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Method for preparing perfluoropolyether with high molecular weight

A technology of perfluoropolyether and high molecular weight, which is applied in the field of new functional materials containing fluorine, and can solve rare and other problems

Inactive Publication Date: 2014-05-14
SHANGHAI ICAN CHEM S&T
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the preparation technology of perfluoropolyether, there are very few reports on the use of phase transfer flower catalyst system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 10.0g of tetramethylammonium fluoride, 10.0g of rubidium fluoride and 500ml of dry tetrahydrofuran into a 10L reaction kettle, adjust the reaction temperature to 25°C, and stir for 24h; After stabilization, add hexafluoropropylene oxide into the polymerization kettle at a rate of 20g / min, and after adding 6000g, stop adding hexafluoropropylene oxide, and then stir for 12h; then raise the temperature of the reactor to 25°C, stir for 2h, The reaction is over. After tetramethylammonium fluoride, rubidium fluoride and tetrahydrofuran were recovered, the reaction product was post-treated to finally obtain the target product 5865g with a yield of 97.7% and a conversion rate greater than 95%. The average molecular weight of the product through infrared and nuclear magnetic analysis is 5292.

Embodiment 2

[0028] Add 10.0g of tetraethylammonium fluoride, 2.0g of lithium fluoride and 800ml of dry propionitrile into a 10L reaction kettle, adjust the reaction temperature to 35°C, and stir for 24h; then adjust the temperature of the reaction kettle to -60°C, and wait After the temperature stabilized, add hexafluoropropylene oxide into the polymerization kettle at a rate of 15g / min. After adding 6800g, stop the addition of hexafluoropropylene oxide and stir for another 12h; then raise the temperature of the reactor to 20°C and stir for 2h , the reaction ends. After recovering tetraethylammonium fluoride, lithium fluoride and propionitrile, the reaction product was post-treated to finally obtain 6560 g of the target product with a yield of 96.5% and a conversion rate greater than 95%. The average molecular weight of the product through infrared and nuclear magnetic analysis is 5956.

Embodiment 3

[0030] Add 10.0g of tetramethylammonium fluoride, 10.0g of sodium fluoride and 800ml of dry dioxane into a 10L reaction kettle, adjust the reaction temperature to 20°C, stir for 24h; then adjust the temperature of the reaction kettle to -60°C , after the temperature is stabilized, add hexafluoropropylene oxide into the polymerization kettle at a rate of 15g / min, after adding 3400g, stop the addition of hexafluoropropylene oxide, and then stir for 12h; then raise the temperature of the reactor to 40°C, Stirring for 2h, the reaction ended. After recovering tetramethylammonium fluoride, sodium fluoride and dioxane, the reaction product was post-treated to finally obtain 3280 g of the target product with a yield of 96.5% and a conversion rate greater than 95%. The average molecular weight of the product through infrared and nuclear magnetic analysis is 5130.

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PUM

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Abstract

The invention discloses a method for preparing perfluoropolyether with high molecular weight. The method comprises the following steps of: polymerizing in an aprotic solvent by the method for controlling the reaction temperature to control the polymerization degree of hexafluoropropylene oxide under a catalyzing system composed of a phase transfer agent and a water-free alkali metal fluoride; post-processing the obtained polymer to obtain perfluoropolyether with high molecular weight.

Description

technical field [0001] The present invention relates to a new functional material containing fluorine, in particular to a composite catalytic system composed of a phase transfer agent and a metal fluoride, using an aprotic solvent as a solvent and hexafluoropropylene oxide as a raw material, and preparing the whole catalyst through a ring-opening addition reaction. Fluoropolyether method. Background technique [0002] Perfluoropolyether is a special kind of perfluoropolymer compound, and there are only three elements of C, F and O in the molecule. At room temperature, its viscosity increases with the increase of the average molecular weight. It has comprehensive characteristics such as chemical inertness, heat resistance, oxidation resistance, non-combustibility, excellent dielectric properties, and good lubricity. The chemical composition and structure of perfluoropolyether determine that perfluoropolyether has good heat resistance, oxidation resistance, radiation resistan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/24
Inventor 张永明裴素朋刘红阳於水新
Owner SHANGHAI ICAN CHEM S&T
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