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Fluorine-containing bisphenol aromatic polyester and preparation method thereof

A technology of aromatic polyester and fluorine-containing aromatics, which is applied in the field of fluorine-containing bisphenol aromatic polyesters and its preparation, can solve the problems of pollution, chemical corrosion resistance, low capacitance, cumbersome steps, etc., and achieve the expansion of application range, The effect of low dielectric constant and easy operation

Inactive Publication Date: 2012-07-04
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] On the other hand, because fluoropolymers have a series of advantages such as aging resistance, chemical corrosion resistance, low capacitance, low flammability, and low refractive index, they have become one of the hotspots of extensive research in various countries. Fluorine compounds and polymers, but there are not many reports on fluorine-containing polyarylates. The domestic patent 200880115258.9 is prepared by emulsion polymerization and using perfluoroester sulfinate as a dispersant. The fluorine-containing polymer contains tetrafluoroethylene polymerized units. , but the prepared fluorine-containing polyesters do not perform well in terms of thermodynamic properties
Domestic patent 200780030813.3 reports the preparation of aliphatic fluoropolymers, which are prepared by polymerization of at least one fluorinated monomer in a reaction medium containing water and a selected low-key polyhydrofluoroether (HFE), and the steps are cumbersome And the prepared fluoropolymer does not guarantee a higher molecular weight
In the fluorine-containing polyester prepared by domestic patent 200510075827.X, although fluorine-containing aromatic monomers are used, the main chain of the polyester contains aliphatic ether structural units and does not contain fluorine, which is not a true fluorine-containing aromatic polyester , and most of the above methods use liquid phase polymerization, solvent recycling is difficult, easy to cause pollution, and is not conducive to large-scale industrial production

Method used

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  • Fluorine-containing bisphenol aromatic polyester and preparation method thereof
  • Fluorine-containing bisphenol aromatic polyester and preparation method thereof
  • Fluorine-containing bisphenol aromatic polyester and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Add hexafluorobisphenol A and acetic anhydride in a three-port reactor at a molar ratio of 1:2, add dropwise the catalyst concentrated sulfuric acid, the amount of which is 0.1% of the total mass of hexafluorobisphenol A and acetic anhydride, reflux and stir for 0.5h, and The reacted solution was poured into ice water, and after the precipitate was precipitated, the mixture of the precipitate and ice water was suction-filtered, and the obtained solid was washed with deionized water until neutral, and dried in a vacuum oven at 60°C for 24 hours to obtain 2,2 - bis(4-acetoxyphenyl)hexafluoropropane.

[0048] Add 2,2-bis(4-acetoxyphenyl)hexafluoropropane, terephthalic acid and isophthalic acid in a molar ratio of 1:0.9:0.1 into the polymerization kettle, and add the initiator zinc acetate in an amount of 0.1% of the total mass of the reactants, stirred and filled with nitrogen, heated to 250 ° C, after 3 hours of reaction, stopped filling nitrogen, vacuumed, the vacuum deg...

Embodiment 2

[0050]Add bis(4-hydroxyphenyl)difluoromethane and acetyl chloride into the three-port reactor at a molar ratio of 1:2.1, and add the catalyst p-toluenesulfonic acid in an amount of bis(4-hydroxyphenyl)difluoromethane and 0.5% of the total mass of acetyl chloride, reflux and stir for 2 hours, pour the reacted solution into ice water, and after the precipitation, filter the mixture of precipitation and ice water, and wash the obtained solid with deionized water until neutral , and dried in a vacuum oven at 60°C for 24 hours to obtain bis(4-acetoxyphenyl)difluoromethane.

[0051] Add bis(4-acetoxyphenyl)difluoromethane, terephthalic acid and isophthalic acid in a molar ratio of 1:0.8:0.2 into the polymerization kettle, add the initiator zinc acetate, and the dosage is the total mass of the reactants 0.2%, stir and fill with nitrogen, heat up to 260°C, after 3 hours of reaction, stop nitrogen filling, vacuumize, the vacuum degree is 25KPa, heat up to 310°C and react for 1 hour, re...

Embodiment 3

[0053] Add 2,2-bis(4-hydroxyphenyl)-1,1,1-trifluoroethane and acetyl chloride into the three-port reactor at a molar ratio of 1:2.1, and add the catalyst p-toluenesulfonic acid, the dosage 1% of the total mass of 2,2-bis(4-hydroxyphenyl)-1,1,1-trifluoroethane and acetyl chloride, stirred at reflux for 1 hour, poured the reacted solution into ice water, and waited for precipitation Finally, the mixture of the precipitate and ice water was suction filtered, the obtained solid was washed with deionized water until neutral, and dried in a vacuum oven at 60°C for 24 hours to obtain 2,2-bis(4-acetoxyphenyl)- 1,1,1-Trifluoroethane.

[0054] Add 2,2-bis(4-acetoxyphenyl)-1,1,1-trifluoroethane and terephthalic acid in a molar ratio of 1.1:1 into the polymerization kettle, and add the initiator zinc acetate, the dosage 0.5% of the total mass of the reactants, stirred and filled with nitrogen, heated up to 260°C, after 3.5 hours of reaction, stopped filling nitrogen, vacuumed, the vacuum...

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Abstract

The invention relates to fluorine-containing bisphenol aromatic polyester and a preparation method thereof. The fluorine-containing bisphenol aromatic polyester comprises a fluorine-containing aromatic bisphenol structural unit and an aromatic dibenzoyl structural unit, and is prepared via fusion and polycondensation of a fluorine-containing aromatic bisphenol compound and an aromatic phthalate acid compound. The aromatic polyester is suitable for large-scale industrial production. Moreover, the prepared aromatic polyester contains fluorine, and the intrinsic viscosity [Eta]is 0.5-7dl / g. In addition to the advantages of ordinary polyarylate, the aromatic polyester also has excellent heat resistance, aging resistance, a low dielectric constant, low capacitance and other electrical properties. The scope of application of the traditional polyarylate is expanded.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a fluorine-containing bisphenol aromatic polyester and a preparation method thereof, in particular to a fluorine-containing bisphenol-type polyester containing a fluorine-containing bisphenol structural unit and an aromatic diformyl structural unit Aromatic polyesters and methods for their preparation. Background technique [0002] Japan's Unitika (Unitika) took the lead in synthesizing a polyarylate (its trade name is U-Polymer basic grade U-100) by mixing diformic acid and bisphenol A. Due to its excellent heat resistance, high strength, high modulus, UV resistance, creep resistance and many other advantages, more and more people have carried out research on it, by studying its structure at the molecular level Modification to improve its processability and endow better performance to meet people's demand for functional materials. Domestic patents 200510060698.7 and 200610022133...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/682C08G63/78
Inventor 钦维民魏朋陈玉伟王心航王燕萍倪建华曹路王依民
Owner DONGHUA UNIV