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Polyarylether with main chain containing bisbenzofiurene and triaryl-s-triazine structure and preparation method of polyarylether

A technology of bisphenyl fluorene and s-triazine, which is applied in the field of polymer material synthesis, can solve problems such as research on synthesis of polyaryl ethers that are not involved, and achieve the effects of improved solubility and excellent solubility

Active Publication Date: 2017-04-26
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, none of the above inventions or work involves the synthesis of polyarylethers containing both triaryl-s-triazine and bisphenylfluorene structures in the main chain

Method used

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  • Polyarylether with main chain containing bisbenzofiurene and triaryl-s-triazine structure and preparation method of polyarylether
  • Polyarylether with main chain containing bisbenzofiurene and triaryl-s-triazine structure and preparation method of polyarylether
  • Polyarylether with main chain containing bisbenzofiurene and triaryl-s-triazine structure and preparation method of polyarylether

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preparation example Construction

[0047] When the polyarylether is prepared by a bisphenol monomer containing bisphenylfluorene and a dihalogen monomer containing triaryl-s-triazine rings, the preparation method includes the following steps in sequence:

[0048] Add the bisphenol monomer containing bisphenylfluorene, alkali catalyst, solvent and dehydrating agent to the reaction kettle with water separator, stirrer, thermometer and nitrogen inlet pipe in sequence, and first raise the temperature to 120℃~150℃ Dehydration for 1-7 hours, distill out the dehydrating agent, cool to room temperature, add equimolar dihalogen monomer containing triaryl-s-triazine ring; then heat up to 100-220°C and react for 1-30 hours, then add precipitant, The polymer is coagulated and precipitated; the copolymer is obtained through suction filtration, separation, washing, drying and other steps; the molar yield is 90-99%.

[0049] The polyaryl ether can also be passed through bisphenol monomers containing bisphenylfluorene, bisphen...

Embodiment 1

[0067] (1) Add 0.1101g of hydroquinone (HQ) and 1.4000g of 9,9-bis(4-hydroxyphenyl)fluorene to a 100mL three-necked flask equipped with mechanical stirring, water separator condenser and nitrogen inlet (BHF), 0.8293g of anhydrous potassium carbonate, 5mL of sulfolane and 20mL of toluene, refluxed at 150°C with water for 3h, distilled off the toluene, and cooled to room temperature.

[0068] (2) Add 1.7267g of 2,4-bis(4-fluorophenyl)-6-phenyl-1,3,5-triazine (BFPT) into the three-necked flask again, and pass N 2 The incoming air was excluded for 20 minutes, the temperature was raised to 190° C. for 7 hours, and the solvent sulfolane was continuously added to obtain the diluted product.

[0069] (3) sink the product after the sulfolane dilution into boiling water containing a small amount of hydrochloric acid and keep stirring to obtain a white strip polymer, the crude product (detected by GPC, which contains about 3% of small molecules, so it is necessary for further purificat...

Embodiment 2

[0078] (1) Add 6.72g of 2,2-bis-(4-hydroxyphenyl)hexafluoropropane (BAF), 7.00g of 9 , 9-bis(4-hydroxyphenyl)fluorene (BHF), 6.40g of anhydrous potassium carbonate, 10mL of N,N-dimethylacetamide and 50mL of toluene, refluxed at 150°C with water for 3h, distilled off the toluene, Cool to room temperature.

[0079] (2) Add 13.80 g of 2,4-bis(4-fluorophenyl)-6-phenyl-1,3,5-triazine (BFPT) into the three-necked flask again, and pass N 2 The air entering was removed for 20 minutes, the temperature was raised to 160°C for 7 hours, and the solvent N,N-dimethylacetamide was continuously added.

[0080] (3) After the reaction is completed, the product diluted with N,N-dimethylacetamide is immersed in boiling water containing a small amount of hydrochloric acid and stirred continuously to obtain a white strip polymer, that is, the crude product.

[0081] (4) Boil the crude product in distilled water until it boils, and keep it for 2 hours, then use a Buchner funnel to suction filter,...

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Abstract

The invention discloses a polyarylether with the main chain containing a bisbenzofiurene and triaryl-s-triazine structure and a preparation method of the polyarylether and belongs to the field of the synthesis of polymer materials. The structure of the polyarylether contains a bisbenzofiurene group and a triaryl-s-triazine group and has a structural formula shown in the formula I. The preparation method includes the steps that a bisbenzofiurene-containing bisphenol monomer, a triaryl-s-triazine-containing bishalogen monomer, a bisbenzofiurene-free bisphenol monomer and a triaryl-s-triazine-free bishalogen monomer as raw materials are subjected to a nucleophilic substitution in the presence of a base catalyst, a solvent and a dehydrating agent to obtain the polyarylether. The polyarylether has better solubility in common organic solvents, at the same time, has a higher glass transition temperature (more than 290 DEG C) and a higher thermal decomposition temperature (the 5% weight loss temperature is more than 500 DEG C), is suitable for use as a high performance structural material, and also can serve as composite matrix resin or a functional membrane material and the like.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis, and specifically relates to a polyarylether having a main chain containing biphenylfluorene and a triaryl-s-triazine structure and a preparation method thereof. Background technique [0002] Polyarylether is a kind of engineering plastic material with excellent comprehensive performance. Its good thermal stability, acid and alkali resistance, radiation resistance and other advantages make it widely used as structural material in aerospace, electronic appliances, nuclear energy industry and civil high-tech field. However, with the continuous improvement of the use temperature and processability requirements of polymer materials in aerospace and other fields, traditional polyarylether materials have been unable to meet such requirements. For example, the traditional bisphenol A polysulfone (PSU) is soluble in commonly used organic solvents, but its use temperature is relatively ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40
CPCC08G65/4037
Inventor 蹇锡高宗立率王锦艳刘程柳承德
Owner DALIAN UNIV OF TECH
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