Preparation method of cyano-modified compounded carbon-based polyaryl ether nitrile composite material

A polyarylene ether nitrile and composite material technology, which is applied in the field of dielectric thin film materials, can solve the problems of rare research on dielectric properties, poor interface compatibility and high dielectric loss, and improve stability and processability. , Good interfacial compatibility, and the effect of improving heat resistance and mechanical properties

Inactive Publication Date: 2018-01-26
DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The surface of graphene oxide is rich in a large number of hydroxyl groups and epoxy groups and a small amount of oxygen-containing functional groups such as carboxyl groups, carbonyl groups, phenol groups, lactones and quinones. The graphene obtained after the reduction of graphene oxide has many properties due to its special structure. Excellent performance, its electron transport speed is 100 times that of silicon, its theoretical specific surface area is as high as 2600㎡ / g, its hardness is greater than that of diamond, and it does not lose its toughness. Therefore, because graphene has high strength, high conductivity and high specific area, It makes the comprehensive performance of graphene-based polymer composites excellent, but at present, graphene is used as a filler, and the research on polyarylether nitrile is rare in terms of dielectric properties.
[0004] Chinese patent CN 105907076A discloses a graphene / polyarylether nitrile composite film and its preparation method. Graphene oxide is uniformly dispersed in N-methylpyrrolidone, polyarylether nitrile is added, and ultrasonically stirred to form a mixed solution. The cast film is obtained by casting film, the solvent is evaporated by heating, and then thermally reduced at high temperature to obtain a graphene / polyarylether nitrile composite film. The film prepared by this method is light in weight and has good interface homogeneity, high conductivity and tensile strength High tensile strength, high dielectric constant, can be used as high dielectric energy storage materials, but in this method, graphene has a very large specific surface area and high surface energy, and it is easy to agglomerate in the polyarylether nitrile matrix, and The interfacial compatibility with the polyarylether nitrile matrix is ​​poor, the bonding fastness is weak, the dielectric loss is high, and the heat resistance is poor. The comprehensive performance of the graphene-based polyarylether nitrile composite film still needs to be improved

Method used

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  • Preparation method of cyano-modified compounded carbon-based polyaryl ether nitrile composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Add 0.2g graphene oxide into 200mL thionyl chloride and stir ultrasonically, under the catalysis of N,N-dimethylformamide, heat and reflux at 60°C for 24h, filter and vacuum dry to obtain acyl chloride graphene , with excess aminophenoxyphthalonitrile and cyano-modified cellulose derivatives, added to toluene solvent, stirred and refluxed at room temperature for 72h, washed and centrifuged and dried to obtain cyano-functionalized graphene / fiber Plain composite material, wherein the content of cellulose is higher than 50wt%.

[0027] (2) Use the cyano-functionalized graphene / cellulose composite material as the carbon source, and use 5wt% ferrocene as the catalyst precursor. Under nitrogen atmosphere, first react at 400°C for 30min, then heat up to 900°C for reaction 5min, high-temperature carbonization to obtain a cyano-functionalized graphene-containing composite carbon material.

[0028] (3) The cyano-functionalized graphene-containing composite carbon material is...

Embodiment 2

[0031] (1) Add 0.3g of graphene oxide into 200mL of thionyl chloride and stir ultrasonically, under the catalysis of N,N-dimethylformamide, heat and reflux at 70°C for 24h, filter and dry in vacuum to obtain acyl chloride graphene , with excess aminophenoxyphthalonitrile and cyano-modified cellulose derivatives, added to toluene solvent, stirred and refluxed at room temperature for 72h, washed and centrifuged and dried to obtain cyano-functionalized graphene / fiber Plain composite material, wherein the content of cellulose is higher than 50wt%.

[0032] (2) Use the cyano-functionalized graphene / cellulose composite material as the carbon source, use 30wt% ferrocene as the catalyst precursor, and react at 450°C for 40min under nitrogen atmosphere, then heat up to 900°C for reaction 15min, high-temperature carbonization to obtain a cyano-functionalized graphene-containing composite carbon material.

[0033] (3) The cyano-functionalized graphene-containing composite carbon materia...

Embodiment 3

[0036] (1) Add 0.25g of graphene oxide into 200mL of thionyl chloride and stir ultrasonically, under the catalysis of N,N-dimethylformamide, heat and reflux at 65°C for 24h, filter and vacuum dry to obtain acyl chloride graphene , with excess aminophenoxyphthalonitrile and cyano-modified cellulose derivatives, added to toluene solvent, stirred and refluxed at room temperature for 72h, washed and centrifuged and dried to obtain cyano-functionalized graphene / fiber Plain composite material, wherein the content of cellulose is higher than 50wt%.

[0037] (2) Use the cyano-functionalized graphene / cellulose composite material as a carbon source, and use 10wt% ferrocene as a catalyst precursor. Under a nitrogen atmosphere, first react at 420°C for 35min, then heat up to 900°C for reaction 10min, high-temperature carbonization to obtain a cyano-functionalized graphene-containing composite carbon material.

[0038] (3) The cyano-functionalized graphene-containing composite carbon materi...

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Abstract

The invention provides a preparation method of a cyano-modified compounded carbon-based polyaryl ether nitrile composite material. The preparation method comprises the following steps: adding oxidizedgraphene into thionyl chloride for ultrasonic stirring, performing heating reflux to obtain acylating chlorinated graphene under the catalytic action of N,N-dimethylformamid, adding excessive aminophenoxyl-o-phthalonitrile and cyano-modified cellulose derivatives into a toluene solvent, stirring and reflux at room temperature to obtain cyano functionalized graphene / cellulose composite material, performing high-temperature carbonization to obtained cyano functionalized graphene-containing composite carbon material; and finally adding cross-linkable polyether nitrile-containing N-methyl pyrrolidone solution, heating in water bath, ultrasonically stirring, performing high-speed ball milling to obtain ash black slurry, centrifugally washing and drying to obtain a product. The prepared composite material is superfine powder, and is high-strength and high-temperature-resistant, and excellent in processability, and dielectric thin film materials can be obtained through melting compression and hot drawing, and can be used in the field of electronic devices.

Description

technical field [0001] The invention belongs to the technical field of dielectric film materials, and in particular relates to a preparation method of a cyano-modified composite carbon-based polyarylether nitrile composite material. Background technique [0002] Polyarylether nitrile is a semi-crystalline polyarylether polymer with cyano groups in the side chain and excellent comprehensive performance. Due to its unique chemical structure, polyarylether nitrile has high mechanical strength, flame retardancy, and Thermal and creep resistance and other advantages, as a new type of engineering resin, is expected to have a wide range of applications in the automotive industry, electronics and aerospace and other fields, but there are still deficiencies in polyarylether nitrile, such as dielectric constant Lower etc., these deficiencies cause poly(arylene ether nitrile) to be limited in many fields. Therefore, in order to improve this situation, adding inorganic nanoparticles wi...

Claims

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Application Information

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IPC IPC(8): C08L71/10C08K9/04C08K3/04C08K7/24C08K7/18C08J5/18
Inventor 陈东进
Owner DONGGUAN LIANZHOU INTPROP OPERATION MANAGEMENT CO LTD
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