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Di(biphenyl) structure-containing polyethersulfones with high heat resistance class and preparation method thereof

A technology of biphenyl sulfone and polybiphenyl ether, which is applied in the field of polymer materials and its preparation, can solve the problems of low operating temperature and failure to meet the application requirements of high temperature fields, and achieve the effect of high heat resistance level

Inactive Publication Date: 2016-02-03
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The early varieties are polysulfone (PSU) synthesized from 4,4'-dichlorodiphenyl sulfone and bisphenol A as polymerized monomers, but its use temperature is low, which cannot meet the application requirements of some high-temperature fields

Method used

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  • Di(biphenyl) structure-containing polyethersulfones with high heat resistance class and preparation method thereof
  • Di(biphenyl) structure-containing polyethersulfones with high heat resistance class and preparation method thereof
  • Di(biphenyl) structure-containing polyethersulfones with high heat resistance class and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Synthesis of 4,4'-bis(4-hydroxyphenyl)diphenylsulfone

[0040] In a 1000mL two-neck flask equipped with a magnetic stirrer, a nitrogen vent, and a spherical condenser, add 15 grams of 4,4'-dichlorodiphenylsulfone, 21 grams of 4-methoxyphenylboronic acid, and 33 grams of anhydrous carbonic acid Sodium hydrogen, 2 g tetrakis(triphenylphosphine) palladium, 250 ml deionized water, 400 ml 1,4-dioxane.

[0041]Subsequently, nitrogen gas was passed, stirring was started, and the temperature was slowly raised to 80° C., and stirred at this temperature (80° C.) for 10 hours. At this time, the reaction process was monitored by thin-layer chromatography. After the reaction was complete, it was cooled to room temperature, the stirring was stopped and the material was discharged into deionized water. The product was washed repeatedly with deionized water until the solution was neutral. Rinse with ethanol for 5 times, and purify the crude product by column chromatography...

Embodiment 2

[0042] Embodiment 2: Synthetic polyether bis-biphenyl sulfone (DBP-PES) (I)

[0043] In a 100ml three-necked flask equipped with a thermometer, a nitrogen vent, a condensing trap and a mechanical stirrer, add 4 grams of 4,4'-difluorodiphenylsulfone, 2.5 grams of sodium carbonate, 4,4'-bis( Add 6 grams of 4-hydroxyphenyl)diphenyl sulfone, add 35 milliliters of organic solvent sulfolane and 10 milliliters of toluene, blow nitrogen, stir and heat to 150 ° C, and the salt-forming reaction begins. The water and toluene in the system were azeotropic, and the cooling liquid began to drip from the condenser tube, and the layers were separated in the water separator. The water-carrying time is 3 hours. After the upper layer of toluene turns from turbid to clear and transparent, continue to reflux for 30 minutes to ensure that the salt-forming reaction is complete, and steam the water-carrying agent. Then raise the temperature to 190°C, react for 3 hours, the viscosity of the system ri...

Embodiment 3

[0044] Embodiment 3: Synthesis of polyether bis-biphenyl sulfone (DBP-PES) (II)

[0045] In a 100ml three-necked flask equipped with a thermometer, a nitrogen port, a condensing trap and a mechanical stirrer, add 4 grams of 4,4'-dichlorodiphenylsulfone, 2.5 grams of sodium carbonate, 4,4'-bis( Add 6 grams of 4-hydroxyphenyl)diphenyl sulfone, add 30 milliliters of organic solvent sulfolane and 10 milliliters of toluene, blow nitrogen, stir and heat to 150 ° C, and the salt-forming reaction begins. The water and toluene in the system were azeotropic, and the cooling liquid began to drip from the condenser tube, and the layers were separated in the water separator. The water-carrying time is 3 hours. After the upper layer of toluene turns from turbid to clear and transparent, continue to reflux for 30 minutes to ensure that the salt-forming reaction is complete, and steam the water-carrying agent. Then raise the temperature to 200°C, react for 3.5 hours, the viscosity of the sys...

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Abstract

The invention provides di(biphenyl) structure-containing polyethersulfones with a high heat resistance class and a preparation method thereof, belonging to the technical field of high polymer materials and preparation technology thereof. According to the invention, 4,4'-dichlorodiphenyl sulfone is used as a reaction raw material, and a novel bisphenol monomer 4,4'-bis(4-hydroxyphenyl)diphenyl sulfone containing a di(biphenyl) structure is prepared by using a Suzuki coupling method; and with bisphenol monomer undergoes nucleophilic substitution polycondensation respectively with 4,4'-dichlorodiphenyl sulfone (or 4,4'-difluorodiphenyl sulfone) and bis-(4-chlorodiphenyl sulfone) so as to prepare novel biphenyl polyethersulfones, i.e., di(biphenyl) polyethersulfone (DBP-PES) and di(biphenyl) biphenyl polyethersulfone (DBP-PESDS). Compared with commercially available polyethersulfones, the di(biphenyl) structure-containing polyethersulfones provided by the invention have a higher heat resistance class.

Description

technical field [0001] The invention belongs to the technical field of polymer materials and their preparation, and in particular relates to a class of high heat-resistant polyethersulfone containing a biphenyl structure and a preparation method thereof. Background technique [0002] As a member of special engineering plastics, a class of amorphous thermoplastic polyarylethersulfone (PAES) resin developed in the 1960s is known for its heat resistance, hydrolysis resistance, creep resistance, dimensional stability, and impact resistance. Non-toxic, non-toxic, flame retardant, easy to process and shape and other excellent comprehensive properties, after years of application and development, it is widely used in electronics, machinery, aerospace, food, medical and other fields. [0003] Polyaryl ether sulfone resins are mostly synthesized by nucleophilic polycondensation reactions, using divalent alkali metal alkoxides or phenoxide alkoxy ions as strong affinity reagents to rep...

Claims

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Application Information

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IPC IPC(8): C08G65/40
Inventor 姜振华朱轩伯刘一凡张海博
Owner JILIN UNIV