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Phenylacetylene-capped polyether-ether-ketone oligomer and preparation method thereof

A technology of polyetheretherketone and phenylacetylene, applied in the field of polyetheretherketone oligomers, polyetheretherketone oligomers and their preparation, to achieve excellent processing performance, high heat resistance, and excellent heat resistance effects

Inactive Publication Date: 2010-06-30
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is not suitable to achieve cross-linkable functionalization with traditional linear PEEK with large molecular weight

Method used

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  • Phenylacetylene-capped polyether-ether-ketone oligomer and preparation method thereof
  • Phenylacetylene-capped polyether-ether-ketone oligomer and preparation method thereof
  • Phenylacetylene-capped polyether-ether-ketone oligomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1: Specific examples of the preparation of hydroxyl-terminated polyether ether ketone oligomers

[0051] 4,4'-difluorobenzophenone (21.82g, 0.1mol), p-hydroxyanisole (26.07g, 0.21mol), anhydrous potassium carbonate (30.43g, 0.2205mol) and N,N-dimethyl Dimethyl formamide (DMF) (200ml), toluene (60ml) is put into the 1000ml three-necked flask that is equipped with mechanical stirring, nitrogen vent, water device, reflux condenser, toluene is refluxed 2 hours, heats up and evaporates toluene, The reaction temperature was controlled at 145° C., and the reaction was continued for 4 hours. Finally, the material is discharged into an aqueous hydrochloric acid solution, washed with deionized water until the aqueous solution is neutral, and then washed three times with ethanol to obtain the initial oligomer, which is dried for later use. The initial oligomer (10.0g) obtained above, hydroiodic acid (50ml) and acetic acid (200ml) are joined in the 250ml three-neck flas...

Embodiment 2

[0052] Embodiment 2: Specific examples of preparation of polyetheretherketone oligomers terminated by phenylacetylene

[0053] The synthesis method adopted in this example is a two-step method. Wherein the process of the first step is described in embodiment 1; Below is the second step.

[0054] The hydroxyl-terminated polyetheretherketone oligomer (1.99g, 0.005mol) obtained in Example 1, anhydrous potassium carbonate (0.8g, 0.0058mol) and N-methylpyrrolidone (NMP) (20ml), toluene (10ml) is put into the 100ml three-neck flask that mechanical stirring, nitrogen vent, belt water device, reflux condenser are housed, toluene refluxes 2 hours, heats up and evaporates toluene, controls reaction temperature 180~190 ℃, continues reaction 4 Hour. Then add 4-fluoro-4'-phenylethynylbenzophenone (FPEB) (0.0105mol, 3.15g), control the reaction temperature at 160-170°C to continue the reaction for 4 hours, and finally discharge the material into an aqueous hydrochloric acid solution, and ...

Embodiment 3

[0055] Embodiment 3: Specific examples of preparation of polyetheretherketone oligomers terminated by phenylacetylene

[0056] The synthesis method adopted in this example is a one-step method. Put biphenyldiphenol (0.9311g, 0.005mol), potassium carbonate (1.38g, 0.01mol) and N-methylpyrrolidone (NMP) (20ml), toluene (10ml) into a device equipped with mechanical stirring, nitrogen vent, In a 100ml three-necked flask with a water device and a reflux condenser, the toluene was refluxed for 2 hours, the temperature was raised and the toluene was evaporated, the reaction temperature was controlled at 180-190° C., and the reaction was continued for 4 hours. Then add 4-fluoro-4'-phenylethynylbenzophenone (FPEB) (0.0105mol, 3.15g), control the reaction temperature at 160-170°C to continue the reaction for 4 hours, and finally discharge the material into an aqueous hydrochloric acid solution, and use Wash with deionized water until the aqueous solution is neutral, then wash with etha...

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Abstract

The invention relates to phenylacetylene capped polyether ether ketone oligomer and a preparation method thereof, belonging to the technical field of high polymer materials and syntheses thereof. The invention relates to a polyether ether ketone oligomer having higher glass transition temperature, good heat resistance and low viscosity, and the polymerization degree n of the oligomer is 1, 2 or 3. The synthesis of the oligomer can adopt a one-step method or a two-step method. The preparation method of the oligomer comprises the following steps of: adding biluorine and bisphenol monomers to anorganic solvent, after reacting water into salts for 2 to 3 hours and polymerizing for 4 to 5 hours, adding a phenylacetylene end capping agent, and then continuing to reacting for 2 to 4 hours; discharging an obtained capped polyether ether ketone oligomer material to a hydrochloric acid aqueous solution; and cleaning and drying to finally obtain a powdered polyether ether ketone oligomer capable of self crosslinking. The polyether ether ketone oligomer is a polymer having self heat crosslinking property and has the processability of thermoplastic resin and the high heat stability of thermosetting resin.

Description

technical field [0001] The polyetheretherketone oligomer containing phenylacetylene capping and the preparation method thereof of the present invention belong to the field of macromolecular materials and their synthesis. In particular, it relates to a polyetheretherketone oligomer terminated with phenylacetylene, which has a low viscosity in a molten state, has a high glass transition temperature and good heat resistance after crosslinking, and the preparation technology of the oligomer . Background technique [0002] In recent years, high temperature resistant polymer materials are a hot research topic in the polymer field. A class of high-performance thermoplastic resins represented by polyether ether ketone has good mechanical properties and processing properties, and has important application prospects in many fields. But they also have shortcomings, the most representative of which is that linear amorphous polymers do not have high enough thermal stability and solvent...

Claims

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Application Information

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IPC IPC(8): C07C49/84C07C45/64
Inventor 姜振华严巍杨延华
Owner JILIN UNIV
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