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Full-biphenyl polyaryletherketone precursor as well as preparation method and application thereof

A technology of polyaryletherketone and all-biphenyl type, which is applied in the field of all-biphenyl type polyaryletherketone precursor and its preparation, can solve the problems of high melting point and high molecular weight, increase the molecular weight of the polymer, and reduce the energy consumption of polymerization , Reduce the effect of side effects and gel content

Inactive Publication Date: 2021-06-18
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the above technical problems, the present invention provides a method of "amorphous polymerization followed by crystallization transformation", which solves the problem of crystallization of oligomers and successfully prepares high molecular weight, All-biphenyl type PEDEK, PEDEKK and PEDEKDK resins with high melting point

Method used

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  • Full-biphenyl polyaryletherketone precursor as well as preparation method and application thereof
  • Full-biphenyl polyaryletherketone precursor as well as preparation method and application thereof
  • Full-biphenyl polyaryletherketone precursor as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Under the protection of a nitrogen atmosphere, 4248g sulfolane (solid content 10wt%), 1010mL toluene, 207g potassium carbonate, 286g difluoromonomer 1 and 186g biphenyldiphenol were successively added to the polymerization reaction system, the temperature was raised to 140°C, and azeotropic removal Water, reflux for 2 hours, remove toluene in the reaction system by distillation, heat up to 190-210°C for 6 hours, pour the reaction product into anhydrous methanol to wash, grind and dry to obtain the precursor, and then dissolve the precursor in 4320mL In THF, after the precursor is completely dissolved, add 540mL of hydrochloric acid solution with pH=0.1 to the solution, reflux for 24h, then wash with ethanol and water and dry to obtain crystalline all-biphenyl type polyether ether ketone (PEDEK), The intrinsic viscosity of PEDEK is 2.09dL / g, T m It is 416.8°C.

Embodiment 2

[0038] Under the protection of nitrogen atmosphere, 976g diphenyl sulfone (solid content 30wt%), 419mL xylene, 158.8g sodium carbonate, 294g difluoromonomer 2 and 204.6g biphenol were added successively to the polymerization reaction system, and the temperature was raised to 180 °C, azeotropically remove water, reflux for 2 hours, remove xylene in the reaction system by distillation, heat up to 180-210 °C for 2 hours, pour the reaction product into anhydrous methanol to wash, crush and dry to obtain the precursor, and then Dissolve the precursor in 4586ml of chloroform. After the precursor is dissolved, add 179g of dimethyl sulfoxide and 211g of 2-iodo-2-methylpropane in sequence. After reacting at 70°C for 48h, pour the reaction product into an anhydrous in methanol, then washed with anhydrous methanol and dried to obtain crystalline all-biphenyl type polyether ether ketone (PEDEK), the intrinsic viscosity of PEDEK is 2.09dL / g, T m It is 416.8°C.

Embodiment 3

[0040] Under the protection of nitrogen atmosphere, add 4575g sulfolane (solid content 10wt%), 1088mL toluene, 196.7g potassium carbonate, 24.4g cesium carbonate, 322.3g difluoromonomer 3 and 186g biphenyldiphenol successively to the polymerization reaction system, heat up To 140°C, azeotropically remove water, reflux for 2h, remove toluene in the reaction system by distillation, raise the temperature to 190°C-210°C for 6h, pour the reaction product into anhydrous methanol to wash, crush and dry to obtain the precursor , then dissolve the precursor in 4683mL DMF, add 585mL methanesulfonic acid solution with pH=0.1 to the solution after the precursor is completely dissolved, reflux for 24h, wash with ethanol and water, and dry to obtain crystalline full-linked Benzene polyether ether ketone (PEDEK), the intrinsic viscosity of PEDEK is 2.09dL / g, T m It is 416.8°C.

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Abstract

The invention provides a full-biphenyl polyaryletherketone precursor as well as a preparation method and application thereof, which belongs to the technical field of high polymer materials. The full-biphenyl polyaryletherketone precursor is obtained by carrying out polymerization reaction on a difluoro monomer and biphenol which are different from the traditional method at a lower temperature of 170-210 DEG C, and then the full-biphenyl polyaryletherketone precursor is subjected to acidification hydrolysis or a one-step reaction or a two-step reaction process to obtain full-biphenyl polyaryletherketone. Compared with the prior art, the method has the advantages that homogeneous polymerization is carried out at a low reaction temperature, and the obtained polymer is of a full-biphenyl structure, so that the rigidity, regularity and molecular weight of a molecular chain of the polymer are remarkably improved, and the prepared polymer has high Tm which reaches 416 DEG C or above, and the intrinsic viscosity reaches 2.09 dL / g or above.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a precursor of all-biphenyl type polyaryletherketone and its preparation method and application. Background technique [0002] Resin-based composites are widely used in various fields due to their light weight, excellent mechanical properties and designability. With the development of the aviation field, the flight speed of the next generation of fighter jets has been further increased, which puts forward higher requirements for the heat resistance of composite materials. The traditional resin matrix has been difficult to meet the requirements of long-term use at 350°C, short-term use at 400°C or high-temperature corrosion environment. Even polyetheretherketone (PEEK), a special engineering plastic, is gradually difficult to meet the national strategic needs. At the same time, foreign countries have begun to develop composite materials based on polyether ke...

Claims

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Application Information

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IPC IPC(8): C08G65/40
CPCC08G65/4031C08G65/4062C08G65/4081C08G65/4093
Inventor 杨砚超王晟道王贵宾庞金辉王岩张淑玲张梅栾加双
Owner JILIN UNIV
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