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Preparation method of high-flame-retardance polyether-ether-ketone oligomer

A technology of polyetheretherketone and oligomers, which is applied in the field of preparation of highly flame-retardant polyetheretherketone oligomers, can solve the problem of reducing the physical properties of polyetheretherketone, failing to ensure the linear distribution of polyetheretherketone molecules, Difficult to process and other problems, to achieve the effect of excellent processability, excellent thermal stability, good processability

Active Publication Date: 2020-11-17
SHANDONG NON METALLIC MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The melting point of the polyaryletherketone resins reported in the literature has been as high as 465 ° C, and the use temperature has been raised to 345 ° C in theory, but it is difficult to process such high melting point materials into practical products. The method of increasing the service temperature of polyaryletherketone materials has reached the limit, so improving the stability at high temperature and having a lower melting point is the ideal polymer material
[0005] The traditional synthesis method of polyether ether ketone is that the linear polyether ether ketone containing 1,4-benzenediol structure needs to be gradually heated during the synthesis process, and the final reaction temperature must exceed 325 ° C, while monomers containing hydroxyl groups need to be heated at this temperature. Decomposition or sublimation may occur under the environment, and the generated polyetheretherketone molecules themselves will also undergo crosslinking, which cannot ensure the linear distribution of polyetheretherketone molecules, thereby reducing the physical properties of polyether ether ketone

Method used

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Embodiment 1

[0052] A preparation method of highly flame-retardant polyetheretherketone oligomer adopts a two-step method, comprising the following steps:

[0053] (1) Specific examples of the preparation of hydroxyl-terminated polyether ether ketone oligomers

[0054] 4,4'-difluorobenzophenone (65.46g, 0.3mol), p-hydroxyanisole (78.21g, 0.63mol), potassium carbonate (91.29g, 0.6615mol) and N,N-dimethyl Formamide (DMF) (400ml), toluene (120ml) is put into the three-necked flask of 2000ml that is equipped with mechanical stirring, nitrogen vent, water device, reflux condenser, toluene refluxes 1.5 hours, heats up and evaporates toluene, control The reaction temperature was 155°C, and the reaction was continued for 1.5 hours. Finally, the material is discharged into an aqueous solution of glacial acetic acid, washed with boiled distilled water until the aqueous solution is neutral, and the initial oligomer is obtained, which is dried for later use. The initial oligomer (30.0g) obtained abo...

Embodiment 2

[0058] A preparation method of highly flame-retardant polyetheretherketone oligomer adopts a one-step method, comprising the following steps:

[0059] Put 1,4-benzenediol (2.7933g, 0.015mol), potassium carbonate (4.14g, 0.03mol) and N,N-dimethylformamide (DMF) (60ml), toluene (30ml) into a In a 100ml three-necked flask with mechanical stirring, a nitrogen vent, a water device, and a reflux condenser, the toluene was refluxed for 2 hours, the temperature was raised to evaporate the toluene, the reaction temperature was controlled at 180-190°C, and the reaction was continued for 4 hours. Then add 4-fluoro-4'-dibromodiphenyl ether base benzophenone (FPEB) (0.0105mol, 3.15g), control the reaction temperature at 160-170°C to continue the reaction for 4 hours, and finally discharge into glacial acetic acid aqueous solution , first washed with distilled water until the aqueous solution was neutral, then washed three times with acetone, and dried to obtain a dibromodiphenyl ether-capp...

Embodiment 3

[0061] The preparation method provided in Example 2 is the same, except that the 1,4-benzenediol in Example 2 is replaced by 3,3'-dimethyl-4,4'-biphenol, the remaining methods and corresponding dosage In exactly the same way, a self-crosslinkable dibromodiphenyl ether-capped polyether ether ketone oligomer can also be obtained, with a yield of more than 90%, a degree of polymerization of n=6, and a resin glass transition temperature of 175.8°C. The thermogravimetric analysis shows that the 5% thermal decomposition temperature of the polymer in nitrogen is 558.5°C.

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Abstract

The invention belongs to the technical field of high polymer materials, and particularly relates to a high-flame-retardancy polyether-ether-ketone oligomer and a preparation method thereof. The methodcomprises the steps that N,N-dimethylformamide or dimethyl sulfoxide serves as a solvent for synthesizing polyether-ether-ketone, a reaction is conducted under specific conditions, dibromo diphenyl ether serves as an end-capping reagent, and the polyether-ether-ketone is obtained after distilled water purification. According to the invention, different from other polyaryletherketones, the polyether-ether-ketone oligomer with high flame retardancy is characterized in that the end group contains a bromine group, so that the polyether-ether-ketone oligomer has higher glass transition temperature, lower melt viscosity and high-temperature thermal stability.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of highly flame-retardant polyether ether ketone oligomers. Background technique [0002] In recent years, flame-retardant polymer materials are a hot research topic in the polymer field. A class of high-performance thermoplastic resin represented by polyether ether ketone has good flame retardancy. Polyetheretherketone can meet the UL94V-0 flame retardancy standard and has important application prospects in many fields. Due to the excellent machinability of polyether ether ketone, it is also often used as a matrix material for composite materials, but there are also shortcomings in using polyether ether ketone as a matrix material, although polyether ether ketone itself can reach UL94 V-0 Flame retardant standard, but the flame retardant performance of composite materials formed after adding other materials will often be reduced by one...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/84C07C45/64
CPCC07C49/84C07C45/64
Inventor 侯倩倩张霞许峰丁文皓张文申赵晓刚荀其宁刘霞冀克俭
Owner SHANDONG NON METALLIC MATERIAL RES INST
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