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Preparation method of graphene modified polyester composite material based on liquid phase stripping

A polyester composite material and graphene modification technology, which is applied in the direction of graphene, chemical instruments and methods, carbon compounds, etc., can solve the problems of complex graphene preparation process, poor graphene integrity, and unfavorable performance. Stability and integrity, prevention of secondary agglomeration, high stability and integrity effects

Inactive Publication Date: 2020-08-28
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention aims to overcome the problems of poor integrity and easy agglomeration of graphene in graphene-modified polyester composite materials in the prior art, and provides a method for preparing graphene-modified polyester composite materials based on liquid phase exfoliation , the method uses graphene-modified polyester composite material exfoliated in liquid phase, which overcomes the shortcomings of complex graphene preparation process, possible environmental pollution, and unfavorable performance, and reduces the agglomeration phenomenon of graphene after liquid phase exfoliation , improve the stability and integrity of graphene, make the physical and chemical properties of graphene better, further increase the uniform dispersion of graphene in the modified polyester composite material, and make the performance of the final product graphene polyester fiber Durable, high wash resistance

Method used

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  • Preparation method of graphene modified polyester composite material based on liquid phase stripping
  • Preparation method of graphene modified polyester composite material based on liquid phase stripping

Examples

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Embodiment 1

[0041] A method of graphene-modified polyester nanocomposite based on liquid phase exfoliation, comprising the following preparation steps:

[0042] 1) Take by weighing 7.68g expanded graphite and join in 396g ethylene glycol solution, then add 7.68g polyhydroxyglucose as dispersant, in ultrasonic cell breaker, ultrasonic 2h under the ultrasonic power of 1620W, obtain graphene dispersion liquid;

[0043] 2) Weigh 664g terephthalic acid, 0.172g titanium silica sol catalyst (titanium element content is 4ppm) and mix with graphene dispersion liquid, under pressure is 0.3Mpa, and temperature is 230 ℃ to carry out esterification reaction, until steamed The water reaches the theoretical value of 144g. Then, the temperature was raised to about 260° C., and the polycondensation reaction was carried out for 2.5 hours under a vacuum condition of 10 Pa to finally obtain a graphene polyester nanocomposite material.

Embodiment 2

[0045] 1) Take by weighing 3.84g expanded graphite and join in 372g ethylene glycol solution, then add 7.68g polyhydroxyglucose as dispersant, in ultrasonic cell breaker, ultrasonic 4h under the ultrasonic power of 1440W, obtain graphene dispersion liquid;

[0046] 2) Weigh 776g dimethyl terephthalate, 0.344g titanium silica sol catalyst (titanium element content is 8ppm) and mix with graphene dispersion liquid, carry out transesterification reaction at the temperature of 210 ℃, until the distilled methanol reaches The theoretical value is 256g. Then, the temperature was raised to about 265° C., and the polycondensation reaction was carried out for 2.7 hours under a vacuum condition of 20 Pa to finally obtain a graphene polyester nanocomposite material.

[0047] The difference with Example 1 is that Example 2 is a DMT transesterification method, while Example 1 is a PTA direct esterification method. Example 1 is easier to industrialize, and has no methanol generation, and the ...

Embodiment 3

[0049] 1) Take by weighing 0.768g expanded graphite and join in 372g ethylene glycol solution, then add 7.68g quinic acid as dispersant, in ultrasonic cell breaker, ultrasonic 2h under the ultrasonic power of 1080W, obtain graphene dispersion liquid;

[0050] 2) Weigh 776g of dimethyl terephthalate, 0.192g of ethylene glycol antimony catalyst and mix them with the graphene dispersion, and carry out transesterification reaction at a temperature of 170°C until the distilled methanol reaches a theoretical value of 256g. Then, the temperature was raised to about 270° C., and the polycondensation reaction was carried out for 2.5 hours under a vacuum condition of 20 Pa to finally obtain a graphene polyester nanocomposite material.

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Abstract

The invention relates to the technical field of graphene composite material preparation, aims at the problems in the prior art that graphene in a graphene modified polyester composite material is poorin integrity and prone to agglomeration, and discloses a preparation method of a graphene modified polyester composite material based on liquid phase stripping. The preparation method comprises the following steps: taking a graphite derivative as a raw material, dispersing the graphite derivative in an organic solvent, adding a dispersing agent, and preparing a graphene dispersion liquid under the ultrasonic-assisted action; mixing the graphene dispersion liquid with a polyester monomer and a catalyst, and performing esterification reaction and condensation polymerization to obtain the graphene polyester nano composite material. According to the method, a liquid-phase stripped graphene modified polyester composite material is adopted, the agglomeration phenomenon of the graphene after liquid phase stripping is reduced, the stability and integrity of the graphene are improved, the physical and chemical properties of the graphene are relatively strong, the uniform dispersity of the graphene in the modified polyester composite material is further improved, and the finally obtained product graphene polyester fiber is durable in performance and high in washing resistance.

Description

technical field [0001] The invention relates to the technical field of preparation of graphene composite materials, in particular to a preparation method of graphene-modified polyester composite materials based on liquid phase exfoliation. Background technique [0002] Graphene is a two-dimensional carbon nanomaterial with honeycomb hexagonal lattice structure, which has excellent physical and chemical properties. In the field of textiles, according to research, graphene plays a leading or synergistic role in the multifunctionality of fibers, and can endow chemical fibers with antistatic, far-infrared, flame-retardant, antibacterial, and anti-ultraviolet properties. Therefore, the development of graphene functional fibers has become a research hotspot for scholars and experts in the textile field. At present, the preparation methods of graphene polyester fibers mainly include in-situ polymerization, melt blending and finishing. For functional graphene polyester fibers prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78C08K3/04C01B32/19C01B32/194
CPCC08G63/183C08G63/78C08K3/042C01B32/19C01B32/194C08K2201/011
Inventor 池玉玲孙妍妍徐伟成
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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