obtained reactant is mixed with 10% The NaOH solution was reacted at 70° C. for 2 hours to obtain 96% perfluoroalkyl glycol. [0004] Patent US685562 discloses a method of adopting CuO-loaded Si-P-Al catalyst and gas-phase hydrolys...

Claims

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Application Information

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IPC IPC(8): C07C31/38C07C29/124C07C29/80C07C1/26C07C11/02
CPCC07C1/26C07C29/124C07C29/80C07C31/38C07C11/02
Inventor 雷志刚徐登平杨海波裴金东
Owner JUHUA GROUP TECH CENT
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