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Perfluoroalkyl ethanol preparation method

A technology of perfluoroalkyl alcohol and perfluoroalkyl ethyl ester, which is applied in the field of preparation of perfluoroalkyl alcohol, can solve the problems of low reaction yield, poor safety, and large environmental pollution of chemical reagents, and achieve simple process, The effect of low cost and high yield

Inactive Publication Date: 2014-05-07
JIANGSU LEE & MAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems in the above prior art that the reaction yield is low, the chemical reagents used in the reaction process pollute the environment and the safety is poor, the present invention provides a more economical, safer and more environmentally friendly The preparation method of fluoroalkyl alcohol

Method used

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preparation example Construction

[0017] General formula (I) of the present invention represents the preparation method of perfluoroalkyl alcohol, is characterized in that, it comprises the following steps:

[0018] CF3(CF2)nCH2CH2OH(I), wherein n=an integer between 0-19;

[0019] Step 1, in a pressure-resistant reactor, add a perfluoroalkyl ethyl iodide represented by the general formula (II) and a carboxylate represented by the general formula (III) and an alcohol solvent, stir and heat to generate an esterification reaction And react for 3~48 hours, the reaction solution is cooled to room temperature, filter and remove the iodine salt precipitation that produces, filtrate distillation reclaims alcohol solvent, then underpressure distillation obtains the carboxylic acid perfluoroalkyl ethyl ester represented by general formula (IV); Step 1 The alcohol solvent is one or more of methanol, ethanol, n-propanol, isopropanol, n-butanol, isobutanol, tert-butanol, n-pentanol, isoamyl alcohol, tert-amyl alcohol, and ...

Embodiment 1

[0025] Preparation of perfluorohexyl ethanol: Weigh 54.5 g of potassium isobutyrate, 171 g of perfluorohexyl ethyl iodide, and 1.25 L of isopropanol into a pressure-resistant reactor, raise the temperature to 180° C., and stir for 8 hours. After cooling down to room temperature, the solid potassium iodide was collected by filtration, and the filtrate was distilled under reduced pressure to obtain 142 g of perfluorohexylethyl isobutyrate. Transfer 142 g of perfluorohexylethyl isobutyrate into a reaction flask, add 1.3 L of methanol, 130 ml of water, and 38 g of KOH, and stir the reaction at room temperature for 10 h. The alcohol-water solvent was removed under reduced pressure, and 1 L of water and 1 L of ether were added to the residue, followed by stirring for 10 minutes. The ether layer was separated, the aqueous layer was extracted once with 1 L of ether, and the combined ether layers were dried over anhydrous sodium sulfate. After filtration, the filtrate was distilled to...

Embodiment 2

[0027] Preparation of perfluorooctyl ethanol: Weigh 54.5 g of potassium isobutyrate, 207 g of perfluorooctyl ethyl iodide, and 1.25 L of isopropanol into a pressure-resistant reactor, raise the temperature to 180° C., and stir for 8 hours. After cooling down to room temperature, the solid potassium iodide was collected by filtration, and the filtrate was distilled under reduced pressure to obtain 171 g of perfluorooctylethyl isobutyrate. Transfer 171 g of perfluorooctylethyl isobutyrate into a reaction flask, add 1.3 L of methanol, 130 ml of water, and 38 g of KOH, and stir the reaction at room temperature for 10 h. The alcohol-water solvent was removed under reduced pressure, and 1 L of water and 1 L of ether were added to the residue, followed by stirring for 10 minutes. The ether layer was separated, the aqueous layer was extracted once with 1 L of ether, and the combined ether layers were dried over anhydrous sodium sulfate. After filtration, the filtrate was distilled to...

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Abstract

The invention discloses a perfluoroalkyl ethanol preparation method. The method comprises the following steps: 1, adding perfluoroalkyl ethyl iodide carboxylate and an alcoholic solvent into a pressure-resistant reaction vessel, carrying out stirring heating for an esterification reaction for 3-48h, cooling the above obtained reaction liquid to room temperature, filtering out a generated iodized salt precipitate, distilling the obtained filtrate to recover the alcoholic solvent, and carrying out reduced pressure distillation to obtain perfluoroalkyl ethyl acrylate; and 2, mixing perfluoroalkyl ethyl acrylate, an alkali and an alcohol-water solvent, stirring at room temperature for 3-48h, carrying out reduced pressure distillation to remove the alcohol-water solvent, adding water and ether to the obtained residues, separating the obtained ether layer, extracting the obtained water layer with ether, drying the obtained ether layer mixture by anhydrous sodium sulfate, filtering, distilling the obtained filtrate to recover ether, and carrying out reduced pressure distillation of the residues to obtain highly-pure perfluoroalkyl ethanol. The method is economic, safe and environmentally-friendly.

Description

technical field [0001] The invention relates to a preparation method, in particular to a preparation method of perfluoroalkyl alcohol. Background technique [0002] Perfluoroalkylethanol is a very important chemical raw material, which can be used to prepare surfactants, lubricants, water and oil repellents, fabric finishing agents, etc., and has a wide range of applications in the fields of papermaking, leather, textiles, and medicine. The current industrial method for preparing perfluoroalkylethanol mainly adopts the hydrolysis reaction of perfluoroalkylethyl iodide. European patent EP0024224 reports the reaction of perfluoroalkylethyl iodide and peroxycarboxylic acid, and the formed perfluoroalkylethyl carboxylate is hydrolyzed to obtain perfluoroalkylethanol. U.S. Patent US3246030 and Chinese Patent CN01105626.6 disclose the reaction of perfluoroalkyl ethyl iodide and nitrite, and the formed nitrite is hydrolyzed to obtain perfluoroalkyl alcohol. The reaction conditions...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/38C07C27/02
CPCC07C29/095C07C67/11C07C31/38C07C69/24C07C69/78
Inventor 欧英勇娄春亮鄢明谢文健陈新滋
Owner JIANGSU LEE & MAN CHEM
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