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Preparation method of graphene-based hyperbranched perylene imide/epoxy composite

A perylene imide and graphene-based technology, applied in the field of hyperbranched polymer modification, can solve the problems of composite materials that have not been reported in the literature, achieve improved mechanical properties and thermal properties, simple synthesis process, and solve the problem of easy aggregation Effect

Active Publication Date: 2015-09-09
绍兴盖诺超菱润滑材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Composite materials prepared by this method have not been reported in the literature

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] (1) Weigh 0.1g of carboxyl-terminated peryleneimide (PBI-COOH), 20ml of N,N′-dimethylformamide and 5ml of aqueous sodium hydride solution (15% by mass), and mix and stir at 70°C After reacting for 2 hours, slowly add 2ml of glycidyl alcohol dropwise, continue the reaction for 10 hours, then precipitate, filter, and dry the precipitate to obtain hyperbranched perylene imide, which is PBI-HPG.

[0021] (2) Weigh 0.05g of graphene treated by high-temperature reduction, disperse it in 8ml of N,N'-dimethylformamide and ultrasonically disperse it for 5h to prepare a mixed solution, then add 0.5g of step (1 ) prepared PBI-HPG, and reacted at 100°C for 20h, and then centrifuged, and the resulting product was dried at 60°C to obtain a graphene-based hyperbranched perylene imide, which is PBI-HPG-g-RGO .

[0022] (3) Add 0.026g of the PBI-HPG-g-RGO prepared in step (2) to 26g of epoxy resin, decompress and pump air, then add 7.8g of curing agent 4,4'-diaminodiphenylsulfone, Aft...

Embodiment 2

[0025] (1) Weigh 0.5g of carboxyl-terminated peryleneimide (PBI-COOH), 20ml of N,N′-dimethylformamide and 5ml of sodium hydride aqueous solution (mass percent concentration: 15%), mix and stir at 70°C After reacting for 2 hours, slowly add 3ml glycidol dropwise, continue to react for 12 hours, then precipitate, filter, and dry the precipitate to obtain hyperbranched perylene imide, which is PBI-HPG.

[0026] (2) Weigh 0.07g graphene after high-temperature reduction treatment, disperse it in 8ml N,N'-dimethylformamide and ultrasonically disperse it for 5h to prepare a mixed solution, then add 0.7g step (1 ) prepared PBI-HPG, reacted at 100°C for 20h, and centrifuged again, and dried the obtained product at 60°C to obtain graphene-based hyperbranched perylene imide, which is PBI-HPG-g-RGO .

[0027] (3) Take 0.042g of PBI-HPG-g-RGO prepared in step (2) and add it to 26g of epoxy resin, depressurize and pump air, then add 7.8g of curing agent 4,4'-diaminodiphenyl sulfone, After...

Embodiment 3

[0030](1) Weigh 0.8g of carboxyl-terminated peryleneimide (PBI-COOH), 30ml of N,N′-dimethylformamide and 5ml of sodium hydride aqueous solution (mass percent concentration: 15%), mix and stir at 70°C After reacting for 2 hours, slowly add 3ml glycidol dropwise, continue to react for 12 hours, then precipitate, filter, and dry the precipitate to obtain hyperbranched perylene imide, which is PBI-HPG.

[0031] (2) Weigh 0.07g graphene after high-temperature reduction treatment, disperse it in 8ml N,N'-dimethylformamide and ultrasonically disperse it for 5h to prepare a mixed solution, then add 0.8g step (1 ) prepared PBI-HPG, and reacted at 80°C for 24h, then centrifuged, and the resulting product was dried at 60°C to obtain a graphene-based hyperbranched perylene imide, which is PBI-HPG-g-RGO .

[0032] (3) Add 0.05g of the PBI-HPG-g-RGO prepared in step (2) to 26g of epoxy resin, depressurize and pump air, then add 7.8g of curing agent 4,4'-diaminodiphenylsulfone, After mixin...

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Abstract

The invention discloses a preparation method of a graphene-based hyperbranched perylene imide / epoxy composite. The preparation method comprises the steps of reacting carboxyl-terminated perylene bisimide, N, N'-dimethylformamide and an alkaline solution for 1-3 hours while stirring at the temperature of 70-100 DEG C, then, dropwise adding glycidol, reacting for 8-12 hours, then, settling, filtering, and drying the sediment to obtain hyperbranched perylene imide; ultrasonically dispersing high-temperature reduced graphene into N, N'-dimethylformamide for 5-6 hours, then, adding hyperbranched perylene imide, reacting at the temperature of 80-100 DEG C for 20-24 hours, then, carrying out centrifugal separation to obtain a product, drying the product at the temperature of 60 DEG C to obtain graphene-based hyperbranched perylene imide, adding graphene-based hyperbranched perylene imide into epoxy resin, and pouring graphene-based hyperbranched perylene imide into a die to cure and mold by taking 4, 4'-diaminodiphenyl sulfone as a curing agent to obtain the graphene-based hyperbranched perylene imide / epoxy composite. The preparation method disclosed by the invention is simple in process, low in production cost, little in pollution and wide in applicability.

Description

technical field [0001] The invention belongs to the technical field of hyperbranched polymer modification, and in particular relates to a preparation method of a graphene-based hyperbranched peryleneimide / epoxy composite material. Background technique [0002] Since Friedlander synthesized peryleneimide in 1913, peryleneimide derivatives have attracted much attention as a kind of dye and optical material in the fields of n-type semiconductors, organic optoelectronic devices and supramolecular assembly. On the one hand, this is mainly because peryleneimides have the advantages of good light and thermal stability, chemical resistance and high fluorescence quantum yield; on the other hand, because peryleneimides have a large co-benzene ring , can be π-π stacked with other molecules that also have a conjugated structure through non-covalent forces, thereby forming a supramolecular structure, making it widely used in supramolecular assembly. However, the solubility of peryleneim...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K9/04C08K3/04
Inventor 陆绍荣潘露露虞锦洪杨瑾罗启云徐旭
Owner 绍兴盖诺超菱润滑材料有限公司
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