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Perfluoropolyether alcohol preparation method

A technology of perfluoropolyether alcohol and perfluoropolyether ester, which is applied in the preparation of ether, preparation of organic compounds, chemical instruments and methods, etc. problems, to achieve good economic value, avoid product losses, and reduce product losses.

Active Publication Date: 2020-03-03
RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0003] At present, there are generally two methods for the preparation of perfluoropolyether alcohols: one, use LiAlH4 or NaBH4 sub> is used as a reducing agent for reaction, and then acidified post-treatment is adopted. However, due to the existence of hydroxyl groups in the product perfluoropolyether alcohol in this method, the product is easy to form gel in water, resulting in unstable product yield, and acidification treatment is easy to make the whole Fluoropolyether alcohol has yellow or white solid particles, which affect the properties of the product; second, hydrogen catalytic reduction is used, but the method has harsh conditions, high temperature and high pressure, and has certain dangers, and the reaction is likely to be incomplete

Method used

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preparation example Construction

[0030] The invention provides a kind of preparation method of perfluoropolyether alcohol, comprising:

[0031] 1) Reaction: react perfluoropolyether carboxylic acid or perfluoropolyether ester in a solvent in the presence of a reducing agent, and the reaction is completed to obtain a reaction mixture;

[0032] 2) Post-treatment: add water, alkaline solution, water and anhydrous sulfate to the above reaction mixture in sequence, stir, leave to stand for stratification, remove the upper solvent, dilute the lower product with a fluorine-containing solvent, filter, rotary evaporate, and wash , distillation to obtain perfluoropolyether alcohol.

[0033] The reducing agent used in some embodiments of the present invention is LiAlH 4 .

[0034] The structure of perfluoropolyether carboxylic acid or perfluoropolyether ester used in some embodiments of the present invention is shown in formula (I):

[0035]

[0036] Wherein, n=1-30; R is H or C 1-6 alkyl.

[0037] In the presen...

Embodiment 1

[0059] Add 100.2 g of perfluoropolyether methyl ester (weight-average molecular weight 1375, n=7.2) and 100 mL of tetrahydrofuran into a 1 L three-necked flask, install a condenser reflux tube, stir mechanically, and slowly add 3.4 g of LiAlH 4 After 2 hours of reaction, the temperature was raised to 30°C, and the reaction was stopped after 5 hours of continuous reaction, followed by adding 3.4g of water, 3.4g of 15% NaOH solution, 10.1g of water and 16.8g of anhydrous sodium sulfate, mechanically stirring for 30 minutes, and then standing for stratification , remove the upper tetrahydrofuran, the lower white product is diluted with 100mL of methyl nonafluorobutyl ether and filtered, and the filtrate is washed with 50mL of solvent n-hexane / ethyl acetate (the volume ratio of n-hexane and ethyl acetate is 1:3) after rotary evaporation The product was produced three times, and finally the low boiling point solvent was distilled off at 100°C to obtain 93.2 g of colorless and transp...

Embodiment 2

[0061] Add 600.0g of perfluoropolyether methyl ester (weight average molecular weight 2300, n=12.8) and 300mL of tetrahydrofuran into a 2L three-necked flask, install a condensing reflux tube, stir mechanically, and slowly add 11.9g of LiAlH under an ice bath 4 After 2 hours of reaction, the temperature was raised to 30°C, and the reaction was stopped after 7 hours of continuous reaction, followed by adding 11.9g of water, 11.9g of 15% NaOH solution, 35.7g of water and 59.5g of anhydrous magnesium sulfate, mechanically stirred for 30min, and allowed to stand for stratification , remove the upper tetrahydrofuran, the lower white product is diluted with 300mL of trifluorotrichloroethane and then suction filtered. After the filtrate is rotary evaporated, the product is washed three times with 200mL of solvent petroleum ether / tetrahydrofuran (the volume ratio of petroleum ether and tetrahydrofuran is 2:1). Finally, the low-boiling-point solvent was distilled off at 100° C. to obtai...

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Abstract

The invention provides a perfluoropolyether alcohol preparation method, which comprises: 1) reaction: carrying out a reaction on perfluoropolyether carboxylic acid or perfluoropolyether ester in a solvent in the presence of a reducing agent to obtain a reaction mixture; and 2) post-treatment: sequentially adding water, an alkaline solution, water and anhydrous sulfate into the reaction mixture, stirring, carrying out standing layering, removing the upper-layer solvent, diluting the lower-layer product with a fluorine-containing solvent, filtering, carrying out rotary evaporation, washing, anddistilling to obtain the perfluoropolyether alcohol. According to the preparation method of the invention, the problem that perfluoropolyether alcohol generates a gel in water can be effectively avoided, the properties of the product can be improved, and the colorless and transparent perfluoropolyether alcohol is obtained.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of perfluoropolyether alcohol. Background technique [0002] Perfluoropolyether alcohol is a good lubricant and can be used as a lubricant for disks. At the same time, perfluoropolyether alcohol is an important intermediate for the preparation of fluorine-containing polyurethane, fluorine-containing medicine, pesticide, fluorine-containing emulsifier, fluorine-containing coating agent, anti-fingerprint agent, electronic protection agent, etc. [0003] At present, the preparation method of perfluoropolyether alcohol generally has two kinds: one, use LiAlH 4 or NaBH 4 It is used as a reducing agent for reaction, and then acidified post-treatment is adopted. However, due to the existence of hydroxyl groups in the product perfluoropolyether alcohol in this method, the product is easy to form gel in water, resulting in unstable product yield, and the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/13C07C41/26C07C41/38C08G65/00
CPCC07C41/26C07C41/38C08G65/00C07C43/137
Inventor 李义涛曾永昌刘群方侯琴卿杨冠欣
Owner RUYUAN DONGYANG LIGHT FLUORIDE CO LTD
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