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Method for preparing benzoxazole functionalized graphene hybrid materials

A benzoxazole-based, functionalized technology, applied in the direction of fibrous fillers, etc., can solve the problems of preparing composite materials, no benzoxazole-based hybrid materials, and inability to disperse, and achieve excellent performance

Active Publication Date: 2013-04-10
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004]However, polybenzoxazole polymers (PBZs) have very good chemical stability, are generally insoluble in water and organic solvents, and can only be used in strong protonic acids dissolving and processing
Studies have also shown that unfunctionalized graphene can only be stably dispersed in neutral or alkaline media, but cannot be uniformly dispersed in acidic media with pH<7.
Therefore, it is impossible to directly use graphene in situ polymerization or blending to prepare polybenzoxazole polymers (PBZs) / graphene (Graphene) composites
[0005] At present, there is no report on the preparation of benzoxazole hybrid materials containing graphene in the existing literature

Method used

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  • Method for preparing benzoxazole functionalized graphene hybrid materials
  • Method for preparing benzoxazole functionalized graphene hybrid materials

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Experimental program
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Effect test

Embodiment 1

[0024] Example 1 (see attached figure 1 )

[0025] The specific steps of the preparation method of the benzoxazole functionalized graphene hybrid material are:

[0026] (1) Prepare single-layer or multi-layer graphite oxide from natural graphite according to the prior art chemical oxidation method (the document is: J. Am. Chem. Soc., 1958, 80, 1339);

[0027] (2) Under the condition of 70 ℃, under the protection of nitrogen, the monolayer graphite oxide obtained in step (1) was reacted with excess thionyl chloride and a small amount of catalyst DMF for 24 hours, and then the excess thionyl chloride was distilled off, Acyl chlorinated graphite oxide (GO-Cl);

[0028] (3) Silylation of 4,6-diaminoresorcinol hydrochloride (4.8 mmol) with N,O-bistrimethylsilylacetamide (10 mmol), and then with terephthaloyl chloride (4.0 mmol) was polycondensed using an ice-water bath at 0 °C to obtain amino-terminated silylated hydroxyamides (SiMe 3 -PHA);

[0029] (4) Mix 50 mg of the aci...

Embodiment 2

[0033] The specific steps of the preparation method of the benzoxazole functionalized graphene hybrid material are:

[0034] (1) (same as embodiment 1);

[0035] (2) (same as embodiment 1);

[0036] (3) Use N,O-bistrimethylsilylacetamide (10mmol) to silanize 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (4.8 mmol), and then react with p-benzene Diformyl chloride (4.0 mmol) was subjected to polycondensation at 0 °C to obtain amino-terminated silylated hydroxyamides (SiMe 3 -6FPHA);

[0037] (4) GO-Cl (50 mg) obtained in step (2) and SiMe obtained in step (3) 3 -6FPHA (0.53 mmol amino equivalent) was blended in anhydrous DMF, sonicated for 30 min and reacted at 60 °C for 72 hours in a nitrogen atmosphere;

[0038] (5) Pour the reaction solution into the mixed solution of water and methanol with a mixing ratio of 1:1, filter with a 0.22 μm membrane, and repeat the following operations for the obtained filter cake three times: ultrasonically dissolve with DMF, mix with wat...

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Abstract

The invention relates to a method for preparing benzoxazole functionalized graphene hybrid materials, which comprises the steps of: preparation of graphene oxide, synthesis of a polybenzoxazole polymer with a two-step method, preparation of a polybenzoxazole polymer functionalized graphene and the like. The preparation method disclosed by the invention has the positive effects of successfully preparing the benzoxazole functionalized graphene hybrid materials which are interlinked by amido bonds by means of condensation and thermal reduction of acyl chloride and amino, solving the problem on the uniform scattering of graphene in acid media with pH of smaller than 7, and laying the foundation for further preparation of graphene benzoxazole composite materials with stable homogeneous phase and excellent performance.

Description

technical field [0001] The invention relates to a preparation method of acid-soluble graphene and benzoxazole functionalized graphene hybrid material. Background technique [0002] With polyphenylene benzobisoxazole [Poly( p -phenylene-2,6-benzobisoxazole), PBO] represented polybenzoxazole polymers (PBZs) are lyotropic liquid crystal polymers. Due to the unique rigid rod-like and aromatic heterocyclic fully conjugated structure of polybenzoxazole polymers (PBZs) molecules, the spun polybenzoxazole polymers (PBZs) fibers have high strength, high modulus, high temperature resistance, Environmental and chemical stability are high, its tensile strength is 5.8GPa, and tensile modulus is 280GPa, twice that of Kevlar fiber respectively. In addition, it also has excellent thermal stability (thermal decomposition temperature as high as 650 ° C), good electron transport and third-order nonlinear optical coefficient, and is currently recognized as the organic polymer fiber material w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/06C08L79/04C08K3/04C09C1/46
Inventor 庄启昕刘熙龙陈一王丹谢众韩哲文
Owner EAST CHINA UNIV OF SCI & TECH
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