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Preparation method of graphene/thermotropic liquid crystal wholly aromatic polyester composite material

A technology of fully aromatic polyester and composite materials, applied in the manufacture of conductive/antistatic filaments, single-component polyester artificial filaments, etc., can solve the problems of poor dispersion and achieve good electrical conductivity and mechanical properties Effect

Active Publication Date: 2013-10-02
WUHAN TEXTILE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] For the deficiencies in the prior art, the object of the present invention is to overcome the simple mixing of graphene and most polymers will show the problem of poor dispersion, utilize the naphthalene ring structure of 6-hydrocarbyl-2-naphthoic acid and graphene oxide The π-π interaction of 6-hydrocarbyl-2-naphthoic acid non-covalent bond modified graphene oxide is obtained, and then the modified graphene oxide is added to the polymerization reaction system for polycondensation, graphene oxide is fully aromatic Graphene is generated by thermal reduction during the polycondensation process of polyester monomers, thereby preparing graphene / thermotropic liquid crystal wholly aromatic polyester composite materials. In order to achieve the above goals, the technical solution is:

Method used

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preparation example Construction

[0018] Described preparation method comprises the following steps:

[0019] a Graphite pre-oxidation: Take 30ml of concentrated sulfuric acid and add it to a 500ml three-necked flask, then weigh 5g of potassium persulfate and slowly add it to the concentrated sulfuric acid, then add 5g of phosphorus pentoxide, raise the temperature to 80°C, and then add 3g of Graphite powder was reacted for 6 hours. After the reaction was completed, it was filtered and washed until no sulfate ions were detected, and then baked in a vacuum oven at 60°C for 3 hours to obtain pre-oxidized graphene. Secondary oxidation of preoxidized graphene: Measure 200ml of concentrated sulfuric acid and add it to a 500ml three-neck flask, place it in an ice bath at 0°C, slowly add preoxidized graphene, and then slowly add 30g of potassium permanganate , raise the temperature to 35°C for 3h, then raise the temperature to 95°C and stir for 15min, then add the reaction solution and transfer it to a 1000ml beaker,...

Embodiment 1

[0026]The first step: pre-oxidation, take 30ml of concentrated sulfuric acid and add it to a 500ml three-necked flask, then weigh 5g of potassium persulfate and slowly add it to the concentrated sulfuric acid, then add 5g of phosphorus pentoxide, heat up to 80°C, and then add 3g of graphite powder, reacted for 6h, filtered and washed after the reaction, and then baked in a 60°C vacuum oven for 3h to obtain pre-oxidized graphene; for secondary oxidation, measure 200ml of concentrated sulfuric acid and add it to a 500ml three-necked flask. In an ice bath at 0°C, slowly add pre-oxidized graphene, then add 30g of potassium permanganate, raise the temperature to 35°C for 3h, then raise the temperature to 95°C and stir for 15min, then add the reaction solution and transfer it to a 1000ml beaker Add 600ml of deionized water, then add 6ml of 30% hydrogen peroxide, then filter, wash with 10% hydrochloric acid and deionized water to neutral, and then bake in a vacuum oven at 60°C for 3 h...

Embodiment 2

[0028] The first step: pre-oxidation, take 30ml of concentrated sulfuric acid and add it to a 500ml three-necked flask, then weigh 5g of potassium persulfate and slowly add it to the concentrated sulfuric acid, then add 5g of phosphorus pentoxide, heat up to 80°C, and then add 3g of graphite powder, reacted for 6h, filtered and washed after the reaction, and then baked in a 60°C vacuum oven for 3h to obtain pre-oxidized graphene; for secondary oxidation, measure 200ml of concentrated sulfuric acid and add it to a 500ml three-necked flask. In an ice bath at 0°C, slowly add pre-oxidized graphene, then add 30g of potassium permanganate, raise the temperature to 35°C for 3h, then raise the temperature to 95°C and stir for 15min, then add the reaction solution and transfer it to a 1000ml beaker Add 600ml of deionized water, then add 6ml of 30% hydrogen peroxide, then filter, wash with 10% hydrochloric acid and deionized water to neutral, and then bake in a vacuum oven at 60°C for 3 ...

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Abstract

The invention relates to a preparation method of a graphene / thermotropic liquid crystal wholly aromatic polyester composite material. According to the invention, 6-alkyl-2-naphthoic acid non-covalent bond modified graphene oxide is obtained through the pi-pi interaction of the naphthalene ring structure of 6-alkyl-2-naphthoic acid and graphene oxide, and the modified graphene oxide is subjected to hot reduction in the polycondensation process of a wholly aromatic polyester monomer to generate graphene, so that the graphene is uniformly dispersed in the thermotropic liquid crystal wholly aromatic polyester resin, thus overcoming the problems that the graphene is difficult to disperse and the lamellar structure is easy to agglomerate when the graphene is directly blended with the thermotropic liquid crystal wholly aromatic polyester. After being processed into fiber, the prepared composite resin has favorable conductivity and mechanical performance. Tests prove that the composite material has stable mechanical performance, the strength of the fiber formed by spinning the composite material is increased by 60% or so in comparison with the simple thermotropic liquid crystal wholly aromatic polyester, the fiber has favorable conductivity, and the mechanical performance of the fiber is even superior to that of the simple TLCP (thermotropic liquid crystal polymer) fiber.

Description

technical field [0001] The invention relates to a preparation method of a composite material, more specifically a preparation method of a graphene / thermotropic liquid crystal wholly aromatic polyester composite material. Background technique [0002] Graphene is a two-dimensional honeycomb planar film composed of carbon atoms in sp2 hybrid orbitals, with high strength (130GPa), high modulus (1TPa), high specific surface area (2630m2 / g), high thermal conductivity High rate (5000w / (m K)), high charge transport capacity (200000cm2 / g) and many other excellent properties, in aerospace military industry, electromagnetic protection, solar cells, super capacitors, flexible displays, sensors, energy storage, adsorption and catalysis Due to the above properties, graphene has broad application prospects in the field of graphene composite materials, and has been extensively studied by many scholars at home and abroad. [0003] Graphene doping will endow TLCP fibers with excellent elec...

Claims

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Application Information

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IPC IPC(8): C08G63/06C08G63/78C08K9/04C08K9/02C08K3/04D01F6/92D01F1/09
Inventor 王罗新汪志王娟吴静王桦周虎
Owner WUHAN TEXTILE UNIV
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