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Double-end perfluoropolyether and preparation method thereof

A perfluoropolyether, double-ended technology, applied in the field of double-ended perfluoropolyether and its preparation, can solve problems such as high technical difficulty and complex process, and achieve high catalytic activity, high yield, and safe and controllable reaction process. Effect

Pending Publication Date: 2022-04-26
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

U.S. Patents US4451646, US3715378, and US3847978 disclose methods for preparing perfluoropolyethers by photocatalytic oxidative polymerization. These methods are usually free radical reaction mechanisms, and the process involves addition of oxygen to central free radicals, perfluoroperoxy radical chain growth, Perfluoroalkoxy chain growth, perfluoroperoxy radical degradation to produce perfluoroalkoxy radicals, perfluoroperoxy radical coupling chain termination reactions, etc. The process is complex and technically difficult, and continuous improvement and improvement are also required. Optimization for Efficient and Safe Preparation of High Molecular Weight Perfluoropolyethers

Method used

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  • Double-end perfluoropolyether and preparation method thereof
  • Double-end perfluoropolyether and preparation method thereof
  • Double-end perfluoropolyether and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In a 1.25L photocatalytic reactor equipped with mechanical stirring and condenser, add 25.0g (62.5mmol) of N,N-bis(pentafluoropropionyloxyethyl)amine and 1.5g (10.0mmol) of cesium fluoride , 400mL of 1,2,2-trifluoro-1,1,2-trichloroethane, replaced with high-purity nitrogen gas twice, started stirring, and reacted for 12h at room temperature with 50ml / min of active fluorine gas mixture, The reaction pressure is 2bar, then the temperature is raised to 80°C and vigorously stirred for 9h, the temperature of the condenser is controlled at about 30°C, then the temperature of the reaction system is lowered to -30°C, and then 1,2,2-trifluoro-1,1,2 -Trichloroethane 550mL, into the mixed gas of oxygen and carbon dioxide (the flow ratio of oxygen and carbon dioxide is 8:2), turn on the LED ultraviolet lamp with a power of 200W (wavelength 254nm), and then pass into tetrafluoroethylene, 2-Chloro-3,3,3-trifluoropropene, during this period, control the molar ratio of oxygen, tetraflu...

Embodiment 2

[0027]In a 1.8L photocatalytic reactor equipped with mechanical stirring and condenser, add 26.6g (62.5mmol) of N,N-bis(pentafluoropropionyloxypropyl)amine and 1.1g (18mmol) of potassium fluoride, Add 400mL of anhydrous acetonitrile, replace it twice with high-purity nitrogen, start stirring, pass through active nitrogen trifluoride at 30°C at 60ml / min for 10h, reaction pressure 1bar, then raise the temperature to 120°C and stir vigorously for 5h, then reduce the reaction The temperature of the system was brought to -60°C, and then, a mixture of oxygen and carbon dioxide was introduced (the flow ratio of oxygen and carbon dioxide was 7:3), and a high-pressure ultraviolet lamp with a power of 500W was turned on, and then hexafluorobutadiene, 2,3,3,3-tetrafluoropropene. During this period, the molar ratio of oxygen, hexafluorobutadiene and 2,3,3,3-tetrafluoropropene is controlled to be 3.0:0.9:0.1, and the reaction pressure is 2bar. After keeping the UV lamp for 30 hours, turn o...

Embodiment 3

[0030] In a 1.25L photocatalytic reactor equipped with mechanical stirring and a condenser, add 44.2g (0.125mol) of N,N-bis(trifluoroacetoxybutyl)amine and 0.9g (8.5mmol) of rubidium fluoride, After two replacements with high-purity nitrogen, lower the reaction temperature to -20°C, inject 200mL of heptafluoropropane, start stirring, and inject activated carbonyl fluoride mixture gas at 40ml / min for 15h, the reaction pressure is 4bar, then raise the temperature to 100°C and stir vigorously for 6h , the temperature of the condenser is controlled at 30°C, and then the temperature of the reaction system is lowered to -50°C, then, about 850mL of pentafluoroethane is added, and a mixture of oxygen and carbon dioxide is introduced (the flow ratio of oxygen to carbon dioxide is 6:4), and the The LED ultraviolet lamp with a power of 100W (wavelength 308nm) is passed into tetrafluoroethylene, hexafluoropropylene, and trifluoroethylene according to a certain ratio. During this period, th...

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Abstract

The invention discloses double-end perfluoropolyether and a preparation method thereof. The structural formula of the double-end perfluoropolyether disclosed by the invention is shown as a formula (I); the preparation method disclosed by the invention mainly comprises the following steps: in the presence of metal fluoride, fluorinating N, N-bis (perfluoroalkyl acyloxy alkyl) amine or bis (perfluoroalkyl acyloxy alkyl) alkylamine through an active fluorine source to obtain dihydric alcohol amine fluoride; the metal fluoride is selected from potassium fluoride, cesium fluoride, rubidium fluoride or silver fluoride; the active fluorine source is obtained by performing ultraviolet irradiation on a fluorination reagent, and the fluorination reagent is fluorine gas, nitrogen trifluoride or mixed gas of carbonyl fluoride and inert gas; under the irradiation of ultraviolet light, carrying out photooxidation polymerization on a perfluoroolefin monomer, a second fluorine-containing olefin monomer, dihydric alcohol amine fluoride and oxygen to obtain a diacyl-terminated polymer; and then carrying out fluorination treatment on the diacyl-terminated polymer at 50-120 DEG C by adopting an active fluorine source to obtain the double-terminated perfluoropolyether. The preparation method is mainly used for preparing the double-end perfluoropolyether containing nitrogen atoms in a main chain structure.

Description

technical field [0001] The invention belongs to the technical field of perfluoropolyether, and in particular relates to a double-end perfluoropolyether prepared by photooxidative polymerization of perfluoroolefin, fluorine-containing olefin, glycol amine fluoride and oxygen-carbon dioxide mixed gas and a preparation method thereof. Background technique [0002] Perfluoropolyether is a high-molecular compound formed by replacing hydrogen in alkanes with fluorine, oxygen, etc., and contains only three elements of C, F, and O in the molecule. Due to the strong electronegativity and pseudo-pseudo effect of fluorine atoms, and the shielding effect of C-F bonds on the C-C bonds of the main chain, perfluoropolyethers generally have low freezing point, high viscosity index and excellent high temperature resistance, corrosion resistance, radiation resistance and Chemical stability, widely used in electrical and electronic, chemical machinery, aerospace, nuclear industry and other fie...

Claims

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Application Information

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IPC IPC(8): C08G65/00
CPCC08G65/007
Inventor 吕剑马辉石坚涂东怀肖啸谷玉杰白彦波田松贾兆华毛伟
Owner XIAN MODERN CHEM RES INST
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