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Preparation method of low-molecular-weight polyether-ether-ketone

A technology of low molecular weight polyether and ether ketone, which is applied in the field of preparation of low molecular weight polyetheretherketone, can solve the problems of difficult preparation and purification of low molecular weight polyetheretherketone, achieve easy operation, simple and controllable operation, and save solvent Effect

Active Publication Date: 2020-04-10
SHANDONG NON METALLIC MATERIAL RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult to prepare low-molecular-weight polyetheretherketone (4000≤MW≤40000) by this method, because the preparation and purification of low-molecular-weight polyetheretherketone have always been difficult, and the existing technology is difficult to solve this problem, which also restricts domestic liquid crystal displays. A material technology factor towards the high end

Method used

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  • Preparation method of low-molecular-weight polyether-ether-ketone
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  • Preparation method of low-molecular-weight polyether-ether-ketone

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Experimental program
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Embodiment 1

[0028] A preparation method of low molecular weight polyether ether ketone, comprising the following steps:

[0029] First, feed high-purity argon into the reactor equipped with a stirrer and a thermometer, then add 510.6 g of hexanamide to the reactor, and heat the reactor to 40°C±5 while continuously feeding high-purity argon. ℃, start the stirrer to 75rpm after the hexanamide is completely melted, then add 218.2g of 4,4'-difluorobenzophenone and 110.1g of 1,4-benzenediol to the reactor, and continue heating to 120 ℃, then adjust the stirrer to 115rpm, add 127.2g sodium carbonate, increase the stirring speed to 140rpm and heat up to 160°C, keep the temperature for 1h, continue heating to 240°C, keep the temperature for 1h, adjust the stirring speed to 95rpm, add 14.4g of 1- After naphthol was maintained at 240°C for 10 minutes, the material in the reactor was poured into cold water to obtain a white to off-white massive solid.

[0030] After crushing the massive solid into ...

Embodiment 2

[0032] First, feed high-purity argon into the reactor equipped with a stirrer and a thermometer, then add 510.6 g of hexanamide to the reactor, and heat the reactor to 40°C±5 while continuously feeding high-purity argon. ℃, start the stirrer to 75rpm after the hexanamide is completely melted, then add 218.2g of 4,4'-difluorobenzophenone and 110.1g of 1,4-benzenediol to the reactor, and continue heating to 120 ℃, then adjust the stirrer to 115rpm, add 165.9g potassium carbonate, increase the stirring speed to 140rpm and heat up to 160°C, keep the temperature for 1h, continue heating to 240°C, keep the temperature for 1h, adjust the stirring speed to 95rpm, add 14.4g of 1 -Naphthol, after maintaining 240° C. for 10 minutes, pour the material in the reactor into cold water to obtain a white to off-white massive solid.

[0033] After crushing the massive solid into granules with a pulverizer, put them into a fat extractor, add 400mL of ether to the fat extractor, extract with ethe...

Embodiment 3

[0035]First, feed high-purity argon into the reactor equipped with a stirrer and a thermometer, then add 510.6 g of hexanamide to the reactor, and heat the reactor to 40°C±5 while continuously feeding high-purity argon. ℃, start the stirrer to 75rpm after the hexanamide is completely melted, then add 218.2g of 4,4'-difluorobenzophenone and 110.1g of 1,4-benzenediol to the reactor, and continue heating to 120 ℃, then adjust the stirrer to 115rpm, add 127.2g sodium carbonate, increase the stirring speed to 140rpm and heat up to 160°C, keep the temperature for 1h, continue heating to 240°C, keep the temperature for 1h, adjust the stirring speed to 95rpm, add 14.4g of 2- After naphthol was maintained at 240°C for 10 minutes, the material in the reactor was poured into cold water to obtain a white to off-white massive solid.

[0036] After crushing the massive solid into granules with a pulverizer, put them into a fat extractor, add 400mL of ether to the fat extractor, extract with...

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Abstract

The invention belongs to the technical field of high polymer materials, and particularly relates to a preparation method of low-molecular-weight polyether-ether-ketone. According to the method, a traditional solvent diphenyl sulfone is replaced by caproamide; 1-naphthol or 2-naphthol is used as an end-capping reagent, the prepared polyether-ether-ketone has short molecular chain length, namely lowmolecular weight, the weight-average molecular weight of the polyether-ether-ketone can reach 4000-10000, the blank in the field is filled, and the corresponding preparation method has the characteristics of being simple, controllable and easy to operate.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of low molecular weight polyether ether ketone. Background technique [0002] Polyether ether ketone is an aromatic linear polymer material, a new type of semi-crystalline aromatic thermoplastic engineering plastic successfully researched and developed in the late 1970s. It has high temperature resistance, chemical corrosion resistance, high strength and high modulus. Physical and chemical properties such as weight, high fracture toughness and excellent dimensional stability. The glass transition temperature (Tg) of polyetheretherketone is 143°C, the melting point (Tm) is 334°C, and the maximum attainable crystallinity is 48%, generally 20% to 30%. Its density in the amorphous state is 1.265g / cm 3 , the density at the maximum crystallinity is 1.32g / cm 3 . Its crystalline form makes it have outstanding heat resistance and mechanical p...

Claims

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Application Information

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IPC IPC(8): C08G65/48C08G65/40
CPCC08G65/48C08G65/4012C08G65/4093
Inventor 侯倩倩郑素萍宋磊李胜凯董雅卓毛如增许峰张文申冀克俭
Owner SHANDONG NON METALLIC MATERIAL RES INST