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Polyaryletherketone containing boric acid ester, azo polyaryletherketone and preparation method thereof

A technology of polyaryletherketone and boric acid ester, which is applied in the field of polymer material preparation, can solve the problems of polymer glass transition temperature drop, and achieve the effect of improving storage stability and good stability

Inactive Publication Date: 2014-03-12
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the grafting method that adopts at present generally is the method for esterification, amidation and Ullman coupling, and these methods all have some shortcomings.
The ester bond and amide bond are easily hydrolyzed under the action of acid or alkali or even water, and the copper catalysis conditions used in Ullmann coupling often cause the degradation of the main chain of polyarylether, which leads to the glass transition temperature of the polymer. decline

Method used

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  • Polyaryletherketone containing boric acid ester, azo polyaryletherketone and preparation method thereof
  • Polyaryletherketone containing boric acid ester, azo polyaryletherketone and preparation method thereof
  • Polyaryletherketone containing boric acid ester, azo polyaryletherketone and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Put 13.6974g of bisphenol A monomer, 13.0920g of 4,4'-difluorobenzophenone monomer and 9.1205g of anhydrous potassium carbonate, 107mL of sulfolane, and 36mL of toluene into a In the three-necked flask of the device, pass nitrogen, start stirring, heat up to 130°C until the azeotropic dehydrating agent refluxes, react for 2 hours, remove the azeotropic dehydrating agent, heat up to 175°C and continue to react for 8 hours; Precipitation in deionized water, crushing, washing and drying to obtain bisphenol A polyaryletherketone polymer.

[0052] The molecular formula is as follows:

[0053]

[0054] Among them, m=15~25.

Embodiment 2

[0056] Firstly, the three-neck flask was baked with a gas lamp under vacuum, then flushed with nitrogen gas after cooling, put in a magnetic stirrer, and added 4.0748g (10mmol) of bisphenol A polyaryletherketone and 2.0316g (8mmol) of bisboronic acid Butyl alcohol ester, then add 0.0806g [IrCl (COD)] 2 and 0.0644g 4,4'-di-tert-butyl-2,2'-bipyridine, vacuumize and fill with high-purity nitrogen, repeat 3 times, inject 50mL tetrahydrofuran to dissolve, seal, react in an oil bath at 80°C for 12 hours; cool After dissolving in chloroform, using chloroform as solvent, filter with thin-layer chromatography silica gel (200-400 mesh), remove tetrahydrofuran by rotary evaporation, wash 5 times with acetone, and dry to obtain light yellow blocky borate-containing bisphenol A type polymer Aryl ether ketone polymer.

[0057] The molecular formula is as follows:

[0058]

[0059] Among them, n=15~25.

Embodiment 3

[0061] Weigh 21.9g (0.1mol) of 4-iodoaniline into a 250ml beaker, add 50mL of water, stir mechanically to form a paste, and add 33.6mL of concentrated hydrochloric acid (12mol / L) drop by drop. After dropping, continue to react for 1.5h and cool to -5°C. Dissolve 6.9 g of sodium nitrite in 50 mL of water, and drop this solution into the above aqueous solution of 4-iodoaniline hydrochloride at -5°C. After filtration, it was added dropwise to 200 mL of aqueous solution containing 16.4 g of sodium acetate and 12.1 g of N,N-dimethylaniline, and the temperature of the solution was controlled at -5°C. After dropping, react at room temperature for 3 to 5 hours. 24 g of aqueous sodium hydroxide solution was added dropwise to the resulting solution for neutralization. After washing with water until neutral, vacuum dry at 60°C in a vacuum oven. Recrystallize with ethanol to obtain 4-iodo-4'-(N,N-dimethylamine)azobenzene monomer in the form of orange powder.

[0062] The molecular for...

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Abstract

The invention discloses polyaryletherketone containing a boric acid ester, azo polyaryletherketone and a preparation method thereof, and belongs to the technical field of preparation of a high polymer material. The method comprises the following steps: firstly, synthetizing bisphenol A polyaryletherketone, and carrying out catalytic boriding reaction under a 1,5-cyclooctadiene chloride iridium dipolymer by using the polyaryletherketone and boron pinacol ester; secondly, synthetizing a 4-iodine-4'-(N,N-dimethyl amine) azobenzene monomer; finally, reacting with the 4-iodine-4'-(N,N-dimethyl amine) azobenzene monomer under catalysis of tetrakispalladium by using a polyaryletherketone material containing the boric acid ester, so as to prepare the azo polyaryletherketone. By adopting the method, an azo monomer can be successfully led to the polyaryletherketone, but the performance of the polyaryletherketone is not affected, biphenyl structure azo polyaryletherketone with stable performance also can be generated, and the storage stability of the azo material can be improved. Therefore, the method is expected to be applied in the aspect of preparation of a novel azo polymer material.

Description

technical field [0001] The invention belongs to the technical field of polymer material preparation, and in particular relates to borate-containing polyaryletherketone materials, azopolyaryletherketone materials prepared therefrom and methods for preparing the two materials. Background technique [0002] Azo polymers exhibit excellent photoresponse behavior due to their photodichroism, photoinduced liquid crystal phase transition, photomechanical effect, nonlinear optical materials, information storage, light-driven molecular switches, and photonic materials. However, it shows great application potential in the fields of reversible optical storage, all-optical switch, integrated optoelectronics and photonic technology. The research and development of azo-based materials, especially the synthesis of new, high-performance photoresponsive polymer materials, and the study of the relationship between structure and performance have always been the focus of researchers. The resear...

Claims

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Application Information

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IPC IPC(8): C08G65/48C08G65/40
Inventor 姜振华王永鹏张海博林英健朱轩伯
Owner JILIN UNIV
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